National Analytical Management Programrmccnetwork.net/sites/default/files/files/Checklist 4 Rad - … · Web view Reanalysis/Recount Performance Testing (PT) Programs A = Acceptable

U.S. Department of Energy

Consolidated Audit ProgramChecklist 4

Data Quality for Radiochemistry AnalysesDoD/DOE QSM - Revision 5.0

Checklist Revision 4.1March 2014

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

OFFICIAL USE ONLYMay be exempt from public release under the Freedom of Information Act(5 U.S.C 552), exemption number and category: Exemption #4: Commercial Proprietary Department of Energy review required before public releaseName/Org: TBD Date: TBD Guidance (if applicable) Memo dated October 30, 2008 from Charles B. Lewis III to Larry Kelly, DM No 419069

Audit ID: Date:

Areas of Review During Audit__ SOPs

__ Yield Monitors

__ Sample Handling

__ Batch Quality Control (QC)

__ Gas Flow Proportional Counting

__ Gamma Spectroscopy

__ Negative Activities

__ MDA and DL

__ Contamination Control

__ Reagents, Standards and Water Quality

__ Instrument Operation and Calibration

__ Alpha Spectroscopy

__ Liquid Scintillation Counting

__ Radon (Lucas Cell)

__ Reanalysis/Recount

__ Performance Testing (PT) Programs

A = AcceptableNO = Not Observed

U = UnsatisfactoryF = Finding

NA = Not ApplicableO = Observation

Referenced regulations are accessible at the following URLs:

https://doecap.oro.doe.gov/

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 all deviation from the LOI or the requirements of QSM Rev. 5.0 and TNI ELV1M6 Refer to Page 67 for the record of revision.

Item Number Line of Inquiry Status Summary of Observations/Objective Evidence

Reviewed Audit Notes1.0 Standard Operating Procedures (SOPs)1.1 Are the methods employed by the laboratory capable of producing data that

meet the minimum method QA/QC requirements (see Tables 16-19 of the QSM Rev. 5.0 for specific requirements)? TNI-EL-V1M6-2009, Section 1.4

1.2 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

1.3 Have non-standardized methods that have been developed by the laboratory been appropriately documented before use? TNI-EL-V1M6-2009, Section 1.4

1.4 Are all procedures being used by the laboratory documented?

TNI-EL-V1M6-2009, Section 1.5.21.5 Does the documentation include the quality system matrix type?

TNI-EL-V1M6-2009, Section 1.5.21.6 Is all supporting data retained by the laboratory?

TNI-EL-V1M6-2009, Section 1.5.21.7 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 1.5.11.8 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 1.5.11.9 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-EL-V1M6-2009, Sections 1.5.2 – 1.5.5.)

TNI-EL-V1M6-2009, Section 1.5.1


Reviewed Audit Notes1.10 Where modifications to the published method have been made, changes are

clearly described and documented.

TNI-EL-V1M6-2009, Section 1.5.11.11 Do the laboratory SOPs document the formulas for calculating the Combined

Standard Uncertainty (CSU) of a result, including both systematic and random error?

QSM Rev. 5.0, Module 6, Section 1.5.4TNI-EL-V1M6-2009, Section 1.5.4ANSI N42.23, Sections 4.1.3.2 and A8

1.12 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 1.5.4ANSI N42.23, Sections 4.1.3.2 and A8

1.13 Are the results reported with the associated measurement uncertainty as a combined standard uncertainty (CSU)?

QSM Rev. 5.0, Module 6, Section 1.5.4ANSI N42.23, Sections 4.1.3.2 and A8

1.14 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 1.5.41.15 Do the laboratory SOPs specify acceptance criteria for QC samples?

QSM Rev. 5.0, Module 6, Section 1.5.42.0 Internal Tracers and Carriers (Indirect Yield Monitors)2.1 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)

2.2 For those methods that employ a tracer or carrier for yield determination, does each sample result have an associated yield calculated and reported?



Reviewed Audit Notes2.3 Is the tracer or carrier yield assessed against the specific acceptance criteria

specified in the laboratory method SOP?


2.4 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)2.5 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

2.6 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 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 Is the technique used for the indirect yield measurements sufficient to maintain relative uncertainties associated with the yield correction below 10% at the 2-sigma level?



Reviewed Audit Notes2.10 Is the uncertainty associated with chemical yield corrections incorporated

into the CSU of the associated sample results?


2.11 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?


2.12 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?

QSM Rev. 5.0, Module 6, Section 1.7.2.3 c) and d)2.13 When the specified yield acceptance criteria are not met, are the specified

corrective actions and contingencies followed?

TNI-EL-V1M6-2009, Section 1.7.2.3 c) and d)2.14 Are the procedures for data reduction, such as use of linear regression,

documented?

TNI-EL-V1M6-2009, Section 1.7.2.4 a)2.15 Is each analytical result with its measurement uncertainty documented in a

report that clearly explains the uncertainty?

TNI-EL-V1M6-2009, Section 1.7.2.4 b)2.16 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)3.0 Negative Activities3.1 All negative activities are reported as such.

QSM Rev. 5.0, Module 6, Section 1.7.2.4 d)


Reviewed Audit Notes3.2 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

4.0 Minimum Detectable Activity (MDA) and Decision Level (DL) Determination4.1 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

4.2 Are all sample-processing steps of the analytical method included in the determination of the MDA?

TNI-EL-V1M6-2009, Section 1.5.2.1a)ANSI N42.23, Section A8

4.3 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)4.4 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)4.5 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)4.6 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)


Reviewed Audit Notes4.7 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)4.8 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)

4.9 Otherwise, is the equation for the MDA appropriately modified to account for the difference in sample and background count times?


4.10 Has the implementation of blank populations for calculation of MDAs been documented and described in detail in a SOP?


4.11 The equations for MDA have the units of dpm/sample. If other units are used, is the appropriate conversion documented in the SOPs?


4.12 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)4.13 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)4.14 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)5.0 Contamination and Cross-Contamination Control


Reviewed Audit Notes5.1 Does the laboratory maintain a radiological control program that addresses

analytical radiological control?

TNI-EL-V1M6-2009, Section 1.7.2.7c)5.2 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)

5.3 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)5.4 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)5.5 There is effective separation between neighboring work areas when activities

therein are incompatible.

TNI EL-V1M2-2009, Section 5.3.35.6 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

ItemNumber Line of Inquiry Status Summary of Observations/Objectives Evidence

Reviewed Audit Notes6.0 Performance Testing (PT) Programs6.1 Can the laboratory demonstrate continued proficiency in either

MAPEP or external performance testing programs?

QSM Rev. 5.0, Module 1, Section 3.2.16.2 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 3.2.27.0 Sample Handling7.1 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) 7.2 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) 7.3 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)

ItemNumber Line of Inquiry Status Summary of Observations/Objectives Evidence

Reviewed Audit Notes8.0 Batch Quality Control (QC) (For all Radiochemistry QC requirements, see QSM Rev. 5.0 Appendix B, Tables 16-19)

8.1 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 1.7.28.2 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 8.3 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)8.4 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)8.5 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)8.6 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 Negative Control – Method Blanks8.7.1 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)8.7.2 Are samples associated with a failed method blank reprocessed for analysis or

the results reported with appropriate data qualifying codes?

TNI EL-V1M6-2009, Section 1.7.2.1 a) 8.7.3 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?

TNI EL-V1M6-2009, Section 1.7.2.1 b)8.7.4 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?

TNI EL-V1M6-2009, Section 1.7.2.1 c)8.7.5 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?

TNI EL-V1M6-2009, Section 1.7.2.1 c)8.7.6 Method Blank Acceptance Criteria

Does the laboratory use one method blank per preparatory batch? (MARLAP 18.4.1)

QSM Rev. 5.0, Module 6, Section 1.7.2.1 e)8.7.7 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 4.1QSM Rev. 5.0, Module 6, Section 1.7.2.1e)

8.7.8 Is the Method Blank MDA less than the Reporting Limit?

QSM Rev. 5.0, Module 6, Section 1.7.2.1e)

8.7.9 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?If the criteria are still not met, are the samples reanalyzed?QSM Rev. 5.0, Module 6, Section 1.7.2.1e)

8.7.10 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)8.7.11 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 project-specific measurement quality objectives?

TNI EL-V1M6-2009, Section 1.7.3.1a) 8.7.12 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) 8.7.13 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?

TNI EL-V1M6-2009, Section 1.7.3.1c)8.7.14 Are samples associated with a failed blank evaluated as to the best corrective

action for the samples (e.g., reprocessing or data qualifying codes)?

TNI EL-V1M6-2009, Section 1.7.3.1c)8.7.15 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 Positive Control – Laboratory Control Sample (LCS)

8.8.1 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”?

TNI EL-V1M6-2009, Section 1.7.2.2 a)8.8.2 Are samples associated with an out-of-control LCS reprocessed for reanalysis

or are the results reported with appropriate data qualifying codes?

TNI EL-V1M6-2009, Section 1.7.2.2 a)8.8.3 Is the LCS analyzed at a minimum of one per preparation batch, except for

those analytes for which no spiking solutions are available?

TNI EL-V1M6-2009, Section 1.7.2.2 b)8.8.4 Is the LCS a quality system matrix, known to be free of analytes of interest,

and spiked with known and verified concentrations of analytes?

TNI EL-V1M6-2009, Section 1.7.2.2 c)8.8.5 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)8.8.6 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?

MARLAP, Chapter 18, Section 4.1QSM Rev. 5.0, Module 6, Section 1.7.2.2 l)

8.8.8 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)8.8.9 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)8.8.10 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?

TNI EL-V1M6-2009, Section 1.7.3.2 a)8.8.11 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)8.8.12 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)8.8.13 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)8.8.14 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)

8.9 Sample Specific Controls – Matrix Spike

8.9.1 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.

TNI EL-V1M6-2009, Section 1.7.2.38.9.2 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.

TNI EL-V1M6-2009, Section 1.7.2.38.9.3 Is the activity of the matrix spike analytes(s) greater than five times the MDA

but not greater than 20 times the RL?

QSM Rev. 5.0, Module 6, Section 1.7.2.3 xii)TNI EL-V1M6-2009, Section 1.7.2.3 a) v)

8.9.4 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.)?

TNI EL-V1M6-2009, Section 1.7.2.3 a) vii)8.9.5 Is the lack of sufficient sample aliquot size to perform a matrix spike noted in

the laboratory report?

TNI EL-V1M6-2009, Section 1.7.2.3 a) iv)8.9.6 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. MARLAP, Chapter 18, Section 4.3QSM Rev. 5.0, Module 6, Section 1.7.2.3 a)xi)

8.9.7 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)8.9.8 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)8.9.9 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?

TNI EL-V1M6-2009, Section 1.7.3.3 a)ii)8.9.12 For matrix spike results outside established criteria, are corrective actions

documented or is the data reported with appropriate data qualifying codes?

TNI EL-V1M6-2009, Section 1.7.3.3 a)ii)8.9.13 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 Replicates / MS Duplicates / LCS Duplicates

8.10.1 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 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)

8.10.3 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)8.10.4 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%.

When the MARLAP, DER or the RPD criteria pass, then the duplicate is acceptable.

MARLAP, Chapter 18, Section 4.1QSM Rev. 5.0, Module 6, Section 1.7.2.3 b)xi)

8.10.5 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)8.10.6 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?

TNI EL-V1M6-2009, Section 1.7.3.3 b)8.10.7 Are the results compared to the acceptance criteria as published in the

mandated method?

TNI EL-V1M6-2009, Section 1.7.3.3 b)8.10.8 Where there are no established criteria, does the laboratory determine internal

criteria and document the method used to establish the limits?

TNI EL-V1M6-2009, Section 1.7.3.3 b)8.10.9 For replicate results outside established criteria, is the corrective action

documented or the data reported with appropriate data qualifying codes?

TNI EL-V1M6-2009, Section 1.7.3.3 b)

8.10.10 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)9.0 Reference Standards, Verification, Water Quality and Support Equipment9.1 Reference Standards

Does the quality control program establish and maintain provisions for radionuclide standards?

TNI EL-V1M6-2009, Section 1.7.2.5 c)9.2 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?

TNI EL-V1M6-2009, Section 1.7.2.5 c)i)9.3 Are reference standards purchased outside the United States traceable back to

each country's national standards laboratory?

TNI EL-V1M6-2009, Section 1.7.2.5 c)i)9.4 Do commercial suppliers of reference standards conform to ANSI N42.22 to

assure the quality of their products?

TNI EL-V1M6-2009, Section 1.7.2.5 c)i)9.5 Are reference standards accompanied with a certificate of calibration and

easily available for review?

TNI EL-V1M6-2009, Section 1.7.2.5 c)ii)9.6 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)9.7 Does the laboratory use only the decay-corrected certified value?

TNI EL-V1M6-2009, Section 1.7.2.5 c)iii)9.8 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 Standards Verification

Are standards verified prior to initial use?QSM Rev. 5.0, Module 6, Section 1.7.2.5 d)i)

9.10 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)

9.11 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)

9.12 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)

9.13 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)

9.14 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)

9.15 If all criteria are met, the certified value shall be used.

QSM Rev. 5.0, Module 6, Section 1.7.2.5 d i) 9.16 Reagent and Water Quality

Is the quality of water sources monitored, documented, and meet method specified requirements?

TNI EL-V1M6-2009, Section 1.7.2.5 b)9.17 Does water used in the laboratory have the purity of at least distilled or

deionized water?

QSM Rev. 5.0, Module 6, Section 1.7.2.5 d)9.18 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.

QSM Rev. 5.0, Section 5.5.13.1 Table ANSI N42.23, Section 5.2.8

9.20 WeightsAre 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 Table9.21 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 Table9.23 Are the daily checks documented in controlled logbooks?

QSM Rev. 5.0, Section 5.5.13.1 Table9.23 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)

9.24 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)

9.25 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))10.0 Instrument Operation and Calibration (General)10.1 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)

10.1.1 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 310.1.2 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?

TNI EL-V1M6-2009, Section 1.7.1a) paragraph 410.1.3 Are calibrations performed with reference standards that have the same

general characteristics (i.e., geometry, homogeneity, density, etc.) as the associated samples?

TNI EL-V1M6-2009, Section 1.7.1a) paragraph 510.1.4 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)10.1.5 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)10.1.6 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)10.1.7 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)

10.1.8 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)10.1.9 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)10.1.10 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)10.1.11 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)10.1.12 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)10.1.13 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)10.1.14 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)10.1.15 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 Instrument Calibration Verification (Performance Checks)

10.2.1 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)10.2.2 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)10.2.3 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?

TNI EL-V1M6-2009, Section 1.7.1b)10.2.4 For gamma-ray spectroscopy systems, are performance checks for detection

efficiency, energy calibration, and peak resolution performed on a day-of-use basis?

TNI EL-V1M6-2009, Section 1.7.1b)i)10.2.5 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?

QSM Rev. 5.0, Module 6, Section 1.7.1b)i)10.2.6 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)10.2.7 Is the measured FWHM resolution trended?

QSM Rev. 5.0, Module 6, Section 1.7.1b)i)10.2.8 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)?

QSM Rev. 5.0, Module 6, Section 1.7.1b)i)10.2.9 Are calibration or QC sources used that will not cause detector contamination

from recoil atoms from the source?

QSM Rev. 5.0, Module 6, Section 1.7.1b)i)

10.2.10 For radon scintillation detectors, is the efficiency verified at least monthly, when the system is in use?

QSM Rev. 5.0, Module 6, Section 1.7.1b)i)10.2.11 For alpha-particle spectroscopy systems, is the performance check for energy

calibration performed on a weekly basis?

TNI EL-V1M6-2009, Section 1.7.1b)ii)10.2.12 For alpha-particle spectroscopy systems, is the performance check for

detection efficiency performed on at least a monthly basis?

TNI EL-V1M6-2009, Section 1.7.1b)ii)10.2.13 For gas-proportional counters (GFPC), liquid scintillation counters (LSC) and

other scintillation counters, are the performance checks for detection efficiency performed on a day-of-use basis?

TNI EL-V1M6-2009, Section 1.7.1b)iii)10.2.14 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 Background Measurement

10.3.1 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?

TNI EL-V1M6-2009, Section 1.7.1c)10.3.2 Are these values subtracted from the total measured activity in the

determination of the sample activity?

TNI EL-V1M6-2009, Section 1.7.1c)10.3.3 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?

QSM Rev. 5.0 Module 6, Section 1.7.1c)i)and ii)TNI EL-V1M6-2009, Section 1.7.1c)i) and ii)

10.3.4 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)TNI EL-V1M6-2009, Section 1.7.1c)i) and ii)

10.3.5 For gas-proportional counters, are long background measurements (to be used for background corrections) performed on a monthly basis, at minimum.

QSM Rev. 5.0, Module 6, Section 1.7.1c)iii)10.3.7 For scintillation counters, are background measurements performed each day

of use?

TNI EL-V1M6-2009, Section 1.7.1c)iv)10.3.9 Are Background Subtraction Count (BSC) measurements conducted after

calibration and monthly thereafter?

QSM Rev. 5.0, Module 6, Section 1.7.1c)10.3.10 Are BSC measurements monitored for trends to ensure that a laboratory

maintains its capability to meet required project objectives?

QSM Rev. 5.0, Module 6, Section 1.7.1c)10.3.11 Are successive long background measurements evaluated as background check

measurements?

QSM Rev. 5.0, Module 6, Section 1.7.1c)10.3.12 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)10.3.13 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)10.3.14 Are background checks being collected before and after any counting chamber

changes are made (i.e., cleaning, liner replacement, or instrument modification)?

QSM Rev. 5.0, Module 6, Section 1.7.1c)

10.3.15 For alpha spectroscopy systems, are monthly background determinations performed for each Region of Interest (ROI)?

QSM Rev. 5.0, Module 6, Section 1.7.1c)ii)10.3.16 Are backgrounds for alpha spectrometers rechecked after being subjected to

high-activity samples?

QSM Rev. 5.0, Module 6, Section 1.7.1c)ii)10.3.17 Are procedures in place to define high activity and counting procedures to

check for gross contamination from high activity samples?

QSM Rev. 5.0, Module 6, Section 1.7.1c)ii)10.3.18 Are backgrounds for gas flow proportional counters rechecked after being

subjected to high-activity samples?

QSM Rev. 5.0, Module 6, Section 1.7.1c)iii)10.3.19 For scintillation counters, is the duration of the background measurement

sufficient to quantify contamination that may affect routine sample measurements?

QSM Rev. 5.0, Module 6, Section 1.7.1c)iv)10.3.20 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)

11.0 Isotopic Determinations by Alpha Spectrometry

11.1 Tracer: Are tracers used for isotope specific analysis by alpha spectrometry?

QSM Rev. 5.0, Module 6, Section 1.8.1a)11.2 Have all tracers used for alpha spectrometry been tested by the laboratory for

contribution in the ROIs of the analytes of interest?

QSM Rev. 5.0, Module 6, Section 1.8.1a)11.3 If a significant contribution is found, is the method for correction accepted by

the site prior to use?

QSM Rev. 5.0, Module 6, Section 1.8.1a)

11.4 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)11.5 Blank Correction:

Blank correction is not performed, except where noted.

QSM Rev. 5.0, Module 6, Section 1.8.1c)11.6 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%, or2. 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, or3. 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?

QSM Rev. 5.0, Module 6, Section 1.8.1d)11.7 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)11.8 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)11.9 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)

11.10 Energy Calibration: Is an energy calibration performed for each alpha detector? Is a curve fit for Energy (Y-axis) versus Channel (X-axis) 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?

QSM Rev. 5.0, Module 6, Section 1.8.1g)11.11 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)11.12 Detector Efficiency (Response) Determination Requirements

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?

QSM Rev. 5.0, Module 6, Section 1.8.1i)

11.13 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)12.0 Gas Flow Proportional Counting12.1 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)12.2 Instrument Calibration:

Is instrument calibration being performed in accordance with the requirements in ANSI N42.25, Calibration and Usage of Alpha/Beta Proportional Counters? NOTE: Where the word “should” is used in ANSI N42.25, calibration shall be performed in accordance with the statement. References are for the current version. When references change, an implementation schedule shall be determined.

QSM Rev. 5.0, Module 6, Section 1.8.4b)12.3 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?

QSM Rev. 5.0, Module 6, Section 1.8.4b)

12.4 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?

QSM Rev. 5.0, Module 6, Section 1.8.4b)12.5 Is the depth, diameter and shape (flat, flanged, ringed, etc.) of the planchets

used for calibration sources, the same as for samples?

QSM Rev. 5.0, Module 6, Section 1.8.4b)12.6 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.

QSM Rev. 5.0, Module 6, Section 1.8.4b)12.7 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? 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).

QSM Rev. 5.0, Module 6, Section 1.8.4d)12.8 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)

13.0 Gamma Spectrometry

13.1 Sample Counting Requirements:Do the SOPs for sample analysis by gamma spectrometry incorporate and

adhere to ANSI N42.14-1999 (or latest version), Calibration and Use of Germanium Spectrometers for the Measurement of Gamma Ray Emission Rate of Radionuclides, and/or ANSI N42.12-1994 (or latest version), Calibration and Usage of Thallium-Activated Sodium Iodide Detector Systems for Assay of Radionuclides?

Do the references reflect the current version of the ANSI documents? When references change, is an implementation schedule determined?

QSM Rev. 5.0, Module 6, Section 1.8.5a)i)13.2 Does the laboratory use Ge detectors of either intrinsic (pure) germanium or

lithium drifted germanium for gamma spectroscopy?

QSM Rev. 5.0, Module 6, Section 1.8.5a)ii)13.3 Does the laboratory use sodium iodide detectors for gamma counting?

QSM Rev. 5.0, Module 6, Section 1.8.5a)ii)13.4 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)13.5 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?

QSM Rev. 5.0, Module 6, Section 1.8.5a)iii))13.6 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?

QSM Rev. 5.0, Module 6, Section 1.8.5a)iv)13.7 Does the laboratory document, review, and provide configuration control for

gamma spectrometry libraries?

QSM Rev. 5.0, Module 6, Section 1.8.5a)iv)13.8 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)

13.9 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: Refer to ANSI N42.14 for guidance on isotope

specific efficiency and efficiency as a function of energy calibrations. Are the efficiency calibration measurements made with at least six peaks

which cover the typical energy range of approximately 0.059 to 2 MeV?

During calibration, 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 used for the efficiency equation (ASTM D 3649-98a)?

2) Sodium Iodide (NaI) Detectors: Refer to ANSI N42.12.Are the efficiencies determined when there is a change in resolution, geometry, or system configuration (ASTM D 3649-98a)?

QSM Rev. 5.0, Module 6, Section 1.8.5b)13.9cont’d

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?

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)

13.10 Energy Calibration Requirements: Each gamma spectrometry system shall be energy calibrated with NIST/international traceable standards or prepared from NIST/international traceable sources.

i) Germanium Detectors: Refer to ANSI N42.14, Section 5.1 for guidance on calibrating gamma-ray energy as a function of channel number at a fixed gain.

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 (ASTM D 3649-98a)?

iii) Is the energy calibration linear and accurate to 0.5 keV?iv) NaI Detectors: Refer to ANSI N42.12, Section 4.3.5

Performance Evaluation:Germanium Detectors: Refer to ANSI N42.14, Section 7.Sodium Iodide Detectors: Refer to ANSI N42.12, Section 4.3.5.

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)14.0 Liquid Scintillation Counting14.1 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)

14.2 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)14.3 SOPs

• Do laboratory SOPs for methods using liquid scintillation counting incorporate and adhere to ANSI N42.15-1997 (or latest version), American National Standard Check Sources for and Verification of Liquid Scintillation Systems?

• Are method references for the current version? • When references are updated, is an implementation schedule determined by

the lab?

QSM Rev. 5.0, Module 6, Section 1.8.3c)14.4 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)14.5 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)

14.6 Constant QuenchIf 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)14.7 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)14.8 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.

QSM Rev. 5.0, Module 6, Section 1.8.3h)15.0 Radon Scintillation (Lucas Cell)15.1 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?

QSM Rev. 5.0, Module 6, Section 1.8.2a)15.2 Is the operating voltage plateau slope for the detector <2%/100V?

QSM Rev. 5.0, Module 6, Section 1.8.2b)15.3 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 Are background measurements for quantitation in each cell carried out prior to each sample measurement?

QSM Rev. 5.0, Module 6, Section 1.8.2d)15.5 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)16.0 Conditions Requiring Reanalysis or Recount16.1 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)16.2 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)16.3 Analytical Batch Conditions:

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 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:

K = detector efficiency * e -ƛt * aliquot fraction * tracer recovery*YieldTS = count time of the sample in minutessb= standard deviation of the blank population where the blank population is in net blank counts in count time TS

ii) Without a Blank Population:MDA for samples without a blank population can be determined if based on appropriate Curie or MARLAP calculations, such as:

Where:K = detector efficiency * e -ƛt * aliquot fraction * tracer Recovery*YieldTS = count time of the sample in minutesTB = count time of the background in minutesb = background count rate in cpmThe 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?

Where:DL = the decision level in disintegrations per minute per unit volume or weight (dpm/unit);

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; andW = 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

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.

Notes:

Notes:

Record of Revision for Checklist 4Data Quality for Radiochemical Analyses

RevisionNumber

EffectiveDate

Reason forRevision

Line ofInquiry

3.5 11/2009 Added - Data analysis software may also be used for the statistical evaluation of data for trends and biases. 14.123.6 11/2010 Revised wording for counting uncertainty and QSAS reference 1.43.6 11/2010 Changed QSAS reference for reporting negative activities 3.13.6 11/2010 Changed QSAS reference for reporting negative activities 3.23.6 11/2010 Changed QSAS reference for NDA 4.13.6 11/2010 Changed QSAS reference for NDA 4.23.6 11/2010 Added requirements for a radiological control program 5.53.6 11/2010 Replaced PE with the term PT Entire Doc.3.6 11/2010 Added requirements for the use of PT samples 6.23.6 11/2010 Changed QSAS reference for standards and reference materials 9.13.6 11/2010 Changed QSAS reference for standards 9.63.6 11/2010 Changed QSAS reference for expiration dates 9.73.6 11/2010 Changed QSAS reference for verification of standards 9.83.6 11/2010 Changed QSAS reference for ROIs 11.43.6 11/2010 Changed QSAS reference for efficiency determination 11.53.6 11/2010 Changed QSAS reference for resolution of tracer peaks 11.63.6 11/2010 Changed QSAS reference for background measurement for counting chamber changes 13.63.6 11/2010 Changed QSAS reference 13.73.6 11/2010 Changed QSAS reference for net counts for efficiency equation 13.103.6 11/2010 Changed QSAS reference for gamma-ray spectra 13.143.6 11/2010 Added requirements for effects of quench on background 14.5

3.7 11/2011 Added the following to the Note section of the checklist: Fully document any deviation from the LOI or the requirements of QSAS 2.7 Page 1

3.8 1/2012 Added the following to the Note section of the checklist: Fully document any deviation from the LOI or the requirements of QSAS 2.8 Page 1

4.0 12/2013 Revised to incorporate QSM Rev. 5.0, TNI ELV1M1, ISO/IEC 17025 All4.1 3/2014 Deletion of quarterly accuracy checks for mechanical pipettes 9.19

Documents

National Analytical Management Programrmccnetwork.net/sites/default/files/files/Checklist 4 Rad - … · Web view__ Reanalysis/Recount __ Performance Testing (PT) Programs A = Acceptable

National Analytical Management Programrmccnetwork.net/sites/default/files/files/Checklist 4 Rad - … · Web view Reanalysis/Recount Performance Testing (PT) Programs A = Acceptable