[35 Pa.B. 519]
[Continued from previous Web Page] § 252.405. Essential quality control requirement--radiochemistry.
(a) In addition to the requirements of § 252.401 (relating to basic requirements), laboratories performing testing or analysis of environmental samples in the area of radiochemistry shall comply with this section.
(b) When the method selected by an environmental laboratory in accordance with § 252.307 (relating to methodology) contains more stringent requirements than the requirements of this section, the environmental laboratory shall follow the more stringent requirements contained in the method.
(c) The requirements for initial calibration are as follows:
(1) An environmental laboratory shall follow the initial calibration requirements of the method or regulation.
(2) Initial calibrations shall be performed using calibration standards that have the same general characteristics as the associated environmental samples, for example geometry, homogeneity and density.
(3) The initial calibration shall include, when applicable, determination of instrument background, efficiency, mass attenuation and energy calibration.
(4) The results of testing or analysis of environmental samples shall be determined from an initial calibration that is not more than 12 months old and may not be determined from any continuing calibration verification, unless otherwise required by regulation, method or program.
(5) The details of the initial calibration procedures including calculations, integrations, acceptance criteria and associated statistics shall be included or referenced in the laboratory's standard operating procedures.
(6) Raw data records shall be retained to permit reconstruction of the initial calibration.
(d) The requirements for an instrument suitability verification are as follows:
(1) An instrument suitability verification standard shall be analyzed at the beginning of each analysis day, unless a higher frequency is required in the method or regulation.
(2) The instrument suitability verification standard shall be a check source that provides adequate counting statistics for a relatively short count time and is sealed or encapsulated to prevent loss of activity and contamination of the instrument and laboratory personnel.
(3) For alpha and gamma spectroscopy systems, the instrument suitability verification standard shall include determination of instrument counting efficiency, energy calibration and peak resolution.
(4) For gas-proportional and liquid scintillation counters, the instrument suitability verification standard shall include determination of instrument counting efficiency.
(5) For scintillation counters, the instrument suitability verification standard shall include determination of instrument counting efficiency.
(6) Details of the instrument suitability verification procedure including calculations, integrations, acceptance criteria and associated statistics shall be included or referenced in the laboratory's standard operating procedures.
(7) Raw data records shall be retained to permit reconstruction of the instrument suitability verification.
(8) Acceptance criteria for instrument suitability verification standards in the method or regulation shall be followed. When there are no established criteria in the method, an environmental laboratory shall determine internal criteria and document the procedure used to establish the criteria.
(9) If an instrument suitability verification standard fails the acceptance criteria, an environmental laboratory shall initiate corrective actions.
(10) Environmental samples not bracketed by acceptable instrument suitability verification standards shall be reanalyzed.
(e) The requirements for an instrument background measurement are as follows:
(1) An instrument background check shall be analyzed every analysis day.
(2) Instrument background values shall be subtracted from the total measured activity in the determination of the sample activity.
(3) Each individual background check shall be compared to the acceptance criteria in the method or regulation. When there are no established criteria in the method or regulation, an environmental laboratory shall determine internal criteria and document the procedure used to establish the limits.
(4) Environmental samples associated with an out of control instrument background check shall be reprocessed and reanalyzed from the beginning of the method or the results reported with the appropriate data qualifiers.
(f) The requirements for a method blank are as follows:
(1) A method blank shall be processed along with and under the same conditions as the associated samples including all steps of the preparation and analytical procedure.
(2) A method blank shall be analyzed at a minimum of one per preparation batch. When no separate preparation method is used, such as gamma analysis in water, the batch shall be defined as no more than 20 environmental samples that are analyzed together using the same method, personnel and lots of reagents.
(3) A method blank shall consist of a matrix that is similar to the associated environmental samples and is free of the isotopes of interest. When a matrix that is similar to the associated environmental samples that is free of the analytes of interest does not exist and cannot be prepared, reagent water or an artificial or simulated matrix may be used.
(4) When an environmental sample is analyzed by gamma spectrometry by placing the sample matrix into a calibrated counting geometry, the method blank shall consist of a similar counting geometry that is filled to a similar volume with reagent water to partially simulate gamma attenuation due to a sample matrix.
(5) The method blank result may not be subtracted from the sample results in the associated preparation or analytical batch unless permitted by the method or regulation.
(6) The method blank shall be prepared with similar aliquot size to that of the routine samples for analysis. The method blank result and acceptance criteria shall be calculated in a manner that compensates for sample results based upon differing aliquot size.
(7) If a contaminant is detected in the method blank, the source of contamination shall be investigated and measures shall be taken to minimize or eliminate the contamination. A method blank is considered contaminated if one of the following applies:
(i) The activity of a target isotope in the method blank is at or above the reporting limit established by the method or by regulation.
(ii) The contamination in the method blank otherwise affects the environmental sample results as described in the method, regulation or in individual project data quality objectives.
(8) Environmental samples associated with a contaminated method blank shall be reprocessed for analysis or the results reported with the appropriate data qualifiers.
(g) The requirements for a laboratory control sample are as follows:
(1) A laboratory control sample shall be processed along with and under the same conditions as the associated environmental samples, including all steps of the preparation and analytical procedure.
(2) The laboratory control sample shall consist of a defined matrix containing known and verified activities of isotopes. When a matrix that is similar to the associated environmental samples that is free of the analytes of interest is not available, reagent water or an artificial or simulated matrix may be used.
(3) A laboratory control sample shall be analyzed at a minimum of one per preparation batch. When no separate preparation method is used, such as gamma analysis in water, the batch shall be defined as no more than 20 environmental samples that are analyzed together with the same method, personnel and lots of reagents.
(4) The activity of the laboratory control sample shall be within the calibration range of the method and one of the following
(i) Two to ten times the detection limit.
(ii) At an activity level comparable to that of the environmental samples being tested or analyzed, if the sample activities are expected to exceed ten times the detection limit.
(5) The standard used to prepare the laboratory control sample shall be from a source independent of the standards used for initial calibration.
(6) When a radiochemical method, other than gamma spectroscopy, has more than one reportable isotope, for example, plutonium, Pu 238 and Pu 239, using alpha spectrometry, only one of the isotopes shall be included in the laboratory control sample. When more than one isotope is present above the specified detection limit, each isotope shall be assessed against the acceptance criteria.
(7) When gamma spectrometry is used to identify and quantitate more than one isotope, the laboratory control sample shall contain isotopes that represent the low, for example americium-241, medium, for example cesium-137, and high, for example cobalt-60, energy range of the analyzed gamma spectra. The isotopes need not exactly bracket the calibrated energy range or the range over which isotopes are identified and quantitated.
(8) Each individual laboratory control sample shall be compared to the acceptance criteria in the method or regulation. When there are no established criteria in the method or regulation, an environmental laboratory shall determine internal criteria and document the procedure used to establish the limits.
(9) Environmental samples associated with an out of control laboratory control sample shall be reprocessed and reanalyzed from the beginning of the method or the results reported with the appropriate data qualifiers.
(h) The requirements for sample duplicates are as follows:
(1) A sample duplicate shall be analyzed at a minimum of one per preparation batch. When no separate preparation method is used, for example gamma analysis in water, the batch shall be defined as no more than 20 environmental samples that are analyzed together using the same method, personnel and lots of reagents.
(2) An environmental laboratory shall document the calculations used for determining the relative percent difference or other statistical method for evaluation of the sample duplicate pairs.
(3) Each sample duplicate relative percent difference shall be compared to the acceptance criteria in the method or regulation. When there are no established criteria in the method or regulation, an environmental laboratory shall determine internal criteria and document the procedure used to establish the acceptance limits.
(4) For sample duplicate results outside established criteria, corrective action shall be documented and the affected data reported with appropriate data qualifiers.
(i) Tracer requirements are as follows:
(1) For those methods that utilize a tracer or internal standard, each sample result shall have an associated tracer or internal standard recovery calculated and reported.
(2) The tracer or internal standard recovery shall be assessed against the acceptance criteria specified in the method or regulation. When there are no established criteria in the method or regulation, an environmental laboratory shall determine internal criteria and document the procedure used to establish the acceptance limits.
(3) For tracer or internal standard recovery outside established criteria, corrective action shall be documented and the data reported with appropriate data qualifiers.
(j) Carrier requirements are as follows:
(1) For those methods that utilize a carrier, each sample must have an associated carrier recovery calculated and reported.
(2) The carrier recovery for each sample shall be assessed against the acceptance criteria specified in the method or regulation. When there are no established criteria in the method or regulation, an environmental laboratory must determine internal criteria and document the procedure used to establish the acceptance limits.
(3) For carrier recovery outside established criteria, corrective action shall be documented and the data reported with appropriate data qualifiers.
(k) The requirements for detection limits are as follows:
(1) A detection limit shall be determined by the protocol in the method or regulation. If the protocol for determining detection limits is not specified in the method or regulation, the environmental laboratory shall select a procedure that reflects instrument limitations and the intended application of the method.
(2) A detection limit shall be initially determined for the isotopes of interest in each method in a matrix in which neither the target isotope nor interferences are at a concentration that would impact the results. The detection limit shall be determined in the matrix of interest.
(3) A detection limit shall be determined each time there is a change in the method that affects how the test is performed or that affects the sensitivity of the analysis.
(4) The sample processing steps of the method shall be included in the determination of the detection limit.
(5) Supporting data shall be retained to permit reconstruction of the detection limit determination.
(6) An environmental laboratory shall have a written procedure to relate detection limits with quantitation limits.
(7) The method's lower limit of quantitation must be established and must be above the detection limit.
(l) Each result shall be reported with the associated measurement uncertainty. The procedures for determining the measurement uncertainty shall be documented and be consistent with the method and regulation.
Subchapter E. PROFICIENCY TEST STUDY REQUIREMENTS Sec.
252.501. Proficiency test study requirements. § 252.501. Proficiency test study requirements.
(a) By _____ (Editor's Note: The blank refers to a date 30 days of the effective date of this chapter), the Department will publish a list of fields of accreditation for which proficiency test studies are available. The Department may update the list of available fields of accreditation by publishing a revised list of available proficiency test studies.
(b) An environmental laboratory shall participate in proficiency test studies, when available, as specified in subsection (a), for each field of accreditation for which the laboratory seeks to obtain or maintain accreditation.
(c) Within the 12 months prior to applying for initial accreditation under this chapter or during the approval process, an environmental laboratory shall successfully analyze at least one single blind, single concentration proficiency test study, when available, as specified in subsection (a), for each field of accreditation for which it seeks accreditation.
(d) An environmental laboratory accredited under this chapter shall successfully analyze at least one single blind, single concentration proficiency test study for each field of accreditation, when available, as specified in subsection (a), for which the laboratory is accredited at least once every 12 months.
(e) Proficiency test studies shall be purchased at the environmental laboratory's expense directly from suppliers approved by the Department as a proficiency test provider.
(f) An environmental laboratory shall ensure that all proficiency test study samples are managed, analyzed and reported in the same manner as real environmental samples and utilize the same staff, procedures, equipment, facilities, number of replicates and methods for the routine analysis of the analyte.
(g) An environmental laboratory may not send a proficiency test study, or a portion of a proficiency test study, to another laboratory for analysis for a field of accreditation for which it seeks accreditation or is accredited prior to the time the results of the study are released by the proficiency test study provider.
(h) An environmental laboratory may not knowingly analyze a proficiency test study, or a portion of a proficiency test study, for another environmental laboratory for which the sending environmental laboratory seeks accreditation or is accredited prior to the time the results of the study are released by the proficiency test study provider.
(i) An environmental laboratory may not communicate with another environmental laboratory, including other laboratories under common ownership, concerning the proficiency test study prior to the time the results of the study are released by the proficiency test study provider.
(j) An environmental laboratory may not attempt to obtain the prepared value of a proficiency test study from the proficiency test study provider prior to the time the results of the study are released by the proficiency test study provider.
(k) If an environmental laboratory fails to successfully analyze a proficiency test study, it shall determine the cause for the failure and take any necessary corrective action. The laboratory shall document the investigation and corrective action.
(l) An environmental laboratory shall direct the proficiency test study provider to report the proficiency test study performance results directly to the Department at the same time that the provider reports the results to the environmental laboratory.
(m) An environmental laboratory shall maintain copies of all raw data associated with proficiency test studies for at least 5 years.
Subchapter F. ONSITE ASSESSMENT REQUIREMENTS Sec.
252.601. Onsite assessment requirements. § 252.601. Onsite assessment requirements.
(a) Prior to accrediting an environmental laboratory, the Department will perform an onsite assessment of the laboratory.
(b) Prior to granting accreditation for an additional field of accreditation to an environmental laboratory, the Department may perform an onsite assessment of the laboratory.
(c) The Department may conduct announced or unannounced onsite assessments of an environmental laboratory to ensure compliance with the conditions of accreditation, this chapter or orders issued by the Department.
(d) The Department will provide the environmental laboratory with an onsite assessment report documenting any deficiencies found by the Department.
(e) An environmental laboratory shall submit a corrective action report to the Department within 60 calendar days from receipt of an onsite assessment report from the Department where the Department has found deficiencies. The corrective action report shall document the corrective action taken by the laboratory to correct each deficiency.
(f) If any portion of the corrective action report is not acceptable, an environmental laboratory shall submit a revised written corrective action report within 30 calendar days from receipt of the Department's response. If the second corrective action report is not acceptable, the Department may revoke accreditation.
(g) Unless otherwise approved by the Department, deficiencies shall be corrected within 120 calendar days of receipt of the onsite assessment report.
(h) The Department may extend the period of implementing corrective actions, for specific deficiencies, for a maximum of 30 calendar days upon receipt of the laboratory's written petition and corrective action report, when the laboratory must take one or more of the following actions:
(1) Purchase new equipment.
(2) Revise the quality manual.
(3) Replace significant laboratory personnel.
Subchapter G. MISCELLANEOUS PROVISIONS Sec.
252.701. Expiration of application. 252.702. Denial of application. 252.703. Revocation. 252.704. Suspension. 252.705. Voluntary relinquishment. 252.706. Use of accreditation. 252.707. Recordkeeping. 252.708. Subcontracting. 252.709. Reporting and notification requirements. § 252.701. Expiration of application.
An environmental laboratory that fails to meet the requirements for accreditation within 1 year from the date the Department receives the application shall submit a new application and pay the appropriate fee to become accredited under this chapter.
§ 252.702. Denial of application.
(a) The Department will deny an application for accreditation or application for renewal of accreditation under one or more of the following circumstances:
(1) The environmental laboratory is in continuing violation of or demonstrates an inability or lack of intention to comply with this chapter or other laws administered by the Department.
(2) The Department revoked the environmental laboratory's certificate of accreditation for all fields of accreditation for failure to correct deficiencies identified in an onsite assessment report within the previous 6 months.
(b) The Department may deny an application for accreditation or application for renewal of accreditation for one or more of the following reasons:
(1) Falsifying analyses.
(2) Selectively reporting data.
(3) Making misrepresentations to the Department.
(4) Engaging in unethical or fraudulent practices.
(5) Analysis of proficiency test studies by personnel other than the analysts associated with the routine analysis of environmental samples in the laboratory.
(6) Failure to submit a complete application.
(7) Failure to pay required fees.
(8) Failure of laboratory staff to meet the personnel qualifications of education, training and experience.
(9) Failure to successfully analyze and report proficiency test studies as required by this chapter.
(10) Failure to respond to an onsite assessment report with a corrective action report within the required timeframes.
(11) Failure to submit an acceptable corrective action report in response to an onsite assessment within the required timeframes.
(12) Failure to implement the corrective actions detailed in the environmental laboratory's corrective action report within a time frame approved by the Department.
(13) Failure to implement a quality assurance program.
(14) Failure to pass an onsite assessment.
(15) Denial of entry to the Department during normal business hours for an onsite assessment.
(16) Violation of a statute, this chapter or an order of the Department.
(17) Failure to meet the requirements of this chapter.
§ 252.703. Revocation.
(a) The Department will revoke an environmental laboratory's accreditation for a field of accreditation when, after being suspended due to failure to participate in a required proficiency test study or due to failure to obtain an acceptable result for a proficiency test study, the laboratory's analysis of the next proficiency test study results in a failed proficiency test study for that field of accreditation.
(b) The Department may revoke an environmental laboratory's accreditation, in part or in total, for one or more of the following reasons:
(1) Failure to respond to an onsite assessment report with a corrective action report within the required timeframes.
(2) Failure to correct deficiencies identified during an onsite assessment of the environmental laboratory.
(3) Failure to implement corrective action related to violations or deficiencies found during an onsite assessment.
(4) Failure of an environmental laboratory that has been suspended to correct all outstanding violations or deficiencies within 6 months of the effective date of the suspension.
(5) Failure to submit an acceptable corrective action report in response to an onsite assessment report within the required timeframes.
(6) Violation of a condition of accreditation.
(7) Violation of a statute, this chapter or an order of the Department.
(8) Falsifying analyses.
(9) Selectively reporting data.
(10) Making misrepresentations to the Department.
(11) Engaging in unethical or fraudulent practices.
(12) Analysis of proficiency test studies by personnel other than the analysts associated with the routine analysis of environmental samples in the laboratory.
(13) Failure to implement a quality assurance program.
(14) Failure to participate in the proficiency test study program as required by this chapter.
(15) Denial of entry to the Department during normal business hours for an onsite assessment.
(16) Failure to comply with the reporting and notification requirements as specified in § 252.709 (relating to reporting and notification requirements).
(17) Failure to employ staff that meets the personnel qualifications for education, training and experience.
(18) Failure to meet the requirements of this chapter.
(c) The environmental laboratory may continue to test or analyze environmental samples for those fields of accreditation not revoked.
(d) Within 72 hours of receiving notice of the revocation of accreditation from the Department, the environmental laboratory shall notify each of its customers affected by the revocation in writing of the revocation on a form approved by the Department.
§ 252.704. Suspension.
(a) Denial of access to the Department during normal business hours will result in immediate suspension of accreditation for all fields of accreditation. Upon notice from the Department, the laboratory shall immediately cease testing or analysis of environmental samples.
(b) The Department will suspend an environmental laboratory's accreditation in total or in part for one or more of the following reasons:
(1) The Department finds that protection of the environment or the public health, safety or welfare requires emergency action.
(2) The environmental laboratory fails to successfully complete a proficiency test study within the previous 12 months.
(3) The environmental laboratory fails two consecutive proficiency test studies for a field of accreditation.
(c) The Department may suspend a laboratory's accreditation in total or in part for one or more of the following reasons:
(1) Failure to comply with the reporting and notification requirements as specified in § 252.709 (relating to reporting and notification requirements).
(2) Failure to implement a quality assurance program.
(3) Failure to employ staff that meets the personnel qualifications for education, training and experience.
(d) A laboratory may continue to test or analyze environmental samples for those fields of accreditation not affected by the suspension.
(e) Within 72 hours of receiving notice of the suspension of accreditation from the Department, the environmental laboratory shall notify each of its customers affected by the suspension in writing of the suspension on a form approved by the Department.
§ 252.705. Voluntary relinquishment.
(a) An environmental laboratory wishing to voluntarily relinquish its certificate of accreditation shall notify the Department in writing.
(b) An environmental laboratory that voluntarily relinquishes its certificate of accreditation shall insure records are maintained in accordance with § 252.707 (relating to recordkeeping).
(c) Within 72 hours of voluntarily relinquishing its certificate of accreditation, the laboratory shall notify each of its customers affected by the voluntary relinquishment in writing of the relinquishment on a form approved by the Department.
§ 252.706. Use of accreditation.
(a) Environmental laboratories accredited by the Department shall:
(1) Post or display their most recent certificate of accreditation for all fields of accreditation in a prominent place in the laboratory.
(2) Make accurate statements concerning their accreditation status.
(3) Not use their certificate of accreditation, accreditation status or the Department's logo to imply endorsement by the Department.
(b) Environmental laboratories using the Department's name, making reference to its accreditation status or using the Department's logo in catalogs, advertising, business solicitations, proposals, quotations, laboratory analytical reports or other materials, shall:
(1) Distinguish between testing for which the laboratory is accredited and testing for which the laboratory is not accredited.
(2) Include the environmental laboratory's accreditation number.
(c) Upon suspension, revocation or voluntary relinquishment of accreditation, a laboratory shall:
(1) Discontinue use of all catalogs, advertising, business solicitations, proposals, quotations, laboratory analytical results or other materials that contain reference to the laboratory's past accreditation status.
(2) Discontinue use or display of the Department's logo.
(3) Return certificates of accreditation to the Department within 48 hours.
(d) NELAP accredited laboratories shall accompany the Department's name or the NELAC/NELAP logo with the phrase ''NELAP accredited'' and the laboratory's accreditation number when using the Department's name or the NELAC/NELAP logo on general literature such as catalogs, advertising, business solicitations, proposals, quotations, laboratory analytical reports or other materials.
(e) NELAP accredited laboratories may not use their NELAP certificate, NELAP accreditation status or NELAC/NELAP logo to imply endorsement by the Department or NELAC.
§ 252.707. Recordkeeping.
(a) An environmental laboratory shall maintain records in a manner accessible by the Department.
(b) An environmental laboratory shall maintain records that allow reconstruction of all laboratory activities associated with the testing or analysis of environmental samples.
(c) Records required under this chapter shall be maintained for a minimum of 5 years unless otherwise specified.
(d) An environmental laboratory shall have a written plan that specifies how records will be maintained or transferred if laboratory transfers ownership or terminates operations.
§ 252.708. Subcontracting.
(a) The subcontracted environmental laboratory shall be indicated on the final report.
(b) An environmental laboratory may not subcontract testing or analysis covered under this chapter to an environmental laboratory that is not accredited and in compliance with this chapter.
§ 252.709. Reporting and notification requirements.
(a) An environmental laboratory conducting testing or analysis of drinking water under Chapter 109 (relating to safe drinking water) shall meet the reporting and notification requirements of that chapter.
(b) An environmental laboratory shall notify the Department, in writing, within 30 calendar days of changes in laboratory supervisors, analysts, supervisor or analyst assignments, testing or analysis equipment and facilities which affect accredited fields of accreditation.
(c) An environmental laboratory shall notify the Department, in writing, within 30 calendar days of a change in the legal name of the laboratory.
(d) An out-of-State environmental laboratory with either primary or secondary accreditation from the Department shall notify, in writing, the Department within 48 hours of any changes in the laboratory's accreditation status from any other primary accrediting authority.
(e) The Department may require additional information or proof of continued capability to perform the testing or analysis for affected fields of accreditation upon receipt of notification under this subsection.
(f) The Department may require an onsite assessment under § 252.601 (relating to onsite assessments) upon receipt of notification under this subsection.
[Pa.B. Doc. No. 05-149. Filed for public inspection January 21, 2005, 9:00 a.m.]
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