U. S. Department of Energy
Consolidated Audit Program Checklist 3 - Data Quality for Inorganic Analyses DoD/DOE QSM 5.0- Version 1.0 of Revision 6.4 Self-Identifying Checklists March 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.
Audit ID: Date: U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
Data Quality for Inorganic Analyses Revision Date: March 2017 Page 1 of 67
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 – GFAA
11.0 Inductively Coupled Plasma Mass Spectrometry (ICP/MS) 12.0 Multipoint Calibration Procedures – ICP-ABS
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 U = Unsatisfactory NA = Not Applicable NO = Not Observed F = Finding O = Observation U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Audit ID: ______Laboratory: ______Auditor:
Areas of Review during Audit Referenced regulations are accessible at the following URLs:
http://www.p2s.com/?page_id=1526 http://www.epa.gov/epawaste/hazard/testmethods/index.htm
NOTE:
When audit findings are written against site-specific documents (i.e., SOPs, QA Plans, licenses, permits, etc.), a copy of 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 the last page of this document for the record of revision. Refer to Errata Document 10-25 for interim changes to the QSM Rev.5.0 requirements U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Audit ID: ______Laboratory: ______Auditor: U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Audit ID: ______Laboratory: ______Auditor:
Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number 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) U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 1.4 Are permanent, bound laboratory notebooks (logbooks) or notebooks used that have measures in place to prevent the removal or addition of pages?
QSM Rev. 5.0, Module 2, Section 4.13.4 a) Are all notebook pages closed when the activities recorded are completed or carried over to another page? b) Does the person responsible for performing the closure is the person who performed the last activity recorded? c) Did Closure occur at the end of the last activity recorded on a page, as soon as practicable thereafter? d) Did documentation of the closure include analyst initials and date?; and e) Does each laboratory notebook have a unique serial number clearly displayed? f) Are laboratory notebook pages pre-numbered? g) Are all entries are signed or initialed and dated by the person responsible for performing the activity at the time the activity is performed? h) Are all entries are recorded in chronological order?
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 U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 1.7 When mistakes occur in records, is each mistake crossed out, not erased, made illegible or deleted, and the correct value entered alongside? ISO/IEC 17025 Clause 4.13.2.3 1.8 Are all such alterations to records are signed or initialed by the person making the correction? ISO/IEC 17025 Clause 4.13.2.3 1.9 In the case of records stored electronically, are equivalent measures taken to avoid loss or change of original data?
ISO/IEC 17025 Clause 4.13.2.3 2.0 Balances 2.1 Is a check of the balance performed 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) U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 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 Table and 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 U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 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 U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objectives Line of Inquiry Status Facility Respoinse/Comments Status Evidence Number 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 repair and 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 the specifications 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) 5.0 Metals Digestion U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objectives Line of Inquiry Status Facility Respoinse/Comments Status Evidence Number Reviewed Audit Notes 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 (“Type II” water or equivalent) for digestion procedures? (ASTM D1193).
EPA SW-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 6010D, Section 7.1 U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Audit ID: ______Laboratory: ______Auditor: U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 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? Limit of Detection (LOD) and Limit of Quantitation (LOQ)
TNI EL-V1M4-2009, Section 1.5.2 6.2 Does the laboratory document how LODs were derived from the method determinations?
TNI ELV1M4-2009, 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?
TNI ELV1M4-2009, 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?
TNI ELV1M4-2009, 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?
TNI ELV1M4-2009, 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?
TNI ELV1M4-2009, Section 1.5.2.1 b) 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) U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 6.8 Is the verification of the LOD completed prior to the use of the LOD for sample analysis?
TNI ELV1M4-2009, Section 1.5.2.1 b) 6.9 Are LODs verified annually for each quality system matrix, technology, and analyte?
TNI ELV1M4-2009, 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)?
TNI ELV1M4-2009, 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?
TNI ELV1M4-2009, 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?
TNI ELV1M4-2009, 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)?
TNI ELV1M4-2009, 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.
TNI ELV1M4-2009, 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? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes
TNI ELV1M4-2009, 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?
TNI ELV1M4-2009, 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?
TNI ELV1M4-2009, Section 1.5.3 b) 6.18 Do precision and bias measurements evaluate the method across the analytical calibration range of the method?
TNI ELV1M4-2009, 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?
TNI ELV1M4-2009, Section 1.5.3 b) 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 U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 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 the details of the initial and continuing instrument calibration procedures including calculations, integrations, acceptance criteria and associated statistics included or referenced in the method SOP and retained for the laboratory for review?
TNI EL-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?
TNI EL-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 instrument calibration verification performed: i. at the beginning and end of each analytical batch. ii. if the time period for calibration or the most recent calibration verification has expired; or iii. for analytical systems that contain a calibration verification requirement?
TNI EL-V1M4-2009, Section 1.7.2 c) 7.9 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 the highest calibration standard at or above the highest concentration for which quantitative data are to be reported? (TNI EL-V1M4-2009, Section 1.7.1.1.g) U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 7.12 Are data reported above the calibration range reported using defined qualifiers and explained in the narrative?
(TNI EL-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?
TNI EL-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? TNI EL-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?
TNI EL-V1M4-2009, Section 1.7.1.1 d) 7.16 Is traceability to a national standard documented, when commercially available?
TNI EL-V1M4-2009, Section 1.7.1.1 d) 7.17 Are data associated with an unacceptable calibration verification reported under the following considerations: i. When the acceptance criteria for the continuing calibration verification are exceeded high (i.e., high bias) and there are associated samples that are non-detects, then those non-detects may be reported. Otherwise the samples affected by the unacceptable calibration verification shall be re-analyzed after a new calibration curve has been established, evaluated and accepted; or ii. When the acceptance criteria for the continuing calibration verification are exceeded low (i.e., low bias), those sample results may be reported if they exceed a maximum regulatory limit/decision level. Otherwise the samples affected by the unacceptable verification shall be re-analyzed after a new calibration curve has been established, evaluated and accepted. U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes TNI EL-V1M4-2009, Section 1.7.2 e) 8.0 Standards and Reference Material 8.1 Does the laboratory ensure that purchased supplies and reagents and consumable materials that affect the quality of tests and/or calibrations are not used until they have been inspected or otherwise verified as complying with standard specifications or requirements defined in the methods for the tests and/or calibrations concerned? ISO/IEC 17025, Clause 4.6.2 8.2 Are records of actions taken to check compliance maintained?
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 purchasing documents for items affecting the quality of laboratory output contain data describing the services and supplies ordered?
ISO/IEC 17025, Clause 4.6.3 8.7 Are purchasing documents for items affecting the quality of laboratory output reviewed and approved for technical content prior to release? 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 U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 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 5.6.4.2 c, 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?
TNI EL-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?
TNI EL-V1M2-2009, Section 4.6.1 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?
TNI ELV1M4-2009, Section 1.7.3.1 a) 9.2 Is the method blank processed through all steps of the analytical procedure? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes
TNI EL-V1M4-2009, Section 1.7.3.1 a) 9.3 Are procedures in place to determine if a method blank is contaminated?
TNI EL-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?
TNI EL-V1M4-2009, Section 1.7.3.1 a) 9.5 Is the method blank analyzed at a minimum of one (1) per preparation batch?
TNI EL-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 the same method and personnel, using the same lots of reagents, not to exceed the analysis of twenty (20) environmental samples, not including method blanks, LCS, matrix spikes and matrix duplicates?
TNI EL-V1M4-2009, Section 1.7.3.1b) 9.7 Does the method blank consist of a matrix that is similar to the associated samples?
TNI-EL-V1M4-2009, Section 1.7.3.c) 9.8 Is the matrix known to be free of the analytes of interest?
TNI-EL-V1M4-2009, Section 1.7.3.c) 9.9 Is the concentration of a targeted analyte in the blank at or above the reporting limit as established by the method or by regulation, AND is greater than 1/10 of the amount measured in the sample?
TNI EL-V1M4-2009, Section 1.7.4.1 a) U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 9.10 If a blank is determined to be contaminated, is the cause investigated and measures taken to minimize or eliminate the problem?
TNI EL-V1M4-2009, Section 1.7.4.1 c) 9.11 Are samples associated with a contaminated blank evaluated for the type of corrective action for the samples (e.g., reprocessing or data qualifying codes).
TNI EL-V1M4-2009, Section 1.7.4.1 c) 9.12 In all cases is the corrective action documented?
TNI-EL-V1M4-2009, Section 1.7.4.1 c) Positive Controls – Method Performance: Laboratory Control Samples 9.13 Are any affected samples associated with an out of control LCS reprocessed for re-analysis or are the results reported with appropriate data qualifier?
TNI EL-V1M4-2009, Section 1.7.3.2.1) 9.14 Are LCS samples analyzed a minimum of one per preparation batch?
TNI EL-V1M4-2009, Section 1.7.3.2.2 9.15 In those instances for which no separate preparation method are used , does the batch consist of environmental samples that are analyzed together with the same method and personnel, using the same lots of reagents, not to exceed the analysis of twenty (20) environmental samples, not including method blanks, LCS, matrix spikes and matrix duplicates?
TNI EL-V1M4-2009, Section 1.7.3.2.2 9.16 Are all reported analytes spiked in the LCS?
QSM Rev. 5, Module 4 Section 1.7.3.2.3 b) 9.17 Is the concentration of the spiked components at or below the midpoint of the calibration if project specific concentrations are not specified? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes QSM Rev. 5, Module 4, Section M4 1.7.3.2.3 b) 9.18 Where there are no established criteria, has the laboratory determined internal criteria and documented the method used to establish the limits or does the laboratory use client specified assessment criteria?
TNI EL-V1M4-2009, Section 1.7.4.2 a) 9.19 When the same analyzed exceeds LCS control limits in 2 out of 3 consecutive LCS determination is a corrective action and reanalysis of the LSC initiated?
QSM Rev. 5, Module 4, Section 1.7.4.2.d) Sample Specific Controls NOTE: Examples of matrix-specific QC include: Matrix Spike (MS), Matrix Spike Duplicate (MSD), sample duplicates, and surrogate spikes. TNI EL-V1M4-2009, Section 1.7.3.3 9.20 Does the laboratory have procedures in place for tracking, managing, and handling matrix-specific QC criteria, including:
1) spiking appropriate components at appropriate concentrations, 2) calculating recoveries and relative percent difference, and 3) evaluating and reporting results based on performance of the QC samples?
TNI EL-V1M4-2009, Section 1.7.3.3 9.21 Does the laboratory have a procedure specifying the frequency for the matrix spike and matrix spike duplicates?
TNI EL-V1M4-2009, Section 1.7.3.3.1 b) Are MS and MSDs spiked with all reported analytes
QSM Rev. 5.o, Module 4, Section 1.7.3.3.1 c) 9.22 For matrix spikes and matrix spike duplicates, does the laboratory document the calculation for %R, RPD or other equations used?
TNI EL-V1M4-2009, Section 1.7.4.3 a) 9.23 For matrix spikes and matrix spike duplicates, are the results compared to the QSM Appendix C limits, if project limits are not specified? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes QSM Rev. 5.0, Appendix C 9.24 Where there are no established criteria (either in the method, specified by the project, or Appendix C of the QSM), has the laboratory determined internal criteria and has it documented the method used to establish the limits?
TNI EL-V1M4-2009, Section 1.7.4.3 a) 9.25 For matrix spike results outside established criteria, is corrective action documented or are the data for that sample reported with appropriate data qualifying codes?
TNI EL-V1M4-2009, Section 1.7.4.3 a) 9.26 For matrix duplicates, does the laboratory document the calculation for relative percent difference or other equations?
TNI EL-V1M4-2009, Section 1.7.4.3 b) 10.0 Multipoint Calibration Procedures - Atomic Absorption Spectrophotometry - EPA SW-846, Method 7000B 10.1 Is reagent grade water used in all tests?
SW-846 Method 7000B, Section 7.2 10.2 Is reagent water free of interferences?
(SW-846 Method 7000B, Section 7.2) 10.3 Does Nitric Acid (concentrated) meet the following? Has spectrograde certification A 1:1 dilution prepared with water does not contain analytes above the lowest limit of quantitation. SW-846 Method 7000B, Section 7.3 10.4 Does Hydrochloric Acid (1:1) meet the following: Has spectrograde certification A 1:1 dilution prepared with water does not contain analytes above the lowest limit of quantitation. SW-846 Method 7000B, Section 7.4 10.5 Is a calibration curve prepared each day and does it consist of a minimum of a calibration blank and three standards? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes (SW-846 Method 7000B, Section 10.2) 10.6 Are calibration standards prepared each day [that analysis is performed]?
SW-846 Method 7000B, Section 10.2 10.7 Is the curve linear and does it have a correlation coefficient (r) of at least 0.995?
SW-846 Method 7000B, Section 10.2 10.8 After calibration, is the calibration curve verified using a calibration blank and a calibration check standard that is derived from a source independent of that used to prepare the initial calibration standards?
SW-846 Method 7000B, Section 10.2.1 10.9 Is an initial calibration verification (ICV) standard prepared at a concentration at or near mid-range of the initial calibration curve
SW-846 Method 7000B, Section 10.2.1 10.10 Is the analytical result of the ICV within 10% of its true value?
SW-846 Method 7000B, Section 10.2.1 10.11 Is the calibration curve verified at the end of each analysis batch and/or after every 10 samples by use of a continuing calibration verification (CCV) standard?
SW-846 Method 7000B, Section 10.2.2 10.12 Is the CCV result within 10% of the true value?
SW-846 Method 7000B, Section 10.2.2 10.13 If the calibration cannot be verified within the specified limits, is the sample analysis discontinued, the cause determined, and the instrument recalibrated?
SW-846 Method 7000B, Section 10.2.2 10.14 Is a laboratory control sample prepared for each batch of samples prepared? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes
SW-846 Method 7000B, Section 9.6 10.15 Is the LCS taken through a process identical to that of the associated samples?
SW-846 Method 7000B, Section 9.6 10.16 Were [LCS] percent recoveries within acceptance criteria? (80-120% for aqueous standards and manufacturer’s control limits for solid standards)?
SW-846 Method 7000B, Section 9.6 10.17 Is the laboratory duplicate (or matrix spike duplicate) prepared for each batch of samples prepared?
SW-846 Method 7000B, Section 9.7 10.18 Was a matrix spike prepared for each batch of samples prepared?
SW-846 Method 7000B, Section 9.7 10.19 Is the laboratory duplicate (MSD) taken through a process identical to that of the associated samples?
SW-846 Method 7000B, Section 9.7 10.20 Is the matrix spike (MS) taken through a process identical to that of the associated samples?
SW-846 Method 7000B, Section 9.7 10.21 Was the matrix spike recovery within ±25% of known value?
SW-846 Method 7000B, Section 9.7 10.22 If matrix spike recovery was not within ±25% was a post-digestion spike analyzed?
SW-846 Method 7000B, Section 9.8 U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 10.23 Dilution Test: Is one diluted sample analyzed per batch? Is the concentration of the analyte at least 25 times the estimated detection limit? Dilute the sample by at least 5 fold and reanalyze. Concentration agreement within 10% between the undiluted and diluted sample indicates the absence of interferences and tis t sample analyzed without using the method of standard additions?
SW-846 Method 7000B, Section 9.8 10.24 Recovery Test: Is a known amount of the analyte added to bring the concentration of the analyte to a minimum level of 10x and a maximum of 100x the lower limit of quantitation?) Is the spike recovery between 80 and 120%? If the % recovery criteria are not met, is the method of standard additions used for all samples in the batch?
SW-846 Method 7000B, Section 9.8.1 10.25 Method of Standard Addition (MSA): Does the laboratory employ the MSA when specified by the specific method, or When interference is suspected, or When a new matrix is encountered?
SW-846 Method 7000B, Section 9.10 11.0 Inductively Coupled Plasma – Mass Spectrometry (ICP-MS), EPA SW-846, Method 6020B U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 11.1 Instrument Detection Limits (IDLs): Are IDLs established by calculating the average of the standard deviations of three runs on three non-consecutive days from the analysis of a reagent blank solution with seven consecutive measurements per day? Is each measurement performed as a separate analytical sample? Are IDLs determined at least every three months and kept with the instrument log book?
SW-846 Method 6020B, Section 9.3 11.2 Is the ICP-MS capable of providing resolution better than or equal to 1.0 atomic mass unit (amu) at 10% peak height?
SW-846 Method 6020B, Section 6.1 11.3 Does the system have a mass range from at least 6 to 240 amu and a data system that allows for corrections for isobaric interferences and the application of the internal standard technique?
SW-846 Method 6020B, Section 6.1 11.4 Is the instrument allowed to equilibrate before analyzing any samples?
SW-846 Method 6020B, Section 11.4 11.5 Is instrument equilibration verified by analyzing a tuning solution at least four times with a relative standard deviation of ≤5% for the analytes in the tuning solution?
SW-846 Method 6020A, Section 11.4
Or Is the instrument tuned by following the instructions provided by the instrument manufacturer?
SW-846 Method 6020B, Section 11.4 11.6 Are mass calibration and resolutions checks conducted in the mass regions of interest prior to analysis? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes
SW-846 Method 6020B, Section 10.2 11.7 If the mass calibration differs by more than 0.1 amu from the true value, is the mass calibration adjusted to the correct value?
SW-846 Method 6020B, Section 10.2 11.8 Is the resolution verified to be less than 0.9 amu full-width at 10% peak height prior to analysis?
SW-846 Method 6020B, Section 10.2 11.9 Is a solution containing elements representing all of the mass regions of interest prepared [and analyzed] to verify that the resolution and mass calibration of the instrument are within the required specifications?
SW-846 Method 6020B, Section 7.10 11.10 For each instrument in use, is a calibration procedure performed for the isotopes of interest using a calibration blank and at least a single standard?
SW-846 Method 6020B, Section 10.4.2 11.11 Is the average of at least three integrations for each standard used to develop the calibration curve?
SW-846 Method 6020B, Section 10.4.2 11.12 Alternatively is a calibration curve developed, which consists of a calibration blank and at least 3 non-zero standards?
SW-846 Method 6020B, Section 10.4.2 11.13 If a calibration curve is used, is the coefficient of correlation ≥0.99?
6020BQSM, Rev. 5.0, Table 9 11.14 If a second-order equation is used for initial calibration, are the recoveries of each standard used in the curve determined?
SW-846 Method 6020B, Section 10.6 11.15 If a second-order equation is used for initial calibration, are the U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes recoveries of each standard within ±10% of reference value (±30% for the low standard)?
SW-846 Method 6020B, Section 10.6 11.16 If a calibration curve is generated for initial calibration, are results not reported below the calibration range defined by the lowest standard in the calibration curve?
SW-846 Method 6020B, Section 10.4.3 11.17 After initial calibration, the calibration curve should be verified by use of an initial calibration verification (ICV) standard analysis? . SW-846 Method 6020B, Section 10.4.3 11.18 Is the ICV prepared from a source differing from that used to calibrate the instrument?
SW-846 Method 6020B, Sections 7.8 and 10.4.3 11.19 Is the ICV recovery within ±10% of reference value?
SW-846 Method 6020B, Section 10.4.3 11.20 Is a low-level initial calibration verification standard run (does not have to be a second-source standard)?
SW-846 Method 6020B, Sections 10.4.2.1 and 10.4.3 11.21 Is the recovery of the low-level initial calibration verification standard within ±20% of reference value?
6020BQSM Rev. 5.0 Table 9 11.22 Is a lower limit of quantitation check sample run at the end of an analytical sequence?
SW-846 Method 6020B, Sections 10.4.4 11.23 Is the lower limit of quantitation check sample recovery within ±30% No updated – Not in Table 9 of of reference value? the QSM
SW-846 Method 6020B, Sections 10.1.3.1, 10.3.2.1, and 10.3.4 U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 11.24 Is a mid-level Continuing Calibration Verification standard prepared in the same matrix using the same standards as the calibration standards?
SW-846 Method 6020B, Section 7.9 11.25 Is a mid-level Continuing Calibration Verification standard run for every 10 samples?
SW-846 Method 6020B, Section 10.4.4 11.26 Is a mid-level Continuing Calibration Verification standard recovery within ±10% of reference value?
SW-846 Method 6020B, Section 10.4.4 11.27 Is an initial or continuing calibration blank (ICB/CCB) analyzed after each ICV/CCV standard?
SW-846 Method 6020B, Section 10.4.4 11.28 Is a corrective action process implemented when the recovery of the ICV/CCV standards are not within 10% of the accepted value?
SW-846 Method 6020B, Sections 10.4.3 and 10.4.4 11.29 If the recovery limit is not met, is the analysis terminated and the problem corrected?
SW-846 Method 6020B, Sections 10.4.3 and 10.4.4 11.30 Are samples associated with the affected calibration reanalyzed?
SW-846 Method 6020B, Section 10.4.4 11.31 Are internal standards no more than 50 amu removed from their associated elements to be quantified?
SW-846 Method 6020B, Section 7.5 11.32 Are the intensities of all internal standards monitored for all analyses?
SW-846 Method 6020B, Section 9.6 11.33 If the intensity levels of any internal standard in the samples within 30- 120% of the intensity of the internal standard in the ICAP blank, is U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Audit ID: ______Laboratory: ______Auditor:
Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes corrective action undertaken?
Criteria – QSM Rev. 5.0, Table 9 11.34 If the intensity results of the internal standards do not meet specifications, is recalibration performed and verified and affected samples reanalyzed?
SW-846 Method 6020B, Section 9.6 11.35 If internal standard recoveries in a sample are not greater than 70%, is the sample diluted?
SW-846 Method 6020B, Section 9.6 11.36 Are samples that exceed the linear dynamic range diluted or reanalyzed on an alternate mass?
SW-846 Method 6020B, Sections 9.5 and 11.6 11.37 Are interference levels corrected by the instrument data system?
SW-846 Method 6020B, Section 7.7 11.38 Are the interference corrections accounted for in the data report?
SW-846 Method 6020B, Section 12.2 11.39 Is the Interference Check Solution (ICS) prepared to contain known concentrations of interfering elements that will demonstrate the magnitude of interferences and provide an adequate test of any corrections?
SW-846 Method 6020B, Section 7.7 11.40 Is the ICS solution prepared from ultra-pure reagents?
SW-846 Method 6020B, Section 7.7.1 11.41 Are both ICSs A and AB analyzed at the beginning of an analytical run, or once every 12 hours, whichever is more frequent?
SW-846 Method 6020B, Section 7.7 11.42 Note: If samples that are more concentrated than the linear range for an U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes analyte (or species needed for a correction) are not diluted to bring them within range, a less abundant isotope may be measured.
Is the linearity of the alternate mass confirmed by calibration?
SW-846 Method 6020B, Section 11.8 11.43 Is the upper limit of the calibration range verified by running a standard at the upper limit of the dynamic range?
SW-846 Method 6020B, Section 10.6 11.44 The following apply to the Post Digestion (Analytical) Spike: Is an analyte spike added to a portion of a prepared sample or its dilution? If the recovery is not within 80-129%, or within the laboratory defined acceptance criteria, is a (serial) dilution test or MSA performed? For samples with concentrations that are minimally a factor of 10 above the lower limit of quantitation before a 1:5 dilution, was the serial dilution %D criterion of 10% met?
SW-846 Method 6020B, Section 9.11.2; QSM Rev. 5.0, Table 9 11.45 Is the post spike addition based on the indigenous concentration of each element in the sample?
SW-846 Method 6020B, Section 9.11.1 11.46 If the spike recovery is outside the specified limits, is the sample diluted and reanalyzed to compensate for the matrix effect?
SW-846 Method 6020B, Section 9.11.1 11.47 For samples with concentrations that are minimally a factor of 50 above the quantitation before a 1:5 dilution, do The results agree to within 10% of the original determination? NOTE: The use of a standard–addition analysis procedure may also be used to compensate for this effect.
SW-846 Method 6020B, Section 9.11.2 U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Audit ID: ______Laboratory: ______Auditor:
Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes 11.48 For each new matrix, is a dilution test performed that:
analyzes a five-fold dilution on a sample containing analytes ≥ 50 times the quantitation limit; has results that agree with ± 10% of the original determination; and if the ± 10% criteria are not met, reported results are qualified “E”?
Is one dilution test included for each batch of 20 samples or less, where native samples results are greater than 50 times the quantitation limits?
SW-846 Method 6020B, Section 9.11.2 12.0 Multipoint Calibration Procedures – Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) Method 6010C 12.1 Linear Dynamic Range (LDR): Are the signal responses from a minimum of three different concentration standards across the range determined? Is the upper range limit an observed signal that is within ±10% of reference value? Are new dynamic ranges determined whenever there is a significant change in instrument response? Are the ranges determined every six months for those analytes that periodically approach the upper limit?
SW-846 Method 6010C, Section 10.4 12.2 Interelement Correction (IEC) Factor: When IEC are applied, is their accuracy verified daily through the analysis of spectral interference check solutions? If the multivariate correction matrices tested on a daily basis are found to be within the 20% criteria for 5 consecutive days, are the required verification frequency of those factors in compliance extended to a weekly basis? NOTE: If the nature of the samples analyzed is such they do not contain concentrations of the interfering elements at ± one reporting limit from zero, daily verification is not required. Are all interelement spectral correction factors or multivariate correction matrices verified and updated every six months or U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes when an instrumentation change, such as in the torch, nebulizer, injector, or plasma conditions occurs? Is data for the initial and periodic verification of the IEC factors maintained in a manner that is readily accessible to the analyst?
SW-846 Method 6010C, Section 4.2.9 12.3 If interelement corrections are not used, are interferences verified to be absent on a sample-by-sample basis (e.g., through use of multiple analyte wavelengths)?
SW-846 Method 6010C, Section 4.2.10 12.4 Is a calibration curve generated each time the instrument is used for sample analysis?
SW-846 Method 6010C, Section 10.3.2 12.5 Is a single standard and blank run as a minimum to calibrate the instrument?
SW-846 Method 6010C, Section 10.3.2 12.6 Alternatively is a calibration curve developed, which consists of at least a calibration blank and 3 non-zero standards?
SW-846 Method 6010C, Section 10.3.2 12.7 If a calibration curve is used, is the coefficient of correlation r2 ≥ 0.99?
QSM Rev. 5.0, Table 8 12.8 If a second-order equation is used for initial calibration, are the recoveries of each standard used in the curve determined?
SW-846 Method 6010C, Section 10.4 12.9 If a second-order equation is used for initial calibration, are the recoveries of each standard within ±10% of reference value (±30% for the low standard)?
SW-846 Method 6010C, Section 10.4 12.10 Are third-order equations or greater not used in instrument calibration? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes
SW-846 Method 6010C, Section 10.4 12.11 Following daily calibration, are an ICV, LLICV, CCV, LLCCV, and CCB analyzed?
SW-846 Method 6010C, Section 11.3 12.12 Is the ICV prepared from a source differing from that used to calibrate the instrument?
SW-846 Method 6010C, Sections 7.6, 10.3.1 and 10.3.3 12.13 Is the LLICV prepared from the same source as that used to calibrate the instrument?
SW-846 Method 6010C, Sections 10.3.3 12.14 Is the ICV recovery within ±10% of reference value?
SW-846 Method 6010C, Section 10.3.2.1 12.15 Is the recovery of the low-level initial calibration verification (LLICV) standard within ±20% of reference value?
QSM Rev. 5.0, Table 8 12.16 Is a lower limit of quantitation check (LLICV) sample run at the end of an analytical sequence?
SW-846 Method 6010C, Sections 10.3.4 and 11.3 12.17 Is the result for the ending LLICV within ±30% of reference value?
SW-846 Method 6010C, Section 10.3.4 12.18 Is a lower limit of quantitation (LLQC) sample analyzed on as as- needed basis after low-level reporting limits are established by the laboratory?
SW-846 Method 6010C, Section 10.1.3.1 12.19 Is the LLQC standard taken through the entire preparatory and analytical process? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Audit ID: ______Laboratory: ______Auditor:
Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes EPA SW-846 Method 6010C, Section 10.1.3.1 12.20 Are a CCB and either a CCV or an ICV analyzed after every tenth sample and at the end of the sample run?
EPA SW-846 Method 6010C, Sections 10.3.4 12.21 When the calibration verification falls outside the method or laboratory established criteria, is the sample analysis discontinued, the cause determined, and the instrument recalibrated
EPA SW-846, Method 6010B, Sections 7.4 and 8.6.1.2 12.22 Are all samples following the last acceptable ICV, CCV, or check standard reanalyzed?
EPA-846, Method 6010B, Sections 7.4 and 8.6.1.2 12.23 Is the analysis data of the calibration blank, check standard, ICV, and CCV kept on file with the sample analysis data?
EPASW-846, Method 6010B, Section 7.4 12.24 Is the blank less than (whichever is greater):
No analytes detected > ½ LOQ or 1/10 the amount measured in any sample or
1/10 the regulatory limit, whichever is greater.
QSM, Rev. 5.0, Table 8 12.25 Is an Interference Check Standard analyzed on a daily basis?
EPA SW-846 Method 6010C, Sections 4.2.9 and 10.1.5.6 12.26 Were the ICSAB recoveries within acceptance criteria of 80-120%?
EPA SW-846 Method 6010C, Section 4.2.10.2 12.27 If interelement corrections are not used, are interferences verified to be absent on a sample-by-sample basis (e.g., through use of multiple analyte wavelengths)? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes EPASW-846 Method 6010C, Section 4.2.10 12.28 Is a dilution test run on a sample that fails both pre- and post-digestion spike analysis?
EPA SW-846 Method 6010C, Section 9.9.1 12.29 For samples with concentrations that are minimally a factor of 50 above the quantitation before a 1:5 dilution, was the serial dilution %D criterion of 10% met?
EPA SW-846 Method 6010C, Section 9.9.2 12.30 If the post-digestion spike recovery is not within 80-120%, is the dilution test or MSA performed?
EPA SW-846 Method 6010C, Section 9.9.1 12.31 Are the results of the dilution test (serial dilution) within ±10% of the original sample concentration?
EPA SW-846 Method 6010C, Section 9.9.2 Multipoint Calibration Procedures - Cold Vapor Atomic Absorption Spectrometry (CVAA) Methods: Hg Analysis by EPA SW-846 Methods 13.0 7470A and 7471A 13.1 Were five standards plus a blank prepared for initial calibration for mercury analysis?
EPA SW-846 Method 7470A, Section 7.2 and Method 7471B, Section 10.1 13.2 Are the working standards and stock dilutions prepared fresh (daily) before the analysis?
EPA SW-846 Method 7470A, Section 5.10 and Method 7471B, Section 5.8 13.3 If the laboratory performs EPA SW-846, Method 7471A, is aqua regia used for sample and standards preparation?
EPASW-846, Method 7471A, Sections 7.1 and 7.3 13.4 If the laboratory performs EPA SW-846, Method 7471A, are triplicate 0.2 g portions of the untreated sample used during sample preparation? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes
EPA SW-846, Method 7471A, Section 7.1 13.5 Are hot plates used for sample preparation adjustable and capable of maintaining a temperature of 90º - 95º C?
EPA SW-846 Method 7470A, Section 4.10 and Method 7471B, Section 4.10 13.6 Was a method blank prepared for each batch of samples prepared?
EPA SW-846 Method 7471B, Section 9.3 13.7 Is the method blank taken through a process identical to that of the associated samples?
EPA SW-846 Method 7471B, Section 9.3 13.8 Was a laboratory control sample prepared for each batch of samples prepared?
EPA SW-846 Method 7471B, Section 9.4 13.9 Is the LCS taken through a process identical to that of the associated samples?
EPA SW-846 Method 7471B, Section 9.4 13.10 Were [LCS] percent recoveries within acceptance criteria? (80-120% for aqueous standards and manufacturer’s control limits for solid standards)?
EPA SW-846 Method 7471B, Section 9.4 13.11 Was a matrix spike prepared for each batch of samples prepared?
EPA SW-846 Method 7471B, Section 9.5 13.12 Was the laboratory duplicate (or matrix spike duplicate) prepared for each batch of samples prepared?
EPA SW-846 Method 7471B, Section 9.5 13.13 Is the matrix spike (MS) taken through a process identical to that of the associated samples? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes
EPA SW-846 Method 7471B, Section 9.5 13.14 Is the laboratory duplicate (MSD) taken through a process identical to that of the associated samples?
EPA SW-846 Method 7471B, Section 9.5 14.0 Quality Control (QC) of Instrument Gases 14.1 For Atomic Absorption methods, are fuel and oxidant gases of the appropriate quality to ensure proper instrument performance used, including, but not limited to, the following: acetylene (high purity) compressed air (“clean and dry”) nitrous oxide;
EPA SW-846, Method 7000B, Section 7.5 For ICP/AES analyses, is the argon gas supply high purity grade (99.99%)?
EPA SW-846, Method 6010c, Section 6.1.6 14.2 For ICP/MS analyses, is the argon gas supply high purity grade (99.99%)?
EPA SW-846, Method 6020B, Section 6.2 15.0 Wet Chemistry Procedures Cyanide Distillation by EPA SW-846, Method 9010, and Analysis by EPA SW-846, Method 9014 15.1 Does the laboratory perform pretreatment on all samples suspected of containing cyanide amenable to chlorination?
EPA SW-846, Method 9010B, Section 7.1 or Method 9010C, Section 7.1 15.2 During the distillation process, if the sample is suspected to contain sulfide, is bismuth nitrate added to the sample?
EPA SW-846, Method 9010B, Section 7.2.3 or Method 9010C, Section 7.2.3 15.3 During the distillation process, if bismuth nitrate has been added to the sample, or if the sample is suspected to contain nitrate or nitrite, is U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Audit ID: ______Laboratory: ______Auditor:
Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes sulfamic acid added to the sample?
EPA SW-846, Method 9010B, Section 7.2.4 or Method 9010C, Section 7.2.4 15.4 Does the laboratory use six standards and a blank for the preparation of the multipoint calibration curve?
EPA SW-846, Method 9014, Sections 7.3 1 15.5 Is at least one matrix spike sample analyzed with each batch of 20 samples or less through the entire sample preparation and analytical process?
EPA SW-846, Method 9010B, Section 8.5 or Method 9010C, Section 8.5; EPA SW-846, Method 9014, Section 8.5 15.6 Is one replicate sample analyzed with each batch of 20 samples or less?
EPA SW-846, Method 9010B, Section 8.4 or Method 9010 C, Section 8.4 15.7 Is one reagent blank analyzed with each analytical batch or per every 20 samples?
EPA SW-846, Method 9010B, Section 8.2. or Method 9010C, Section 8.2 15.8 Is one check standard analyzed with every analytical batch?
EPA SW-846, Method 9010B, Section 8.3 or Method 9010C, Section 8.3; EPA SW-846, Method 9014, Section 8.3 15.9 Is the method of standard additions used for analysis of all samples that suffer from matrix interference?
EPA SW-846, Method 9010B, Section 8.7 or Method 9010C, Section 8.7; EPA SW-846, Method 9014, Section 8.6 16.0 Reactivity Determinations - Colorimetric Cyanide by EPA SW-846, Method 9012A and 9012B 16.1 Is pre-treatment performed on all samples suspected to be amenable to chlorination? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes EPA SW-846, Method 9012A, Section 7.1 or Method 9012B, Section 7.1 16.2 During distillation, is bismuth nitrate added to samples suspected to contain sulfides?
EPA SW-846, Method 9012A, Section 7.1.6 or Method 9012B, Section 7.1.6 16.3 During distillation, is sulfamic acid added to samples suspected to contain nitrites or nitrates, or samples to which bismuth sulfate was previously added?
EPA SW-846, Method 9012A, Section 7.2.3 or Method 9012B, Section 7.2.3 16.4 Is a standard curve prepared by plotting absorbance versus concentration?
EPA SW-846, Method 9012A, Sections 7.4.4 and 7.5.2 or Method 9012B, Sections 7.4.4 and 7.5.2 16.5 Is the calibration curve verified with every sample batch by analyzing a mid-range standard?
EPA SW-846, Method 9012A, Section 8.2 or Method 9012B, Section 8.2 16.6 Is a matrix spike sample run for every 10 samples?
(Note: QSM, Table 11 states one per preparatory batch)
EPA SW-846, Method 9012A, Section 8.3 or Method 9012B, Section 8.3 17.0 Reactivity Determinations - Titrimetric Sulfide – EPA SW-846, Method 9034 17.1 Is a reagent blank analyzed once every 20 samples, or with each analytical batch, whichever is more frequent?
EPA SW-846, Method 9034, Section 8.2 17.2 Is a check standard analyzed once every 20 samples, or with each analytical batch, whichever is more frequent? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Audit ID: ______Laboratory: ______Auditor:
Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes
EPA SW-846, Method 9034, Section 8.3 17.3 Is a matrix spike sample analyzed once every 20 samples, or with each analytical batch, whichever is more frequent?
EPA SW-846, Method 9034, Section 8.4 18.0 TCLP Extractions – EPA SW-846, Method 1311, Toxicity Characteristic Leaching Procedure (TCLP) 18.1 Does the agitation apparatus rotate at 30 ± 2 rpm?
EPA SW-846, Method 1311 Section 4; 18.2 Is the verification of the rotation documented and a frequency for the verification of the rotation defined?
EPA SW-846, Method 1311 Section 4; 18.3 Are zero Headspace Extraction (ZHE) units leak checked after every extraction by monitoring the pressure gauge or by pressurizing the unit, submerging in water, and checking for bubbles?
EPA SW-846, Method 1311, Section 4.2.1 18.4 Does the laboratory have a corrective action procedure for handling leaking ZHE vessels?
EPA SW-846, Method 1311, Section 4.2.1 18.5 ZHE Extract Collection Devices:
Is the final extract for ZHE collected in Tedlar bags or glass, stainless steel, or polytetrafluoroetylene (PTFE) gas-tight syringes?
EPA SW-846, Method 1311, Section 4.6 18.6 Extraction Fluid Reagents: • Is the extraction fluid reagents prepared using ASTM Type II water and reagent grade chemicals or equivalent? 18.7 • Is the pH of extraction fluid 1 4.93 ± 0.05 (4.88-4.98)? 18.8 • Is the pH of extraction fluid 2 2.88 ±0.05 (2.83-2.93)? 18.9 • Is the pH of the extraction fluid reagents checked prior to use? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes EPA SW-846, Method 1311, Section 5.7 18.10 Determination of Percent Solids: If the percent solid is determined to be < 0.5%, is the sample filtered through 0.6-0.8µm filter paper, solids are discarded, and the liquid analyzed? If the percent solid is determined to be ≥ 0.5% is the liquid, if any, separated from the solid phase and stored for later analysis? Is the solid phase extracted using the amount of extraction fluid equal to 20 times the weight of the solid phase? Following extraction is the liquid extract filtered through 0.6-0.8µm glass fiber filter?
EPA SW-846, Method 1311, Sections 2.1 and 2.2 18.11 In determination of particle size reduction, is particle size reduced to < 9.5mm?
EPA SW-846, Method 1311, Section 7.1.3 18.12 Determination of Appropriate Extraction Fluid:
For ZHE extraction, is fluid #1 used? For TCLP extraction, is fluid determination based on pH? if pH < 5, is fluid #1 used; if pH > 5, even after addition of HCl, Is fluid #2 used?
EPA SW-846, Method 1311, Section 7.1.4 18.13 Is the room temperature maintained at 23 ± 2°C during agitation?
EPA SW-846, Method 1311, Sections 7.2.11 and 7.3.12.3 18.14 Are TCLP and ZHE extraction devices rotated at 30 ± 2 rpm for 18 ± 2 hours?
EPA SW-846, Method 1311, Sections 7.2.11 and 7.3.12.3 18.15 Immediately following TCLP extraction collection, is the pH of the extract recorded and the extract preserved for analysis? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes
EPA SW-846, Method 1311, Section 7.2.14 18.16 Are metals aliquots acidified with nitric acid to pH < 2 and organic aliquots refrigerated?
EPA SW-846, Method 1311, Section 7.2.14 18.17 Is the method blank for TCLP/ZHE of the same extraction fluid as the sample(s), tumbled in an extraction vessel, and filtered in the same manner as the sample(s)?
EPA SW-846, Method 1311, Section 8.1 18.18 Is a minimum of one matrix spike performed for each batch?
EPA SW-846, Method 1311, Sections 8.2 and 8.2.1 18.19 Are matrix spikes added after filtration of the TCLP/ZHE extract and prior to preservation?
EPA SW-846, Method 1311, Sections 8.2 and 8.2.1 Ignitability Test: EPA SW-846, Methods 1010, Pensky-Martin Closed Cup, and 1020A (Seta-Flash Closed Cup), ASTM D93-06 (Pensky- 19.0 Martens), or ASTM D3278-96 (Seta-Flash) 19.1 Are the stirring and heat-up rates monitored and documented?
ASTM Methods (D93-06 and D3278-96) 19.2 Does the apparatus employed by the laboratory meet the requirements of either ASTM D93-94 (Pensky-Martens) or ASTM D3278-82 (Seta- Flash)?
ASTM Methods (D93-06 and D3278-96) 19.3 When samples contain non-filterable suspended solids or liquids that form surface films, is the Pensky-Martens method used?
ASTM Methods (D93-06 and D3278-96) 19.4 Are calibrations verified using a fluid with a known flash point?
ASTM Methods (D93-06 and D3278-96) 19.5 Is the calibration verification performed immediately after calibration, U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Audit ID: ______Laboratory: ______Auditor:
Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes at the beginning of each analytical batch, and after the last site sample has been analyzed?
ASTM Methods (D93-06 and D3278-96) 19.6 If the Seta Flash method is used, are two measurements obtained for each sample?
ASTM Methods (D93-06) 19.7 Is a corrective action process initiated if duplicate measurement results are not within established limits?
ASTM Methods (D93-06) 19.8 (Requirements 19.6 and 19.7 do not apply for the Pensky-Martens method.)
ASTM Methods (D93-06) 20.0 Corrosivity Determination: pH Electrometric Measurement by EPA SW-846, Method 9040B, and Method 9040C 20.1 Do the pH meters in operation at the time of the audit have the following characteristics: temperature compensating, and capable of measuring sample and reference standards temperatures?
EPA SW-846, Method 9040B, Sections 4.5 and 7.0 or EPA SW-846 Method 9040C, Sections 4.5 and 7.0 20.2 Does the apparatus include a magnetic stirrer with stirring bar made of non-reactive material, such as Teflon?
EPA SW-846, Method 9040B, Section 4.4 or 9040C, Section 4.4 20.3 Are the following calibration criteria met: are calibrations performed daily and each time the instrument is set up; does the curve contains a minimum of two points that are at ~ 3 pH units apart; is verification performed immediately after calibration and after the last site sample is analyzed? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Audit ID: ______Laboratory: ______Auditor:
Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes EPA SW-846 ,Method 9040B, Section 7.1 and Method 9040C, Section 7.1; 21.0 Corrosivity Towards Steel by EPA SW-846, Method 1110 21.1 Does the test apparatus for corrosivity towards steel include: kettle or flask; reflux condenser; thermowell; temperature regulating device; heating device; and specimen support system?
EPA SW-846, Method 1110, Section 4.1 or Method 1110A, Section 4.1 21.2 Is the minimum ratio of volume of waste to area of the metal coupon to be used 40 ml/cm2?
EPA SW-846, Method 1110, Section 4.5.3 or Method 1110A, Section 4.5.3 21.3 Are coupons cleaned after immersion and prior to weighing?
EPA SW-846, Method 1110, Section 7.6 or Method 1110A, Section 7.6 21.4 Is a blank cleaned with the test coupons and its weight loss subtracted from that calculated for the test coupons?
EPA SW-846, Method 1110, Section 7.7 or Method 1110A, Section 7.7 21.5 Are duplicate samples analyzed on a routine basis?
EPA SW-846, Method 1110, Section 8.2 or Method 1110A, Section 8.2 22.0 Total Organic Carbon (TOC) by EPA SW-846, Method 9060A 22.1 Are samples stored at 4 ± 2°C?
EPA SW-846, Method 9060A, Section 6.2 22.2 Are samples homogenized?
EPA SW-846, Method 9060A, Section 7.1 22.3 Is the calibration of the instrument verified by an independently U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes prepared check standard every 15 samples?
EPA SW-846, Method 9060A, Section 8.3 22.4 Are blanks processed and analyzed with each batch?
EPA SW-846, Method 9060A, Section 8.2 22.5 Is one spike duplicate sample analyzed for every 10 samples?
EPA SW-846, Method 9060A, Section 8.4 22.6 Are samples analyzed in quadruplicate as required by the method?
Are both the average and the range reported?
EPA SW-846, Method 9060A, Section 7.6 23.0 Total Organic Halogens (TOX) by EPA SW-846, Methods 9020B and 9022 23.1 Is the purity of the activated carbon verified before use?
EPA SW-846, Method 9020B, Section 3.2; EPA SW-846, Method 9022, Section 3.2 23.2 For calibration, is the repeatability of the method background established each day by analysis of nitrate wash blanks?
EPA SW-846, Method 9020B, Section 7.2.2; EPA SW-846 Method 9022, Section 7.2.2 23.3 For calibration, are duplicate calibration standards and the blank standard pyrolized each day before analysis?
EPA SW-846, Method 9020B, Section 7.2.3 25.4 Is an independent calibration check standard run after calibration?
EPA SW-846, Method 9020B, Section 8.4 23.5 For neutron activation, is calibration performed daily using radioactive standards?
EPA SW-846, Method 9022, Section 7.2.3 23.6 For neutron activation, is an independent calibration check standard run U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Audit ID: ______Laboratory: ______Auditor:
Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes every 15 samples?
EPA SW-846, Method 9022, Section 8.5 23.7 Are samples analyzed in duplicate?
EPA SW-846, Method 9020B, Section 8.2 23.8 Are at least two blanks analyzed to establish the repeatability of the method background prior to sample analysis?
Are method blanks analyzed between every eight analytical determinations?
EPA SW-846, Method 9020B, Section 8.3 23.9 For neutron activation, at minimum, is one blank per sample batch run?
EPA SW-846, Method 9022, Section 8.4 23.10 Is a matrix spike sample run every 10 samples?
EPA SW-846, Method 9020B, Section 8.5; EPA SW-846, Method 9022, Section 8.6 24.0 Biological Oxygen Demand (BOD) Determinations - EPA Method 405.1 and Standard Methods (SM) 5210B 24.1 Is the dissolved oxygen meter calibration verified before use?
SM 4500-G, Section 3 24.2 Is the incubator or water bath thermostatically controlled at 20º ± 1º C?
SM 5210B, Section 2b 24.3 Is the dilution water checked for purity?
SM 5210B, Section 4b 24.4 Is the seed control performed to determine seed Dissolved Oxygen (DO) uptake?
SM 5210B, Section 4d.2 24.5 Is a dilution water blank performed and the acceptance limit for DO U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes uptake not more than 0.2 mg/l?
SM 5210B, Section 4b 24.6 Are the samples incubated for five days at 20º C in the dark?
EPA Method 405.1 25.0 Chemical Oxygen Demand (COD) Determinations – EPA Method 410.1; 410.2; 410.3 or 410.4 and Standard Methods (SM) 5220 25.1 Has the proper COD method been selected?
SM 5220A, Section 2 25.2 Have interferences and limitations been adequately addressed?
SM 5220A, Section 2; EPA Methods 410.1, 410.2, and 410.4, Section 4.0
25.3 If the samples require preservation, is the sample preserved with H2SO4 to a pH of < 2?
EPA Methods 410.1, 410.2, and 410.3, Section 3.0 25.4 If EPA Method 5220D is employed, does the calibration curve contain at least five standards with COD equivalents to cover each concentration range?
SM 5220D, Section 4c 25.5 Is a new calibration curve prepared for each new lot of tubes or ampules, or when standards prepared differ by 5% or more from the standard calibration curve?
SM 5220D, Section 4c Total Phosphorus, Nitrate/Nitrite and Anions Determinations: EPA SW-846, Method 9056, Determination of Inorganic Anions by Ion 26.0 Chromatography (chloride, fluoride, bromide, nitrate, nitrite, phosphate, and sulfate) 26.1 Are all reported results within the working range of the instrument?
EPA SW-846, Method 9056A, Section 11.2.5 26.2 Does the calibration curve consist of, at a minimum, three concentration levels for each analyte of interest and a blank? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes EPA SW-846, Method 9056A, Section 7.6; SM 1020B 22nd Edition,, Section 11 26.3 Is a midrange calibration standard analyzed after every 10 injections?
SM 1020B, 22nd Edition, Section 11.c Is the instrument recalibrated if the response changes more than 10%?
EPA SW-846, Method 9056A, Section 10.7 26.4 A duplicate sample is analyzed with every batch.
EPA SW-846, Method 9056A, Section 8.3; SM 4020A-, 22nd Edition, Section 2.f, as applies to Total Phosphorous 26.5 Is a linear calibration plot with an acceptable correlation coefficient (≥0.995), intercept, and slope calculated?
EPA SW-846, Method 9056A, Section 10.5 26.6 Are samples filtered or allowed to settle prior to analysis? Are samples that contain particles larger than 0.45µm and reagent solutions that contain particles larger than 0.20 µm filtered to prevent damage to instrument columns and flow systems? NOTE: This does not apply to reagent filtration
EPA SW-846, Method 9056A, Section 4.4; SM 4500-P B, Section 1 26.7 Is the retention time for each analyte within 3 standard deviations of the calibration standard’s average retention time (anion analysis only)?
Are retention times documented?
EPA SW-846, Method 9056A, Section 11.2.4 NOTE: This does not apply to Total Phosphorous. 27.0 Kinetic Phosphorescence Analysis 27.1 Are water samples evaporated to dryness and wet-ashed
ASTM Method D5174 – 02, Section 4.2 Is reagent grade water used to prepare samples, reagents, standards, and 27.2 for the rinsing of glassware for the determination of low-level uranium U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes by KPA?
ASTM Method D5174 – 02 For all low-level uranium analysis, prior to initial use, are all new 27.3 glassware with the exception of cuvettes used in KPA measurements, soaked in hot 8M nitric acid for at least two hours and then in room temperature 8M nitric acid overnight?
ASTM Method D5174 – 02 For each sample, are both the sample and sample-plus-spike measured 27.4 to demonstrate that there are no quenching interferences?
ASTM Method D5174 – 02 Is a new aliquot of the sample prepared when the following 27.5 documented acceptance criteria are not met: phosphorescence lifetimes fall in the range of 150s to 350s ; linear regression coefficient of the decay plot is > 0.96 for samples where the measured concentration is greater than the RDL; standard addition recovery is greater than 90% when Analyte concentration is in the range of the calibration curve used reference ratio is between 0.9 and 1.1; and continuing calibration check standard is within 10% of the known value?
ASTM Method D5174 – 02 27.6 Is the KPA calibrated daily when in use? Is the order for performing instrument calibration: background, calibration curve, and calibration check standard?
ASTM Method D5174 - 02, Section 9.2 27.7 Are the following requirements implemented for calibration curves: the background is sufficiently low to permit attaining RDLs; U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes at least three standards are used for each calibration range; the calibration range includes the range of the sampled to be measured; and the linear regression coefficient (R2) for the calibration curve is > 0.99?
ASTM Method D5174 – 02 27.8 Are the following requirements implemented for calibration check standards: the performance check is performed using a separately prepared standard at a different concentration from the calibration standards;
the performance check is performed upon completion of calibration and subsequently after every 10 samples are analyzed; and
the relative bias of the calibration check standards is in the range -0.10 to +0.10?
ASTM Method D5174 – 02 28.0 Colorimetric Hexavalent Chromium 28.1 Are samples stored at 0-6°C until analyzed?
QSM, Rev.5.0, Section 5.5.13.1 f (Table) Are samples analyzed within 24 hours after extraction? 28.2 SW-846-Method 7196-A, Section 6.3 Is a daily initial calibration (ICAL) analyzed? 28.3 QSM Rev 5.0, Appendix B, Table 10 Does the ICAP meet the r 2 ≥ 0.99? 28.4 QSM Rev 5.0, Appendix B, Table 10 Once after each ICAL, is an initial calibration verification (ICV) 28.5 standard from a second source analyzed? U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes
Is the result of the ICV within ±10% of the true value?
QSM Rev 5.0, Appendix B, Table 10 28.6 Is a continuing calibration verification (CCV) standard analyzed daily before sample analysis, after every 15 file samples, and at the end of the analysis sequence?
QSM Rev 5.0, Appendix B, Table 10 28.7 Is the result of the CCV within ±10% of the true value?
QSM Rev 5.0, Appendix B, Table 10 28.8 Is a method blank analyzed once per preparatory batch
QSM Rev 5.0, Appendix B, Table 10 28.9 Does the method blank meet the following acceptance criteria”
(a) no analytes detected (b) >1/2 LOQ>1/2 LOQ (c) > 1/10 the amount measured in any sample or 1/10 the regulatory limit, whichever is greater.
QSM Rev 5.0, Appendix B, Table 10 28.10 Is a laboratory controls sample (LCS) analyzed with each preparatory batch?
QSM Rev 5.0, Appendix B, Table 10 28.11 Does the LCS meet the acceptance criteria limits in QSM Appendix C Limits for batch control if project limits are not specified
QSM Rev 5.0, Appendix B, Table 10 28.12 Is a matrix spike sample analyzed once per preparatory batch?
QSM Rev 5.0, Appendix B, Table 10 28.13 Does the matrix spike meet the acceptance criteria limits in QSM Appendix C Limits for batch control if project limits are not specified U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes QSM Rev 5.0, Appendix B, Table 10 28.14 Is a matrix spike or matrix spike duplicate analyzed once per preparatory batch?
QSM Rev 5.0, Appendix B, Table 10 28.15 If a matrix spike duplicate is analyzed, does the matrix spike duplicate meet the acceptance criteria limits in the QSM Appendix C Limits for batch control if project limits are not specified?
QSM Rev 5.0, Appendix B, Table 10 28.16 Does the sample/matrix duplicate or matrix spike/matrix spike duplicate RPD meet the acceptance criteria of ≤ 20%?
QSM Rev 5.0, Appendix B, Table 10 28.17 For solid samples, is a soluble and insoluble pre-digestion matrix spike analyzed per preparatory batch?
QSM Rev 5.0, Appendix B, Table 10 28.18 Is the recovery for the soluble and insoluble pre-digestion matrix spike within 75-125%
QSM Rev 5.0, Appendix B, Table 10 28.19 For solid samples, is a post-digestion matrix spike analyzed per preparatory batch analyzed?
QSM Rev 5.0, Appendix B, Table 10 28.20 Is the recovery for the post-digestion matrix spike within 85-115%
QSM Rev 5.0, Appendix B, Table 10 29.0 Sample Dilutions 29.1 When sample results exceed the quantitation range, are the samples diluted and reanalyzed (when sufficient sample volume and holding time permits) to bring sample results within the quantitation range?
QSM Rev. 5.0, Module 4, Section 1.7.1.1 g) 29.2 Are sample results outside the quantitation range reported as estimated U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Item Summary of Observations/Objective Line of Inquiry Status Facility Response/Comments Status Evidence Number Reviewed Audit Notes values and qualified using qualifiers that are explained in the case narrative?
QSM Rev. 5.0, Module 4, Section 1.8.6 g) 30.0 Data Review 30.1 Is data review inclusive of all quality related steps in the analytical process, including sample preparation, dilution calculations, chromatography, and spectral interpretations?
QSM Rev. 5.0, Module 2, Section 4.2.8.4 x) 30.2 Is data review documented and records maintained?
QSM Rev. 5.0, Module 2, Section 4.2.8.4 x) 30.3 Spreadsheets used for calculations are verified before use and documentation is readily available for review.
QSM Rev. 5.0, Module 2, Section M2 5.4.7.2 h) U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Record of Revision for Checklist 3 Data Quality for Inorganic Analyses
Revision Effective Reason for Line of Number Date Revision Inquiry Changed reference for laboratory notebooks from Section 4.12 4.3 11/2009 1.3 DOE-5 to DOE-6 Changed reference for closure of laboratory notebooks from Section 4.3 11/2009 1.4 4.12 DOE-5 to DOE-6 Add requirement purity checks for reagents (QSAS Section 5.6 4.3 11/2009 7.6 DOE-1) 5.3 11/2010 No Changers or Revisions Added to the Note section of the checklist: Fully document 5.4 1/2012 Page 1 any deviation from the LOI or requirements of QSAS 2.8 Full revision based on the DoD/QSM Rev. 5.0, TNI-ELV1- 6.0 11/2013 All 2009, and ISO/IEC 17025:2005 6.1 2/2014 Minor revision following first audit of FY14 All Deletion of quarterly accuracy checks for mechanical 6.2 3/2014 3.3 pipettes Updated reference to promulgated Method 6010D and 6.3 10/2015 5.4 changed wording to match the update 6.3 10/2015 Changed reference to QSM Appendix C 9.23 Changed acceptance criteria to the method, project specified, 6.3 10/2015 9.24 or QSM Appendix C 6.3 10/2015 Updated Section 11.0 to Method 6010B 11.0 Added alternate language for the instrument tuning per 6.3 10/2015 11.5 6010B and left the old LOI for 6010A 6.3 10/2015 Global change 6020A to 6020B All Changed coefficient correlation criteria to ≥ 0.99 per QSM 6.3 10/2015 11.13 Rev. 5.0, Table 9 Changed the low-level initial calibration verification 6.3 10/2015 11.21 standard criteria to ±20% 6.3 10/2015 Revised intensity levels for any internal standard to QSM 11.33 U.S. Department of Energy Consolidated Audit Program DOECAP Audit Checklist: 3 Rev. 6.4
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Table 9.0 Revised the post digestion spike criteria to 80-120% per 6.3 10/2015 11.44 QSM Table 9.0 6.3 10/2015 Revised the calibration curve criteria to r2 ≥ 0.99, Table 8 12.7 Revised the LLICV criteria to ± 20%, QSM Rev. 5.0, Table 6.3 10/2015 12.15 8 Revised the blank acceptance criteria as defined QSM Rev. 6.3 10/2015 12.24 5.0, Table 8 6.3 10/2015 Changes temperature requirement to 0 to 6°C 28.1 6.3 10/2015 Changed LCS acceptance criteria limits 28.11 6.3 10/2015 Changed MS acceptance criteria limits 28.13 6.3 10/2015 Added matrix duplicate to the LOI 28.14 6.3 10/2015 Changed MSD acceptance criteria limits 28.15 Added acceptance criteria for the sample/matrix duplicate or 6.3 10/2015 28.16 matrix spike/matrix spike duplicate RPD 6.3 10/2015 Revised numbering for 28.17 – 28.20 Section 28 Revised legend for area of review to include Colorimetric 6.3 10/2015 Hexavalent Chromium and renumbered Sample Dilution, Page 1 and Data Review to correspond to Sections 28. 29. and 30. 6.3 10/2015 Addition of Colorimetric Hexavalent Chromium Section 28 6.3 10/2015 Renumbered Section 28 to Section 29 for Sample Dilution Section 29 6.3 10/2015 Renumber Section 29 to Section 30 for Data Review Section 30 6.4 3/2017 Removal of Official Use Only