OFFICIAL USE ONLY

U. S. Department of Energy

Consolidated Audit Program

Checklist 3

Data Quality for Inorganic Analyses

DoD/DOE QSM5.0- Revision 6.5

January 2017

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:

OFFICIAL USE ONLY

OFFICIAL USE ONLY

U.S. Department of Energy Consolidated Audit Program
Data Quality for Inorganic Analyses
/ DOECAP Audit Checklist: 3 Rev. 6.5
Revision Date: January 2017 Page 1 of 79
Audit ID: ______Laboratory: ______Auditor:
Areas of Review during Audit
1.0 Standard Operating Procedures (SOPs) / 2.0 Balances
3.0 Thermometers and Pipettes / 4.0 Other Support Equipment (Ovens, Water Baths, Incubators)
5.0 Metals Digestion / 6.0 Limit of Detection (LOD) / Limit of Quantitation (LOQ)
7.0 Instrument Operations and Maintenance / 8.0 Standards and Reference Material
9.0 Negative and Positive Controls / 10.0 Multipoint Calibration Procedures – AAS
11.0 Inductively Coupled Plasma Mass Spectrometry (ICP/MS) / 12.0 Multipoint Calibration Procedures – ICP-OES
13.0 Multipoint Calibration Procedures – CVAA / 14.0 Quality Control (QC) of Instrument Gases
15.0 Wet Chemistry Procedures – Cyanide Distillation / 16.0 Reactivity Determinations – Colorimetric Cyanide
17.0 Reactivity Determinations – Titrimetric Sulfide / 18.0 Toxicity Characteristic Leaching Procedure (TCLP) Extractions
19.0 Ignitability Tests / 20.0 Corrosivity Determination
21.0 Corrosivity Towards Steel / 22.0 Total Organic Carbon (TOC)
23.0 Total Organic Halogens (TOX) / 24.0 Biological Oxygen Demand (BOD) Determinations
25.0 Chemical Oxygen Demand (COD) Determinations / 26.0 Total Phosphorous,Nitrate/Nitrite, &Anions Determination
27.0 Kinetic phosphorescence Analysis / 28.0 Colorimetric Hexavalent Chromium
29.0 Sample Dilution / 30.0 Data Review
A = Acceptable
NO = Not Observed / U = Unsatisfactory
F = Finding / NA = Not Applicable
O = Observation

Areas of Review during Audit

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 QSM Rev. 5.0, Appendix A, Pages 110 - 138
  • Refer to Page 69for the record of revision.
  • Refer to Errata Document Revision 11-30-16, Revision 3 for interim changes to the QSM Rev.5.0 requirements

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?
QSM Rev. 5.0, Module 2, Section 4.2.8.5; TNI EL-V1M2-2009, Sections 4.2.8.5 e)
1.2 / Does each method contain:
  • 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;
  • 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, Method 2, Section 4.2.8.5; TNI EL-V1M2-2009, Sections 4.2.8.5 f)
1.3 / Does the manual consist of copies of published or referenced test methods or SOPs that have been written by the laboratory?
QSM Rev. 5.0, Module 2, Section 4.2.8.5; TNI EL-V1M2-2009, Sections 4.2.8.5 f)
1.4 / Are permanent,boundlaboratorynotebooks(logbooks)ornotebooksused that have measuresinplace to preventthe removaloradditionofpages?
QSM Rev. 5.0, Module 2, Section 4.13.4
a)Are allnotebookpagesclosedwhen theactivitiesrecordedarecompletedorcarriedovertoanotherpage?
b)Does theperson responsible forperforming theclosureis the person whoperformedthe lastactivity recorded?
c)DidClosureoccuratthe end ofthelastactivityrecordedonapage,assoonaspracticablethereafter?
d)Did documentation of the closureincludeanalystinitialsanddate?;and
e)Does eachlaboratorynotebookhave a uniqueserialnumber clearly displayed?
f)Are laboratorynotebookpagespre-numbered?
g)Areallentries are signedorinitialedanddatedbythepersonresponsibleforperforming the activityatthetimethe activity isperformed?
h)Areallentries are recordedinchronologicalorder?
QSM Rev. 5.0, Method 2, Section 4.13.4 a) – c)
1.5 / Is a system in place to ensure that quality records are legible, stored, and retained in such a way that they are readily retrievable in facilities that provide a suitable environment to prevent damage or deterioration and to prevent loss?
ISO/IEC 17025 Clause 4.13.1.2
1.6 / Is there an independent review of records, logbooks, and similar documentation to ensure they are legible, accurate, and complete?
QSM Rev.5, Module 2, Section 4.13.5
1.7 / Whenmistakes occur in records, is eachmistakecrossed out, noterased,made illegibleor deleted,and thecorrect valueenteredalongside?
ISO/IEC 17025 Clause 4.13.2.3
1.8 / Are allsuchalterations torecords are signedor initialed bythepersonmakingthecorrection?
ISO/IEC 17025 Clause 4.13.2.3
1.9 / Inthecase of records stored electronically, are equivalentmeasurestakentoavoidlossorchangeoforiginaldata?
ISO/IEC 17025 Clause 4.13.2.3
2.0 / Balances
2.1 / Is a check of the balanceperformed daily?
QSM Rev. 5.0, Module 2,Section 5.5.13.1 Table and TNI EL-V1M2-Section 5.5.13.1 d)
2.2 / Do the balance checks bracket the range of use?
QSM Rev. 5.0, Module 2, Section 5.5.13.1 Table
2.3 / Are daily balance checks documented?
QSM Rev. 5.0,Module 2, Section 5.5.13.1 Table and TNI EL-V1M2 Section 5.5.13.1 d)
2.4 / 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.
QSM Rev. 5.0, Module 2, Section 5.5.13.1 and TNI EL-V1M2-2009, Section 5.5.13.1 b)
2.5 / 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?
QSM Rev. 5.0, Module 2, Section 5.5.13.1 and TNI EL-V1M2-2009, Section 5.5.13.1 b)
2.6 / 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 f)
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 Tableand TNI EL-V1M2-2009, Section 5.5.13.1 d)
2.8 / Are the acceptance criteria for a top-loading balance ±2% or ±0.02 grams whichever is greater?
QSM Rev. 5.0, Module 2, Section 5.5.13.1 Table
2.9 / 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
3.0 / Thermometers and Pipettes
3.1 / Are liquid in-glass thermometers are calibrated against a NIST-traceable standard before the first use and annually?
QSM Rev. 5.0, Module 2, Section 5.5.13.1 Table and TNI EL-V1M2-2009, Section 5.5.13.1 b)
3.2 / For electronic thermometers, are the checked before use and on a quarterly basis?
QSM Rev. 5.0, Module 2, Section 5.5.13.1 Table
3.3 / 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
Item
Number / Line of Inquiry / Status / Summary of Observations/Objectives Evidence
Reviewed Audit Notes
4.0 Other support equipment – Ovens, Water Baths, and Incubators
4.1 / Is support equipment maintained in proper working order and are records of all repairand maintenance activities, including service calls, maintained?
TNI EL-V1M2-2009, Section 5.5.13.1 a)
4.2 / Is the support equipment calibrated or verified at least annually, using a recognized National Metrology Institute, such as NIST, traceable references when available, bracketing the range of use?
TNI EL-V1M2-2009, Section 5.5.13.1 b)
4.3 / In the event that the results of such calibration or verification are not within thespecifications required of the application for which the equipment is used, does the laboratory?
i)remove the equipment from service until repaired, and/or
ii)Maintain records of established correction factors to correct all measurements
TNI EL-V1M2-2009, Section 5.5.13.1 b)
4.4 / Are raw data retained to document equipment performance?
TNI EL-V1M2-2009, Section 5.5.13.1 c)
4.5 / On each day the equipment is used, is the equipment checked and documented?
TNI EL-V1M2-2009, Section 5.5.13.1 d)
4.6 / Does the laboratory have established criteria for acceptability for use or continued use of supporting equipment based on the needs of the analysis or application for which the equipment is being used?
TNI EL-V1M2-2009, Section 5.5.13.1 d)
Item
Number / Line of Inquiry / Status / Summary of Observations/Objective Evidence
Reviewed Audit Notes
5.0 / Metals Digestion
5.1 / On each day that metals digestation equipment (hotplate, hot block, water baths, etc.) is the temperature checked and documented?
TNI EL-V1M2-2009 Section 5.5.13.1 d)
5.2 / Does the laboratory have established criteria for acceptability for use or continued use based on the referenced methods temperature range specification?
TNI EL-V1M2-2009 Section 5.5.13.1 d)
5.3 / Does the laboratory use water meeting ASTM performance specifications (“TypeII” water or equivalent) for digestion procedures? (ASTM D1193).
EPASW-846, Chapter One, Section 5.0, Definitions – Reagent Water
5.4 / Does the laboratory use reagent or when necessary, ultra-high purity-grade acid for digestion procedures?
EPA SW-846, Method 6010 C and D, Section 7.1
Item
Number / Line of Inquiry / Status / Summary of Observations/Objective Evidence
Reviewed Audit Notes
6.0 / 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. (TNI EL-V1M4-2009m Section 1.5.2.1)
6.1 / Does the laboratory maintain procedures for determining limits of detection and the frequency of verification?
TNIEL-V1M4-2009, Section 1.5.2
6.2 / Does the laboratory document how LODs were derived from the method determinations?
TNIELV1M4-2009, Section 1.5.2.1
6.3 / Are all sample-processing and analysis steps of the analytical method included in the determination or validation of the LOD?
TNIELV1M4-2009, Section 1.5.2.1
6.4 / Is the validity of the LOD verified by detection (a value above zero) of the analyte(s) in QC sample in each matrix?
TNIELV1M4-2009, Section 1.5.2.1 b)
6.5 / 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?
TNIELV1M4-2009, Section 1.5.2.1 b)
6.6 / Has the laboratory performed a LOD on every instrument this to be used for analysis of samples and reporting of data?
TNIELV1M4-2009, Section 1.5.2.1 b)
Item
Number / Line of Inquiry / Status / Summary of Observations/Objective Evidence
Reviewed Audit Notes
6.7 / Is the validity of the LOD verified as part of the LOD determination process?
TNI ELV1M4-2009, Section 1.5.2.1 b)
NOTE: A LOD study is not required for any component for which spiking solutions or quality control samples are not available such as temperature.
TNI ELV1M4-2009, Section 1.5.2.1 c)
6.8 / Is the verification of the LOD completed prior to the use of the LOD for sample analysis?
TNIELV1M4-2009, Section 1.5.2.1 b)
6.9 / Are LODs verified annually for each quality system matrix, technology, and analyte?
TNIELV1M4-2009, Section 1.5.2.1 f)
6.10 / Are all sample-processing and analysis steps of each applicable analytical method included in the determination of the limit of quantitation (LOQ)?
TNIELV1M4-2009, Section 1.5.2.2 a)
6.11 / Is the validity of the LOQ verified by successful analysis of a QC sample containing the analytes of concern in each matrix at 1 to 2 times the claimed LOQ?
TNIELV1M4-2009, Section 1.5.2.2 c)
6.12 / Is the criteria for analysis of the LOQ based on the recovery of each analyte within the laboratory established method acceptance criteria or client data quality objectives for accuracy?
TNIELV1M4-2009, Section 1.5.2.2 c)
6.13 / Is the LOQ above the LOD, if the LOD is determined by the laboratory (See Note below LOI 7.0)?
TNIELV1M4-2009, Section 1.5.2.2 d)
6.14 / Is the LOQ verified annually for each quality system matrix, technology, and analyte?
NOTE: The annual LOQ verification is not required if the LOD was determined or verified annually on that instrument.
TNIELV1M4-2009, Section 1.5.2.2 e)
6.15 / Has the laboratory evaluated the precision and bias of a reference method for each analyte of concern for each matrix or alternate documented procedure when the analyte cannot be spiked into the sample matrix and where QC samples are not commercially available?
TNIELV1M4-2009, Section 1.5.3 a)
6.16 / For laboratory-developed methods or non-reference methods that were not in use by the laboratory before July 2003, has the laboratory developed and documented a procedure to evaluate precision and bias?
TNIELV1M4-2009, Section 1.5.3 b)
6.17 / Has the laboratory also compared results of the precision and bias measurements with criteria established by the client, by criteria given in the reference method or criteria established by the laboratory?
TNIELV1M4-2009, Section 1.5.3 b)
6.18 / Do precision and bias measurements evaluate the method across the analytical calibration range of the method?
TNIELV1M4-2009, Section 1.5.3 b)
6.19 / Has the laboratory also evaluated precision and bias in the relevant matrices and processed the samples through the entire measurement system for each analyte of interest?
TNIELV1M4-2009, Section 1.5.3 b)
Item
Number / Line of Inquiry / Status / Summary of Observations/Objectives Evidence
Reviewed Audit Notes
7.0 / Instrument Operations and Maintenance
7.1 / Are controlled procedures readily available that list requirements for instrument calibration?
ISO/IEC 17025:2005 Clause 5.4.1 (General Requirement)
EPA SW-846, Chapter One, Section 4.3.5
7.2 / Is equipment consistently found to be out-of-calibration isolated to prevent its use and clearly labeled or marked as being out of service until it has been repaired and shown by calibration or test to perform correctly?
ISO/IEC 17025:2005 Clause 5.5.7
7.3 / Are calibration results maintained as permanent laboratory records?
TNI EL-V1M2-2009, Section 5.5.13.1 c) and ISO/IEC 17025:2005, Clause 4.13.2.1
7.4 / Do calibration results contain sufficient information to allow monitoring of instrument performance over time?
TNI EL-V1M2-2009, Section 5.5.13.1 c) and ISO/IEC 17025:2005, Clause 4.13.2.1
7.5 / Are thedetailsoftheinitial and continuing instrumentcalibrationproceduresincludingcalculations,integrations,acceptancecriteriaandassociatedstatisticsincludedorreferencedinthemethodSOP and retained for the laboratory for review?
TNIEL-V1M4, 2009, Section 1.7.1.1 a); Section 1.7.2 a)
7.6 / Are acceptance criteria defined and documented for all initial calibration and continuing calibration requirements?
TNIEL-V1M4, 2009, Section 1.7.1.1 e); Section 1.7.2 e)
7.7 / 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
7.8 / Is instrumentcalibrationverification performed:
i.atthebeginningandendofeachanalyticalbatch.
ii.ifthetimeperiodforcalibrationorthemostrecentcalibrationverificationhasexpired;or
iii.foranalyticalsystemsthatcontainacalibrationverificationrequirement?
TNI EL-V1M4-2009, Section 1.7.2 c)
7.0 / Is the lowest calibration standard for the initial calibration at or below the limit of quantitation?
TNI EL-V1M4-2009, Section 1.7.1.1 f)
7.10 / Are data reported below the LOQ reported using defined qualifiers?
TNI EL-V1M4-2009, Section 1.7.1.1 f)
7.11 / Is thehighestcalibrationstandardatorabovethehighestconcentrationforwhich quantitativedataaretobereported?
(TNIEL-V1M4-2009, Section 1.7.1.1.g)
7.12 / Aredatareportedabovethecalibrationrangereportedusingdefined qualifiersandexplainedinthenarrative?
(TNIEL-V1M4-2009, Section 1.7.1.1.g)
7.13 / If the initial calibration data are outside established acceptance criteria are corrective actions performed and associated sample reanalyzed?
TNIEL-V1M4-2009, Section 1.7.1.1 i)
7.14 / If the continuing calibration verification results are outside the established acceptance criteria and analysis of second consecutive (immediate) calibration fails to produce results within acceptance criteria, are corrective actions performed?
TNIEL-V1M4-2009, Section 1.7.2 e)
7.15 / Are initial calibrations verified with a standard obtained from a second manufacturer or from a different lot number?
TNIEL-V1M4-2009, Section 1.7.1.1 d)
7.16 / Is traceability to a national standard documented, whencommercially available?
TNIEL-V1M4-2009, Section 1.7.1.1 d)
7.17 / Are dataassociatedwithanunacceptablecalibrationverificationreportedunder the following considerations:
i.Whentheacceptancecriteriaforthecontinuingcalibrationverificationareexceededhigh(i.e.,highbias)andthereareassociatedsamplesthatarenon-detects, thenthosenon-detectsmaybereported. Otherwisethesamplesaffectedbytheunacceptablecalibrationverificationshall bere-analyzedafteranewcalibrationcurvehasbeenestablished,evaluatedandaccepted;or
ii.Whentheacceptancecriteriaforthecontinuingcalibrationverificationareexceededlow(i.e.,lowbias), thosesampleresultsmaybereportediftheyexceedamaximumregulatorylimit/decisionlevel. Otherwisethesamplesaffectedbytheunacceptableverificationshall bere-analyzedafteranewcalibrationcurvehasbeenestablished,evaluatedandaccepted.
TNI EL-V1M4-2009, Section 1.7.2 e)
8.0 / Standards and Reference Material
8.1 / Does thelaboratoryensurethatpurchasedsuppliesandreagentsandconsumablematerialsthat affectthequality oftestsand/orcalibrationsarenotuseduntiltheyhavebeeninspectedorotherwiseverifiedascomplyingwithstandardspecifications orrequirements definedinthemethods forthetestsand/orcalibrationsconcerned?
ISO/IEC 17025, Clause 4.6.2
8.2 / Are records ofactionstakentocheckcompliancemaintained?
ISO/IEC 17025, Clause 4.6.2
8.3 / Does the laboratory maintain documentation for reagents and solvents?
QSM Rev, 5.0, Section 5.6.4.2
8.4 / Are reagents and solvents checked to ensure that the stated purity meets the intended use?
QSM Rev, 5.0, Section 5.6.4.2
8.5 / Are supporting records of the reagents and solvent checks filed so that they are retrievable??
QSM Rev, 5.0, Section 5.6.4.2
8.6 / Do purchasingdocuments foritems affectingthequalityof laboratoryoutputcontain datadescribingtheservicesandsuppliesordered?
ISO/IEC 17025, Clause 4.6.3
8.7 / Are purchasingdocumentsfor items affecting the quality of laboratory outputreviewedandapprovedfortechnicalcontentpriortorelease?
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
8.8 / 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
8.9 / Are prepared standards, reference materials, and reagents assigned a unique identification number traceable to the original standards?
TNI EL-V1M2-2009, Section 5.6.4.2c, d)
8.10 / Are the unique identification numbers and dates placed on the prepared standard, reference material and reagent containers?
TNI EL-V1M2-2009, Section 5.6.4.2 d)
8.11 / Are standards and reference materials traceable to a national standard or other certified standards?
QSM Rev. 5.0, Module 2, Section 5.6.3.2
8.12 / Are the certificates of authenticity kept on file?
TNIEL-V1M2-2009 Section 5.6.4.2 a
8.13 / Do procedures exist for the storage of reagents and laboratory consumable materials relevant for the tests and calibrations?
TNIEL-V1M2-2009, Section 4.6.1
Item
Number / Line of Inquiry / Status / Summary of Observations/Objective Evidence
Reviewed Audit Notes
9.0 / Negative Control – Method Performance: Method Blank
9.1 / Is the method blank processed along with and under the same conditions as the associated samples?
TNIELV1M4-2009, Section 1.7.3.1 a)
9.2 / Is the method blank processed through all steps of the analytical procedure?
TNIEL-V1M4-2009, Section 1.7.3.1 a)
9.3 / Are procedures in place to determine if a method blank is contaminated?
TNIEL-V1M4-2009, Section 1.7.3.1 a)
9.4 / Are any affected samples associated with a contaminated method blank reprocessed for analysis or are the results reported with appropriate data qualifiers?
TNIEL-V1M4-2009, Section 1.7.3.1 a)
9.5 / Is the method blank analyzed at a minimum of one (1) per preparation batch?
TNIEL-V1M4-2009, Section 1.7.3.1b)
9.6 / In those instances for which no separate preparation method are used (for example, volatiles in water),does the batch consist of environmental samples that are analyzed together with thesame method and personnel, using the same lots of reagents, not to exceed the analysis oftwenty (20) environmental samples, not including method blanks, LCS, matrix spikes andmatrix duplicates?