'739 - Digital Library/67531/metadc... · MDC for methods and systems used to discriminate between...
Transcript of '739 - Digital Library/67531/metadc... · MDC for methods and systems used to discriminate between...
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651 '739 ........... . . . .. . . . . . . . . . . . . . . . ___. . . . Pagal O f &
ENGINEERING CHANGE NOTICE
2. ECN Category (mark one) 3. Originatoh Name, Organization. MSIN, and Telephone No. 4. USQ Required? 5. Date
0 @Yes ONO 09-14-99
0 0
0
Supplemental CE wills, WRAP Engineering, DiredRevision @ T4-52, 373-9844 Change ECN
Temporary
Standby Supersedure sheet no. and rev.)
7. Bldg./Sys./Fac. No.
2336-W Q
6. Approval Designator 6. Project TtlelNo.fWork Order No.
WRAP Facility/AJ60
Q. Document Numbers Changed by this ECN (includes 10. Related ECN No(s). 11. Related PO No.
CancelNoid 0 HNF-4051, Rev. L A , All I N/A I N/A 0 Yes (fill out Elk. 12b) 0 No NA Blks. 12b,
1% Modification Work 12b. Work Package No. 12c. Modification WorkCompleted 12d. Restored to Ori inal Condition (Temp. or Standby ECds only)
N/A N/A N/A Design AuthoritylCo Engineer Signature 8 Design AuthoritylCo Engineer Signature 8
!2c, 12d) d i t e d i t e
13a. Description of Change 13b. Design Baseline Document? 0 Yes @ No
Newly generated QAO data has been added to more completely describe instrument performance over the range of analysis. In addition, Minimum Detectable Concentration calculations are provided for the IPAN and GEA Systems.
1 4 . Justification (markone) I&. Justification Details
Criteria Change 0 Design verification not required Design Improvement 0
0 Environmental Additions made in response to WIPP audit comments
USQ WRP-99- (99 Facilty Deadivation
As-Found
Faciltate Const.
See attached distribution sheet
A-79M)-0152 (10B7) A-780&0151
I I 1. ECN (use no. from oa. 1
6. Design Verification Required
ENGINEERING CHANGE NOTICE
17. Cost impact 18. Schedule Impact (days) ENGINEERING CONSTRUCTiON
. - Page 2 of 2 ECN-651739
@ No Savings 0 $ N/A Savings 0 $ N/A Delay O N / A 0 Yes I Additional 0 $ N/A Additional 0 $ N/A I Improvement 0 N/A
- SDDmD 0 Fundional Design Criteria 0 Operating Specification 0 Criticality Specification 0 Conceptual Design Report 0 Equipment Spec. 0 Const. Spec. 0 Procurement Spec. 0 Vendor Information 0 OM Manual 0 FSAWSAR 0 Safety Equipment List 0 Radiation Work Permit 0
Environmental Report 0 Environmental impact Statement 0
Seismicistress Analysis
StresdDesign Report
Interface Control Drawing 0 Calibration Procedure 0 Installation Procedure
Maintenance Procedure 0 Engineering Procedure 0 Operating lnstrudion 0 Operating Procedure 0
IEFD Drawing 0 Cell Arrangement Drawing 0
Fac. Proc. Samp. Schedule 0 Inspection Plan 0
Operational Safety Requirement 0
Essential Material Specification
Tank Calibration Manual 0 Health Physics Procedure 0 Spares Multiple Unit Listing 0
Component Index 0 ASME Coded Item 0
Computer Software 0 Electric Circuit Schedule 0 ICRS Procedure 0
Process Flow Chart
Purchase Requisition 0 Tickler File 0 None El
Test ProceduredSpecification 0
Human Factor Consideration 0
Process Control Manualplan 0
Environmental PermR 0 Inventory Adjustment Request 0 0. Other Affected Documents: (NOTE: Documents listed below will not be revised by this ECN.) Signatures below indicate that the signing
organization has been notified of other affected documents listed below. Document NumberiRevision Document NumberIRevision Document NumberiRevision
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ADDITIONAL
A-7WJ-0133 (10197)
-___-_I..- .-
HNF-4051, Rev. 2
Quality Assurance 0 bjectives for Nondestructive Assay at The Waste Receiving and Processing Faci I ity
CE Wills Waste Management Federal Services of Hanford, Inc., Richland, Wa. 99352 Richland, WA 99352 U.S. Department of Energy Contract DE-AC06-96RL13200
EDTIECN: ECN- 65173 9 u c : 506
Org Code: 32600 Charge Code: AJ60 B&R Code: EW02J16 Total Pages: 31
Keywords: QAP, NDA, WRAP, WIPP, TRU, CAO, Source Certificates
Abstract: This report summarizes the validation of the WRAP NDA systems against the various QAOs. A brief description of each test and any significant conclusions is included. Variables which may have affected test outcomes are examined. This report will be reviewed semi-annually and updated as necessary.
TRADEMARK DISCLAIMER. Reference herein to any specific commercial product, process. or service by trade name trademark, manufacturer, or otherwise, does not necessarily constitute or imply Rs endorsement, recommendation. or favoring by the United States Government or any agency thereof or its contractors or subcontractors
Prinlea n tne LnRed Stales of Amerca To onain copies of this OocLmenl. contact DocLment Contro Serv ces P 0 Box 950 Mailstop ri6CB. Richland WA 99352. Pnone (5091 372-2420, Fax (509) 37649
4 I 15 I94 Release Approval bate I
DATE: HANFORD
GLUJ Release StamD
Approved For Public Release
A-6400073.1 (1w97)
( 1 ) Document Nunber RECORD OF REVISION
QUALITY ASSURANCE OBJECTIVES FOR NONDESTRUCTIVE ASSAY AT THE WRAP F A C I L I T Y
I I
I
I I I
A-7320.005 (08/91) UEF168
_.
HNF-405 1, Revision 2
Quality Assurance Objectives for Nondestructive Assay at the Waste Receiving and Processing Facility
Craig Wills and Michael G. Cantaloub, Waste Management Hanford
HNF 4051 Rev. 2 I
Executive Summary
The Waste Receiving and Processing (WRAP) facility, located on the Hanford Site in southeast Washington, is a key link in the certification of transuranic (TRU) waste for shipment to the Waste Isolation Pilot Plant (WIPP). Waste characterization is one of the vital functions performed at WRAP, and nondestructive assay (NDA) measurements of TRU waste containers is one of two required methods used for waste characterization. The WIPP Quality Assurance Program Plan (WIPP-QAPP) specifies a series of quality assurance objectives (QAOs) which each NDA system must meet before a site can be certified to ship TRU waste to WIPP. These QAOs ensure that systems meet minimum standards for measurement parameters such as precision and accuracy.
This report summarizes the validation of the WRAP NDA systems against the various QAOs. A brief description of each test and any significant conclusions is included. Variables which may have affected test outcomes are examined. This report will be reviewed semi-annually and updated as necessary.
HN F 40s I
Table of Contents
Rev. 2 -
.. Executive Summary ......................................................................................................................... 11
Table of Contents ..................... Introduction ..... . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . .. . . . . . . . . . . . . . . . . . . . . . . . . .. . .. . . . . . . . . . . . . . .. . . . . . . . . . .. . . . . . .. . . . . . .. . .. . . . . . . . .. . .. . .. . . . 1 Descnption of Tests ...................................................................................................................... 4 Summary of IPAN A Tests - Accuracy, Precision and Bias ......................................................... 6 Summary of GEA A Tests - Accurancy, Precision and Bias ..................................................... 10 Summary of IPAN Tests - Minimum Detectable Concentration ............................................... 14 Summary of GEA A Tests - Minimum Detectable Concentration ........................................... 15 Discussion of Results .................................................................................................................. 16 Future Considerations .................................. .................................................... ........................... 18 Attachments . . . . . . . . . .. . . . . . . . .. . . . . . . . . .. . . . . . .. . .. . . . . . .. .. . .. . . . . . . . .. . . . . . . . . . . . . . .. . . . . . .. . . . . . . . . . . . .. . . . . . .. . . . . . . . . . . . . . . . ._ . . . .
... . . . . . , . . . . . .................................................................. 111
. .
... 111
HNF4051 Rev.2
Introduction
The WRAP facility has four primary NDA systems: two imaging passive/active neutron (IPAN) systems and two gamma energy assay (GEA) systems. The two IPAN units are identical, as are the GEA units, thus the systems are designated as follows: IPAN A, IPAN B, GEA A, and GEA B. This report documents the conformance of IPAN A and GEA A to the precision, accuracy and minimum detectable concentration (MDC) NDA QAOs for WIPP. The total measurement uncertainty (TMU) QAO required for each system is addressed in a separate document (HNF 4050).
WIPP sets forth four nominal testing points for NDA. Although these are normally defined in alpha curies, they are also defined in grams of Pu-239. Due to the nature of available sources, WRAP uses the nominal Pu gram quantities for testing. This report documents testing of the IPAN A and GEA A systems at the 0.1 g, 1 .O g, 10 g, and 160 g levels for the precision and accuracy QAOs. MDCs for the IPANs and GEA-A are also reported. The MDC QAO is predominately determined from instrument background evaluations. As such, no TRUiradioactive sources were required for the MDC QAO.
Precision and Accuracy
To comply with QAO requirements, facilities must determine precision and accuracy values obtained for 15 replicate measurements of waste containers containing known quantities of TRU isotopes at the nominal test points. This must be done for each system which is to be certified. The equations used to determine these values, tabulated later in this report, are listed below.
Equation 1 calculates precision as the %RSD of the distribution of 15 replicate measurements:
S % RSD= = * 100
Y
where
%RSD = percent relative standard deviation; s = standard deviation; y = mean of the replicate measurements.
Equation 2 determines the standard deviation:
where s = standard deviation; Yi = the measured value of the i" replicate measurement; Y = the mean of the replicate measurements; n = the number of replicate measurements.
Equation 3 determines the accuracy for a standard reference material as percent recovery:
I
HNF 405 1 Rev. 2
C % R = A * 1 0 0 C s m
where
%R = percent recovery; Cm = Cvm=
average result of the 15 replicate determinations; known value for the waste container used in the measurements.
The minimum detectable concentration (MDC) provides the smallest concentration of material which can be detected with 95% confidence, while also having 95% confidence that “activity” is not detected falsely from a null sample. For an MDC determined from a blank - a drum with as similar a matrix as an expected sample but with no known activity added - the calculated value is an a priori estimate of the best sensitivity that can be expected from the sample measurements and conditions. When MDC is determined from an actual sample specbum, the background at the energy or region of interest will most likely be higher. This increase is due to the continuum generated by Compton scattering and by bremsstrahlung. Thus the MDC from an actual sample, calculated a posleriori, is expected to be slightly higher than the a priori estimate. WRAP is required to demonstrate compliance with the MDC for methods and systems used to discriminate between TRU and LLW or methods and systems used to define a waste stream as TRU.
Satisfaction of the MDC QAO requires the MDC be determined from the appropriate relationship using nominal facility values and the data collected from 15 replicate measurements performed on an appropriate waste container. Equation 4 gives the expression for determining MDC:
MDC =KlK,(2.71+4.65*s,)
where
KI = the proportionality constant relating the detector response (counts) to the activity, such as,K =l/e where e is an overall detection efficiency, or K = 1/I& where I, is the gamma ray emission probability per decay and q is the detection efficiency for the gamma ray;
the factor which relates the total activity determined by the measurement system to an activity concentration in waste under a given set of measurement conditions, for example, the weight of waste assayed and a self-adsorption correction;
K2 =
Sb = the standard deviation or uncertainty of the background.
For calculating the MDC, the variance or standard deviation of the background is determined by the expression:
2
HNF 4051 Rev. 2 I
where
counts =
CR =
Tc =
the total counts acquired in the region of interest for a photon of energy E;
count rate in the region of interest for a photon of energy E(cps);
count time for the assay (second)
Substituting appropriate terms for the GEA system into Equation 4 yields the final expression for determining the MDC on the GEA system:
where
CR(W =
Tc
e(&) =
I(&) =
M =
37 =
count rate in the region of interest for a photon of energy E (cps);
count time for the assay (second);
the detection efficiency for the photon of energy E (countsiphoton);
yield or intensity for the photon of energy E(photon/second);
mass of the drum matrix (8);
conversion factor relating decays per second to nCi (dpsinci);
- ~
A similar expression is used to determine the MDC for the IPAN system for 'active mode' operation:
(2.71 + 4 . 6 5 G )
(IR)( WGE)(12.3)(1 0-9)M MDC =
where
[CBKGD]'' = overall background uncertainty in light matrix background counts for the 28 detector bundles (counts);
instrument fissile material conversion factor for a light matrix (counts/g Pu-239);
weapons grade Pu enrichment conversion factor (g Pu-239/ g WGPu);
IR =
WGE =
3
HNF 405 1 Rev. 2
Source Pu Quantity QAo19 ID (grams)
NTP-0068 0.03
12.3 = weapons grade Pu to Ci Pu conversion factor (g WGPdCi - typical value for Hanford waste);
mass of the drum matrix (g); M =
10-9 = Ci to nCi conversion.
QAOZO qa021 QA024 QAO-W21
T1, P3 T2,PlO
DescriDtion of Tests
NTP-0070 NTP-0075 NTP-0077 NTP-0084 NTP-0089
Precision and Accuracy
For testing of the NDA systems against the WIPP QAO requirements, the PDP “combustibles” matrix drum was loaded with sources to approximate the nominal test points. The combustibles drum was selected because it is the nearest approximation to the prevalent waste matrix for WRAP. The table below shows the arrangement of sources within the test drum. The test arrangement number (e.g., QA021) is shown in the next section where specific test results are tabulated.
0.03 T2, P1S T3,P19 t1,p0 0.03 T3, P18 0.03 Tl,PO T1P9 0.03 Tl,Pl8 0.30 T2, P6
NTP-0091 NTP-0098 NTP-0 103
0.30 T3, P6 0.30 T3,PO 0.30 T233
NTP-0119 NTP-0126
WRAP-2KiPU
NTP-0105 1 0.30 1 T1,PlS I T1,PlS 1 NTP-0112 I 3.00 I T1. P6 I I 1 1
3.00 T2, P1S 3.00 T3, P1S 5.00 T3, P19
A
HNF 405 1 Rev. 2
The “T” and “ P references are to tube number and pin height, respectively. Tube 1 is centered in the drum, while tube 2 is located about halfway between the center and the outer wall of the drum. Tube 3 is located near the outer wall of the drum, opposite tube 2. The pin numbers refer to height (in inches) above the bottom of the drum at which the source is placed. The sources are composed of Pu dispersed in diatomaceous earth, doubly enclosed in concentric stainless steel cylinders. They are nine inches long and about two inches in diameter.
The GEA system MDC was determined by using the daily operations checks background drum (drum ID: GEABKGD). The drum has a matrix density that most closely approximates the present WRAP waste stream. No activity was added (Le. a confounding matrix) as current waste streams contain few fission products or radioactive components other than Pu and Am. Data was acquired for 15 replicate counts on the GEABKGD drum using the WRAP operating procedures for the GEA system (WRPl- OP-0906).
No background measurements were conducted on the IPAN for use in determining the MDC. The data required to calculate the MDC for active IPAN analysis can he found in the active matrix library file, KEHam. This file contains the value of the fissile signal background for each of the 28 grouped detector packages, the error associated with each background value, as well as the fissile signal value per 0.500 g Pu-239 for each detector package and the 20 defined spatial locations. The K E H a m file is stored on the instrument with the IPAN system files and is accessed during sample analysis. The MDC calculation is based on the ‘‘light’’ matrix library file, the most non-interfering matrix for which the system is calibrated. Being identically built, both IPANs use the same KEHamx file, and therefore the MDC calculation applies to both IPAN A and IPAN B.
Test Results
Results for the IPAN and GEA systems are presented in tabular form on the following pages. Tables for the precision and accuracy QAOs (IPAN then GEA) are given first, followed by the MDC results for the IPAN and GEA-A system.
5
HNF4051 Rev.2 I
QAO-W21 IPAN A
Summary of IPAN A Tests - Accuracv. Precision and Bias
IPAN A 160.00 g Pu (160 g nominal test value) 93.8% Pu-239
Pu-239 Mass %Actual Pu- (9) 239 Value
Run 1 1
Pu-239 7.54EM1 50.25
Pu-239 I 7.54E+01 I 50.27
Pu-239 7.47EM1 49.76 Pu-239 7.54EM1 50.26 Pu-239 7.42EMl 49.46 Pu-239 7.44EM1 49.56
Run 10 Pu-239 49.96
Run 13 Run 14 Run 15
Pu-239 7.62E+01 50.76 Pu-239 7.62E+01 50.79 Pu-239 7.45E+01 49.67
I I I 1 Averaee I Pu-239 I 7.52E+01 I 50.08
%R = 50.08
6
HNF 405 I Rev. 2
QA019
Run 1 Run 2 Run 3 Run 4
_____ IPAN A Pu-239 Mass %Actual Pu-
(8) 239 Value
Pu-239 1.03E+01 111.71 Pu-239 1.03E+01 111.38 Pu-239 I .04E+OI 112.14 Pu-239 1.04E+01 112.57
Run 5 Pu-239 I 1.05E+01 I 113.33 Run 6 I Pu-239
Average 1 Pu-239 I I.O4E+Ol I 111.96
std dev = 6.30E02 Precision I % RSD = n.61
~~~~ ....
Accuracy 1 %R = 11 1.96 TotalBias 1 110.84% (Low) to 113.33% (High)
7
HNF 405 1 Rev. 2
IPAN A 0.99 g Pu (1 .O g nominal test value) 94% Pu-239
QA020 IPAN A Pu-239 Mass % Actual Pu- (9) 239 Value
Average I Pu-239 1 9.62601 1 103.91
Accuracy
std dev = 6.0SE-02 Precision I % RSD = 6.29
% R = 103.91 Total Bias
8
94.53% (Low) to 114.51% (High)
HNF 405 1 Rev. 2
QA02 1 IPAN A Pu-239 Mass YO Actual Pu- (8) 239 Value
Run 1 Run 2 Run 3 Run 4 Run 5
Run 13 I Pu-239 I 7.69E-02 I 91.38 Run 14 1 Pu-239 I 7.80E-02 I 92.69
Pu-239 8.1 OE-02 96.26 Pu-239 1 .04E-O 1 123.95 Pu-239 8.96E-02 106.48 Pu-239 8.99E02 106.83 Pu-239 9.02E-02 107.19
~
Run 15 I Pu-239 I 8.54E-02 I 101.49 1 I I
Precision
, I I
Average 1 Pu-239 I 8.59E-02 I 102.12
% RSD = 12.23 I standard deviation = 1.05E-02
Total Bias 77.84% (Low) to 123.95% (High)
9
HNF 4051 Rev. 2 I
QAO-W2 1 Sum Seg Pu-239 Mass Activity (8)
(PCi)
Run 1 7.38EM6 1.19EM2
Summary of GEA A Tests - Accuracv and Precision
GEA A 160.00 g Pu (160 g nominal test value) 93.8% Pu-239
% Actual Pu- Comb All Pu-239 Mass %Actual h- 239 Value Activity (g) 239 Value
(KO __
79.26 7.68E+06 1.24EM2 82.48 Run 2 Run 3 Run 4 Run 5 Run 6
7.33EM6 1 . I 8E+02 78.72 7.69E+06 1.24E+02 82.59 7.39EM6 1.19EM2 79.37 7.64E+06 1.23E+02 82.05 7.41 E+06 1 .19E+02 79.58 7.80E+06 1.26E+02 83.77 7.30E+06 I . 1 8E+02 78.40 7.60E+06 1.23E+02 81.62 7.36E+06 1 .19E+02 79.05 7.73E+06 I .25E+02 83.02
Run 7 1 7.32E+06 I 1.18E+02 1 78.62 I 7.58E+06 I 1.22E+02 1 81.41 Run 8 I 7.34E+06 1 1.18E+02 1 78.83 1.23E+02 1 81.95
Precision Accuracy * Total Bias
Run 10 I 7.34E+06 I 1.1
std dev = 7.39E-01 % RSD = 0.62
78.08% (Low) to 79.69% (High)
std dev = 1.28E+00 % RSD = 1.03
80.66% (Low) to 83.77% (High) %R =78.83 %R = 82.35
- . . . ._ - - . . Run 15 I 7.27E+06 I 1.17E+02 I 78.08 I 7.51E+06 I 1.21E+02 I 80.
I I I I I 1 Average I 7.34E+06 I 1.18EM2 I 78.83 1 7.67EM6 1 1.24EM2 I 82.35
. ... ..
HNF 405 1 Rev. 2
GEA A 9.90 g Pu (10 g nominal test value) 94% Pu-239
Precision Accuracy * Total Bias
stddev = 1.26E-01 % RSD = 1.74
74.48% (Low) to 80.02% (High)
stddev = 1.44E-01 % RSD = 1.65
90.24% (Low) to 96.13% (High) %R = 71.17 %R =93.69
HNF 4051 Rev. 2
GEA A 0.99 g Pu (1.0 g nominal test value) 94% Pu-239
Precision
Total Bias Accuracy *
Run 15 1 4.64E+04 1 7.48E-01 1 80.37 I 4.90EM4 I 7.90E01 I 84.87 I I I I I I
std dev = 8.78E-02 % RSD = 12.25
46.25% (Low) to 85.56% (High)
std dev = 6.25E-02 % RSD = 7.80
71.53% (Low) to 97.34% (High) %OR = 77.03 %OR = 86.06
Average 1 4.45E+04 1 7.17E-01 I 77.03 1 4.97EM4 I 8.01E-01 I 86.06
QA024 Sum Seg Pu-239 Mass %Actual Pu- Comb All Pu-239 Mass % Actual h- Activity (8) 239 Value Activity (g) 239 Value
(PCO (KO
Run 6 1 3.59E+03 5.79E-02 I 68.71 I 4.28E+02 I 6.90E-03 I 8.20 Run 7 1 2.68E+03 1 4.32E-02 1 5 I .33 I 4.96E102 I 7.99E-03 I 9.50
Run 1 Run 2 Run 3 Run 4 Run 5
4.32EM3 6.9 6 E 0 2 82.75 I .14E+03 1.84E-02 21.84 4.33E+03 6.98E-02 82.94 4.33E+03 6.98E-02 82.94 4.53E+03 7.30E-02 86.77 1.02E+03 1.64E-02 19.54 4.46E+03 7.19E-02 85.43 1 .12E+03 1.8 1 E-02 2 I .45 3.68E+03 5.93E-02 70.49 5.1 5Ei-02 8.30E-03 9.86
13
Run 8 Run 9 Run 10 Run I 1 Run 12
3.71 E+03 5.98E-02 71.06 1 . 5 5 ~ ~ 3 2.50E-02 29.69 4.50E+03 7.25E-02 86.20 1.42EM3 2.29E-02 27.20 3.72E+03 6.00E-02 71.26 3.72E+03 6.OOE-02 71.26 4.75E+03 7.66E-02 90.98 4.75E+03 7.66E-02 90.98 5.22E+03 8.4 1 E-02 99.99 9.87E+02 1.59E-02 18.91
HNF 4051 Rev. 2 I
Summary of IPAN Tests - MDC
As mentioned previously, no background measurements were required for determining the IPAN MDC. The background information and instrument response factors are contained in the system operating files and were supplied by the manufacturer The uncertainty in the average neutron background for the 28 neutron detector bundles obtained from the active matrix library file is
==63 counts
The total instrument response is 237,529 counts per gram Pu-239 for the light matrix. The Pu-239 weapons grade enrichment (WGE) is 0.94, while the nominal matrix mass for a low-density or light matrix material is 15.6 kg.
Using these values and the expression derived for the IPAN yields and MDC of
[2.71+ 4.65(63)Eounts 237_529counts)[ - 0.94gPu239)( 12.3g W G P L I ] ~ ~ O ~ ~ O - ~ O C / / nCi 115,600g))
MDc=(( gPu239 g WGPu Ci Pu
MDC = 6.9nCiig
14
~ . . . .
HNF4051 Rev.2 I
Average Std dev + 20
Summary of GEA A Tests - MDC
GEA A Minimum Detectable Concentration
5.68 0.027 Average 8.34 39 0.601 0.001 5 Std dev 0.88 2.2 6.88 0.030 i 20 10.1 1 44
Measurements performed on “GEABKGD drum Nominal count time for drum assay is 300 seconds Nominal mass for 55-gallon (208 L) drum containing a low density matrix is 15,600 grams
15
.
HNF 405 I Rev. 2
Discussion of Results
The following table, taken from Table 9-1 of HNF-2599, Final Hunford Site Transuranic Waste Churacterization Quality Assurance Project Plan, shows the requirements for QAO validation.
Nominal compliance Parameter
Range of waste point activity in a-Curies” PrecisionC Accuracyd Total biase Completeness‘ MDC a-Curies” (g WG P u ) ~ (%RSD) (%R) (”/.I (%) (nCi/g)
>0.02 to 0.2
>0.2 to 2.0 High 300
High 150
a Applicable range of TRU activity in a 208-L (55-gal.) waste container to which the QAOs apply, units are Curies of alpha-emiding TRU isotopes with half-lives greater than 20 years.
The nominal activity (or weight of Fu) in the 208-L (55-gal.) waste container used to demonsbate that QAOs can be achieved for the corresponding range in column I , values in parentheses are the approximate equivalent weights of WG Pq 15 years a%r purification; for purposes of demonstrating QAOs, “nominalll means within 10 percent.
One standard deviation based on I5 replicate measurements o f a noninterfering matrix.
Ratio of measured to known values based on the average of 15 replicate measurements of a noninterfering matrix.
95 percent confidence bounds for system bias established by studies to determine contributions to total unce6nly from all significant sources. Units are confidence bound divided by true value, expressed as a percent. Requirement for the QAO for total uncertainly is to determine and document
Valid radioassay data are required for all waste containers.
b
e
It should be noted that a noninterfering matrix is a virtual impossibility. In the case of W”, a light (debris or combustibles) matrix was used; while the interference of this matrix is relatively small, it exists nonetheless. Of greater concern are the test sources themselves. Even if an empty drum matrix was used, the two walls of stainless steel surrounding the Pu source material do attenuate both neutron and gamma flux. The physics behind the neutron attenuation are obvious. The primary energy line used for gamma detection of Pu-239 is 414 keV, but at extremely low mass levels (such as 0.lg) the yield fraction of the 414 keV gamma is too low to be consistently detectable. At these mass values, the primary energy line becomes 129 keV, since it has a significantly higher yield fraction than the 414 keV line. This relatively low (129 keV) energy line can be easily attenuated by the encapsulating steel walls of the source. A preliminary review of test results shows this effect to be about 10-15%.
Precision and Accuracy
Comparison of the results tabulated earlier against the requirements listed above shows that both systems under test pass easily at the two middle points tested (1 g and 10 g). The GEA “Combine All
16
HNF 4051 Rev. 2
Results” fails at the 0.1 g level, and the IPAN fails at the 160 g level. For the IPAN units, only the active assay results are reported. As improvements are made to the passive algorithms, the passive results will be tested and documented as necessary. For the GEA units, the “Combine All Results” algorithm is preferred at all save the lowest gram levels; at approximately 0.5 g Pu the “Sum Segments” algorithm takes over. In the GEA, “Sum Segments” is also preferred for a lumped source up to about 2 g Pu. The table below summarizes the results, and shows the operating range for each system and for each method or algorithm. Results outside these ranges require validation through further testing. Refer to HNF-5140, Validation Data for NDA Systems ut WRAP, for details and supporting analysis.
Nominal Pu Value
0.10 g 1.00 g
10.0 g I60 g
Pu Mass WAN GEA Range Active Passive Combine All Sum Segments
0- 0.25 g I’;1ss U!\ Fail I%lSS
0.25 - 2.5 g I?lSS \1/ \ I?lSS I’ass 2.5-25g 1,. .lhS Ni.\ I’nss I’ms
> 2 5 g Fail \,‘?I I’ess I’ass
All testing was performed using the WRAP operating procedures for the IPAN and GEA systems (WRP1-OP-0905 and WRP1-OP-0906, respectively). The standard operating software for the systems was used to acquire data and report results. Testing was performed for 55-gallon (208 liter) waste drum configurations only.
For these results to be valid, full independence of source materials must be maintained. The QAO tests are performed using plutonium sources, each with its own pedigree and documentation. The IPAN units were calibrated using depleted uranium and californium sources, while the GEA calibrations utilize mixed sources containing cobalt, barium, cesium, and americium. No sources used in calibration are used in any testing.
MDC
The GEA-A MDC satisfies the 60 nCi/g QAO requirement. The average MDC from the replicate background runs is 39 nCUg for Pu-239 as determined from the region of the 129 keV line and 0.026 nCi/g for Am-241 using the 59.6 keV line. The low MDC for Am-241 is not surprising given the high yield and relatively high detection efficiency for the 59.6 keV photon. Similar to the GEA precision and accuracy requirements, at low plutonium masses the 129 keV photon becomes the dominant photon for the purpose of analysis. The calculated MDCs correspond to absolute TRU masses of 10 mg Pu-239 and 0.1 pg Am-241 respectively. MDC’s based on other regions of the spectrum (Le U- 235 at 185.7 keV) were not evaluated as Pu-239, and to a lesser extent Am-241, is the dominant waste stream isotope.
The IPAN MDC was determined to be 7 nCUg based on the background uncertainty and fissile signal data file for a light density matrix obtained from the IPAN active matrix library. The MDC is valid essentially for Pu-239 as that is the predominant waste stream isotope and the primary fissile nuclide detected during active operation of the IPAN-A system.
17
HNF 405 1 Rev. 2 I
Future Considerations
As further testing is completed this report will be revised to include validation of the IPAN B and GEA B systems at all four levels. QAO tests will be performed periodically as called out in WMH- 350 Section 2.4. Testing will be repeated annually, as a minimum, in order to meet the QAPjP (Section 9.5) requirement that “calibrations are verified for at least one counting geomebylsample matrix combination on an annual basis.”
HNF 405 1 Rev. 2 1
Los Alamos National Laboratory Ctrtificate of content anb Erateatiritp
Pu02-Diatomaceous Earth Standard WRAP-2 5.0GPU
Thls M)A standard contains high purity plutonium dioxide dispersed in diatomaceous earth. Quantitative information and uncertainties on the nuclear content of this W R i i a re listed below. Complete information regarding the P u and Am content, Pu isotopic ratios, chemical composition, eiemental impurities, containment, and fabrication procedures are retained-in files by the Los Alamos National Laboratory CMR Analytical Chemistry Group.
NUCLEAR MATERIAL CONTENT
The nuclear material content and total alpha activity for this standard a re listed below. Also listed are overall uncertainty estimates a t 95% confidence intervals (CI) for each component.
Component PuOz in standard
P u Assay Pu in standard
I4'Am Assay "'Am in standard
Quantity o r Value 5.71060 grams
5.01 168 grams 1128.9 pg/g PuOz*
5.66 mg*
87.761 %'of PuOz*
95 % CI * 0.00021 grams
I O . 0 8 1 % (b) & 0.00472 grams ('I
i 0.3 pg/g (dl
t. 0.04 mg (')
Isotopic Weight Fraction*
'38Pu
"9Pu
"""
'"PU
0.00014
0.93809
0.05939
0.00185
0.00054
I0.000005 ('
i 0.000015('
I 0.000007 ('
i 0.000009 (o
i 0.000003 ('
Total Alpha Activity in standard 342.5 mCi** 1.267E+10 Bq I 3E+07 Bq I 5 0.9 m c i (E)
I *Decay corrected value on 1/21/99 ** Effective 1/21/99
Mi!&+ Robert S. Marshall, Project Manager EDA WRM Production
19
-. -I_.
HNF 405 1 Rev. 2 I
MEASUlUCMIShT METHOD AM) TRACEABILITY
The nuclear COOtCdb of this standard were characterized and quantaed wing the following methods with traceabaty to the National Institute of Standards and Technology (NIST) or New Bruoswick Laboratory (NBL) standards.
Measurement Measurement Method Reference Material
Wcighlng 5 place analytical balance NIST traceable weights h Assay Controlled Potential Coulometry NBL CRM # 126 Am &Y Isotope Dilution Mass Spectrometry NJ3L CkM # 128
Pu Isotopic Total Evaporation Mass Specirometry NBL CRM # 128 Alpha Activity Calculated from Pu and Am ms, and
isotope alpha specific activities listed below. Pu tln as stated for NET S W 4 6
Am tyl as stated for NET SILM4322B
338 3a9 The stated Alpha Activity was calculated using tbe.following isotope half lives (in years): 24,119; Pu: 6,560; ’“Pu: 14.34; Pu: 387,000; and ’“Am: 432.2.
PU: 87.74; Pu: 140 142
NOTES
Random and systematic error teims were combined and reported as 95% confidence intervals. Error t e r m include estimates of the following:
(a) Balance precision, buoyancy, standard wcight bias, and transfer lass. (b) Long and short term precision, control check bias, weighing precbion and bias (c) Above weighing and assay terms, and transfer lass (d) Long a n d short term precision, and bias. (e) Above wcighing t e rm, Am assay terms, and transfer loss. (0 Long and short term precision, and bias. (g) Based on propagated uncertainties on the PU mass, “‘Am mass and PU isotopic uncertainties M e d
above. No half-life uncertainty components a r e included and it is recommended that all facilities participating i n tbc hD.4 PDP program use the half-lives b t e d above to preclude Eacility-to-facility
’crror t c r m introduced by using different half life values.
20
HNF 405 I Rev. 2
Los Alamos National Laboratory Certificate of Content anb. QLrateabiIitp
Pu02-Diatomaceous Earth Standard WRAP-3 5.0GPU
This NDA standard contains high purity plutonium dioxide dispersed in diatomaceous earth. Quantitative information and uncertainties on the nuclear content of this WRM are listed below. Complete information regarding the Pu and Am content, Pu isotopic ratios, chemical composition, clemental impurities, . containment, and fabrication procedures are retainedjn files by the Los Alamos Nalional Laboratory CMR Analytical Chemistry Group.
NUCLEAR MATERIAL CONTENT
The nuclear maferial content and total alpha activity for this standard a re listed below. Also listed are overall uncertainty estimates a t 95% confidence intervals (CI) for each component.
ComDoncnt PuO, i n standard
Pu Assay Pu in standard
'"Am Assay "'Am in standard
Quantity o r Value 5.69429 grams
4.99736 grams 1128.9 pg/g Pu02*
5.64 mg*
87.761 Yo ofPuO,*
95 Yo CI * 0.00031 grams ('I
* 0.081 % (b) * 0.00476 gra'ms ('I
6 0.3 pglg * 0.04 mg (')
Isotopic Weight Fraction*
"'Pu
l'9PU
lraP u
'I'PU
'41Pu
0.00014
0.93809
0.05939 '
0.00185
0.00054
,* 0.000005 (0
* 0.000015 (0
* 0.000009 (0 * 0.000007 "
i 0.000003
Total Alpha Activity i n standard 311.5 mCi'* 1.263Ec10 Bq
i 0.9 mCi (e) 3E+07 Bq ('I
'Decay corrected value on 1121199 ** Eflcctive 1/21/99
B i d J h & erlev, G r o u D h e a b r C h R Analyticai C h e m l i t w
obert S. Marshall, LU&,L3 Project Manager
NDA WRM Production
21
HNF4051 Rev.2
MEASUREMJZNT METHOD AND TRACEABILITY
The nuclear contents of this standard were characterized and quantified wing the following methods with traceability to the National Institute of Standards and Technology (NIST) or New Brunswick Laboratory (NBL) standards.
Measurement Measurement Method Reference Material
Wcighlng 5 place analytical balance NlST traceable weights Pu Assay Controlled Potential Coulometry NBL CRM # 126 Am k Y Isotope Dilution Mass Spectrometry NBL CiRM # 128 Pu Isotopic Total Evaporation Mass Spectrqinetry NBLCRM#128
Alpha Activity Calculated from Pu and Am ma%, and isotope alpba specific activities listed below.
hr tln as stated for NIST SRM946 Am tin as stated for NIST
SRM4322B
ud The stated Alpha Activity WPS calcula!ed using the following isotope half lives (in years): 24,119; "'PP,: 6,560; Pu: 14.34; Pu: 387,000; and"'Am: 432.2.
Pu: 87.74; "$u: 141 242
=S
Random and systematic c r ror t e r m were combined and reported as 95% confidence intervals. Er ror terms include estimates of the following:
(a) Balance precision, buoyancy, standard weight bias, and transfer loss. (b) Long and short term precision, control check bias, weighing precision and bias. (c) Above weighing and assay terms, and transfer loss. (d) Long and short term precision, and bias. (e) Above wcighig terms, Am assay terms, and transfer loss. (0 Long aod short term precision, and bias. (s) Based on propagated unccrtaintics on the Pu mass, "'Am mass and h isotopic uncertainties listed
above. No half-life uncertainly components a re inclnded and i t is recommended that all iacilitiea participating in the ND.4 PDP program use the half-lives listed above to preclude facilitY-td.WiliQ'
. crror t e r m introduced by using different half Life values.
22
HNF 405 I Rev. 2 J
Los Alamos National Laboratory Certifitate of amtent anb. QhateabiIifp
Pu02-Diatomaceous Earth Standard WRAPlOGPU
This NDA standard contains high purity plutonium dioxide dispersed in diatomaceous earth. Quantitative information and uncertainties on the nuclear content of this WRM are listed below. Complete information regardinz the Pu and Am content, Pu isotopic ratios, chemical composition, elemental impurities, containment, and fabrication procedures a re retained i n files by the Los Alamos National Laboratory CMR Analytical Chemlrtry Group.
' ' NUCLEAR MATERIAL CONTENT
The nuclear material content and total alpha activity for this standard are listed below. Also listed a re overall uncertainty estimates a t 95% confidence intervals (CI) for each component.
Component Quantity o r Value 95 % CI PuO, in standard 11.40156 grams * O.OOOd9 grams ('I
P u in standard 10.00612.grams & 0.00945 grams(') Pu Assay 87.761 % of PuOi* * 0.081 % @)
"'Am Assay 1128.9 pg/gPuOl* * 0.3 pp/p (dl
,'"Am in standard 11.30 mg* * 0.09 mg+)
Isotoptc Weigh1 Fraction*
a'aPu 0.00014 * 0.000005
"'PU 0.93809 i 0.000015 ('
"OPU 0.05939 * 0.000007 "
l"Pu 0.00185 * 0.000009
XPu 0.00054 f 0.000003 ('
* 1.8 mCi (8'
* 7Et07 Bq (') Total Alpha Activity in standard 683.7 mCi**
2.530E+10 Bq
*Decay corrected value on 1/21/99 * & Effective 1/21/99
NDA WRM Production
23
_I . . . ..... .. . . . . . -. -
HNF 405 1 Rev. 2
MFASZTREMENT METHOD AND TRACEABILITY
The nuclear contenB of thic standard were characterized and quantified using the following methods with traceability to the National Institute of Standards and Technology (NIST) or New Brunswick Laboratory (NBL) standards.
Measurement Measurement Method Reference Material
W e i gh i n g
Pu &say Controlled Potential Coulometry NBL CRM # 126
5 place analytical balance NISI Paceable weigbh
A m - Y Isotope Dilution Mass Spectrometry Pu Isotopic Tolal Evaporation Mass SpecG9inett-j
NBL CRh? # 128
N B L c R M # 1 2 8 Alpha Activity Calculated &om Pu and Am ma, and
isotope alpha specific activities listed below. Pu tlp. as stated for NIST SRM946
Am tm as stated for NIST SRM4322B
118 The stated Alpha Activity was calculated using the following isotope half lives (in years): 24,119; "'Pu: 6,560; F'u: 14.34; "hu: 387,000; and "'Am: 432.2.
PU: 87.74; "'PU: I41
NOTES
Random and systematic error terms were combined and reported as 95% confidence intervals. E r ro r t e r m include estimates of the following:
(a) Balance precision, buoyancy, standard weight bias, and transfer loss. (b) Long and short term precision, control check bias, weighing precision and bias. (c) Above weighing and assay terms, and transfer loss. (d) Long and sbort term precision, and bias. (e) Above wc igh ig terms, Am assay terms, and transfer loss. (r) Long and short term precision, and bias. (s) Based on propagated uncertainties on the Pu mass, Am mass and Pu &topic uncertainties listed
above. No half-life uncertainty components are inclnded and i t is recommended that all facilities participating in the NDA PDP program use the half-lives listed above to preclude facilitY-t*&cmQ' crror terms introduced by using different half Life values.
1 4 1
24
HNF4051 Rev.2 I
Los Alamos National Laboratory UCertifitate of (Eontent anb ZErateabiIitp
Pu02-Diatomaceous Earth Standard WRAPZOGPU
This NDA standard contalns high purity plutonium dioxide dispersed in diatomaceous earth. Quantitative information and uncertainties on the nuclear content or this WRM are listed below. Complete information regarding the Pu and Am content, Pu isotopic ratios, chemical composition, elimental Impurities, contalnment, and fabrication procedures are retained .in files by the LQS Alamos National Laboratory CMR Analytical Chemistry Group.
NUCLEAR MATERIAL CONTENT
The nuclear material content and total alpha activity for thls standard a re listed below. Also listed a re overall uncertainty estimates a t 95% confidence intervals (CI) for each component.
Component Quantity or Value 95 % (71
Pu Assay 87.761 % of PuO,* * 0.081 % (b)
PuOl in standard 22.19925 grams f 0.00062 grams (I)
Pu In standard 20.00884 grams rt 0.01875 grams '"Am Assay 1128.9 pg/gPu02* * 0.3 pg/g (d)
"'Am in standard 22.59 mg* i 0.17 mg ('I
Isotopic Weight Fraction*
'"PU
u9Pu
lroPu
IJiPU
'JzPu
0.00014
0.93809
0.05939
0.00185
0.00054
* 0.000005 (r)
f 0.000015 (O
rt 0.000007 (O
* 0.000009 (0
i 0.000003
Total Alpha Activity in standard 1367 mCi** 5.059E+10 Bq
i 4 m ~ i (9)
i 1E+08 Bq (e)
*Decay corrected value on 3/21/99 ** Effective 1121199
' * Kerley,Gro p eader CMR Analytical C h e m w y
--,. J Robert S. Marshall, Project Manage M)A WRM Production
HNF 405 1 Rev. 2
MEASUREMENT METHOD AND TRACEABILITY
The nuclear content8 of this standard were characterized and qnantified midg the following methods with traceability to the National Institute of Standards and Technology (NET) o r New B w m k k Laboratory (NEIL) standards.
Measurement Measurement Method Reference Material
Wcighing 5 place analytical balance NISI' traceable weights Pu Assay Controlled Potential Coulometry NBL CRM # 126 Am Isotope Dilution Mass Spectrometry NBL CR&5 # 128
Pu Isotopic Total Evaporation Mess Spectrometry NBL CRM # 128 Alpha Activity Calculated from Pu and Am mass, and
isotope alpha specific activities listed below. Pu tln as stated for NIST SRM946
Am tm as stated for NIST rnX4322B
lJ8 a9 ,The stated Alpha Activity was calculated using the following lrotope half lives (in years): Po: 87.74; PU:
140 mi 142 24,119; Pu: 6,560; Pu: 14.34; Pu: 387,000; and '"Am: 432.2.
NorES
Random and systematic error tcrms wcre combined and reported as 95% confidence intervals. Error terms include estimates of the following:
(a) Balance precision, buoyancy, standard wcight bias, and transfer loss. (b) Loug and short term precision, control check bias, weighing precision aud b i a s (c) Above weighing and assay terms, and transfer loss. (d) Long and short term precision, and bias. (e) Above weighing terms, Am assay terms, and transfer loss. (0 Long and short term precision, and bias. (9) Based on propagated uncertainties on the Pu mass, "'Am m a s s and Pu isotopic uncertainties listed
above. No balf-life uncertainty component$ a re included and it is recommended tha t all facilities participating in thc NDA PDP p r q r a m use the half-lives W e d above to preclude facility-t*faCxV
' crror tcrms introduced by using different half Life values.
26
DISTRIBUTION SHEET ~
To
D i s t r i b u t i o n
From Page 1 of 1 WRAP Engineer ing Date 09/14/99
MG Cantaloub
JK Kersten
JA Maupin
MA Purce l l
WR Thackaberry
CE Tay lo r
JR Weidert
CE W i l l s
DOE/RL Reading Room
Engineer ing F i l e s
Project Title/Work Order
WRAP Q A O ' s FOR NDA, HNF-4051, Rev. 2
T4-52
T4-52
T4-06
T6-50
T4-52
T4-52
T4-52
T4-52
H2-53
81-07
EDTNo. N/A
ECN NO. ECN-651739
X
X
X
X
Name
x X
X
X
Text Text Only Attach./ EDT/ECN MSlN With All Appendix Only
Attach. Only
A-6000-135 (01/93) UEF067
_.. ... . . . ~ . . __