[35 Pa.B. 519]
[Continued from previous Web Page] § 252.303. Grandfathering provisions for laboratory supervisors.
(a) A person who does not meet the education credential requirements for a laboratory supervisor but possesses the requisite years of experience required by § 252.302 (relating to qualifications of the laboratory supervisor) shall qualify as laboratory supervisor subject to the following conditions:
(1) The person shall be a laboratory supervisor of the environmental laboratory on the date the environmental laboratory becomes subject to accreditation.
(2) The person shall have been a laboratory supervisor of the environmental laboratory for at least 12 months for the fields of accreditation for which the environmental laboratory is applying.
(b) A person will be approved as a laboratory supervisor only for those fields of accreditation for which the person has been laboratory supervisor of the environmental laboratory for at least 12 months.
(c) The Department may approve a person, qualified as a laboratory supervisor under this section, for additional fields of accreditation if the person has the appropriate knowledge, skills and abilities to perform and supervise the testing or analyses on environmental samples for the requested fields of accreditation.
§ 252.304. Personnel requirements.
(a) General requirements for technical staff.
(1) An environmental laboratory shall have sufficient personnel with the necessary education, training, technical knowledge and experience for their assigned functions.
(2) Each member of the environmental laboratory technical staff shall be responsible for complying with quality assurance and quality control requirements that pertain to their organizational or technical function.
(3) Each environmental laboratory technical staff member shall have a combination of experience and education to adequately demonstrate a specific knowledge of their particular function and a general knowledge of laboratory operations, test methods, quality assurance and quality control procedures and records management.
(b) Laboratory management responsibilities. The environmental laboratory management shall be responsible for:
(1) Defining the minimal level of qualification, experience and skills necessary for all positions or work cells in the environmental laboratory.
(2) Ensuring and documenting that the environmental laboratory technical staff members or work cells have demonstrated capability in the activities for which they are responsible.
(3) Ensuring and documenting that the training and competency of each member of the environmental laboratory technical staff is kept up to date by maintaining records demonstrating the following:
(i) That each employee has read, understood and is using the latest version of the environmental laboratory's quality manual that relates to each employee's job responsibilities.
(ii) That each employee has read, understood and is using the latest versions of the environmental laboratory's standard operating procedures that relate to each employee's job responsibilities.
(iii) Participation in training courses or workshops on specific equipment, analytical techniques or laboratory procedures that relate to each employee's job responsibilities.
(iv) Participation in training courses in ethical and legal responsibilities including the potential liabilities for improper, unethical or illegal actions.
(v) That each employee has read, understood and acknowledged his personal ethical and legal responsibilities including the potential punishments and penalties for improper, unethical or illegal actions.
(vi) An initial demonstration of capability for each method that relates to the employee's job responsibilities.
(vii) A demonstration of continued proficiency by at least one of the following every 12 months for each method that relates to the employee's job responsibilities:
(A) Another initial demonstration of capability.
(B) Acceptable performance of blind performance samples (single blind to the analyst).
(C) Successful analysis of blind proficiency test samples on a similar test method using the same technology (for example--GC/MS volatiles by purge and trap for EPA Methods 524.2, 624 or 5035/8260 would require documentation for only one of the test methods.)
(D) At least four consecutive laboratory control samples with acceptable levels of precision and accuracy.
(E) Analysis of at least ten authentic samples with results statistically indistinguishable from those obtained by another trained analyst. The samples must include samples free of the analyte of interest and samples containing the analyte of interest at measurable concentrations.
(4) Documenting analytical and operational activities of the laboratory.
(5) Supervising personnel employed by the laboratory.
(6) Establishing and implementing procedures and processes for permitting departures from documented policies and procedures.
(7) Ensuring that sample acceptance criteria are verified and that samples are logged into the sample tracking system and properly labeled and stored.
(8) Documenting the quality of data reported by the laboratory.
(9) Developing a proactive program for prevention and detection of improper, unethical, or illegal actions. Components of this program may include the following:
(i) Internal proficiency testing (single and double blind).
(ii) Postanalysis electronic data and magnetic tape audits or reviews.
(iii) Separate standard operating procedures identifying appropriate and inappropriate laboratory and instrument manipulation practices.
(c) An environmental laboratory shall maintain records on initial demonstrations of capability, demonstrations of continued proficiency, proficiency test samples for each laboratory method and the qualifications, training, skills and experience of the laboratory technical staff members.
§ 252.305. Physical facilities.
(a) An environmental laboratory shall have accommodations, work areas, energy sources, lighting, heating and ventilation necessary to assure proper performance of tests and analyses.
(b) The environment in which testing or analysis of environmental samples is undertaken may not adversely affect the results of the testing or analysis or the required accuracy of measurement.
(c) An environmental laboratory shall document its monitoring and control of environmental conditions where monitoring or control of environmental conditions is specified in a method or by regulation.
(d) There must be effective separation between neighboring work areas and between work areas and nonwork areas when the activities performed in the different areas are incompatible.
(e) Adequate measures shall be taken to ensure that contamination does not adversely affect data quality.
§ 252.306. Equipment, supplies and reference materials.
(a) An environmental laboratory shall be furnished with all items of equipment, including reference materials, required for the correct performance of tests or analyses for which accreditation is sought.
(b) An environmental laboratory shall maintain records of each item of equipment significant to the testing or analysis performed. These records must include documentation on the following:
(1) The name of the item of equipment.
(2) The manufacturer's name, type identification, and serial number or other unique identification.
(3) The date received and date placed in service (if available).
(4) The current location, when appropriate.
(5) If available, condition when received (for example, new, used or reconditioned).
(6) A copy of the manufacturer's instructions, where available.
(7) The dates and results of calibrations or verifications.
(8) The manufacturer's instructions, if available, or reference their location.
(9) The details of maintenance performed.
(10) A history of damage, malfunction, modification or repair.
(c) An environmental laboratory shall assure that the test instruments consistently operate within the specifications required of the application for which the equipment is used.
(d) Equipment shall be properly maintained, inspected and cleaned.
(e) Any item of equipment that has been subjected to overloading, mishandling, gives suspect results or has otherwise been shown to be defective, shall be taken out of service and clearly identified 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 testing or analysis.
(f) The following pieces of equipment shall be maintained according to this subsection.
(1) Certified NIST-reference thermometer.
(i) A certified NIST-reference thermometer must have appropriate graduations and a range that spans the requirements of the method.
(ii) The certified NIST-reference thermometer shall be recalibrated at least once every 5 years at the temperatures of use.
(iii) An environmental laboratory shall retain a certificate documenting traceability of the calibration to NIST standards.
(2) Working thermometers.
(i) Working thermometers must have appropriate graduations and a range that spans the requirements of the method.
(ii) Working thermometers may be glass, dial or electronic and shall be calibrated against a certified NIST-reference thermometer as follows:
(A) Glass and electronic thermometers and continuous recording devices shall be calibrated every 12 months at the temperature used.
(B) Dial thermometers shall be calibrated every 3 months at the temperature used. Dial thermometers that cannot be calibrated may not be used.
(C) An environmental laboratory shall maintain records in a laboratory notebook for each working thermometer that documents the date of calibration, NIST reference thermometer identification, working thermometer identification, reference thermometer temperature reading, working thermometer temperature reading, correction factor and the initials of the individual conducting the calibration.
(D) Working thermometers shall be uniquely identified and labeled with the date of calibration and correction factor.
(iii) The fluid column in glass thermometers may not be separated.
(iv) A working thermometer that differs by more than 1.0°C from the reference thermometer may not be used.
(3) ASTM type 1, 2 or 3 (Class S or S-1) certified reference weights.
(i) The mass of ASTM type 1, 2 or 3 (Class S or S-1) certified reference weights shall be recertified at least once every 5 years.
(ii) An environmental laboratory shall retain a certificate documenting traceability of the calibration to ASTM standards.
(4) Analytical or pan balances.
(i) Analytical or pan balances must provide sufficient accuracy and sensitivity for the weighing needs of the method.
(ii) An environmental laboratory shall verify the calibration of an analytical balance daily or before each use, whichever is less frequent.
(iii) An environmental laboratory shall verify the calibration of a pan balance monthly or before each use, whichever is less frequent.
(iv) A reference weight that is damaged or corroded may not be used for calibration of balances.
(v) Balance calibration shall be verified using a minimum of three ASTM type 1, 2 or 3 (Class S or S-1) certified reference weights that bracket the effective range of the balance's use.
(vi) An environmental laboratory shall maintain records in a laboratory notebook of balance calibrations that document the balance identification, date of calibration verification, reference weights used and initials of the individual performing the calibration. Correction factors shall be documented and used.
(vii) A qualified person shall service and calibrate analytical balances at least once per year.
(viii) Records of annual service shall be maintained and the service date shall be recorded on the balance.
(5) pH meter.
(i) A pH meter must be equipped with an appropriate electrode and have scale graduations and accuracy appropriate to the method.
(ii) An environmental laboratory shall utilize either a thermometer or a temperature sensor for automatic compensation to make corrections for pH measurements.
(iii) The pH meter shall be standardized daily or before each use, whichever is less frequent, by one of the following:
(A) With at least three standard buffers which are at least three pH units apart and which bracket the expected pH range of the samples.
(B) Use a pH 7.0 and either a pH 4.0 or 10.0 standard buffer; whichever range covers the desired pH range of use.
(iv) Aliquots of standard buffers may not be used for longer than 1 analysis day.
(v) Records of pH meter standardization shall be maintained in a laboratory notebook that documents the date of standardization, calibration buffers used and initials of the individual conducting the standardization.
(6) Conductivity meter.
(i) A conductivity meter must have a probe of sufficient sensitivity for the method. The scale must have readability in appropriate units, for example micromhos or microsiemens per centimeter.
(ii) An in-line conductivity meter that cannot be calibrated may not be used.
(iii) An environmental laboratory shall calibrate the conductivity meter daily or before each use whichever is less frequent, by one of the following:
(A) With certified and traceable standard solutions within the range of interest.
(B) By determining the cell constant utilizing the method described in currently approved editions of Standard Methods for the Examination of Water and Wastewater (available from American Public Health Association, 1015 Fifteenth Street NW, Washington, D.C. 20005.)
(iv) Records of conductivity meter calibrations shall be maintained in a laboratory notebook that documents the date of calibration, standards used, results of calibration or cell constant determined and the initials of the individual conducting the calibration.
(7) Refrigeration equipment and freezers.
(i) An environmental laboratory shall maintain one thermometer immersed in liquid (except electronic thermometers) to the appropriate immersion line for each refrigerator or freezer. The thermometer must be graduated in increments no larger than 1°C.
(ii) Calibration-corrected temperatures for each refrigerator and freezer shall be recorded once a day for each day in use for all laboratory activities. The date, refrigerator or freezer identification, calibration corrected temperature and initial of responsible individual shall be recorded.
(iii) Samples and standards shall be stored in separate refrigerators where the potential for cross-contamination exists.
(iv) Samples which require thermal preservation shall be stored at a temperature which is + 2°C of the specified preservation temperature unless method specific criteria exist. For samples with a storage temperature of 4°C, storage at a temperature of 0.5°C to 6°C is acceptable.
(v) Freezer temperatures must be less than 0°C.
(8) Incubators, water baths and heating blocks.
(i) An environmental laboratory shall control and monitor the temperature of incubators, water baths and heating blocks in accordance with the method or as specified by regulations.
(ii) An environmental laboratory shall maintain a minimum of one thermometer per incubator, water bath or heating block immersed in liquid (except electronic thermometers) to the appropriate immersion line. When used as an incubation unit for microbiology, a minimum of one working thermometer shall be on the top and bottom shelf of the use area in each incubator.
(iii) When used as an incubation unit for microbiology, a water bath must be equipped with a gable cover and a pump or paddles to circulate the water.
(iv) Calibration-corrected temperatures for each incubator, water bath or heating block shall be recorded once a day for each day in use for all laboratory activities. When used as an incubation unit for microbiology, the calibration-corrected temperature shall be recorded at least twice per day in use with the readings separated by at least four hours. The incubator, water bath or heating block identification, date, time, calibration corrected temperature and the initials of the responsible individual shall be recorded.
(9) Volumetric dispensing devices. Except for Class A glassware, mechanical volumetric dispensing devices including burettes, autopipetors and dilutors, must be of sufficient sensitivity for the application. Delivery volumes of mechanical volumetric dispensing devices shall be checked using a gravimetric method at least once every 3 months.
(10) Graduated sample containers. When graduation marks on clear glass or plastic funnels or sample bottles are used to measure sample volume, an environmental laboratory shall verify and document the accuracy of the volume of each lot or at least once per year, whichever is more frequent.
(11) Visual comparison devices. Visual comparison devices must be calibrated according to the manufacturer's specifications or test methods. An environmental laboratory shall maintain records of the calibrations.
(g) An environmental laboratory shall maintain records for all reference materials, reagents and support services utilized by the laboratory for testing or analysis.
(h) Reference materials and reagents used for environmental testing must meet the following minimum requirements:
(1) Analytical reagent grade chemicals or equivalent are acceptable, unless a method specifies other reagent purity grade requirements.
(2) Reagent and standard solutions shall be checked regularly for signs of decomposition, evaporation, and expiration. An environmental laboratory shall maintain standard and reagent preparation logs for all stock and working standard solutions in a laboratory notebook. Standards and reagent preparation logs must contain identification of the compound, concentration, date prepared, initials of the individual preparing the solution and expiration date.
(3) Reagent and standard solution containers shall be labeled with identification of the compound, concentration, date prepared, initials of the individual who prepared the solution and expiration date.
(4) Purchased chemicals, solutions and standards shall be labeled with date of receipt and the date when the container is opened. Purchased chemicals, solutions and standards without an expiration date on the original container shall be discarded after 10 years from the date of receipt.
(5) When reagents are removed from a container, the amount removed shall be used entirely or the unused portion discarded.
(6) Compressed gases must be of commercial grade, unless a method specifies other requirements.
(i) Plastic and glassware shall be cleaned to meet the sensitivity of the test method. Any cleaning and storage procedures that are not specified by the method shall be documented in a laboratory standard operating procedure.
§ 252.307. Methodology.
(a) An environmental laboratory shall follow the requirements for testing or analysis, sample collection, sample preservation and holding times specified in this section.
(b) An environmental laboratory shall select an analytical method for a specific test or analysis that meets the following criteria:
(1) The method is appropriate for the analyte and sample matrix.
(2) The method is required by applicable State or Federal regulations, a permit, an order, or is an approved alternate method under subsection (c).
(3) The method enables the laboratory to quantitate at required levels.
(c) When a method meeting the requirements of subsection (b) is not available, an environmental laboratory may apply to the Department to use alternate or experimental procedures.
(1) The Department will approve the use of alternate methodologies if the EPA has approved their use. An environmental laboratory shall submit a copy of the EPA's written approval for the use of the alternate method to the Department.
(2) The Department may allow alternate methods that use new or innovative technologies on a case-by-case basis.
(3) An environmental laboratory shall submit a request for use of new or innovative technology in writing to the Department. The request must include the reasons for proposing the method and the potential scope of use for the method.
(4) The Department will establish criteria for validating the method.
(5) Upon receipt of the method validation data that meets the established criteria, the Department will approve or deny the request within 90 days. The evaluation for approval will include consideration of the demonstrated need for the new or innovative technology, reasons for using the method, performance of the method, method validation data and applicability of the method to the matrix.
(d) An environmental laboratory shall develop and maintain written standard operating procedures for all fields of accreditation.
(1) The environmental laboratory's standard operating procedures must accurately reflect all aspects of the testing or analysis for the fields of accreditation, including the following:
(i) Identification of the method.
(ii) Effective date.
(iii) Scope, including applicable matrix or matrices.
(iv) Equipment and supplies.
(v) Reagents and standards.
(vi) Quality control.
(vii) Calibration and standardization.
(viii) Analytical procedure.
(ix) Calculations.
(x) Corrective actions or contingencies for handling out-of-control or unacceptable quality control data.
(xi) Reporting of results.
(2) The standard operating procedures may consist of copies of published or referenced test methods or standard operating procedures that have been written by the environmental laboratory. When modifications to the published or referenced method have been made by the laboratory or when the published or referenced method is ambiguous or provides insufficient detail, the changes or clarifications shall be clearly described.
(e) An environmental laboratory shall make copies of the standard operating procedures, the promulgated method, Department regulations and Department guidance pertaining to testing or analysis of environmental samples available to the technical staff.
(f) When an environmental laboratory collects a sample to be analyzed, the sample collection method required by applicable State and Federal laws, regulations or permit conditions shall be followed.
(g) An environmental laboratory shall follow the sample container, preservation procedures and holding times required by State and Federal regulations. If the sample container, preservation procedures and holding times are not required by State or Federal regulations, an environmental laboratory shall follow the sample container, sample preservation procedures and holding time established in the method.
(h) The range of quantitation and detection limit shall be determined for each analyte reported by an environmental laboratory in accordance with a method specified by the Department.
(i) When a method specifies a validation procedure, the validation procedure shall be completed before environmental samples may be analyzed and reported. The results of this validation procedure shall be documented and kept on file for the duration of use of the method and for at least 5 years after the method is no longer in use.
(j) The initial demonstration of capability requirements are as follows:
(1) Prior to the use of any method, an initial demonstration of capability is required.
(2) An initial demonstration of capability shall be completed each time there is a change in instrument type, personnel, or method.
(3) An initial demonstration of capability must include all sample preparation and analytical steps contained in the method.
(4) If the method or State or Federal regulations specify a procedure for the initial demonstration of capability, that procedure shall be followed, otherwise, an initial demonstration of capability shall be performed as follows:
(i) The analyte shall be diluted in a volume of clean matrix sufficient to prepare four aliquots at the concentration specified in the method. If the method does not specify a concentration, the concentration must be approximately ten times the detection limit.
(ii) At least four aliquots of the quality control sample shall be prepared and analyzed according to the method.
(iii) Using all of the results, calculate the mean recovery and the standard deviation of the mean recovery for the population sample in the same units used to report environmental samples. When it is not possible to determine mean and standard deviation, such as for presence-absence and logarithmic values, the environmental laboratory shall assess method performance using criteria from the method or other established and documented criteria.
(iv) Compare the information from subparagraph (iii) to the corresponding acceptance criteria for precision and accuracy in the method. To be considered acceptable, an initial demonstration of capability must meet all acceptance criteria.
(5) When a method has been in use by an environmental laboratory prior to January 1, 2005, and there have been no changes in instrument type, personnel or method, an initial demonstration of capability is not required. An environmental laboratory shall have records on file to demonstrate that an initial demonstration of capability is not required.
(6) The laboratory shall retain all data necessary to reproduce the initial demonstration of capability.
(7) The work cell as a unit shall meet the requirements of this paragraph.
(i) When a member of a work cell changes, the new employee shall work with an experienced analyst in the work cell.
(ii) When a member of a work cell changes, the new work cell shall demonstrate capability by means of acceptable quality control performance checks on four consecutive batches. The acceptable performance shall be documented. If any quality control performance check within the four consecutive batches following the change in personnel fails to meet acceptance criteria, an initial demonstration of capability shall be completed.
(iv) If the entire work cell is changed, an initial demonstration of capability shall be completed.
Subchapter D. QUALITY ASSURANCE AND QUALITY CONTROL REQUIREMENTS Sec.
252.401. Basic requirements. 252.402. Essential quality control requirements-chemistry. 252.403. Essential quality control requirements-toxicity testing. 252.404. Essential quality control requirement-microbiology. 252.405. Essential quality control requirement-radiochemistry. § 252.401. Basic requirements.
(a) An environmental laboratory shall develop and maintain a quality manual appropriate to the type, range and volume of testing and analysis of environmental samples. The quality manual shall be available to and used by environmental laboratory personnel.
(b) The quality manual must state the environmental laboratory's policies, operational procedures, protocols and practices established to meet the requirements of this chapter.
(c) An environmental laboratory shall have a document control system that provides procedures for control and maintenance of all documents. The document control system must ensure that standard operating procedures, methods, manuals or documents clearly indicate the time period during which the procedure or document was in force.
(d) An environmental laboratory shall develop and maintain an ethics policy statement relevant to the employee's duties and responsibilities under the act. The laboratory shall have procedures for educating and training personnel in their ethical and legal responsibilities under the act.
(e) An environmental laboratory shall maintain records of the technical personnel, which include dates of employment, signatures, initials and a list of persons authorized to approve or release reports of testing or analysis of environmental samples.
(f) An environmental laboratory shall establish procedures for handling environmental samples.
(g) An environmental laboratory shall have a sample acceptance policy that clearly outlines the circumstances under which environmental samples will be accepted or rejected. The environmental sample acceptance policy must include the following areas:
(1) Sample identification, location, date and time of collection, collector's name, preservation type and sample type.
(2) Sample labeling.
(3) Use of appropriate containers and sample preservation method.
(4) Adherence to holding times specified in the regulation and when not specified by the regulation, adherence to the holding times specified by the method.
(5) Sufficient sample volume shall be available to perform the necessary testing and analysis, including any required quality control testing or analysis.
(6) Procedures to be used when samples show signs of damage, contamination or inadequate preservation.
(h) An environmental laboratory shall document the laboratory management's processes and procedures for permitting departures from the method, quality manual, established policies and procedures or standard operating procedures.
(i) An environmental laboratory shall establish procedures for detecting when departures from the method or quality manual have occurred. These procedures must include the following:
(1) Identify the individuals responsible for assessing each quality control type.
(2) Identify the individuals responsible for initiating or recommending, or both, corrective actions.
(3) Define how the analyst shall treat the results of testing or analysis of environmental samples if the associated quality control measures fail to meet the requirements of the method.
(4) Specify how out-of-control situations and subsequent corrective actions are to be documented.
(5) Specify procedures for the laboratory supervisor to review corrective action reports.
(j) An environmental laboratory shall develop procedures for reporting results of testing or analysis of environmental samples.
(k) An environmental laboratory shall implement procedures or practices to monitor the quality of the laboratory's analytical activities. Examples of the procedures or practices are:
(1) Internal quality control procedures using statistical techniques.
(2) Participation in proficiency testing, other interlaboratory comparisons, or round robin testing.
(3) Analysis of split samples by different laboratories.
(4) Use of certified reference materials or in-house quality control using secondary reference materials, or both.
(5) Replicate testing using the same or different test methods.
(6) Retesting of retained samples.
(7) Correlation of results for different but related analysis of a sample (for example, total phosphorus should be greater than or equal to orthophosphate).
(l) To the extent possible, results of testing or analysis of environmental 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 results of the testing or analysis of environmental samples are to be reported, all environmental samples associated with the failed quality control measure shall be documented and the results flagged in an unambiguous manner on the sample analysis report with the appropriate data qualifiers.
(m) Policies, procedures, protocols and practices specified in this section must be in writing and be followed.
§ 252.402. Essential quality control requirements-chemistry.
(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 chemistry 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) Initial calibration requirements are as follows:
(1) An environmental laboratory shall follow the initial calibration requirements of the method.
(2) The results of testing or analysis of environmental samples shall be determined from an initial calibration and may not be determined from any continuing calibration verification, unless otherwise required by regulation, method or program.
(3) 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 procedure.
(4) Raw data records shall be retained to permit reconstruction of the initial calibration.
(5) Initial calibrations shall be verified with a standard obtained from a second manufacturer or with a standard from the same manufacturer if the verification standard is documented by the manufacturer as prepared independently of the standard used during initial calibration.
(6) Results not bracketed by the initial calibration standards shall be reported with appropriate qualifiers.
(7) The lowest standard used for initial calibration may not be below the detection limit. The lowest standard must be at or below the lower limit of the range of quantitation.
(d) Except for methods that explicitly allow initial calibration using a single concentration of standard, initial calibration shall be done using multiple concentrations of standards according to the requirements of this subsection.
(1) Unless otherwise specified in the method, the initial calibration must meet one of the following criteria:
(i) A relative standard deviation of less than 20% for the calculated response factors.
(ii) A correlation coefficient (r) of 0.99 for a linear calibration curve.
(iii) A correlation coefficient (r) of 0.999 for a nonlinear calibration curve or as otherwise specified by the Department.
(2) If the initial calibration fails to meet established acceptance criteria, corrective action shall be performed and all associated environmental samples shall be reanalyzed after an acceptable initial calibration is obtained. If reanalysis of the environmental samples is not possible, a new environmental sample shall be collected.
(3) If the results of testing or analysis of environmental samples that are below the initial calibration range are reported, the results shall be reported with appropriate data qualifiers.
(4) If the results of testing or analysis of environmental samples are above the initial calibration range, the environmental sample shall be diluted and reanalyzed or the results reported with appropriate data qualifiers. Sample results within the established calibration range will not require data qualifiers.
(5) The lowest calibration standard may not be below the detection limit and may not be above the MCL.
(6) If the method does not specify the number of calibration standards, the minimum number of calibration standards, not including blanks or a zero standard, shall be determined as follows:
(i) For an initial calibration covering a range up to 20 times the lowest quantitation level, a minimum of three calibration standards shall be used.
(ii) For an initial calibration covering a range from greater than 20 times and up to 50 times the lowest quantitation level, a minimum of four calibration standards shall be used.
(iii) For an initial calibration covering a range greater than 50 times and up to 100 times the lowest quantitation level, a minimum of five calibration standards shall be used.
(e) For a method that explicitly allows calibration using a single concentration of a standard, not including a blank or zero concentration standard, the initial calibration shall meet the requirements of this subsection.
(1) Prior to the testing or analysis of environmental samples, the linear range of the instrument shall be established by analyzing a series of standards, one of which shall be at the lowest quantitation level.
(2) An initial calibration using a single calibration standard and a zero point shall be performed at the beginning of each analysis day.
(3) A standard corresponding to the lowest quantitation level must be analyzed with each analytical batch and must meet the acceptance criteria established by the method. When there are no established criteria in the method, an environmental laboratory shall determine internal criteria and document the procedure used to establish the acceptance limits.
(4) If the results of testing or analysis of environmental samples that are below the lowest quantitation level verification standard, specified in paragraph (3), are to be reported, the results shall be reported with appropriate data qualifiers.
(5) If the results of testing or analysis of environmental samples produce a result above the associated single point standard, the environmental laboratory shall do one of the following:
(i) Analyze a standard at or above the sample concentration that meets established acceptance criteria to validate linearity.
(ii) Dilute the sample so that the result falls below the single point calibration concentration.
(iii) Report the data with an appropriate data qualifier.
(f) Calibration verification requirements are as follows:
(1) A calibration verification standard shall be analyzed at the beginning and end of each analysis day. For methods that use an internal standard, a calibration verification standard is not required at the end of the analysis day unless specified in the method, or State or Federal law or regulation.
(2) A calibration verification standard shall be analyzed after every ten samples, unless a different frequency is specified in the method.
(3) At a minimum, the concentration of the calibration verification standard shall be alternated between a low and a high level.
(i) The concentration of the low calibration verification standard shall be within the lower 20% of the calibration curve and not more than five times the lowest quantitation level.
(ii) The concentration of the high calibration verification standard shall be within the upper 20% of the calibration curve.
(4) Details of the calibration verification procedure including calculations, integrations, acceptance criteria and associated statistics shall be included or referenced in the laboratory's standard operating procedure.
(5) Raw data records shall be retained to permit reconstruction of the calibration verification.
(6) Acceptance criteria for calibration verification standards in the method 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 acceptance limits.
(7) If a calibration verification standard fails the established acceptance criteria, an environmental laboratory shall initiate corrective actions. If the corrective actions fail to produce an immediate consecutive calibration verification standard within the acceptance criteria, a new calibration verification standard shall be prepared. If the freshly prepared calibration verification standard fails to produce a result within the established acceptance criteria, the environmental laboratory shall recalibrate the test or analysis according to the method or as set forth in subsection (c) and as set forth in either subsection (d) or subsection (e).
(8) To the extent possible, and as provided by paragraph (1), environmental samples not bracketed by acceptable calibration verification standards shall be reanalyzed. If the calibration verification standard is found to be out of control, and the results of the testing or analysis of environmental samples are to be reported, all environmental samples associated with the failed calibration verification standard shall be documented and the results flagged in an unambiguous manner on the sample analysis report with the appropriate data qualifiers. Sample results associated with an unacceptable calibration verification may be useable under the following conditions:
(i) When the acceptance criteria for the calibration verification are exceeded high and associated sample results are below the lowest level of quantitation for the analyte of interest.
(ii) When the acceptance criteria for the calibration verification are exceeded low and associated sample results are above the maximum regulatory limit for the analyte of interest.
(g) Method blank requirements are as follows:
(1) A method blank shall be processed along with and under the same conditions as the associated environmental samples including all steps of the analytical procedure.
(2) A method blank shall be analyzed at a minimum of one per preparation batch. When no separate preparation method is used (example: volatiles 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 analytes of interest. 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.
(4) A method blank is considered contaminated if one of the following applies:
(i) The concentration of a target analyte in the method blank is at or above the reporting limit established by the method, by the laboratory or by regulation.
(ii) The contamination in the method blank otherwise affects the environmental sample results as described in the method or in individual project data quality objectives.
(5) 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 problem.
(6) To the extent possible, any environmental samples associated with a contaminated method blank shall be reprocessed for analysis. If a contaminated method blank is found to be out of control, and the results of the testing or analysis of environmental samples are to be reported, all environmental samples associated with the contaminated method blank shall be documented and the results flagged in an unambiguous manner on the sample analysis report with the appropriate data qualifiers.
(h) Laboratory control sample requirements 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 concentrations of analytes. The Department will allow the use of an artificial or simulated matrix when a defined matrix is not commercially available.
(3) An environmental laboratory shall analyze a laboratory control sample at a minimum of one per preparation batch. When no separate preparation method is used, for example volatiles 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) All analyte concentrations in the laboratory control sample shall be within the calibration range of the method and at or below the maximum contaminant level.
(5) The components to be spiked into the laboratory control sample shall be as specified by the method or other regulatory requirement. In the absence of specified components, the environmental laboratory shall use the following:
(i) For those components that interfere with an accurate assessment, such as spiking simultaneously with technical chlordane, toxaphene and PCBs, the laboratory control sample shall represent the chemistries and elution patterns of the components to be reported.
(ii) For methods with more than ten analytes, a representative number may be chosen. The analytes selected shall be representative of all chemistries and analytes reported and shall be chosen using the following criteria:
(A) Targeted components shall be included in the laboratory control sample over a 2-year period.
(B) For methods that include 1-10 components, the laboratory control sample must contain all components.
(C) For methods that include 11-20 components, the laboratory control sample must contain at least ten components or 80%, whichever is greater.
(D) For methods with more than 20 components, the laboratory control samples must contain at least 16 components.
(6) Each individual laboratory control sample shall be compared to the acceptance criteria in the method. When there are no established criteria in the method, an environmental laboratory shall determine internal criteria and document the procedure used to establish the limits.
(7) 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.
(i) Sample duplicate requirements are as follows:
(1) A sample duplicate or matrix spike duplicate shall be analyzed at a minimum of one per preparation batch. When no separate preparation method is used, for example volatiles 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 duplicate pairs.
(3) Each duplicate relative percent difference shall be compared to the acceptance criteria in the method. When there are no established criteria in the method, an environmental laboratory shall determine internal criteria and document the procedure used to establish the acceptance limits.
(4) For duplicate results outside established criteria, corrective action shall be documented and the data reported with appropriate data qualifiers.
(j) Surrogate spike requirements are as follows:
(1) Surrogate compounds, when commercially available, shall be added to all samples, standards and blanks for all organic chromatography test methods.
(2) Surrogate compounds shall be chosen to represent the various chemistries of the target analytes in the method.
(3) The results of the surrogate spike shall be compared to the acceptance criteria published in the method. When there are no established acceptance criteria for surrogate recovery in the method, the environmental laboratory shall establish internal criteria and document the method used to establish the acceptance limits.
(4) For surrogate spike results outside established criteria, corrective action shall be documented and the data reported with appropriate data qualifiers.
(k) Detection limit requirements 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 study is not required for any component for which spiking solutions or quality control samples are not available, such as temperature. A detection limit study is not required for testing or analysis where the results are logarithmic, such as pH, or when the results are expressed as presence or absence.
(3) A detection limit shall be initially determined for the compounds of interest in each method in a matrix in which neither the target analyte nor interferences are at a concentration that would impact the results. The detection limit shall be determined in the matrix of interest.
(4) 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.
(5) The sample processing steps of the method shall be included in the determination of the detection limit.
(6) Supporting data shall be retained to permit reconstruction of the detection limit study.
(7) An environmental laboratory shall have an established procedure to relate detection limits with quantitation limits.
(8) The method's lower limit of quantitation shall be established and shall be above the detection limit.
(l) When retention times are used for the identification of an analyte, an environmental laboratory shall develop and document acceptance criteria for retention time windows. The laboratory shall document acceptance criteria for mass spectral tuning.
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