N.J. Admin. Code § Tit. 7, ch. 26E, app A
LABORATORY DATA DELIVERABLES FORMATS
I. Full Laboratory Data Deliverables are required for the following analytical data:
(a) Potable water data are to be submitted according to data deliverables listed in the version of the Professional Laboratory Analytical Services contract for potable water issued by the New Jersey Department of Treasury, Division of Purchase and Property in effect as of the date of sample analysis by the laboratory.
(b) Air (including sub-slab, indoor and ambient) analyzed by NJDEP Method LLTO-15 or USEPA Method TO-15.
Data are to be submitted according to the most recent update of the NJDEP-SRWM Low Level USEPA Method TO-15 (NJDEP-LL TO-15-3/2007 for Ambient Air, NJDEP Regulatory Data Report Format -- Appendix 1 March 2007) in effect as of the date of sample analysis by the laboratory with the following exceptions and additions:
1. Additional deliverables for NJDEP Method LLTO-15 or USEPA Method TO-15:
i. The terms "Laboratory Control Sample" and "Blank Spike" may be used in addition to "Reporting Limit Laboratory Control Sample";
ii. The paper copies contained in the extended data report (deliverable package) must not be reduced in size from its original format (Appendix 1, Section 2.4.6);
iii. The laboratory sample numbers must be in increasing sequential order with regards to laboratory identification (ID) number (Appendix 1, Section 4.2.8);
iv. In the sample data summary, the laboratory shall place sample packages in order of increasing sample number considering laboratory ID numbers (Appendix 1, Section 6.0);
v. The laboratory shall report all compounds detected other than those noted in Table 1 of Appendix 1 as Tentatively Identified Compounds (TICs) for all samples, blanks, and clean canister certification data (Appendix 1, Section 6.11);
vi. For TO-15 analyses only, the instrument run log for the continuing calibration shall start with the injection of the continuing calibration verification standard and end with the last sample analyzed within the 24 hour sequence (Appendix 1, Section 10.3); and
vii. For TO-15 analyses only, the laboratory control sample data.
2. For TO-15 analysis only, the following do not need to be included:
i. Initial Calibration Verification Sample Standard Summary (Appendix 1, Section 7.1.2);
ii. Initial Calibration Verification Sample Standard Form Summary and Raw Data (Appendix 1, Section 7.2);
iii. The Closing Continuing Calibration Verification analysis (Appendix 1, Section 7.3);
iv. Initial Calibration Verification Sample Standard Summary (Appendix 1, Section 9.1.6);
v. Standards Data-Initial Calibration Verification Sample Standard Summary and Closing Continuing Calibration Verification Summary (Appendix 1, Table 2); and
vi. Clean Canister Certification Data-Initial Calibration Verification Sample Standard Summary and Closing Continuing Calibration Verification Summary (Appendix 1, Table 2).
(c) Air (including sub-slab, indoor and ambient) analyzed by methods other than NJDEP Method LLTO-15 or USEPA Method TO-15.
Deliverables are to be those as defined in I.(b) above where appropriate based on method specific procedures.
(d) Polychlorinated dibenzo-p-dioxins/Polychlorinated dibenzofurans (PCDDs/PCDFs)
Data are to be submitted according to the data deliverables defined in Section 2 - Reporting Requirements and Deliverables for each of the following method specific USEPA Region 2 Standard Operating Procedures (SOPs), incorporated herein by reference (http://www.epa.gov/region02/qa/documents.htm):
1. USEPA Method 1613B Region 2 SOP HW-25 Revision 3;
2. USEPA SW-846 Method 8290 Region 2 SOP HW-19 Revision 1; and
3. USEPA SW-846 Method 8280 Region 2 SOP HW-11 Revision 2.
(e) Hexavalent Chromium
The following information shall be provided. If data are contained in a laboratory notebook, instrument print out and/or chromatogram, then a copy of the pertinent laboratory note book page, instrument print out and/or chromatogram is to be submitted.
1. Date of sampling;
2. Date of digestion;
3. Date of analysis;
4. Sample weight/volumes for all samples, initial calibration standards, calibration check standards, calibration blanks, preparation blanks/method blanks, pre-digestion (for soluble and insoluble) spike samples, post-digestion spike samples, duplicate analyses, and if performed, laboratory control samples;
5. pH of the sample digestate and standards, from both the preparative and analytical protocols;
6. Percent moisture log;
7. Digestion log (digestion temperature at 30 minutes and 60 minutes of at least one sample must be monitored and recorded) and color of digestates;
8. Absorbance readings for all samples, initial calibration standards, calibration check standards, calibration blanks, preparation blanks/method blanks, pre-digestion spike samples, post-digestion spike samples, duplicate analyses, and if performed, laboratory control samples;
9. Background readings for all samples, initial calibration standards, calibration check standards, calibration blanks, preparation blanks/method blanks, pre-digestion spike samples, post-digestion spike samples, duplicate analyses, and if performed, laboratory control samples;
10. All calibration curves (including a blank as one point of the curve) listing the concentration of the standards with their absorbance and the correlation coefficient calculated;
11. Calibration check standards results including the true values and the percent recoveries calculated;
12. Calibration blank results;
13. Preparation blank/method blank results;
14. If required, the pre-digestion spikes (for soluble and insoluble) analyses including the spike amount used and the spike recoveries;
15. Post-digestion spike analysis results including the spike amount used and the spike recoveries;
16. Duplicate analysis results including the relative percent difference;
17. Laboratory Control Sample (LCS) results including the true value and the calculated percent recovery;
18. Eh-pH graph from Method 3060A for all nonaqueous samples plotting the pH and Eh data for each sample with each sample clearly labeled on the graph; and
19. Final concentrations corrected for percent moisture.
(f) USEPA/CLP Analyses
Data deliverables are defined in each Statement of Work offered by the USEPA. (http://www.epa.gov/superfund/programs/clp/) As such, data are to be submitted according to the data deliverables listed in the Statements of Work used by the laboratory and in effect as of the date of sample analysis by the laboratory. Additionally, mass spectral negative proofs[LESS THAN]1[GREATER THAN] are required where applicable, "clean" soil method blanks[LESS THAN]2[GREATER THAN] for nonaqueous samples are not permitted, and laboratory internal chain of custody documentation is required.
1 A negative proof is a mass spectrum offered as evidence to support an analyst's decision to negate the presence of a contaminant which has been qualitatively identified and reported by the instrument's data system.
2 Method blanks for nonaqueous samples shall consist of performing the entire analytical procedure without any actual sample being present. The appropriate amount of sodium sulfate as specified in the current Statements of Work for Organics would be substituted as the "sample" for the semivolatile and pesticide/arochlor fractions.
(g) Extractable Petroleum Hydrocarbons
Data are to be submitted according to data deliverables listed in the Department's Extractable Petroleum Hydrocarbon Methodology, "Analysis of Extractable Petroleum Hydrocarbon Compounds (EPH) in Aqueous and Soil/Sediment/Sludge Matrices" in effect as of the date of sample analysis by the laboratory. (http://www.nj.gov/dep/srp/guidance/srra/eph_method.pdf)
(h) Methods other than (a) through (g) above:
In the absence of a method-defined data deliverable, the laboratory may use the applicable deliverables of a USEPA Statement of Work that is procedurally similar to the method employed.
II. Reduced Laboratory Data Deliverables
(a) General Requirements
1. The data deliverable package shall be bound and paginated with margins, bindings and of reproduction quality such that all pages are legible;
2. Title/Cover Page:
The format for quality assurance/quality control (QA/QC) documentation shall be simplified as much as possible for ease of review and reference. The report shall begin with a cover page that includes the laboratory certification number, if applicable, main laboratory phone number, signature of laboratory director, facility name, address and date of report preparation and date of sampling and receipt. The report shall include a summary table that cross-references the field ID number to the laboratory ID number for each sample;
3. Table of Contents;
4. Chain of Custody;
5. Methodology Review:
The Methodology Review shall list method numbers and revision, with a detailed discussion of any method modification;
6. Laboratory Chronicle:
The laboratory chronicle shall detail actual sample holding times and specify the sample condition upon receipt at the laboratory (including sample temperature and pH when pH adjustment is required);
7. Conformance/Non-Conformance Summary:
A conformance/non-conformance summary shall be completed and signed by the laboratory. This summary shall state that the laboratory has reviewed the QA/QC measures for sample analysis and has identified any deviations from the acceptable performance criteria or results.
(b) Gas chromatography/mass spectrometry (GC/MS) Requirements for each analytical fraction
1. Analytical Results Summary Form -- An analytical results summary form shall be submitted for each sample and for each GC/MS analytical fraction (i.e., volatiles and semi-volatiles). Each form shall contain the following information: date sample collected, date sample received, date sample extracted, date sample analyzed, sample weight/volume/units, sample ID numbers, sample delivery group (SDG), sample matrix, level, sample moisture content, dilution factor, GC column used, list of analytes, reporting limit, method detection limit, and detected analyte concentrations;
2. Tentatively Identified Compound (TIC) Summary - Each TIC shall be identified by compound name or class (if it can be determined) and Chemical Abstract Service (CAS) number along with its retention time and estimated concentration;
3. Tuning Results Summary Form - Tuning results for all initial and continuing calibrations that are associated with all samples shall contain the following information: laboratory file ID, instrument ID, injection date and time, the m/e (mass to ion charge) listing for the key ions, the reported ion relative abundance, the ion abundance criteria and a listing of all standards, blanks, QC samples and field samples (including date, lab file ID and time of analysis) associated with the tune;
4. Method Blank Results Summary Form - An analytical results form shall be submitted for all method blanks associated with all field samples for all analytical fractions. Each form shall contain the information listed in Section II (b) 1 above, as well as a listing of all field and QC samples associated with each method blank. In addition, a separate form for TICs shall be submitted which contains the information listed in Section II(b)2 above;
5. Calibration Summary - A summary of all initial and continuing calibrations that are associated with all samples and blanks shall be submitted for each GC/MS analytical fraction. The following information shall be provided for each initial calibration: instrument ID, calibration date and time, listing of standard concentrations used, laboratory file ID for each calibration standard, listing of all associated field samples, QC samples and blanks, retention times for each target analyte and surrogate compound, listing of the relative response factor (RRF) for each target analyte and surrogate compound, the average RRF for each target analyte and surrogate compound, and percent relative standard deviation for each target analyte and surrogate compound. The following information shall be provided for each continuing calibration: instrument ID, calibration date and time, date and time of the associated initial calibration, the standard concentration used, the laboratory file ID for the calibration standard, listing of all associated field samples, QC samples and blanks, retention times for each target analyte and surrogate compound, the average RRF for each target analyte and surrogate compound from the associated initial calibration, the RRF for each target analyte and surrogate compound from the continuing calibration and the percent difference for each target analyte and surrogate compound;
6. Surrogate Compound Recovery Results Summary - If required by the analytical method, a summary form shall be submitted which contains the following information for all field samples, method blanks and QC samples for each GC/MS analytical fraction: sample ID number, sample matrix, surrogate compound names, concentration of surrogate compounds used, surrogate compound recoveries and QC limits for each surrogate compound;
7. Matrix Spike/Matrix Spike Duplicate Results Summary - If required by the analytical method, a summary form shall be submitted for each sample matrix and each GC/MS analytical fraction which contains the following: sample ID number for the sample selected for spiking, list of compounds being spiked, concentration of each spiked compound, matrix spike concentration, matrix spike percent recovery, matrix spike duplicate concentration, matrix spike duplicate percent recovery, relative percent difference and QC limits for percent recovery and relative percent difference;
8. Internal Standard Summary - A summary form shall be submitted which contains the following information for all standards, field samples, method blanks and QC samples for each analytical fraction: sample ID number, ID of laboratory calibration standard, internal standard compound names, concentration of internal standards compounds, retention times of each internal standard, area of each internal standard, and QC criteria (where applicable) for internal standard areas and retention times;
9. Chromatograms -- The total ion chromatograms for all field samples and method blanks shall be submitted. All peaks on the chromatograms shall be identified as either an internal standard, surrogate compound, target compound or non-target compound. All peaks on a chromatogram shall also be associated with retention times, either directly on the chromatogram or identified and cross-referenced in tabular form;
10. Laboratory Control Sample Results Summary -- When specified by the analytical method, the results of the laboratory control sample (LCS) shall be submitted. The following information shall be reported: laboratory SDG number, control sample matrix, list of all target analytes, the true concentration for each analyte in the control sample, the reported concentration for each target analyte in the control sample, the percent recovery for each target analyte and the QC limit for percent recovery for each target analyte.
(c) GC Requirements
1. Analytical Results Summary - An analytical results form shall be submitted for each sample. Each form shall contain the information contained in Section II(b)1 above;
2. Method Blank Results Summary - An analytical results form shall be submitted for all method blanks as well as a listing of all field and QC samples associated with each method blank. Each form shall contain the information contained in Section II(b)4 above;
3. Standards Summary - A summary form containing GC standards information for all associated samples shall be submitted for both primary and confirmation (if applicable) analyses. This summary shall contain the following information: instrument ID number, GC column used and notation if primary or confirmation analysis, date and time of standard(s) analysis, listing of all associated field, QC and method blank samples, listing of target compounds, retention time windows of each target compound and calibration factor for each target compound;
4. Surrogate Compound Recovery Results Summary - If required by the analytical method, a summary form shall be submitted which contains the following information for all field samples, method blanks, and QC samples: sample ID number, sample matrix, surrogate compound names, concentration of surrogate compounds used, surrogate compound recoveries and QC limits for each surrogate compound;
5. Matrix Spike/Matrix Spike Duplicate Results Summary - If required by the analytical method, a summary form shall be submitted for each sample matrix which contains the information contained in Section II(b)7 above;
6. Retention Time Shift Summary - If required by the analytical method, a summary form containing retention time shift results shall be submitted for both the primary and confirmation (if applicable) analyses. The form shall contain the following information: instrument ID number, GC column used and notation if primary or confirmation column analysis, name of retention time shift marker compound, list of all field samples, method blanks and QC samples, date and time of analysis of all field samples, method blanks and QC samples, percent difference of the retention time shift and QC limits for the retention time shift;
7. Chromatograms -- The primary analysis chromatograms and confirmation analysis chromatogram (when applicable) for all field samples and method blanks shall be submitted. All peaks on the chromatogram attributable to target and surrogate compounds shall be identified as such along with the retention time for each peak. The reference standard chromatogram for all multi-peak target compounds (e.g., toxaphene, PCBs) for both the primary and the confirmation analysis (when applicable) shall also be submitted;
8. Laboratory Control Sample Results Summary -- When specified by the analytical method, the results of the laboratory control sample (LCS) shall be submitted. The following information shall be reported: laboratory SDG number, control sample matrix, list of all target analytes, the true concentration for each analyte in the control sample, the reported concentration for each target analyte in the control sample, the percent recovery for each target analyte and the QC limit for percent recovery for each target analyte.
(d) Metals Requirements
1. Analytical Results Summary -- An analytical results form shall be submitted for each sample. Each form shall contain the following information: sample ID number (laboratory and/or field ID), laboratory SDG number, sample matrix, date sample collected, date sample received, date sample analyzed, sample moisture content, dilution factor (if any), list of target analytes, detected analyte concentrations, reporting limits, and method detection limits;
2. Blank Results Summary -- A blank results form shall be submitted for all instrument calibration blanks and reagent blanks associated with all field and QC samples. Each form shall contain the following information: a list of all target analytes, matrix of the reagent blank, concentration units of the reagent blank, reported concentration of all target analytes found in all calibration and reagent blanks, reporting limits, and method detection limits;
3. Calibration Summary -- A calibration summary shall be submitted for all initial calibration standards and continuing calibration standards associated with field samples, blanks and QC samples. Each form shall contain the following information: laboratory SDG number, initial and continuing calibration source, list of all target analytes, the true concentration for the initial and continuing calibration standards, the reported (or found) concentrations for the initial calibration standards and continuing calibration standards, the percent recovery for each initial calibration standard and continuing calibration standard and the percent recovery QC limits for each target analyte. In addition, this form shall also list the reporting limit, method detection limit, and instrument detection limit for each target analyte;
4. ICP Interference Check Sample Results Summary - If metals analysis is being conducted by ICP methodology, results of the interference check samples analysis shall be reported. The following information shall be reported: laboratory SDG number, interference check sample source, instrument ID number, list of all target analytes in the interference check sample, the true concentration of analytes in the interference check sample, the reported concentrations of analytes found in the interference check sample for both the initial and final check samples analyses, the percent recovery of the target analytes found in the initial and final check samples analyses and the QC control limits for percent recovery values;
5. Spike Sample Results Summary - A summary of the spike sample analysis shall be submitted. The following information shall be reported: laboratory SDG number, ID number of the sample chosen for spiking, sample matrix, percent solids, the concentration of each spiked target analyte, the results of the unspiked sample analysis, the results of the spiked sample analysis, the percent recovery for each spiked analyte and the QC limit for percent recovery for each spiked analyte;
6. Duplicate Sample Results Summary - A summary of the duplicate sample analysis shall be submitted. The following information shall be reported: laboratory SDG number, ID number of the original sample and the duplicate samples, sample matrix, percent solids, results of the original sample analysis, results of the duplicate sample analysis, the relative percent difference of each target analyte for the original duplicate sample analyses and the QC limit for relative percent difference for each target analyte;
7. Laboratory Control Sample Results Summary - When specified by the analytical method, the results of the laboratory control (quality control) sample shall be submitted. The following information shall be reported: laboratory SDG number, control sample matrix, list of all target analytes, the true concentration for each analyte in the control sample, the reported concentration for each target analyte in the control sample, the percent recovery for each target analyte and the QC limit for percent recovery for each target analyte;
8. Serial Dilution Summary - If required by the analytical method, a summary of the serial dilution results shall be submitted. The following information shall be reported: laboratory SDG number, ID number of the original sample and the serial dilution sample, sample matrix, results of the original sample analysis, results of the serial dilution sample analysis, the percent difference of each target analyte compared to the original target analyte results and the QC limit for percent difference for each target analyte;
9. Internal Standard Summary - A summary form shall be submitted for each ICP/MS analytical run which contains the following information: laboratory SDG number, date analyzed, method reference, sample ID number, ID of laboratory calibration standard, calibration and method blanks ID, QC sample ID, internal standard compound names, percent recoveries of internal standard compounds, and QC criteria for internal standard areas;
10. Analysis Run Log - The following information shall be reported: laboratory SDG number, instrument ID number, date and time of sample analysis, any dilution factors used, the analytical run sequence of all samples, standards and blanks and the list of all target analytes;
11. Digestion Log - The following information shall be reported: date of sample digestion, laboratory SDG number, batch number, matrix, sample numbers, initial weight/volume, final volume and digestion method.
(e) General Chemistry Requirements
1. Analytical Results Summary -- An analytical results form shall be submitted for each sample. Each form shall contain the following information: sample ID number (laboratory and/or field ID), sample matrix, date sample collected, date sample received, date sample analyzed, sample moisture content, dilution factor (if any), list of target analytes and detected analyte concentrations, reporting limits, and method detection limits;
2. Calibration Summary - A calibration summary shall be submitted for all initial calibration standards and check standards associated with field samples, blanks and QC samples. Each form shall contain the following information: list of all target analytes, the true concentration for the initial calibration standards and check standards, the reported (or found) concentrations for the initial calibration standards and check standards, the percent recovery for each initial calibration standard and check standard and the percent recovery QC limits for each target analyte;
3. Blank Results Summary - A blank results form shall be submitted for all method blank samples associated with all field and QC samples. Each form shall contain the following information: list of all target analytes, matrix of the method blank, concentration units of the method blank, reported concentration of all target analytes found in all method blanks;
4. Spike Sample Results Summary - A summary of the spike sample analysis shall be submitted. The following information shall be reported: ID number of the sample chosen for spiking, sample matrix, the concentration of each spiked target analyte, the results of the unspiked sample analysis, the results of the spiked sample analysis, the percent recovery for each spiked analyte and the QC limit for percent recovery for each spiked analyte;
5. Duplicate Sample Results Summary - A summary of the duplicate sample analysis shall be submitted. The following information shall be reported: ID number of the original sample and the duplicate sample, sample matrix, results of the original sample analysis, results of the duplicate sample analysis, the relative percent difference of each target analyte for the original duplicate sample analyses and the QC limit for relative percent difference for each target analyte;
6. Laboratory Control Sample Results Summary / Quality Control Check Standard Summary - When specified by the analytical method, the results of the laboratory control (quality control check) sample shall be submitted. The following information shall be reported: control sample matrix, list of all target analytes, the true concentration for each analyte in the control sample, the reported concentration for each target analyte in the control sample, the percent recovery for each target analyte and the QC limit for percent recovery for each target analyte.
N.J. Admin. Code Tit. 7, ch. 26E, app A