Part II. Standards
Article 1
Personnel
1VAC30-45-200. Laboratory manager.
A. Laboratory manager - general.
1. Each environmental laboratory shall designate a person to be responsible for the general oversight of the operation of the laboratory in accordance with this chapter, including the day-to-day functioning and administration of the laboratory, the technical operations, supervision of laboratory procedures, reporting of laboratory results, and implementation of any corrective actions.
2. The title of this person may include but is not limited to laboratory director, technical director, laboratory supervisor or laboratory manager.
3. A laboratory may appoint one or more technical directors for the appropriate fields of certification for which the laboratory seeks certification.
B. Laboratory manager - qualifications.
1. For an environmental laboratory that performs procedures beyond simple test procedures, a laboratory manager shall have two years of experience managing an environmental laboratory or performing the analyses for which the environmental laboratory seeks certification or both.
2. For an environmental laboratory that performs only simple test procedures, there are no qualification requirements for a laboratory manager except that the responsible official shall designate the laboratory manager.
3. A full-time employee of a drinking water or wastewater treatment facility who holds a valid treatment plant operator's certificate appropriate to the nature and size of such facility shall be deemed to meet the educational and experience requirements serving as the laboratory manager of the certified laboratory devoted exclusively to the examination of environmental samples taken within such facility system and limited to the scope of that facility's regulatory permit.
4. A full-time employee of an industrial waste treatment facility with a minimum of one year of experience under supervision in environmental analysis shall be deemed to meet the requirements for serving as the laboratory manager of a certified laboratory devoted exclusively to the examination of environmental samples taken within such facility for the scope of that facility's regulatory permit.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-210. Quality assurance officer.
A. The laboratory shall have a quality assurance officer who shall be responsible for the quality system and its implementation. Where staffing is limited, the quality assurance officer may also be the laboratory manager. The quality assurance officer may be employed on a part-time basis or be a consultant.
B. The quality assurance officer shall have documented training or experience in quality assurance and quality control procedures and be knowledgeable in the quality system as defined in Article 4 (1VAC30-45-600 et seq.) of Part II of this chapter. The quality assurance officer shall have a general knowledge of the analytical test methods for which data review is performed.
C. The responsibilities of the quality assurance officer shall include, but not be limited to, the implementation and oversight of the quality system, the implementation of new quality assurance and control practices, periodic audits of the quality system in place, periodic review of final data reports, and documentation of laboratory quality system deficiencies.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-220. Laboratory personnel requirements and management responsibilities.
A. The laboratory shall have sufficient personnel, having the necessary education, training, technical knowledge and experience for their assigned functions.
B. The laboratory manager shall ensure that the training of the laboratory personnel is kept up to date.
C. Laboratory personnel shall be responsible for complying with all quality systems requirements set out in Article 4 (1VAC30-45-600 et seq.) of Part II of this chapter that are pertinent to their assigned functions.
D. The laboratory manager shall ensure that laboratory personnel have demonstrated initial and ongoing capability to perform their assigned functions. See 1VAC30-45-730 E and F.
E. Records on the relevant qualifications, training skills and experience of the laboratory personnel, including records on demonstrated proficiency for each test method, shall be maintained by the laboratory manager.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-230. Absence of laboratory manager.
When a laboratory manager will be absent for a period exceeding 15 consecutive calendar days, the laboratory shall designate a qualified replacement to perform the manager's function.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-240. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-250. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-260. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-270. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-280. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-290. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
Article 2
On-Site Assessment
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 initially.
2. DCLS shall reassess each certified laboratory 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.
1. If DCLS identified a deficiency on a previous on-site assessment, the agency may conduct a follow-up on-site assessment.
2. 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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-310. Announced and unannounced on-site assessments.
A. 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, DCLS, 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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-320. Request for records.
Prior to the actual site visit, DCLS may request in writing from a laboratory those records required to be maintained by this chapter.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-330. Areas to be assessed.
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.
10. Recordkeeping.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
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 DCLS in writing of any information that is controlled for national security reasons and cannot be released to the public.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
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 documented by DCLS. The team leader for the assessment personnel shall notify 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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-360. On-site laboratory records review and collection.
A. Records shall be reviewed by assessment personnel for accuracy, completeness and the use of proper methodology for each analyte and test method to be evaluated.
B. Records required to be maintained pursuant to this chapter shall be examined as part of an assessment for certification.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-370. Observations of and interviews with laboratory personnel.
A. As an element of the assessment process, the assessment team shall evaluate an analysis regimen by requesting that the analyst normally conducting the procedure give a step-by-step description of exactly what is done and what equipment and supplies are needed to complete the regimen. Any deficiencies shall be noted and discussed with the analyst. In addition, the deficiencies shall be discussed in the closing conference.
B. Assessment personnel may conduct interviews with appropriate laboratory personnel.
C. Calculations, data transfers, calibration procedures, quality control and quality assurance practices, adherence to test methods, and report preparation shall be assessed for the complete scope of certification with appropriate laboratory analysts.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
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 DCLS.
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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-390. Follow-up and reporting procedures..
A. 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 DCLS. This response shall be called a corrective action 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 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 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.
E. DCLS shall determine and shall notify the laboratory within 30 calendar days of receipt whether the corrective action plan is an acceptable response to the deficiencies identified in the assessment report.
F. If the corrective action plan (or a portion of the plan) is determined to be unacceptable to remedy the deficiency, 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 plan acceptable to DCLS.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-400. Documentation of on-site assessment.
A. Checklists. The checklists used by assessment personnel during the assessment shall become a part of DCLS's 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;
h. Summary;
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 DCLS five days prior to visiting DCLS. A laboratory may request copies of its documents without visiting DCLS. A reasonable fee may be charged for copying, mailing, and staff time.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-410. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-420. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-430. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-440. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-450. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-460. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-470. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-480. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-490. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
Article 3
Proficiency Testing
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 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 notify DCLS of the fields of certification for which the laboratory chooses to become certified and shall participate in the appropriate PT studies.
2. For all fields of 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 chapter.
C. Reporting results. Each laboratory shall authorize the PT study provider to release the results of the final evaluation report of the laboratory's PT study directly to DCLS, in addition to the laboratory.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-510. Requirements for laboratory testing of PT study samples.
A. 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 during on-site assessments of the laboratory.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-520. PT criteria for laboratory certification.
A. Result categories.
1. The criteria described in this section apply individually to each 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 one PT study for each requested FoC.
2. Once a laboratory has been granted certification status, it shall continue to complete PT studies for each FoPT and maintain a history of at least one acceptable PT study each calendar year. The laboratory shall complete its PT studies by September 30 of each calendar year.
3. 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.
4. For a laboratory performing supplemental testing, the PT studies shall be at least seven calendar days apart from the closing date of one study to the opening date of another study for the same FoPT.
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.
D. Withdrawal from PT studies. A laboratory may withdraw from a PT study for 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 continued certification.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016; Volume 38, Issue 12, eff. April 1, 2022.
1VAC30-45-530. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-540. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-550. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-560. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-570. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-580. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-590. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
Article 4
Quality System
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.
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.
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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-610. Quality manual.
A. General.
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 subsections B and C of this section.
B. The elements of a quality manual shall include but not be limited to:
1. A document title;
2. The laboratory's full name and address;
3. The name, address (if different from above), and telephone number of the responsible official, laboratory manager, and quality assurance officer;
4. The laboratory facility or facilities covered by the quality manual;
5. Signed and dated concurrence, with appropriate titles, of the responsible official, laboratory manager, and quality assurance officer;
6. The effective date of the quality manual;
7. Table of contents and applicable lists of references, glossaries, and appendices; and
8. A quality policy statement, including objectives of the quality system and commitment to ethical laboratory practices and to upholding the requirements of this chapter's standards.
C. The quality manual shall include or reference but not be limited to:
1. The organization and management structure of the laboratory, its place in any parent organization and relevant organizational charts.
2. Job descriptions of key staff and reference to the job descriptions of other staff.
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.
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.
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.
6. Procedures for dealing with complaints.
7. Procedures for audits and data review.
8. Verification practices that may include inter-laboratory comparisons, proficiency testing programs, use of reference materials and internal quality control schemes.
9. Procedures to be followed for feedback and corrective action whenever testing discrepancies are detected, or departures from documented policies and procedures occur.
10. The laboratory management arrangements for permitting departures from documented policies and procedures or from standard specifications when the departures are planned and controlled.
11. The major equipment and reference measurement standards used as well as the physical facility and environment used by the laboratory in conducting tests.
12. Procedures for calibration, verification and maintenance of equipment.
13. A list of all technology/methods under which the laboratory performs its certified testing.
14. Procedures for achieving traceability of measurements, including standards.
15. Procedures for receiving, handling, storing, and disposing of submitted samples.
16. Procedures for reporting analytical results.
17. Policy addressing the use of unique electronic signatures, where applicable.
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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-620. Organization.
The laboratory shall specify and document the functional responsibility, level of authority, and interrelationship or lines of communication of all personnel who manage, perform or verify work affecting the quality of tests, analyses, measurements and monitoring. One person may cover more than one organizational function. Each manager and employee of the laboratory shall have a clear understanding of his or her duties and responsibilities and the relationship of those responsibilities to the overall work of the laboratory.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-630. Records.
The laboratory shall maintain a record system to suit its particular circumstances and comply with any applicable regulations. This system shall produce unequivocal, accurate records that document all laboratory activities.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-640. Recordkeeping system and design.
A. The laboratory shall have a recordkeeping system that allows historical reconstruction of all laboratory activities that produced the analytical data. The history of the sample shall be readily understood through the documentation. This shall include inter-laboratory transfers of samples or extracts or both.
B. The records shall include the identity of personnel involved in sampling, sample preservation, sample receipt, preparation, calibration or testing, all documentation sent by the person transmitting the sample, including a chain of custody record form, if utilized.
C. The laboratory shall document all information relating to the laboratory facility's equipment, analytical test methods, and related laboratory activities, such as sample receipt, sample preparation, or data verification.
D. The laboratory shall have a recordkeeping system that facilitates the retrieval of all working files and archived records for inspection and verification purposes, e.g., set format for naming electronic files.
E. Responsible staff shall sign or initial all changes to records. The reason for the signature or initials shall be clearly indicated in the records such as "sampled by," "prepared by," or "reviewed by."
F. All generated data except those that are generated by automated data collection systems, shall be recorded directly, promptly and legibly in permanent ink.
G. Entries in records shall not be obliterated by methods such as erasures, overwritten files or markings. All corrections to recordkeeping errors shall be made by one line marked through the error. The individual making the correction shall sign or initial and date the correction. These criteria also shall apply to electronically maintained records.
H. The laboratory shall keep computer and electronic data records in accordance with the pertinent provisions of this section, 1VAC30-45-650 C and E and 1VAC30-45-730 K.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-650. Records management and storage.
A. The laboratory shall keep all records, certificates, and reports as required by applicable state and federal recordkeeping laws and regulations. The laboratory shall safely store these records and hold them secure.
B. The laboratory shall retain all records for a minimum of three years from generation of the last entry in the records, or longer, if required by an applicable regulatory program, whichever is greater. The laboratory shall maintain all information necessary for the historical reconstruction of data, including all original observations, calculations and derived data, calibration records and a copy of the test report.
C. Records that are stored only on electronic media shall be supported by the hardware and software necessary for their retrieval. Records that are stored or generated by computers or personal computers shall have hard copy or write-protected backup copies.
D. The laboratory shall establish a record management system for control of laboratory notebooks, instrument logbooks, standards logbooks, and records for data reduction, validation storage and reporting.
E. The laboratory shall protect these records against fire, theft, loss, environmental deterioration, vermin and, in the case of electronic records, electronic or magnetic sources.
F. The laboratory shall have a plan to ensure that the records are maintained or transferred in the event that a laboratory transfers ownership or goes out of business. In addition, in cases of bankruptcy, the laboratory shall follow appropriate regulatory and state legal requirements concerning laboratory records.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 38, Issue 12, eff. April 1, 2022.
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 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 (e.g., 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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-670. Audits.
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 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 plans.
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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-680. Subcontracting analytical samples.
A. Where a laboratory subcontracts any part of the testing covered under this chapter, the testing shall only be subcontracted to a laboratory certified under 1VAC30-46.
B. The report from the subcontractor shall be a separate part of the laboratory report and identified as laboratory testing done by a subcontractor.
C. The laboratory shall retain records demonstrating that the requirements of this section have been met.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-690. Outside support services and supplies.
A. The laboratory shall have a policy and procedures for the selection and purchasing of services and supplies it uses that affect the quality of environmental tests. Procedures shall exist for the purchase, reception and storage of reagents and laboratory consumable materials relevant for the environmental tests.
B. The laboratory shall ensure that purchased equipment and consumable materials are not used until they have been inspected, calibrated or otherwise verified as complying with standard specifications or requirements defined in the methods for the tests concerned. These services and supplies used shall comply with specified requirements. Records of actions taken to check compliance shall be maintained.
C. The laboratory shall maintain records of all suppliers from whom it obtains support services or supplies required for tests.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-700. Complaints.
The laboratory shall have documented policy and procedures for the resolution of complaints about the laboratory's activities. Where a complaint or any other circumstance raises doubt concerning the laboratory's compliance with the laboratory's policies or procedures, or with the requirements of this chapter or otherwise concerning the quality of the laboratory's calibrations or tests, the laboratory shall ensure that those areas of activity and responsibility involved are promptly audited in accordance with 1VAC30-45-670 A. Records of the complaint and subsequent actions shall be maintained.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-710. Environment and work areas.
Laboratory accommodations, test areas, energy sources, lighting, heating and ventilation shall be such as to facilitate proper performance of tests. Laboratories shall meet the requirements of subdivisions 1 through 8 of this section as appropriate to provide compliance with this requirement.
1. The environment in which these activities are undertaken shall not invalidate the results or adversely affect the required accuracy of measurement. Particular care shall be taken when such activities are undertaken at sites other than the permanent laboratory premises.
2. The laboratory shall provide for the effective monitoring, control and recording of environmental conditions as appropriate. Such environmental conditions may include biological sterility, dust, electromagnetic interference, humidity, mains voltage, temperature, and sound and vibration levels.
3. In instances where monitoring or control of any of the above-mentioned items are specified in a test method or by regulation, the laboratory shall meet and document adherence to the laboratory facility requirements.
4. There shall be effective separation between neighboring areas in which there are incompatible activities including culture handling or incubation areas and volatile organic chemical handling areas. The laboratory shall take measures to prevent cross-contamination.
5. Access to and use of all areas affecting the quality of these activities shall be defined and controlled.
6. Adequate measures shall be taken to ensure good housekeeping in the laboratory and to ensure that any contamination does not adversely affect data quality.
7. Work spaces shall be available to ensure an unencumbered work area.
8. Work areas include:
a. Access and entryways to the laboratory;
b. Sample receipt areas;
c. Sample storage areas;
d. Chemical and waste storage areas; and
e. Data handling and storage areas.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
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 nonroutine 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. Current location, where appropriate;
4. Copy of the manufacturer's instructions, where available;
5. Dates and results of calibrations or verifications or both and date of the next calibration or verification;
6. Details of maintenance carried out to date and planned for the future; and
7. History of any damage, malfunction, modification or repair.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
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.
C. SOPs for laboratory methods.
1. The laboratory shall have and maintain an SOP for each certified analyte or test method.
2. This 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;
c. Limits of detection or quantitation;
d. Scope and application, including parameters to be analyzed;
e. Summary of the test method;
f. Definitions;
g. Interferences;
h. Safety;
i. Equipment and supplies;
j. Reagents and standards;
k. Sample collection, preservation, shipment, and storage;
l. Quality control;
m. Calibration and standardization;
n. Procedure;
o. 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 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.
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 method), for example, drinking water, solids, biological tissue, and air. Laboratories shall follow the procedure in subsection F of this section to demonstrate capability.
2. Thereafter, 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 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 required.
4. In cases where a laboratory analyzes samples using a test method that has not been in use by an individual in the laboratory for at least one 12-month period, another successful demonstration of capability in accordance with subsection F of this section shall be required for that individual to resume testing by the method.
5. In all cases, the laboratory shall document each demonstration of capability as required by subsection G of this section.
6. 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.
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 this standard (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 one to four 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 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. 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.
2. Matrix.
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 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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016; Volume 38, Issue 12, eff. April 1, 2022.
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 independent analysis.
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.
d. 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 (e.g., 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 (e.g., 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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
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 or 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 sample (e.g., total phosphate should be greater than or equal to orthophosphate).
B. Essential quality control procedures. The general quality control principles in subsection C 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. 1VAC30-45-770 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 toxicity, radiochemical, or asbestos testing shall meet the quality control standards for the specific method and the specific type of testing in Modules 3, 6, and 7 of Volume 1 of the 2016 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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016; Volume 38, Issue 12, eff. April 1, 2022.
1VAC30-45-760. Quality control requirements.
A. General.
1. The quality control protocols specified by the laboratory's SOPs shall be followed (1VAC30-45-730 C). The laboratory shall ensure that either the (i) applicable essential standards outlined in this section through 1VAC30-45-775, 1VAC30-45-790 through 1VAC30-45-798, and 1VAC30-45-810 through 1VAC30-45-818 or (ii) mandated methods or regulations, whichever are more stringent, are incorporated into their method SOPs. When it is not apparent which is more stringent, the quality controls in the mandated method or regulations are to be followed.
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 than microbiology, the requirements of subdivisions 1 and 2 of this subsection apply. For microbiology testing, the initial test method evaluation requirements are contained in 1VAC30-45-790 through 1VAC30-45-798. 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 when the testing is conducted using approved methods listed in 40 CFR Part 136 for a program under the federal Clean Water Act, except when the procedure for Determination of Method Detection Limit at 40 CFR Part 136 Appendix B states the procedure is not applicable to a measurement.
b. The laboratory shall determine the LOD for the method for each target analyte of concern in the quality system matrices when test results are to be reported to the LOD (versus the limit of quantitation or working range of instrument calibration), according to 1VAC30-45-771 and 1VAC30-45-814. Where an LOD study is not performed, the laboratory may not report a value below the limit of quantitation.
c. When the LOD is required under subdivision 1 a or 1 b of this subsection, all sample processing steps of the analytical method shall be included in the determination of the LOD.
d. The validity of the LOD shall be confirmed as described in 40 CFR Part 136 Appendix B as applicable, or by qualitative identification of the analyte or analytes 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.
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 at a concentration at or below the LOQ or no more than two times the concentration of 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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016; Errata, 32:24 VA.R. 3395 July 25, 2016; Volume 38, Issue 12, eff. April 1, 2022.
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 (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 | Five |
|
| 71‑90 | Four |
|
| 51‑70 | Three |
|
| 31‑50 | Two |
|
| 11‑30 | One |
|
| Fewer than 11 | None |
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 measurement 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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
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. LOD determination and validation are required as specified by 1VAC3045-760 B 1. 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 LOD shall be verified annually for each quality system matrix, method and analyte according to the procedure as 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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016; Volume 38, Issue 12, eff. April 1, 2022.
1VAC30-45-772. Chemical testing: data reduction.
The procedures for data reduction, such as use of linear regression, shall be documented.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-773. Chemical testing: quality of standards and reagents.
A. The source of standards shall comply with 1VAC30-45-740 C.
B. Reagent quality, water quality and checks.
1. Reagents. In methods where the purity of reagents is not specified, analytical reagent grade shall be used. Reagents of lesser purity than those specified by the test method shall not be used. The labels on the container should be checked to verify that the purity of the reagents meets the requirements of the particular test method. Such information shall be documented.
2. Water. The quality of water sources shall be monitored and documented and shall meet method specified requirements.
3. The laboratory will verify the concentration of titrants in accordance with written laboratory procedures.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-774. Chemical testing: selectivity.
A. The laboratory shall evaluate selectivity by following the checks established within the method, which 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.
B. A confirmation shall be performed to verify the compound identification when positive results are detected on a sample from a location that has not been previously tested by the laboratory. Such confirmations shall be performed on organic tests such as pesticides, herbicides, or acid extractable or when recommended by the analytical test method except when the analysis involves the use of a mass spectrometer. Confirmation is required unless stipulated in writing by the client. All confirmation shall be documented.
C. The laboratory shall document acceptance criteria for mass spectral tuning.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
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. Any cleaning and storage procedures that are not specified by the test method shall be documented in laboratory records and SOPs.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-780. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-781. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-782. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-783. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-784. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-785. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-786. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-787. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-788. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-789. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-790. Microbiology testing: general.
These standards apply to laboratories undertaking microbiological analysis of environmental samples. Microbiological testing refers to and includes the detection, isolation, enumeration, or identification of microorganisms and/or their metabolites, or determination of the presence or absence of growth in materials and media.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
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 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 or organism, and that the medium produces the specified or expected reaction to the target organism or 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 nontarget organisms or does not demonstrate the typical positive reaction of the target 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 culture controls (i.e., nontarget organisms) as appropriate to the method. This shall be done prior to first use of the medium.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016; Errata, 32:24 VA.R. XXX July 25, 2016.
1VAC30-45-792. Microbiology testing: test variability and reproducibility.
For test methods that specify colony counts such as membrane filter or plated media, duplicate counts shall be performed monthly on one positive sample, for each month that the test is performed. If the lab has two or more analysts, each analyst shall count typical colonies on the same plate. Counts shall be within 10% difference to be acceptable. In a laboratory with only one microbiology analyst, the analyst shall count the same plate twice, with no more than 5.0% difference between the counts.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-793. Microbiology testing: method evaluation.
A. Laboratories are required to demonstrate proficiency with the test method prior to first use. This shall be achieved by comparison to a method already approved for use in the laboratory, or by analyzing a minimum of 10 spiked samples whose quality system matrix is representative of those normally submitted to the laboratory, or by analyzing and passing one proficiency test series provided by an approved proficiency sample provider. The laboratory shall maintain this documentation as long as the method is in use and for at least five years past the date of last use.
B. Laboratories shall participate in the proficiency test programs required by Article 3 (1VAC30-45-500 et seq.). The results of these analyses shall be used to evaluate the ability of the laboratory to produce acceptable data.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-794. Microbiology testing: test performance.
A. All growth and recovery media shall be checked to assure that the target organism(s) respond in an acceptable and predictable manner (see 1VAC30-45-791 B).
B. To ensure that analysis results are accurate, target organism identity shall be verified as specified in the method, e.g., by use of the completed test, or by use of secondary verification tests such as a catalase test.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-795. Microbiology testing: data reduction.
The calculations, data reduction and statistical interpretations specified by each test method shall be followed.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
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 of media received, date of receipt, expiration date of the media, and pH of the media.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-797. Microbiology testing: selectivity.
In order to ensure identity and traceability, reference cultures used for positive and negative controls shall be obtained from a recognized national collection, organization, or manufacturer. Microorganisms may be single use preparations or cultures maintained by documented procedures that demonstrate the continued purity and viability of the organism.
1. Reference cultures may be revived (if freeze-dried) or transferred from slants and subcultured once to provide reference stocks. The reference stocks shall be preserved by a technique that maintains the characteristics of the strains. Reference stocks shall be used to prepare working stocks for routine work. If reference stocks have been thawed, they shall not be refrozen and reused.
2. Working stocks shall not be sequentially cultured more than five times and shall not be subcultured to replace reference stocks.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
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 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.
2. Autoclaves.
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, 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.
a. The uniformity of temperature distribution 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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-800. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-801. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-802. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-803. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-804. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-805. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-806. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-807. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-808. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-809. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-810. Air testing: general.
These standards shall apply to samples that are submitted to a laboratory for the purpose of analysis. They do not apply to field activities such as source air emission measurements or the use of continuous analysis devices.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
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. 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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-812. Air testing: analytical variability/reproducibility.
Matrix spike duplicates (MSDs) or laboratory duplicates shall be analyzed at a minimum of one in 20 samples per sample batch. The laboratory shall document their procedure to select the use of appropriate types of spikes and duplicates. The selected samples(s) shall be rotated among sampling points or sampling locations so that various sample matrix problems may be noted and/or addressed. Poor performance in the spikes and duplicates may indicate a problem with the sample composition and shall be reported to the client.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-813. Air testing: method evaluation.
In order to ensure the accuracy of the reported result, the following procedures shall be in place:
1. Demonstration of capability shall be performed prior to the analysis of any samples and with a significant change in instrument type, personnel, quality system matrix, or test method.
2. Calibration. Calibration protocols specified in 1VAC30-45-740 shall be followed.
3. Proficiency test samples. The results of such analyses shall be used by the laboratory to evaluate the ability of the laboratory to produce accurate data.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-814. Air testing: limit of detection.
The requirements of 1VAC30-45-771 shall apply.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-815. Air testing: data reduction.
The procedures for data reduction, such as use of linear regression, shall be documented.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-816. Air testing: quality of standards and reagents.
A. The source of standards shall comply with 1VAC30-45-740 C.
B. The purity of each analyte standard and each reagent shall be documented by the laboratory through certificates of analyses from the manufacturer/vendor, manufacturer/vendor specifications, and/or independent analysis.
C. In methods where the purity of reagents is not specified, analytical reagent grade or higher quality, if available, shall be used.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-817. Air testing: selectivity.
The laboratory shall develop and document acceptance criteria for test method selectivity such as absolute and relative retention times, wavelength assignments, mass spectral library quality of match, and mass spectral tuning.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-818. Air 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. The laboratory shall document that all sampling equipment, containers and media used or supplied by the laboratory meet required test method criteria.
C. If supplied or used by the laboratory, procedures for field equipment decontamination shall be developed and their use documented.
D. The laboratory shall have a documented program for the calibration and verification of sampling equipment such as pumps, meter boxes, critical orifices, flow measurement devices and continuous analyzers, if these equipment are used or supplied by the laboratory.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-819. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-820. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-821. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-822. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-823. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-824. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-825. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-826. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-827. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-828. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-829. (Repealed.)
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; repealed, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-830. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
1VAC30-45-840. (Reserved).
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.
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°C of the required temperature or the method specified range. For samples with a specified temperature of 4°C, samples with a temperature of ranging from just above freezing temperature of water to 6°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 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 collection.
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°C of the specified preservation temperature unless method specific criteria exist. For samples with a specified storage temperature of 4°C, storage at a temperature above the freezing point of water to 6°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 secure (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.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009; amended, Virginia Register Volume 32, Issue 22, eff. September 1, 2016.
1VAC30-45-860. Laboratory report format and contents.
A. The results of each test or series of tests carried out by the laboratory shall be reported accurately, clearly, unambiguously and objectively. The results shall normally be reported in a test report required by regulation and shall include all the information necessary for the interpretation of the test results and all information required by the method used.
B. Where the certificate or report contains results of tests performed by subcontractors, these results shall be clearly identified by subcontractor name or applicable certification number.
C. After issuance of the report, the laboratory report shall remain unchanged. Material amendments to a calibration certificate, test report or test certificate after issue shall be made only in the form of a further document, or data transfer including the statement "Supplement to Test Report or Test Certificate, serial number... (or as otherwise identified)," or equivalent form of wording. Such amendments shall meet all the relevant requirements of this article.
Statutory Authority
§ 2.2-1105 of the Code of Virginia.
Historical Notes
Derived from Virginia Register Volume 25, Issue 7, eff. January 1, 2009.