Data Quality Organic Analyses

Data Quality Organic Analyses

OFFICIAL USE ONLY
U.S. Department of Energy Consolidated Audit Program
Data Quality Organic Analyses
/ DOECAP Audit Checklist: 2Rev. 4.3
Revision Date: March 2014Page 1 of 37
Audit ID: ______Laboratory: ______Auditor:______

U. S. Department of Energy

Consolidated Audit Program

Checklist 2

Data Quality for Organic Analyses

DoD/DOE QSM - Revision 4.3

October2015

Use of this DOECAP checklist is authorized only if the user has satisfied the copyright restrictions associated with TNI-EL-V1-2009 and ISO 17025:2005. DOECAP does not control or restrict the use of copyrighted standards that have been incorporated into this checklist; however, TNI and ISO do restrict use of their standards.

OFFICIAL USE ONLY
May be exempt from public release under the Freedom of Information Act
(5 U.S.C 552), exemption number and category: Exemption #4: Commercial Proprietary
Department of Energy review required before public release
Name/Org:Documents Originator/DOE Consolidated Audit Program

Date:TBD

Guidance (if applicable)Memo dated December 22, 2016 from Steve Clark to Beth Pearson, Pro2Serve

Audit ID: / Date:
Areas of Review During Audit
1.0 Standard Operating Procedures (SOPs) / 10.0 Carryover Minimization
2.0 Sample Preparation/Extraction / 11.0 Spike Recovery Requirements
3.0 Cleanup Methods / 12.0 Second-Column Confirmation
4.0 Initial and Continuing Calibration / 13.0 Method Performance
5.0 Standards and Reference Materials / 14.0 Analytical Worksheets
6.0 Method Proficiency / 15.0 Instrument Operation
7.0 Limit of Detection (LOD) and Limit of Quantitation (LOQ) / 16.0 Contamination Control
8.0 Precision and Accuracy / 17.0 Data Review
9.0 Instrument Run Logs
A=Acceptable / U=Unacceptable / NA=Not Applicable
F=Finding / NO=Not Observed / O=Observation
Referenced regulations are accessible at the following URLs:
NOTE:
  • When audit findings are written against site-specific documents (i.e., SOPs, QA Plans, licenses, permits, etc.), a copyof the pertinent requirement text from that document must be attached to this checklist for retention in DOECAP files.
  • Fully document any deviation from the LOI or the requirements of QSM Version 5.0, ISO 17025:2005, and TNI ELV1
  • For method specific quality control criteria, please refer to Appendix B of the DoD/DOE QSM
  • Refer to Page 39 for the record of revision.
  • For method specific quality control requirements, refer to QSM Rev. 5.0, Appendix A, Pages 77 – 109.

Item Number / Line of Inquiry / Status / Summary of Observations/Objective Evidence
Reviewed Audit Notes
1.0 / Standard Operating Procedures (SOPs)
1.1 / Does the laboratory have and maintain an in-house methods manual(s) for each accredited analyte or test method. The manual consists of copies of published or referenced test methods or SOPs that have been written by the laboratory. Each method contains:
  • identification of the test method;
  • applicable matrix or matrices;
  • detection limit;
  • scope and application, including components to be analyzed;
  • summary of the test method;
  • definitions;
  • interferences;
  • safety;
  • equipment and supplies;
  • reagents and standards;
  • sample collection, preservation, shipment, and storage;
  • QC;
  • calibration and standardization;
  • procedure;
  • calculations;
  • method performance;
  • pollution prevention;
  • data assessments and acceptance criteria for QC measures;
  • corrective actions for out-of-control data;
  • contingencies for handling out-of-control or unacceptable data;
  • waste management;
  • references; and
  • any tables, diagrams, flowcharts, and validation data.
QSM Rev. 5.0, Module 2, Section 4.2.8.5; TNI Standard, EL-V1-2009, Sections 4.2.8.5 a) through f)
1.2 / When utilized, are permanent,boundlaboratorynotebooks(logbooks)ornotebooks withmeasuresinplace to preventthe removaloradditionofpagesarerequired,ifutilized?
Electroniclogbooksareacceptable. For permanent, bound logbooks are thefollowingapplied:
a)Are laboratorynotebookpagespre-numbered,allentries are signedorinitialedanddatedbythepersonresponsibleforperforming the activityatthetimethe activity isperformed,andallentries are recordedinchronologicalorder?;
b)Are allnotebookpagesclosedwhen theactivitiesrecordedarecompletedorcarriedovertoanotherpage?
c)Istheperson responsible forperforming theclosurethe same person whoperformedthe lastactivity recorded?
d)Didclosureoccuratthe end ofthelastactivityrecordedonapage,assoonaspracticablethereafter?
e)Did documentation of the closureincludeanalystinitialsanddate?;and
f)Does eachlaboratorynotebookhave a uniqueserialnumber clearly displayed?
QSM Rev. 5.0, Module 2, Section 4.13.4
1.3 / Is a system in place to ensure that quality records are legible, accurate, and complete, e.g., independent review of records, logbooks, etc.?
ISO/IEC 17025 Clause 4.13.1.2
1.4 / Whenmistakes occur in records, are they crossed out with a single line, corrected, and initialed and dated?
Are allsuchalterationstorecordsinitialed bythepersonmakingthecorrection?
Inthecase of records stored electronically, are equivalentmeasurestakentoavoidlossorchangeoforiginaldata?
ISO/IEC 17025 Clause 4.13.2.3
2.0 / Sample Preparation/Extraction
2.1 / In order to minimize instrument contamination and downtime, does the laboratory employ a sample screening procedure prior to extraction and analysis?
EPA SW-846, Method 8000B, Section 3.2
2.2 / Does the laboratory have a documented procedure for the determination of extraction level?
EPA SW-846, Chapter One, Section 4.3.4
2.3 / Are glassware and containers designated as disposable or cleaned according to an SOP?
EPA SW-846, Chapter One, Section 4.3.3
2.4 / General Facility:
  • Is the laboratory clean and organized?
  • Is sample preparation performed on a clean tabletop?
  • Are hoods clutter free; and
  • Is workspace adequate?
EPA SW-846, Chapter One, Section 4.1
2.5 / Is check weighing performed daily using NIST-traceable weights?
Do the balance checks bracket the range of use?
Are daily balance checks documented?
QSM Rev. 5.0,Module 2, Section 5.5.13.1 Table and TNI 5.5.13.1 b)
2.6 / Are Class 1 (formerly referred to as Class S) certified check weights calibrated every five years using recognized National Metrology Institute, such as NIST, traceable references, when available?
NOTE: The date for recalibration of the check weights is stated on the certificate of calibration supplied by the accredited calibration firm.
Are all support equipment, including balances, calibrated or verified at least annually, using a recognized National Metrology Institute, such as NIST, traceable references when available, bracketing the range of use?
Does the laboratory maintain a copy of the Certificate of Calibration from an ISO/IEC accredited calibration laboratory?
QSM Rev. 5.0, Module 2, Section 5.5.13.1 Table and TNI EL-V1-2009, Section 5.5.13.1 b) and d)
2.7 / Prior to use, are balances checked on a daily basis using two standards weights that bracket the expected mass?
QSM Rev. 5.0, Module 2, Section 5.5.13.1 Table
2.8 / Are the acceptance criteria for a top-loading balance ±2% or ±0.02 grams whichever is greater?
Are the acceptance criteria for an analytical balance ±0.1% or ±0.5 mg. whichever is greater?
QSM Rev. 5.0, Module 2, Section 5.5.13.1 Table
2.9 / Are liquid in-glass thermometers calibrated against a NIST-traceable standard before the first use and annually?
Are electronic thermometerschecked before use and on a quarterly basis?
QSM Rev. 5.0, Module 2, Section 5.5.13.1 and TNI EL-V1-2009, Section 5.5.13.1 d)
2.10 / Are mechanical volumetric pipettes checked daily before use and is the bias within ± 2% of the nominal volume?
NOTE: For variable volume pipettes, the nominal value is the volume of use.
QSM Rev. 5.0, Module 2, Section 5.5.13.1 Table
2.11 / Are samples stored according to the conditions specified by the preservation protocol?
For samples that require thermal preservation stored under refrigeration that is ±2°C of the specified preservation temperature unless regulatory or method specific criteria exist?
NOTE: For samples with a specified storage temperature of 4°C, storage at a temperature above the freezing point of water to 6°C shall acceptable.
Note: EPA has recently promulgated temperature conditions of 0°Cto 6°C, with a footnote “above freezing” and the QSM Rev. 5.0, Section 5.5.13.1 f) Table also requires the same temperature ranges. The existing LOI can be used or the revision may be applied.
TNI-EL-V1M2, Section 5.8.9 a) and i)
2.12 / Are refrigerator temperatures are monitored daily and recorded in a logbook or via electronic media such as a data logger?
NOTE: Daily temperature monitoring of refrigerators and freezers is required for all samples that require temperature preservation. Daily monitoring for rad samples other than Tritium will not be required.
The requirement for daily monitoring for sample storage refrigerators and freezers will not apply in the event that samples are not being stored from a DOE site.
QSM Rev. 5.0, Module 2, Section 5.5.13.1 f)
2.13 / Does the laboratory have procedures for recording catastrophic failure of support equipment (e.g., refrigerators, freezers) and that addresses identification of affected samples and customer notification?
QSM Rev. 5.0, Module 2, Section 5.5.13.1
2.14 / Are refrigerator storage blanks present for the storage of all volatile organic samples and include the following:
  • Is a refrigerator storage blank present for the storage of all volatile organic samples?

  • Are specific procedures for assessing the adequacy of storage blank data and taking action for nonconforming conditions established?

  • When samples are stored in refrigerators, are associated storage blanks analyzed every 14 days?

  • Are the storage blanks stored in the same manner as the client samples?

  • Is the data from the analysis of the refrigerator storage blank available for review?
QSM Rev. 5.0, Module 2, Section 5.3.3 a) b) and c)
2.15 / Does the sample preparation documents indicate the following:
  • extraction procedure,
  • matrix,
  • identification number of standards and spikes added,
  • spike composition,
  • blanks,
  • volume/concentration of standards/spikes added,
  • name of analyst,
  • volume/weight of sample used,
  • final concentrated volume,
  • dilution information,
  • cleanup steps,
  • reagent log numbers,
  • start/stop dates/time for soxhlet and continuous liquid/liquid extraction, and
  • observations?
EPA SW-846, Chapter One, Sections 4.3.4, 4.3.10, and 4.6
2.16 / Do sample preparation practices assure homogenization so that a representative aliquot is obtained for analysis?
EPA SW-846, Method 3550 B, Section 7.1
2.17 / Sonication equipment is tuned prior to use to ensure optimum performance.
EPA SW-846, Method 3550B, Section 7.0
2.18 / For solids extraction using ultrasonic extraction are surrogate and spiking solutions added prior to solid prior to adding extraction solvent.
EPA SW-846, Method 3550, Section 7.3
2.19 / Does the Chain of Custody contain all signatures of all personnel that handled the sample(s)?
QSM Rev. 5.0, Module 2, Section 5.8.8 b)
3.0 / Cleanup Methods
3.1 / Does the laboratory maintain and follow SOPs for all cleanup methods performed at their facility including, but not limited to:
  • Gel-Permeation Chromatography (GPC),
  • florisil,
  • silica gel,
  • alumina, and
  • sulfur cleanup?
EPA SW-846, Chapter One, Section 4.3
3.2 / Is the laboratory’s selection of cleanup methods appropriate for the matrix of concern and for the potential interference?
EPA SW-846, Method 8000B, Section 3.4; EPA SW-846, Method 3600C, Sections 1.0 and 7.3
3.3 / When sample extracts are subjected to cleanup procedures, is the associated quality control samples (e.g. spikes, blanks, replicates, and duplicates processed through the same cleanup procedure?
EPA SW-846,Method 3600C, Section 8.3.2
3.4 / Is the GPC calibrated at least once per week during operation?
EPA SW-846, Method 3640A, Section 7.5
3.5 / When GPC is used, does the final sample concentration calculations account for the volume of sample lost in the dump of the instrument?
EPA SW-846, Method 3640A, Section 7.7
3.6 / Are instrument and maintenance logs maintained for the GPC?
TNI-ELV1M2, Section 5.5.5
3.7 / Are florisil lot checks performed to ensure adequate recovery of target analytes and adequate exclusion of interferences (e.g., trichlorophenol)?
EPA SW-846, Method 3620B, Section 8.0
3.8 / Are biological matrices cleaned using a method that effectively excludes fats and lipids (e.g., sulfuric acid and cleanup)?
EPA SW-846, Method 8290, Section 2.4
3.9 / Is sulfuric acid cleanup not used for analytes that are destroyed by acids (e.g., some pesticides and herbicides)?
EPA SW-846, Method 3665A, Section 1.1
4.0 / Initialand Continuing Calibration
4.1 / Are controlled procedures present at the workstation and do they that list requirements for instrument calibration and tuning?
ISO/IEC 17025:2005 Clause 5.4.1 (General Requirement), EPA SW-846, Chapter One, Section 4.3.5
4.2 / Is out-of-calibration equipment tagged or segregated and not used until it has been re-calibrated?
QSM Rev. 5.0, Section 5.5.13.1 f)
4.3 / Is equipment consistently found to be out-of-calibration repaired or replaced?
QSM Rev. 5.0, Module 2, Section 5.5.13.1 f)
4.4 / If a linear calibration is to be used:
  • doesthe relative standard deviation for calibration standard responses meet defined acceptance criteria or does the linear calibration least squares regression meet defined acceptance criteria, and
  • the curve is not forced through zero?
EPA SW-846, Method 8000B, Section 7.5
4.5 / Does the laboratory follow a documented procedure for the determination and verification of retention time windows for Gas Chromatography (GC) and High Performance Liquid Chromatography (HPLC) methods that do not employ internal standard calibration?
QSM Rev. 5.0, Module 2, Organic QC Tables, EPA SW-846, Method 8000B, Section 7.6
4.6 / For GC analysis, are retention time windows established for each analyte of concern and each column?
NOTE: In some cases pattern recognition can be used in lieu of retention time identification.
EPA SW-846, Method 8000B, Section 7.6.6
4.7 / Are retention time windows established so as to minimize false positive or false negative results?
EPA SW-846, Method 8000B, Section 7.6
4.8 / Are thedetailsoftheinitial and continuing instrumentcalibrationproceduresincludingcalculations,integrations,acceptancecriteriaandassociatedstatisticsincludedorreferencedinthemethodSOP and retained for the laboratory for review?
TNI-EL-V1M4, 2009, Section 1.7.1.1 a); Section 1.7.2 a)
4.9 / Are acceptance criteria defined and documented for all initial calibration andcontinuing calibration requirements?
TNI-EL-V1M4, 2009, Section 1.7.1.1 e); Section 1.7.2 e)
4.10 / If the initial calibration is not performed on the day of analysis, is the validity of the initial calibration verified by continuing calibration verification with each analytical batch?
TNI EL-V1M4-2009, Section 1.7.2
4.11 / Is instrumentcalibrationverificationperformed:
i.once after each instrument calibration (ICAL)
ii.after the analysis of a second source standard prior to sample analysis
QSM Rev. 5.0, Table 1 Organic Analysis by GC and Table 4 Organic Analysis by GC/MS
4.12 / Is the lowest calibration standard for the initial calibration at or below the limit of quantitation?
Are data reported below the LOQ reported using defined qualifiers?
TNI EL-V1M4-2009, Section 1.7.1.11 f)
4.13 / Is thehighestcalibrationstandardatorabovethehighestconcentrationforwhich quantitativedataaretobereported?
Is datareportedabovethecalibrationrangereportedusingdefined qualifiersorexplainedinthenarrative?
QSM Rev. 5.0, Module 4, Section 1.7.1.1.g)
4.14 / If the initial calibration data are outside established acceptance criteria are corrective actions performed and associated sample reanalyzed?
TNI-EL-V1M4-2009, Section 1.7.1.1i)
4.15 / If the continuing calibration verification (CCV) results are outside the established acceptance criteria and analysis of two additional consecutive (immediate) CCVs fails to produce results within acceptance criteria, are corrective actions performed?
NOTE: Immediately is defined as starting a consecutive pair within one hour; no samples can be analyzed between the failed CCV and the two additional CCVs.
QSM Rev. 5.0, Module 4, Section 1.7.2 i)
4.16 / Are initial calibrations verified with a standard obtained from a second manufacturer or from a different lot number?
QSM Rev. 5.0, Module 4, Section 1.7.1.1 d)
5.0 / Standards and Reference Material
5.1 / Does thelaboratoryensurethatpurchasedsuppliesandreagentsandconsumablematerialsthat affectthequality oftestsand/orcalibrationsarenotuseduntiltheyhavebeeninspectedorotherwiseverifiedascomplyingwithstandardspecifications orrequirements definedinthemethods forthetestsand/orcalibrationsconcerned?
Do the purchased supplies and reagents comply with specified requirements?
Are records ofactionstakentocheckcompliancemaintained?
ISO/IEC 17025, Clause 4.6.2
5.2 / Does the laboratory maintain documentation for reagents and solvents and are they checked to ensure that the stated purity meets the intended use?
Are records of purity checks filed in a manner that is retrievable?
QSM Rev, 5.0, Module 2, Section 5.6.4.2
5.3 / Do purchasingdocuments foritems affectingthequalityof laboratoryoutputcontain datadescribingservicesandsupplies?
Are thepurchasingdocumentsreviewedandapprovedfortechnicalcontentpriortorelease?
NOTE: The description may include type, class, precise identification, specifications, drawings, inspection instructions, and other technical data including approval of test results, the quality required and the management system standard under which they were made.
ISO/IEC 17025, Clause 4.6.3
5.4 / Do records for services and supplies that may affect the quality of environmental tests include the following, where applicable:
a) Date of receipt;
b) Expiration date;
c) Source;
d) Lot or serial number;
e) Calibration and verification records; and
f) Accreditation or certification scopes/certificates
QSM Rev. 5.0, Module 2, Section 4.6.1
5.5 / Are calibration standards assigned a unique identification number traceable to the original standards, lot number and an expiration date?
Are these numbers and dates placed on the standards container?
TNI EL-V1M2-2009, Section 5.6.4.2
5.6 / Are standards and reference materials traceable to NIST or other certified standards, including:
  • initial calibration standards,
  • continuing calibration standards,
  • spiking standards, and
  • surrogates.
TNI-EL-V1M2-2009 Section 5.6.3.2 / .
5.7 / Are calibration standards prepared using certified standards traceable to a nationally recognized or consensus source, and are the certificates of authenticity are kept on file?
TNI-EL-V1M2-2009 Section 5.6.3.2
5.8 / Do procedures exist for the storage of reagents and laboratory consumable materials?
TNI-EL-V1M2-2009, Section 4.6.1
5.9 / Do the procedures require organic standards be properly refrigerated and stored as required by the specific EPA method?
TNI-EL-V1M2-2009, Section 4.6.1
5.10 / Are the following calibration criteria met:
  • appropriate number, type and range of calibration standards are used as required by the EPA method;
  • for each analyte and surrogate of interest, initial calibration standards are prepared at a minimum of 5 different concentrations.
EPA SW-846, Method 8000B, Sections 7.4.1.1 and 7.4.1.4
6.0 /

Method Proficiency

6.1 / Has the laboratory performed and documented the results of a method validation study for each method.
TNI EL-V1M4-2009, Section 1.5.1a)
6.2 / Has the laboratory validated all non-reference methods or laboratory developed methods?
Are the results of the method validation documented and readily available for review?
TNI EL-V1M4-2009, Section 1.5.1b)
6.3 / Are samples that were initially diluted and had no identified compounds reanalyzed at a lower dilution, if required by client specific instructions?
QSM Rev. 5.0, Module 4, Section 1.7.1.1 g)
7.0 / Limit of Detection (LOD) and Limit of Quantitation (LOQ)
Note: If the laboratory is not reporting a value below the Limit of Quantitation, a Limit of Detection study is not required.
7.1 / Does the laboratory maintain procedures for determining limits of detection and the frequency of verification?
TNI-ELV1M4-2009, Section 1.5.2
7.2 / Does the laboratory document how LODs were derived from the method determinations?
TNI-ELV1M4-2009, Section 1.5.2.1
7.3 / Are all sample-processing and analysis steps of the analytical method included in the determination or validation of the LOD?
TNI-ELV1M4-2009, Section 1.5.2.1
7.4 / Is the validity of the LOD verified by detection (a value above zero) of the analyte(s) in QC sample in each quality system matrix and the does the QC sample contain the analyte at no more than 3 times the LOD for single analytes and 4 times the LOD for multiple analyte tests?
Top View