N.J. Admin. Code § 7:18-5.5

Current through Register Vol. 56, No. 21, November 4, 2024

Section 7:18-5.5 - Requirements for quality assurance/quality control program

(a) The laboratory shall develop and keep current a quality assurance/quality control manual. The laboratory shall not perform analyses of regulatory samples without having a current quality assurance/quality control manual covering the analysis in question. In the manual, the laboratory shall describe the following:

1. The procedures that the laboratory will use in meeting the quality control requirements of this subchapter, N.J.A.C. 7:18-3, and all applicable DSAMs, including, but not limited to, requirements pertaining to laboratory equipment, instrumentation and supplies; and

2. The frequency with which the laboratory will perform the procedures listed pursuant to (a)1 above.

(b) The laboratory shall develop and implement a written methods manual containing a standard operating procedure (SOP) for each DSAM, in accordance with the criteria and procedures of the DSAM and this chapter. A laboratory shall not perform analyses using a DSAM unless it has developed and implemented such an SOP for the DSAM.

1. The laboratory shall update the manual to reflect any changes in the procedures practiced by the laboratory.

2. The laboratory shall keep copies of the methods manual in the immediate bench area of personnel engaged in the analysis of samples and related procedures within the chemical testing Categories.

3. In the manual, the laboratory shall properly designate by revision number and date the standard operating procedure (SOP) for a specified analytical method for a particular type of analysis.

4. Changes to SOPs are effective only if:

i. The change is made by the manager, supervisor or quality assurance officer of the laboratory; and

ii. The manager, supervisor or quality assurance officer makes the change in writing, signed and dated by the manager, supervisor or quality assurance officer.

5. The laboratory shall make manufacturers' instruction manuals and any applicable regulations readily available to laboratory personnel at all times. Textbooks may be used to supplement written instructions, but shall not be used in lieu thereof.

(c) A laboratory performing chemical testing shall conduct the quality control checks specified in the applicable DSAMs, and the following additional checks:

1. The laboratory shall calibrate dissolved oxygen instruments against air or air saturated water before each use or weekly, whichever is less frequent. The laboratory shall test dissolved oxygen instruments weekly using the Winkler method (azide modification) 4500-OC set forth in SM-18 or ASTM method D88-92(A), or another Winkler method promulgated by the USEPA.

2. The laboratory shall calibrate standards incorporated in visual comparison devices at least once every six months. The laboratory shall maintain records of the date and method of each such calibration in accordance with 7:18-5.6. The laboratory shall prepare visual calibration standards according to the applicable DSAM. The laboratory shall plot concentrations of the calibration standards against those of the incorporated standards, and calculate a correction factor. The laboratory shall document this correction factor and apply it to all future results until the factor is redetermined at the next six-month interval;

3. The laboratory shall check the wavelength setting of each spectrophotometer at least annually, by comparing the wavelength setting to the absorption maxima of colored standards or filters such as didymium glass. For each check, the laboratory shall record in a log book the date on which it performed the check, the wavelength observed, and the correction factor. The record shall include the analyst's signature;

4. The laboratory shall prepare calibration curves used in the spectrophotometric analysis and ion-selective electrode analysis of inorganic parameters as follows:

i. When using new calibration standards or quarterly, the laboratory shall prepare new calibration curves consisting of at least one reagent blank and five standards. The calibration coefficient shall be [GREATER THAN] 0.995.

ii. The laboratory shall verify the calibration curve with the calibration check standard daily or after every 20 samples, whichever is more frequent. For analyses under the Drinking Water Program, the laboratory shall use a calibration check standard with a concentration at or near the maximum contaminant level (MCL). For analyses under other regulatory programs, the laboratory shall use a calibration check standard with a concentration at or near the middle of the concentration range of the calibration curve. If the applicable DSAM does not specify the permitted deviation, a verification is satisfactory only if the concentration as determined from the calibration curve is within a percent difference (PD) of 10 percent of the true concentration of the calibration check standard. If the PD is greater than 10 percent, the laboratory shall prepare a new calibration curve.

iii. The laboratory shall record all data used in determining the calibration curve, and have the record signed by the analyst. In the record, the laboratory shall include the date of calibration, identification and concentration standards;

5. The laboratory shall prepare calibration curves used in the analysis of metal parameters in Categories DW06, DW07, DW13, NPW07, NPW08, NPW16, SCM06, SCM07, SCM14, AE02, AE06, BT03, BT04, and BT08. When the laboratory uses computer-controlled equipment, the laboratory shall follow the requirements for calibration curves in (c)4 above, except that a minimum of one reagent blank and three standards shall be required, and the laboratory shall follow the manufacturer's instructions for calibrating the instrument and shall verify the calibration curve with two calibration check standards, one at the low end of the concentration range and the other at the high end;

6. The laboratory shall analyze blanks at the frequencies required by the applicable DSAM. For methods used in categories AE01, AE02, AE03, AE04, and AE06 that do not address method blank requirements, method blanks shall be performed at a frequency of at least one per batch of 20 environmental samples or less per sample preparation method, or at least once each day of instrument operation, whichever is more frequent. If the method blank result is greater than the detection limit and contributes greater than 10 percent of the total amount of analyte found in the sample, the source of contamination must be investigated and measures taken to eliminate the source of the contamination. If contamination is found, the data shall be qualified in the report;

7. For parameters in Categories DW03, DW05-DW07, DW13, NPW03, NPW05, NPW07-NPW08, NPW16, SCM03-SCM04, SCM06-SCM07, SCM14, AE01-AE04, AE06, BT01, BT03-BT04, and BT08, the laboratory shall conduct quality control (QC) check sample analyses to verify the accuracy of the analytical system for the parameter. For each QC check sample analysis, the laboratory shall record the results of the analysis, the date on which the verification analysis was performed, and the method of verification. The laboratory shall have the analyst who performed the analysis sign the record.

i. If the laboratory analyzes 20 or more samples in a calendar month, it shall analyze one QC sample for every 20 samples analyzed during the month. If the laboratory analyzes fewer than 20 samples in a calendar month, it shall analyze one QC sample during the month;

ii. The laboratory shall calculate the percent recovery (% R) for each parameter in the QC sample. The % R shall be within the limits listed in the applicable DSAM. If the applicable DSAM does not list such limits, the laboratory shall calculate such limits from its experimental data, using the procedure in (c)9 below. If the % R is not within three standard deviations of the limits, the laboratory shall re-analyze the samples in question; and

iii. For categories AE01-AE04 and AE06, if a spiking solution is not available, a calibration solution, whose concentration approximates that of the samples, shall be included in each batch and with each lot of media. If a calibration solution must be used for the QC sample, the client will be notified prior to the start of analysis. The concentration of the QC sample shall be relevant to the intended use of the data and either at a regulatory limit or below it.

8. In all cases, the laboratory shall conduct matrix spike and matrix spike duplicate sample analyses to verify the accuracy and precision of the DSAM for the applicable parameters in the Categories DW03, DW05-07, DW13, NPW03, NPW05, NPW07-NPW08, NPW16, SCM03-SCM04, SCM06-SCM07, SCM14, AE01-AE04, AE06, BT01, BT03-BT04, and BT08.

i. The laboratory shall verify the accuracy and precision of its analyses of parameters in the above categories. The laboratory shall maintain records of such verifications, signed by the analyst performing the verification. In the records, the laboratory shall include the date on which it performed the verification, the method of verification, and the results;

ii. If the laboratory analyzes 20 or more samples for any one parameter in a calendar month, it shall verify the accuracy and precision of such analyses on at least one of every 20 samples analyzed during the month. If the laboratory analyzes fewer than 20 samples for any one parameter in a calendar month, it shall verify the precision of the analysis once a month;

iii. The laboratory shall calculate the percent recovery (% R) for each matrix spike and the relative percent difference (RPD) between the matrix spike and matrix spike duplicate for each parameter. The % R and RPD shall meet requirements of the applicable DSAM. If the method does not list limits for % R and RPD values, the laboratory shall establish these limits from its experimental data, using the procedure in (c)9 below;

iv. For categories AE01-AE04, and AE06, matrix spikes and matrix spike duplicates are not required for those air samples that are introduced directly into an analytical instrument from SUMMA sampling canisters, sorbent tubes, or polyurethane foam (PUF) traps.

9. In all cases, the laboratory shall calculate and document standard deviations for all applicable measurements conducted in Categories DW03, DW05-07, DW13, NPW03, NPW05, NPW07-NPW08, NPW16, SCM03-SCM04, SCM06-SCM07, SCM14, AE01-AE04, AE06, BT01, BT03-BT04, and BT08, in accordance with the following requirements:

i. The laboratory shall calculate standard deviations for n-1 degrees of freedom (n samples - 1) for all % R and RPD measurements in (c)7 and 8 above. For this calculation in connection with (c)7 above, the laboratory shall use ongoing data collected from the analysis of 10 QC samples; for this calculation in connection with (c)8 above, the laboratory shall use ongoing data collected from the analysis of 10 matrix, matrix spike pairs. For parameters in Category DW03 and DW05-DW07, the laboratory shall use samples that have been prepared at the MCL. For other parameters, the laboratory shall use samples that have been prepared to approximate the middle of the concentration range normally encountered in the analysis. The laboratory shall record the theoretical or true value. The laboratory shall calculate and plot the mean value, the warning limits (two standard deviations), and the corrective action limits (three standard deviations); and

ii. The laboratory shall record subsequent quality control results for each parameter, and compare the results against its control limits. The control limits shall be updated after a batch of 20 new measurements.

10. A certified environmental laboratory or a laboratory that is applying for certification shall determine its own MDLs in reagent water. MDL data are required for all DSAMs containing reference MDL data for which the laboratory possesses or is applying for certification. The laboratory shall make the MDL determinations in accordance with 40 CFR 136 Appendix B. The Office of Quality Assurance may require the laboratory to determine MDLs for any DSAMs for which it possesses certification. This data is required to support Water Technical Programs N.J.A.C. 7:9-4 and 6:

i. For analyses in the Clean Air Program, the laboratory shall utilize a test method that provides a detection limit that is appropriate and relevant for the intended use of the data. Detection limits shall be determined by the protocol in the mandated test method or in accordance with 40 CFR Part 136, Appendix B. If the protocol for determining detection limits is not specified, the selection of the procedure shall reflect instrument limitations and the intended application of the test method. A detection limit study is not required for any component for which spiking solutions are not available. All procedures shall be documented. Documentation shall include the matrix type. All supporting data shall be retained. The laboratory shall have established procedures to tie detection limits with quantitation limits.

11. A certified environmental laboratory shall determine its MDL data (as stated in (c)10 above) annually. All regulatory sample data except CERCLA CLP shall include the most recent MDL values determined by the laboratory;

12. The laboratory shall maintain a permanent maintenance record containing the following information for each instrument:

i. The date of instrument installation;

ii. The date and a description of repairs, modifications, and preventive maintenance;

iii. The signature of the person performing the maintenance; and

iv. Chromatographic column information and installation date.

13. The laboratory shall maintain a bound notebook containing records of the preparation of standards. The laboratory shall include the following information in the records:

i. The manufacturer's name and lot number of reagent, date received, percent purity, name of chemical, concentrations if a solution;

ii. The identification number of the concentrated stock standard solution, date of preparation, expiration date, signature of the analyst who prepared the solution, all chemical compounds in the solution, purity, gross weight, tare weight, net weight, adjusted net weight (corrected for purity of primary standard) (only net weight and adjusted net weight are required when using balances with automatic tare features), dilution volume, and concentration in specified units;

iii. The identification number of the intermediate concentration standard solution (if needed), date of preparation, expiration date, signature of the analyst who prepared the solution, all chemical compounds in the solution, identification number of the concentrated stock, strength of concentrated stock, aliquot of concentrated stock, dilution volume, and final concentration in specified units; and

iv. The identification number of the working standard solution, date of preparation, expiration date, signature of the analyst who prepared the solution, all chemical compounds in the solution, identification number of the intermediate concentration standards, concentration of intermediate standards, aliquot volumes, dilution volumes, and final concentrations in specified units.

N.J. Admin. Code § 7:18-5.5

Amended by 47 N.J.R. 782(a), effective 4/20/2015.