Section 2.2-1105 of the Code of Virginia directs the Division
of Consolidated Laboratory Services to establish a program to certify
environmental laboratories that perform tests, analyses, measurements or monitoring
required pursuant to the Commonwealth's air, waste and water laws and
regulations. This chapter sets out the required standards and the process by
which owners of noncommercial environmental laboratories may obtain
certification for their laboratories.
1VAC30-46 covers commercial
environmental laboratories and NELAP-accredited environmental laboratories
seeking reciprocal accreditation in Virginia.
A. This chapter applies to any owner of a noncommercial environmental laboratory.
B. Any environmental laboratory owned by an agency of the federal government may be certified as follows:
DGS-DCLS DCLS to the standards set out in
this chapter; or
2. By a federal primary
accrediting authority accreditation
body to the standards established by the National Environmental
Laboratory Accreditation Conference TNI.
C. Citizen monitoring groups. Section 62.1-44.19:11 of the
Code of Virginia both establishes a citizen water quality monitoring program
for Virginia and encourages the growth of the program. The Department of
Environmental Quality (DEQ) has a separate program of quality assurance and
quality control (QA/QC) standards for citizen monitoring groups and their
laboratories to follow. The following laboratories shall meet the [
DEQ ] QA/QC requirements developed for the purposes of citizen
monitoring of water quality in lieu of the requirements of 1VAC30-45 or
1. Laboratories owned by citizen monitoring groups.
2. Laboratories at institutions of higher education affiliated with citizen monitoring groups for the purposes of analyzing samples for the groups.
Environmental research performed by environmental
laboratories owned by institutions of higher education. Institutions of
higher education. Environmental laboratories owned by institutions of
higher education located in Virginia that perform analyses for the purpose of
providing environmental research data to DEQ at DEQ's request shall meet the
QA/QC requirements specified by DEQ. An environmental laboratory owned by an
institution of higher education located in Virginia that performs environmental
research for DEQ shall not be subject to the requirements of either 1VAC30-45
or 1VAC30-46 unless DEQ requires the laboratory to do so.
Where a term is defined in this section, the term shall
have no other meaning, even if it is defined differently in the Code of
Virginia or another regulation of the Virginia Administrative Code. Unless specifically
defined in this section, the terms used in this chapter shall have the meanings
commonly ascribed to them by recognized authorities. The following words
and terms when used in this chapter shall have the following meanings unless
the context clearly indicates otherwise.
"Acceptance criteria" means specified limits placed on characteristics of an item, process, or service defined in requirement documents.
"Accuracy" means the degree of agreement between an observed value and an accepted reference value. Accuracy includes a combination of random error (precision) and systematic error (bias) components that are due to sampling and analytical operations. Accuracy is an indicator of data quality.
"Algae" means simple single-celled, colonial, or multicelled, mostly aquatic plants, containing chlorophyll and lacking roots, stems and leaves that are either suspended in water (phytoplankton) or attached to rocks and other substrates (periphyton).
"Aliquot" means a portion of a sample taken for analysis.
"Analyte" means the substance or physical property to be determined in samples examined.
"Analytical method" means a technical procedure for providing analysis of a sample, defined by a body such as the Environmental Protection Agency or the American Society for Testing and Materials, that may not include the sample preparation method.
"Assessment" means the evaluation process used to measure or establish the performance, effectiveness, and conformance of an organization and its systems or both to defined criteria.
"Assessor" means the person
who performs on-site
assessments of laboratories' capability and capacity for meeting the
requirements under this chapter by examining the records and other physical
evidence for each one of the tests for which certification has been requested
assigned by DCLS to perform, alone or as part of an assessment team, an
assessment of an environmental laboratory.
"Audit" means a systematic evaluation to determine the conformance to quantitative and qualitative specifications of some operational function or activity.
"Authority" means, in the context of a governmental body or local government, an authority created under the provisions of the Virginia Water and Waste Authorities Act, Chapter 51 (§ 15.2-5100 et seq.) of Title 15.2 of the Code of Virginia.
"Batch" means environmental samples that are prepared together or analyzed together or both with the same process and personnel, using the same lot or lots of reagents. "Analytical batch" means a batch composed of prepared environmental samples (extracts, digestates or concentrates) that are analyzed together as a group. An analytical batch can include prepared samples originating from various environmental matrices and can exceed 20 samples. "Preparation batch" means a batch composed of one to 20 environmental samples of the same matrix that meets the criteria in this definition for "batch" and with a maximum time between the start of processing of the first and last sample in the batch to be 24 hours.
"Benthic macroinvertebrates" means bottom dwelling animals without backbones that live at least part of their life cycles within or upon available substrates within a body of water.
"Blank" means a sample that has not been exposed to the analyzed sample stream in order to monitor contamination during sampling, transport, storage or analysis. The blank is subjected to the usual analytical and measurement process to establish a zero baseline or background value and is sometimes used to adjust or correct routine analytical results. Blanks include the following types:
1. Field blank. A blank prepared in the field by filling a clean container with pure deionized water and appropriate preservative, if any, for the specific sampling activity being undertaken.
2. Method blank. A sample of a matrix similar to the batch of associated samples (when available) that is free from the analytes of interest and is processed simultaneously with and under the same conditions as samples through all steps of the analytical procedures, and in which no target analytes or interferences are present at concentrations that impact the analytical results for sample analyses.
"Calibration" means to determine, by measurement or comparison with a standard, the correct value of each scale reading on a meter, instrument or other device. The levels of the applied calibration standard should bracket the range of planned or expected sample measurements.
"Calibration curve" means the graphical relationship between the known values, such as concentrations, of a series of calibration standards and their instrument response.
"Calibration standard" means a substance or reference material used to calibrate an instrument.
"Certified reference material" means a reference material one or more of whose property values are certified by a technically valid procedure, accompanied by or traceable to a certificate or other documentation that is issued by a certifying body.
"Client" or "customer" means the Department of Environmental Quality (DEQ) when used in the context of quality assurance and specific quality control provisions.
"Commercial environmental laboratory" means an environmental laboratory where environmental analysis is performed for another person.
"Corrective action" means the action taken to eliminate the causes of an existing nonconformity, defect or other undesirable situation in order to prevent recurrence.
"DGS-DCLS" "DCLS" means the
Division of Consolidated Laboratory Services of the Department of General
"Demonstration of capability" means the procedure to establish the ability of the analyst to generate data of acceptable accuracy and precision.
"Detection limit" means the lowest concentration or amount of the target analyte that can be determined to be different from zero by a single measurement at a stated degree of confidence.
"Environmental analysis" or "environmental analyses" means any test, analysis, measurement, or monitoring used for the purposes of the Virginia Air Pollution Control Law, the Virginia Waste Management Act or the State Water Control Law (§ 10.1-1300 et seq., § 10.1-1400 et seq., and § 62.1-44.2 et seq., respectively, of the Code of Virginia). For the purposes of these regulations, any test, analysis, measurement, or monitoring required pursuant to the regulations promulgated under these three laws, or by any permit or order issued under the authority of any of these laws or regulations is "used for the purposes" of these laws. The term shall not include the following:
1. Sampling of water, solid and chemical materials, biological tissue, or air and emissions.
2. Field testing and measurement of water, solid and chemical materials, biological tissue, or air and emissions, except when performed in an environmental laboratory rather than at the site where the sample was taken.
3. Taxonomic identification of samples for which there is no national accreditation standard such as algae, benthic macroinvertebrates, macrophytes, vertebrates and zooplankton.
4. Protocols used pursuant to § 10.1-104.2 of the Code of Virginia to determine soil fertility, animal manure nutrient content, or plant tissue nutrient uptake for the purposes of nutrient management.
5. Geochemical and permeability testing for solid waste compliance.
6. Materials specification for air quality compliance when product certifications specify the data required by an air permit such as fuel type, Btu content, sulfur content, or VOC content.
"Environmental laboratory" or "laboratory" means a facility or a defined area within a facility where environmental analysis is performed. A structure built solely to shelter field personnel and equipment from inclement weather shall not be considered an environmental laboratory.
"Establishment date" means the date set for the accreditation program under 1VAC30-46 and the certification program to be established under this chapter.
"Establishment of certification program" or
"established program" means that
DGS-DCLS DCLS has
completed the initial accreditation of environmental laboratories covered by
1VAC30-46 and the initial certification of environmental laboratories covered
"Facility" means something that is built or installed to serve a particular function.
"Field of certification" or "FoC"
an approach to certifying laboratories by those matrix,
technology/method, and analyte/analyte group analyte
combinations for which DCLS offers certification.
"Field of proficiency testing" or "FoPT" means analytes for which a laboratory is required to successfully analyze a PT sample in order to obtain or maintain certification, collectively defined as matrix, technology/method, and analyte.
"Field testing and measurement" means any of the following:
1. Any test for parameters under 40 CFR Part 136 for which the holding time indicated for the sample requires immediate analysis; or
2. Any test defined as a field test in federal regulation.
The following is a limited list of currently recognized field
tests or measures that is not intended to be inclusive: continuous emissions
on-line online monitoring; flow monitoring; tests for
pH, residual chlorine, temperature and dissolved oxygen; and field analysis for
"Finding" means an assessment conclusion
identifies a condition having a significant effect on an item or activity. An
assessment finding is normally a deficiency and is normally accompanied by
specific examples of the observed condition. referenced to a laboratory
certification standard and supported by objective evidence that identifies a
deviation from a laboratory certification standard requirement.
"Governmental body" means any department, agency, bureau, authority, or district of the United States government, of the government of the Commonwealth of Virginia, or of any local government within the Commonwealth of Virginia.
(or maximum allowable holding time)"
means the maximum time that a sample may be held prior to analysis and still
be considered valid or not compromised can elapse between two specified
activities. "Initial certification period" means the period
during which DGS-DCLS is accepting and processing applications for the first
time under this chapter as specified in 1VAC30-45-60.
"International System of Units (SI)" means the coherent system of units adopted and recommended by the General Conference on Weights and Measures.
"Laboratory control sample" or "LCS" means a sample matrix, free from the analytes of interest, spiked with verified known amounts of analytes or a material containing known and verified amounts of analytes. It is generally used to establish intra-laboratory or analyst specific precision and bias or to assess the performance of all or a portion of the measurement system. "Laboratory control sample" or "LCS" may also be named laboratory fortified blank, spiked blank, or QC check sample.
"Laboratory manager" means the person who has overall responsibility for the technical operation of the environmental laboratory and who exercises actual day-to-day supervision of laboratory operation for the appropriate fields of testing and reporting of results. The title of this person may include but is not limited to laboratory director, technical director, laboratory supervisor or laboratory manager.
"Legal entity" means an entity, other than a natural person, who has sufficient existence in legal contemplation that it can function legally, be sued or sue, and make decisions through agents as in the case of corporations.
"Limit of detection" or "LOD" means an estimate of the minimum amount of a substance that an analytical process can reliably detect. An LOD is analyte and matrix specific and may be laboratory dependent.
"Limit of quantitation" or "LOQ" means the minimum levels, concentrations, or quantities of a target variable (e.g., target analyte) that can be reported with a specified degree of confidence.
"Local government" means a municipality (city or town), county, sanitation district, or authority.
"Macrophytes" means any aquatic or terrestrial plant species that can be identified and observed with the eye, unaided by magnification.
"Matrix" means the component or substrate that may contain the analyte of interest. A matrix can be a field of certification matrix or a quality system matrix.
1. Field of certification matrix. These matrix definitions shall be used when certifying a laboratory.
Non-potable Nonpotable water. Any aqueous
sample that has not been designated a potable or potential potable water
source. Includes surface water, groundwater, effluents, water treatment
chemicals, and TCLP or other extracts.
b. Solid and chemical materials. Includes soils, sediments, sludges, products and byproducts of an industrial process that results in a matrix not previously defined.
c. Biological tissue. Any sample of a biological origin such as fish tissue, shellfish, or plant material. Such samples shall be grouped according to origin.
d. Air and emissions. Whole gas or vapor samples including those contained in flexible or rigid wall containers and the extracted concentrated analytes of interest from a gas or vapor that are collected with a sorbent tube, impinger solution, filter or other device.
2. Quality system matrix. For purposes of batch and quality control requirement determinations, the following matrix types shall be used:
a. Drinking water. Any aqueous sample that has been designated a potable or potential potable water source.
b. Aqueous. Any aqueous sample excluded from the definition of drinking water matrix or saline/estuarine source. Includes surface water, groundwater, effluents, and TCLP or other extracts.
c. Saline/estuarine. Any aqueous sample from an ocean or estuary, or other salt water source.
d. Nonaqueous liquid. Any organic liquid with less than 15% settleable solids.
e. Biological tissue. Any sample of a biological origin such as fish tissue, shellfish, or plant material. Such samples shall be grouped according to origin.
f. Solids. Includes soils, sediments, sludges and other matrices with more than 15% settleable solids.
g. Chemical waste. A product or
of an industrial process that results in a matrix not previously defined.
h. Air and emissions. Whole gas or vapor samples including those contained in flexible or rigid wall containers and the extracted concentrated analytes of interest from a gas or vapor that are collected with a sorbent tube, impinger solution, filter or other device.
"Matrix spike (spiked sample or fortified sample)" means a sample prepared by adding a known mass of target analyte to a specified amount of matrix sample for which an independent estimate of target analyte concentration is available. Matrix spikes are used, for example, to determine the effect of the matrix on a method's recovery efficiency.
"Matrix spike duplicate (spiked sample or fortified sample duplicate)" means a second replicate matrix spike prepared in the laboratory and analyzed to obtain a measure of the precision of the recovery for each analyte.
"National Environmental Laboratory Accreditation
Conference (NELAC)" means a voluntary organization of state and federal
environmental officials and interest groups with the primary purpose to
establish mutually acceptable standards for accrediting environmental
A subset of NELAP. "National Environmental Laboratory Accreditation
Program (NELAP)" means the overall National Environmental Laboratory
Accreditation Program of which NELAC is a part.
"National Institute of Standards and Technology" or "NIST" means an agency of the U.S. Department of Commerce's Technology Administration that is working with EPA, states, NELAC, and other public and commercial entities to establish a system under which private sector companies and interested states can be certified by NIST to provide NIST-traceable proficiency testing (PT) samples.
"Negative control" means measures taken to ensure that a test, its components, or the environment do not cause undesired effects, or produce incorrect test results.
"Noncommercial environmental laboratory" means either of the following:
1. An environmental laboratory where environmental analysis is performed solely for the owner of the laboratory.
2. An environmental laboratory where the only performance of environmental analysis for another person is one of the following:
a. Environmental analysis performed by an environmental laboratory owned by a local government for an owner of a small wastewater treatment system treating domestic sewage at a flow rate of less than or equal to 1,000 gallons per day.
b. Environmental analysis performed by an environmental laboratory operated by a corporation as part of a general contract issued by a local government to operate and maintain a wastewater treatment system or a waterworks.
c. Environmental analysis performed by an environmental laboratory owned by a corporation as part of the prequalification process or to confirm the identity or characteristics of material supplied by a potential or existing customer or generator as required by a hazardous waste management permit under 9VAC20-60.
d. Environmental analysis performed by an environmental laboratory owned by a Publicly Owned Treatment Works (POTW) for an industrial source of wastewater under a permit issued by the POTW to the industrial source as part of the requirements of a pretreatment program under Part VII (9VAC25-31-730 et seq.) of 9VAC25-31.
e. Environmental analysis performed by an environmental laboratory owned by a county authority for any municipality within the county's geographic jurisdiction when the environmental analysis pertains solely to the purpose for which the authority was created.
f. Environmental analysis performed by an environmental laboratory owned by an authority or a sanitation district for any participating local government of the authority or sanitation district when the environmental analysis pertains solely to the purpose for which the authority or sanitation district was created.
"Owner" means any person who owns, operates, leases or controls an environmental laboratory.
"Person" means an individual, corporation, partnership, association, company, business, trust, joint venture or other legal entity.
"Physical," for the purposes of fee test categories, means the tests to determine the physical properties of a sample. Tests for solids, turbidity and color are examples of physical tests.
"Positive control" means measures taken to ensure that a test or its components are working properly and producing correct or expected results from positive test subjects.
"Precision" means the degree to which a set of observations or measurements of the same property, obtained under similar conditions, conform to themselves. Precision is an indicator of data quality. Precision is expressed usually as standard deviation, variance or range, in either absolute or relative terms.
accrediting authority accreditation
body" means the agency or department designated at the territory,
state or federal level as the recognized authority with the responsibility and
accountability for granting NELAC accreditation to a specific laboratory for a
specific field of accreditation body responsible for assessing a laboratory's
total quality system, on-site assessment, and PT performance tracking for
fields of accreditation.
"Proficiency test or testing (PT)" means evaluating a laboratory's performance under controlled conditions relative to a given set of criteria through analysis of unknown samples provided by an external source.
"Proficiency test (PT) field of testing" means
the approach to offer proficiency testing by maxtrix, technology/method, and
"Proficiency test (PT) sample" means a sample, the
composition of which is unknown to
both the analyst and the laboratory and
is provided to test whether the analyst or laboratory or both laboratory
can produce analytical results within specified acceptance criteria.
"Proficiency testing (PT) program" means the aggregate of providing rigorously controlled and standardized environmental samples to a laboratory for analysis, reporting of results, statistical evaluation of the results and the collective demographics and results summary of all participating laboratories.
"Program," in the context of a regulatory program, means the relevant U.S. Environmental Protection Agency program such as the water program under the Clean Water Act (CWA), the air program under the Clean Air Act (CAA), the waste program under the Comprehensive Environmental Response, Compensation and Liability Act (CERCLA or Superfund) or the waste program under the Resource Conservation and Recovery Act (RCRA).
"Publicly Owned Treatment Works (POTW)" means a treatment works as defined by § 212 of the CWA, which is owned by a state or municipality (as defined by § 502(4) of the CWA). This definition includes any devices and systems used in the storage, treatment, recycling, and reclamation of municipal sewage or industrial wastes of a liquid nature. It also includes sewers, pipes, and other conveyances only if they convey wastewater to a POTW treatment plant. The term also means the municipality as defined in § 502(4) of the CWA, which has jurisdiction over the indirect discharges to and the discharges from such a treatment works.
"Quality assurance" or "QA" means
an integrated system of management activities involving planning,
control, quality implementation, assessment, reporting and quality
improvement to ensure that a product process, item, or service meets
defined standards of quality with a stated level of confidence is of the
type and quality needed and expected by the client.
"Quality assurance officer" means the person who has responsibility for the quality system and its implementation. Where staffing is limited, the quality assurance officer may also be the laboratory manager.
"Quality control" or "QC" means the
overall system of technical activities
whose purpose is to measure and
control the quality of a product or service so that it meets the needs of users
that measures the attributes and performance of a process, item, or service
against defined standards to verify that they meet the stated requirements
established by the customer; operational techniques and activities that are
used to fulfill requirements for quality; and also the system of activities and
checks used to ensure that measurement systems are maintained within prescribed
limits, providing protection against "out of control" conditions and
ensuring that the results are of acceptable quality.
"Quality manual" means a document stating the management policies, objectives, principles, organizational structure and authority, responsibilities, accountability, and implementation of an agency, organization, or laboratory, to ensure the quality of its product and the utility of its product to its users.
"Quality system" means a structured and documented management system describing the policies, objectives, principles, organizational authority, responsibilities, accountability, and implementation plan of an organization for ensuring quality in its work processes, products (items), and services. The quality system provides the framework for planning, implementing, and assessing work performed by the organization and for carrying out required quality assurance and quality control activities.
"Range" means the difference between the minimum and maximum of a set of values.
"Reference material" means a material or substance one or more properties of which are sufficiently well established to be used for the calibration of an apparatus, the assessment of a measurement test method, or for assigning values to materials.
"Reference standard" means a standard, generally of the highest metrological quality available at a given location, from which measurements made at that location are derived.
"Responsible official" means one of the following, as appropriate:
1. If the laboratory is owned or operated by a private corporation, "responsible official" means (i) a president, secretary, treasurer, or a vice-president of the corporation in charge of a principal business function, or any other person who performs similar policy-making or decision-making functions for the corporation or (ii) the manager of one or more manufacturing, production, or operating facilities employing more than 250 persons or having gross annual sales or expenditures exceeding $25 million (in second-quarter 1980 dollars), if authority to sign documents has been assigned or delegated in accordance with corporate procedures.
2. If the laboratory is owned or operated by a partnership, association, or a sole proprietor, "responsible official" means a general partner, officer of the association, or the proprietor, respectively.
3. If the laboratory is owned or operated by a governmental body, "responsible official" means a director or highest official appointed or designated to oversee the operation and performance of the activities of the environmental laboratory.
4. Any person designated as the responsible official by an
individual described in subdivision 1, 2 or 3 of this definition, provided the
designation is in writing, the designation specifies an individual or position
with responsibility for the overall operation of the environmental laboratory,
and the designation is submitted to
"Sampling" means the act of collection for the purpose of analysis.
"Sanitation district" means a sanitation district created under the provisions of Chapters 3 (§ 21-141 et seq.) through 5 (§ 21-291 et seq.) of Title 21 of the Code of Virginia.
"Sewage" means the water-carried human wastes from residences, buildings, industrial establishments or other places together with such industrial wastes and underground, surface, storm, or other water as may be present.
"Simple test procedures" or "STP" means any of the following:
1. Field testing and measurement performed in an environmental laboratory.
2. The test procedures to determine:
a. Biochemical oxygen demand (BOD) or carbonaceous BOD (CBOD);
b. Fecal coliform;
c. Total coliform;
d. Fecal streptococci;
e. E. coli;
g. Settleable solids (SS);
h. Total dissolved solids (TDS);
i. Total solids (TS);
j. Total suspended solids (TSS);
k. Total volatile solids (TVS); and
l. Total volatile suspended solids (TVSS).
"Standard operating procedure
"SOP" means a written document that details the method of an
operation, analysis or action whose techniques and procedures are thoroughly
prescribed and which is accepted for an operation, analysis, or action
with thoroughly prescribed techniques and steps. An SOP is officially approved
as the method for performing certain routine or repetitive tasks.
"Standardized reference material
"SRM" means a certified reference material produced by the U.S.
National Institute of Standards and Technology or other equivalent organization
and characterized for absolute content, independent of analytical method.
"System laboratory" means a noncommercial laboratory that analyzes samples from multiple facilities having the same owner.
"TCLP" or "toxicity characteristic leachate
procedure" means Test Method 1311 in "Test Methods for Evaluating
Solid Waste, Physical/Chemical Methods," EPA Publication SW-846, as
incorporated by reference in 40 CFR 260.11. This method is used to determine
whether a solid waste exhibits the characteristic of toxicity (see 40 CFR
"Test" means a technical operation that consists of the determination of one or more characteristics or performance of a given product, material, equipment, organism, physical phenomenon, process or service according to a specified procedure.
"Test, analysis, measurement or monitoring required pursuant to the Virginia Air Pollution Control Law" means any method of analysis required by the Virginia Air Pollution Control Law (§ 10.1-1300 et seq.); by the regulations promulgated under this law (9VAC5) including any method of analysis listed either in the definition of "reference method" in 9VAC5-10-20, or listed or adopted by reference in 9VAC5; or by any permit or order issued under and in accordance with this law and these regulations.
"Test, analysis, measurement or monitoring required pursuant to the Virginia Waste Management Act" means any method of analysis required by the Virginia Waste Management Act (§ 10.1-1400 et seq.); by the regulations promulgated under this law (9VAC20), including any method of analysis listed or adopted by reference in 9VAC20; or by any permit or order issued under and in accordance with this law and these regulations.
"Test, analysis, measurement or monitoring required pursuant to the Virginia Water Control Law" means any method of analysis required by the Virginia Water Control Law (§ 62.1-44.2 et seq.); by the regulations promulgated under this law (9VAC25), including any method of analysis listed or adopted by reference in 9VAC25; or by any permit or order issued under and in accordance with this law and these regulations.
"Test method" means an adoption of a scientific technique for performing a specific measurement as documented in a laboratory standard operating procedure or as published by a recognized authority.
"The NELAC Institute" or "TNI" means the organization whose standards environmental laboratories must meet to become accredited under 1VAC30-46, the regulation governing commercial environmental laboratories in Virginia.
"Toxicity characteristic leachate procedure" or "TCLP" means Test Method 1311 in "Test Methods for Evaluating Solid Waste, Physical/Chemical Methods," EPA Publication SW-846, as incorporated by reference in 40 CFR 260.11. This method is used to determine whether a solid waste exhibits the characteristic of toxicity (see 40 CFR 261.24).
"Traceability" means the property of a result of a measurement whereby it can be related to appropriate standards, generally international or national standards, through an unbroken chain of comparisons.
"U.S. Environmental Protection Agency" or "EPA" means the federal government agency with responsibility for protecting, safeguarding and improving the natural environment (i.e., air, water and land) upon which human life depends.
"Virginia Air Pollution Control Law" means Chapter 13 (§ 10.1-1300 et seq.) of Title 10.1 of the Code of Virginia, which is titled "Air Pollution Control Board."
"Virginia Environmental Laboratory Accreditation Program" or "VELAP" means the program DCLS operates to certify environmental laboratories under this chapter.
"Wastewater" means liquid and water-carried industrial wastes and domestic sewage from residential dwellings, commercial buildings, industrial and manufacturing facilities and institutions.
"Waterworks" means each system of structures and appliances used in connection with the collection, storage, purification, and treatment of water for drinking or domestic use and the distribution thereof to the public, except distribution piping.
"Zooplankton" means microscopic animals that float freely with voluntary movement in a body of water.
1VAC30-45-50. Scope of certification.
A. Noncommercial environmental laboratories shall be certified based on the general laboratory standards set out in Part II (1VAC30-45-200 et seq.) of this chapter and on the specific test methods or analysis, monitoring or measurement required by regulatory permit or other requirement under the Virginia Air Pollution Control Law, Virginia Waste Management Act, or Virginia Water Control Law, the regulations promulgated under these laws, and by permits and orders issued under and in accordance with these laws or regulations.
DGS-DCLS DCLS shall review alternative test
methods and procedures for certification when these are proposed by the
applicant laboratory. The provisions of 1VAC30-45-70 E and 1VAC30-45-90 B
govern alternative test methods and procedures.
C. Certification shall be granted for one or more fields of
certification, including the matrix, the technology and methods
used by the
noncommercial environmental laboratory, and the individual analytes or
analyte groups determined by the particular method used by the
1VAC30-45-60. General: certification requirements.
A. Components of certification. The components of certification include review of personnel qualifications, on-site assessment, proficiency testing, and quality systems. The criteria for these components, set out in Part II (1VAC30-45-200 et seq.) of this chapter, shall be fulfilled for certification.
B. Individual laboratory sites and mobile laboratories.
1. Individual laboratory sites are subject to the same application process, assessments, and other requirements as environmental laboratories. Any remote laboratory sites are considered separate sites and subject to separate on-site assessments.
2. Laboratories located at the same physical location shall be considered an individual laboratory site if these laboratories are owned by the same person, and have the same laboratory manager and quality system.
3. Laboratories located at separate, noncontiguous physical
locations may request to be considered as an individual laboratory site if
these laboratories are owned by the same person and have the same laboratory
manager and quality system. 4. 3. A mobile laboratory, which is configured
with equipment to perform analyses, whether associated with a fixed-based
laboratory or not, is considered an environmental laboratory and shall require
separate certification. This certification shall remain with the mobile
laboratory and be site independent. Moving the configured mobile laboratory to
a different site will not require a new or separate certification. Before
performing analyses at each new site, the laboratory shall ensure that
instruments and equipment have been checked for performance and have been
1VAC30-45-70. Process to apply and obtain certification.
A. Duty to apply. All owners of noncommercial environmental laboratories shall apply for certification as specified by the provisions of this section. Applications for certification must be obtained from DCLS program staff by email at Lab_Cert@dgs.virginia.gov.
B. Timely initial applications. 1. Owners of noncommercial environmental laboratories
applying for certification under this chapter for the first time shall submit
an application to DGS-DCLS no later than September 29, 2009. 2. Owners of noncommercial environmental laboratories that
come into existence after January 1, 2009, shall submit an initial application
to DGS-DCLS no later than 180 calendar days prior to beginning operation. C. Timely renewal applications. The owner of a certified
noncommercial environmental laboratory shall submit an application for renewal
of certification at least 90 calendar days prior to expiration of
B. Owners of noncommercial environmental laboratories applying for certification under this chapter for the first time shall submit an application to DCLS as specified under subsection F of this section.
C. Renewal and reassessment.
1. DCLS shall renew certification annually for the certified laboratory provided the laboratory does the following:
a. Maintains compliance with this chapter.
b. Attests to this compliance by signing the certificate of compliance provided under subdivision F 3 of this section.
c. Reports acceptable proficiency test values as required by Article 3 (1VAC30-45-500 et seq.) of Part II of this chapter.
d. Pays the fee required by 1VAC30-45-130.
2. DCLS shall reassess the certified environmental laboratory during an on-site assessment as required by Article 2 (1VAC30-45-300 et seq.) of Part II of this chapter.
D. Responsibilities of the owner and operator when the laboratory is owned by one person and operated by another person.
1. When an environmental laboratory is owned by one person but is operated by another person, the operator may submit the application for the owner.
2. If the operator fails to submit the application, the owner is not relieved of his responsibility to apply for certification.
DGS-DCLS DCLS may notify noncommercial
environmental laboratories of the date their applications are due, failure of DGS-DCLS
DCLS to notify does not relieve the owner of his obligation to apply
under this chapter.
E. Submission of applications for modifications to
certification. An owner of a certified noncommercial environmental laboratory
shall follow the process set out in 1VAC30-45-90 B
to add a new matrix,
technology/method, an analyte or analyte group, modify a test method or
institute use of a method or technology not in the laboratory's standard
operating procedures, including alternative test methods or procedures to
modify the laboratory's scope of certification.
F. Contents of application.
1. Applications shall include but not be limited to the following information and documents:
a. Legal name of laboratory;
b. Name of owner of laboratory;
c. Name of operator of laboratory, if different than owner;
d. Street address and description of location of laboratory;
e. Mailing address of laboratory, if different from street address;
f. Address of owner, if different from laboratory address;
g. Name, address, telephone number, facsimile number and
h. Name, address, telephone number, facsimile number and
i. Name, address, telephone number, facsimile number and
title, and telephone number of laboratory
k. Laboratory type (e.g., public water system, public wastewater system or combination of the two, or industrial (with type of industry indicated));
l. Laboratory hours of operation;
m. Fields of certification (matrix, technology/method, and
group) analyte) for which certification is sought; n. Methods employed, including analytes; o. n. The results of the three most recent
proficiency test studies one successful unique PT study for each field
of proficiency testing as required by Article 3 (1VAC30-45-500 et seq.) of Part
II of this chapter; p. o. Quality assurance manual; and q. Lab identification number (for renewal only); and r. p. For mobile laboratories, a unique vehicle
identification number, such as a manufacturer's vehicle identification number
(VIN#), serial number, or license number.
2. Fee. The application shall include payment of the fee as specified in 1VAC30-45-130.
3. Certification of compliance.
a. The application shall include a "Certification of Compliance" statement signed and dated by the responsible official, by the quality control officer and by the laboratory manager.
b. The certification of compliance shall state: "The applicant understands and acknowledges that the laboratory is required to be continually in compliance with the Virginia environmental laboratory certification program regulation (1VAC30, Chapter 45) and is subject to the provisions of 1VAC30-45-100 in the event of noncompliance. I certify under penalty of law that this document and all attachments were prepared under my direction or supervision in accordance with a system designed to assure that qualified personnel properly gather and evaluate the information submitted. Based on my inquiry of the person or persons who manage the laboratory or those persons directly responsible for gathering and evaluating the information, the information submitted is, to the best of my knowledge and belief, true, accurate and complete. Submitting false information or data shall result in denial of certification or decertification. I hereby further certify that I am authorized to sign this application."
G. Completeness determination.
DGS-DCLS DCLS shall determine whether an
application is complete and notify the laboratory of the result of such
determination. During the initial certification period, DGS-DCLS DCLS
shall provide this notice within 90 calendar days of its receipt of a
laboratory's initial application. Following the initial certification
period, DGS-DCLS shall provide this notice within 60 calendar days of DGS-DCLS's
receipt of a laboratory's initial application and within 30 calendar days of
DGS-DCLS' receipt of a laboratory's renewal application.
2. An application shall be determined complete if it contains
all the information required pursuant to subsection F of this section and is
sufficient to evaluate the laboratory prior to the on-site assessment.
Designating an application complete does not preclude
from requesting or accepting additional information.
DGS-DCLS DCLS determines that an application
is incomplete, DGS-DCLS's the DCLS notification of such
determination shall explain why the application is incomplete and specify the
additional information needed to make the application complete.
Except during the initial certification period, if If
DCLS makes no determination is made within 60 within 90
calendar days of DGS-DCLS's its receipt of either (i) the
application or (ii) additional information, in the case of an application
determined to be incomplete, the application shall be determined to be
complete. During the initial certification period, the time period shall be
90 calendar days.
5. If the laboratory has not submitted the required additional
information within 90 days of receiving a notice from
requesting additional information, DGS-DCLS DCLS may return
the incomplete application and inform the laboratory that the application
cannot be processed. The laboratory may then submit a new application.
H. Grant of interim certification pending final determination on application.
DGS-DCLS DCLS shall grant a laboratory interim
certification status under the following conditions:
a. The laboratory's application is determined to be complete;
b. The laboratory has satisfied all the requirements for certification, including all requests for additional information, with the exception of on-site assessment; and
DGS-DCLS DCLS is unable to schedule the
on-site assessment within 90 120 days of its determination that
the application is complete (for initial applications) or before the
laboratory's certification expires (for renewal applications).
2. A laboratory with interim certification status shall have
the same rights and status as a laboratory that has been granted certification
3. Interim certification expires when
issues a final determination on certification.
I. On-site assessment.
1. An on-site assessment shall
be performed and the follow-up and reporting procedures for such assessments
shall be completed in accordance with Article 2 (1VAC30-45-300 et seq.) of Part
II of this chapter prior to issuance of a final determination on certification.
2. Alternative on-site assessment option. If DGS-DCLS is
unable to schedule an on-site assessment under the conditions of subsection H 1
c of this section, the owner of the applicant laboratory may use third-party
on-site assessors instead of DGS-DCLS on-site assessors under the following
conditions: a. The third-party on-site assessors are on a
DGS-DCLS-approved list of on-site assessors; and b. The owner of the applicant laboratory agrees to pay the
third-party on-site assessors.
J. Final determination on certification.
completion of the certification review process and corrective action, if any, DGS-DCLS
DCLS shall grant certification in accordance with subsection K of this
section or deny certification in accordance with subsection L of this section. 2. Except during the initial certification period, DGS-DCLS
shall complete action on a laboratory's application within nine months from the
time a completed application is received from the laboratory.
K. Grant of certification.
1. When a laboratory meets the requirements specified for
DGS-DCLS DCLS shall issue a certificate
to the laboratory. The DCLS shall send the certificate shall
be sent to the laboratory manager , and shall notify the
responsible official shall be notified.
2. The director of
DGS-DCLS DCLS or his designee
shall sign the certificate. The certificate shall include the following
a. Name of owner of laboratory;
b. Name of operator of laboratory, if different from owner;
c. Name of responsible official;
d. Address and location of laboratory;
e. Laboratory identification number;
f. Fields of certification (matrix, technology/method,
group) and analyte) for which certification is granted;
g. Any addenda or attachments; and
h. Issuance date and expiration date.
3. The laboratory shall post the most recent certificate of
certification and any addenda to the certificate issued by
in a prominent place in the laboratory facility.
4. Certification shall expire
two years one year
after the date on which certification is granted.
L. Denial of certification.
DGS-DCLS DCLS shall deny certification to an
environmental laboratory in total if the laboratory is found to be falsifying
any data or providing false information to support certification.
2. Denial of certification in total or in part.
DGS-DCLS DCLS may deny certification to an
environmental laboratory in total or in part if the laboratory fails to do any
of the following:
(1) Pay the required fees.
(2) Employ laboratory staff to meet the personnel qualifications as required by Part II (1VAC30-45-200 et seq.) of this chapter.
(3) Successfully analyze and report proficiency testing samples as required by Part II of this chapter.
(4) Submit a corrective action
report plan in
accordance with Part II of this chapter in response to a deficiency report from
the on-site assessment team within the required 30 calendar days.
(5) Implement the corrective actions detailed in the
report plan within the [ time frame
timeframe ] specified by DGS-DCLS DCLS.
(6) Pass required on-site assessment as specified in Part II of this chapter.
(7) Implement a quality system as defined in Part II of this chapter.
DGS-DCLS DCLS may deny certification to an
environmental laboratory in total or in part if the laboratory's application is
not determined to be complete within 90 calendar days following notification of
incompleteness because the laboratory is delinquent in submitting information
required by DGS-DCLS DCLS in accordance with this chapter.
DGS-DCLS DCLS may deny certification to an
environmental laboratory in total or in part if the DGS-DCLS DCLS
on-site assessment team is unable to carry out the on-site assessment pursuant
to Article 2 (1VAC30-45-300 et seq.) of Part II of this chapter because a
representative of the environmental laboratory denied the team entry during the
laboratory's normal business hours that it specified in its application.
DGS-DCLS DCLS shall follow the process
specified in 1VAC30-45-110 when denying certification to an environmental
M. Reapplication following denial of certification.
denial of certification, the laboratory shall wait six months before reapplying
for certification. 2. DGS-DCLS DCLS shall not waive application fees
for a laboratory reapplying for certification.
1VAC30-45-80. Maintaining certification.
A. Certification remains in effect until withdrawn by
DCLS, withdrawn voluntarily at the written request of the certified
laboratory, or until expiration of the certification period. To maintain certification,
the certified laboratory shall comply with the elements listed in this section
and in 1VAC30-45-90.
B. Quality systems. Laboratories seeking to maintain certification under this chapter shall assure consistency and promote the use of quality assurance and quality control procedures. Article 4 (1VAC30-45-600 et seq.) of Part II of this chapter specifies the quality assurance and quality control requirements that shall be met to maintain certification.
C. Proficiency tests. Laboratories seeking to maintain certification under this chapter shall perform proficiency tests as required under Article 3 (1VAC30-45-500 et seq.) of Part II of this chapter.
D. Recordkeeping and retention. All laboratory records
associated with certification parameters shall be kept as provided by the
requirements for records under Part II (1VAC30-45-200 et seq.) of this chapter.
These records shall be maintained for a minimum of three years unless the
records are required to be maintained for a longer period by another section of
this regulation or another regulation. All such records shall be available to
DCLS upon request.
1VAC30-45-90. Notifications and changes to certification elements and status.
A. Changes to key certification criteria. The certified
laboratory shall notify
DGS-DCLS DCLS in writing of any changes in
key certification criteria within 30 calendar days of the change. Key
certification criteria are laboratory ownership, location, key personnel, and
B. Changes to scope of certification.
DGS-DCLS DCLS may approve a laboratory's application
to add a new matrix, technology, analyte, or test method to a laboratory's
scope of certification or to otherwise modify the laboratory's scope of
certification by performing a data review.
2. To apply, the owner of the certified laboratory shall submit
the following to
letter written request signed by the owner
that briefly summarizes the addition to be made to the laboratory's scope of
b. Pertinent information demonstrating the laboratory's
capability to perform the additional matrix, technology/method, or
group analyte, such as proficiency testing performance and quality
c. A written standard operating procedure covering the new
matrix, technology/method, or
analyte/analyte group analyte.
DGS-DCLS DCLS may approve a laboratory's
application for modification to its scope of certification by performing a
review of the application materials submitted, without an on-site assessment.
The addition of a technology or test method requiring the use of specific
equipment may require an on-site assessment. Other reviews of performance and
documentation may be carried out by DGS-DCLS DCLS depending on
the modification for which the laboratory applies.
4. Within 90 calendar days of the receipt of the application
from the certified environmental laboratory,
DGS-DCLS DCLS shall
review and determine whether the proposed modification may be approved.
5. If the proposed modification to the laboratory's scope of
certification is approved,
DGS-DCLS DCLS shall amend the
laboratory's certificate of certification.
6. DCLS shall not send the amended certificate of certification to the laboratory until DCLS receives the payment of the fee required under 1VAC30-45-130 F 1.
C. Change of ownership or location of laboratory.
1. The certified laboratory shall submit a written notification
DGS-DCLS DCLS of the change of ownership or location of the
laboratory within 30 calendar days of the change. This requirement applies
only to fixed-based and not pertaining to change of location does not
apply to mobile laboratories.
2. Certification may be transferred when the legal status or ownership of a certified laboratory changes as long as the transfer does not affect the laboratory's personnel, equipment, or organization.
3. If the laboratory's personnel, equipment, or organization
are affected by the change of legal status or ownership,
may require recertification or reapplication in any or all of the categories
for which the laboratory is certified.
DGS-DCLS DCLS may require an on-site
assessment depending on the nature of the change of legal status or ownership. DGS-DCLS
DCLS shall determine the elements of any on-site assessment required. 5. When there is a change in ownership, the new owner of the
certified laboratory shall assure historical traceability of the laboratory
identification numbers. 6. 5. When there is a change in ownership, the
new owner of the certified laboratory shall keep all records and analyses
performed by the previous owner under his scope of pertaining to
certification for a period of three years, or longer if required by other
regulations. These records and analyses are subject to inspection by DGS-DCLS
DCLS during this three-year period. This provision applies regardless of
change of ownership, accountability or liability.
D. Voluntary withdrawal. Any environmental laboratory owner
who wishes to withdraw the laboratory from its certification status or from
being certified, in total or in part, shall submit written notification to
no later than 30 calendar days before the end of the laboratory's certification
term DCLS. Within 30 calendar days, DGS-DCLS DCLS
shall provide the laboratory with a written notice of withdrawal.
1VAC30-45-95. Suspension of certification.
A. DCLS may suspend certification from an environmental laboratory in total or in part to allow the laboratory time to correct the reason for which DCLS may withdraw certification. Suspension is limited to the reasons listed in subsection B of this section.
B. DCLS may suspend certification from an environmental laboratory in part or in total when the laboratory has failed to do any of the following:
1. Participate in the proficiency testing program as required by Article 3 (1VAC30-45-500 et seq.) of Part II of this chapter.
2. Satisfactorily complete proficiency testing studies as required by Article 3 (1VAC30-45-500 et seq.) of Part II of this chapter.
3. Maintain a quality system as defined in Article 4 (1VAC30-45-600 et seq.) of Part II of this chapter.
4. Employ staff that meets the personnel qualifications of Article 1 (1VAC30-45-200 et seq.) of Part II of this chapter.
5. Notify DCLS of any changes in key certification criteria as set forth in 1VAC30-45-90.
C. Process to suspend certification.
1. When DCLS becomes aware of a cause to suspend a laboratory, the agency shall send notification to the responsible official and the laboratory manager stating it appears to DCLS that the laboratory has failed to meet the 1VAC30-45 standards for one or more of the reasons listed in subsection B of this section. DCLS shall send the notification by certified mail.
2. The DCLS notification shall do the following:
a. Require the laboratory to provide DCLS with documentation of the corrective action already taken with regard to its failure to meet a standard under subsection B of this section.
b. State the corrective action the laboratory must take and the time allowed for this corrective action to be completed in order to retain certification.
3. The environmental laboratory may proceed to correct the deficiencies for which DCLS may suspend the laboratory's certification.
4. Alternatively the laboratory may state in writing that DCLS is incorrect in its observations regarding potential suspension and give specific reasons why the laboratory believes DCLS should not suspend certification. The laboratory has the right to due process as set forth in 1VAC30-45-110, the Administrative Process Act (§ 2.2-4000 et seq. of the Code of Virginia), and Part 2A of the Rules of the Supreme Court of Virginia.
5. With the exception of subdivision B 4 of this section, DCLS may allow the laboratory up to 60 days to correct the problem for which it may have its certification suspended.
6. DCLS shall set a date for suspension that follows the period provided under subdivision 5 of this subsection to restore certification.
7. If the laboratory does not correct its deficiencies within the time period allowed or pursue options under subdivision 4 of this subsection, DCLS may suspend a laboratory in part or in total.
8. DCLS shall notify the laboratory by letter if the laboratory's certification is suspended in part or in total. DCLS shall send the notification by certified mail. DCLS shall also notify the pertinent Virginia state agency of the laboratory's suspension status.
9. The laboratory may provide information demonstrating why suspension is not warranted in accordance with subdivision 4 of this subsection.
D. Responsibilities of the environmental laboratory and DCLS when certification has been suspended.
1. The term of suspension shall be limited to six months or the period of certification whichever is longer.
2. The environmental laboratory shall not continue to analyze samples or report analysis for the fields of certification for which DCLS has suspended certification.
3. The environmental laboratory shall retain certification for the fields of certification, methods, and analytes where it continues to meet the requirements of this chapter.
4. The laboratory's suspended certification status shall change to certified when the laboratory demonstrates to DCLS that the laboratory has corrected the deficiency or deficiencies for which its certification was suspended.
5. An environmental laboratory with suspended certification shall not have to reapply for certification if the cause or causes for suspension are corrected within the term of suspension.
6. If the laboratory fails to correct the causes of suspension within the term of suspension, DCLS shall decertify the laboratory in total or in part.
DGS-DCLS DCLS shall decertify an
environmental laboratory in total if the laboratory is found to be falsifying
any data or providing false information to support certification.
DGS-DCLS DCLS may decertify an environmental
laboratory in part or in total when the laboratory has failed to do any of the
1. Participate in the proficiency testing program as required by Article 3 (1VAC30-45-500 et seq.) of Part II of this chapter.
Complete Satisfactorily complete proficiency
testing studies and maintain a history of at least two successful
proficiency testing studies for each affected certified field of testing out of
the three most recent proficiency testing studies as defined in as required
by Article 3 (1VAC30-45-500 et seq.) of Part II of this chapter.
3. Maintain a quality system as defined in Article 4 (1VAC30-45-600 et seq.) of Part II of this chapter.
4. Employ staff that
meet meets the personnel
qualifications in Article 1 (1VAC30-45-200 et seq.) of Part II of this chapter.
5. Submit an acceptable corrective action
after two opportunities as specified in 1VAC30-45-390.
6. Implement corrective action specified in the laboratory's
report plan as set out under 1VAC30-45-390.
DGS-DCLS DCLS of any changes in key
certification criteria as set forth in 1VAC30-45-90.
8. Use accurate references to the laboratory's certification status in the laboratory's documentation.
9. Allow a DCLS assessment team entry during normal business hours to conduct an on-site assessment required by Article 2 (1VAC30-45-300 et seq.) of Part II of this chapter.
10. Pay the required fees specified in 1VAC30-45-130.
DGS-DCLS DCLS shall follow the process
specified in 1VAC30-45-110 when decertifying an environmental laboratory.
D. Responsibilities of the environmental laboratory and
DCLS when certification has been withdrawn.
1. Laboratories that lose their certification in full shall
return their certificate to
2. If a laboratory loses certification in part,
to the certificate shall be issued by DGS-DCLS DCLS shall issue a
revised certificate to the laboratory.
3. When the environmental laboratory has lost certification in full or in part, the laboratory shall not continue to analyze samples or report analyses for the fields of certification that DCLS has decertified.
E. After correcting the reason or cause for decertification
1VAC30-45-100 subsection A or B of this section, the
laboratory owner may reapply for certification under 1VAC30-45-70.
1VAC30-45-110. Procedures to deny certification
, to or
decertify a laboratory , and; appeal procedures.
DGS-DCLS believes it has grounds DCLS
becomes aware of a cause to deny certification or to decertify an
environmental laboratory, DGS-DCLS DCLS shall notify the
environmental laboratory in writing of its intent to hold an informal fact
finding under § 2.2-4019 of the Code of Virginia in order to make a decision on
the denial of certification or decertification this information and require
a response from the responsible official. DGS-DCLS DCLS shall
send this notification by certified mail to the responsible official and
provide a copy to the manager of the environmental laboratory. The notice of
informal fact finding shall provide a detailed explanation of the basis for the
2. For a potential denial of certification, the notice shall state that the laboratory has failed to meet the 1VAC30-45 standards and shall specify one or more of the reasons for denial of certification under 1VAC30-45-70 L, providing a detailed explanation of the basis for the denial of certification.
3. For a potential decertification, the notice shall state that the laboratory has failed to meet the 1VAC30-45 standards and shall specify one or more of the reasons for decertification under 1VAC30-45-100 A or B, providing a detailed explanation of the basis for decertification.
4. In its notice, DCLS shall request the laboratory to notify DCLS in writing if the laboratory believes the agency is incorrect in its determination. Before rendering a decision on decertification or denial of certification, DCLS shall provide the opportunity for the laboratory to meet with DCLS in an informal fact-finding proceeding pursuant to § 2.2-4019 of the Code of Virginia.
5. If the laboratory believes DCLS to be incorrect in its determination, the laboratory shall provide DCLS with a detailed written demonstration of why DCLS should not deny certification to or decertify the laboratory. The laboratory shall include this demonstration in the response required under subdivision 6 of this subsection.
6. The laboratory shall provide DCLS with a written response within 30 calendar days of the date of notification from DCLS. The laboratory shall indicate whether it disputes the DCLS determination provided in the agency notice and whether the laboratory requests an informal fact-finding proceeding. If the laboratory does not respond, DCLS shall render its case decision.
B. Following the informal fact finding held pursuant to §
2.2-4019 of the Code of Virginia, the director shall render a decision
regarding certification, and shall send this notification by certified mail to
the responsible official and provide a copy to the manager of the environmental
laboratory. If the director's decision is adverse to the environmental
laboratory, the responsible official may appeal this decision in accordance
with § 2.2-4026 of the Code of Virginia and Part 2A of the Rules of the Supreme
Court of Virginia. C. The provisions of this section do not preclude informal
discussions between DGS-DCLS and any environmental laboratory that has been
notified of a possible denial of certification or of decertification. These
informal discussions to resolve the concerns that prompted the notice shall be
held prior to the informal fact-finding proceeding.
B. An environmental laboratory may appeal a final decision by DCLS to deny certification to or decertify a laboratory pursuant to the Administrative Process Act (§ 2.2-4000 et seq. of the Code of Virginia).
D. C. The certification status of an
environmental laboratory appealing decertification shall not change pending the
final decision of the appeals filed under the Virginia Administrative Process
Act (§ 2.2-4000 et seq. of the Code of Virginia) and Part 2A of the Rules of
Supreme Court of Virginia.
DGS-DCLS DCLS may grant a partial or full
exemption from the requirements of this chapter based on compliance and
DGS-DCLS DCLS may consider granting an
exemption if a laboratory applies for an exemption and has met all
certification requirements for a period of four consecutive years.
C. An environmental laboratory may apply for an exemption by submitting a request. The request shall include the following information:
1. The scope of the requested exemption;
2. Whether the exemption should be partial or total;
3. If partial, what form the exemption will take; and
4. Why the exemption is appropriate.
D. Upon receiving an application for an exemption,
DCLS shall provide notice of the request for an exemption in the
Virginia Register of Regulations.
E. The notice shall provide a 30-day comment period on the request and shall specify the nature of the request.
DGS-DCLS DCLS shall grant or deny the
exemption request and provide a written response to the requesting laboratory
within 90 calendar days of receipt of the request.
G. Exemptions granted by
DGS-DCLS DCLS shall be
for a period of no more than 24 months.
Fees shall be submitted with all applications, including
reapplications, for certification and all renewal applications for
certification. Applications shall not be designated as complete until the fee
is received by DGS-DCLS. Environmental laboratories shall pay a fee with
all applications, including reapplications, for certification. DCLS shall not
designate an application as complete until it receives payment of the fee.
2. Each certified environmental laboratory shall pay an annual fee to maintain its certification. DCLS shall send an invoice to the certified environmental laboratory.
3. Fees shall be nonrefundable.
B. Fee computation. 1. Fees shall be computed based on the test methods for
which a laboratory seeks certification and on the laboratory type. For the
purpose of fee calculation, the designations for the laboratory type are (i) a
general environmental laboratory or (ii) an environmental laboratory performing
only simple test procedures. 2. The fee shall be the total of the base fee and the test
category fees for the specific laboratory type to be certified. 3. The test category fees cover categories for the test
methods to be certified as specified in the laboratory's application. 4. If the total of the base fee and the test category fees
is more than the maximum fee designated for the specific laboratory type to be
certified, the laboratory shall pay the maximum fee. C. Laboratories B. Environmental laboratories
performing only simple test procedures shall pay an annual fee of $600. 1. The base fee shall be $100. 2. The maximum fee shall be $600. D. General environmental laboratories. 1. The base fee shall be $1,700. 2. The maximum fee shall be $5,200. E. Test category fees. 1. Fees shall be charged for each category of tests to be
certified. 2. The fee for each category includes one or more analytical
methods unless otherwise specified. With the exception of the test categories
labeled oxygen demand and physical, test categories related to test methods for
water are defined by 40 CFR 136.3. 3. Fees.
C. Fee computation for general environmental laboratories.
1. Fees shall be applied on an annual basis.
2. Environmental laboratories shall pay the total of the base fee and the test category fees set out in subsections D and E of this section.
D. Base fees for general environmental laboratories.
1. DCLS determines the base fee for a laboratory by taking into account both the total number of methods and the total number of field of certification matrices for which the laboratory would be certified.
2. DCLS shall charge the base fees set out in Table 1. The base fee for a laboratory is located by first finding the row for the total number of methods to be certified and then finding the box on that row located in the column headed by the total number of matrices to be certified. For example, DCLS charges a base fee of $1300 to a laboratory performing a total of eight methods for one matrix.
TABLE 1: BASE FEES
Number of Methods
1 - 9
10 - 29
30 - 99
E. Test category fees for general environmental laboratories.
1. The test category fees cover the types of testing for which a laboratory may be certified as specified in the laboratory's application or as certified at the time of annual billing.
2. Fees shall be charged for each category of tests to be certified.
3. Fees shall be charged for the total number of field of certification matrices to be certified under the specific test category. For example, if a laboratory is performing inorganic chemistry for both nonpotable water and solid and chemical materials matrices, the fee for this test category would be found in the column for two matrices.
4. The fee for each category includes one or more analytical methods unless otherwise specified.
5. DCLS shall charge the test category fees set out in Table 2. The test category fees for a laboratory are located by first finding the row with the total number of test methods for the test category to be certified. The fee to be charged for the test category will be found on that row in the column headed by the total number of matrices to be certified. A laboratory performing four test methods for inorganic chemistry in nonpotable water and solid and chemical materials (two matrices) would be charged a test category fee of $375.
6. Noncommercial environmental laboratories that perform toxicity, radiochemical, or asbestos testing shall pay the test category fees established for these types of testing in 1VAC30-46-150.
TABLE 2: TEST CATEGORY FEES
Fees by Number of Matrices
Bacteriology, 1 - 3 total methods
Bacteriology, 4 or more total methods
Physical, 1 - 5 total methods
Physical, 6 - 10 total methods
Inorganic chemistry, 1 - 10 total methods
Inorganic chemistry, 11 - 20 total methods
Inorganic chemistry, 21 - 49 total methods
Chemistry metals, 1 - 5 total methods
Chemistry metals, 6 - 20 total methods
Organic chemistry, 1 - 5 total methods
Organic chemistry, 6 - 20 total methods
7. Fee examples. Three examples are provided.
a. Example 1:
One matrix and four test methods
Test Category Fees
Bacteriology (2 methods)
Oxygen demand (1 method)
b. Example 2:
One matrix and 15 test methods
Test Category Fees
Bacteriology (2 methods)
Inorganic chemistry (9 methods)
Chemistry metals (2 methods)
Oxygen demand (1 method)
c. Example 3:
Two matrices and 27 test methods
Test Category Fees
Bacteriology (4 methods)
Oxygen demand (1 method)
Solid and Chemical Materials
Chemistry metals (1 method)
Nonpotable Water and Solid and Chemical Materials
Inorganic chemistry (13 methods)
Nonpotable Water and Solid and Chemical Materials
Physical (7 methods)
F. Additional fees. Additional fees shall be charged to
laboratories applying for the following: (i) modification to scope of
certification under 1VAC30-45-90 B, (ii) transfer of ownership under
1VAC30-45-90 C, (iii) exemption under 1VAC30-45-120,
(iv) request that
multiple noncontiguous laboratory sites be considered as one site under
1VAC30-45-60 B 3, or (v) (iv) petition for a variance under
1. For any certified environmental laboratory that applies to modify its scope of certification as specified under 1VAC30-45-90 B, DCLS shall assess a fee determined by the method in subsection G of this section.
2. Under 1VAC30-45-90 C, DCLS may charge a transfer fee to a certified laboratory that transfers ownership. A fee shall be charged if DCLS (i) needs to review documentation sent by the laboratory about the transfer of ownership or (ii) determines that an on-site assessment is necessary to evaluate the effect of the transfer of ownership. DCLS shall assess a fee determined by the method in subsection G of this section. If, under 1VAC30-45-90 C, DCLS determines that the change of ownership or location of laboratory requires recertification of or reapplication by the laboratory, the laboratory shall pay the application fees required under this section.
1. 3. General environmental laboratories applying
for an exemption under 1VAC30-45-120 shall pay an initial application
fee of $250 and if the exemption is granted, up to an additional $1,000
depending on the scope of the exemption. $700 plus an additional fee
based on the actual time needed for DCLS to assess the exemption request. The
total fee shall not exceed the actual time DCLS takes to assess the exemption
request. Laboratories performing only simple test procedures applying for
an exemption under 1VAC30-45-120 shall pay an initial application fee of
$100 and if the exemption is granted, up to an additional $1,000 depending
on the scope of the exemption. The fee assessed for the scope of the exemption
shall be based on the actual time needed for DGS-DCLS to make the determination
$300 plus an additional fee based on the actual time needed for DCLS to
assess the exemption request. The total fee shall not exceed the actual time
DCLS takes to assess the exemption request. The fee assessed shall be
calculated using the method in subsection G of this section. 2. For any certified environmental laboratory that applies
to modify its scope of certification as specified under 1VAC30-45-90 B,
DGS-DCLS shall assess a fee determined by the method in subsection G of this
section. 3. Under 1VAC30-45-90 C, DGS-DCLS may charge a transfer fee
to a certified laboratory that transfers ownership. A fee shall be charged if
DGS-DCLS (i) needs to review documentation sent by the laboratory about the
transfer of ownership or (ii) determines that an on-site assessment is
necessary to evaluate the effect of the transfer of ownership. DGS-DCLS shall
assess a fee determined by the method in subsection G of this section. If
DGS-DCLS determines that a fee should be charged, the fee shall be a minimum of
$100 and a maximum of $1,000. If, under 1VAC30-45-90 C, DGS-DCLS determines
that the change of ownership or location of laboratory requires recertification
of or reapplication by the laboratory, the laboratory shall pay the application
fees required under this section. 4. Under 1VAC30-45-60 B 3, the owner of multiple
noncontiguous laboratories may request that DGS-DCLS consider these
laboratories to be one site. If, as a result of the request being granted,
DGS-DCLS needs to perform multiple on-site assessments, DGS-DCLS shall charge a
fee for the additional on-site assessments. The fee shall be the sum of
reasonable travel costs and labor charges for the additional on-site
assessments. The labor charges will be determined following the method in
subsection G of this section. 5. 4. Under 1VAC30-45-140, any person regulated
by this chapter may petition the director to grant a variance from any
requirement of this chapter. DGS-DCLS DCLS shall charge a an
initial fee for the time needed of $700 plus an additional fee
based on the actual time needed for DCLS to review the petition, including
any on-site assessment required. The total fee shall not exceed the actual
time DCLS takes to review and make a determination on the request for a
variance. The fee shall be determined by the method specified in subsection
G of this section.
G. Fee determination.
1. The fee shall be the sum of the total hourly charges for all reviewers plus any on-site review costs incurred.
2. An hourly charge per reviewer shall be determined by (i) obtaining a yearly cost by multiplying the reviewer's annual salary by 1.35 (accounts for overhead such as taxes and insurance) and then (ii) dividing the yearly cost by 1,642 (number of annual hours established by Fiscal Services, DGS, for billing purposes).
3. The charge per reviewer shall be determined by multiplying the number of hours expended in the review by the reviewer's hourly charge.
4. If an on-site review is required, travel time and on-site review time shall be charged at the same hourly charge per reviewer, and any travel expenses shall be added.
H. Out-of-state laboratories - travel costs. The owner of an environmental laboratory located in another state who applies for certification under this chapter shall also pay a fee equal to the reasonable travel costs associated with conducting an on-site assessment at the laboratory. Reasonable travel costs include transportation, lodging, per diem, and telephone and duplication charges.
DGS-DCLS DCLS shall derive the travel costs
charged under subsections G and H of this section from the Commonwealth of
Virginia reimbursement allowances and rates for lodging, per diem, and mileage.
1VAC30-45-300. Frequency of on-site assessment.
A. [ Frequency.
1. ] A comprehensive on-site assessment shall be
conducted of each laboratory as a condition for granting certification
and at renewal every two years.
[ 2. ] DCLS shall reassess each certified
every two years at least once every
three years ] starting from the date of the previous assessment
plus or minus six months.
[ 3. DCLS may conduct an on-site assessment of a laboratory every two years plus or minus six months under any of the following circumstances:
a. When a laboratory has received "not acceptable" PT results.
b. When a laboratory's corrective action presented to VELAP for "not acceptable" PT studies does not identify and correct the root cause of the PT study failure.
c. When DCLS has suspended certification for a laboratory in full or in part.
d. When on-site observations include nonconformances previously identified at an on-site assessment, indicating the corrective action was not implemented or not maintained.
e. When on-site observations include failure to qualify nonconforming data to the data user.
f. When on-site observations indicate the laboratory's failure to monitor and maintain regulatory conformance in documentation, traceability, or quality control requirements such that data generated by the laboratory are of questionable quality or defensibility. ]
B. Other on-site assessments.
DGS-DCLS DCLS identified a deficiency on a
previous on-site assessment, the agency may conduct a follow-up on-site
DGS-DCLS DCLS may conduct an on-site
assessment when a laboratory applies to modify its scope of certification ,;
when a transfer of owner occurs that affects personnel, equipment, or the
laboratory facilities ,; or when a laboratory applies for an
exemption or a variance. Any other change occurring in a laboratory's
operations that might reasonably be expected to alter or impair analytical
capability and quality may trigger an on-site assessment.
1VAC30-45-310. Announced and unannounced on-site assessments.
DGS-DCLS DCLS may conduct, at its discretion,
either announced or unannounced on-site assessments.
B. Advance notice of an assessment shall not be necessary.
C. To the maximum extent practical,
when necessary, shall work with the owner of an environmental laboratory to
obtain government security clearances for assessment personnel as far in
advance as possible. The owner of the environmental laboratory shall facilitate
expeditious attainment of the necessary clearances.
D. To the maximum extent practical, assessment personnel shall minimize disruption of a laboratory's operations and take into account competing demands on the time of laboratory personnel.
1VAC30-45-320. Request for records.
Prior to the actual site visit,
may request in writing from a laboratory those records required to be
maintained by this chapter.
1VAC30-45-330. Areas to be assessed.
DGS-DCLS DCLS shall assess the laboratory
against the personnel and quality control standards in Article 1 (1VAC30-45-200
et seq.) and Article 4 (1VAC30-45-600 et seq.) of this part. The specific areas
evaluated in an on-site assessment shall include but not be limited to:
1. Adequacy of the laboratory facility.
2. Organization and management of the laboratory.
3. Qualifications and experience of laboratory personnel.
4. Receipt, tracking and handling of samples.
5. Quantity, condition, and performance of laboratory instrumentation and equipment.
6. Preparation and traceability of calibration standards.
7. Test methods (including the adequacy of the laboratory's standard operating procedures as well as confirmation of the analyst's adherence to SOPs, and the analyst's proficiency with the described task).
8. Data reduction procedures, including an examination of raw data and confirmation that final reported results can be traced to the raw data/original observations.
9. Quality assurance and quality control procedures, including adherence to the laboratory's quality assurance plan and adequacy of the plan.
1VAC30-45-340. National security considerations.
A. Assessments at facilities owned or operated by federal agencies or contractors may require security clearances, appropriate badging, or a security briefing before the assessment begins.
B. The laboratory shall notify
DGS-DCLS DCLS in
writing of any information that is controlled for national security reasons and
cannot be released to the public.
1VAC30-45-350. Arrival, admittance, and opening conference.
A. Arrival. Assessment personnel shall arrive at the laboratory during established working hours. The laboratory manager (or, if unavailable, the laboratory manager's designee) shall be located as soon as possible after the assessment personnel arrive on the premises.
B. Admittance of assessment personnel.
1. A laboratory's refusal to admit the assessment
personnel for an on-site assessment shall result in an automatic failure of the
laboratory to receive certification or loss of an existing certification by the
laboratory, unless there are extenuating circumstances that are accepted and
DGS-DCLS DCLS. The team leader for the assessment
personnel shall notify DGS-DCLS DCLS as soon as possible after
refusal of entry.
2. DCLS shall consider any verbal or physical threat to the health and safety of its assessors or any overt antagonism towards its assessors as a refusal to admit the assessors for the purpose of on-site assessment. The assessors shall vacate the laboratory and shall notify DCLS as soon as possible of the circumstances of this refusal to admit. This refusal to admit shall result in an automatic failure of the laboratory to receive certification or the automatic loss of an existing certification by the laboratory.
C. Health and safety.
1. Under no circumstance, and especially as a precondition to gain access to a laboratory, shall assessment personnel be required or even allowed to sign any waiver of responsibility on the part of the laboratory for injuries incurred during an assessment.
2. Assessment personnel shall comply with all facility and laboratory safety procedures.
D. Opening conference. An opening conference shall be conducted and shall address the following topics:
1. The purpose of the assessment;
2. The identification of assessment personnel;
3. The test methods that will be examined;
4. Any pertinent records and procedures to be examined during the assessment and the names of the individuals in the laboratory responsible for providing assessment personnel with such records;
5. The roles and responsibilities of laboratory staff and managers;
6. Any special safety procedures that the laboratory may think necessary for the protection of assessment personnel;
7. The standards and criteria that will be used in judging the adequacy of the laboratory operation;
8. Confirmation of the tentative time for the exit conference; and
9. Discussion of any questions the laboratory may have about the assessment process.
1VAC30-45-380. Closing conference.
A. Assessment personnel shall meet with representatives of the laboratory following the assessment for a closing conference.
B. During the closing conference, assessment personnel shall
inform the laboratory of the preliminary findings and the basis for such
findings. The laboratory shall have an opportunity to provide further
explanation or clarification relevant to the preliminary findings. If the
laboratory objects to the preliminary findings during the closing conference,
all objections shall be documented by the assessment personnel and included in
the final report to
C. Additional problem areas may be identified in the final report.
D. Any potentially illegal activity that may be the subject of further action shall not be discussed in the closing conference.
1VAC30-45-390. Follow-up and reporting procedures.
DGS-DCLS DCLS shall present an assessment
report to the laboratory within 30 calendar days of the assessment.
B. If there are deficiencies identified in the assessment
report, the laboratory shall have 30 calendar days from the date of its receipt
of the assessment report to provide a response to
This response shall be called a corrective action report plan.
C. An exception to the deadlines specified in subsections A
and B of this section may occur in appropriate circumstances. Two circumstances
that may be considered appropriate by
DGS-DCLS DCLS are where a
possible enforcement investigation or other action has been initiated or where
the laboratory shows good cause for an extension.
D. The corrective action
report plan shall
include the following:
1. Any objections that the laboratory has with regard to the assessment report;
2. The action that the laboratory proposes to implement to correct each deficiency identified in the assessment report; and
3. The time period required to accomplish the corrective action.
DGS-DCLS DCLS shall determine and shall
notify the laboratory within 30 calendar days of receipt whether the corrective
action report plan is an acceptable response to the deficiencies
identified in the assessment report.
F. If the corrective action
report plan (or a
portion of the report) plan) is determined to be unacceptable to
remedy the deficiency, DGS-DCLS DCLS shall provide written
notification to the responsible official and manager of the laboratory
including a detailed explanation of the basis for such determination. Following
receipt of such notification, the laboratory shall have an additional 30
calendar days to submit a revised corrective action report plan
acceptable to DGS-DCLS DCLS.
1VAC30-45-400. Documentation of on-site assessment.
A. Checklists. The checklists used by assessment personnel
during the assessment shall become a part of
file for the laboratory.
B. Assessment report format.
1. The final assessment report shall contain a narrative description of the adequacy of the laboratory as it relates to the assessment standards specified in this chapter and in 1VAC30-45-330.
2. Assessment reports shall contain:
a. Name of owner of the laboratory (or operator of the laboratory, if different from the owner);
b. Identification of the laboratory assessed;
c. Date of the assessment;
d. Identification and affiliation of all assessment personnel;
e. Identification of participants in the assessment process;
f. Identification of analytes and test methods assessed;
g. Statement of the objective of the assessment;
i. Assessment observations, findings (including any deficiencies), objections noted by the laboratory, and requirements; and
j. Comments and recommendations.
3. The assessment findings and requirements shall be referenced to the standards in Part II (1VAC30-45-200 et seq.) of this chapter so that both the finding is understood and the specific requirement is outlined. The assessor shall specify the laboratory records, documents, equipment, procedures, or staff evaluated and the observations that contributed to each identified deficiency. The assessment report shall support with sufficient data all assessment findings and the overall evaluation of the laboratory.
4. The comments and recommendations section may be used to convey recommendations aimed at helping the laboratory improve.
C. Release of report.
1. The assessment report shall be released initially by
DCLS to the responsible official and the laboratory manager. The
assessment report shall not be released to the public until findings of the
assessment and the corrective actions have been finalized, all information
relating to national security has been stricken from the report in accordance
with prescribed procedures, and the report has been provided to the laboratory.
2. Once the assessment report has been released to the laboratory, any member of the public may request a copy of the report under the requirements of the Virginia Freedom of Information Act (§ 2.2-3700 et seq. of the Code of Virginia).
3. Checklists used by assessment personnel during the on-site assessment shall be provided to the laboratory with the final on-site assessment report [ upon request ].
D. The laboratory shall have access to documentation
pertaining to any on-site assessment of its facilities. Any laboratory wishing
to review its files shall request such assistance of
five days prior to visiting DGS-DCLS DCLS. A laboratory may
request copies of its documents without visiting DGS-DCLS DCLS. A
reasonable fee may be charged for copying, mailing, and staff time.
1VAC30-45-500. Laboratory enrollment in proficiency testing program.
A. Required level of participation.
1. To be certified initially and to maintain certification,
a laboratory shall participate in two single-blind, single-concentration PT
studies, where available, per year for each PT field of testing for which it
seeks or wants to maintain certification. Laboratories applying to be certified
for environmental toxicology (aquatic toxicity, sediment toxicity, or soils
toxicity) shall meet the requirements of subdivision 3 of this subsection. 2. Laboratories shall obtain PT samples from any PT provider
approved under the requirements of the NELAC standards for proficiency test
providers set out in Chapter 2 of the 2003 standards such as NIST. For PT
fields of testing having no approved providers listed by NELAC, the laboratory
shall consult DGS-DCLS for an approved provider. 3. Laboratories applying to be certified for environmental
toxicology (aquatic toxicity, sediment toxicity, or soils toxicity). To be
certified initially and to maintain certification, a laboratory shall
participate in at least one PT study per year (i.e., not more than 12 months
apart), when available, for each method code (matrix, organism, exposure system
and endpoint) for which it seeks or wants to maintain certification.
Laboratories seeking certification for aquatic toxicity testing shall meet the
requirements of 1VAC30-45-530.
1. To be certified initially and to maintain certification, a laboratory shall participate in PT studies as specified in 1VAC30-45-520 B for the fields of certification (FoC) for which the laboratory seeks or wants to maintain certification.
2. The applicant laboratory shall obtain PT samples from a PT provider approved by TNI. If a PT sample is not available from a TNI-approved provider, the laboratory shall consult DCLS for an approved provider.
B. Requesting certification.
1. When applying for certification, the laboratory owner shall
DGS-DCLS DCLS of the fields of testing certification
for which the laboratory chooses to become certified and shall participate in
the appropriate PT studies.
2. For all fields of
testing certification for
which PT samples are not available, the laboratory shall ensure the reliability
of its testing procedures by maintaining a quality system that meets all
applicable requirements of Article 4 (1VAC30-45-600 et seq.) of Part II of this
C. Reporting results.
1. Each laboratory shall
authorize the PT study provider to release all certification and remediation
results and "acceptable" or "not acceptable" status the
results of the final evaluation report of the laboratory's PT study
directly to DGS-DCLS DCLS, in addition to the laboratory. 2. The results of all of the PT sample tests including
"acceptable" or "not acceptable" status shall be part of
the public record.
1VAC30-45-510. Requirements for laboratory testing of PT study samples.
The samples shall be analyzed and the results returned
to the PT study provider no later than 45 calendar days from the scheduled
study shipment date. Samples for environmental toxicology shall be analyzed
within 45 calendar days of sample receipt. The laboratory shall report the
result within 45 calendar days of completion of the PT. The laboratory
shall report the analytical results from its analysis of the PT study to the PT
provider on or before the closing date of the study using the reporting format
specified by the PT provider.
B. The laboratory's management and all analysts shall ensure that all PT samples are managed, analyzed, and reported in the same manner as real environmental samples utilizing the same staff, methods as used for routine analysis of that analyte, procedures, equipment, and facilities. When analyzing a PT sample, the laboratory shall employ the same calibration, laboratory quality control and acceptance criteria, sequence of analytical steps, number of replicates and other procedures as used when analyzing routine samples.
C. Restrictions on exchanging information. Laboratories shall comply with all of the following restrictions on the transfer of PT samples and communication of PT sample results prior to the time the results of the study are released. Laboratory management or staff shall not:
1. Send any PT sample, or a portion of a PT sample, to another laboratory for any analysis for which it seeks certification or is certified.
2. Knowingly receive any PT sample or portion of a PT sample from another laboratory for any analysis for which the sending laboratory seeks certification or is certified.
3. Communicate with any individual at another laboratory (including intra-company communication) concerning the PT sample.
4. Attempt to obtain the assigned value of any PT sample from their PT provider.
D. Maintenance of records. The laboratory shall maintain
copies of all written, printed, and electronic records, including but not
limited to bench sheets, instrument strip charts or printouts, data
calculations, and data reports, resulting from the analysis of any PT sample
for three years or for as long as is required by the applicable regulatory
program. These records shall include a copy of the PT study report forms used
by the laboratory to record PT results. All of these laboratory records shall
be made available to the DCLS assessors
of DGS-DCLS during
on-site audits assessments of the laboratory.
1VAC30-45-520. PT criteria for laboratory certification.
A. Result categories.
1. The criteria described in this section apply individually to
PT field of testing FoPT, as defined by the laboratory
seeking to obtain or maintain certification in its certification request. These
criteria apply only to the PT portion of the overall certification standard.
2. There are two PT result categories: "acceptable" and "not acceptable."
B. Initial and continuing certification.
1. A laboratory seeking to obtain or maintain certification
shall successfully complete
two PT studies one PT study for each
requested PT field of testing within the most recent three rounds attempted
2. Once a laboratory has been granted certification status, it
shall continue to complete PT studies for each
PT field of testing FoPT
and maintain a history of at least two one acceptable PT studies
for each PT field of testing out of the most recent three study each
calendar year. The laboratory shall complete its PT studies by September 30 of
each calendar year.
For a laboratory seeking to obtain initial certification,
the most recent three rounds attempted shall have occurred within 18 months of
the laboratory's application date. When the PT sample used for initial
certification was analyzed by the laboratory prior to the date of application,
the analysis date of the PT sample shall be no more than 12 months prior to the
application date of certification.
For a laboratory seeking initial certification, or for
For a laboratory performing supplemental testing, the PT studies shall
be at least 15 calendar days apart from the closing date of one study to the
shipment date of another study for the same PT field of testing FoPT. 5. For a laboratory to maintain certification, completion
dates of successive proficiency rounds for a given PT field of testing shall be
approximately six months apart. Failure to meet the semiannual schedule is
regarded as a failed study.
5. When the PT study result is reported by the PT provider as "acceptable" the environmental laboratory has satisfied the PT requirement.
6. When the PT study result is "not acceptable," the environmental laboratory shall follow the procedure in subsection C of this section.
7. DCLS shall consider a laboratory's analytical result for a FoPT not acceptable when the laboratory makes any reporting error or omission that results in a nonspecific match between the analytical result for the FoPT and any criterion that identifies the laboratory or the field of certification for which the PT sample was analyzed for the purpose of initial or continued certification.
C. Procedure and requirements for "not acceptable" PT study results.
1. When a laboratory receives a PT study result of "not acceptable," the laboratory shall determine the cause for the failure and perform and document corrective action. The corrective action documentation shall be completed within 30 days of receiving the "not acceptable" PT study result and be submitted to DCLS upon request. [ DCLS may extend the time for corrective action and documentation. ]
2. Upon completion of the corrective action the laboratory shall perform another PT study for each FoPT that had a "not acceptable" result.
3. If the laboratory successfully completes the makeup PT study by receiving an "acceptable" result before December 31, DCLS shall not suspend the laboratory's certification for the pertinent FoC.
4. If the laboratory receives a "not acceptable" result on the makeup PT study, DCLS shall notify the laboratory that there is cause to suspend the laboratory's certification for the FoC for which the PT study was "not acceptable."
5. DCLS shall not extend the period for annual PT study completion beyond December 31 each year. Failure to satisfactorily complete a PT study [ , including any corrective action and makeup PT study, ] by December 31 shall result in suspension of certification in total or in part.
6. If the laboratory receives a "not acceptable" result on three successive PT studies, DCLS shall decertify the laboratory for the pertinent FoC until such time that the laboratory:
a. Completes corrective action for all failed studies and submits its corrective action report to DCLS;
b. Obtains an "acceptable" result for the PT studies; and
c. Applies for a change to its scope of certification and pays applicable fees required by 1VAC30-45-90 B and 1VAC30-45-130 F.
7. DCLS shall follow the provisions of 1VAC30-45-110 in decertifying the laboratory.
C. Supplemental studies. 1. A laboratory may elect to participate in PT studies more
frequently than required by the semiannual schedule. This may be desirable, for
example, when a laboratory first applies for certification or when a laboratory
fails a study and wishes to quickly reestablish its history of successful
performance. 2. These additional studies shall be reported and are
counted and scored the same way as routinely scheduled studies and shall be at
least 15 calendar days apart. D. Failed studies and corrective action. 1. Whenever a laboratory fails a study, it shall determine
the cause for the failure and take any necessary corrective action. It shall
then document in its own records and provide to DGS-DCLS both the investigation
and the action taken. 2. If a laboratory fails two out of the three most recent
studies for a given field of testing, its performance is considered
unacceptable for that field. The laboratory shall then meet the requirements of
initial certification as described in subsection B of this section. E. Second failed study. 1. The PT provider reports laboratory PT performance results
to DGS-DCLS at the same time that it reports the results to the laboratory. 2. If a laboratory fails a second study out of the most
recent three, as described in subdivision D 2 of this section, DGS-DCLS shall
take action within 60 calendar days to determine the certification status for
the unacceptable PT field of testing. F. Scheduling of PT studies. Laboratories shall determine
the schedule for their PT studies. G. D. Withdrawal from PT studies. A laboratory
may withdraw from a PT study for an analyte or analytes or for the entire
study if the laboratory notifies both the PT provider and DGS-DCLS before the
closing date of the PT study. This does not exempt the laboratory from
participating in the semiannual schedule. any FoPT on or before the
close date of the study. Withdrawing from a study shall not exempt the
laboratory from meeting the annual analysis requirements necessary for
Special requirements for aquatic toxicity.
(Repealed.) A. Laboratories seeking certification for aquatic toxicity
testing shall be assessed through on-site assessment and evaluation of EPA
Discharge Monitoring Report-Quality Assurance (DMR-QA) test results when
available. A failed DMR-QA endpoint shall require both of the following: 1. A formal response to DGS-DCLS with an explanation of the
probable cause for the endpoint failure and description of corrective actions
to be taken (where appropriate). 2. A decision by DGS-DCLS to accept the response or require
additional actions on the part of the laboratory or by DGS-DCLS. B. If a laboratory's response is unacceptable and DGS-DCLS
does not require additional on-site assessments, the laboratory shall complete
another study. Such additional studies shall be conducted at least 15 calendar
days from the previous study until the results are acceptable to DGS-DCLS.
DGS-DCLS may conduct additional on-site assessments as necessary based on the
results of any additional studies. C. When the DMR-QA whole effluent toxicity portion does not
include all test procedures required for a permit, the laboratory shall perform
a proficiency test for aquatic toxicity testing. D. DGS-DCLS shall not base loss of certification for
aquatic toxicity testing solely on PT results.
1VAC30-45-600. Quality system.
A. This article sets out the general requirements that an environmental laboratory has to successfully demonstrate to be recognized as competent to carry out specific environmental tests. The environmental laboratory shall establish, implement and maintain a quality system based on the required elements contained in this article.
B. The quality system shall be appropriate to the type, range and volume of testing, analysis, measurement or monitoring performed by the laboratory.
C. The quality system's documentation shall be communicated to, understood by, available to, and implemented by the appropriate personnel. All personnel concerned with testing and calibration activities within the laboratory shall familiarize themselves with the quality documentation and implement the policies and procedures in their work.
C. D. If more stringent standards or
requirements are included in a mandated test method or by regulation, the
laboratory shall demonstrate that such requirements are met. If it is not clear
which standard or requirement is more stringent, the standard or requirement
from the method or regulation is to be followed. D. E. Provisions pertaining to the management of
the quality system appear in 1VAC30-45-610 through 1VAC30-45-700. Provisions
pertaining to the technical requirements for the quality system appear in
1VAC30-45-710 through 1VAC30-45-770.
1VAC30-45-610. Quality manual.
1. The laboratory shall document its quality system in a quality manual. The quality manual shall reflect all quality assurance and quality control practices and programs used by the laboratory. The required elements of the quality system may be described in more than one document.
2. The quality manual shall be maintained current under the responsibility of the quality assurance officer.
3. The quality manual and any related documents shall be communicated to, understood by, available to, and implemented by all laboratory personnel.
4. The quality manual shall include but not be limited to the
elements listed in
subsection subsections B and C of this
B. The elements of a quality manual shall include but not be limited to:
1. Title page. The quality manual shall list the following
items on the title page: a. 1. A document title; b. 2. The laboratory's full name and address; c. 3. The name, address (if different from
above), and telephone number of the responsible official, laboratory manager,
and quality assurance officer; d. 4. The laboratory facility or facilities
covered by the quality manual; e. 5. Signed and dated concurrence, with appropriate
titles, of the responsible official, laboratory manager, and quality assurance
officer; and f. 6. The effective date of the quality manual .; 2. 7. Table of contents . and applicable
lists of references, glossaries, and appendices; and 3. 8. A quality policy statement, including
objectives of the quality system and commitment to good ethical
laboratory practices and to upholding the requirements of this chapter's
C. The quality manual shall include or reference but not be limited to:
4. 1. The organization and management structure
of the laboratory, its place in any parent organization and relevant
organizational charts. 5. The relationship between management, technical
operations, support services and the quality system. 6. The capabilities of the laboratory or scope of its
operation. 7. 2. Job descriptions of key staff and reference
to the job descriptions of other staff. 8. 3. Processes or procedures for establishing
that personnel have adequate training and experience in the duties they are
expected to carry out and are receiving any needed training. 9. Ethics policy statement developed by the laboratory.
Processes and procedures for educating and training personnel in their ethical
and legal responsibilities including the potential penalties for improper,
unethical or illegal actions. 10. 4. Mechanisms for ensuring that the
laboratory reviews all new work to ensure that it has the appropriate
facilities and resources before commencing such work. 11. 5. Procedures to ensure that all records
required by this chapter are retained, as well as procedures for control and
maintenance of documentation through a document control system that ensures
that all standard operating procedures, manuals, or documents clearly indicate
the time period during which the procedure or document was in force. 12. 6. Procedures for dealing with complaints. 13. 7. Procedures for audits and data review. 14. Reference to verification 8. Verification
practices that may include inter-laboratory comparisons, proficiency testing
programs, use of reference materials and internal quality control schemes. 15. 9. Procedures to be followed for feedback and
corrective action whenever testing discrepancies are detected, or departures
from documented policies and procedures occur. 16. 10. The laboratory management arrangements
for permitting departures from documented policies and procedures or from
standard specifications when the departures are planned and controlled. 17. Reference to the 11. The major equipment and
reference measurement standards used as well as the physical facility and
environment used by the laboratory in conducting tests. 18. Reference to procedures 12. Procedures for
calibration, verification and maintenance of equipment. 19. 13. A list of all technology/methods under
which the laboratory performs its certified testing. 20. The laboratory's procedures 14. Procedures
for achieving traceability of measurements, including standards. 21. 15. Procedures for receiving, handling,
storing, and disposing of submitted samples. 22. Reference to procedures 16. Procedures for
reporting analytical results.
17. Policy addressing the use of unique electronic signatures, where applicable.
C. D. Review and approval of quality manual.
1. The quality assurance officer shall review the laboratory's quality assurance program, manual and any related documentation whenever there is any change in test methods employed by the laboratory, change in equipment, or any other change in the laboratory that affects the quality assurance program.
2. The quality assurance manual shall be reviewed and approved by the quality assurance officer, the laboratory manager, and the responsible official at least annually.
1VAC30-45-660. Required records.
A. Sample handling.
1. The laboratory shall maintain a record of all procedures to which a sample is subjected while in the possession of the laboratory. These shall include but are not limited to all records pertaining to sample preservation, identification, receipt, acceptance or rejection, log-in, storage and tracking. The laboratory shall also maintain sampling information on each sample. This includes time and date of collection, type of sample (grab or composite), type of container, sampling point and preservation.
2. The laboratory shall have documented procedures for the receipt and retention of samples, including provisions necessary to protect the integrity of the samples.
B. Laboratory support activities. The laboratory shall retain the following documents and data:
1. All original raw data, whether hard copy or electronic, for calibrations, samples and quality control measures, including analysts' work sheets and data output records (chromatograms, strip charts, and other instrument response readout records).
2. A written description or reference to the specific test method used that includes a description of the specific computational steps used to translate parametric observations into a reportable analytical value.
3. Copies of final reports.
4. Archived standard operating procedures.
5. Correspondence relating to laboratory activities.
6. All corrective action
reports plans, audits,
and audit responses.
7. Proficiency test results and raw data.
8. Results of data review, verification, and cross-checking procedures.
C. Analytical records. The laboratory shall retain essential
information associated with analytical documents, such as strip charts, tabular
printouts, computer data files, analytical notebooks, and run logs. This
information includes, but is not limited to, all manual calculations
manual integrations); sample preparation; standard and reagent origin,
receipt, preparation, and use; quality control protocols and assessment; and
method performance criteria.
D. Administrative records. The laboratory shall maintain the following administrative records:
1. Personnel qualifications, experience and training records.
2. Records of demonstration of capability for each analyst or work cell.
3. A log of names, initials and signatures for all individuals who are responsible for signing or initialing any laboratory record.
A. Internal audits.
1. The laboratory shall arrange for annual internal audits to verify that its operations continue to comply with the requirements of the laboratory's quality system. It is the responsibility of the quality assurance officer to plan and organize audits as required by a predetermined schedule and requested by management.
2. Trained and qualified personnel who are, wherever resources permit, independent of the activity to be audited, shall carry out these audits. Personnel shall not audit their own activities except when it can be demonstrated that an effective audit will be carried out.
3. Where the audit findings cast doubt on the correctness or validity of the laboratory's calibrations or test results, the laboratory shall take immediate corrective action.
4. A laboratory may have an audit performed under contract by an outside source competent to audit the laboratory's operations.
B. Managerial review.
1. The laboratory management shall conduct a review, at least annually, of its quality system and its testing and calibration activities to ensure its continuing suitability and effectiveness and to introduce any necessary changes or improvements in the quality system and laboratory operations.
2. The review shall take account of reports from managerial and supervisory personnel, the outcome of recent internal audits, assessments by external bodies, the results of inter-laboratory comparisons or proficiency tests, corrective actions and other relevant factors.
3. The laboratory shall have a procedure for review by management and maintain records of review findings and actions.
4. Where the staff of a laboratory is limited to a single analyst, a supervisor may perform a managerial review.
C. Audit review. All audit and review findings and any
corrective actions that arise from them shall be documented. The laboratory
management shall ensure that these actions are discharged within the agreed
time frame timeframe ] as indicated in the quality
manual or standard operating procedures or both. For clarification,
documentation of audit and review findings should be a simple procedure,
essentially a memorandum setting out the findings of the audit and managerial
review and any action to follow.
D. Corrective actions.
1. In addition to providing acceptance criteria and specific protocols for corrective actions in the method standard operating procedures, the laboratory shall implement general procedures to be followed to determine consistently when departures from documented policies, procedures and quality control have occurred. These procedures may include but are not limited to the following:
a. Identify the individual or individuals responsible for assessing each quality control data type;
b. Identify the individual or individuals responsible for initiating or recommending corrective actions or both;
c. Define how the analyst shall treat a data set if the associated quality control measurements are unacceptable;
d. Specify how out-of-control situations and subsequent corrective actions are to be documented; and
e. Specify procedures for management (including the quality
assurance officer) to review corrective action
2. To the extent possible, samples shall be reported only if all quality control measures are acceptable. If a quality control measure is found to be out of control, and the data are to be reported, all samples associated with the failed quality control measure shall be reported with the appropriate data qualifiers.
1VAC30-45-720. Equipment and reference materials.
A. The laboratory shall be furnished with all items of equipment, including reference materials, required for the correct performance of tests for which certification is sought. The laboratory shall maintain records of reference materials sufficient to provide proper performance of tests. In those cases where the laboratory needs to use equipment outside its permanent control it shall ensure that the relevant requirements of this article are met.
B. All equipment shall be properly maintained, inspected and cleaned. Maintenance procedures shall be documented.
C. Any item of the equipment that has been subjected to overloading or mishandling, or that gives suspect results, or has been shown by verification or otherwise to be defective shall be taken out of service immediately, clearly identified as being out of service and, wherever possible, stored at a specified place until it has been repaired and shown by calibration, verification or test to perform satisfactorily. The laboratory shall examine the effect of this defect on previous calibrations or tests.
D. Each item of equipment including reference materials shall be labeled, marked or otherwise identified to indicate its calibration status.
E. Records of each major item of equipment significant to the tests performed shall be maintained. These records shall include documentation on all routine and non-routine maintenance activities. The laboratory shall maintain records of reference materials sufficient to provide proper performance of tests. The records shall include:
1. The name of the item of equipment;
2. The manufacturer's name, type identification, and serial number or other unique identification;
3. Date received and date placed in service (if available); 4. 3. Current location, where appropriate; 5. If available, condition when received (e.g., new, used,
reconditioned); 6. 4. Copy of the manufacturer's instructions,
where available; 7. 5. Dates and results of calibrations or
verifications or both and date of the next calibration or verification; 8. 6. Details of maintenance carried out to date
and planned for the future; and 9. 7. History of any damage, malfunction,
modification or repair.
1VAC30-45-730. Test methods and standard operating procedures.
A. Methods documentation.
1. The laboratory shall have documented instructions on the use and operation of all relevant equipment, on the handling and preparation of samples, and for calibration or testing, where the absence of such instructions could jeopardize the calibrations or tests.
2. All instructions, standards, manuals and reference data relevant to the work of the laboratory shall be maintained up to date and be readily available to the staff.
B. Standard operating procedures (SOPs).
1. Laboratories shall maintain SOPs that accurately reflect all phases of current laboratory activities such as assessing data integrity, corrective actions, handling customer complaints, and all test methods. These documents, for example, may be equipment manuals provided by the manufacturer or internally written documents. The test methods may be copies of published methods as long as any changes or selected options in the methods are documented and included in the laboratory methods manual.
2. The SOPs shall be organized. Each SOP shall clearly indicate the effective date of the document, the revision number, and the signature or signatures of the responsible laboratory manager or managers.
3. Copies of all SOPs shall be accessible to all personnel.
Laboratory methods manuals. SOPs for laboratory
1. The laboratory shall have and maintain an
methods manual or manuals SOP for each certified analyte or test
manual may consists of copies of published or
referenced methods or standard operating procedures that have been SOP
may be a copy of a published or referenced method or may be written by the
laboratory. In cases where modifications to the published method have been made
by the laboratory or where the referenced test method is ambiguous or provides
insufficient detail, these changes or clarifications shall be clearly
described. Each test method shall include or reference where applicable:
a. Identification of the test method;
b. Applicable matrix or matrices;
Method detection limit Limits of detection or
d. Scope and application, including
to be analyzed;
e. Summary of the test method;
i. Equipment and supplies;
j. Reagents and standards;
k. Sample collection, preservation, shipment and storage;
l. Quality control;
m. Calibration and standardization;
Calculations Data analysis and calculations;
p. Method performance;
q. Pollution prevention;
r. Data assessment and acceptance criteria for quality control measures;
s. Corrective actions for out-of-control data;
t. Contingencies for handling out-of-control or unacceptable data;
u. Waste management;
v. References; and
w. Any tables, diagrams, flowcharts and validation data.
D. Test methods.
1. Laboratories shall use (i) promulgated test methods in
accordance with the Code of Federal Regulations; (ii) test methods stated in
any current permit issued by
Virginia the State Air Pollution
Control Board, the Virginia Waste Management Board, or the State Water Control
Board; or (iii) alternate test procedures approved by the board issuing the
permit or the Department of Environmental Quality, including applicable quality
assurance requirements, and sample preservation, container, storage, and
holding time requirements. [ Laboratories shall use the latest valid
edition of a method unless it is not appropriate to do so. ]
2. The laboratory shall use appropriate test methods and procedures for all tests and related activities within its responsibility (including sample handling, transport and storage, preparation and analysis). The method and procedures shall be consistent with the accuracy required and with any standard specifications relevant to the calibrations or tests concerned.
3. When the use of reference test methods for a sample analysis is mandated, only those methods shall be used.
4. Where test methods are employed that are not required, as in the Performance Based Measurement System approach, the methods shall be fully documented and validated (see subsection E of this section).
E. Demonstration of capability.
1. Prior to acceptance and institution of any test method,
satisfactory initial demonstration of method capability is required. In
general, this demonstration does not test the performance of the method in real
world samples, but in the applicable and available clean quality system matrix
sample (a quality system matrix in which no target analytes or interferences
are present at concentrations that impact the results of a specific test
e.g. for example, drinking water, solids, biological
tissue and air. Laboratories shall follow the procedure in subsection F of this
section to demonstrate capability.
continuing ongoing demonstration
of method performance, such as laboratory control samples, is required.
3. In cases where a laboratory analyzes samples using a test
method that has been in use by the laboratory
before July 1999 for at
least one year prior to applying for certification, and there have been no
significant changes in instrument type, personnel or test method, the
continuing demonstration of method performance and the analyst's documentation
of continued proficiency shall be acceptable. The laboratory shall have records
on file to demonstrate that an initial demonstration of capability is not
4. In all cases, the laboratory shall [
retain a certification statement and shall make the statement available upon
request. The laboratory shall retain all associated supporting data necessary
to reproduce the analytical results summarized in the certification statement
document each demonstration of capability as required by subsection G of
this section ].
5. The laboratory shall complete a demonstration of capability each time there is a change in instrument type, personnel or test method, including the addition of an analyte to a certified test method.
6. In laboratories with specialized work cells (a group
consisting of analysts with specifically defined tasks that together perform
the test method), the group as a unit shall meet the criteria of this
subsection. This demonstration of capability shall be fully documented.
F. Procedure for demonstration of capability. The following
steps shall be performed for mandated test methods. However, before any results
are reported using this method, actual sample spike results may be used to meet
, (i.e., at least four consecutive matrix spikes
within the last 12 months). For analytes that do not lend themselves to
spiking , (e.g., TSS) , the demonstration of
capability may be performed using quality control samples. The laboratory may
document that other approaches to demonstration of capability are adequate.
This documentation shall be included in the laboratory's quality manual:
1. A quality control (QC) sample may be obtained from an outside source or may be prepared by the laboratory using alternate source stock standards that are prepared independently from those used in instrument calibration.
2. The analyte or analytes shall be diluted in a volume of clean quality system matrix sufficient to prepare four aliquots at the concentration specified, or if unspecified, to a concentration of 1-4 times the limit of quantitation.
3. At least four aliquots shall be prepared and analyzed according to the test method either concurrently or over a period of days.
4. Using all of the results, calculate the mean recovery in the appropriate reporting units (such as g/L) and the standard deviations of the population sample (n-1) (in the same units) for each parameter of interest. When it is not possible to determine mean and standard deviations, such as for presence or absence of the analyte and logarithmic values, the laboratory shall assess performance against established and documented criteria.
5. Compare the information from subdivision 4 of this subsection to the corresponding acceptance criteria for precision and accuracy in the test method (if applicable) or in laboratory-generated acceptance criteria (if there are not established mandatory criteria). If all parameters meet the acceptance criteria, the analysis of actual samples may begin. If any one of the parameters do not meet the acceptance criteria, the performance is unacceptable for that parameter.
6. When one or more of the tested parameters fail at least one
of the acceptance criteria, the analyst shall proceed according to either
subdivision 6 a or 6 b
below of this subsection.
a. Locate and correct the source of the problem and repeat the test for all parameters of interest beginning with subdivision 3 of this subsection.
b. Beginning with subdivision 3 of this subsection, repeat the test for all parameters that failed to meet criteria. Repeated failure, however, confirms a general problem with the measurement system. If this occurs, locate and correct the source of the problem and repeat the test for all compounds of interest beginning with subdivision 3 of this subsection.
G. Certification statement. The following
certification statement shall be used to document the completion of each
demonstration of capability. A copy of the certification statement shall be
retained in the personnel records of each affected employee. Demonstration of Capability
Date: Page __of __ Laboratory Name: Laboratory Address: Analyst(s) Name(s): Matrix: (examples: laboratory pure water, soil, air, solid,
biological tissue) Method number, SOP#, Rev#, and Analyte, or Class of Analytes
or Measured Parameters (examples: barium by 200.7, trace metals by 6010 B, benzene
by 8021 B, etc.) We, the undersigned, CERTIFY that: 1. The analysts identified above, using the cited test
method(s), which is in use at this facility for the analyses of samples under
the Virginia Environmental Laboratory Certification Program, have met the
Demonstration of Capability. 2. The test method(s) was performed by the analyst(s)
identified on this certification. 3. A copy of the test method(s) and the laboratory-specific
SOPs are available for all personnel on-site. 4. The data associated with the demonstration capability are
true, accurate, complete and self-explanatory(1). 5. All raw data (including a copy of this certification
form) necessary to reconstruct and validate these analyses have been retained
at the facility, and that the associated information is well organized and
available for review by authorized assessors. Laboratory Manager's Name and Title________________
Signature________________ Date_______ Quality Assurance Officer's Name___________________
Signature________________ Date_______ (1)True - consistent with supporting data.
Accurate - based on good laboratory practices consistent with sound scientific
principles and practices. Complete - includes the results of all supporting
performance testing. Self-explanatory - data properly labeled and stored so
that the results are clear and require no additional explanation.
G. Documentation of demonstration of capability. The laboratory shall document each demonstration of capability so that the following information shall be readily available for each employee:
1. Analyst or analysts involved in preparation and analysis.
3. Analytes, class of analytes, measured parameters, or organisms.
4. Identification of methods performed.
5. Identification of laboratory-specific SOP used for analysis, including revision number.
6. Date or dates of analysis.
7. All raw data necessary to reconstruct and validate the analyses.
8. Data evaluation required by subsection F of this section. ]
H. Sample aliquots. Where sampling (as in obtaining sample aliquots from a submitted sample) is carried out as part of the test method, the laboratory shall use documented procedures and appropriate techniques to obtain representative subsamples.
I. Data verification. Calculations and data transfers shall be subject to appropriate checks. The laboratory shall establish standard operating procedures to ensure that (i) the reported data are free from transcription and calculation errors and (ii) all quality control measures are reviewed and evaluated before data are reported. The laboratory also shall establish standard operating procedures addressing manual calculations including manual integrations.
J. Documentation and labeling of standards and reagents. Documented procedures shall exist for the reception and storage of consumable materials used for the technical operations of the laboratory.
1. The laboratory shall retain records for all standards, reagents, reference materials and media including the manufacturer/vendor, the manufacturer's Certificate of Analysis or purity (if available), the date of receipt, recommended storage conditions, and an expiration date after which the material shall not be used unless its reliability is verified by the laboratory.
2. Original containers (such as provided by the manufacturer or vendor) shall be labeled with an expiration date if this date is provided by the manufacturer or vendor.
3. Records shall be maintained on standard and reference material preparation. These records shall indicate traceability to purchased stocks or neat compounds, reference to the method of preparation, date of preparation, expiration date and preparer's initials.
4. Sufficient identification of containers of prepared reagents and standards shall be provided to ensure proper performance of tests.
K. Computers and electronic data related requirements. Where computers, automated equipment or microprocessors are used for the capture, processing, manipulation, recording, reporting, storage or retrieval of test data, the laboratory shall ensure the following:
1. Computer software developed by the user is documented in sufficient detail and is suitably validated as being adequate for use.
2. Procedures are established and implemented for protecting the integrity of data, such as integrity of data entry or capture, data storage, data transmission and data processing.
3. Computer and automated equipment are maintained to ensure proper functioning and provided with the environmental and operating conditions necessary to maintain the integrity of calibration and test data.
4. Appropriate procedures are established and implemented for the maintenance of security of data including the prevention of unauthorized access to, and the unauthorized amendment of, computer records.
1VAC30-45-740. Measurement traceability and calibration.
A. General requirements. All equipment used for environmental tests, including equipment for subsidiary measurements (e.g., for environmental conditions) having a significant effect on the accuracy or validity of the result of the environmental test or sampling shall be calibrated before being put into service and on a continuing basis. The laboratory shall have an established program and procedure for the calibration of its equipment. This includes balances, thermistors, thermometers and control standards. Such a program shall include a system for selecting, using, calibrating, checking, controlling and maintaining measurement standards, reference materials used as measurement standards, and measuring and test equipment used to perform environmental tests.
B. Traceability of calibration.
1. The laboratory shall ensure that the equipment used can provide the uncertainty of measurement needed.
2. The overall program of calibration or verification or both and validation of equipment shall be designed and operated so as to ensure that measurements made by the laboratory are traceable to national standards of measurement.
3. Where traceability of measurements to the International
System of Units (SI) is not possible or not relevant, the same requirements for
traceability to, for example, certified reference materials, agreed methods
or consensus standards, are required. The laboratory shall provide
satisfactory evidence of correlation of results, for example by participation
in a suitable program of inter-laboratory comparisons, proficiency testing, or
C. Reference standards and reference materials.
1. Reference standards. The laboratory shall have a program and procedure for the calibration of its reference standards. Reference standards of measurement shall be calibrated by a body that can provide traceability as described in subsection B of this section. Such reference standards of measurement held by the laboratory (such as Class S or equivalent weights or traceable thermometers) shall be used for calibration only and for no other purpose, unless it can be demonstrated that their performance as reference standards would not be invalidated. Where commercially available, this traceability shall be to a national standard of measurement.
2. Reference materials. Reference materials shall, where commercially available, be traceable to SI units of measurement, or to certified reference materials. Where possible, traceability shall be to national or international standards of measurement, or to national or international standard reference materials. Internal reference materials shall be checked as far as is technically and economically practicable.
D. Calibration. Calibration requirements are divided into two parts: (i) requirements for analytical support equipment and (ii) requirements for instrument calibration. In addition, the requirements for instrument calibration are divided into initial instrument calibration and continuing instrument calibration verification.
1. Support equipment. These standards apply to all devices that may not be the actual test instrument, but are necessary to support laboratory operations. These include but are not limited to balances, ovens, refrigerators, freezers, incubators, water baths, temperature measuring devices (including thermometers and thermistors), thermal/pressure sample preparation devices and volumetric dispensing devices (such as Eppendorf®, or automatic dilutor or dispensing devices) if quantitative results are dependent on their accuracy, as in standard preparation and dispensing or dilution into a specified volume.
a. All support equipment shall be maintained in proper working order. The records of all repair and maintenance activities, including service calls, shall be kept.
b. All support equipment shall be calibrated or verified at least annually, using NIST traceable references when available, over the entire range of use. The results of such calibration shall be within the specifications required of the application for which this equipment is used. If not, the laboratory shall either (i) remove the equipment from service until repaired or (ii) maintain records of established correction factors to correct all measurements.
c. Raw data records shall be retained to document equipment performance.
Prior to use on each working day On each day the
equipment is used, balances, ovens, refrigerators, freezers, and water
baths shall be checked in the expected use range, with NIST traceable
references where available. The acceptability for use or continued use shall be
according to the needs of the analysis or application for which the equipment
is being used.
e. Mechanical volumetric dispensing devices including burettes (except Class A glassware) shall be checked for accuracy on at least a quarterly use basis. Glass microliter syringes are to be considered in the same manner as Class A glassware, but shall come with a certificate attesting to established accuracy or the accuracy shall be initially demonstrated and documented by the laboratory.
f. For chemical tests, the temperature, cycle time and pressure of each run of autoclaves shall be documented by the use of appropriate chemical indicators or temperature recorders and pressure gauges.
g. For biological tests that employ autoclave sterilization, the following requirements apply:
(1) The performance of each autoclave shall be initially evaluated by establishing its functional properties and performance, for example heat distribution characteristics with respect to typical uses. Autoclaves shall meet specified temperature tolerances. Pressure cookers fitted only with a pressure gauge are not recommended for sterilization of media or decontamination of wastes.
(2) Records of autoclave operations including temperature and time shall be maintained. This shall be done for every cycle. Acceptance and rejection criteria shall be established and used to evaluate the autoclave efficiency and effectiveness.
2. Instrument calibration.
a. This standard specifies the essential elements that define the procedures and documentation for initial instrument calibration and continuing instrument calibration verification to ensure that the data shall be of known quality and be appropriate for a given regulation or decision. This standard does not specify detailed procedural steps for calibration, but establishes the essential elements for selection of the appropriate technique or techniques. If more stringent standards or requirements are included in a mandated test method or by regulation, the laboratory shall demonstrate that such requirements are met. If it is not apparent which standard is more stringent, then the requirements of the regulation or mandated test method are to be followed.
b. Initial instrument calibrations. The following items are essential elements of initial instrument calibration:
(1) The laboratory shall include or reference the details of the initial instrument calibration procedures, including calculations, integrations, acceptance criteria and associated statistics in the standard operating procedure for the test method. When initial instrument calibration procedures are referenced in the test method, then the laboratory shall retain the referenced material and make it available for review.
(2) The laboratory shall retain sufficient raw data records to
permit reconstruction of the initial instrument calibration
calibration date, test method, instrument, analysis date, each analyte name,
analyst's initials or signature, concentration and response, calibration curve
or response factor, or unique equation or coefficient used to reduce instrument
responses to concentration).
(3) Sample results shall be quantitated from the initial instrument calibration and may not be quantitated from any continuing instrument calibration verification unless otherwise required by regulation, method, or program.
(4) All initial instrument calibrations shall be verified with a standard obtained from a second manufacturer or lot. Traceability shall be to a national standard, when available. This element does not apply to laboratories performing only simple test procedures.
(5) Criteria for the acceptance of an initial instrument
calibration shall be established
, (e.g., correlation coefficient
and relative percent difference). The criteria used shall be 0.995 or
greater for the calibration coefficient unless a different criterion is
included in the method being used.
(6) Results of samples not bracketed by initial calibration
standards (within calibration range) shall be reported as having less certainty
(e.g., defined qualifiers or flags or explained in the case narrative).
The lowest calibration standard shall be above the detection limit.
(7) If the initial instrument calibration results are outside established acceptance criteria, corrective actions shall be performed. Data associated with an unacceptable initial instrument calibration shall not be reported.
(8) Calibration standards shall include concentrations at or below the regulatory limit or decision level, if these limits or levels are known by the laboratory, unless these concentrations are below the laboratory's demonstrated detection limits.
(9) If a reference or mandated method does not specify the number of calibration standards, the minimum number is two, not including blanks or a zero standard. The laboratory shall have a standard operating procedure for determining the number of points for establishing the initial instrument calibration.
c. Continuing instrument calibration verification.
(1) When an initial instrument calibration is not performed on the day of analysis, the validity of the initial calibration shall be verified prior to sample analyses by a continuing instrument calibration check with each analytical batch. This provision does not apply to laboratories performing only simple test procedures.
(2) The following items are essential elements of continuing instrument calibration verification:
(a) The laboratory shall include or reference the details of the continuing instrument calibration procedure, calculations and associated statistics in the standard operating procedure for the test method.
(b) The laboratory shall verify calibration for each compound, element, or other discrete chemical species, except for multicomponent analytes such as Aroclors, Total Petroleum Hydrocarbons, or Toxaphene where a representative chemical related substance or mixture can be used.
(c) The laboratory shall perform a continuing instrument calibration verification as follows:
(i) At the beginning and end of each analytical batch. If an internal standard is used, only one verification needs to be performed at the beginning of the analytical batch;
(ii) Whenever it is expected that the analytical system may be out of calibration or might not meet the verification acceptance criteria;
(iii) If the time period for calibration or the most previous calibration verification has expired; or
(iv) For analytical systems that contain a calibration verification requirement.
(d) Sufficient raw data records shall be retained to permit
reconstruction of the continuing instrument calibration verification
or test method, instrument, analysis date, each analyte name, concentration and
response, calibration curve or response factor, or unique equations or
coefficients used to convert instrument responses into concentrations).
Continuing calibration verification records shall explicitly connect the
continuing verification data to the initial instrument calibration.
(e) Criteria for the acceptance of a continuing instrument
calibration verification shall be established
, (e.g., percent
recovery or relative percent difference).
(f) If the continuing instrument calibration verification results obtained are outside established acceptance criteria, corrective actions shall be performed. If routine corrective action procedures fail to produce a second consecutive (immediate) calibration verification within acceptance criteria, then either the laboratory has to demonstrate acceptable performance after corrective action with two consecutive successful calibration verifications, or a new initial instrument calibration shall be performed. If the laboratory has not verified calibration, sample analyses shall not occur until the analytical system is calibrated or calibration verified. If samples are analyzed using a system on which the calibration has not yet been verified, the results shall be flagged. Data associated with an unacceptable calibration verification may be fully useable under the following special conditions:
(i) When the acceptance criteria for the continuing
calibration verification are exceeded high
, (i.e., high bias ,)
and there are associated samples that are nondetects, then those nondetects may
be reported. Otherwise the samples affected by the unacceptable calibration
verification shall be reanalyzed after a new calibration curve has been established,
evaluated and accepted.
(ii) When the acceptance criteria for the continuing
calibration verification are exceeded low
, (i.e., low bias ,)
those sample results may be reported if they exceed a maximum regulatory limit
or decision level. Otherwise the samples affected by the unacceptable
verification shall be reanalyzed after a new calibration curve has been
established, evaluated and accepted.
1VAC30-45-750. Quality assurance.
A. General. The laboratory shall have quality control procedures for monitoring the validity of environmental tests undertaken. The resulting data shall be recorded in such a way that trends are detectable and, where practicable, statistical techniques shall be applied to the reviewing of the results. This monitoring shall be planned and reviewed and may include, but not be limited to, the following:
1. Regular use of certified reference materials
internal quality control using secondary reference materials or both.
2. Participation in interlaboratory comparison or proficiency testing program.
3. Replicate tests using the same or different methods.
4. Retesting of retained samples.
5. Correlation of results for different characteristics of a
(for example (e.g., total phosphate should be greater than
or equal to orthophosphate).
B. Essential quality control procedures. The general quality
control principles in [
subsections subsection ] C
[ through F ] of this section shall apply, where applicable,
to all environmental laboratories. The manner in which they are implemented is
dependent on the types of tests performed by the laboratory. 1VAC30-45-760
through 1VAC30-45-829 specify quality control requirements for specific test
types. 1VAC30-45-770 through 1VAC30-45-775, 1VAC30-45-790 through
1VAC30-45-798, and 1VAC30-45-810 through 1VAC30-45-818 specify quality control
requirements for chemical testing, microbiological testing, and air testing,
respectively. Noncommercial environmental laboratories that analyze
environmental samples using other types of testing such as toxicity,
radiochemical, or asbestos testing shall meet the quality control standards for
the specific method and the specific type of testing in the 2009 TNI Standards
for Environmental Laboratories. The standards for any given test type shall
assure that the applicable principles are addressed.
C. All laboratories shall have detailed written protocols in place to monitor the following quality controls:
1. Positive and negative controls to monitor tests such as blanks, spikes, reference toxicants.
2. Tests to define the variability or repeatability of the laboratory results or both such as replicates.
3. Measures to assure the accuracy of the test method including calibration or continuing calibrations or both, use of certified reference materials, proficiency test samples, or other measures.
4. Measures to evaluate test method capability, such as method detection limits and quantitation limits or range of applicability such as linearity.
5. Selection of appropriate formulae to reduce raw data to final results such as regression analysis, comparison to internal and external standard calculations, and statistical analyses.
6. Selection and use of reagents and standards of appropriate quality.
7. Measures to assure the selectivity of the test for its intended purpose.
8. Measures to assure constant and consistent test conditions (both instrumental and environmental) where required by the test method such as temperature, humidity, light, or specific instrument conditions.
1VAC30-45-760. Quality control requirements.
1. The quality control protocols specified by the laboratory's
manual SOPs shall be followed (1VAC30-45-730 C). The laboratory shall
ensure that either the (i) applicable essential standards outlined in this
section through 1VAC30-45-829 1VAC30-45-775, 1VAC30-45-791 through
1VAC30-45-798, and 1VAC30-45-811 or (ii) mandated methods or regulations,
whichever are more stringent, are incorporated into their method manuals
SOPs. When it is not apparent which is more stringent, the quality control
controls in the mandated method or regulations is are to
2. All quality control measures shall be assessed and evaluated on an ongoing basis and quality control acceptance criteria shall be used to determine the validity of the data. The laboratory shall have procedures for the development of acceptance/rejection criteria where no method or regulatory criteria exists.
B. Initial test method evaluation. For all test methods other
toxicity and microbiology, the requirements of subdivisions 1 and 2
of this subsection apply. For toxicity and microbiology testing, the
initial test method evaluation requirements are contained in 1VAC30-45-780
through 1VAC30-45-788 and 1VAC30-45-790 through 1VAC30-45-798 ,
respectively. For the evaluation of precision and bias (subdivision 3 of
this subsection), the requirements of subdivision 3 a of this subsection apply
to standard methods. The requirements of subdivision 3 b of this subsection
apply to the methods referenced in that subdivision.
1. Limit of detection (LOD).
a. The laboratory shall determine the LOD for the method for each target analyte of concern in the quality system matrices. All sample processing steps of the analytical method shall be included in the determination of the LOD.
b. The validity of the LOD shall be confirmed by qualitative
identification of the [
analyte(s) analyte ] in a
quality control sample in each quality system matrix containing the analyte at
no more than two to three times the LOD for single analyte tests and one to
four times the LOD for multiple analyte tests. This verification shall be
performed on every instrument that is to be used for analysis of samples and
reporting of data.
c. An LOD study is not required for any component for which
spiking solutions or quality control samples are not available such as
temperature, or, when test results are not to be reported to the LOD (versus
the limit of quantitation or working range of instrument calibration),
according to 1VAC30-45-771
, 1VAC30-45-805, and 1VAC30-45-814 ,
and 1VAC30-45-826. Where an LOD study is not performed, the laboratory may
not report a value below the limit of quantitation.
2. Limit of quantitation (LOQ).
a. The laboratory shall determine the LOQ for each analyte of concern according to a defined, documented procedure.
b. The LOQ study is not required for any component or property for which spiking solutions or quality control samples are not commercially available or otherwise inappropriate (e.g., pH).
c. The validity of the LOQ shall be confirmed by successful analysis of a QC sample containing the analytes of concern in each quality system matrix one to two times the claimed LOQ. A successful analysis is one where the recovery of each analyte is within the established test method acceptance criteria or client data quality objectives for accuracy. This single analysis is not required if the bias and precision of the measurement system is evaluated at the LOQ.
3. Evaluation of precision and bias.
a. Standard methods. The laboratory shall evaluate the precision and bias of a standard method for each analyte of concern for each quality system matrix according to either of the following:
(1) The single-concentration four-replicate recovery study procedures in 1VAC30-45-730 F; or
(2) An alternate procedure documented in the quality manual when the analyte cannot be spiked into the sample matrix and quality control samples are not commercially available.
b. Nonstandard methods.
(1) For laboratory-developed test methods or nonstandard test methods that were not in use by the laboratory before July 2003, the laboratory shall have a documented procedure to evaluate precision and bias. The laboratory shall also compare results of the precision and bias measurements with criteria given in the reference method or criteria established by the laboratory.
(2) Precision and bias measurements shall evaluate the method across the analytical calibration range of the method. The laboratory shall also evaluate precision and bias in the relevant quality system matrices and shall process the samples through the entire measurement system for each analyte of interest.
(3) The following are examples of a systematic approach to evaluate precision and bias:
(a) Example 1. Analyze QC samples in triplicate containing the analytes of concern at or near the limit of quantitation, at the upper-range of the calibration (upper 20%) and at a mid-range concentration. Process these samples on different days as three sets of samples through the entire measurement system for each analyte of interest. Each day one QC sample at each concentration is analyzed. A separate method blank shall be subjected to the analytical method along with the QC samples on each of the three days. (Note that the three samples at the LOQ concentration can demonstrate sensitivity as well.) For each analyte, calculate the mean recovery for each day, for each level over days, and for all nine samples. Calculate the relative standard deviation for each of the separate means obtained. Compare the standard deviations for the different days and the standard deviations for the different concentrations. If the different standard deviations are all statistically insignificant (e.g., F-test), then compare the overall mean and standard deviation with the established criteria from above.
(b) Example 2. A validation protocol such as the Tier I, Tier II, and Tier III requirements in U.S. EPA Office of Water's Alternate Test Procedure (ATP) approval process.
4. Evaluation of selectivity. The laboratory shall evaluate selectivity by following the checks established within the method. These checks may include mass spectral tuning, second column confirmation, ICP inter-element interference checks, chromatography retention time windows, sample blanks, spectrochemical absorption or fluorescence profiles, co-precipitation evaluations, and electrode response factors.
1VAC30-45-770. Chemical testing: positive and negative controls.
A. Negative control method performance.
1. Purpose. The method blank is used to assess the preparation batch for possible contamination during the preparation and processing steps. The method blank shall be processed along with and under the same conditions as the associated samples to include all steps of the analytical procedure. Procedures shall be in place to determine if a method blank is contaminated. Any affected samples associated with a contaminated method blank shall be reprocessed for analysis or the results reported with appropriate data qualifying codes.
2. Frequency. The method blank shall be analyzed at a minimum
of one per preparation batch. In those instances for which no separate
preparation method is used
(example: (e.g., volatiles in water)
the batch shall be defined as environmental samples that are analyzed together
with the same method and personnel, using the same lots of reagents, not to
exceed the analysis of 20 environmental samples.
3. Composition. The method blank shall consist of a quality system matrix that is similar to the associated samples and is known to be free of the analytes of interest.
4. Evaluation criteria and corrective action. While the goal is to have no detectable contaminants, each method blank shall be critically evaluated as to the nature of the interference and the effect on the analysis of each sample within the batch. The source of contamination shall be investigated and measures taken to minimize or eliminate the problem and affected samples reprocessed or data shall be appropriately qualified if:
a. The concentration of a targeted analyte in the blank is at or above the reporting limit as established by the test method or by regulation, and is greater than 1/10 of the amount measured in any sample.
b. The blank contamination otherwise affects the sample results as per the test method requirements or the individual project data quality objectives.
c. When a blank is determined to be contaminated, the cause shall be investigated and measures taken to minimize or eliminate the problem. Samples associated with a contaminated blank shall be evaluated as to the best corrective action for the samples (e.g., reprocessing or data qualifying codes). In all cases the corrective action shall be documented.
B. Positive control method performance. Laboratory control sample (LCS).
1. Purpose. The LCS is used to evaluate the performance of the total analytical system, including all preparation and analysis steps. Results of the LCS are compared to established criteria and, if found to be outside of these criteria, indicates that the analytical system is "out of control." Any affected samples associated with an out of control LCS shall be reprocessed for re-analysis or the results reported with appropriate data qualifying codes.
2. Frequency. The LCS shall be analyzed at a minimum of one per preparation batch. Exceptions would be for those analytes for which no spiking solutions are available such as total suspended solids, total dissolved solids, total volatile solids, total solids, pH, color, odor, temperature, dissolved oxygen or turbidity. In those instances for which no separate preparation method is used (example: volatiles in water) the batch shall be defined as environmental samples that are analyzed together with the same method and personnel, using the same lots of reagents, not to exceed the analysis of 20 environmental samples.
3. Composition. The LCS is a quality system matrix, known to be free of analytes of interest, spiked with known and verified concentrations of analytes. NOTE: the matrix spike may be used in place of this control as long as the acceptance criteria are as stringent as for the LCS. Alternatively the LCS may consist of a media containing known and verified concentrations of analytes or as Certified Reference Material (CRM). All analyte concentrations shall be within the calibration range of the methods. The following shall be used in choosing components for the spike mixtures:
The components to be spiked shall be as specified by the mandated test method or other regulatory requirement or as requested by the client. In the absence of specified spiking components the laboratory shall spike per the following:
a. For those components that interfere with an accurate assessment such as spiking simultaneously with technical chlordane, toxaphene and PCBs, the spike should be chosen that represents the chemistries and elution patterns of the components to be reported.
b. For those test methods that have extremely long lists of
analytes, a representative number may be chosen. The analytes selected should
be representative of all analytes reported. The following criteria shall be
used for determining the minimum number of analytes to be spiked. However, the
laboratory shall insure that all targeted components are included in the spike
mixture over a two-year period. For methods that include 1-10 targets, spike
all components; for methods that include 11-20 targets, spike at least
10 components or 80%, whichever is greater; and for methods with more
than 20 targets, spike at least 16 components.
4. Evaluation criteria and corrective action.
a. The results of the individual batch LCS are calculated in percent recovery or other appropriate statistical technique that allows comparison to established acceptance criteria. The laboratory shall document the calculation.
b. The individual LCS is compared to the acceptance criteria as published in the mandated test method. Where there are no established criteria, the laboratory shall determine internal criteria and document the method used to establish the limits or utilize client specified assessment criteria.
c. A LCS that is determined to be within the criteria effectively establishes that the analytical system is in control and validates system performance for the samples in the associated batch. Samples analyzed along with a LCS determined to be "out of control" shall be considered suspect and the samples reprocessed and re-analyzed or the data reported with appropriate data qualifying codes.
5. If a large number of analytes are in the LCS, it becomes statistically likely that a few will be outside control limits. This may not indicate that the system is out of control, therefore corrective action may not be necessary. Upper and lower marginal exceedance (ME) limits can be established to determine when corrective action is necessary. A ME is defined as being beyond the LCS control limit (3 standard deviations), but within the ME limits. ME limits are between 3 and 4 standard deviations around the mean.
a. The number of allowable marginal exceedances is based on the number of analytes in the LCS. If more analytes exceed the LCS control limits than is allowed, or if any one analyte exceeds the ME limits, the LCS fails and corrective action is necessary. This marginal exceedance approach is relevant for methods with long lists of analytes. It will not apply to target analyte lists with fewer than 11 analytes.
b. The number of allowable marginal exceedances is as follows:
Number of analytes in LCS
Number of analytes allowed in ME of the LCS control limit
Greater than 90
Fewer than 11
c. Marginal exceedances shall be random. If the same analyte exceeds the LCS control limit repeatedly, it is an indication of a systemic problem. The source of the error shall be located and corrective action taken. Laboratories shall have a written procedure to monitor the application of marginal exceedance allowance to the LCS to ensure random behavior.
C. Sample specific controls - general.
1. The laboratory shall document procedures for determining the effect of the sample matrix on method performance. These procedures relate to the analyses of quality system matrix specific Quality Control (QC) samples and are designed as data quality indicators for a specific sample using the designated test method. These controls alone are not used to judge laboratory performance.
2. Examples of matrix specific QC include: Matrix Spike (MS); Matrix Spike Duplicate (MSD); sample duplicates; and surrogate spikes. The laboratory shall have procedures in place for tracking, managing, and handling matrix specific QC criteria including spiking appropriate components at appropriate concentrations, calculating recoveries and relative percent difference, evaluating and reporting results based on performance of the QC samples.
D. Sample specific controls - matrix spike and matrix spike duplicates.
1. Purpose. Matrix specific QC samples indicate the effect of the sample matrix on the precision and accuracy of the results generated using the selected method. The information from these controls is sample/matrix specific and would not normally be used to determine the validity of the entire batch.
2. Frequency. The frequency of the analysis of matrix specific samples shall be determined as part of a systematic planning process (e.g., Data Quality Objectives) or as specified by the test method.
3. Composition. The components to be spiked shall be as specified by the mandated test method. Any permit specified analytes, as specified by regulation or client requested analytes shall also be included. If there are no specified components, the laboratory shall spike per the following:
a. For those components that interfere with an accurate assessment such as spiking simultaneously with technical chlordane, toxaphene and PCBs, the spike should be chosen that represents the chemistries and elution patterns of the components to be reported.
b. For those test methods that have extremely long lists of analytes, a representative number may be chosen using the following criteria for choosing the number of analytes to be spiked. However, the laboratory shall insure that all targeted components are included in the spike mixture over a two-year period.
(1) For methods that include 1-10 targets, spike all components;
(2) For methods that include 11-20 targets, spike at least
10 components or 80%, whichever is greater;
(3) For methods with more than 20 targets, spike at least 16 components.
4. Evaluation criteria and corrective action.
a. The results from matrix spike/matrix spike duplicate are primarily designed to assess the precision and accuracy of analytical results in a given matrix and are expressed as percent recovery (%R), relative percent difference (RPD), or other appropriate statistical technique that allows comparison to established acceptance criteria. The laboratory shall document the calculation for %R, RPD or other statistical treatment used.
b. The results are compared to the acceptance criteria as published in the mandated test method. Where there are no established criteria, the laboratory shall determine internal criteria and document the method used to establish the limits. For matrix spike results outside established criteria corrective action shall be documented or the data reported with appropriate data qualifying codes.
E. Sample specific controls - matrix duplicates.
1. Purpose. Matrix duplicates are defined as replicate aliquots of the same sample taken through the entire analytical procedure. The results from this analysis indicate the precision of the results for the specific sample using the selected method. The matrix duplicate provides a usable measure of precision only when target analytes are found in the sample chosen for duplication.
2. Frequency. The frequency of the analysis of matrix duplicates may be determined as part of a systematic planning process (e.g., Data Quality Objectives) or as specified by the mandated test method.
3. Composition. Matrix duplicates are performed on replicate aliquots of actual samples. The composition is usually not known.
4. Evaluation criteria and corrective action.
a. The results from matrix duplicates are primarily designed to assess the precision of analytical results in a given matrix and are expressed as relative percent difference (RPD) or another statistical treatment (e.g., absolute differences). The laboratory shall document the calculation for relative percent difference or other statistical treatments.
b. Results are compared to the acceptance criteria as published in the mandated test method. Where there are no established criteria, the laboratory shall determine internal criteria and document the method used to establish the limits. For matrix duplicates results outside established criteria corrective action shall be documented or the data reported with appropriate data qualifying codes.
F. Sample specific controls - surrogate spikes.
1. Purpose. Surrogates are used most often in organic chromatography test methods and are chosen to reflect the chemistries of the targeted components of the method. Added prior to sample preparation/extraction, they provide a measure of recovery for every sample matrix.
2. Frequency. Except where the matrix precludes its use or when not commercially available, surrogate compounds shall be added to all samples, standards, and blanks for all appropriate test methods.
3. Composition. Surrogate compounds are chosen to represent the
various chemistries of the target analytes in the method or [
quality objectives ]. They are often specified by the mandated method
and are deliberately chosen for their being unlikely to occur as an
environmental contaminant. Often this is accomplished by using deuterated
analogs of select compounds.
4. Evaluation criteria and corrective action. The results are compared to the acceptance criteria as published in the mandated test method. Where there are no established criteria, the laboratory should determine internal criteria and document the method used to establish the limits. Surrogates outside the acceptance criteria shall be evaluated for the effect indicated for the individual sample results. Data quality objectives or other site-specific requirements may guide the appropriate corrective action. Results reported from analyses with surrogate recoveries outside the acceptance criteria should include appropriate data qualifiers.
1VAC30-45-771. Chemical testing: limit of detection and limit of quantitation.
A. General. All procedures used shall be documented. Documentation shall include the quality system matrix type. All supporting data shall be retained.
B. Limit of detection (LOD). The laboratory shall utilize a test method that provides an LOD that is appropriate and relevant for the intended use of the data. An LOD is not required for a test method when test results are not reported outside of the calibration range. LODs shall be determined by the protocol in the mandated test method or applicable regulation. If the protocol for determining LODs is not specified, the selection of the procedure shall reflect instrument limitations and the intended application of the test method.
1. The LOD shall be initially determined for the compounds of interest in each test method in a quality system matrix in which there are no target analytes or interferences at a concentration that would impact the results. Alternatively the LOD shall be determined in the quality system matrix of interest (see definition of matrix).
2. LODs shall be determined each time there is a change in the test method that affects how the test is performed, or when a change in instrumentation occurs that affects the sensitivity of the analysis.
3. The laboratory shall have established procedures to
relate LOD with LOQ. 4. 3. The LOD shall be verified annually for each
quality system matrix, method and analyte according to the procedure specified
in 1VAC30-45-760 B 1.
C. Limit of quantitation (LOQ).
1. Any established LOQ shall be above the LOD.
2. The LOQ shall be verified annually for each quality system
matrix, method and analyte according to the procedure specified in
1VAC30-45-760 B 2. Alternatively, the annual LOQ verification is not required
if the LOD is reevaluated or verified according to subdivision B [
3 ] of this section.
1VAC30-45-775. Chemical testing: constant and consistent test conditions.
A. The laboratory shall assure that the test instruments consistently operate within the specifications required of the application for which the equipment is used.
B. Glassware cleaning. Glassware shall be cleaned to meet
the sensitivity of the test method. C. B. Any cleaning and storage procedures that
are not specified by the test method shall be documented in laboratory records
Toxicity testing: general. (Repealed.) These standards apply to laboratories measuring the
toxicity and/or bioaccumulation of contaminants in effluents (aquatic
toxicity), receiving waters, sediments, elutriates, leachates and soils. In
addition to the essential quality control standards set out in 1VAC30-45-781
through 1VAC30-45-788, some methods may have additional or other requirements
based on factors such as the type of quality system matrix evaluated.
Toxicity testing: positive and negative
controls. (Repealed.) A. Positive control. Reference toxicant tests demonstrate a
laboratory's ability to obtain consistent results with the test method and evaluate
the overall health and sensitivity of test organisms over time. 1. The laboratory shall demonstrate its ability to obtain
consistent results with standard reference toxicants (SRT) and complete an
initial Demonstration of Capability (DOC) in order to attain accreditation in
toxicity testing methods. a. An initial DOC shall consist of five or more acceptable
SRT tests for each test method, species and endpoint with different batches of
organisms. Appropriate negative controls (water, sediment, or soil) shall be
tested at the frequency and duration specified in the test method. Initial DOCs
shall be prepared in accordance with the requirements of 1VAC30-45-730 F. b. Initial DOC is established by maintenance of SRT test
results on control charts. A laboratory shall record the control performance
and statistical endpoints (such as NOEC or ECp) for each method species and
endpoint on control charts. Initial DOC is established where 95% of the test
results required in subdivision A 1 a of this section fall within the control
limits established in accordance with subdivision A 1 c of this section and
meet test acceptability criteria (TAC). The laboratory shall evaluate precision
(i.e., coefficient of variation (CV)) or sensitivity (i.e., statistical minimum
significant difference (SMSD) measures; see subdivision A 1 d of this section)
for these tests against method-specific or, lacking the former,
laboratory-derived criteria to determine validity of the initial DOC. c. For endpoints that are point estimates (ICp, ECp),
control charts are constructed by plotting the cumulative mean and the control
limits that consist of the upper and lower 95% confidence limits (+/- 2
standard deviations). In case of highly variable point estimates that exceed
method-specific criteria, the control chart limits are adjusted accordingly.
For endpoints from hypothesis tests (NOEC, NOAEC), the values are plotted
directly and the control limits consist of one concentration interval above and
below the concentration representing the central tendency (i.e., the mode). d. For endpoints that are point estimates, the cumulative
mean CV is calculated and for endpoints from hypothesis tests, the SMSD is
calculated. These values are maintained on a control chart. 2. Ongoing laboratory performance shall be demonstrated by
routine SRT testing for each test method and species and endpoint in accordance
with the minimum frequency requirements specified in subdivision A 3 of this
section. a. Intralaboratory precision is determined on an ongoing basis
through the use of control charts as established in subdivision A 1 b of this
section. The control charts shall be plotted as point estimate values, such as
EC25 for chronic tests and LC50 for acute tests, or as appropriate hypothesis
test values, such as the NOEC or NOAEC, over time within a laboratory. b. After initial laboratory DOC is determined, the control
limits and CV for an individual test method, endpoints and species shall be
adjusted as additional test results are obtained. After 20 data points are
collected for a test method and species, the control chart is maintained using
only the last 20 data points, i.e., each successive mean value and control
limit is calculated using only the last 20 values. c. Control chart limits are expected to be exceeded
occasionally regardless of how well a laboratory performs. Acceptance limits
for point estimates (ICp, ECp) that are based on 95% confidence limits should
theoretically be exceeded for one in 20 tests. Depending on the dilution factor
and test sensitivity, control charts based on hypothesis test values (NOEC,
NOAEC) may be expected to be exceeded on a similar frequency. Test results that
fall outside of control chart limits at a frequency of 5.0% or less, or that
fall just outside control chart limits (especially in the case of highly
proficient laboratories that may develop relatively narrow acceptance limits
over time), are not rejected de facto. Such data are evaluated in comparison
with control chart characteristics including the width of the acceptance limits
and the degree of departure of the value from acceptance limits. d. Consistent with the test methods used, laboratories
shall develop acceptance/rejection policies for SRT data that consider the
source of test organisms, the direction of the deviation, test dilution factor,
test sensitivity (for hypothesis test values), testing frequency,
out-of-control test frequency, relative width of acceptance limits, inter-test
CV, and degree of difference between test results and acceptance limits. e. In the case of reference toxicant data that fails to
meet control chart acceptance criteria, the test data are examined for defects,
corrective action taken, and the test repeated if necessary, using a different
batch of organisms or the data is qualified. 3. The frequency of ongoing laboratory reference toxicant
testing shall be as follows unless the method specifically requires less
frequent SRT tests (e.g., sediment tests): a. For test methods conducted at a frequency of monthly or
greater, SRT tests shall be conducted at an ongoing frequency of monthly. b. For test methods and species commonly used in the
laboratory, but that are tested at a frequency of less than monthly, SRT tests
shall be conducted concurrently with the environmental test. c. If the test organisms are obtained from an outside
source the sensitivity of each batch of organisms received from a supplier
shall be determined via a concurrent SRT test unless the supplier can provide
control chart data for the last five SRT tests using the same SRT and test
conditions. Supplied SRT data may not be older than six months. d. The DOC for an analyst shall be consistent with
1VAC30-45-220 B but the frequency need not exceed the method-specified
requirements and subdivision A 3 a and A 3 b of this section. 4. These standards do not currently specify a particular
reference toxicant and dilution series. If the permitting authority identifies
a reference toxicant or dilution series for a particular test, the laboratory
shall follow the specified requirements. All reference toxicant tests conducted
for a given test method and species shall use the same reference toxicant, test
concentrations, dilution water and data analysis methods. A dilution factor of
0.5x or greater shall be used for both acute and chronic tests. 5. The reference toxicant tests shall be conducted following
the same procedures as the environmental toxicity tests for which the precision
is being evaluated, unless otherwise specified in the test method (for example,
10-day sediment tests employ 96-h water-only reference toxicant tests). The
test duration, laboratory dilution water, feeding, organism age, range and
density, test volumes, renewal frequency, water quality measurements, and the
number of test concentrations, replicates and organisms per replicate shall be
the same as specified for the environmental toxicity test. B. Negative control: control, brine control, control
sediment, control soil or dilution water. 1. The standards for the use, type and frequency of testing
of negative controls are specified by the test methods and by permit or
regulation and shall be followed. A negative control is included with each test
to evaluate test performance and the health and sensitivity of the specific
batch of organisms. 2. Appropriate additional negative controls shall be
included when sample adjustments (for example, addition of thiosulfate for
dechlorination) or solvent carriers are used in the test. 3. Test acceptability criteria (TAC). The test acceptability
criteria specified in the test method shall be achieved for both the reference
toxicant and the effluent or environmental sample toxicity test. The criteria
shall be calculated and shall meet the method specified requirements for
performing toxicity tests.
Toxicity testing: variability and/or
reproducibility. (Repealed.) Intralaboratory precision shall be determined on an ongoing
basis through the use of further reference toxicant tests and related control charts
as described in 1VAC30-45-840 A.
Toxicity testing: accuracy. (Repealed.) This principle is not applicable to toxicity testing.
Toxicity testing: test sensitivity. (Repealed.) A. The statistical minimum significant difference (SMSD)
shall be calculated according to the formula specified by the test method and
reported with the test results. B. Point estimates: (LCp, ICp, or ECp) Confidence intervals
shall be reported as a measure of the precision around the point estimate
value, when the calculation is possible. C. The SMSD shall be calculated and reported for only
hypothesis test values, such as the NOEC or NOAEC.
Toxicity testing: selection of appropriate
statistical analysis methods. (Repealed.) A. If required, methods of data analysis and endpoints are
specified by language in the regulation, permit or the test method. B. Dose response curves. The data shall be plotted in the
form of a curve relating the dose of the chemical or concentration of sample to
cumulative percentage of test organisms demonstrating a response such as death.
Evaluation criteria shall be established for interpretation of concentration or
dose response curves.
Toxicity testing: selection and use of
reagents and standards. (Repealed.) A. The grade of all reagents used in toxicity tests is
specified in the test method except the reference standard. All reference standards
shall be prepared from chemicals that are analytical reagent grade or better.
The preparation of all standards and reference toxicants shall be documented. B. All standards and reagents associated with chemical
measurements, such as dissolved oxygen, pH or specific conductance, shall
comply with the standards outlined in 1VAC30-45-740 D 1 d. C. Only reagent-grade water collected from distillation or
deionization units is used to prepare reagents.
Toxicity testing: selectivity. (Repealed.) The permit or regulation specifies the selectivity of the
Toxicity testing: constant and consistent test
conditions. (Repealed.) A. If closed refrigerator‑sized incubators are used,
culturing and testing of organisms shall be separated to avoid cross‑contamination. B. Laboratory space shall be adequate for the types and
numbers of tests performed. The building shall provide adequate cooling,
heating and illumination for conducting testing and culturing; hot and cold
running water shall be available for cleaning equipment. C. Air used for aeration of test solutions, dilution waters
and cultures shall be free of oil and fumes. D. The laboratory or a contracted outside expert shall
positively identify test organisms to species on an annual basis. The taxonomic
reference (citation and page(s)) and the names(s) of the taxonomic expert(s)
shall be kept on file at the laboratory. When organisms are obtained from an
outside source, the supplier shall provide this same information. E. Instruments used for routine support measurements of
chemical and physical parameters such as pH, DO, conductivity, salinity,
alkalinity, hardness, chlorine, ammonia, and weight shall be calibrated, and/or
standardized per manufacturer's instructions. As these are support
measurements, only the calibration and verification requirements specified at
1VAC30-45-740 D 1 apply. All measurements and calibrations shall be documented. F. Test temperature shall be maintained as specified for
the test method. Temperature control equipment shall be adequate to maintain
the required test temperature(s). The average daily temperature of the test
solutions shall be maintained within the method-specified range. The minimum
frequency of measurement shall be once per 24-hour period. The test temperature
for continuous-flow toxicity tests shall be recorded and monitored
continuously. Where electronic data loggers are used, temperature shall be
monitored at a frequency sufficient to capture temporal variations of the
environmental control system. G. Reagent-grade water, prepared by any combination of
distillation, reverse osmosis, ion exchange, activated carbon and particle
filtration, shall meet the method specified requirements. H. The quality of the standard dilution water used for
testing or culturing shall be sufficient to allow satisfactory survival, growth
and reproduction of the test species as demonstrated by routine reference
toxicant tests and negative control performance. Water used for culturing and
testing shall be analyzed for toxic metals and organics whenever the minimum
acceptability criteria for control survival, growth or reproduction are not met
and no other cause, such as contaminated glassware or poor stock, can be
identified. It is recognized that the analyte lists of some methods manuals may
not include all potential toxicants, are based on estimates of chemical
toxicity available at the time of publication and may specify detection limits
that are not achievable in all matrices. However, for those analytes not
listed, or for which the measured concentration or limit of detection is
greater than the method-specified limit, the laboratory shall demonstrate that
the analyte at the measured concentration or reported limit of detection does
not exceed one-tenth of the expected chronic value for the most sensitive
species tested and/or cultured. The expected chronic value is based on
professional judgment and the best available scientific data. The "USEPA
Ambient Water Quality Criteria Documents" and the EPA AQUIRE database
provide guidance and data on acceptability and toxicity of individual metals
and organic compounds. I. The quality of the food used for testing or culturing
shall be sufficient to allow satisfactory survival, growth and reproduction of
the test species as demonstrated by routine reference toxicant tests and
negative control performance. The laboratory shall have written procedures for
the evaluation of food acceptance. J. A subset of organisms used in bioaccumulation tests
shall be analyzed at the start of the test (baseline) for the target compounds
to be measured in the bioaccumulation tests. K. Test chamber size and test solution volume shall be as
specified in the test method. All test chambers used in a test shall be
identical. L. Test organisms shall be fed the quantity and type food
or nutrients specified in the test method. They shall also be fed at the
intervals specified in the test methods. M. All organisms in a test shall be from the same source.
Where available certified seeds are used for soil tests. N. All organisms used in tests, or used as broodstock to
produce neonate test organisms (for example cladocerans and larval fish), shall
appear healthy, show no signs of stress or disease and exhibit acceptable
survival (90% or greater) during the 24-hour period immediately preceding use
in tests. O. All materials used for test chambers, culture tanks,
tubing, etc., and coming in contact with test samples, solutions, control
water, sediment or soil or food shall be nontoxic and cleaned as described in
the test methods. Materials shall not reduce or add to sample toxicity.
Appropriate materials for use in toxicity testing and culturing are described
in the referenced manuals. P. Light intensity shall be maintained as specified in the
methods manuals. Measurements shall be made and recorded on a yearly basis.
Photoperiod shall be maintained as specified in the test methods and shall be
documented at least quarterly. For algal and plant tests, the light intensity
shall be measured and recorded at the start of each test. Q. The testing laboratory shall document the health and
culturing conditions of all organisms used for testing. Such documentation
shall include culture conditions (e.g., salinity, hardness, temperature, pH)
and observations of any stress, disease or mortality. When organisms are
obtained from an outside source, the laboratory shall obtain written
documentation of these water quality parameters and biological observations for
each lot of organism received. These observations shall adequately address the
24-hour time period referenced in subsection N of this section. The laboratory
shall also record each of these observations and water quality parameters upon
the arrival of the organisms at the testing laboratory. R. Age and the age range of the test organisms shall be as specified
in the test method. Supporting information, such as hatch dates and times,
times of brood releases and metrics (for example, chironomid head capsule
width) shall be documented. S. The maximum holding time of effluents (elapsed time from
sample collection to first use in a test) shall not exceed 36 hours; samples
may be used for renewal up to 72 hours after first use except as prescribed by
the method and approved by the regulatory agency having authority for program
oversight. T. All samples shall be chilled to 0 to 6°C during or
immediately after collection except as prescribed by the method. U. Organisms used in a given test shall be from the same
batch. V. All tests shall have the minimum number of replicates
per treatment as prescribed by the method. W. The control population of Ceriodaphnia in chronic
effluent or receiving water tests shall contain no more than 20% males. X. The culturing of C. dubia shall be adequate such that
blocking by parentage can be established. Y. Dissolved oxygen and pH in aquatic tests shall be within
acceptable range at test initiation and aeration (minimal) is provided to tests
if, and only if, acceptable dissolved oxygen concentrations cannot be otherwise
maintained or if specified by the test method. Z. Test soils or sediments shall be within the geochemical
tolerance range of the test organism. AA. An individual test may be conditionally acceptable if
temperature, dissolved oxygen, pH and other specified conditions fall outside
specifications, depending on the degree of the departure and the objectives of
the tests (see test conditions and test acceptability criteria specified for
each test method).
1VAC30-45-791. Microbiology testing: sterility checks and blanks, positive and negative controls.
A. Sterility checks and blanks. The laboratory shall demonstrate that the filtration equipment and filters, sample containers, media and reagents have not been contaminated through improper handling or preparation, inadequate sterilization, or environmental exposure.
1. A sterility blank shall be analyzed for each lot of pre-prepared, ready-to-use medium (including chromofluorogenic reagent) and for each batch of medium prepared in the laboratory. This shall be done prior to first use of the medium.
2. For filtration technique, the laboratory shall conduct one
beginning and one ending sterility check for each
laboratory sterilized filtration
unit used in a filtration series. The filtration series may include single
or multiple filtration units, which have been sterilized prior to beginning the
series. For presterilized single use funnels a sterility check shall be
performed on one funnel per lot. The filtration series is considered ended when
more than 30 minutes elapses between successive filtrations. During a
filtration series, filter funnels shall be rinsed with three 20-30 ml portions
of sterile rinse water after each sample filtration. In addition, laboratories
shall insert a sterility blank after every 10 samples or sanitize filtration
units by UV light after each sample filtration.
3. For pour plate technique, sterility blanks of the medium shall be made by pouring, at a minimum, one uninoculated plate for each lot of pre-prepared, ready-to-use media and for each batch of medium prepared in the laboratory.
4. Sterility checks on sample containers shall be performed on at least one container for each lot of purchased, presterilized containers with nonselective growth media. For containers prepared and sterilized in the laboratory, a sterility check shall be performed on one container per sterilized batch with nonselective growth media.
5. A sterility blank shall be performed on each batch of dilution water prepared in the laboratory and on each batch of pre-prepared, ready-to-use dilution water with nonselective growth media.
6. At least one filter from each new lot of membrane filters shall be checked for sterility with nonselective growth media.
B. Positive controls.
1. Positive culture controls demonstrate that the medium can
support the growth of the target [
organism(s) organism ],
and that the medium produces the specified or expected reaction to the target
[ organism(s) organism ].
2. Each preprepared, ready-to-use lot of medium (including chromofluorogenic reagent) and each batch of medium prepared in the laboratory shall be tested and demonstrate a known positive response. This shall be done prior to first use of the medium.
C. Negative controls. The provisions of this subsection shall not apply to wastewater treatment plants.
1. Negative culture controls demonstrate that the medium does
not support the growth of [
non-target nontarget ]
organisms or does not demonstrate the typical positive reaction of the target organism(s)
organism or organisms.
2. Each pre-prepared, ready-to-use lot of selective medium
(including chromofluorogenic reagent) and each batch of selective medium
prepared in the laboratory shall be analyzed with one or more known negative
, (i.e., nontarget organisms ,) as
appropriate to the method. This shall be done prior to first use of the medium.
1VAC30-45-796. Microbiology testing: quality of standards, reagents, and media.
A. The laboratory shall ensure that the quality of the reagents and media used is appropriate for the test concerned.
B. Culture media may be prepared from commercial dehydrated powders or may be purchased ready to use. The laboratory may prepare media from basic ingredients when commercial media are not available or when it can be demonstrated that commercial media do not provide adequate results. Media prepared by the laboratory from basic ingredients shall be tested for performance (e.g., for selectivity, sensitivity, sterility, growth promotion, growth inhibition) prior to first use. Detailed testing criteria information shall be defined in either the laboratory's test methods, SOPs, quality manual, or similar documentation.
C. Reagents, commercial dehydrated powders and media shall be used within the shelf-life of the product and shall be documented according to 1VAC30-45-730 J.
D. Distilled water, deionized water or reverse osmosis produced water free from bactericidal and inhibitory substances shall be used in the preparation of media, solutions and buffers. The quality of the water shall be monitored for chlorine residual, specific conductance, and heterotrophic bacteria plate count monthly (when in use), when maintenance is performed on the water treatment system, or at startup after a period of disuse longer than one month.
E. Analysis for metals and the Bacteriological Water Quality Test (to determine presence of toxic agents or growth promoting substances) shall be performed annually. Results of these analyses shall meet the specifications of the required method and records of analyses shall be maintained for three years. (An exception to performing the Bacteriological Water Quality Test shall be given to laboratories that can supply documentation to show that their water source meets the criteria, as specified by the method, for Type I or Type II reagent water.)
F. Media, solutions and reagents shall be prepared, used and
stored according to a documented procedure following the manufacturer's
instructions or the test method. Documentation for media prepared in the
laboratory shall include date of preparation, preparer's initials, type and
amount of media prepared, manufacturer and lot number, final pH of the media,
and expiration date. Documentation for media purchased pre-prepared, ready to
use shall include manufacturer, lot number, type
and amount of media
received, date of receipt, expiration date of the media, and pH of the media.
1VAC30-45-798. Microbiology testing: constant and consistent test conditions.
A. Laboratory facilities. Floors and work surfaces shall be nonabsorbent and easy to clean and disinfect. Work surfaces shall be adequately sealed. Laboratories shall provide sufficient storage space, and shall be clean and free from dust accumulation. Plants, food, and drink shall be prohibited from the laboratory work area.
B. Laboratory equipment.
1. Temperature measuring devices. Temperature measuring devices
such as liquid-in-glass thermometers, thermocouples, and platinum resistance
thermometers used in incubators, autoclaves and other equipment shall be the
appropriate quality to meet
specification(s) specifications in the
test method. The graduation of the temperature measuring devices shall be
appropriate for the required accuracy of measurement and they shall be
calibrated to national or international standards for temperature (see
1VAC30-45-740 C). Calibration shall be done at least annually.
a. The performance of each autoclave shall be initially evaluated by establishing its functional properties and performance, for example, heat distribution characteristics with respect to typical uses. Autoclaves shall meet specified temperature tolerances. Pressure cookers shall not be used for sterilization of growth media.
b. Demonstration of sterilization temperature shall be provided by use of continuous temperature recording device or by use of a maximum registering thermometer with every cycle. Appropriate biological indicators shall be used once per month to determine effective sterilization. Temperature sensitive tape shall be used with the contents of each autoclave run to indicate that the autoclave contents have been processed.
c. Records of autoclave operations shall be maintained for every cycle. Records shall include date, contents, maximum temperature reached, pressure, time in sterilization mode, total run time (may be recorded as time in and time out) and analyst's initials.
d. Autoclave maintenance shall be performed annually,
either internally or by service contract,
shall be performed annually
and shall include a pressure check and calibration of temperature device.
Records of the maintenance shall be maintained in equipment logs. If the
laboratory demonstrates regular monitoring of pressure (e.g., for each
autoclaved batch) and annual calibration of the maximum registering
thermometer, the annual autoclave pressure and temperature device checks shall
not be required.
e. The autoclave mechanical timing device shall be checked quarterly against a stopwatch and the actual time elapsed documented.
3. Volumetric equipment. Volumetric equipment shall be calibrated as follows:
a. Equipment with movable parts such as automatic dispensers, dispensers/diluters, and mechanical hand pipettes shall be verified for accuracy quarterly.
b. Equipment such as filter funnels, bottles, nonclass A glassware, and other marked containers shall be calibrated once per lot prior to first use.
c. The volume of the disposable volumetric equipment such as sample bottles and disposable pipettes shall be checked once per lot.
4. UV instruments. UV instruments used for sanitization shall be tested quarterly for effectiveness with an appropriate UV light meter or by plate count agar spread plates. Replace bulbs if output is less than 70% of original for light tests or if count reduction is less than 99% for a plate containing 200 to 300 organisms.
5. Conductivity meters, oxygen meters, pH meters, hygrometers, and other similar measurement instruments shall be calibrated according to the method specified requirements (see 1VAC30-45-740 D 1 d).
6. Incubators, water baths, and ovens.
stability and uniformity of temperature distribution
and time required after test sample addition to reestablish equilibrium
conditions in incubators and water baths shall be established. Temperature
of incubators and water baths shall be documented twice daily, at least four
hours apart, on each day of use.
b. Ovens used for sterilization shall be checked for sterilization effectiveness monthly with appropriate biological indicators. Records shall be maintained for each cycle that include date, cycle time, temperature, contents and analyst's initials.
7. Labware (glassware and plasticware).
a. The laboratory shall have a documented procedure for washing labware, if applicable. Detergents designed for laboratory use shall be used.
b. Glassware shall be made of borosilicate or other noncorrosive material, free of chips and cracks, and shall have readable measurement marks.
c. Labware that is washed and reused shall be tested for possible presence of residues that may inhibit or promote growth of microorganisms by performing the Inhibitory Residue Test annually, and each time the lab changes the lot of detergent or washing procedures.
d. Washed labware shall be tested at least once daily, each day of washing, for possible acid or alkaline residue by testing at least one piece of labware with a suitable pH indicator such as bromothymol blue. Records of tests shall be maintained.
Radiochemical testing: general. (Repealed.) These standards apply to laboratories undertaking the
examination of environmental samples by radiochemical analysis. These
procedures for radiochemical analysis may involve some form of chemical
separation followed by detection of the radioactive decay of analyte (or
indicative daughters) and tracer isotopes where used. For the purpose of these
standards, procedures for the determination of radioactive isotopes by mass
spectrometry (e.g., ICP-MS or TIMS) or optical (e.g., KPA) techniques are not
Radiochemical testing: negative and positive
controls. (Repealed.) A. Negative controls. 1. Method blank shall be performed at a frequency of one per
preparation batch. The results of this analysis shall be one of the quality control
measures to be used to assess the batch. The method blank result shall be
assessed against the specific acceptance criteria specified in the laboratory
method manual. When the specified method blank acceptance criteria is not met,
the specified corrective action and contingencies shall be followed and results
reported with appropriate data qualifying codes. The occurrence of a failed
method blank acceptance criteria and the actions taken shall be noted in the
laboratory report. 2. In the case of gamma spectrometry, generally a
nondestructive analysis, a method blank shall be prepared using a calibrated
counting geometry similar to that used for the samples. The container of the
appropriate geometry can be empty or filled to similar volume to partially
simulate gamma attenuation due to a sample matrix. 3. There shall be no subtraction of the required method
blank result from the sample results in the associated preparation or
analytical batch unless permitted by method or program. This does not preclude
the application of any correction factor (e.g., instrument background, analyte
presence in tracer, reagent impurities, peak overlap, etc.) to all analyzed
samples, both program/project submitted and internal quality control samples.
However, these correction factors shall not depend on the required method blank
result in the associated analytical batch. 4. The method blank sample shall be prepared with similar
aliquot size to that of the routine samples for analysis and the method blank
result and acceptance criteria shall be calculated in a manner that compensates
for sample results based upon differing aliquot size. B. Positive controls. 1. Laboratory control samples shall be performed at a
frequency of one per preparation batch. The results of this analysis shall be
one of the quality control measures to be used to assess the batch. The
laboratory control sample result shall be assessed against the specific
acceptance criteria specified in the laboratory method manual. When the
specified laboratory control sample acceptance criteria is not met the
specified corrective action and contingencies shall be followed. The occurrence
of a failed laboratory control sample acceptance criteria and the actions taken
shall be noted in the laboratory report. 2. Matrix spike shall be performed at a frequency of one per
preparation batch for those methods that include a chemical separation process
without the use of an internal standard or carrier, and where there is
sufficient sample to do so. Although gross alpha, gross beta and tritium
measurements do not involve a chemical separation process, matrix spikes shall
be performed for these analyses on aqueous samples. The results of this
analysis shall be one of the quality control measures to be used to assess the
batch. The matrix spike result shall be assessed against the specific
acceptance criteria specified in the laboratory method manual. When the
specified matrix spike acceptance criteria is not met, the specified corrective
action and contingencies shall be followed. The occurrence of a failed matrix
spike acceptance criteria and the actions taken shall be noted in the
laboratory report. The lack of sufficient sample aliquot size to perform a
matrix spike shall be noted in the laboratory report. 3. The activity of the laboratory control sample shall (i)
be at least five times the limit of detection and (ii) at a level comparable to
that of routine samples when such information is available if the sample
activities are expected to exceed five times the limit of detection. 4. The activity of the matrix spike analytes(s) shall be
greater than five times the limit of detection. 5. The laboratory standards used to prepare the laboratory
control sample and matrix spike shall be from a source independent of the
laboratory standards used for instrument calibration and shall meet the
requirements for reference standards provided in 1VAC30-45-807 A. 6. The matrix spike shall be prepared by adding a known
activity of target analyte after subsampling if required but before any chemical
treatment (e.g., chemical digestion, dissolution, separation, etc.). Where a
radiochemical method, other than gamma spectroscopy, has more than one
reportable analyte isotope (e.g., plutonium, Pu 238 and Pu 239, using alpha
spectrometry), only one of the analyte isotopes need be included in the
laboratory control or matrix spike sample at the indicated activity level.
However, where more than one analyte isotope is present above the specified
limit of detection, each shall be assessed against the specified acceptance
criteria. 7. Where gamma spectrometry is used to identify and
quantitate more than one analyte isotope, the laboratory control sample shall
contain isotopes that represent the low (e.g., americium-241), medium (e.g.,
cesium-137) and high (e.g., cobalt-60) energy range of the analyzed gamma
spectra. As indicated by these examples the isotopes need not exactly bracket
the calibrated energy range or the range over which isotopes are identified and
quantitated. 8. The laboratory control sample shall be prepared with
similar aliquot size to that of the routine samples for analyses. C. Other controls. 1. Tracer. For those methods that utilize a tracer (i.e.,
internal standard) each sample result shall have an associated tracer recovery
calculated and reported. The tracer shall be added to the sample after
subsampling if required but before any chemical treatment (e.g., chemical
digestion, dissolution, separation, etc.) unless otherwise specified by the
method. The tracer recovery for each sample result shall be one of the quality
control measures to be used to assess the associated sample result acceptance.
The tracer recovery shall be assessed against the specific acceptance criteria
specified in the laboratory method manual. When the specified tracer recovery
acceptance criteria is not met the specified corrective action and
contingencies shall be followed. The occurrence of a failed tracer recovery
acceptance criteria and the actions taken shall be noted in the laboratory
report. 2. Carrier. For those methods that utilize a carrier for
recovery determination, each sample shall have an associated carrier recovery
calculated and reported. The carrier shall be added to the sample after
subsampling if required but before any chemical treatment (e.g., chemical
digestion, dissolution, separation, etc.) unless otherwise specified by the
method. The carrier recovery for each sample shall be one of the quality
control measures to be used to assess the associated sample result acceptance.
The carrier recovery shall be assessed against the specific acceptance criteria
specified in the laboratory method manual. When the specified carrier recovery
acceptance criteria is not met the specified corrective action and
contingencies shall be followed. The occurrence of a failed carrier recovery
acceptance criteria and the actions taken shall be noted in the laboratory
Radiochemical testing: analytical
variability/reproducibility. (Repealed.) A. Replicate shall be performed at a frequency of one per
preparation batch where there is sufficient sample to do so. The results of
this analysis shall be one of the quality control measures to be used to assess
batch acceptance. The replicate result shall be assessed against the specific
acceptance criteria specified in the laboratory method manual. When the
specified replicate acceptance criteria is not met the specified corrective
action and contingencies shall be followed. The occurrence of a failed
replicate acceptance criteria and the actions taken shall be noted in the
laboratory report. B. For low level samples (less than approximately three
times the limit of detection) the laboratory may analyze duplicate laboratory
control samples or a replicate matrix spike (matrix spike and a matrix spike
duplicate) to determine reproducibility within a preparation batch.
Radiochemical testing: method evaluation. (Repealed.) In order to ensure the accuracy of the reported result, the
following procedures shall be in place: 1. Initial demonstration of capability shall be performed initially
(prior to the analysis of any samples) and with a significant change in
instrument type (e.g., different detection technique), personnel or method. 2. Proficiency test samples. The laboratory shall use the
results of such analysis to evaluate its ability to produce accurate data.
Radiochemical testing: radiation measurement
instrumentation. (Repealed.) A. General. Because of the stability and response nature of
modern radiation measurement instrumentation, it is not typically necessary to verify
calibrate these systems each day of use. However, verification of calibration
is required as outlined in subsection B of this section. This section addresses
those practices that are necessary for proper calibration and those
requirements of 1VAC30-45-740 D (instrument calibrations) that are not
applicable to some types of radiation measurement instrumentation. B. Instrument calibration. 1. Given that activity detection efficiency is independent
of sample activity at all but extreme activity levels, the requirements of
1VAC30-45-740 D 2 b (7) are not applicable to radiochemical method calibrations
except mass attenuation in gas-proportional counting and sample quench in
liquid scintillation counting. Radiation measurement instruments are subject to
calibration prior to initial use, when the instrument is placed back in service
after malfunctioning and the instrument's response has changed as determined by
a performance check or when the instrument's response exceeds predetermined
acceptance criteria for the instrument quality control. 2. Instrument calibration shall be performed with reference
standards as defined in 1VAC30-45-807 A. The standards shall have the same
general characteristics (i.e., geometry, homogeneity, density, etc.) as the
associated samples. 3. The frequency of calibration shall be addressed in the
laboratory method manual if not specified in the method. A specific frequency
(e.g., monthly) or observations from the associated control or tolerance chart,
as the basis for calibration shall be specified. C. Continuing instrument calibration verification
(performance checks). Performance checks shall be performed using appropriate
check sources and monitored with control charts or tolerance charts to ensure
that the instrument is operating properly and that the detector response has
not significantly changed and, therefore, the instrument calibration has not
changed. The same check source used in the preparation of the tolerance chart
or control chart at the time of calibration shall be used in the calibration
verification of the instrument. The check sources shall provide adequate
counting statistics for a relatively short count time and the source should be
sealed or encapsulated to prevent loss of activity and contamination of the
instrument and laboratory personnel. 1. For gamma spectroscopy systems, the performance checks
for efficiency and energy calibration shall be performed on a day-of-use basis
along with performance checks on peak resolution. 2. For alpha spectroscopy systems, the performance check for
energy calibration shall be performed on a weekly basis and the performance
check for counting efficiency shall be performed on at least a monthly basis. 3. For gas-proportional and liquid scintillation counters,
the performance check for counting efficiency shall be performed on a
day-of-use basis. For batches of samples that uninterruptedly count for more
than a day a performance check can be performed at the beginning and end of the
batch as long as this time interval is no greater than one week. Verification
of instrument calibration does not directly verify secondary calibrations,
e.g., the mass efficiency curve or the quench curve. 4. For scintillation counters the calibration verification
for counting efficiency shall be performed on a day of use basis. D. Background measurement. Background measurements shall be
made on a regular basis and monitored using control charts or tolerance charts
to ensure that a laboratory maintains its capability to meet required data
quality objectives. These values may be subtracted from the total measured
activity in the determination of the sample activity. 1. For gamma spectroscopy systems, background measurements
shall be performed on at least a monthly basis. 2. For alpha spectroscopy systems, background measurements
shall be performed on at least a monthly basis. 3. For gas-proportional counters, background measurements
shall be performed on at least on a weekly basis. 4. For scintillation counters, background measurements shall
be performed each day of use. E. Instrument contamination monitoring. The laboratory
shall have a written procedure for monitoring radiation measurement
instrumentation for radioactive contamination. The procedure shall indicate the
frequency of the monitoring and shall indicate criteria, which initiates
Radiochemical testing: Minimum detectable
activity (MDA)/Minimum detectable concentration (MDC)/Lower level of detection
(LLD). (Repealed.) A. MDA/MDC/LLD shall be determined prior to sample analysis
and shall be redetermined each time there is a significant change in the test
method or instrument type. B. The procedures employed shall be documented and
consistent with mandated method or regulation.
Radiochemical testing: data reduction. (Repealed.) A. The requirements of 1VAC30-45-730 K apply. B. Measurement uncertainties. Each result shall be reported
with the associated measurement uncertainty. The procedures for determining the
measurement uncertainty shall be documented and be consistent with mandated
method and regulation.
Radiochemical testing: quality of standards
and reagents. (Repealed.) A. The quality control program shall establish and maintain
provisions for radionuclide standards. 1. Reference standards that are used in a radiochemical laboratory
shall be obtained from the National Institute of Standards and Technology
(NIST), or suppliers who participate in supplying NIST standards or NIST
traceable radionuclides. Any reference standards purchased outside the United
States shall be traceable back to each country's national standards laboratory.
Commercial suppliers of reference standards shall conform to ANSI N42.22 to
assure the quality of their products. 2. Reference standards shall be accompanied with a
certificate of calibration whose content is as described in ANSI N42.22 - 1995,
Section 8, Certificates. 3. Laboratories should consult with the supplier if the
laboratory's verification of the activity of the reference traceable standard
indicates a noticeable deviation from the certified value. The laboratory shall
not use a value other than the decay corrected certified value. The laboratory
shall have a written procedure for handling, storing and establishment of
expiration dates for reference standards. B. All reagents used shall be analytical reagent grade or
Radiochemical testing: constant and consistent
test conditions. (Repealed.) The laboratory shall maintain a radiological control
program that addresses analytical radiological control. The program shall address
the procedures for segregating samples with potentially widely varying levels
of radioactivity. The radiological control program shall explicitly define how
low level and high level samples will be identified, segregated and processed
in order to prevent sample cross-contamination. The radiological control
program shall include the measures taken to monitor and evaluate background
activity or contamination on an ongoing basis.
1VAC30-45-811. Air testing: negative and positive controls.
A. Negative controls.
1. Method blanks shall be performed at a frequency of at least one per batch of 20 environmental samples or less per sample preparation method. The results of the method blank analysis shall be used to evaluate the contribution of the laboratory provided sampling media and analytical sample preparation procedures to the amount of analyte found in each sample. If the method blank result is greater than the limit of quantitation and contributes greater than 10% of the total amount of analyte found in the sample, the source of the contamination shall be investigated and measures taken to eliminate the source of contamination. If contamination is found, the data shall be qualified in the report.
2. Collection efficiency. Sampling trains consisting of multiple sections (e.g., filters, sorbent tubes, impingers) that are received intact by the laboratory shall be separated into "front" and "back" sections if required by the client. Each section shall be processed and analyzed separately and the analytical results reported separately.
B. Positive controls. Laboratory control sample (LCS) shall be
analyzed at a rate of at least one per batch of 20 or fewer samples per sample
preparation method for each analyte. If a spiking solution is not available, a
calibration solution whose concentration approximates that of the samples shall
be included in each batch and with each lot of media.
If a calibration solution
must be used for the LCS, the client will be notified prior to the start of
analysis. The concentration of the LCS shall be relevant to the intended
use of the data and either at a regulatory limit or below it.
C. Surrogates shall be used as required by the test method.
D. Matrix spike shall be used as required by the test method.
Asbestos testing: general. (Repealed.) These standards apply to laboratories undertaking the
examination of asbestos samples. These standards are organized by analytical
technique, including transmission electron microscopy (TEM) for the analysis of
water, wastewater, air, and bulk samples; phase contrast microscopy (PCM) for
analysis of workplace air; and polarized light microscopy (PLM) for analysis of
bulk samples. These procedures for asbestos analysis involve sample preparation
followed by detection of asbestos. If NIST SRMs specified below are
unavailable, the laboratory may substitute an equivalent reference material
with a certificate of analysis.
Asbestos testing: negative controls. (Repealed.) A. Transmission electron microscopy. 1. Water and wastewater. a. Blank determinations shall be made prior to sample
collection. When using polyethylene bottles, one bottle from each batch, or a
minimum of one from each 24 shall be tested for background level. When using
glass bottles, four bottles from each 24 shall be tested. An acceptable bottle
blank level is defined as ≤0.01 MFL > 10 μm. (EPA/600/R-94/134,
Method 100.2, Section 8.2) b. A process blank sample consisting of fiber-free water
shall be run before the first field sample. The quantity of water shall be ≥10
mL for a 25-mm diameter filter and ≥ 50 mL for a 47-mm diameter filter.
(EPA/600/R-94/134, Method 100.2, Section 11.8) 2. Air. a. A blank filter shall be prepared with each set of
samples. A blank filter shall be left uncovered during preparation of the
sample set and a wedge from that blank filter shall be prepared alongside
wedges from the sample filters. At minimum, the blank filter shall be analyzed
for each 20 samples analyzed. (40 CFR Part 763, Appendix A to Subpart E
(AHERA), Table 1) b. Maximum contamination on a single blank filter shall be
no more than 53 structures/mm2. Maximum average contamination for
all blank filters shall be no more than 18 structures/mm2. (AHERA,
III.F.2) 3. Bulk samples. a. Contamination checks using asbestos-free material, such
as the glass fiber blank in SRM 1866 (Page C-3, NIST Handbook 150-3, August
1994) shall be performed at a frequency of one for every 20 samples analyzed.
The detection of asbestos at a concentration exceeding 0.1% will require an
investigation to detect and remove the source of the asbestos contamination. b. The laboratory shall maintain a list of nonasbestos
fibers that can be confused with asbestos (Section 7.5, Page C-8, NIST Handbook
150-3, August 1994). The list shall include crystallographic and/or chemical
properties that disqualify each fiber being identified as asbestos (Section
22.214.171.124.1 Identification, Page 54, EPA/600/R-93/116). c. The laboratory should have a set of reference asbestos
materials from which a set of reference diffraction and X-ray spectra have been
developed. B. Phase contrast microscopy. At least two field blanks (or
10% of the total samples, whichever is greater) shall be submitted for analysis
with each set of samples. Field blanks shall be handled in a manner
representative of actual handling of associated samples in the set with a single
exception that air shall not be drawn through the blank sample. A blank
cassette shall be opened for approximately 30 seconds at the same time other
cassettes are opened just prior to analysis. Results from field blank samples
shall be used in the calculation to determine final airborne fiber
concentration. The identity of blank filters should be unknown to the counter
until all counts have been completed. If a field blank yields greater than
seven fibers per 100 graticule fields, report possible contamination of the
samples. C. Polarized light microscopy. 1. Friable materials. At least one blank slide shall be
prepared daily or with every 50 samples analyzed, whichever is less. This is
prepared by mounting a subsample of an isotropic verified non-ACM (e.g.,
fiberglass in SRM 1866) in a drop of immersion oil (nD should
reflect usage of various nD's) on a clean slide, rubbing preparation
tools (forceps, dissecting needles, etc.) in the mount and placing a clean
coverslip on the drop. The entire area under the coverslip shall be scanned to
detect any asbestos contamination. A similar check shall be made after every 20
uses of each piece of homogenization equipment. An isotropic verified non-ACM
shall be homogenized in the clean equipment, a slide prepared with the material
and the slide scanned for asbestos contamination. (This can be substituted for
the blank slide mentioned in this section.) 2. Nonfriable materials. At least one non-ACM nonfriable
material shall be prepared and analyzed with every 20 samples analyzed. This
non-ACM shall go through the full preparation and analysis regimen for the type
of analysis being performed.
Asbestos testing: test
variability/reproducibility. (Repealed.) A. Transmission electron microscopy. Quality assurance
analyses shall be performed regularly covering all time periods, instruments, tasks,
and personnel. The selection of samples shall be random and samples of special
interest may be included in the selection of samples for quality assurance
analyses. When possible, the checks on personnel performance shall be executed
without their prior knowledge. A disproportionate number of analyses shall not
be performed prior to internal or external audits. It is recommended that a
laboratory initially be at 100% quality control (all samples reanalyzed). The
proportion of quality control samples can later be lowered gradually, as
control indicates, to a minimum of 10%. 1. Water and wastewater. All analyses shall be performed on
relocator grids so that other laboratories can easily repeat analyses on the
same grid openings. Quality assurance analyses shall not be postponed during
periods of heavy workloads. The total number of QA samples and blanks shall be
greater than or equal to 10% of the total sample workload. Precision of
analyses is related to concentration, as gleaned from interlaboratory proficiency
testing. Relative standard deviations (RSD) for amphibole asbestos decreased
from 50% at 0.8 MFL to 25% at 7 MFL in interlaboratory proficiency testing,
while RSD for chrysotile was higher, 50% at 6 MFL. a. Replicate. A second, independent analysis shall be
performed on the same grids but on different grid openings than used in the
original analysis of a sample. Results shall be within 1.5X of Poisson standard
deviation. This shall be performed at a frequency of 1 per 100 samples.
(EPA/600/R-94/134, Method 100.2, Table 2) b. Duplicate. A second aliquot of sample shall be filtered
through a second filter, prepared and analyzed in the same manner as the
original preparation of that sample. Results shall be within 2.0X of Poisson
standard deviation. This shall be performed at a frequency of one per 100
samples. (EPA/600/R-94/134, Method 100.2, Table 2) c. Verified analyses. A second, independent analysis shall
be performed on the same grids and grid openings used in the original analysis
of a sample. The two sets of results shall be compared according to Turner and
Steel (NISTIR 5351). This shall be performed at a frequency of one per 20
samples. Qualified analysts shall maintain an average of ≥ 80% true
positives, ≤ 20% false negatives, and ≤ 10% false positives. 2. Air. a. All analyses shall be performed on relocator grids so
that other laboratories can easily repeat analyses on the same grid openings. b. The laboratory and TEM analysts shall obtain mean
analytical results on NIST SRM 1876b so that trimmed mean values fall within
80% of the lower limit and 110% of the upper limit of the 95% confidence limits
as published on the certificate. These limits are derived from the allowable
false positives and false negatives given in subdivision A 2 e (3) of this
subsection. SRM 1876b shall be analyzed a minimum of once per year by each TEM
analyst. c. The laboratory shall have documentation demonstrating
that TEM analysts correctly classify at least 90% of both bundles and single
fibrils of asbestos structures greater than or equal to 1 mm in length in known
standard materials traceable to NIST, such as NIST bulk asbestos SRM 1866. d. Interlaboratory analyses shall be performed to detect
laboratory bias. The frequency of interlaboratory verified analysis shall
correspond to a minimum of 1 per 200 grid square analyses. e. If more than one TEM is used for asbestos analysis,
intermicroscope analyses shall be performed to detect instrument bias. (1) Replicate. A second, independent analysis shall be
performed in accordance with Section D.126.96.36.199.a. (AHERA, Table III) (2) Duplicate. A second wedge from a sample filter shall be
prepared and analyzed in the same manner as the original preparation of that
sample. Results shall be within 2.0X of Poisson standard deviation. This shall
be performed at a frequency of 1 per 100 samples. (AHERA, Table III) (3) Verified analyses. A second, independent analysis shall
be performed on the same grids and grid openings in accordance with subdivision
A 1 c of this section. 3. Bulk samples. Determination of precision and accuracy
should follow guidelines in NISTIR 5951, Guide for Quality Control on the
Qualitative and Quantitative Analysis of Bulk Asbestos Samples: Version 1.
Because bulk samples with low (< 10%) asbestos content are the most
problematic, a laboratory's quality control program should focus on such
samples. At least 30% of a laboratory's QC analyses shall be performed on
samples containing from 1.0% to 10% asbestos. a. Intra-analyst precision. At least one out of 50 samples
shall be reanalyzed by the same analyst. For single analyst laboratories, at
least one out of every 10 samples shall be reanalyzed by the same analyst. b. Inter-analyst precision. At least one out of 15 samples
shall be reanalyzed by another analyst. Inter-analyst results will require
additional reanalysis, possibly including another analyst, to resolve
discrepancies when classification (ACM vs. non-ACM) errors occur, when asbestos
identification errors occur, or when inter-analyst precision is found to be
unacceptable. c. Inter-laboratory precision. The laboratory shall
participate in round robin testing with at least one other laboratory. Samples
shall be sent to this other lab at least four times per year. These samples
shall be samples previously analyzed as QC samples. Results of these analyses
shall be assessed in accordance with QC requirements. As a minimum, the QC
requirements shall address misclassifications (false positives, false
negatives) and misidentification of asbestos types. B. Phase contrast microscopy. 1. Inter-laboratory precision. Each laboratory analyzing air
samples for compliance determination shall implement an inter-laboratory
quality assurance program that as a minimum includes participation of at least
two other independent laboratories. Each laboratory shall participate in round
robin testing at least once every six months with at least all the other
laboratories in its inter-laboratory quality assurance group. Each laboratory
shall submit slides typical of its own workload for use in this program. The
round robin shall be designed and results analyzed using appropriate
statistical methodology. Results of this QA program shall be posted in each
laboratory to keep the microscopists informed. 2. Intra- and inter-analyst precision. Each analyst shall
select and count a prepared slide from a "reference slide library" on
each day on which air counts are performed. Reference slides shall be prepared
using well-behaved samples taken from the laboratory workload. Fiber densities
shall cover the entire range routinely analyzed by the laboratory. These slides
shall be counted by all analysts to establish an original standard deviation
and corresponding limits of acceptability. Results from the daily reference
sample analysis shall be compared to the statistically derived acceptance
limits using a control chart or a database. It is recommended that the labels
on the reference slides be periodically changed so that the analysts do not
become familiar with the samples. Intra- and inter-analyst precision may be
estimated from blind recounts on reference samples. Inter-analyst precision
shall be posted in each laboratory to keep the microscopists informed. C. Polarized light microscopy. Refer to subdivision A 3 of
Asbestos testing: other quality control
measures. (Repealed.) A. Transmission electron microscopy. 1. Water and wastewater. a. Filter preparations shall be made from all six asbestos
types from NIST SRMs 1866 and 1867. These preparations shall have
concentrations between one and 20 structures (> 10 μm) per 0.01 mm2.
One of these preparations shall be analyzed independently at a frequency of one
per 100 samples analyzed. Results shall be evaluated as verified asbestos
analysis in accordance with Turner and Steel (NISTIR 5351). b. NIST SRM 1876b shall be analyzed annually by each
analyst. Results shall be evaluated in accordance with limits published for
that SRM. This SRM is not strictly appropriate for waterborne asbestos but
analysts can demonstrate general TEM asbestos competence by producing results
within the published limits of this (the only recognized TEM counting standard)
SRM. 2. Air. a. Filter preparations shall be made from all six asbestos
types in accordance with subdivision A 1 a of this section. b. NIST SRM 1876b shall be analyzed annually in accordance
with subdivision A 1 b of this section. 3. Bulk samples. All analysts shall be able to correctly
identify the six regulated asbestos types (chrysotile, amosite, crocidolite,
anthophyllite, actinolite, and tremolite). Standards for the six asbestos types
listed are available from NIST (SRMs 1866 and 1867). These materials can also
be used as identification standards for AEM (Section 3.2.1 Qualitative
Analysis, Page 57, EPA/600/R-93/116). B. Phase contrast microscopy. 1. Test for nonrandom fiber distribution. Blind recounts by
the same analyst shall be performed on 10% of the filters counted. A person
other than the counter should re-label slides before the second count. A test
for type II error (NIOSH 7400, Issue 2, 15 August 1994, Section 13) shall be
performed to determine whether a pair of counts by the same analyst on the same
slide should be rejected due to nonrandom fiber distribution. If a pair of
counts is rejected by this test, the remaining samples in the set shall be
recounted and the new counts shall be tested against first counts. All rejected
paired counts shall be discarded. It shall not be necessary to use this statistic
on blank recounts. 2. All individuals performing airborne fiber analysis shall
have taken the NIOSH Fiber Counting Course for sampling and evaluating airborne
asbestos dust or an equivalent course. 3. All laboratories shall participate in a national sample
testing scheme such as the Proficiency Analytical Testing (PAT) program or the
Asbestos Analysts Registry (AAR) program, both sponsored by the American
Industrial Hygiene Association (AIHA), or equivalent. C. Polarized light microscopy. 1. Friable materials. Because accuracy cannot be determined
by reanalysis of routine field samples, at least one out of 100 samples shall
be a standard or reference sample that has been routinely resubmitted to
determine analyst's precision and accuracy. A set of these samples should be
accumulated from proficiency testing samples with predetermined weight
compositions or from standards generated with weighed quantities of asbestos
and other bulk materials (Perkins and Harvey, 1993; Parekh et al., 1992; Webber
et al., 1982). At least half of the reference samples submitted for this QC
shall contain between 1.0% and 10% asbestos. 2. Nonfriable materials. At least one out of 100 samples
shall be a verified quantitative standard that has routinely been resubmitted
to determine analyst precision and accuracy.
Asbestos testing: method evaluation. (Repealed.) In order to ensure the accuracy of reported results, the
following procedures shall be in place: 1. Demonstration of capability shall be performed initially (prior
to the analysis of any samples) and with a significant change in instrument
type, personnel, or method. 2. Performance audits. The results of such analyses shall be
used by the laboratory to evaluate the ability of the laboratory to produce
Asbestos testing: asbestos calibration. (Repealed.) Refer to methods referenced in the following sections for
specific equipment requirements. 1. Transmission electron microscopy: general. Analytical electron
microscopy equipment will not be discussed in this document. 2. Transmission electron microscopy: water and wastewater.
All calibrations listed below (unless otherwise noted) shall be performed under
the same analytical conditions used for routine asbestos analysis and shall be
recorded in a notebook and include date and analyst's signature. Frequencies
stated below may be reduced to "before next use" if no samples are
analyzed after the last calibration period has expired. Likewise, frequencies
may have to be increased following non-routine maintenance or unacceptable
calibration performance. a. Magnification calibration. Magnification calibration
shall be done at the fluorescent screen, with the calibration specimen at the
eucentric position, at the magnification used for fiber counting, generally
10,000 and 20,000x. A logbook shall be maintained with the dates of the
calibration recorded. Calibrations shall be performed monthly to establish the
stability of magnification. Calibration data shall be displayed on control
charts that show trends over time. (EPA/600/R-94/134, Method 100.2, Section
10.1) b. Camera constant. The camera length of the TEM in the
Selected Area Electron Diffraction (SAED) mode shall be calibrated before SAED
patterns of unknown samples are observed. The diffraction specimen shall be at
the eucentric position for this calibration. This calibration shall allow
accurate (< 10% variation) measurement of layer-line spacings on the medium
used for routine measurement, i.e., the phosphor screen or camera film. This
shall also allow accurate (< 5.0% variation) measurement of zone axis SAED
patterns on permanent media, e.g., film. Calibrations shall be performed
monthly to establish the stability of the camera constant (EPA/600/R-94/134,
Method 100.2, Section 10.2). Where nonasbestiform minerals may be expected
(e.g., winchite, richterite, industrial talc, vermiculite, etc.), an internal
camera constant standard such as gold, shall be deposited and measured on each
sample to facilitate accurate indexing of zone axis SAED patterns. In such
cases, layer line analysis alone shall not be used. Calibration data shall be
displayed on control charts that show trends over time. c. Spot size. The diameter of the smallest beam spot at
crossover shall be less than 250 nm as calibrated quarterly. Calibration data
shall be displayed on control charts that show trends over time.
(EPA/600/R-94/134, Method 100.2, Section 10.3) d. Beam dose. The beam dose shall be calibrated so that
beam damage to chrysotile is minimized, specifically so that an electron
diffraction pattern from a single fibril ≥1 μm in length from a NIST
SRM chrysotile sample is stable in the electron beam dose for at least 15
seconds. e. EDXA system. (1) The x-ray energy vs. channel number for the EDXA system
shall be calibrated to within 20 eV for at least two peaks between 0.7 keV and
10 keV. One peak shall be from the low end (0.7 keV to 2 keV) and the other
peak from the high end (7 keV to 10 keV) of this range. The calibration of the
x-ray energy shall be checked prior to each analysis of samples and
recalibrated if out of the specified range. (2) The ability of the system to resolve the Na Ka line
from the Cu L line shall be confirmed quarterly by obtaining a spectrum from
the NIST SRM 1866 crocidolite sample on a copper grid. (3) The k-factors for elements found in asbestos (Na, Mg,
Al, Si, Ca, and Fe) relative to Si shall be calibrated semiannually, or anytime
the detector geometry may be altered. NIST SRM 2063a shall be used for Mg, Si,
Ca, Fe, while k-factors for Na and Al may be obtained from suitable materials
such as albite, kaersutite, or NIST SRM 99a. The k-factors shall be determined
to a precision (2s) within 10% relative to the mean value obtained for Mg, Al,
Si, Ca, and Fe, and within 20% relative to the mean value obtained for Na. The
k-factor relative to Si for Na shall be between 1.0 and 4.0, for Mg and Fe
shall be between 1.0 and 2.0, and for Al and Ca shall be between 1.0 and 1.75.
The k-factor for Mg relative to Fe shall be 1.5 or less. Calibration data shall
be displayed on control charts that show trends over time. (4) The detector resolution shall be checked quarterly to
ensure a full-width half-maximum resolution of <175 eV at Mn Ka (5.90 keV).
Calibration data shall be displayed on control charts that show trends over
time. (5) The portions of a grid in a specimen holder for which
abnormal x-ray spectra are generated under routine asbestos analysis conditions
shall be determined and these areas shall be avoided in asbestos analysis. (6) The sensitivity of the detector for collecting x-rays
from small volumes shall be documented quarterly by collecting resolvable Mg
and Si peaks from a unit fibril of NIST SRM 1866 chrysotile. f. Low temperature asher. The low temperature asher shall
be calibrated quarterly by determining a calibration curve for the weight vs.
ashing time of collapsed mixed-cellulose-ester (MCE) filters. Calibration data
shall be displayed on control charts that show trends over time. g. Grid openings. The magnification of the grid opening
measurement system shall be calibrated using an appropriate standard at a
frequency of 20 openings/20 grids/lot of 1000 or one opening/sample. The
variation in the calibration measurements (2s) is <5.0% of the mean calibration
value. 3. Air. All calibrations shall be performed in accordance
with subdivision 2 of this section, with the exception of magnification.
Magnification calibration shall be done at the fluorescent screen, with the
calibration specimen at the eucentric position, at the magnification used for
fiber counting, generally 15,000 to 20,000x (AHERA, III.G.1.c). A logbook shall
be maintained with the dates of the calibration recorded. Calibrations shall be
performed monthly to establish the stability of magnification. 4. Bulk samples. All calibrations shall be performed in
accordance with subdivision 3 of this section. 5. Phase contrast microscopy. a. At least once daily, the analyst shall use the telescope
ocular (or Bertrand lens, for some microscopes) supplied by the manufacturer to
ensure that the phase rings (annular diaphragm and phase-shifting elements) are
concentric. b. The phase-shift limit of detection of the microscope
shall be checked monthly or after modification or relocation using an HSE/NPL
phase-contrast test slide for each analyst/microscope combination (refer to
NIOSH 7400, Issue 2, 15 August 1994, Section 10b). This procedure assures that
the minimum detectable fiber diameter (< ca. 0.25mm) for this microscope is
achieved. c. Prior to ordering the Walton-Beckett graticule,
calibration, in accordance with NIOSH 7400, Issue 2, 15 August 1994, Appendix
A, shall be performed to obtain a counting area 100 mm in diameter at the image
plane. The diameter, dc (mm), of the circular counting area and the
disc diameter shall be specified when ordering the graticule. The field
diameter (D) shall be verified (or checked), to a tolerance of 100 μm ± 2
μm, with a stage micrometer upon receipt of the graticule from the
manufacturer. When changes (zoom adjustment, disassembly, replacement, etc.)
occur in the eyepiece-objective-reticle combination, field diameter shall be
remeasured (or recalibrated) to determine field area (mm2).
Recalibration of field diameter shall also be required when there is a change
in interpupillary distance (i.e., change in analyst). Acceptable range for
field area shall be 0.00754 mm2 to 0.00817 mm2. The
actual field area shall be documented and used. 6. Polarized light microscopy. a. Microscope alignment. To accurately measure the required
optical properties, a properly aligned polarized light microscope (PLM) shall
be utilized. The PLM shall be aligned before each use. (Section 188.8.131.52.3,
EPA/600/R-93/116, July 1993) b. Refractive index liquids. Series of nD = 1.49
through 1.72 in intervals less than or equal to 0.005. Refractive index liquids
for dispersion staining, high-dispersion series 1.550, 1.605, 1.680. The
accurate measurement of the refractive index (RI) of a substance requires the
use of calibrated refractive index liquids. These liquids shall be calibrated
at first use and semiannually, or next use, whichever is less frequent, to an
accuracy of 0.004, with a temperature accuracy of 2°C using a refractometer or
RI glass beads.
Asbestos testing: analytical sensitivity. (Repealed.) A. Transmission electron microscopy. 1. Water and wastewater. An analytical sensitivity of
200,000 fibers per liter (0.2 MFL) is required for each sample analyzed (EPA/600/R-94/134,
Method 100.2, Section 1.6). Analytical sensitivity is defined as the waterborne
concentration represented by the finding of one asbestos structure in the total
area of filter examined. This value will depend on the fraction of the filter
sampled and the dilution factor (if applicable). 2. Air. An analytical sensitivity of 0.005
structures/cm2 is required for each sample analyzed. Analytical
sensitivity is defined as the airborne concentration represented by the finding
of one asbestos structure in the total area of filter examined. This value will
depend on the effective surface area of the filter, the filter area analyzed,
and the volume of air sampled (AHERA, Table I). 3. Bulk samples. a. The range is dependent on the type of bulk material
being analyzed. The sensitivity may be as low as 0.0001% depending on the
extent to which interfering materials can be removed during the preparation of
AEM specimens. (Section 2.5.2 Range, Page 51, EPA/600/R-93/116) b. There should be an error rate of less than 1.0% on the
qualitative analysis for samples that contain chrysotile, amosite, and
crocidolite. A slightly higher error rate may occur for samples that contain
anthophyllite, actinolite, and tremolite, as it can be difficult to distinguish
among the three types. (Section 3, Page 10, NIST Handbook 150-3, August 1994) B. Phase contrast microscopy. The normal quantitative
working range of the test method is 0.04 to 0.5 fiber/cm2 for a 1000
L air sample. An ideal counting range on the filter shall be 100 to 1300
fibers/mm2. The limit of detection (LOD) is estimated to be 5.5
fibers per 100 fields or 7 fibers/mm2. The LOD in fiber/cc will
depend on sample volume and quantity of interfering dust but shall be <0.01
fiber/cm2 for atmospheres free of interferences. (NIOSH 7400, Issue
2, 15 August 1994) C. Polarized light microscopy. The laboratory shall utilize
a test method that provides a limit of detection that is appropriate and
relevant for the intended use of the data. Limit of detection shall be determined
by the protocol in the test method or applicable regulation.
Asbestos testing: data reduction. (Repealed.) A. Transmission electron microscopy. 1. Water and wastewater. a. The concentration of asbestos in a given sample shall be
calculated in accordance with EPA/600/R-94/134, Method 100.2, Section 12.1.
Refer to 1VAC30-45-730 K for additional data reduction requirements. b. Measurement uncertainties. The laboratory shall
calculate and report the upper and lower 95% confidence limits on the mean
concentration of asbestos fibers found in the sample (EPA/600/R-94/134, Method
100.2, Section 12.2.2). 2. Air. a. The concentration of asbestos in a given sample shall be
calculated in accordance with the method utilized, e.g., AHERA. Refer to
1VAC30-45-730 K for additional data reduction requirements. b. Measurement uncertainties. The laboratory shall
calculate and report the upper and lower 95% confidence limits on the mean
concentration of asbestos fibers found in the sample. 3. Bulk samples. a. The concentration of asbestos in a given sample shall be
calculated in accordance with the method utilized (e.g., EPA/600/R-93/116, July
1993). Refer to 1VAC30-45-730 K for additional data reduction requirements. b. Measurement uncertainties. Proficiency testing for floor
tiles analyzed by TEM following careful gravimetric reduction (New York ELAP
Certification Manual Item 198.4) has revealed an interlaboratory standard
deviation of approximately 20% for residues containing 70% or more asbestos. Standard
deviations range from 20% to 60% for residues with lower asbestos content. B. Phase contrast microscopy. 1. Airborne fiber concentration in a given sample shall be
calculated in accordance with NIOSH 7400, Issue 2, 15 August 1994, Sections 20
and 21. Refer to 1VAC30-45-730 K for additional data reduction requirements. 2. Measurement uncertainties. The laboratory shall calculate
and report the intra-laboratory and inter-laboratory relative standard
deviation with each set of results. (NIOSH 7400, Issue 2, 15 August 1994) 3. Fiber counts above 1300 fibers/mm2 and fiber
counts from samples with >50% of the filter area covered with particulate
should be reported as "uncountable" or "probably biased."
Other fiber counts outside the 100-1300 fibers/mm2 range should be
reported as having "greater than optimal variability" and as being
"probably biased." C. Polarized light microscopy. 1. The concentration of asbestos in a given sample shall be
calculated in accordance with the method utilized (e.g., EPA/600/R-93/116, July
1993). Refer to 1VAC30-45-730 K for additional data reduction requirements. 2. Method uncertainties. The individual laboratory shall
determine precision and accuracy for the percent range involved. If point
counting and/or visual estimates are used, a table of reasonable expanded
errors (refer to EPA/600/R-93/116, July 1993, Table 2-1) should be generated
for different concentrations of asbestos.
Asbestos testing: quality of standards and
reagents. (Repealed.) A. Transmission electron microscopy. 1. The quality control program shall establish and maintain
provisions for asbestos standards. a. Reference standards that are used in an asbestos
laboratory shall be obtained from the National Institute of Standards and
Technology (NIST), EPA, or suppliers who participate in supplying NIST
standards or NIST traceable asbestos. Any reference standards purchased outside
the United States shall be traceable back to each country's national standards
laboratory. Commercial suppliers of reference standards shall conform to ANSI
N42.22 to assure the quality of their products. b. Reference standards shall be accompanied with a
certificate of calibration whose content is as described in ANSI N42.22-1995,
Section 8, Certificates. 2. All reagents used shall be analytical reagent grade or
better. 3. The laboratory shall have mineral fibers or data from
mineral fibers that will allow differentiating asbestos from at least the
following "look-alikes": fibrous talc, sepiolite, wollastonite,
attapulgite (palygorskite), halloysite, vermiculite scrolls, antigorite,
lizardite, pyroxenes, hornblende, richterite, winchite, or any other
asbestiform minerals that are suspected as being present in the sample. B. Phase contrast microscopy. Standards of known
concentration have not been developed for this testing method. Routine workload
samples that have been statistically validated and national proficiency testing
samples such as PAT and AAR samples available from the AIHA may be utilized as
reference samples (refer to 1VAC30-45-822 B 2) to standardize the optical
system and analyst. All other testing reagents and devices (HSE/NPL test slide
and Walton-Beckett Graticule) shall conform to the specifications of the method
(refer to NIOSH 7400, Issue 2, 15 August 1994). C. Polarized light microscopy. Refer to 1VAC30-45-828 A.
Asbestos testing: constant and consistent test
conditions. (Repealed.) The laboratory shall establish and adhere to written
procedures to minimize the possibility of cross-contamination between samples.
1VAC30-45-850. Sample handling, sample acceptance policy, and sample receipt.
While the laboratory may not have control of field sampling activities, the following are essential to ensure the validity of the laboratory's data.
1. Sample tracking. The laboratory shall have a documented system for uniquely identifying the items to be tested to ensure that there can be no confusion regarding the identity of such items at any time. This system shall include identification for all samples, subsamples and subsequent extracts or digestates or both. The use of container shape, size or other physical characteristic, such as amber glass or purple top, is not an acceptable means of identifying the sample. System laboratories shall use a permanent chronological record such as a logbook or electronic database to document receipt of all containers. This sample receipt log shall record the following at a minimum: name of facility where sample was taken, date and time of laboratory receipt, unique laboratory ID code, and signature or initials of the person making the entries.
2. Sample acceptance policy. The laboratory shall have a written sample acceptance policy that clearly outlines the circumstances under which samples shall be accepted or rejected. The policy shall ensure that only properly obtained samples with appropriate sampling records (see 1VAC30-45-640 B) are analyzed and that the samples are handled properly. This sample acceptance policy shall be made available to sample collection personnel. The policy shall include elements such as appropriate documentation of the sample's identification, use of appropriate sample containers, adherence to specified holding times, adequate sample volume to perform necessary tests, and procedures to be used when samples show signs of damage, contamination or inadequate preservation.
3. Sample receipt protocols.
a. Upon receipt, the condition of the sample, including any abnormalities or departures from standard condition as prescribed in the relevant test method, shall be recorded. All items specified by the sample acceptance policy shall be checked.
b. All samples that require thermal preservation shall be
considered acceptable if the arrival temperature is either within 2
Celsius °C of the required temperature or the method specified
range. For samples with a specified temperature of 4 degrees Celsius °C,
samples with a temperature of ranging from just above freezing temperature of
water to 6 degrees Celsius °C shall be acceptable. Samples that
are hand delivered to the laboratory immediately after collection or on the
same day that are collected may not meet this these criteria. In
these cases, the samples shall be considered acceptable if there is evidence
that the chilling process has begun such as arrival on ice. Thermal
preservation is not required in the field if the laboratory receives the sample
and either begins the analysis or refrigerates the sample within 15 minutes of
c. The laboratory shall implement procedures for checking chemical preservation using readily available techniques, such as pH or free chlorine prior to or during sample preparation or analysis.
d. The results of all checks required by the sample acceptance policy and relevant test method shall be recorded.
4. Storage conditions.
a. The laboratory shall have documented procedures and appropriate facilities to avoid deterioration, contamination or damage to the sample during storage, handling, preparation, and testing. Any relevant instructions provided with the item shall be followed. Where items have to be stored or conditioned under specific environmental conditions, these conditions shall be maintained, monitored and recorded.
b. Samples shall be stored according to the conditions specified by preservation protocols:
(1) Samples that require thermal preservation shall be stored
under refrigeration that is within 2
degrees Celsius °C of the
specified preservation temperature unless method specific criteria exist. For
samples with a specified storage temperature of 4 degrees Celsius °C,
storage at a temperature above the freezing point of water to 6 degrees
Celsius °C shall be acceptable.
(2) Samples shall be stored away from all standards, reagents, food and other potentially contaminating sources. Samples shall be stored in such a manner to prevent cross contamination.
c. Sample fractions, extracts, leachates and other sample preparation products shall be stored according to subdivision 4 a of this section or according to specifications in the test method.
d. Where a sample or portion of the sample is to be held
(for example (e.g., for reasons of record, safety or
value, or to enable check calibrations or tests to be performed later), the
laboratory shall have storage and security arrangements that protect the
condition and integrity of the secured items or portions concerned.
5. Sample disposal. The laboratory shall have standard operating procedures for the disposal of samples, digestates, leachates and extracts or other sample preparation products.
Application for Certification of Environmental Laboratories DGS‑21‑156 (eff. 1/09) (Application for Certification under 1VAC30-45 must be obtained from DCLS program staff at Lab_Cert@dgs.virginia.gov)
DOCUMENTS INCORPORATED BY REFERENCE (1VAC30-45)
The Standards for Environmental Laboratories and Accreditation Bodies, 2009, The NELAC Institute (TNI), P.O. Box 2439, Weatherford, TX 76086; www.nelac-institute.org: