U.S. Department of Energy
Consolidated Audit Program
Checklist 4 - Data Quality for Radiochemistry Analyses
DoD/DOE QSM – Version 1.0 - Revision 4.3
Self-Identifying Checklist – 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 Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Laboratory:
__ SOPs
__ Yield Monitors
__ Negative Activities
__ MDA and DL
__ Contamination Control
__ Performance Testing (PT) Programs
A = Acceptable
NO = Not Observed
Rev. 4.3
Page 1 of 60
Auditor:
Areas of Review During Audit
__ Sample Handling
__ Gas Flow Proportional Counting
__ Batch Quality Control (QC)
__ Gamma Spectroscopy
__ Reagents, Standards and Water Quality __ Liquid Scintillation Counting
__ Instrument Operation and Calibration
__ Radon (Lucas Cell)
__ Alpha Spectroscopy
__ Reanalysis/Recount
U = Unsatisfactory
F = Finding
NA = Not Applicable
O = Observation
Referenced regulations are accessible at the following URLs:
NOTE:

http://www.p2s.com/?page_id=1526

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 all deviation from the LOI or the requirements of QSM Rev. 5.0 and TNI ELV1M6
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 Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
1.0
1.1
1.2
1.3
1.4
1.5
1.6
1.7
Laboratory:
Line of Inquiry
Standard Operating Procedures (SOPs)
Where referenced methods are required, are they referenced to
nationally accepted sources, such as EPA methods, DOE
Methods Compendium, HASL 300 methods, etc., where
applicable?
TNI-EL-V1M6-2009, Section 1.4
Have non-standardized methods that have been developed by
the laboratory been appropriately documented before use?
TNI-EL-V1M6-2009, Section 1.4
Are all procedures being used by the laboratory documented?
TNI-EL-V1M6-2009, Section 1.5.2
Does the documentation include the quality system matrix
type?
TNI-EL-V1M6-2009, Section 1.5.2
Is all supporting data retained by the laboratory?
TNI-EL-V1M6-2009, Section 1.5.2
Has the laboratory validated non-standard methods,
laboratory-designed/developed methods, reference methods
used outside their published scope, and amplifications and
modifications of reference methods to confirm that the
methods are fit for the intended use?
TNI-EL-V1M6-2009, Section 1.5.1
Has the validation of non-standardized methods been extensive
enough to meet the needs of the given application and
documentation is available?
TNI-EL-V1M6-2009, Section 1.5.1
Rev. 4.3
Page 2 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
1.8
Laboratory:
Line of Inquiry
Has the laboratory recorded the results obtained, the procedure
used for the validation, and a statement as to whether the
method is fit for the intended use? (The minimum
requirements for method validation are given in TNI-ELV1M6-2009, Sections 1.5.2 – 1.5.5.)
1.0
TNI-EL-V1M6-2009, Section 1.5.1
Where modifications to the published method have been made,
changes are clearly described and documented.
1.10
TNI-EL-V1M6-2009, Section 1.5.1
Do the laboratory SOPs document the formulas for calculating
the Combined Standard Uncertainty (CSU) of a result,
including both systematic and random error?
1.11
1.12
1.13
QSM Rev. 5.0, Module 6, Section 1.5.4
TNI-EL-V1M6-2009, Section 1.5.4
ANSI N42.23, Sections 4.1.3.2 and A8
Do all radiochemical measurements provide the uncertainty of
each quantitative result at the 95% or 2 sigma confidence
level?
QSM Rev. 5.0, Module 6, Section 1.5.4
ANSI N42.23, Sections 4.1.3.2 and A8
Are the results reported with the associated measurement
uncertainty as a combined standard uncertainty (CSU)?
QSM Rev. 5.0, Module 6, Section 1.5.4
ANSI N42.23, Sections 4.1.3.2 and A8
In the case of a result having zero (0) counts, is the counting
uncertainty is assumed to be the square root of one (1) count?
QSM Rev. 5.0, Module 6, Section 1.5.4
Rev. 4.3
Page 3 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
1.14
Laboratory:
Line of Inquiry
Do the laboratory SOPs specify acceptance criteria for QC
samples?
QSM Rev. 5.0, Module 6, Section 1.5.4
Rev. 4.3
Page 4 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
2.0
2.1
2.2
2.3
2.4
2.5
Laboratory:
Line of Inquiry
Internal Tracers and Carriers
Is each sample in a QC batch (including QC samples), spiked
with a tracer or yield carrier, when applicable, that chemically
mimics and does not interfere with the target analyte through
radiochemical separations?
QSM Rev. 5.0, Module 6, Section 1.7.2.3 c) and d)
TNI-EL-V1M6-2009, Section 1.7.2.3 c) and d)
For those methods that employ a tracer or carrier for yield
determination, does each sample result have an associated
yield calculated and reported?
QSM Rev. 5.0, Module 6, Section 1.7.2.3 c) and d)
TNI-EL-V1M6-2009, Section 1.7.2.3 c) and d)
Is the tracer or carrier yield assessed against the specific
acceptance criteria specified in the laboratory method SOP?
QSM Rev. 5.0, Module 6, Section 1.7.2.3 c) and d)
TNI-EL-V1M6-2009, Section 1.7.2.3 c) and d)
In the event of a failed tracer or carrier yield, are the corrective
actions taken noted in the laboratory report to the client?
TNI-EL-V1M6-2009, Section 1.7.2.3 c) and d)
Are tracers or carriers are added at the very beginning of the
sample preparation process, after subsampling but before any
chemical treatment, to accurately trace any losses of analytes
of interest early in the preparation process, unless otherwise
specified by the method?
QSM Rev. 5.0, Module 6, Section 1.7.2.3 c) and d)
TNI-EL-V1M6-2009, Section 1.7.2.3 c) and d)
ANSI N42.23, Section 5.27
Rev. 4.3
Page 5 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
2.6
Laboratory:
Line of Inquiry
For solid samples, is the tracer added after grinding, sieving,
etc., but prior to any muffling or dissolution?
QSM Rev. 5.0, Module 6, Section 1.7.2.3 c) and d)
ANSI N42.23, Section 5.27
2.7
Are radiometric results corrected for chemical yield using
‘indirect’ yield measurement techniques such as gravimetric
measurement of added carriers or a second radiometric
measurement of added tracer?
2.8
QSM Rev. 5.0, Module 6, Section 1.7.2.3 c) and d)
TNI-EL-V1M6-2009, Section 1.7.2.3 c) and d)
Does the chemical yield for each sample determined using an
indirect yield measurement method, fall within the range 30%
- 110% or as specified by the client?
2.9
QSM Rev. 5.0, Module 6, Section 1.7.2.3 c) and d)
TNI-EL-V1M6-2009, Section 1.7.2.3 c) and d)
Is the technique used for the carrier measurements sufficient to
maintain relative uncertainties associated with the yield
correction below 10% at the 2-sigma level?
2.10
2.11
QSM Rev. 5.0, Module 6, Section 1.7.2.3 and d)
TNI-EL-V1M6-2009, Section 1.7.2.3 c) and d)
Is the uncertainty associated with chemical yield corrections
incorporated into the CSU of the associated sample results?
QSM Rev. 5.0, Module 6, Section 1.7.2.3 c) and d)
TNI-EL-V1M6-2009, Section 1.7.2.3 c) and d)
Is the tracer activity and sample count duration adequate to
achieve relative uncertainties for the tracer measurement of
less than 10% at the 2-sigma level?
QSM Rev. 5.0, Module 6, Section 1.7.2.3 c) and d)
TNI-EL-V1M6-2009, Section 1.7.2.3 c) and d)
Rev. 4.3
Page 6 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
2.12
Laboratory:
Line of Inquiry
Are sample results with yields below 30% considered
quantitative and acceptable if:
• The relative uncertainty associated with the yield
correction is less than 10% (2-sigma);
• Spectral resolution requirements are met and there are no
indications of spectral interferences; and
• Detection limit requirements are met?
2.13
QSM Rev. 5.0, Module 6, Section 1.7.2.3 c) and d)
When the specified yield acceptance criteria are not met, are
the specified corrective actions and contingencies followed?
2.14
TNI-EL-V1M6-2009, Section 1.7.2.3 c) and d)
Are the procedures for data reduction, such as use of linear
regression, documented?
2.15
TNI-EL-V1M6-2009, Section 1.7.2.4 a)
Is each analytical result with its measurement uncertainty
documented in a report that clearly explains the uncertainty?
2.16
TNI-EL-V1M6-2009, Section 1.7.2.4 b)
Does the report indicate whether the uncertainty is the
combined standard uncertainty (“one sigma”) or an expanded
uncertainty?
For expanded uncertainties, does the report indicate the
coverage factor (k) and optionally the approximate level of
confidence?
TNI-EL-V1M6-2009, Section 1.7.2.4 b)
Rev. 4.3
Page 7 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
3.0
3.1
Laboratory:
Line of Inquiry
Negative Activities
All negative activities are reported as such.
QSM Rev. 5.0, Module 6, Section 1.7.2.4 d)
3.2
Are negative results below -3 sigma (combined standard
uncertainty) evaluated to determine whether the cause is
random or systematic?



If the cause is systematic, is the problem corrected?
If the cause is random, is the problem addressed in the
case narrative?
Are recurrent problems with significant negative
results investigated and is the resolution documented?
QSM Rev. 5.0, Module 6, Section 1.7.2.4 d)
ANSI N42.23, Sections 5.2.8, 5.2, and A.5.2.3
Rev. 4.3
Page 8 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
4.0
4.1
4.2
4.3
4.4
4.5
4.6
Laboratory:
Line of Inquiry
TNI-EL-V1M6-2009, Section 1.5.2.1a)
ANSI N42.23, Section A8
Is the MDA initially determined for the analytes of interest in
each method in a quality system matrix in which there are no
target analytes and no interferences at levels that would impact
the results?
TNI-EL-V1M6-2009, Section 1.5.2.1b)
Is the MDA determined each time there is a change in the
method that affects how the test is performed, or when a
change in instrumentation occurs that affects the analytical
detection capability?
TNI-EL-V1M6-2009, Section 1.5.2.1c)
Do the SOPs document and incorporate equations to calculate
the minimum detectable activity (or concentration) and the
decision level?
QSM Rev. 5.0, Module 6, Section 1.5.2.1e)
Are the factors that affect the MDA (sample size, count
duration, tracer chemical recovery, detector background, blank
standard deviation, and detector efficiency) being optimized
such that the sample MDAs are less than or equal to the
required detection Reporting Limits (RLs)?
QSM Rev. 5.0, Module 6, Section 1.5.2.1.1b)
Page 9 of 60
Auditor:
Status
Facility Response/Comments
Minimum Detectable Activity (MDA) and Decision Level (DL) Determination
Does the laboratory determine the MDA for the method for
each target analyte of concern in the quality system sample
matrices?
TNI-EL-V1M6-2009, Section 1.5.2.1a)
ANSI N42.23, Section A8
Are all sample-processing steps of the analytical method
included in the determination of the MDA?
Rev. 4.3
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
4.7
4.8
4.9
4.10
4.11
4.12
Laboratory:
Line of Inquiry
If the RLs are not achieved, is the cause being addressed in the
case narrative?
QSM Rev. 5.0, Module 6, Section 1.5.2.1.1b)
If the sample and background count times are of the same
duration, is the calculation defined in the QSM Rev. 5.0 being
used?
(See Appendix A for these equations)
QSM Rev. 5.0, Module 6, Section 1.5.2.1.1c)
Otherwise, is the equation for the MDA appropriately
modified to account for the difference in sample and
background count times?
(See Appendix A for these equations)
QSM Rev. 5.0, Module 6, Section 1.5.2.1.1c)
Has the implementation of blank populations for calculation of
MDAs been documented and described in detail in a SOP?
(See Appendix A for these equations)
QSM Rev. 5.0, Module 6, Section 1.5.2.1.1c)
The equations for MDA have the units of dpm/sample. If
other units are used, is the appropriate conversion documented
in the SOPs?
(See Appendix A for these equations)
QSM Rev. 5.0, Module 6, Section 1.5.2.1.1c)
Are the aliquant sizes appropriate for the activity levels in the
sample and large enough to generate data which meet the
following criteria:
 The measurement uncertainty shall not be greater than
10% (1 sigma) of the sample activity.
 The MDA for the analysis shall be a maximum of 10%
of the sample activity?
QSM Rev. 5.0, Module 6, Section 1.5.2.1.1b) thru d)
Rev. 4.3
Page 10 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
4.13
4.14
Laboratory:
Line of Inquiry
If sample-specific MDAs are calculated and reported, is that
clearly stated in the data package?
QSM Rev. 5.0, Module 6, Section 1.5.2.1.1 d)iv)
Are the laboratory procedures that incorporate the MDA
equation consistent with the mandated method or regulation?
QSM Rev. 5.0, Module 6, Section 1.5.2.1e)
Rev. 4.3
Page 11 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
5.0
5.1
5.2
5.3
5.4
5.5
5.6
Laboratory:
Line of Inquiry
Contamination and Cross-Contamination Control
Does the laboratory maintain a radiological control program
that addresses analytical radiological control?
TNI-EL-V1M6-2009, Section 1.7.2.7c)
Does the program address the procedures for segregating
samples with potentially widely varying levels of
radioactivity?
QSM Rev. 5.0, Module 6, Section 1.7.2.7d)
TNI-EL-V1M6-2009, Section 1.7.2.7c)
Does the radiological control program explicitly define how
low-level and high-level samples will be identified, segregated
and processed in order to prevent sample cross-contamination?
TNI-EL-V1M6-2009, Section 1.7.2.7c)
Does the radiological control program include the measures
taken to monitor and evaluate background activity or
contamination on an ongoing basis?
TNI-EL-V1M6-2009, Section 1.7.2.7c)
There is effective separation between neighboring work areas
when activities therein are incompatible.
TNI EL-V1M2-2009, Section 5.3.3
Adequate measures are taken to ensure good housekeeping in
the laboratory and to ensure that any contamination does not
adversely affect data quality.
TNI EL-V1M2-2009, Section 5.3.5
Rev. 4.3
Page 12 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
Laboratory:
Line of Inquiry
6.0
Performance Testing (PT) Programs
6.1
Can the laboratory demonstrate continued proficiency in either
MAPEP or external performance testing programs?
6.2
Rev. 4.3
Page 13 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
QSM Rev. 5.0, Module 1, Section 3.2.1
Does the laboratory document the cause(s) for failed PT
results and develop corrective action(s) to address the causes
within 21 calendar days from receipt of the results?
QSM Rev. 5.0, Module 1, Section 3.2.2
7.0
7.1
7.2
7.3
8.0
8.1
Are samples that require thermal preservation considered
acceptable if the arrival temperature of a representative sample
container is either within 2°C of the required temperature or
the method specified range?
TNI EL-V1M2-2009, Section 1.7.4a)
For samples with a specified temperature of 4°C, are samples
with a temperature ranging from just above the freezing
temperature of water to 6°C acceptable?
TNI EL-V1M6-2009, Section 1.7.4a)
Does the laboratory procedures for checking chemical
preservation using readily available techniques, such as pH or
chlorine, prior to or during sample preparation or analysis?
TNI EL-V1M6-2009, Section 1.7.4b)
Batch Quality Control (QC) (For all Radiochemistry QC requirements, see QSM Rev. 5.0 Appendix B, Tables 16-19)
Are all QC samples (method blanks, laboratory control
samples, duplicates, and matrix spikes) processed along with
and under the same conditions as the associated samples and
include all steps of the preparation, counting and analytical
procedures?
QSM Rev. 5.0, Module 6, Sections 1.7.2
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
8.2
8.3
8.4
8.5
8.6
Laboratory:
Line of Inquiry
Do all method QC samples follow the QSM Rev. 5.0
Appendix B requirements, as appropriate?
QSM Rev. 5.0, Module 6, Section 1.7.2
Are the laboratory standards used to prepare LCS and matrix
spikes from a source independent of the laboratory standards
used for instrument calibration.
TNI EL-V1M6-2009,Section 1.7.2.2 f) and 1.7.2.3 a)vi)
Are all QC samples counted for a sufficient time to meet the
required detection limit (except in the case where the
achieved MDA is calculated from the standard deviation of a
blank population) in which case, the method blanks are
counted for the same count time as the samples?
QSM Rev. 5.0, Module 6, Sections 1.7.2.1d), 1.7.2.2j) and
1.7.2.3 a) xiii)
Are the QC samples prepared with an aliquot size similar to
that of the routine samples being analyzed?
TNI EL-V1M6-2009, Section 1.7.2.1 c) and 1.7.2.2 i)
Is the QC sample matrix the same as the field samples, as can
be reasonably achieved, and is documented in the case
narrative?
QSM Rev. 5.0, Module 6, Section 1.7.2.1d), 1.7.2.2k)
8.7
8.7.1
8.7.2
Negative Control – Method Blanks
Are procedures in place to determine if a method blank
result is significantly different from zero?
TNI EL-V1M6-2009, Section 1.7.2.1 a)
Are samples associated with a failed method blank
reprocessed for analysis or the results reported with
appropriate data qualifying codes?
Rev. 4.3
Page 14 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
8.7.3
Laboratory:
Line of Inquiry
TNI EL-V1M6-2009, Section 1.7.2.1 a)
Are method blanks analyzed at a minimum of one (1) per
preparation batch, which shall be a maximum of twenty (20)
field samples, for all radiochemical methods except gross
alpha/beta in solid matrices and gamma-ray spectrometry?
8.7.4
TNI EL-V1M6-2009, Section 1.7.2.1 b)
Does the method blank consist of a quality system matrix
that is similar to the associated samples and is known to be
as free of the analytes of interest as possible?
8.7.5
TNI EL-V1M6-2009, Section 1.7.2.1 c)
Unless permitted by method or program, does the laboratory
not subtract the method blank result from the sample results
in the associated preparation or analytical batch?
8.7.6
TNI EL-V1M6-2009, Section 1.7.2.1 c)
Method Blank Acceptance Criteria
Does the laboratory use one method blank per preparatory
batch? (MARLAP 18.4.1)
8.7.7
8.7.8
8.7.9
QSM Rev. 5.0, Module 6, Section 1.7.2.1 e)
Does the laboratory use either the method blank acceptance
criteria of |ZBlank |≤ 3 or in-house control limits of ±3 σ of
the mean?
MARLAP, Chapter 18, Section 4.1
QSM Rev. 5.0, Module 6, Section 1.7.2.1e)
Is the Method Blank MDA less than the Reporting Limit?
QSM Rev. 5.0, Module 6, Section 1.7.2.1e)
If the above criteria are not met, are corrective actions taken
(e.g., recount, interferent cleanup, as appropriate), unless all
sample results are greater than five times the blank activity?
Rev. 4.3
Page 15 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
8.7.10
8.7.11
Laboratory:
Line of Inquiry
If the criteria are still not met, are the samples reanalyzed?
QSM Rev. 5.0, Module 6, Section 1.7.2.1e)
Are the following method blank matrices used for all
radiochemistry analyses;
• Distilled or deionized water, radon free;
• Characterized solid material representative of the
sample matrix;
• Filters, physically and chemically identical filter media,
analyte free (if supplied to the laboratory by
customer)?
QSM Rev. 5.0, Module 6, Section 1.7.2.1f)
Method Blank Data Acceptance / Rejection Criteria
Are samples reprocessed or is data appropriately qualified
if:
• the absolute value of the activity of a targeted analyte in
the blank exceeds three times its combined standard
uncertainty, AND is greater than 1/10 of the activity
measured in any sample; or
• the method blank result otherwise affects the sample
results as per the method requirements or the projectspecific measurement quality objectives?
8.7.12
TNI EL-V1M6-2009, Section 1.7.3.1a)
Are the acceptance criteria for samples associated with a
failed method blank calculated in a manner that
compensates for sample results based on differing aliquot
sizes?
TNI EL-V1M6-2009, Section 1.7.3.1b)
Rev. 4.3
Page 16 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
8.7.13
Laboratory:
Line of Inquiry
When a blank result is determined to be significantly
different from zero, is the cause investigated and are
measures taken to minimize or eliminate the problem?
8.7.14
TNI EL-V1M6-2009, Section 1.7.3.1c)
Are samples associated with a failed blank evaluated as to
the best corrective action for the samples (e.g., reprocessing
or data qualifying codes)?
8.7.15
TNI EL-V1M6-2009, Section 1.7.3.1c)
Are failed method blanks and associated corrective actions
noted in the laboratory report to the client?
TNI EL-V1M6-2009, Section 1.7.3.1d)
8.8
8.8.1
Positive Control – Laboratory Control Sample (LCS)
Are the results of the LCS compared to established criteria
and, if found to be outside of these criteria, indicate that the
analytical system is “out of control”?
8.8.2
TNI EL-V1M6-2009, Section 1.7.2.2 a)
Are samples associated with an out-of-control LCS
reprocessed for reanalysis or are the results reported with
appropriate data qualifying codes?
8.8.3
TNI EL-V1M6-2009, Section 1.7.2.2 a)
Is the LCS analyzed at a minimum of one per preparation
batch, except for those analytes for which no spiking
solutions are available?
8.8.4
TNI EL-V1M6-2009, Section 1.7.2.2 b)
Is the LCS a quality system matrix, known to be free of
analytes of interest, and spiked with known and verified
concentrations of analytes?
Rev. 4.3
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Item
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8.8.5
8.8.6
Laboratory:
Line of Inquiry
TNI EL-V1M6-2009, Section 1.7.2.2 c)
Is the activity of the laboratory control sample: (1) at least
ten (10) times the MDA, and (2) at a level comparable to
that of routine samples when such information is available if
the sample activities are expected to exceed ten times the
MDA?
TNI EL-V1M6-2009, Section 1.7.2.2 e)
Is the LCS counted for a sufficient time to meet the required
detection limit?
QSM Rev. 5.0, Module 6, Section 1.7.2.2 j)
8.8.7
Laboratory Control Sample Acceptance Criteria
Is the laboratory using the LCS Acceptance Criteria of |ZLCS|
≤ 3 or in-house control limits of LCS ± 3 σ of the mean
which are within 25% of the known LCS value?
8.8.8
MARLAP, Chapter 18, Section 4.1
QSM Rev. 5.0, Module 6, Section 1.7.2.2 l)
Is the LCS the same element as the sample analyte and at
least five times, but not greater than 20 times the RL, with
the following exceptions;
• For RLs of low activity, the analyte shall be at a level
where the random counting error does not exceed 10%
in the counting time required to attain the RL.
• Analytes for gamma spectroscopy need not be the same
as the sample analyte but should fall in the approximate
energy region of the spectrum (low, mid-range, and high
energy).
• For gross alpha and/or gross beta analysis, the analytes
in the LCS shall be the same analytes used for the
calibration curve.
QSM Rev. 5.0, Module 6, Section 1.7.2.2m)
Rev. 4.3
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8.8.9
8.8.10
Laboratory:
Line of Inquiry
Is the LCS traceable to the NIST or an accepted
international standard, or a working reference material as
described in ASTM C 1128 (current version), and may be
used repeatedly for different analytical batches as long as it
is appropriate for the matrix and geometry of the batch?
QSM Rev. 5.0, Module 6, Section 1.7.2.2n)
LCS Data Acceptance / Rejection Criteria
Are the results of the individual batch LCS calculated in
percent recovery or other appropriate statistical technique
that allows comparison to established acceptance criteria?
Has the laboratory documented the calculation?
8.8.11
8.8.12
8.8.13
8.8.14
TNI EL-V1M6-2009, Section 1.7.3.2 a)
Is the individual LCS compared to the acceptance criteria as
published in the mandated method?
TNI EL-V1M6-2009, Section 1.7.3.2 b)
Where there are no established criteria, has the laboratory
determined internal criteria and documented the method
used to establish the limits or utilize client specified
assessment criteria?
TNI EL-V1M6-2009, Section 1.7.3.2 b)
Are samples analyzed along with an LCS determined to be
“out of control” considered suspect, and the samples
reprocessed and re-analyzed or the data reported with
appropriate data qualifying codes?
TNI EL-V1M6-2009, Section 1.7.3.2 c)
Are failed LCS samples and associated corrective actions
noted in the laboratory report to the client?
TNI EL-V1M6-2009, Section 1.7.3.2 d)
Rev. 4.3
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8.9
8.9.1
Laboratory:
Line of Inquiry
Sample Specific Controls – Matrix Spike
Has the laboratory documented its procedures for
determining the effect of the sample matrix on method
performance?
NOTE: These procedures relate to the analyses of quality system
matrix specific quality control (QC) samples and are designed as
data quality indicators for a specific sample using the designated
method.
8.9.2
TNI EL-V1M6-2009, Section 1.7.2.3
Does the laboratory have procedures in place for tracking,
managing, and handling matrix-specific QC criteria
including spiking appropriate components at appropriate
concentrations, calculating recoveries and relative percent
difference, evaluating and reporting results based on
performance of the QC samples?
NOTE: Examples of matrix-specific QC include: Matrix Spike
(MS); Matrix Spike Duplicate (MSD); and replicates.
8.9.3
TNI EL-V1M6-2009, Section 1.7.2.3
Is the activity of the matrix spike analytes(s) greater than
five times the MDA but not greater than 20 times the RL?
8.9.4
QSM Rev. 5.0, Module 6, Section 1.7.2.3 xii)
TNI EL-V1M6-2009, Section 1.7.2.3 a) v)
Is the matrix spike prepared by adding a known activity of
target analyte after sub-sampling, if required, but before any
chemical treatment (e.g., chemical digestion, dissolution,
separation, etc.)?
8.9.5
TNI EL-V1M6-2009, Section 1.7.2.3 a) vii)
Is the lack of sufficient sample aliquot size to perform a
matrix spike noted in the laboratory report?
Rev. 4.3
Page 20 of 60
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Audit ID:
Item
Number
8.9.6
Laboratory:
Line of Inquiry
TNI EL-V1M6-2009, Section 1.7.2.3 a) iv)
Matrix Spike Acceptance Criteria
Are matrix spike recoveries within the control limits of 60 140%, or as specified by client?
NOTE: Matrix spike samples for which the sample activity is
greater than five times the spiking level are not required to meet
this criterion. If activity of the MS > 5 times the unspiked sample,
use |ZMS |≤ 3.
8.9.7
8.9.8
8.9.9
MARLAP, Chapter 18, Section 4.3
QSM Rev. 5.0, Module 6, Section 1.7.2.3 a)xi)
Is the matrix spike counted for a sufficient time to meet the
required detection limit?
QSM Rev. 5.0, Module 6, Section 1.7.2.3 a)xiii)
Where the original (unspiked) sample contains significantly
elevated activity, is the matrix spike counted for a duration
equal to that of the associated original sample?
QSM Rev. 5.0, Module 6, Section 1.7.2.3 a)xiii)
Matrix Spike Data Acceptance / Rejection Criteria
Are the %R or RPD results compared to the acceptance
criteria as published in the mandated method?
TNI EL-V1M6-2009, Section 1.7.3.3 a)ii)
8.9.10
Does the laboratory document the calculation for percent
recovery (%R), relative percent difference (RPD) or other
statistical treatment used?
TNI EL-V1M6-2009, Section 1.7.3.3 a)i)
8.9.11
Where there are no established criteria, has the laboratory
determined internal criteria and documented the method
used to establish the limits?
Rev. 4.3
Page 21 of 60
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Laboratory:
Line of Inquiry
8.9.12
TNI EL-V1M6-2009, Section 1.7.3.3 a)ii)
For matrix spike results outside established criteria, are
corrective actions documented or is the data reported with
appropriate data qualifying codes?
8.9.13
TNI EL-V1M6-2009, Section 1.7.3.3 a)ii)
Are failed matrix spikes and associated corrective actions
noted in the laboratory report to the client?
TNI EL-V1M6-2009, Section 1.7.3.3 a)iii)
8.10
8.10.1
Replicates / MS Duplicates / LCS Duplicates
Is at least one duplicate sample prepared and analyzed with
every analytical batch of samples?
QSM Rev. 5.0, Module 6, Section 1.7.2.3 b)vii)
8.10.2
8.10.3
8.10.4
Is the duplicate counted for the same duration of time to
meet the required detection limit?
QSM Rev. 5.0, Module 6, Section 1.7.2.3 b)ix)
When the sample does not contain significantly elevated
activity, are the QC samples counted for a duration equal to
that of the associated original sample?
QSM Rev. 5.0, Module 6, Section 1.7.2.3 b)x)
Replicate/Duplicate Acceptance Criteria
Are duplicates evaluated using the following three possible
criteria:
• |ZDup | ≤ 3 if using MARLAP;
• the duplicate error ratio (DER) between the sample and
the duplicate is <3;
• the relative percent difference (RPD) is <25%.
Rev. 4.3
Page 22 of 60
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Laboratory:
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When the MARLAP, DER or the RPD criteria pass, then the
duplicate is acceptable.
8.10.5
8.10.6
MARLAP, Chapter 18, Section 4.1
QSM Rev. 5.0, Module 6, Section 1.7.2.3 b)xi)
Are duplicates that do not meet the above requirements due
to difficulty in subsampling, described in the case narrative?
QSM Rev. 5.0, Module 6, Section 1.7.2.3 b)xi)
Replicate/Duplicate Acceptance/Rejection Criteria
Does the laboratory document the calculation for relative
percent difference or other statistical treatments?
Are the results compared to the acceptance criteria as
published in the mandated method?
8.10.7
TNI EL-V1M6-2009, Section 1.7.3.3 b)
Are the results compared to the acceptance criteria as
published in the mandated method?
8.10.8
TNI EL-V1M6-2009, Section 1.7.3.3 b)
Where there are no established criteria, does the laboratory
determine internal criteria and document the method used to
establish the limits?
8.10.9
TNI EL-V1M6-2009, Section 1.7.3.3 b)
For replicate results outside established criteria, is the
corrective action documented or the data reported with
appropriate data qualifying codes?
8.10.10
TNI EL-V1M6-2009, Section 1.7.3.3 b)
In the event of a failed replicate and any associated actions,
noted in the laboratory report to the client?
TNI EL-V1M6-2009, Section 1.7.3.3 b)
Rev. 4.3
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Revision Date: March 2017
Audit ID:
Item
Number
9.0
9.1
9.2
Laboratory:
Line of Inquiry
Reference Standards, Verification, Water Quality and
Support Equipment
Reference Standards
Does the quality control program establish and maintain
provisions for radionuclide standards?
TNI EL-V1M6-2009, Section 1.7.2.5 c)
Are reference standards that are used in a radiochemical
laboratory obtained from NIST or suppliers who participate
in supplying NIST standards or NIST traceable
radionuclides?
9.3
TNI EL-V1M6-2009, Section 1.7.2.5 c)i)
Are reference standards purchased outside the United States
traceable back to each country's national standards
laboratory?
9.4
TNI EL-V1M6-2009, Section 1.7.2.5 c)i)
Do commercial suppliers of reference standards conform to
ANSI N42.22 to assure the quality of their products?
9.5
TNI EL-V1M6-2009, Section 1.7.2.5 c)i)
Are reference standards accompanied with a certificate of
calibration and easily available for review?
9.6
9.7
TNI EL-V1M6-2009, Section 1.7.2.5 c)ii)
Does the laboratory consult with the supplier if the lab's
verification of the activity of the reference traceable
standard indicates a noticeable deviation from the certified
value?
TNI EL-V1M6-2009, Section 1.7.2.5 c)iii)
Does the laboratory use only the decay-corrected certified
value?
Rev. 4.3
Page 24 of 60
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Revision Date: March 2017
Audit ID:
Item
Number
9.8
Laboratory:
Line of Inquiry
TNI EL-V1M6-2009, Section 1.7.2.5 c)iii)
Does the laboratory have a written procedure for handling,
storing, and establishing expiration dates for reference
standards?
TNI EL-V1M6-2009, Section 1.7.2.5 c)iii)
9.9
9.10
9.11
9.12
9.13
9.14
9.15
Standards Verification
Are standards verified prior to initial use?
QSM Rev. 5.0, Module 6, Section 1.7.2.5 d)i)
Are preparations of standards solutions used for a period of
time exceeding one year verified annually, at a minimum,
and documented in a logbook?
QSM Rev. 5.0, Module 6, Section 1.7.2.5 d)i)
Are corrections for radioactive decay and/or ingrowth of
progeny performed for radionuclide standards?
QSM Rev. 5.0, Module 6, Section 1.7.2.5 d)ii)
Are a minimum of three verification measurements of a
standard used to determine the mean value and standard
deviation of the verification results?
QSM Rev. 5.0, Module 6, Section 1.7.2.5 d)i)
Is the mean value within 5% of the decay corrected certified
value?
QSM Rev. 5.0, Module 6, Section 1.7.2.5 d)i)
Does the 2-sigma value used for the 95% confidence
interval of the mean exceed 10% of the mean value of the
three verification measurements?
QSM Rev. 5.0, Module 6, Section 1.7.2.5 d)i)
If all criteria are met, the certified value shall be used.
QSM Rev. 5.0, Module 6, Section 1.7.2.5 d i)
Rev. 4.3
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Revision Date: March 2017
Audit ID:
Item
Number
9.16
Laboratory:
Line of Inquiry
Reagent and Water Quality
Is the quality of water sources monitored, documented, and
meet method specified requirements?
9.17
TNI EL-V1M6-2009, Section 1.7.2.5 b)
Does water used in the laboratory have the purity of at least
distilled or deionized water?
9.18
QSM Rev. 5.0, Module 6, Section 1.7.2.5 d)
In methods where reagent purity is not specified, are
reagents of analytical reagent grade or better?
TNI EL-V1M6-2009, Section 1.7.2.5 a)
9.19
Pipettes
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.
9.20
QSM Rev. 5.0, Section 5.5.13.1 Table
ANSI N42.23, Section 5.2.8
Weights
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, Section 5.5.13.1 Table
Rev. 4.3
Page 26 of 60
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Revision Date: March 2017
Audit ID:
Item
Number
9.21
9.22
9.23
9.24
9.25
Laboratory:
Line of Inquiry
Are daily check weighings performed using NIST-traceable
weights that bracket the range used for weighings on the
balances.
QSM Rev. 5.0, Section 5.5.13.1 Table
Are the daily checks documented in controlled logbooks?
QSM Rev. 5.0, Section 5.5.13.1 Table
Balances
Are all support equipment, including balances, calibrated or
verified at least annually, using recognized National
Metrology Institute traceable references, such as NIST,
when available, bracketing the range of use?
QSM M2, Rev. 5.0, Section 5.5.13.1(d) Table
TNI EL-V1M6-2009, Section 5.5.13.1b) and d)
Does the laboratory maintain a copy of the Certificate of
Calibration from an ISO/IEC accredited calibration
laboratory?
QSM M2, Rev. 5.0, Section 5.5.13.1 Table
TNI EL-V1M6-2009, Section 5.5.13.1b) and d)
Glassware Cleaning.
Is glassware cleaned to meet the sensitivity requirements of
the methods?
Are cleaning and storage procedures that are not specified
by the method documented in laboratory records and SOPs?
NOTE: Some applications may require single-use glassware.
TNI EL-V1M6-2009, Section 1.7.2.7 b))
Rev. 4.3
Page 27 of 60
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Revision Date: March 2017
Audit ID:
Item
Number
10.0
10.1
10.1.1
10.1.2
Laboratory:
Line of Inquiry
Instrument Operation and Calibration (General)
Initial Calibration – General
Does the laboratory assure that the test instruments
consistently operate within the specifications required of the
application for which the equipment is used?
TNI EL-V1M6-2009, Section 1.7.2.7a)
Are the nuclear counting instruments calibrated at the
following situations;
•prior to initial use,
•when the instrument is placed back into service after
major repairs and the instrument’s response has
changed as determined by a performance check, or
•when the instrument’s response exceeds predetermined
acceptance criteria for the instruments quality control?
TNI EL-V1M6-2009, Section 1.7.17a), paragraph 3
Is a specific calibration frequency specified (e.g., annually)
or is calibration based on observations from the associated
control or tolerance chart as specified in the laboratory
method SOP?
10.1.3
TNI EL-V1M6-2009, Section 1.7.1a) paragraph 4
Are calibrations performed with reference standards that
have the same general characteristics (i.e., geometry,
homogeneity, density, etc.) as the associated samples?
10.1.4
TNI EL-V1M6-2009, Section 1.7.1a) paragraph 5
Do initial calibration procedures include calculations,
acceptance criteria and associated statistics as identified in
the method SOP?
TNI EL-V1M6-2009, Section 1.7.1a)i)
Rev. 4.3
Page 28 of 60
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Revision Date: March 2017
Audit ID:
Item
Number
10.1.5
10.1.6
10.1.7
10.1.8
10.1.9
Laboratory:
Line of Inquiry
Are sufficient raw data records retained to permit
reconstruction of the initial instrument calibration (e.g.,
calibration date, method, instrument, analysis date, each
analyte name, analyst’s initials or signature; activity and
response, calibration curve or response factor; or unique
equation or coefficient used to reduce instrument responses
to activity or concentration)?
TNI EL-V1M6-2009, Section 1.7.1a)ii)
Are sample results quantitated from the initial instrument
calibration and not from any continuing instrument
calibration verification unless otherwise required by
regulation, method, or program?
TNI EL-V1M6-2009, Section 1.7.1a)iii)
Are initial instrument calibrations verified with a standard
obtained from a second manufacturer or lot, if the lot from
the manufacturer can be demonstrated as prepared
independently from other lots?
TNI EL-V1M6-2009, Section 1.7.1a)iv)
Is the detection efficiency determined with sources that are
traceable to NIST or accepted international standards, or
with sources prepared from NIST/international traceable
standards, when available?
QSM Rev. 5.0, Module 6, Section 1.7.1a)viii)
When sources used for determinations for detection
efficiency are prepared from NIST/international traceable
standards, are they defined as “working reference materials”
as defined in ASTM C1128 (current version)?
QSM Rev. 5.0, Module 6, Section 1.7.1a)viii)
Rev. 4.3
Page 29 of 60
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Revision Date: March 2017
Audit ID:
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Number
10.1.10
10.1.11
10.1.12
10.1.13
10.1.14
Laboratory:
Line of Inquiry
Are the appropriate criteria for the acceptance of an initial
instrument calibration established and appropriate to the
calibration technique employed (e.g., correlation coefficient
or relative percent difference)?
TNI EL-V1M6-2009, Section 1.7.1a)v)
If the initial instrument calibration results are outside
established acceptance criteria, are corrective actions
performed and all associated samples re-analyzed?
If reanalysis of the samples is not possible, is the data
associated with an unacceptable initial instrument
calibration reported with appropriate data qualifiers?
TNI EL-V1M6-2009, Section 1.7.1a)vi)
If a reference or mandated method does not specify the
number of calibration standards, does the laboratory have a
written procedure for determining the number of points for
establishing the initial instrument calibration?
TNI EL-V1M6-2009, Section 1.7.1a)vii)
For alpha spectrometry, is a material balance check done on
each source to clearly demonstrate accountability of all
activity by mass balance? (The material balance check
includes the fraction remaining from the neodymium
fluoride precipitation, or the electro-deposition, plus all
rinses from an adequate cleaning of any vessel used in the
process.)
QSM Rev. 5.0, Module 6, Section 1.7.1a)ix)
Is the estimated error in preparing the source propagated
into the error of the efficiency determination?
QSM Rev. 5.0, Module 6, Section 1.7.1a)ix)
Rev. 4.3
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Revision Date: March 2017
Audit ID:
Item
Number
10.1.15
Laboratory:
Line of Inquiry
Are check sources used only to verify that efficiencies have
not changed and not used to determine efficiencies?
QSM Rev. 5.0, Module 6, Section 1.7.1a)x)
10.2
10.2.1
10.2.2
10.2.3
Instrument Calibration Verification (Performance
Checks)
Are performance checks performed using appropriate check
sources and monitored with control charts or tolerance
charts to ensure that the instrument is operating properly, the
detector response has not significantly changed, and
therefore the instrument calibration has not changed?
TNI EL-V1M6-2009, Section 1.7.1b)
Is the same check source used in the preparation of the
tolerance chart or control chart at the time of calibration also
used in the calibration verification of the instrument
(performance checks)?
TNI EL-V1M6-2009, Section 1.7.1b)
Do the check sources provide adequate counting statistics
for a relatively short count time and the source is sealed or
encapsulated to prevent loss of activity and contamination of
the instrument and laboratory personnel?
10.2.4
TNI EL-V1M6-2009, Section 1.7.1b)
For gamma-ray spectroscopy systems, are performance
checks for detection efficiency, energy calibration, and peak
resolution performed on a day-of-use basis?
10.2.5
TNI EL-V1M6-2009, Section 1.7.1b)i)
For systems using sample changers and/or long count times
that run more than a day, is the energy calibration checked
before each analytical batch?
Rev. 4.3
Page 31 of 60
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Revision Date: March 2017
Audit ID:
Item
Number
10.2.6
10.2.7
10.2.8
Laboratory:
Line of Inquiry
QSM Rev. 5.0, Module 6, Section 1.7.1b)i)
Is the Full-Width-Half-Maximum (FWHM) resolution of
the alpha or gamma detector evaluated prior to instrument
use and following repair or loss of control (MARLAP
18.5.6.2)?
QSM Rev. 5.0, Module 6, Section 1.7.1b)i)
Is the measured FWHM resolution trended?
QSM Rev. 5.0, Module 6, Section 1.7.1b)i)
Are detector response (counting efficiency) determinations
performed when the check source count is outside the
acceptable limits of the control chart (reference ANSI
N42.23, Annex A5)?
10.2.9
QSM Rev. 5.0, Module 6, Section 1.7.1b)i)
Are calibration or QC sources used that will not cause
detector contamination from recoil atoms from the source?
10.2.10
QSM Rev. 5.0, Module 6, Section 1.7.1b)i)
For radon scintillation detectors, is the efficiency verified at
least monthly, when the system is in use?
10.2.11
QSM Rev. 5.0, Module 6, Section 1.7.1b)i)
For alpha-particle spectroscopy systems, is the performance
check for energy calibration performed on a weekly basis?
10.2.12
TNI EL-V1M6-2009, Section 1.7.1b)ii)
For alpha-particle spectroscopy systems, is the performance
check for detection efficiency performed on at least a
monthly basis?
10.2.13
TNI EL-V1M6-2009, Section 1.7.1b)ii)
For gas-proportional counters (GFPC), liquid scintillation
counters (LSC) and other scintillation counters, are the
Rev. 4.3
Page 32 of 60
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performance checks for detection efficiency performed on a
day-of-use basis?
10.2.14
TNI EL-V1M6-2009, Section 1.7.1b)iii)
For batches of GFPC and LSC samples that uninterruptedly
count for more than a day, are performance checks
performed at the beginning and end of the batch as long as
this time interval is no greater than one week?
TNI EL-V1M6-2009, Section 1.7.1b)iii)
10.3
10.3.1
Background Measurement
Are background measurements made on a regular basis and
monitored using control charts or tolerance charts to ensure
that a laboratory maintains its capability to meet required
measurement quality objectives?
10.3.2
TNI EL-V1M6-2009, Section 1.7.1c)
Are these values subtracted from the total measured activity
in the determination of the sample activity?
10.3.3
TNI EL-V1M6-2009, Section 1.7.1c)
For alpha-particle and gamma-ray spectroscopy systems, are
long background measurements (to be used for background
corrections) performed on at least a monthly basis?
10.3.4
QSM Rev. 5.0 Module 6, Section 1.7.1c)i)and ii)
TNI EL-V1M6-2009, Section 1.7.1c)i) and ii)
Is the duration of the background measurement sufficient to
quantify contamination that may affect routine sample
measurements (the count time for the background
measurement shall be at least as long as the sample count
time.)?
QSM Rev. 5.0, Module 6, Section 1.7.1c)i)and ii)
Rev. 4.3
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10.3.5
TNI EL-V1M6-2009, Section 1.7.1 c)i) and ii)
For gas-proportional counters, are long background
measurements (to be used for background corrections)
performed on a monthly basis, at minimum.
10.3.6
QSM Rev. 5.0, Module 6, Section 1.7.1c)iii)
For scintillation counters, are background measurements
performed each day of use?
10.3.7
TNI EL-V1M6-2009, Section 1.7.1 c)iv)
Are Background Subtraction Count (BSC) measurements
conducted after calibration and monthly thereafter?
10.3.8
QSM Rev. 5.0, Module 6, Section 1.7.1c)
Are BSC measurements monitored for trends to ensure that
a laboratory maintains its capability to meet required project
objectives?
10.3.9
QSM Rev. 5.0, Module 6, Section 1.7.1c)
Are successive long background measurements evaluated as
background check measurements?
10.3.10
10.3.11
QSM Rev. 5.0, Module 6, Section 1.7.1c)
Is the duration of the background check measurements of
sufficient duration (i.e., at least as long as the sample count
time) to quantify contamination that may impact routine
sample measurements?
QSM Rev. 5.0, Module 6, Section 1.7.1c)
If the background check is conducted less frequently than
daily, are any associated sample results released for use
prior to a making a (bracketing) background check meeting
all acceptance criteria?
QSM Rev. 5.0, Module 6, Section 1.7.1c)
Rev. 4.3
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10.3.12
Laboratory:
Line of Inquiry
Are background checks being collected before and after any
counting chamber changes are made (i.e., cleaning, liner
replacement, or instrument modification)?
10.3.13
QSM Rev. 5.0, Module 6, Section 1.7.1c)
For alpha spectroscopy systems, are monthly background
determinations performed for each Region of Interest
(ROI)?
10.3.14
QSM Rev. 5.0, Module 6, Section 1.7.1c)ii)
Are backgrounds for alpha spectrometers rechecked after
being subjected to high-activity samples?
10.3.15
QSM Rev. 5.0, Module 6, Section 1.7.1c)ii)
Are procedures in place to define high activity and counting
procedures to check for gross contamination from high
activity samples?
10.3.16
QSM Rev. 5.0, Module 6, Section 1.7.1c)ii)
Are backgrounds for gas flow proportional counters
rechecked after being subjected to high-activity samples?
10.3.17
QSM Rev. 5.0, Module 6, Section 1.7.1c)iii)
For scintillation counters, is the duration of the background
measurement sufficient to quantify contamination that may
affect routine sample measurements?
10.3.18
QSM Rev. 5.0, Module 6, Section 1.7.1c)iv)
Does the daily instrument check for LSC include a check with
an unquenched, sealed background vial (which should never
be used to correct sample results for background
measurements, since it is not in the same configuration as
samples)?
QSM Rev. 5.0, Module 6, Section 1.7.1c)iv)
Rev. 4.3
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11.0
Isotopic Determinations by Alpha Spectrometry
11.1
Tracer:
Are tracers used for isotope specific analysis by alpha
spectrometry?
11.2
QSM Rev. 5.0, Module 6, Section 1.8.1a)
Have all tracers used for alpha spectrometry been tested by
the laboratory for contribution in the ROIs of the analytes
of interest?
11.3
QSM Rev. 5.0, Module 6, Section 1.8.1a)
If a significant contribution is found, is the method for
correction accepted by the site prior to use?
11.4
11.5
11.6
QSM Rev. 5.0, Module 6, Section 1.8.1a)
Background Correction:
Are the gross counts in each target analyte and tracer ROI
corrected for the particular detector’s background
contribution in those same ROIs?
QSM Rev. 5.0, Module 6, Section 1.8.1b)
Blank Correction:
Blank correction is not performed, except where noted.
QSM Rev. 5.0, Module 6, Section 1.8.1c)
Conditions Requiring Reanalysis:
Does the laboratory consider the following conditions as
requirements for reanalysis of a particular sample and
analyte:
1. If the tracer recovery for the sample does not fall
within 30% - 110%, or
Rev. 4.3
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2. If the FWHM for the tracer peak exceeds 100 keV
and/or the peak energy does not fall within ± 50 keV
of the known peak energy, or
3. If the target analyte and tracer peaks are not resolved
because the target analyte activity is significantly
larger than the tracer activity, or
4. If the sample analyte spectrum contains significant
interferences with the analyte and/or tracer ROIs,
reanalysis is required?
11.7
11.8
11.9
QSM Rev. 5.0, Module 6, Section 1.8.1d)
Analytical Batch Conditions: If the tracer chemical
recovery for the Method Blank does not fall within 30% 110%, will reanalysis of the entire Analytical Batch,
beginning with the preparation be required if sufficient
sample is available?
QSM Rev. 5.0, Module 6, Section 1.8.1d)
Instrument Calibration:
Does the calibration of each alpha spectrometry detector
used to produce data include channel vs. energy
calibration?
QSM Rev. 5.0, Module 6, Section 1.8.1e)
Efficiency
Does the laboratory make efficiency and background
determinations for each alpha spectrum region of interest
(ROI)?
QSM Rev. 5.0, Module 6, Section 1.8.1f)
Rev. 4.3
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11.10
Laboratory:
Line of Inquiry
Energy Calibration:
 Is an energy calibration performed for each alpha
detector?
 Is a curve fit for Energy (Y-axis) versus Channel (Xaxis) and the equation with the slope and Y-intercept for
the fit documented?
 Is the slope of the equation <15 keV/channel?
 Is the energy calibration performed using at least three
isotopes within the energy range of 3 to 6 MeV?
 Are the final peak energy positions of all observed
isotopes within ±50 keV of the expected peak energy?
11.11
11.12
QSM Rev. 5.0, Module 6, Section 1.8.1g)
Background Requirements:
 Are the background total counts (or counts per unit
time) for each target analyte and tracer isotope ROI
analyzed on each detector and documented?
 Is the background for each ROI sufficiently low to
ensure that required detection limits are met?
 Are the limits of acceptability for each background ROI
documented and set such that RLs can be obtained for
backgrounds at the limit of acceptability?
 Are background count times equal to or longer than
sample count times?
QSM Rev. 5.0, Module 6, Section 1.8.1h)
Detector Efficiency (Response) Determination
Requirements
Rev. 4.3
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 Are the efficiency counts for the ROI background
corrected using the same ROI for the background unless
the background is less than 0.5% of the total counts in
the ROI?
 Is the efficiency determined on at least 3,000 net counts
in the ROI (after background correction)?
 Are check source counts used to verify detector
efficiency determined on at least 2,000 counts?
 Are the detector efficiency and detector efficiency error
documented?
 Is the detector efficiency check as determined by the
check source and/or pulsar count and the associated
error and limits of acceptability for the check source
result documented?
11.13
QSM Rev. 5.0, Module 6, Section 1.8.1i)
Spectrum Assessment:
 Are ROIs clearly indicated either graphically or in
tabular form on alpha printouts?
 Are spectra with ROIs saved and made available for
review upon request?
 Is the FWHM resolution for each sample and QC
sample tracer peak ≤100 keV?
 Is the tracer peak energy for each sample and QC
sample within ±50 keV of the expected energy?
 Is each sample and QC sample spectrum assessed for
correctly chosen ROIs, acceptable spectral resolution,
acceptable energy calibration and interferences with the
analyte and tracer ROIs?
QSM Rev. 5.0, Module 6, Section 1.8.1j)
Rev. 4.3
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12.0
12.1
12.2
Laboratory:
Line of Inquiry
Gas Flow Proportional Counting
Planchets:
 Are planchets being thoroughly cleaned before use to
ensure that there are no interfering residues or
contamination?
 Are all planchets being prepared so as not to exceed
sample weights in excess of the calibrated ranges of
established self-absorption curves?
 Are sample weights being documented and stable
prior to counting?
 Planchets that exhibit physical characteristics notably
different from the self-absorption standards (e.g.,
evidence of corrosion) are not being counted unless
remediation efforts such as additional sample
preparation and remounting or flaming prove
unsuccessful?
 Are all non-routine counting situations being
documented in the case narrative?
QSM Rev. 5.0, Module 6, Section 1.8.4a)
Instrument Calibration:
a) Is instrument calibration being performed in
accordance with the requirements in ANSI N42.25
(current version), Calibration and Usage of
Alpha/Beta Proportional Counters unless otherwise
defined in the QSM or as documented by the
laboratory?
b) Have deviations or changes from the standard been
provided to clients as necessary for acceptance?
c) Are method references for the current version of the
standard?
Rev. 4.3
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d) When references are updated, is an implementation
schedule determined by the lab?
12.3
QSM Rev. 5.0, Module 6, Section 1.8.4b;Errata Reference
1.8.4
Are the calibration sources so radioactive as to cause pulse
pileups or dead time that is significantly different from that
to be expected from routine analyses?
12.4
QSM Rev. 5.0, Module 6, Section 1.8.4b)
Is the geometry of the calibration sources used for efficiency
and self-absorption/crosstalk curves the same as that of the
prepared sample and QC sample planchets?
12.5
QSM Rev. 5.0, Module 6, Section 1.8.4b)
Is the depth, diameter and shape (flat, flanged, ringed, etc.)
of the planchets used for calibration sources, the same as for
samples?
12.6
QSM Rev. 5.0, Module 6, Section 1.8.4b)
Are the sources used for the determination of self-absorption
and cross talk of similar isotope content to that of the
analytical samples?
NOTE: Am-241; Po-210; or Th-230 shall be used for
alpha and Cs-137 or Sr-90/Y-90 for beta.
12.7
QSM Rev. 5.0, Module 6, Section 1.8.4b)
Self-Absorption and Crosstalk Curves:
 Are self-absorption curves generated for both alpha and
beta counting?
 Is a crosstalk curve established for alpha to beta crosstalk
versus residue weight?
Rev. 4.3
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 Does the data used to generate self-absorption and
crosstalk curves consist of at least seven points, well
distributed throughout the mass range?
 Is each alpha and beta calibration standard counted to an
accumulation of at least 10,000 counts minimum for the
initial calibration and 5,000 counts minimum for the
calibration verification?
 Are new cross-talk curves measured prior to initial use,
after loss of control, and upon incorporation of new or
changed instrument settings? (MARLAP 18.5.6.1).
12.8
QSM Rev. 5.0, Module 6, Section 1.8.4d)
Check Source Requirements:
 Are the alpha and beta response and corresponding
crosstalk of each detector used to count analytical
samples or QC samples checked daily with separate
alpha and beta emitting sources?
 When performing analyses with extended count times,
are check source measurements performed between
sample sets?
 Following gas bottle changes, are check sources and
backgrounds analyzed before samples are counted?
 Is check source data documented and retained?
QSM Rev. 5.0, Module 6, Section 1.8.4e)
Rev. 4.3
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13.0
13.1
Laboratory:
Line of Inquiry
Gamma Spectrometry
Sample Counting Requirements:
a) Do the SOPs for sample analysis by gamma
spectrometry incorporate and adhere to ANSI N42.14
(current version), Calibration and Use of Germanium
Spectrometers for the Measurement of Gamma Ray
Emission Rate of Radionuclides, and/or ANSI N42.12
(current version), Calibration and Usage of ThalliumActivated Sodium Iodide Detector Systems for Assay
of Radionuclides unless otherwise defined in the QSM
or as documented by the laboratory?
b) Have deviations or changes from the standard been
provided to clients as necessary for acceptance?
c) Do the references reflect the current version of the
documents?
d) When references change, is an implementation
schedule determined?
13.2
QSM Rev. 5.0, Module 6, Section 1.8.5ai);Errata Reference
1.8.5
Does the laboratory use Ge detectors of either intrinsic
(pure) germanium or lithium drifted germanium for gamma
spectroscopy?
13.3
QSM Rev. 5.0, Module 6, Section 1.8.5a)ii)
Does the laboratory use sodium iodide detectors for gamma
counting?
QSM Rev. 5.0, Module 6, Section 1.8.5a)ii)
Rev. 4.3
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13.4
13.5
Laboratory:
Line of Inquiry
Are the detectors calibrated for the specific geometry and
matrix considerations used in the sample analysis?
QSM Rev. 5.0, Module 6, Section 1.8.5a)iii)
Does the laboratory have the capability to seal soil samples in
airtight cans or equivalent in order to allow ingrowth of radon
for accurate analysis of Ra-226 or its progeny by gamma
spectroscopy when requested?
13.6
QSM Rev. 5.0, Module 6, Section 1.8.5a)iii))
Does the laboratory identify and document the spectral data
reference used for the half-life, abundance, and peak energy of
all nuclides used in its gamma spectral libraries?
13.7
QSM Rev. 5.0, Module 6, Section 1.8.5a)iv)
Does the laboratory document, review, and provide
configuration control for gamma spectrometry libraries?
13.8
13.9
QSM Rev. 5.0, Module 6, Section 1.8.5a)iv)
Are the assumptions made for libraries (i.e., half-lives based
on supported/unsupported assumptions, inferential
determinations (e.g., Th-234 = U-238 because supported))
documented and narrated?
QSM Rev. 5.0, Module 6, Section 1.8.5a)iv)
Efficiency Calibration Requirements:
i) ) Is each gamma spectrometry system efficiency
calibrated for each sample geometry and matrix, with
NIST traceable or accepted international standards or
prepared from NIST/international traceable sources?
1) Germanium Detectors:
Are the efficiency calibration measurements made with
at least six peaks which cover the typical energy range
of approximately 0.059 to 2 MeV?
Rev. 4.3
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13.9
cont’d
Laboratory:
Line of Inquiry
During calibration, are at least 10,000 net counts (total
counts minus the Compton continuum and ambient
background) accumulated in each full-energy gammaray peak of interest used for the efficiency equation?
2) Sodium Iodide (NaI) Detectors:
Are the efficiencies determined when there is a change
in resolution, geometry, or system configuration?
QSM Rev. 5.0, Module 6, Section 1.8.5b);Errata Reference
ii) Does the laboratory use software that does not require a
physical calibration standard to obtain efficiencies for various
matrices and geometries (where a standard calibration source
of known matrix and geometry cannot be specified, ie, waste
or debris)?
When such software is used, does the laboratory supply
detailed information and documentation regarding the
selection of parameters used to specify the efficiency
calibration and sample models?
When selected for analysis using this type of calibration, does
each sample have a unique set of model parameters associated
with it?
When such models are used, is the model closest to the actual
sample selected?
13.10
Is the model selected for each sample presented in the case
narrative and includes a discussion of actual and predicted
peak ratios for isotopes with multiple gamma energies present
in the sample?
QSM Rev. 5.0, Module 6, Section 1.8.5a)ii); Errata Reference
Energy Calibration Requirements:
Rev. 4.3
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Each gamma spectrometry system shall be energy
calibrated with NIST/international traceable standards or
prepared from NIST/international traceable sources.
i) Germanium Detectors:
Are the energy calibration measurements made using at
least six peaks which cover the energy range from 0.059 to
approximately 2 MeV?
ii) Are at least 10,000 net counts (total counts minus the
Compton continuum and ambient background)
accumulated in each full-energy gamma-ray peak of
interest?
iii) Is the energy calibration linear and accurate to 0.5 keV?
Performance Evaluation:
Germanium Detectors:
Are performance tests performed on a regularly scheduled
basis and in accordance with the user manual instructions?
Sodium Iodide Detectors:
Are performance tests performed on a regularly scheduled
basis and in accordance with the user manual instructions?
Spectrum Assessment:
Are each sample and QC sample spectrum assessed for
acceptability of key peak width and shape, and interference
due to superimposed peaks or other sources?
Are all major contributors to the spectrum that are noted as
unidentified peaks discussed in the case narrative?
QSM Rev. 5.0, Module 6, Section 1.8.5c), d) and e); Errata
Reference
Rev. 4.3
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14.0
14.1
14.2
14.3
Laboratory:
Line of Inquiry
Liquid Scintillation Counting
Tritium in Water:
• Are water samples for tritium analysis and all associated
QC samples distilled prior to analysis unless specified
otherwise by the client?
• Does the applicable preparation SOP specify the fraction to
be collected and is the same fraction collected for samples
and all associated QC samples?
QSM Rev. 5.0, Module 6, Section 1.8.3a)
Counting Vial Preparation:
• Are samples counted in vials equivalent to or superior to
low potassium glass vials or high density polyethylene
vials?
• Are scintillation vials “dark adapted” for a minimum of 30
minutes or according to the cocktail manufacturer’s
specifications before counting?
• Are the prepared vials inspected to verify that the sample
loaded properly in the cocktail?
QSM Rev. 5.0, Module 6, Section 1.8.3b)
SOPs
a) Do laboratory SOPs for methods using liquid
scintillation counting incorporate and adhere to ANSI
N42.15 (current version), American National Standard
Check Sources for and Verification of Liquid
Scintillation Systems unless otherwise defined in the
QSM or as documented by the laboratory?
b) Have deviations or changes from the standard been
provided to clients as necessary for acceptance?
c) Are method references for the current version of the
standard?
Rev. 4.3
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Number
14.4
14.5
Laboratory:
Line of Inquiry
d) When references are updated, is an implementation
schedule determined by the lab?
QSM Rev. 5.0, Module 6, Section 1.8.3c; Errata Reference
1.8.3
Instrument Background:
• Has the instrument background vial for all tritium
matrices been prepared with low-tritium or “dead”
water?
• Has the instrument background vial been prepared
with the same water to cocktail ratio as the samples
are prepared?
• Has the type of water used to prepare the instrument
background vial been explicitly noted on the
preparation and counting documentation?
• Is an instrument background run with each sample
batch?
• Unless calculated from a running average of
background counts or a background quench curve, is
the most recent background count being used to
calculate sample activities and MDAs?
• Is the effect of quench on background evaluated and
corrected using a background quench curve if it is
significant?
QSM Rev. 5.0, Module 6, Section 1.8.3d)
Quench Curves:
For analysis methods using quench curves to determine
individual sample detection efficiency or background,
are the quench curves generated at least yearly and
verified after any instrument maintenance?
QSM Rev. 5.0, Module 6, Section 1.8.3e)
Rev. 4.3
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14.6
14.7
14.8
Laboratory:
Line of Inquiry
Constant Quench
If the calibration method is constant quench, is the
detection efficiency checked at least weekly when in
use or with each counting batch?
QSM Rev. 5.0, Module 6, Section 1.8.3f)
Sample-Specific Conditions:
Are the following conditions that require reanalysis for a
particular sample and analyte, beginning with the
preparation or recounting, as appropriate being
followed?.
i) If the constant quench method of calibration is used,
the quench of each sample analyzed shall fall within
+/-5% relative to the average efficiency at that
quench level. If this condition is not met, the sample
must be reanalyzed beginning with vial preparation.
ii) If the sample quench does not fall within the range of
the quench curve, the samples shall be reanalyzed
such that the sample quench is in the range of a
quench curve.
QSM Rev. 5.0, Module 6, Section 1.8.3g)
Spectrum Assessment:
Are the following guidelines being followed for analytes
requiring separations other than distillation?
i) Sample spectra shall be retained (electronic or
hardcopy) for each sample and QC sample including
identification of ROIs.
ii) Each sample and QC sample spectrum shall be
assessed for correctly chosen ROIs, acceptability of
peak shape, and interferences due to non-target
analytes or luminescence.
Rev. 4.3
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QSM Rev. 5.0, Module 6, Section 1.8.3h)
Rev. 4.3
Page 50 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
15.0
15.1
Laboratory:
Line of Inquiry
Radon Scintillation (Lucas Cell)
SOPS
a) Do the procedures for sample analyses by Lucas Cell
incorporate and adhere to ASTM D3454 (current
version), Standard Test Method for Radium-226 in
Water unless otherwise defined in the QSM or as
documented by the laboratory?
b) Have deviations or changes from the standard been
provided to clients as necessary for acceptance?
c) Are method references for the current version of the
standard?
d) When references are updated, is an implementation
schedule determined by the lab?
15.2
15.3
QSM, Rev. 5.0, Module 6, Section 1.8.2a;
Errata Reference 1.8.2
Is the operating voltage plateau slope for the detector
<2%/100V?
QSM Rev. 5.0, Module 6, Section 1.8.2b)
Are new Lucas Cells calibrated every month for the first six
months of use and then annually after the initial six months
of use?
15.4
QSM Rev. 5.0, Module 6, Section 1.8.2c)
Are background measurements for quantitation in each cell
carried out prior to each sample measurement?
15.5
QSM Rev. 5.0, Module 6, Section 1.8.2d)
When consistent with MQO, Are Rn-222 ingrowth times
shortened to the degree permitted by EPA Method 903.1?
QSM Rev. 5.0,Module 6, Section 1.8.2a)
Rev. 4.3
Page 51 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
16.0
16.1
16.2
16.3
Laboratory:
Line of Inquiry
Conditions Requiring Reanalysis or Recount
If reanalysis is not possible, is the client contacted for specific
guidance or requirements?
General Conditions:
i) If the RLs could not be achieved because of laboratory
errors or oversights such as inadequate count times,
inadequate aliquot size, inappropriate dilution, low
detector efficiencies, high detector backgrounds, etc.,
then is the sample reanalyzed under more optimal
conditions?
ii) If the RLs could not be achieved because of problems
associated with the sample such as inadequate sample
provided, elevated radioactivity levels, sample matrix
interferences such as high amounts of suspended solids,
multiphase liquids, etc., then are such problems
explained in the case narrative?
QSM Rev. 5.0, Module 6, Section 1.8.6a)
Sample and Analyte-Specific Conditions:
Does the laboratory document conditions that require
reanalysis for a particular sample and analyte, such as;
i) If, for any reason, sample or batch QC integrity
becomes suspect (e.g., spillage, mis-identification,
cross-contamination), all potentially affected samples
shall be reanalyzed from a point before that at which the
integrity came into question. If new batch QC must be
prepared for reanalysis, samples for reanalysis shall be
restarted at the normal point of initiation for the batch
QC.
ii) All samples associated with expired standards.
QSM Rev. 5.0, Module 6, Section 1.8.6b)
Analytical Batch Conditions:
Rev. 4.3
Page 52 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Laboratory:
Item
Number
Line of Inquiry
Status
QSM Rev. 5.0, Module 6, Section 1.8.6c)
Conditions Requiring a Re-count:
If the RL was not achieved due to inadequate count
duration, low detector efficiencies, or high detector
backgrounds, is the sample re-counted under more optimal
conditions, and are the reasons for the re-count
documented in the case narrative?
QSM Rev. 5.0, Module 6, Section 1.8.6d)
Appendix A
The following general equations are derived from the work of
L. A. Curie being used to calculate the MDA.
i) With a Blank Population:
MDA 
3.29 * sb
3

KTS
KTS
K = detector efficiency * e -ƛt * aliquot fraction * tracer
recovery*Yield
TS = count time of the sample in minutes
sb= standard deviation of the blank population where
the blank population is in net blank counts in count
time TS
ii) Without a Blank Population:
Page 53 of 60
Auditor:
Except where noted otherwise, does the laboratory require
reanalysis of the entire analytical batch, beginning with the
preparation for batches that failed the Method Blank or
LCS criteria?
16.4
Rev. 4.3
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Laboratory:
Item
Number
Line of Inquiry
MDA for samples without a blank population can be
determined if based on appropriate Curie or MARLAP
calculations, such as:
3.29 *
MDA 
b
b

TS TB
K

3
K * TS
Where:
K = detector efficiency * e -ƛt * aliquot fraction * tracer
Recovery*Yield
TS = count time of the sample in minutes
TB = count time of the background in minutes
b = background count rate in cpm
The above equation is used when sample and
background count times are different.
QSM Rev. 5.0, Module 6, Section 1.5.2.1.1
The Decision Level (DL) can either be based on the Combined
Standard Uncertainty (CSU) of the blank (preparation or
method), or the standard deviation determined from a set of
appropriate blanks.
Decision Level (DL): The DL is sometimes called the critical
level (Lc) or critical value (MARLAP). Is the following
general equation being used to calculate the decision level?
DL 
(t  S B )  RB
E  R  IDF  W
Where:
DL = the decision level in disintegrations per minute
per unit volume or weight (dpm/unit);
Rev. 4.3
Page 54 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Item
Number
Laboratory:
Line of Inquiry
SB = the standard deviation of a set of appropriate blank
net count rate after background subtraction for blanks
counted for the same length of time as the sample;
RB = the average blank count rate in counts per minute
(cpm);
t = the student t factor for appropriate degrees of
freedom and confidence level;
E = the fractional detector efficiency (c/d) for the
sample;
R = the fractional chemical yield for the sample;
IDF = the ingrowth or decay factor for the sample; and
W = the weight or volume of the sample.
DLs are used as the default detection threshold. Alternatively,
the client may use/specify detection thresholds that meet
project/site-specific requirements.
QSM Rev. 5.0, Module 6, Section 1.5.2.1.2
Rev. 4.3
Page 55 of 60
Auditor:
Status
Facility Response/Comments
Status
Summary of Observations/Objective
Evidence
Reviewed Audit Notes
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Laboratory:
Rev. 4.3
Page 56 of 60
Auditor:
References cited in this checklist:
ANSI N42.12-1994, American National Standard Calibration and Usage of Thallium-Activated Sodium Iodide Detector Systems for Assay of Radionuclides.
ANSI N42.14-1999, American National Standard for Calibration and Use of Germanium Spectrometers for the Measurement of Gamma-Ray Emission Rates of
Radionuclides.
ANSI N42.15,-1997 American National Check Sources for and Verification of Liquid-Scintillation Counting Systems.
ANSI N42.23-1996, American National Standard Measurement and Associated Instrumentation Quality Assurance for Radioassay Laboratories.
ANSI N42.25-1997, American National Standard Calibration and Usage of Alpha/Beta Proportional Counters.
ASTM D 5174 – 97, American Society for Testing and Materials, Standard Test Method for Trace Uranium in Water by Pulsed-Laser Phosphorimetry.
U.S. Department of Energy, 2006, US DOE Quality Systems for Analytical Services (QSAS), Revision 2.2.
Multi-Agency Radiological Laboratory Analytical Protocols (MARLAP) Manual, NUREG-1576, EPA 402-B-04-001A, July 2004.
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Notes:
Laboratory:
Rev. 4.3
Auditor:
Page 57 of 60
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Notes:
Laboratory:
Rev. 4.3
Auditor:
Page 58 of 60
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Laboratory:
Rev. 4.3
Page 59 of 60
Auditor:
Record of Revision for Checklist 4
Data Quality for Radiochemical Analyses
Revision
Number
3.5
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
Effective
Date
11/2009
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
11/2010
3.7
11/2011
3.8
1/2012
4.0
4.1
12/2013
3/2014
Reason for
Revision
Added - Data analysis software may also be used for the statistical evaluation of data for trends and biases.
Revised wording for counting uncertainty and QSAS reference
Changed QSAS reference for reporting negative activities
Changed QSAS reference for reporting negative activities
Changed QSAS reference for NDA
Changed QSAS reference for NDA
Added requirements for a radiological control program
Replaced PE with the term PT
Added requirements for the use of PT samples
Changed QSAS reference for standards and reference materials
Changed QSAS reference for standards
Changed QSAS reference for expiration dates
Changed QSAS reference for verification of standards
Changed QSAS reference for ROIs
Changed QSAS reference for efficiency determination
Changed QSAS reference for resolution of tracer peaks
Changed QSAS reference for background measurement for counting chamber changes
Changed QSAS reference
Changed QSAS reference for net counts for efficiency equation
Changed QSAS reference for gamma-ray spectra
Added requirements for effects of quench on background
Added the following to the Note section of the checklist: Fully document any deviation from the
LOI or the requirements of QSAS 2.7
Added the following to the Note section of the checklist: Fully document any deviation from the
LOI or the requirements of QSAS 2.8
Revised to incorporate QSM Rev. 5.0, TNI ELV1M1, ISO/IEC 17025
Deletion of quarterly accuracy checks for mechanical pipettes
Line of
Inquiry
14.12
1.4
3.1
3.2
4.1
4.2
5.5
Entire Doc.
6.2
9.1
9.6
9.7
9.8
11.4
11.5
11.6
13.6
13.7
13.10
13.14
14.5
Page 1
Page 1
All
9.19
U.S. Department of Energy Consolidated Audit Program
DOECAP Checklist: 4
Data Quality for Radiochemistry Analyses
Revision Date: March 2017
Audit ID:
Revision
Number
4.2
4.2
4.2
4.2
4.2
4.2
4.2
4.2
4.2
4.2
4.2
4.3
Laboratory:
Effective
Date
10/2015
10/2015
10/2015
10/2015
10/2015
10/2015
10/2015
10/2015
10/2015
10/2015
10/2015
3/2017
Rev. 4.3
Page 60 of 60
Auditor:
Reason for
Revision
Added link to the DOECAP website
Added reference to the QSM Errata Document for interim changes
Deleted LOI 1.1 and renumbered LOIs through 1.14
Removed indirect yield monitoring from Section 2.0 header
Remove indirect to carrier and revised reference to 1.7.2.3 d)
Revised text to remove dates from ANSI standards and other changes
Revised text to remove dates from ANSI standards and other changes
Revised efficiency calibration requirements for gamma spec
Revised requirements for gamma spec
Revised text to remove dates from ANSI standards and other changes for liquid scintillation
Revised text to remove dates from ANSI standards and other changes for sample analysis by Lucas Cell
Removal of Official Use Only
Line of
Inquiry
Page 1
Page 1
1.1 – 1.14
Section 2.0
2.9
12.2
13.1
13.9
13.10
14.3
15.1