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HNF-4051 Rev 3 Quality Assurance Objectives for NDA at the WRAP N/A

Date 01/27/00

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HNF-4051 Rev 3

Qua I i ty Assu rance 0 bjeCtlVeS for Nondes t ruc t ive Assay at The Waste Receiving and Processing Facility

CB Will. Fluor Hanford Inc Richland Wa 99352 Richland WA 99352 U S Department of Energy Contract DE AC06 96RL13200

EDT/ECN ECN-655134 uc 506 Org Code 3 5 0 0 0 Charge Code AJ60 B&R Code EW02J16 Total Pages &54* iJ27fffo

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

*Genie PC is a registered trademark of Digital E q u l p Corp Huston TX

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2uality Assurnace Ob~ectives for Non-Destructive Assay at the WRAP Facility

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HNF-405 1, Revision 3

Quality Assurance Objectives for Nondestructive Assay at the Waste Receiving and Processing Facility

Crag Wills and Michael G Cantaloub, Fluor Hanford Inc

I

J

HNF4051 Rev 3

Executwe Summaw

The Waste Receiving and Processing (WRAP) facility, located on the Hanford Site m southeast Wastungton is a key llnk m the certificahon of transurmc (TRU) waste for shpment to the Waste Isolation Pilot Plant (WIPP) Waste charactenzahon is one of the viti$ hnchons performed at WRAP, and nondestruchve assay (NDA) measurements of TRU waste contamers is one of two required methods used for waste charactenzahon The Waste Acceptance Cntena for the Waste Isolafion Pilot Plant, DOEYWIPP-069 (WIPP-WAC) delmeates the quality assurance objectives wtuch have been established for NDA measurement systems Sites must demonstrate that the quality assurance objectives can be acheved for each radioassay system over the applicable ranges of measurement

Tlus report summanzes the validahon of the WRAP NDA systems agamt the radioassay quality assurance objectives or QAOs A bnef descnption of the each test and sigmficant conclusions are included Vanables that may have affected test outcomes and system response are also addressed

HNF-4051 REV 3

Table of Contents

Executive Summary Table of Contents Introduction Descnption of Tests Summary of GEA A Tests - Accurancy, Precision and Bias Summary of GEA A Tests - Mlnunum Detectable Concentration Discussion of Results Attachments

11

111

1 4 6

10 11 15

HNF4051 Rev 3

Introducbon

The WRAP facility has four pnmary NDA systems two maging passive/active neutron (IPAN) systems and two gamma energy assay (GEA) systems The two IPAN mts are idenhcal, as are the GEA mts, thus the systems are designated as follows IPAN A, IPAN B, GEA A, and GEA B ThIs report documents the conformance of GEA-A to the precision and accuracy radioassay QAOs, and reports the rrrrmmum detectable concentration (MDC) The QAOs were demonstrated for 55-gallon (208 L) waste contamers only A separate document, HNF-4050 addresses the total measurement uncertamty cluu) for the GEA system whle HNF-5148 addresses system calibration

WIPP sets forth four nomnal testmg pomts for NDA whch are in alpha cunes and grams of weapons grade (WG) Pu-239 Due to the nature of avalable sources WRAP used the nominal WG Pu gram quanhties for testmg This report documents testmg of the GEA-A system at the 0 1 g, 1 0 g 10 g, and 160 g levels for the QAOs wth system calibration established in October of 1998

The MDC was d e t e m e d as a function of waste density and Pu-239 transitions of particular interest Up to five drums contiumng non-interfenng matnx matenal for a density range of 0 046 to 1 56 k g L were assayed The MDC reflects the best sensihmty for a part~cular assay system and specific assay condtions (1 e count hme, sample configmtion) when no added radoactivity is present As such no radioactive sources were required for the MDC determlnation As wth the accuracy and precision QAOs, the MDC is valid for 55-gallon waste contamers only The assay data for the MDC calculations was obtiuned from December 1999 into early January 2000 The instrument response and the documented results are applicable to the current waste stream undergoing analysis at WRAP

Precision and Accuracy

To comply wth QAO reqwrements facilihes must detemne precision and accuracy values obtamed for 15 replicate measurements of appropnate sue mock waste contamers contiumng nominal test quantihes of TRU isotopes dstnbuted in a non-interfenng matnx ThIs must be done for each system whch is to be cerhfied The equations used to determine these values, tabulated later III t lus report, are listed below

Equahon 1 calculates precision as the percent relative standard deviahon (%RSD) of the distnbuhon of 15 replicate measurements

S % RSD= = * 100

Y

where

%RSD = percent relahve standard deviahon, - s = standarddeviation, y = mean of the replicate measurements

Equahon 2 determines the standard deviation

I

HNF-405 1 REV 3

where s = standarddeviabon, - y, = the measured value of the ith replicate measurement, y = the mean of the replicate measurements, n = the number of replicate measurements

Equabon 3 determines the accuracy as percent recovery for replicate measurements

% R = * 100 C,

where %R = percentrecovery, C, = average result of 15 replicate determinabons, C, = known value for the isotope standard used ln the replicate measurements

Mmmum Detectable Concentrabon

The WIPP-WAC defines the MDC as that radioactivity concentrabon whlch, if present, yields a measured value greater than the cntical level wth 95% probability, where the cntical level is defined as that value whch measurements of the background wll exceed wth 5% probability No value is specified for the MDC TRU waste destlned for WIPP must have a TRU alpha activity concentration greater than 100 nCdg The MDC for the waste stream and the assay condibons must be less than the TRU alpha concentrabon determined rn the waste contamer Instruments performing TRUAow-level waste discminabon measurements must effectively have an MDC of 100 nCdg or less Th~s sets an effectwe ‘mmmum’ MDC of 100 nCdg

Equation 4 gives the base expression used for d e t e m g the MDC

MDC = K,(2 71+4 65 * s b )

where

KI = propomonality constant relabng the detector respnse (counts) to actiwty concentration KI lncorporates factors such as the detecbon efficiency and branclung rabo for the gamma ray under conslderabon, the collection live time, waste weight and conversion factors The magmtude of KI is expected to change depending on the charactenstics of the waste matnx (e g density) as t h ~ s affects detecbon efficiency

sb = the standard deviahon or uncertiunty of the background

With respect to equation 4, the standard deviabon of the background is determined as

2

HNF-4051 REV 3

where

counts CR Tc = count tune (real tune) for the assay (second)

= the total counts acqured m the region of interest for a photon of energy E, = count rate in the region of mterest for a photon of energy E (cps),

Substituting terms appropnate for gamma spectroscopy (GEA) into KI yields a final equation (Equahon 5) for representing the MDC for the GEA system

where

CR&) = Tc - e(Er) I&) = M = 37 =

count rate in the region of interest for a photon of energy E (cps), count hme for the assay (second), the detection efficiency for the photon of energy E (countdphoton) yield or intensity for the photon of energy E(photonkecond), mass of the drum waste matnx (g), conversion factor relating decays per second to nCi (dpdnci)

- - -

%le equation 5 is the base equahon for MDC calculations, it was not explicitly evaluated in determimng the assay MDC values The GEA system software sute (Canbem G e m PC) calculates and reports a m m w n detectable activity (MDA) for nuclides listed m the analysis library, but not idenhfied in the sample spectrum If a specified peak exceeds the decision level inherent in equation 5 the software reports the nuclide othennse the MDA for the nuclide is reported The system operahng manual (Geme-PC Volume Two, Algonthms Appendix B) descnbes the analysis algonthm The MDA value reported is determmd from expressions identical to equaoon 4 and 5 ) As configured at WRAP, the software reprt provldes an MDA (in @I) for all 'undetected' radionuclides listed in the search library The system reported MDA can be converted to a MDC by use of the appropnate waste matnx mass and conversion factor as shown in equation 6

MDA(E,)* 1000 M*1000

MDC(E,) =

where

MDC&) = mimmum detectable concentration for a specific nuclide based upon emssion of a photon of energy E (ncdg),

3

HNF4051REV3

system reported m i m u m detectable activity for the specified nuclide photon of energy E (pCi) mass of the waste matnx (kg) conversion factor relatmg nCi to pCi and kg to grams -1000 nCdpCi, 1000 g per kg (nC1 k&Wig)

MDA(E+) =

M 1000/1000 =

- -

Descnphon of Tests

Precision and Accuracy

For testing of the NDA systems agamst the WIPP QAO requirements, the PDP “combushbles” matnx drum was loaded wth sources to apprommate the nommal test pomts Selechon of the combushbles drum was based upon its having the nearest apprommation to the prevalent waste stream matnx being processed at WRAP The table below shows the arrangement of sources wthm the test drum The test arrangement number (e g , QA021) is shown in the next section where specific test results are tabulated

The ‘T and “F”‘ references are to tube number and pin height, respechvely Tube 1 is centered in the drum, whle tube 2 is located about halfway between the center and the outer wall of the drum Tube

4

HNF4051REV3

3 is located near the outer wall of the drum, opposite tube 2 The pm numbers refer to height (m inches) above the bottom of the drum at whch the source is placed The sources are composed of Pu dispersed III diatomaceous earth, doubly enclosed m concentnc stamless steel cylinders They are m e inches long and about two inches in diameter Sources are of two “ongins” Sources identified as NTP were from completed PDP cycles as authonzed m the WIPP-WAC (DOWPP-069,

Appendix A) Sources designated ‘WRAP’ were purchased by WRAP for NDA (GEA and IPAN) operations and were not part of the PDP cycle All assays were performed using the WRAP GEA operahng procedure (Wl-OP-0906)

MDC

The GEA system MDC was determined from replicate measurements of drums over a matnx density of 0 046 to 1 56 k g L (g/cm3) The drum matnx was urnform and contamed no lstnbuted radioactive sources or mterfenng components Addihonally, no raloactwe sources were added to the drums Data was acqlured for 15 replicate assays at three different drum densifies using a nominal (5 minute) countmg tune AdlQonally two 60-minute assays were performed on the same set of drums The system reported MDA values (pCi) were converted to MDC values through equafion 6 and the appropnate drum mass As above, all assays conducted for the MDC determinahon were performed in accordance wth the WRAP GEA operahng procedure (Wl-OP-0906)

Test Results

Results for the GEA-A system are presented in tabular and graphcal form on the followmg pages Tables for the precision and accuracy QAOs are addressed first The results of the MDC determinations appear next

5

HNF-405 1 REV 3

Preclslon Accuracy * Total Bias

Summary of GEA A Tests - Accuracv and Precision

GEA A 160 00 g Pu (160 g nommal test value) 93 8% Pu-239

std dev = 7 39E-01

%R = 78 83 78 08% (Low) to 79 69% (High)

std dev = 1 28E+OO

%R = 82 35 80 66% (Low) to 83 77% (High)

%RSD =062 % R S D = 1 0 3

6

HNF 4051 REV 3

GEA A 9 90 g PU (1 0 g nominal test value) 94% Pu-239

Precision Accuracy * Total Bias

I I I I I I Average 1 449EM5 I 724EMO I 77 77 I 541EM5 I 872E+00 I 93 69

std dev = 1 26501 %RSD = I 74

74 48% (Low) to 80 02% (High)

stddev = 144E 01 %RSD = 165

90 24% (Low) to 96 13% (High) %R =7777 %R =93 69

7

% Actual Pu 239 Value

-

86 78 92 32 89 89 86 78 89 72 91 45 91 28 97 34 86 08 81 75 74 65 71 53 82 27 84 18 84 87

86 06

QAOZO Sum Seg Pu 239 Mass % Actual Pu Comb All Pu 239 Mass Activity (9) 239 Value Activity (g)

(FCO (PCO

8

Precision Accuracy * Total Bias

std dev = 8 78E 02

%R = 77 03 46 25% (Low) to 85 56% (High)

std dev = 6 25E-02

%R = 86 06 71 53% (Low) to 97 34% (High)

%RSD=1225 % RSD= 7 80

HNF-405 1 REV 3

Run 13 Run 14 Run 15

Average

GEA A 0 09 g Pu (0 1 g nominal test value) 94% Pu-239

5 29EM3 8 53E-02 101 33 5 29EM3 8 53E-02 3 95EM3 6 37E02 75 66 7 34EM2 1 18E02 3 06EM3 4 93E02 58 61 1 26EM3 2 03E 02

4 12EM3 664E 02 78 90 1 92EM3 3 09E02

Precision Accuracy * Total Bias

% Actual h- 239 Value

21 84 82 94 I9 54 21 45 9 86 8 20 9 50 29 69 27 20 71 26 90 98 18 91

101 33 I4 06 24 13

36 73

std dev = 1 18502 % RSD = 17 79

%R = 78 48 51 33%(Low)to 101 33%(Hieh)

std dev = 2 72E02 % RSD= 87 94

%R = 36 53 8 20% (Low) to 101 33% (Hi&)

9

HNF-4051 REV 3

Summary of GEA A Tests - Minimum Detectable Concentrahon

Figure 1 shows MDC determinahons as a funcbon of a non-interfenng matnx density for Pu-239B (414 keV) and Pu-239A (129 keV) Each data point represents the average, software 'sum segments' MDA value for 15 replicate measurements, adjusted per equation 6 to yield an MDC The smooth curves are power function fits of the data pomts The MDC d e t e m e d using the lightest matnx

Pu 2398 (414 keV) Pu 239A (129 keV)

MDC = 15 84(density) MDC = 5 74(density) 063 R2 = 0 98 R2 = 0 99

0 00 0 20 0 40 0 60 0 80 1 00 120 1 40 1 60

Drum matrix density (kglL)

I

I I

Figure 1 Minimum Detectable Concentration (MDC) as a function of drum

Data is the average sum segment from 15 replicate measurements at a nominal count time of five minutes

matrix density based on Pu 239A (129 keV) and Pu 239B (414 keV) peaks I

(0 046 kgL -first data point) is 40 nCdg for the 129 keV peak of Pu (Pu-239A) and 130 nCdg for the 414 keV Pu-239 emssion (Pu-239B) It is worth notmg that the MDC determined from the 129 keV data is in excellent agreement wth the 39 f 2 nCdg value reported in rension 2 of t h ~ s document The 100 nCdg effective lower limt for the MDC would clearly be met for all waste densities for assay results based upon the 129 keV Pu-239 emission For the 414 keV peak, the data indicates that the 100 nCdg m i m u m h4DC would be met for all but the lightest density waste Based upon the displayed regression, a waste density of 0 068 or - 0 07 kgL yields a 100 nCdg, TRU-low level waste MDC cutoff cntena Based upon a review of over 100 waste stream drums assayed at WRAP, the average waste density is 0 24 kgL, w~th a m i m u m observed density of 0 094 kgL More than 95% of the waste drums assayed to date had waste densities greater than 0 10 kgL

Using the actual waste densities and the power function determined in Figure 1, the expected MDCs for the current waste stream utihzmg the Pu-239B and Pu-239A lmes (414 and 129 keV respectively) can be determined Figure 2 shows thls data The largest MDC of 80 nCdg would occur at an

IO

HNF-4051 REV 3

observed waste density of 0 094 kg/L For 98% of the waste drums assayed at WRAP to date, the maxllllum MDC would be 66 and 21 nCdg as determined from the 414 keV and 129 keV Pu-239 lmes respectively

~~ ~ Pu 239B (414 keV) 125

~~ nroC=IW*

Mx)=574afisltyp

100 - ~

DPU 239A (129 keV line) ~~~~

~ ~ 50 ~~

~

, 0 , 0 00 0 20 0 40 0 60 0 80 1 00 I 20 1 40 1 60

Measured Drum Waste Density (kglL)

Figure 2 Minimum detectable concentrations for Pu 2398 (414 keV) 8 Pu 239A (129 keV) calculated for processed waste densities using the derived MDC function for 5 minute assays I

I

Discussion of Results

The followng table taken from Table E-1 of HNF-2600, Hanford Sire Transuranic Waste CertrJicafzon Plan gives the precision and accuracy QAO validation requirements

Nominal Parameter compliance

Ranae of waste Point Precision' Accuracp activitv in a-Cunesa (%RSD) (%R) ' a-Curiesa (g WG P u ) ~ 0 to 0 02 0 008 ~~ <20 70-1 30 -

70-1 30 (0 1)

>o 02 to 0 2 0 08 - 4 5 (1 0)

>o 2 to2 0 0 8 - < I O (10)

>2 0 12 8 - <5 (160)

70-1 30

70-1 30

a Applicable range of TRU activity in a 208 L (55gal )waste container to which the QAOs apply untts are Cunes of alphaemitting TRU isotopes with half lives greater than 20 years

HNF-4051 REV 3

The nominal activity (or weight of Pu) used to demonstrate that QAOs can be achieved for the corresponding range in mlumn 1 Values in parentheses are the appropriate equivalent weights of weapons grade plutonium (wc Pu) 15 years after punfication for purposes of demonstrattng QAOs nominal means within i50 percent except for the highest range where nominal means Y 5 percent

i One standard deviatton based on 15 replicate measurements of a noninterfenng matnx The calculated standard deviabon is compared with the mean measured value of the QAO source to obtain the %RSD

Percent recovery(%R) determined from the ratio of measured to known values based on the average of 15 replicate measurements of a noninteanng matnx

It should be noted that a nomnterfenng matnx is a wlual lmpossibility In the case of WRAP a light (debns or combusbbles) matnx was used, whle the interference of tlus matnx is relatively small, it exists nonetheless Of greater concern are the test sources themselves Even if an empty drum matnx was used the two walls of strunless steel surrounding the Pu source matenal does attenuate gamma flux The pnmary energy h e 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 pnmary energy line becomes 129 keV since it has a sipficantly hgher yield fraction than the 414 keV line This relatively low (129 keV) energy llne can be easily attenuated by the encapsulatmg steel walls of the source A prelmlnary review of test results shows tlus effect to be about 10-15%

Precision and Accuracy

Companson of the results tabulated earlier agamst the reqlurements 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 Results’ fals at the 0 1 g level For GEA A, the Comblne All Results” algonthm is preferred at all save the lowest gram levels, at appronmately 0 5 g Pu the “Sum Segments” algonthm takes over In the GEA, “Sum Segments” is also preferred for a lumped source up to about 2 g Pu The table below summanzes the results, and shows the operating range for each system and for each method or algonthm Results outside these ranges reqlure validabon through further testing

Nominal Pu Value

0 l o g 1 oog

l0Og 160 g

Pu Mass GEA Range Combine All Sum Segments

0- 0 2 5 g r UI I’ I \ \

0 2 5 - 2 5 8 I’ I\\ P I\*

2 5 - 2 5 g I’rrr I’ I \ \

> 2 5 g I’ I\< I’ I \ \

All testmg was performed using the WRAP GEA operating procedure (WRP1-OP-0906) The standard operatlng software for the system was used to acquire data and report results Testmg was performed for 55-gallon (208 liter) waste drum configurations only

For these results to be valid, 111 independence of source matenals must be mantamed The QAO tests were performed using plutomum sources, each \nth its own pedigree and documentabon The GEA calibrahons ublize mixed sources contamng CO-60 Ba-133, Ce-137, and Am-241 No sources used in calibrabon are used in QAO validation

HNF-4051 REV 3

Mimmum Detectable Concentration

The MDC curves presented in Figure 1 and Figure 2 demonstrate the effect of matnx density on the

e MDC (nCilg) 5 minute count (routine)

-120 -- ’ MDC (nCiIg) 1 hour count time ~ -~ ~

2 ,A l - a 0 A MDA (uCi) I hour count ,- $js I’

-7

, , ,

~ ~~ ~

I 1200; I -

The curves in figure 3 are consistent wth the expected instrument response and equabons 5-6 for MDC and MDA Plotting the MDA (pCi) values along wth the MDC for the one-hour assays illustrates several lmportant factors From the MDC plot, one might conclude that assay sensibnty mcreases wth increasing matnx density The MDA plot in Figure 4 demonstrates the true response As drum density mcreases, the magmtude of the measured MDA increases, whch is eqwvalent to a decrease m assay sensihvlty Thls is consistent wth the factors contnbutmg to MDC and MDA The first is the drop m detector efficiency wth increased matnx density Efficiency appears in the denominator of equation 5 The detection efficiency drops as a result of increased attenuahon by the

13

HNF-4051 REV 3

sample matnx necessitating an increase in the MDA In other words, more activity is requlred for the true signal to be reliably recogmzed as a true signal

The increase in waste density also contnbutes to a loss m assay sensihvity as result of increased background Sources of background at WRAP include the natural radiation m the budding matenals, includmg the detector and matenals around the facility Radiahon from manmade radionuclides onginating fkom adjacent waste drums may also contnbute to h s background The mcrease in matnx density does not change the background radiahon flux at the detector Rather having a more dense matnx increases the probability of these emissions interactmg wth the matnx and being detected as either discrete lines or contnbutmg to the detector continuum

The combined effect of increased interactions of the background radiation and the decreased efficiency associated wth a more dense matnx, results in the loss of measurement sensihvity Th~s is illustrated by the increase in MDA values wth density Yet the MDC decreases w~th matnx density This is a direct result of the MDC being defined as a concentrahon, having mass (grams) as its basis Waste mass is directly proportional to waste density wth the net effect bemg the decrease m the MDC wth increasing waste mass despite the loss of assay sensitwity The power function regressions in figure 1 help illustrate the effect If the MDC were solely a fimction of sample density (I e detection efficiency and background were independent of density) the regression formulae would show an x ' or kgK ' [I/(kgiL,)] dependence

One final comment on MDC for the GEA systems is prudent It must be remember that the mimmum detectable concentration value is an aprzon eshmate of the m i m u m activity that would result in a net signal that could be reliably quanhfied by the GEA system It is dependent on both the samples being analyzed, and the parameters of the assay (e g count time) and is thus specific for the part~cular assay condibon

14

HNF 4051 Rev 3

0J.erfifirnfe nf &dent anh ‘Illraceabilrfg

Department of Energy Cnrlsbad Area Office ’Worhng Reference Material # NTP-0068

PuO2-Diatornaceous Enrth

This Worhing Reference Materill (WRM) contaiiis high purity plutonium dioxide dispersed In diitomaceour ear th Quinti tative information nnd uncertainties on the nuclear content of this WRM nre listed below Complete Information regnrdlng the Pu and Am content, Pu Isotopic ratios, chemical composition, elementnl inipurities, containment, n n d WRM Inbrication procedure i s described in the NDA PDP W R M Phase 1 Production Plan, CST 8 PLA STD 104, and In files reliined n t tlic Idnlio hational Engineering Laborator) by the Locl.heed Marlin Idnho Technology Co Transuranic Wiste Department and a t the Los Alimos National Laboratory Inorganic Ciementil Analysis C r o u p

M ,*

NUCLEAR MATERIAL CONTENT

T h e nuclear m i t e r i i l content nnd total nlphi nctitity Tor this WRM arc llsted belor3 Also listed nre overall uncertainty estimates a t 93% confidence intervnls (CI) for each componenl

Component PuO, i n WRM Pu Assny Pu i n W R M ’“Am Ass?)

“‘Am in WRhI

Quantitv or Vnlue 0 03405 grams

87 s27 Yo of PUO, 0 02993 grams

766 7 pglgPuO,* 0 0361 mg

95 % CI t 0 OOOOS grams I 1

rt 0 072 % tbl 5 0 00007 grams (4

-L 2 2 pglg (9 i- 0 00012 mg

Isotopic Weight Fraction

U’PU 0 000145

W’PU 0 937614

‘“P u 0 059445

’“PU 0 002237” ‘ Pu 0 000559

5 0 000008 (0

t 0 000013

~ l Y o o o o o s ~ Q t 0 00000s (0

& 0 000001 (0

Toti l Alpha Actitin i n Jl’Rhl 2 30s mCi*” S 5dlC+O7 Bq

= 0 009 m c i (a1 & 3L~05 Bq

*hleisured , d u e on 711519. * * Errccti , e 7/15/95

HNF-4051 Rev 3

JVIVICASURCMENT METHOD AND TRACEABILITY

T h e nuclear coiitcnls of thls W R M were characterized nnd quantified using the folloiving methods with traceability to the National Institute o l Standards and Tcchnology (NIST) o r New Brunsvricl. Laborator) (NDL) standards .

Measurementr Measuremenl Melliod -c ,

Weighlng 5 place analytical balance

Reference FrIiteri?l

NIST traceable ~ c i g h t s Pu Assay Controlled Potential Coulomctrj h B L CRM f 126

Ani Assa) Isotope Dilution Mass Spectrometry NRL CRM f 128

Pu 'Isotopic Total Evaporation Mass Speclrometry NBL CRhI # 128 Alpha Activity Calculated from P u a n d Am mass, and

isotope olphn specific activities listed below Pu t,, as staled forNISTSRM916

Am ti, ns slated for NIST SRM4323B

113 119 The stated Alph? Activity \>as calculated using the following isotope half lives (in years) 21,119, 3J0Pu 6,560, Pu 14 34,

Pu 87 74, Pu 1JI 341 Pu 387,000, a n d l4’Am 432 2

NOTES Rnndom nnd systematic error terms were combined and reported as93% confidenceintervals E r r o r terms include estimates o l the following

(n) Balance precision, buoyincj, standard weight bias (b) Lone n n d short term precision, control checl bins, weighing precision and bias (c) Above weighing and nssay terms, and corrections for transler loss (d) Long and short term precision, and bins (e) Above lbeighlng terms, Am assay terms, and corrections lor transfer loss (0 Long mid short term precision, and bias (g) h s e d on propag?ted uncertainties on the P u mass, 241Am mass and Pu isotopic uncertainties listed

abobc ho halflife unccrlaint} components a r c included and it i s recommended that all facililies participating i n the hDA PDP program use thc half li\es listed above to preclude facililj to facil io error terms introduced b) using different half life values

HNF 4051 Rev 3

- 95 ?A ct Comooneot guan t i tv or Value

t 0 00012 g r a m s I

t 0 00011 g r a m s io

0 03602 gram3

0 03163 grams

0 0276 mg

PuO, in WRbM

Pu i n W R M Pu Assay 87 827 %Of PuO, * 0 0 7 2 % Ibi

"'Am Assay, 7 6 6 7 pg/g PuO,* *22pg/gtdd' I 0 00016 mg1'I 1 a''Am i n W R M

I Isotopic Weight Fraction

Cerfificnte of Cunfenf nnb Krncenbrlrtn w

"Pu

U'PU

'UP u

"'Pu

0 000115

0 937615

0 059145

0 00??37*

1"Pu 0 000539

Total Alpha Activity in WRhl 2 339 mCP' 9 026E+07 Bq

* 0 000008 in

t O O O O O 1 3 ' ~

t 0 000005'0

I 0 000008 1"

I 0 000004 (0

'Measured balue on 7/15/95 .* Eflectibe 711519s

Robert S Varshail Prolect M a n a e e r Inorganic ElementaiAn~al\sis

17

HNF-4051 Rev 3

- JVIEASUREMCNT M E r H O D AND TRACEADIL3TY

The nuclcar contenls of this W R M were characterized end quantified using the following mcthods with traceability to the National Institute of Standards and Technology (NIST) or New Brunswich Laboratory (NBL) standards .

pleasuremen\: .Measurement Method 4

Reference MiteriTl

Welghlng 5 place analytical balance NIST traceable vclghts Pu Assay Controlled Potential Coulomclr) h B L CRM f: 126 Ant Assay Isotope Dilution Mass Spectrometry NELCRMP 128 Pu Isotoplc Total Evaporation Mass Spectrometry NBL CRbI f: 128

Alphi ActivlW Cnlculated from Pu and Am mass, and isotope alphn specific acltvlties listed bclow

Pu t,, as staled for NIST SRM946 Am ti, ns stated lor NIST SRM4322B

111 The slated Alplii Ac,t!b'Ity $)as calculated using the fdfovllng isotope half lives (In )ears) 24,119, '"Pu 6,560, Pu 14 34, "'Pu 387,000, and 1 Am 432 2

Pu 87 74, '"Pu

NOTES

Rnndom and systematic error terms were combined and reported as 93% confidence intervals Error terms include estimates 01 the following

(n) Bnlance precision, buoynncy, slandard weight bias (b) Long and short term precision, control cliecl bias, weighing precision and bias (c) Above rseighlng nnd essay terms, and corrections for t ranskr loss (d) Long and shorl term precision, and bins (e) Above weighing terms, Am ussay terms, and corrections lor transrer loss (0 Long and short term precision, and bias (9) Bnscd on propagited uncertainties on thc Pu mass, 24lAm mass and Pu isotopic uncertainties listed

abose ho halflife uncertaint) components a r c included and I t IS recommended that all facililies participntingin the NDA PDP program use the half Ines lisled above to precludc facilitj to facility error terms lnlroduced b) using different half life values

HNF 4051 Rev 3

Department of Energ) CnrIsbTd Area Office W o r h n g Reference Material # NTP-0075

Pu02-Diatomnceous Earth

This Worhing Reference Material (WRiV) contains high purity plutonium dioxide dispersed in diatomnceous ea r th Quantltative information a n d uncerti inties on t h e nuclear content of this WRhI a r e listed belor5 Complete information regarding the P u a n d A m content, Pu isotopic rntios, chemical composition, elementil impurities, containment, and W R M fabrication procedure is described in the N D A PDP WRM Phase 1 Production Plan, CST 8 PLA STD 104, a n d i n files retained a t the Id iho National Engineering Laborntory by the Lockheed Martin Idaho Technology Co Transu ran ic Waste Department and a t the Los Alamos Nitionnl Laboratory Inorg2nic Elemental Analysis G r o u p

NUCLEAR M A T E R I A L COX'TENT

T h e nuclear material content a n d total a lpha activity fo r this WRM are listed below Also listed a r e overall uncerti int) estimates at 95% confidence intervals (CI) fo r each component

Component Q u i n t i t v or Value 95 % C I PuO, i n WRM 0 03391 g r i m s f 0 00006 g rams ('I

Pu in WRM 0 02978 g rams f t D 00006 grams'" P u Assay 87 827 Yo OtPuO, t 0 072 % Ib)

"'Am Ass?) 166 I pglg PuO,* f 2 2 pglg "'Am in lVRM 0 0260 mg tao0011 mg")

Isotopic Weight Fraction

JPU a 000145 "9Pu 0 937614

"SPu 0 059413

"Pu a o o m 7 -

' Pu 0 000559

f 0 000008 (0

f 0 000013 (O

f 0 000005 (0

t 0 00000s (0

= 0 000004 (0

Total Alphi Actnit) i n WRM 2 296 rnCi*" = 0 009 niCi " S 497C-07 Bq - 3EL05 Bq '

"h Ievured k i l u e on 7/15/93 *" E f i e c t n e 7/15/93

;< tc..&Y/W*/ Robert S hlarshall Proiect Min iee r

L

hDA PDP WRhI Production

19

HNF-4051 Rev 3

MEASUREMENT METHOD AND TRACEAUILITY

The nucleir contents of this W R M \yere characterized and quantified using the following methods with traceibility to the National Institute of Standirds and Technology (NIST) or New Brunswich Laboratory (NBL) standards

Measurement Measurement Method Reference M i t e r i i l

Weighing 5 place analytical balance NIST traceable weights

Pu Assay Controlled Potential Coulometrj h B L C R M # 126 Ani Assay Isotope Dilution Mass Spectrometry NBL C R M # 128 Pu Isotopic Total Evaporation Mass Spectrometry NBL CWI t: 128

Alpha Activity Calculated from Pu and Am mass, and isotope alpha specific activities listed below

Pu t,, as stoted for NIST SRM946 Am ti,. ns stated for NIST SRM4322B

218 a19 The stated Alphi Activity \)as calculated using the following isotope half lives (in qenrs) 21,119, Pu 6,560, Pu 14 34, Pu 387,000, andaJiAm 4322

Pu 87 74, Pu a m a i i 2dl

NOTCS

Random and systematic e r r o r terms were combined and reported as 93% confidence intervals E r r o r terms include estimates of the following

(a) Balance precision, buoyincy, s tandard weight bias (b) Long nnd short term precision, control cliecl bias, weighing precisian and bias (c) Above weighing and assay terms, and corrections for transfer loss (d) Long and short term preclsion, a n d bias ( e ) Above weighing terms, Am assay terms, and corrections for transfer loss (0 Long and short term precision, and bias (g) Bired on propagated uncertainties on the Pu mass, 24lAm mass and Pu isotopic uncertainties listed

aboie ho half life uncertaint i components are included and i t is recommended tha t all facilities participating i n the NDA P D P program use the half lives listed above to preclude facilit) to facility error terms introduced by using different half life values

HNF4051 Rev 3

aerirfirnte af Guitfenf anb 'IUmceattrltfo =

Department of Energy Carlsbad Area Office Worlung Reference Material # NTP-0077

PuOz-Diatomaceous Earth

This Worklng Rererence Material (WRM) contains high purity plutonium dioxide dispersed in diatomaceous earth Quantitative information and uncertainties on the nuclear content of this WRU a r e listed belo% Complete information regarding the Pu and Am content, Pu isotopic r~ t ios , chemical composition, elemental impurities, containment, and WRM fabrication procedure is described In the NDA PDP WRM Phase 1 Production Plan, CST 8 PLA-STD 104 and in files retained at the Idaho National Engineering Laborator\ by the Cockheed Martin Idaho Technology Co Transuranic Waste Department and at the Los Alamos National Laboratory Inorganic Elemental Analysis Group

h U C L E 4 R hlATERIAL CONTEhT

The nuclear material content and total alpha activity for this WRM are listed below Also listed a r e o\erall uncertainty estimates a t 95% confidence inter\als (Ct) for each componenL

ComDonenr , Quanta) or Value 95 % CI PuO, in WRM 0 03355 grams * 0 00006 grams '

87 827 % or PUO, Pu in WRM 0 02946 grams * 0 00006 grams

766 7 pg/g PuO,' "'Am In WRM 0 0257 mg *000011 mg"'

Pu Assay I O 072 % 'bl

"'Am Assay * 2 2 pg/g Id)

Isotopic Weight Fraction

U'PU

1"Pu

"OPU

"'Pu

I' Pu

0 000143

0 937614

0 059445

0 002237"

0 000559

I Total Alpha Activity in WRM 2 272 mCP* 8.107E+07 Bq

I 0 000008 (0

* 0 000013 VI L 0 000005 io

5 0 000008 ' O

I 0 000004 1"

-L o 009 m c i '1'

-L 3E+O5 Bq I:' I I ''Measured value on 7/15/95 ** Effective 7/15/9>

L7ddSjk?d& Robert S Marshall, Proiect Manaeer - I I

hD4 PDP WRM Production

21

HNF 4051 Rev 3

MEASUREMENT METHOD AND TRACEABILITY

T h e nuc le i r contents or this WRM were characterized and quantified using the following methods with traceability to the National Institute of S t a n d i r d s a n d Technology (NIST) o r New Brunwick Labora tor ) (NBL) standards .

Measurement Measurement Method Reference M i t e r n 1

Weighing 5 place analylical balance NIST traceable \$eights

Pu Assay Controlled Potential Coulometr) h B L C R M # 126

Ani Assay Isotope Dilution Mass Spectrometry N U C R M # 128

Pu Isotopic Total Evnporation Mass Spectrometry NBL CRM f: 128

Alpha ActiviW Cnlculnted from P u a n d A m mass, and isotope a lpha specinc activities listed below

Pu ti, as staled for N E T SRM9-16 Am ti, ns stated for NIST SRhIJ322B

111 119 T h e slated Alphi Activity \)as calculated using the following isotope half lives (in )ears) 21,119, Pu 6,560, Pu 1434, Pu 387,000, andZ4 'Am 4322

P u 87 74, P u u a 1 4 1 241

NOTES Random and systematic e r ro r terms were combined a n d reported as 95% conndence intervals E r r o r terms include estimates or the following

(n) Balance precision, buoynncy, s tandard weight bias (b) Long and short term precision, control checl bins, weighing precision and bias (c) Above ~ e i g h i n g and assay terms, and corrections fo r transfer loss (d) Long and short term precision, a n d bias (e) Above weighing terms, Am assay terms, a n d corrections for transfer loss ( f ) Long and short term precision, and bias (g) Bised on propagqted uncertainties on the Pu mass, 2-11Am mass and Pu isotopic uncertainties listed

a b o i e h o half life uncerlaint) components a r e Included and it is recommended tha t all facilities pirticipating in the NDA PDP program use the ha l f lives listed above to preclude facilitj to facilit) e r ro r terms introduced b} using different ha l f life values

22

HNF 4051 Rev 3

Merfrficnie of Gonfenf nnb tErucenbtltfg

Department of Energj Carlsbad Area Office Worlung Reference Material # NTP-0083

Pu02-Diatomaceous Earth

This Working Reference Material (WRhI)contalnr high purity plutonium dioxide dispersed i n diatomnccou, earth Q u a n t i t a h e information and uncertainties o n the nuclear content of this \VRM a r e listed belou Complete Information regarding the Pu and Am content Pu Isotopic ratios, chemical composition, elernenid1 impurities, containment, and WRM fabrication procedure IS described in the NDA PDP W R M Phase I Production Plan, CST 8 PLA STD 104 and i n tiles retained a t the ldaho National Engineering Laborsior, by the Lochheed lrlartin ldaho Technology Co Transuranic Waste Department and at the Los Ahrnos National Labora tow Inorganic Elemental Analysis Group

hUCLE'4R MATERIAL COWENT

T h e nuclear material content and total alpha activitv for this W R M are listed belon Also listed a r e overall uncertainty estimates a t 95% confidence intervals (CI) for each component

Cornvonent P u O i n W R M

Pu Assay Pu i n WRM "'Am Assay

'"Am i n W R M

Isotopic Weight Fraction

"'Pu

U'PU

"QPU

1"Pu

"'Pu

Total Alpha Activity i n WRM

Quant i ty or Value 0 03191 grams

0 03066 grams 766 7 p& $uO,'

0 0268 mg

87 827 % Of PUO,

0 000145

0 937614

0 059445

0 002237"

0 000559

2 361 mCi-• 8 747Et07 Bq

95 % ci * 0 00007 grams '

5 0 072 % Ib1

* 0 00006 g rams * 2 ? pglg Id)

-L 0 00011 mg'"

f 0 000008

* 0 000013 Io

-L 0 000005

* 0 000008

-L 0 000004 '0

.L 0 009 mCi * 3E+Os Bq (I i

I I

*hleasured \slue on 7/15/95 ** Effective 7/15/95

n

/

cKerlej , G r o a e a d e r Inorganic Elemental Analysis

rj&A&L%@ Robert S Marshall Project hlanager hDA PDP WRM Production

23

HNF-4051 Rev 3

MEASUREMENT METHOD AND TRACEABILITY

The nuclcar contents of this W R M were characterized arid quantified using thc following methods with traceability to the National Institute of Standlrds and Technology (NIST) o r New Brunswich Laboratory (NBL) standards

Measurement Measurement Method Reference Miteri-il

Weighing 5 place analytical balance NIST traceable \$eights

Pu Assay Controlled Potential Coulomctrj h B L C R M f: 126

Ani Assay Isotope Dilution Mass Spectrometry NRL CRM t: 128

Pu Isotopic Total Evaporation Mass Spectrometry NBL CmI t: 128

Alpha Activity Calculated from Pu and Am mass, and isotope alpha specific activities listed below

Pu ti, as stated for NIST SRR.1946 Am ti, ns stated for NIST SRM4322B

113 119 The stated Alph? Activity was calculated using the following isotope half lives (in )ears) 24,119, "'Pu 6,560,

Pu 87 74, Pu 1 J I 1 4 2 Pu 14 34, Pu 387,000, and '"Am 432 2

NOTES

Random nnd systematic error terms were combined and reported as 93% confidence intervnls E r r o r terms include estimates of the following

( 7 ) Balance precision, buoyancy, s tandard weight bias (b) Long and short term precision, control checl bias, weighing precision and bias (c) Above weighing and assay terms, and corrections for transfer loss (d) Long and short term precision, and bias (e) Above weighing terms, Am ussay terms, and corrections for translcr loss (0 Long and short term precision, and bias (9) Bised on propagated uncertainties on thc Pu mass, 241Am mass and Pu isotopic uncertainties listed

abose h o half life uncertaintj components are included and it i s recommended tha t all facilitics participating I n the NDA PDP program use the half lives listed above to preclude facilitj to facilitj error terms Introduced by using different half life yalucs

24

HNF 4051 Rev 3

Department of Energy Cqrlsbad Are? Office Working Reference Material t: NTP-0089

PuOz-Diatomaceous Enrth

This Worhing Reference Material (WRM) contains high pui i ty plutonium diovide dispersed In diatomaceous ear th Quantitative information nnd uncertainties o n the nuclear content of this W R M a r e listed below Complcte information regarding the Pu nnd Ani content, Pu isotopic ratios, clieniicil composition, elcment?I impurities, containment, and WRM f-ibrication procedure i s described in the NDA P D P WRM Pl i i se 1 Production P l in , CST 8 PLA STD 104, nnd in files retained at the Idaho Nstionnl Engineering Laborn to ry by the Lochheed Mir t in Idaho Technology Co Trnnsuranic Waste Department and at the Los Alamos National Laboratory Inorganic Elemental Anilysis G r o u p

NUCLEAR M A T E R I A L CONTENT

T h e nuclear material content a n d total n l p h i activity fo r this WRM are listed below Also listed a r e overall uncertainty estimites at 95% confidence intervals (C1) f o r each component

Commnent O u i n t i t v or Value 95 % CI PuO, in W R M 0 34955 grams

Pu Assq 8 7 827 Yo OiPUO, * 0 0 7 2 % ' " * 0 00032 grams (a)

Pu i n WRM 0 30700 grams I O 00028 g r a m s ('I "'Am Assay 766 7 pg/g PuO,* -L 2 2 pg/g (dl

"'Am III W R M 0 2680 mg I 0 00078 rng"

Isotopic Weight Fraction

0 000145

0 937614

0 059-145

0 002237-

0 000559

t 0 0 0 0 0 0 s ~ ~

I 0 000013

i 0 000005 (0

t 0 00000s (Q

= 0 00000-1 10

23 67 mCi** S 759C+OS Bq

t 0 09 mCi + 3C+OG Bq (

Total Alphi Acti\it\ in WRhI

*hle isured r i l u e on ill5193 * - Lflecti\ c 1/15/93

liiorganic Elemental 4 n a l ~ s i s Robert S hl-irshall, Project L\Iin?pei - - h D A PDP W R Y Production

25

HNF-4051 Rev 3

MEASUREMENT METHOD AND TRACEAUILTTY

The nuclear contents of this WRM were characterized and quantified using the folloiving methods with traceability to the National Institute of Standqrds and Technology (NIST) o r New BrunswicL Laboratory (NBL) standards

Measurement Measurement Method Reference M i t e r i i l

Weighing 5 place analytical balance NIST traceable \$eights

Pu Assay Controlled Potential Coulometrj PiBL CRM X 126 Ani Assay Isotope Dilution Mass Spectrometry NEL CRM t: 128

Pu Isotopic Total Evaporation Mass Spectrometry NBL CRM f: 128 Alpha ActiviW Calculated from Pu and Am mass, and

isotope alpha specific activities listed below Pu I,? as stated for NIST SRM9-16

Am t,, ns sfated for NIST SRMJ322B

111 119 The stated Alph? Activity was calculated using the following Isotope half lives (in )ears) 21,119, '"Pu 6,560,

Pu 87 74, Pu 241 1 4 2

Pu 1 4 34, Pu 387,000, and"IAm 432 2

NOTES

Random and systematic error terms were combined and reported as 93% confidence intervals E r r o r terms include estimates of the following

(7) Balance precision, buoymcy, standard weight bias (b) Long and short term precision, control cliecl bias, weighing precision and bias (c) Above neighing and assay terms, and corrections for transfer loss (d) Long and short term precision, and bias (e) Above weighing terms, Am assay terms, and corrections for transfer loss (I) Long and short term precision, and bias (9 ) Bised on propngited uncertainties on the Pu mass, 24lAm mass and Pii isotopic uncertainties listed

abo\e h o half life uncertaintj components are included and i t is reconimended t h i t all facilities participating in the NDA PDP program use the hall I i >es listed above to preclude facilitj to facilitj error terms introduced b) using diflerent half life values

26

HNF-4051 Rev 3

Department of Energy Carlsbad Area Office Workmg Reference Material # NTP-OOY 1

PuO2-Diatomaceous Earth

This Working Reference Material (WRM) contains high purity plutonium dioxide dispersed in diatomaceous ear th Quantitative information and uncertainties on the nuclear content of this W R M a r e listed beion Complete Information regarding the Pu and Am content, Pu isotopic ratios chemical composition elemental impurities, containment, and WRM fabrication procedure is described i n the NDA PDP W R M Phase i Production Plan, CST 8 PLA STD 104 and i n files retained a t the Idaho National Engineering Laboratorb by the tochheed Martin Idaho Technology Co Transuranic Waste Department a n d a t t h e Los Alamos National Labora to r j Inorganic Elemental Analysis Group

hUCLEAR ,MATERIAL CONTENT

T h e nuclear material content a n d total alpha activity for this W R M are listed below Also listed a r e orerail uncertainty estimates a t 95% confidence intervals (CI) for each component

Comvonent PuO, in W R M

Pu Assay P u in WRM "'Am Assay

'"Am i n W R M

Isotopic Weight Fraction

"'Pu

2'9Pu

I'QPu

"Pu

Z'lPu

Tota l Alpha Activity i n WRM

Ouantitv o r Value 0 34034 grams

0 29891 grams 766 7 pglg PuO,*

0 2609 mg

87 827 % of PuO,

0 000145

0 937614

0 059445

0 002237* 0 000559

23 05 mCi*' 8 529E+08 Bq

95 % C I f 0 00031 grams I" i 0 072 % ib)

f 0 00027 grams (') i 2 2 pg/gid' i 0 00076 mg

I O 000008 (0

* 0 000013 I O 000005 1"

.L 0 000008 1"

I 0 000004 ' 0

*Measured balue on 7/15/95 ** Effectire 7/15/95

inorganic Elemental Analysis

27

HNF 4051 Rev 3

MEASUREMENT METHOD AND TRACEABILITY

The nuclear contents of this 'WRM were characterized and quantified using the following methods with traceability to the National Institute of S t a n d i r d s and Technology (NIST) o r New Brunswick Labora to ry (NBL) standards

Measurement Measurement Method Reference M i t e r i i l

Weighing 5 place analytical balance NIST traceable \\eights

Pu Assay Controlled Potential Coulometry h B L C R M # 126 Ani Assay Isotope Dilution Mass Spectrometry NE& C R M # 128 Pu Isotopic Tota l Evaporation Mass Spectrometry NBL CRM# 128

Alpha Activity Cnlculated from Pu a n d A m mass, and isotope a lpha specific activities listed below

Pu ti, as stated for NIST SRM9-16 Am t,, ns stated for NIST SRM4322B

211 119 T h e stated Alphi Activity \\as calculated using the following isotope half lives (in )ears) 24,119, "'Pu 6,560,

Pu 87 74, Pu 111 241 Pu 14 34, Pu 387,000, a n d '"Am 432 2

NOTES

Random nnd systematic e r r o r terms were combined and reported as 93% confidence intervals E r r o r te rms include estimates of the following

(a) Balance precision, buoyincy, s t anda rd weight bias (b) Long and short term precision, control cliecl bias, weighing precision and bias (c) Above weighing nnd nssay terms, a n d corrections fo r transfer loss (d) Long and short term precision, a n d bias (e) Above weighing terms, Am assay terms, a n d corrections for traiislcr loss ( f ) Long and short term precision, a n d bias (g) Bised on propagited uncertainties o n t h e Pu mass, 24lAm mass and Pu tsotopic uncertainties listed

abo ie ho half life uncertaint) components a r e included and i t i s recommended t h a t all facilities participating i n the NDA P D P p rogram use the half Ines listed above to preclude facilit) t o facil i t j e r r o r terms introduced b) using different ha l f life values

28

HNF4051 Rev 3

QTerfifrmte of Confenf XKII Erxcexbilifg

Department of Energv Carlsbad Area Office Worhng Reference Material # NTP-0098

PuO2-Diatomaceous Earth

This Working Reference Material (WRM) contains high purity plutonium dioxide dispersed i n diatomaceous earth Quantitative information and uncertainties on the nuclear content of this WRM a r e listed belon Complete information regarding the Pu and Am content, Pu isotopic ratios, chemical composition, elemental impurihes, containment, and WRM fabrication procedure is described i n the NDA PDP WRM Phase I Production Plan, CST-8 PLA STD 104 and in files retained at t h e Idaho National Engineering Laboraton by the Lockheed Martin Idaho Technology C o Transuranic Waste Department a n d a t the Los Alamos National Laboratory Inorganic Elemental Analysis Group

hUCLEAR MATERIAL COhTENT

T h e nuclear material content and total alpha activity for this WRM are listed below Also listed a r e overall uncertainty estimates at 95% confidence intervals (CI) for each component

PuO, in W R M Pu Assay

Pu i n WRM '''Am Assay

"'Am i n W R M

0 34054 grams

0 20909 grams 766 7 pug PuO,*

0 2611 mg

87 827 % o f PuO, i 0 00030 grams 1

f 0 072 % Ib) f 0 00027 grams ''I

i 0 00076 mg ' i 2 2 pglg id)

Isotopic Weight Fraction

rl'Pu

U'PU

I'oP u

"1Pu

1"Pu

Total Alpha Activitv i n WRM

0 000143

0 937614

0 0594.15

0 002237*

0 OOOm9

23 06 rnCi** 8 534E+08 Bq

i 0 000008 1"

i 0 000013 lo

i 0 000005

i 0 000008 (0

-+ 0 000004 (0

* 0 08 mCi (I) i 3E+06 Bq

*Measured >slue on 7/15/95 -* Effective 7lIY9s - Bill J , cherleb.Gro Leader Inorganic Elemental Analbsis

Robert S Marshall Project Manager hD4 PDP WRM Production

29

HNF 4051 Rev 3

MEASUREMENT M E rHOD AND TRACEABILITY

T h e nuclear contents of this WRM were characterized and quantified using the following methods with traceability to the National Insti tute of S t and i rds and Technology (NIST) o r New Brunswich Labora tory (NBL) standards

Measurement Measurement Method Reference bvI?teri?l

Weighing 5 place analytical balance NIST triceable \\eights

Pu Assay Controlled Potential Coulometry h B L CRM # 126 Ani Assay Isotope Dilution Mass Spectrometry N a L C R M # 128 Pu Isotopic Total Evnporation Mass Spectrometry N B L CRM # 128

Alpha Activity Calculated from Pu and Am mass, and isotope a lpha specific activlties listed below

Pu t,, as stated for N E T SRM946 Am ti, ns stated for NIST SRM4322B

211 l J 9 T h e staled Alph i Activity \>as calculated using the following Isotope half llves (in )ears) 21,119, Pu 6,560, P u 14 34, Pu 387,000,and1"Am 4 3 2 2

P u 8 7 7 4 , Pu 210 1 4 1 a a

NOTES

Random nnd systematic e r r o r t e rms were combined and reported as 93% confidence intervals E r r o r terms include estimntes of t h e follov/ing

(a) Balance precision, buoymcy , s t anda rd weight bias (h) Long and shor t t e rm precision, control checl bins, weighing precision and bias (c) Above neighing a n d assay terms, a n d corrections for transfer loss (d) Long and shor t t e rm precision, a n d bias (e) Above weighing terms, Am assay terms, and corrections for transfer loss (0 Long and short t e rm precision, a n d bias (g) Bised on propagated uncertainties on the Pu mass, 2.llAm mass and Pu lsotopic uncertainties listed

abo\e h o half life unce r t a in t j components a r e included and i t IS recommeiided t h a t all facilities participating i n t h e NDA PDP program use the half Iibes listed above to preclude facilltj t o facilit) e r ror terms introduced b) w i n g difrerent half life values

30

HNF-4051 Rev 3

Department of Energy Carlsbad Area Office Worlung Reference M?terial# NTP-0103

PuOZ-Diatomaceous Earth

This WorLing Reference Material (WRM) contains high purity plutonium dionde dispersed in diitoniiceous earth Quantitative information and uncertainties on the nuclear content of this \VRM are listed below Complete info~mation regarding the Pu and A m content, Pu isotopic ratios, chemicil composition, elemental impurities, containment, and WRM fabrication procedure IS described i n the NDA PDP W R M Phase 1 Production Plin, CST S PLA STD 104, and in files retnined at thc Idaho Nationil Engineering Laboratory by the Lockheed hlarlin Idaho Technology C o Transuranic Waste Department and n t the Los Alamos National Laborator) Inorginic Elemental Analysis G r o u p

NUCLEAR MATERIAL CONTENT

T h e nuclear material content and total s l p h i activity for this WRM ?re listed below Also listed i r e overall uncertainty estimates at 95% confidence intervals (Ci) for e ich component

Component Quant i tv o r Value 95 % CI PuO, in \Wl 0 34013 grams * 0 00031 grams

87 827 % of PuO, f 0 072 % Ib) Pu Ass?) Pu in WRM 0 29572 grams 0 00027 grams (') "'Am Assay 766 7 pglg PuO,* * 2 7. pglg la)

"'Am in WRM 0 2605 mg * DO0076 mg )

Isotopic Weight Fraction

"APU 0 000145

"PPU 0 937614

"P u 0 059445

"1PU 0 002237'

i Pu 0 000559

* 0 000005 (0

I O 000013 lo

I O 000005 '0

* 0 000006 (0

I 0 000004 (0

23 04 mCi-* 6 523E+OS Bq

= 0 0s m c i ( = 3C+06 Bq ( ' Tot11 Alphi A c t i r i t ~ i n WRhI

I

"hlcisurcd \ i l u e on 7/15/95 -" Effec tne 7/15/95

r

- h D A PDP \\ Rh1 Production

HNF 4051 Rev 3

M E A S U R E M E N T MCTROD AND TRACEAUILITY

The nuclear contents of this 'WRM w e r e characterized and quantified using thc following me thods with traceability to the National Ins t i tu te of S t a n d i r d s and Technology (NIST) o r New BrunswicL L a b o r a t o r y (NBL) standards

Measurement Measurement Method Reference M i t e r i i l

Weighing 5 place analytical balance NIST traceable weights

Pu Assaj Cont ro l led Potential Coulometrj IYBL C R M t: 126 Ani Assay Isotope Dilution Mass Spectrometry NBL C R M # 128

P u Isotopic To ta l Evapora t ion Mass Spectrometry N B L CRM t: 128

Alpha AcliviW Cnlculated f rom Pu a n d Am mass, and isotope n lphn specific activities listed below

Pu ti, as stated fo r N I S T SRhT9-16 Am ti, os stated for N I S T SRM4322B

313 139 The stated Alphi Activity \>as calculated using the following isotope half lives (in )ears) 24,119, Pu 6,560, P u 1434, Pu 387,000,and1'iAm 4322

Pu 8 7 74, Pu 140 111 ZJZ

NOTES Random and systematic e r r o r t e r m s were combined and reported as 93% confidence intervals E r r o r t e rms include estimates of the following

(I) Balance precision, buoyincy , s t a n d a r d w i g h t bias (b) Long and short t e rm precision, cont ro l checl bias, weighing precision and bias (c) Above weighing a n d assay te rms , a n d corrections for transfer loss (d) Long and short t e rm precision, a n d bias (e) Above weighing terms,Am nssay te rms , a n d corrections for transfer loss (0 Long and short t e rm precision, a n d bias (g) Bised on propagited uncertainties o n the Pu mass, Z41Am mass and Pu isotopic uncer ta in t ies listed

aboie h o half life unce r t a in t j components n re included and i t is reconimended t h a t all facilities participating i n the NDA PDP p r o g r a m use t h e half lives listed above to preclude facil i t j t o f ac i l i b e r r o r terms introduced by using d i f fe ren t half life values

32

HNF-4051 Rev 3

Department of Energy Carlsbad Area Officc Worlung Reference Material # NTP-0105

Pu02-Diatomaceous Earth

This Working Reference Material (WRM) contains high purity plutonium dioxide dispersed in diatomaceous earth Quantitatne information and uncertainties on the nuclear content of this WRM a r e listed belov Complete information regarding the Pu and Am content, Pu Isotopic ratios, chemical composition, elemental impurities, containment, and WRM fabrication procedure i s described in the NDA PDP WRM Phase 1 Productlon Plan, CST-8 PLA-STD 104, and in files retained at the Idaho National Engineering Laboraton by the Lockheed Martin Idaho Technologv Co Transuranic Waste Department and at the Los Alamos National Laboratory Inorganic Elemental Analysis Group

NUCLEAR MATERIAL CONTENT

The nuclear material content and total alpha actirity for this WRM are listed below Also listed are overall uncertainty estimates a t 95% confidence intervals (CI) for each component

ComDonent PuO, in W R M

Pu Assay Pu in W R M '"Am Assay

"'4m in W R V

Isotopic Weight Fraction

"'Pu

U'PU

ZJQPU

InPu

'"PU

Puantitv o r Value 0 35174 grams

0 30893 grams 766 7 pg/g PuO,'~

0 2697 mg

87 827 % or PUO,

0 000145

0 931614

0 059445

0 002237*

0 000559

95 Yo CI f 0 00032 grams ' i 0 072 %o 'b)

f 0 00028 grams id

h 0 00079 m g O iZZpg/g'd'

f 0 000008 (0

i 0 000013'"

-L 0 000005 '0

i 0 000008 (0

-C- 0 000004'"

I Total Alpha Activity in WRM 23 82 mCi** 8 811Et08 Bq

* 0 09 mC1'" i 3E+06 Bq

I *Measured value on 7/15/95 * * Effectire 7/15/95

L & g & l L / dill h c K e r l e y , C r o u h e a d e r Inorganic Elemental A n x s i s

Jz@44mv& Robert S Varshall Proiect Manaeer

33

HNF-4051 Rev 3

MEASUREMENT METHOD AND TRACEABILITY

T h e nuclear contents of this W R M were characterized and quantified using the following methods with traceability to the National Institute of S tandards and Technology (NIST) o r New BrunswicL Labora tory (NBL) standards .

Measurement Measurement Method Reference M i t e r i i l

Weighing 5 place analytical balance NIST traceable !>eights

Pu Assay Controlled Potential Coulometrj hBL C R M 126

Ani Assay Isotope Dilution Mass Spectrometry NRL C R M 128 P u Isotopic Total Evaporation Mass Spectrometry NBL CRM P 128

Alpha Activi€y Calculated from Pu and Am mass, and Isotope alpha specific activities listed below

Pu ti, as stated for NIST SRkI9-16 Am t,, ns stated for NIST SRM-13228

213 219 T h e stated A l p h i Activity n a s calculated using the followng Isotope half lives (in years) 24,119, "'Pu 6,560,

Pu 87 74, Pu I J I I42

Pu 14 34, Pu 387,000, and"'Am 432 2

NOTES Random and systematic e r ro r tei ms were combined and reported as 95% confidence intervals E r r o r te rms include estimates of the following

(a) Balance precision, buoyincy, s tandard weight bias (b) Long and shor t t e rm precision, control cliecl bias, weighing precision a n d bias (c) Above weighing a n d assay terms, and corrections for transfer loss (d) Long and shor t t e rm precision, and bias (e) Above weighing terms, Am assay terms, and Corrections for transrer loss (i) Long and short te rm precision, and bias (g) Bised on propagi ted uncertainties o n the Pu mass, 2-1lAm mass and Pu isotopic uncertainties listed

abo\e h o half life uiicertaint) components a r e included and i t is recommended tha t all facilities pirticipating i n the NDA P D P program use the ha l l lives listed abore to preclude facilitj to fac i l ib e r r o r terms introduced b) using diiierent half life values

34

HNF 4051 Rev 3

Merfificnte of Monfent nnb ~ m c e n b r l i f a 1

Department of Energy Carlsbad Area Office Worlung Reference Material f# NTP-0112

Pu02-Diatomaceous Earth

This Working Reference Material ( W h v contains high purity plutonium dioxide dispersed in diatomnceous earth Quantitative information and uncertainties on the nuclear content of this WRM a r e listed below Complete information regarding the Pu and Am content, Pu isotopic ratios, chemical composition elemental impurities, containment, and W R M fabrication procedure is described io the NDA PDP WRM Phase 1 Production Plan, CST-8 PLA STD 104, and In files retained at the Idaho National Engineering Laboratorv by the Lockheed Martin Idaho Technology C o Transuranic Waste Department and at the Los Alamos National Laboratory Inorganic Elemental Analysis Group

NUCLEAR MATERIAL CONTENT

The nuclear material content and total alpha activitv for thls WRM are listed below Also listed a r e overall uncertainty estimates a t 95% confidence intervals (CI) for each component

ComDonent PuO, in WRM

Pu Assay Pu in WRM "'Am Assay

"'Am in WRM

Isotopic Weight Fraction

-Pu

="Pu

,roPu

'JtPU

" Pu

Total Alpha Activity i n W R M

Quantitv or Value 3 3588 grams

87 827 % O f PuO, 2 9500 grams

766 7 p u g PuO,* 2 575 mg

0 000145

0 937614

0 059445

0 002237*

0 000559

227 5 mCi'* 8 417E+09 Bq

95 % C I f 0 0028 grams 1') f 0 072 % (b)

-+ 0 0025 grams (')

i 0 0072 mg 10

i 2 2 pg/gld'

i 0 000008 (0

f 0 000013 (0

i 0 000005

i 0 000008

* 0 000004 ( 0

* 0 8 mCi (1)

* 3E+07 Bq I')

.- Inorganic Elemental Analysis

35

HNF-4051 Rev 3

MEASUREMENT METHOD AND TRACEABILITY

The nuclear contents of this WRM were characterized and quantified using the following methods with traceability to the National Insti tute 01 S t a n d i r d s and Technology (NIST) or New Brunswich Labora to ry (NBL) standards

Measurement Measurement Method Reference M ? t e r i i l

'Weighing 5 place analytical balance NIST traceable \>eights Pu Assay Controlled Potential Coulometrj k B L C R M t: 126 Ani Assay Isotope Dilution Mass Spectrometry NE& CRRI i: 128

Pu Isotopic Tota l Evapora t ion Mass Spectrometry N B L CRM 128

Alpha ActiviW Calculated from Pu a n d Am mass, and isotope a l p h a specific activities listed below

Pu ti, as stated f o r N I S T SRM946 Am ti, ns stated fo r NIST SRM4322B

111 119 The stated Alph? Activity r tas Calculated using the following isotope half lives (in )ears) 21,119, "oPu 6,560, Pu 14 34, Pu 387,000, nnd"lAm 4322

P u 87 74, Pu 1 4 1 111

NOTCS

Random and systematic e r r o r t e rms were combined and reported as 93% confidence intervals E r r o r tcrms include estimates 01 the following

(7) Balance precision, buoyincy, s t a n d a r d weight bias (b) Long and short t e rm precision, control cliecl bins weighing precision and bias (e) Above weighing a n d assay te rms , a n d corrections for transfer loss (d) Long and short t e rm precision, a n d bias (e) Above weighing terms, A m assay te rms , and corrections for transfer loss (l) Long nnd short t e rm precision, a n d bias (9) Bised on propagi ted uncertainties o n the Pu mass, 24lAm mass and Pu isotopic uncer ta in t ies listed

aboie h o half life unce r t a in t j components a re included a n d i t is recommended t h a t all facilities participating i n t h e NDA PDP p r o g r a m use the half l i%es listed abope to preclude lacilit) to facil i t j e r ro i terms introduced b) using d i l fe ren t half lire values

36

HNF 4051 Rev 3

PuO, i n WRM Pu Assay

Pu in WRM '4iAm Assay

"'Am in WRM

I Isotopic Weight Fraction

"'Pu

"9Pu

""u

"'Pu

"'Pu

@..ertrficnfe of Cunfent nnb 7Li:rarenbrltto I

Department ofEnergy Carlsbad Area Office U orkmg Reference Material NTP-0119

PuO2-Diatomaceous Earth

This Worhlng Reference Material (WRWT) contains high purity plutonium dioxide dispersed in diatomaceous earth Quantitative information and uncertainties on the nuclear content of this W R M are listed below Complete information regarding the Pu and Am content, Pu lsotoplc ratias chemical composition, elemental impurittes, containment, a n d WRM fabrication procedure is described i n the NDA PDP WRM Phase I Production Plan, CST-8 PLA-STD 104 and in files retained a t the Idaho National Engineering Laborator) by the Lockheed Martin Idaho Technology Co Transuranic Waste Department and at the Los Alamos National Laboratory Inorganic Elemental Analysis Group

NUCLEAR MATERIAL CONTENT

The nuclear material content and total alpha activity for this WRM are listed below Also listed a r e overall uncertainty estimates a t 95% confidence Intervals (CI) for each component

~ I Comoonent Q u a n t i t v o r Value 95 Yo C I 3 4962 grams

87 827 yo or PUO, 3 0706 grams

2 681 mg

f 0 0029 grams * 0 072 % tbl

f 0 0026 grams ''I 766 7 pglg PuO,' f 2 2 pglg 'd'

* 0 0075 mg

0 000145

0 937614

0 059445

0 002237*

0 000559

f 0 000008 In

f 0 000013

i 0 000005 In

f 0 000008 In

* 0 000004 1"

I Total Alpha Activity i n WRM 236 8 mCi** 8 761E+09 Bq

*Measured value on 7/15/95 * * Erfecti>e 7/15/95

cKerlev Crb& Leader Inorganic Elemental Analysis

b.k.b& 5- !&-I& Robert S Marshall, Project Manager . - NDA PDP W R M Production

HNF4051 Rev 3

MEASUREMENT MEI n m AND TRACCAUILITY

The nuclear contents of this WRM were characterized and quantified using the following methods n i t h traceability t o the National Insti tute of S t a n d i r d s and Technology (NIST) or New Brunswicl, Labora to ry (NBL) standards

Measurement Measurement Method Reference FyIiteriil

'Weighing 5 place analytical balance NIST traceable !!eights Pu Assay Controlled Potential Coulomctrj PiBL C R M # 126 Ani Assay Isotope Dilution Mass Spectrometry NBL C R M t: 128 Pu Isotopic Tota l Evapora t ion Mass Spectrometry NBL C R M # 128

Alphn Activity Calculated f rom Pu a n d Am mnss, and isotope nlphn specific activities listed below

Pu t,, as stated for NIST SRbI9.16 Am I,, ns stated for NIST SRMJ322B

>)I I J 9 T h e stated Alphi Activity Ifas calculated using the following isotope half lives (in )ears) 21,119, "'Pu 6,560,

P u 87 74, Pu 241 2J2 Pu 14 34, P u 387,000, and"'Am 432 2

NOTES

Random and systematic e r r o r t e rms were combined and reported as 95% confidence intervals E r r o r te rms include cstimntes of the following

(n) Balance precision, buoyincy , s t anda rd weight bias ( b ) Long and short t e rm precision, control cliecl bias weighing precision and bias (c) Above weighing a n d nssay te rms a n d corrections for transfer loss (d) Long and short t e rm precision, a n d bias (e) Above weighing terms, A m assay terms, a n d corrections for transfer loss (0 Long and short term precision, a n d bias (g) Bised on propagited uncertainties o n t h e Pu mass, 241Am mass and Pu isotopic uncertainties listed

abo le ho half life unce r t a in t j components a r e included and i t 1s reconiineiided t h a t all facilities participating in the NDA PDP program use the half 1 1 5 ~ s listed above to preclude facilitj to fac i l ib e r r o r terms introduced b) using different half life values

38

HNF4051 Rev 3

Department of Energy Carlsbad Area Office Worlung Reference Material # NTP-0126

Pu02-Diatomaceous Earth

This Worhing Reference Material (WRM) contains high purity plutonium dioxide dispersed in diatomaceous earth Quantitative information and uncertainties on the nuclear content of this WRM a r e listed b 10," Complete Information regarding the Pu and Am content, Pu isotopic ratios, chemical composition elemental impurifies, containment, a n d WRM fabrication procedure i s described in the NDA PDP W R M Phase 1 Production Plan, CST-8-PLA-STD-104 and in files retained at the Idaho National Engineering Laborator) bv the Lockheed Martin Idaho Technology Co Transuranic Waste Department and a t the Los Alamor hational Laboratory Inorganic Elemental Analysis Group

NUCLEAR M4TERIAL COhTEhT

The nuclear material content and total alpha activit) for this WRM are listed below Also listed a r e overall uncertainty estimates at 95% confidence intervals (CI) for each component

Component Quanti& or Value 95 % CI PuO, in WRM

Pu Assay Pu In WRM

3 4068 grams 87 827 Yo of PuO,

2 9921 grams

f 0 0029 grams,' ' -+ 0 072 O h Ib)

f 0 0025 grams w '*'Am Assay 766 7 pglg PuO,* a22pglg'd'

"'Am in WRM 2 612 mg f 0 0073 mg

Isotopic Weight Fraction

1"Pu 0 OOOl45

"'Pu 0 937614

"OPU 0 059445

"'Pu 0 002237*

"ZPU 0 000559

f 0 000008 (0

f 0 000013 '" -L 0 000005 m

I 0 000008 '0

I 0 000004

Total Alpha Activity in WRM 230 7 mCP* i O 8 m C i " ' 8 537Et09 Bq f 3E+07 Bq 111

*hleasured salue on 7/15/95 * * Effective 7/15/95

y i ? 9 , L L W d3ilhL\lcKerlev, C r Leader Inorganic Elemental Analysis

P\-W Robert S Marshall Proiect Vanager ND-\ PDP WRM Production

39

HNF 4051 Rev 3

MCASUREMCNT METHOD AND TRACEAUILITY

The nuclear contents of this WRM were characterized and quantified using the following methods with trace?bility to the National Insti tute of Stand?rds and Technology (NIST) o r New BrunswicL Labora to ry (NBL) standards

Measurement Measurement Method Reference Mi te r i ? l

Weighing 5 place analytical balance NIST tr iceable \>eights

Pu Assay Controlled Potential Coulometr) PiBL C R M f: 126

Ani Assay Isotope Dilution Mass Spectrometry N U C R M g 128 P u Isotopic Tota l Evaporation Mass Spectrometry NBL CRM t: 128

Alpha Activily Calculated from Pu and Am mass, and isotope a lpha specific activities listed below

Pu ti, as stated for NIST SRM9.16 Am ti, ns stated for NIST SRMJ3ZZB

JII 119 T h e stated Alplii Activity v a s calculated using the following Isotope half lives (in ).ears) 21,119, P u 6,560, Pu 1434, Pu 387,000,and2'iAm 4322

P u 87 74, P u I40 111 IJI

NOTES

Rnndom and systematic e r r o r te rms were combined and reported as 92% confidence intervals E r r o r t e rms include estimates of the following

(n) Balance precision, buoyincy , s t anda rd w i g h t bias (b) Long and short t e rm precision, control checl bias, weighing precision and bias (c) Above weighing a n d assay terms, a n d corrections for transfer loss (d) Long and short t e rm precision, a n d bias (e) Above weighing terms, Am -issay terms, and corrections for transfer loss (0 Long and short t e rm precision, a n d biis (g) Bised on propagated uncertainties on the Pu mass, 211Am mass and Pu lsotoplc uncertainties listed

abobe ho half life uiicertaint} components a t e included a n d i t i s recommended t h l t all facilities pr t ic ipa t ing i n t he NDA P D P p rogram use the half lires listed above to preclude facilitj to facility e r r o r terms introduced by using clirferent half life values

40

HNF-4051 Rev 3

I Isotopic Weight Fraction%

""U

'40Pu

''fPU

'.I P u

Pu03-Diatomaceous Earth Standard WRAP-2 5 OGPU

Thls N D A standard contains high puri ty plutonlum dlorlde dispersed in diatomaceous ear th Quantitative lnformelion and uncertainties on the nuclear content of this WR.M are listed below Complete Information regarding the P u a n d Am content, P u Isotopic ratios, chemical composltlon, elemental impurities, containment, and fabrication procedures are retained in files by the Los Alarnos National Laboratory CMR Analytical Chemistry G r o u p

JWCLCAR MATERIAL CONTEhT

The nuclear material content a n d total alpha activity Tor this standard are listed below Also listed are oberall uncertainty estimates at 95% conlidence Intervals (CI) for each component

Component PuO, in s tandard

Pu Asssy Phi i n s tandard

"'Am Assay '"Ani i n s tandard

Q u a n t i t v o r v a l u e 95 % CI 571060 grams

81 761 % of PuOi* 5 01168 grams

1128 9 pg/gPuO,* 5 66 mg*

* o 00021 grams ( t 0 081 % (5)

rt o 00412 grams(') -L 0 3 pg/g (') t 0 04 rng (*I

0 00014

0 93809

0 05939

0 00185

0 00054

I 0 000005

I O 000015 ( O

I O 000007

5 0 000009 ( O

t 0 000003 "

Total Alpha Activity i n s tandard 342 5 rnCI** 1 267J3-10 Bq t3Et07 Bq"

-L o 9 mCi (I'

"Decay corrected value on 1121199 ** Effective 1121199

Robert S Msrshall, Project M a n a z e r hDA WRM Production

41

HNF4051 Rev 3

MEASUREMENT METHOD AND T R A C E h U I l ~

The nuclcar coiltents or this WRM were characterized and quantified using the following methods with traceability t o the National Institute or S t a n d i r d s and Technology (NIST) o r New Brunswicl, Labora to r ) (NBL) standards

Measurement Measurement Method Reference M i t e r i i l

Weighing 5 place analytical balance NIST traceable \>eights

Pu Assay Controlled Potential Coulometrj h B L C R M g 126

Ani Assay Isotope Dilution Mass Spectrometry NBL C R M G 128 Pu Isotopic Tota l Evaporation Mass Spectrometry NBL CRM # 126

Alpha Activ!ly Calculated f rom Pu a n d Am mass, and isotope a lpha specific activities listed below

Pu t , , as stated for NIST SRM9J6 Am ti, ns stated for NIST SRM4322B

IIJ 11) The stated Alph i Activity \)as calculated using the following isotope half lives (in j e i r s ) 23,119, P u 6,560, Pu 1 4 3 4 , Pu 387,000,and'"Am 4322

P u 87 74 , Pu 1 4 0 1 4 1 I11

Random and systematic e r r o r terms were combined and reported as 93% confidence intervals E r r o r te rms include estimates of the following

(7) Balance precision, buoymcy, s t anda rd weight bias (b) Long and short term precision, control cliecl biis, weighing precision arid bias (c) Above weighing and assay terms, and corrections for transfer loss (d) Long a n d short term precision, and bias ( e ) Above weighing terms, Am assay terms, and corrections for transfer loss (0 Long and short term precision, and b i i s (9) Bised on propigated uncertainties o n the Pu mass 2 4 l A m inass and Pu isotopic uncertainties listed

abo \e h o hall l ire uncer ta in t j components a r c included and i t is recoinmendcd t h i t all facilities pirticipating i n the NDA PDP program use the half Iibes listed above t o preclude Iacilitj t o facility e r r o r terms introduced b) using difrerent half life values

42

HNF-4051 Rev 3

Los Allamos National. Laboratory

PuO, Diatomaceous Earth Standard WRAP-3 5 OGPU

This NDA standard contains high purity plutanlum dioxlde dispersed in dlatomaceous earth Quantitative information a n d uncertainties on the nuclcar content of this W I W are listed below Cdmplele information regarding thc P u and Am content, Pu rsotopic ratios, chernlcal composilion, clemental impurities, containment, and fabrication procedures arc rttaincd in files by the Lor Alamos National Laboratory CMR Analytical Chemistry Group

NUCLEAR MATERLAL CONTENT

The nuclear matcrial content and total alpha activi(y for this standard a r e llrted below Also listed are overall uncertainty estimates a t 95% confidencc Intcrvals (CT) for each component

Component Ouantity o r Value 95 % CI PuOl in standard

Pu Assay Pu in standard

"'Am Assay

5 69429 grams 87 761 % of PuOf

4 99136 grams 1128 9 p d g PuOI*

& 0 00031 grams (') -L 0 081 % (b)

& 0 00476 grams ('I 5 0 3 pglg (d)

"'Am i n standard 5 64 rng" -L 0 04 rng

Isotopic Wcight Fraction"

0 00014

0 93809

0 05939

0 00185

0 00054

3. 0 000005

3.0 000015

-L 0 000007 (O

c 0 000009 (0

-L 0 000003 ('

Total Alpha Activity I n s f a n d i r d 311 5 rnCi** t o 9 mCi ( ' 1263E+10 Bq x 3E+07 Bq ( '

*Decay corrccled valuc on 1121199 ** Elkct iye 1121199

n

obert S h.lars%all, Projecl Manager hDA WRM Production

43

HNF 4051 Rev 3

MEASUREMENT METHOD AND TRACEAD11 ITJ

The nuclear coiitents of this WRM were characterized and quantified using the following niethods with traceability to the National Insti tute of S t a n d i r d s and Technology (NIST) o r New DrunstvicL Labora to ry (NBL) standards

Measurement Measurement Method Reference M i t e r i i l

Weighing 5 place analytical balance NIST triceable rteights

Pu Assay Controlled Potential Coulometrj hBL CRM # 126 Ani Assay Isotope Dilution Mass Spectrometry NE& C R M # 128

Pu Isotopic Tota l Evapora t ion Mass Spectrometry NBL CRkI # 128

Alpha Activity Calculated f rom Pu and Am mass, and isotope a lpha specific activities listed below

Pu ti, as stated for NIST SRM9-16 Am ti, ns stated for N E T SRh14322B

213 139 The stated Alphi Activity !>as calculated using the follotving isotope half lives (in Sears) 21,119, '"Pu 6,560,

Pu 87 7 4 , Pu 111 I12

Pu 14 34, Pu 387,000, and'"Am 432 2

NOTES Random and systematic e r r o r t e rms were conibined arid reported as 93% confidence intervnls E r r o r te rms include estimates or the following

(1) Balance precision, buoyincy, s t a n d a r d weight bias (b) Long and short term precision control checl bias, weighing precision and bi3s (c) Above weighing a n d assay terms, a n d corrections for transfer loss (d) Long and short t e rm precision, a n d bias (e) Above weighing terms, Am I s say terms, and corrections lor transfer loss (0 Long and short term precision, a n d bias (g) Blsed on propng?ted uncertainties on the Pu mass 241Am mass a n d Pu isotopic uncertainties listed

abo\e h o half life uncertaint) components a r e includcd i n d i t IS recommended t h a t all facilities pirticipating i n the NDA PDP p r o g r a m use the half lives listed abo,e to preclude facilit} to facilit) e r r o r terms introduced b) using different half life values

44

HNF 4051 Rev 3

h s A h n o s National. Laboratory Certificate of Eontent anti Qikaceabditp

Pu02-Diatomaceous Earth Sfandard WRAPlOGPU

Thk NDA standard contalns hlgh putity plutonium dioxide dispersed la diatomaceous enrih Quantitat~vc information and uncertainties on the nuclear content or thls WRM a r e listed below Cohplete information regarding thc Pu a n d Am content, Pu isotopic rallos, chemlcal composition, elemental impurities, containment, and fabrication procedures a r e rctalncd 111 Iiles by the Los Alamos Nationel Laboratory CMR Analytical Chernlstry Group

JiUCLEAR MATERIAL CONTENT

The nuclear matcrial content a n d total alpha activity for thls standard are listed bclow Also listed a r e overall uncertainty estimates at 95% conndencc intervals (CI) for each component

ComDoncnt Q u a n t i t y orValuc PuO, In s tandard 11 40156grams rt 0 00049 grams ('I

87 761 % oIPuO>* * 0 081 Yo @)

1 0 00612 grams & 0 00945 grams (') '"Am Assay 1128 9 pg/gPuO,* 5 0 3 pg/g("

11 30 mg* 5 0 09 mg (4

Pu Assay Pu i n standard

"'Am in standard

Ysotoplc Wcight Fraction"

'"PU

u9Pu

"'PU

"iPu

l' Pu

0 00014

0 93803

0 05939

0 00165

0 00054

t 0 000005 ( 0

-I 0 000015 ( O

t 0 000007

J 0 000009 "

-L 0 000003 ('

Total Alpla A c h i t y in standard 683 7 m W h .L 1 E ~ C I (e'

2 530Et10 Bq rt 7 E 4 7 Bq (d

*Dccaj corrcctcd value on 1121199 Effective 1121199

N D A WRMProduction

45

HNF 4051 Rev 3

MCASURCMENT M E r H O D AND TRACEADIISTY

T h e nuclear contents of this WRM w e r e characterized and quantified using the following melhods with traceability to the National Insti tute of S t and i rds and Technology (NIST) o r New Brunswich Laborator) (NBL) standards

Measurement Measurement Method Reference M i t e r i i l

Weighing 5 place analytical balance NIST triceable \\eights

Pu Assay Controlled Potential Coulometrj lvBL C R M f: 126

Ani Assay Isotope Dilution Mass Spectrometry N U C R M E 128 Pu Isotopic Total Evaporation Mass Spectrometry NBL CmI f: 128

Alpha ActiviW Calculated from Pu and Am mass, and isotope a lpha specific activities listed below

Pu t,, as stated for NIST SRiV19-16 Am ti, ns stated for NIST SRhl1322B

IIJ 119 The stated Alph? Activity \>as calculated using the following isotope half lives (in )ears) 21,119, Pu 6,560, Pu 14 31, Pu 387,000,and"lAm 4322

Pu 87 74, Pu 240 1JI 141

Random nnd systematic e r r o r t e i ms were combined and reported as 93% confidence intervals E r r o r ternis include estimates 01 the following

(i) Balance precision, buoyincy, s t anda rd weight bias ( b ) Long and short t e rm precision, control checl bias, weighing precision and bias (c) Above weighing ?nd assay terms, a n d corrections for transfer loss (d) Long and short t e rm precision, a n d bias (e) Above weighing terms, Am i s s a y te rms and corrections for transfer loss ( f ) Long i n d short t e rm precision, a n d bias (g) Bised on propagited uncertainties on the Pu mass, 2-1lAm mass and PI] isotopic uncertainties l i s t e d

a b o i e h o half life uiicertaint) components are included and i t i s recommended t h a t all facilitie> pirticipating in the h D A PDP program use the half b e s listed above to preclude facilitj to facilit) error tei ms introduced b) usiiig different ha l f life values

46

HNF-4051 Rev 3

r Component Quantitv or Value 9s 7 0 a

Pu Assay 87 761 % ofPuO,* * 0 081 % PuO, in standard 22 19925 grams & 0 00062 grams(')

$os Marnos Nationall Laboratory

PuOz-Diatomaceous Bartb Standard WRAP20GPU

This NDA standard contalns hlgh purity plutonium dioxide dispersed In diatomaceous earth Quantitative information and uncertainties on the nuclear content of this 'WRM a re listed below Complete information regarding t h e Pu a n d Am content, Pu lsotopic ratios, chemlcal cornpodtion, elemental impurities, contalnment, and fabrication procedures a t e retained in flies by the Los Alamos National Laboratory ChfR Analytical Chemistry Group

NUCLEAR MATERIAL CONTENT

The nuclear materlal content a n d total alpha ac(ivity for this slandard a re Iisfed below Also listed a r e overall uncerlainly estimates a t 95% confidence In t ena l s (CI) f o r each component

Isotopic Vfcight Fraction"

1JJp U

s'Pli

'%I

'%I

PU

I 0 00014

0 93809

0 05939

0 00185

0 00054

rt o OOOOOj (0 ct 0 000015

ct 0 000007 lo

A 0 000009 (0

ct 0 000003

Total Alpha Activity in standard 1367 tnCi** 5 039E+10 Bq

-L 4 rnCi Q'

-I 1EtO8 Bq (

*Decaycorrcctcd \ d u e on lRll99 ** Eflec l i re 1/21/99

A

. . N D A WRhlProduclion

47

HNF 4051 Rev 3

MEASUREMENT M C rHOD AND T R A C C A B W

The nuclear coiitenls of this WRM were characterized and quantified using the following methods with traceibility to the National Inslitute of S t and i rds and Technology (hIST) o r New Brunswich Labora to r ) (NBL) standards

Measurement 'Measurement Method Reference Mi ter i71

Weighing 5 place analytical balance N E T traceable rtcights Pu Assay Controlled Potential Coulometrj m L CRM f: 126 Ani Assay Isotope Dilution Mass Spectrometry N!lL C R M i: 128

Pu Isotopic Tota l Evaporation Mass Spectrometry NBL CRM f: 128

h l p h i Activity Calculated from Pu and Am mass, and isotope a lpha specific activities listed below

Pu ti, as slated for NIST SRM9JG Am ti, ns stated for NIST SRMJ322B

113 119 T h e slaled Alplii Activity !\as calculated using the following isotope half lives (in years) 24,119, Pu 6,560, Pu 14 34, Pu 387,000,and1'iAm 4322

Pu 87 7 4 , Pu 110 1 3 1 l a 1

NOTCS

Random and systematic e r r o r te rms were combined and reported as 93% confidence intervals E r r o r terms include estimates of t h e follo~ving

(9) Balance precision, buoyincy , s t anda rd w i g h t bias (b) Long and short t e rm precision, control cliecl bias, weighing precision and bias (c) Above weighing ?nd assay terms, a n d corrections for transfer loss (d) Long and short t e rm precision, a n d bias (e) Abovc weighing terms, Ani ?say terms, and corrections for translcr loss (0 Long and short t e rm precision, a n d bi is (g) B x e d on propngited uncertainties on the Pu mass, 211Am i n a s s and Pu isotopic uncertainties listed

abole h o half life unccrtaint) components a re included and i t i s recommended t h i t all f tcilitie, pirticipating i n the NDA PDP program u s e the half I i b e s listed ibo,e to preclude facilitj to fac i l i t j e r ror terms introduced b j using different half life values

48

HNF4051 Rev 3

Los Alamos National Laboratory

PuOl-Diatomateous Earth Standard W " 3 0 G P U

Thls NDA standard contains high purity plutonium dioxide dispersed lo diatomaceous ear th Quantitative Information and uncertainties on the nuclear content of this WRM are listed below Complete Information regarding thc Pu and Am content, Pu Isotopic ratios, chemlcal composition, elemental impurities, containment, and fabrication procedures are retained u1 f i les by the Los Alarnos National Laboratory CMR Analytical Chemistry Group

p

The nuclear material content and total alpha activity for this standard are listed below Also listed a r e overall uncertainty estimates a t 95% confidence Intervals (C1) for each component

Component Quantity or Value 95 % CI PuO, in s landard

Pu Assay 34 19337 grams i o 00101 grams ('1

87 761 Yo of PUO,* h 0 081 % (b) Pu i n s tandard 30 00842 grams * 0 02815 grams

33 88 mg* '"Am Assay 1128 9 pg/g PuOl* * 03 pp/g (dl

"'Am in standard A 0 26 mg ")

Isotopic Weight Fraction"

P u nil

"9Pu

""PU

ar'Pu

2 ' ~ P U

0 00014

0 93809

0 05939

0 00185

0 00054

-J: 0 000005 (O

5 0 000015 ('

i 0 000007

* 0 000009 (' rt 0 000003 ('

Total Alpha Aclivity in standard 2051 mCi** 7 587Et10 Bq

* 5 mCi ( ' f 2Et08 Bq @'

*Decay corrected value on 1/21/99 ** Effective lnll99

- NDA WRM Production

49

HNF 4051 Rev 3

M E A S U R E M E N T METHOD AND TRACEABILITY

The nucleat Contents of t h standard were characterucd and quankfied nsldg the follomng methods pnth traceabhly to the National Institute of Standards and Technology (NIST) or New B m m c k Laboratory (NBL) standards

Measurement Meawrement Method Reference Matenal

Weighing 5 placc analytical hahnce MST traceable weighis Pu Assay Controlled Potentlal Coulometry NBL CRM # 126 Am Assay Isotope Diluhon Mass Spectrometry NBL CRii # 128 Pu Isotopic Total Evaporahon hiass Spectrometry NBL CRM # 128

Alpha Actinty Calculated f rom Pu and Am mss, and isotope alpha specific achnties luted below

Pu tip as stated for N E T SRh1946 Am tip as staled for NLST

SRiX4322B

IM U P The stated AJpba Actinty was calculated using the followng lsotope balf lives (in years) 24,119, "oPpu 6,560,

Po 87 74, Pu 241 1 4 1 Pu 14 34, Pu 387,000, and"'Am 432 2

Random and systemnhc crror t e r m wcrc combmed and reportcd as 95% confidence intervals E r r o r terms mclude e s t m t e s of the follomng

(a) Balance prccuion, buoyancy, s tandard wcight bms, and transfer lass (h) Long and short term precuion, control check bias, weighing precrsion and bas. (c) Above weigbmg and assay terms, and transfer loss. (d) Long and short term precsion, and bias (e) Above wclgblng t e r m , Am assay t e r m , and transfer loss ( f ) Long and short term precwion and b a s (s) Based 00 propagated uncertaintics on the h mass, "'Am mass and Pu lsoloplc uncertambc3 listed

above No half Me uncertainty componeois are locloded and 11 is recommended tha t all facdities participamg rn the hD% PDP program l~pe the halllwes W e d above to preclude f a c h t ) tO-.faCaty crror t c r m introduced by usmg different half W e values

50

HNF4051 Rev 3

Los Alamos National Laboratory UCertifitate of Content anb. 7Eracea'btlitp

PuOz-Diatomaceous Earth Standard WRAP40GPU

This NDA standard contalns high purity plutonium dioxide dispersed In diatomaceous ear th Quanhtative Information and uncertainties on the nuclear content of this WRM are listed below Complete information regarding the Pu and Am Content, Pu isotopic ratios, chemlcal composition, elemental impurities, containment, and fabrication procedures a r e retained In files by the Los Alamos hational Laboratory C m Analytical Chemlslry Group

NUCLEAR MATERIAL CONTENT

The nuclear material content a n d total alpha activity for this standard are listed below Also listed are overall uncertainty estimates a t 95% confidence intervals (CI) for each component

Comvonent Quantitv o r Value 95 Yo CI PuOl in standard 45 58093 grams * o 00111 g r a m s (

87 161 % OiPuOl' Pu in standard 40 00226 grams f 0 03740 grams

45 16 mg*

Pu Assay * 0 081 % 0)

"'Am Assay 1128 9 pglg PUOlt t: 0 3 pg/g "'Am in standard -L 0 35 mg (')

Isotopic Weight Fraction*

''sPu

l'9PU

"DPU

2'iPu

9 u

0 00014

0 93809

0 05939

0 00185

0 00054

* 0 000005 (0 t: 0 000015 (O

* 0 000007

i 0 000009 (r)

* 0 000003 (O

Total Alpha Activity in standard 2733 mCi** 1 OllE+11 Bq

I I mCi b' t: 3E+08 Bq (4

*Decay corrected value on 1121199 ** Eiiective 1/21/99

p4k.A cKerley, C a p Leader khTR Analytical Chemistry

.

NDA WRM Production

5 1

HNF 4051 Rev 3

MEASCTREMCNT METHOD AND TRACEABILUY

The nuclear contents of thcl standard were characterrzcd and quantTied wmg the follornng methods w t h traceabhty to the National Institute of Standards and Technology (NIST) or New B r u n m c k Laboratory (NBL) standerds

Measurement Measurement Method Reference Matenal

Weighing 5 place analytical balance NISI traceable w e l a b Pu Assay Controlled Potentlal Coulometry NBL CRM# 126

Am Assay Isotope Diluhon Mass Spectrometry NEIL CRi i # 128 Pu I501opic Total Evaporahon hiass Spectrometry NBLCRM#128

Alpha Activlty Calculated f r o m P u and Am mu, and isotope alpha specific achntier luted below

Pu t ip as stated for NIST SRh1946 Am tlr as staled for NJST

~ ~ ~ 4 3 2 2 ~

IYI 2 9 The stated Alpha Actinty was calculated using the follornng lsotope half lives (in years) 24,119, Pu 6,560, Pu 14 34, Pu 387,000, and "'Am 432 2

Po 87 74, Pu I40 141 241

NOTES

Random and systcmnhc error t e r m wcre combmed and reported as 95% confidence intervals Error terms mclutle estimates of the follomng

(a) Balance precuion, buoyancy, standard wcight bms and transfer loss (b) Long and short term precuion, control check bias, weighing precision and bas. (c) Above welgbmg and assay terms, and transfer loss. (d) Long and short term precsion, and bias (e) Above wclgbuig terms, Am assay terms, and transfer loss (0 Long and short term precwion, and bms (9, Based on propagated unccrtaintics on the Pu mass, "'Am m s s and Pu rsotoplc unccrtamhcs h t c d

above No halfllfe uncertainty components are mclnded and i t IS recommended that all ficdities participahng i n thc h34 PDP prugram use the half lives b t e d above to preclude faclbty twfachty crror tcrms introduced by usmg different half M e values

52

HNF 4051 Rev 3

Los Alamos National Laboratory &ertifitate of Content anh @rateabilrtp

PuO~-D~atomaceous Earth Standard W " 5 0 G P U

Thb NDA standard contalns high purity plutonium dioxide dispersed In diatomaceous earth Quantitative Information and uncerlalntiec on the nuclear content of this WRM are listed below Complete mformation regardlng the Pu and Am content, Pu isotopic ratios, chemical composition, elemental Impurrtiu, contalnmenl, and fabrication procedures a r e retained h filer by the Los Alamos National Laboratory CMR Analytical Chemistry Group

NUCLEAR MATERIAL CONTENT

The nuclear malerial content and total alpha activity for this standard are listed below Also listed a r e overall uncertainly estimates a t 95% confidence Intervals (CI) for each component

ComDonent Quantitv o r Value 95 % CI PuO, In standard 56 99360 grams i 0 0 0 1 1 ~ g r a m s ( ' )

50 01813 grams I 0 04664 grams ('I "'Am Assay 1128 9 pglg Pu02' & 0 3 pg/g(d'

Pu Assay 87 761 % OTPUO,* to081 % 0)

Pu in standard

'"Am in standard 56 47 mg' -L 0 43 mg

Isotopic Weight Fraction"

U'PU

"9Pu

'%I

"IPU

",PU

0 00014

0 93809

0 05939

0 00185

0 00054

i 0 000005 I'

t 0 000015 ('

-I 0 000007 ('

i 0 000009 I'

& 0 000003 ('

Total Alpha Activity in standard 3418 mCP' t :gmCi(" 1 265E+11 Bq t3Et08 Bq (*

*Decay corrected value on 1/21/99 '* Effective 1/21/99

h

Kerley, G r o a e a d e r CMR Analytical Chemistry NDA WRM Production

53

HNF4051 Rev 3

MEASUREMCNT METHOD AND TRACEABIZTTY

Tbe nuclear contents of t h u standard were characterucd and quantfied mldg the follomng methods m t h traceabhty to the National Inrtitute of Standards and Technolow (NLST) or New B r u n m c k Laboratory (NBL) standards

Measurement Measurement Method Reference Matenal

Wclghlng 5 place ana lyka l balance MST traceable weighb Pu Assay Controlled Potential Coulometry NBL CRM 8 1 2 6

Am Assay Isotope Diluhon M a s Spectrometry NEIL CRM # 128

Pu Ltotopic Total Evaporahon Mass Spectrometry NEIL CRM # 128 Alpha A c t h t y Calculated from Pu and Am mas, and

isotope alpha specific achnties llsted below Pu t ip as stated for NIST SRhI946

Am tlr as staled for NLST SKM4322B

a s 219 The stated Alpha Activ~ty was calculated using the followrng uotope balf lives (in years) 24,119, Pu 6,560, Pu 14 34 , Pu 387,000, and "'Am 432 2

Po 87 7 4 , Pu 140 141 1 4 1

Random and systemahc error terms wcre combtned and reported as 95% confidence intervals Error terms mclude estunates of the follomng

(a) Balance prccrsion, buoynncj, standard wclght bus , and transfer loss (b) Long and short term precuion, control check bias, weighing precwon and bias. (c) Above welghlng and asssy terms, a n d transfer loss. (d) Long and short term precwon, and bias (e) Ahwe welghlng terms, Am assay t e r m , and transfer loss (0 Long and short term precuion, and bus

a 4 1 (g, Based on propagated unccrtamtics on the Pu mass, Am m s s and Pu lsotoprc uncertatnhcs M e d above No halfllre uncertainty components are mcladed and i t i s recommended that all f2cditie3 participatmg i n the hD4 PDP program LLP~ the halfhves b t e d above to preclude facrhty t c r k c a t y error t c r m introduced by ustng different balf hfe values

54