ML20209D165

RO Insp Rept 70-1193/73-03 on 720117-730312.Noncompliances Illegible

ML20209D165
Person / Time
Site:	07001193
Issue date:	08/15/1986
From:	Hind J NRC OFFICE OF INSPECTION & ENFORCEMENT (IE REGION III)
To:
Shared Package
ML20209D148	List: ML20209D144 ML20209D165 ML20209D191 ML20209D202 ML20209D214 ML20209D237 ML20209D247 ML20209D259 ML20209D265 ML20209D276 ML20209D281 ML20209D289 ML20209D303 ML20209D322 ML20209D331 ML20209D337 ML20209D355 ML20209D364 ML20209D778
References
FOIA-86-281 70-1193-73-03, 70-1193-73-3, NUDOCS 8609090222
Download: ML20209D165 (30)

Text

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. ,eNUCLEAR MATERI) LS SAFEGUARDS INSPECTION , ,

0F SPECIAL NUCLEAR MATERIAL AT

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KERR-Mc 1EE CORPORATION -

dIMARRON P. UTONIUM FACILITY ,

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,CRESCf. IT, OKLAHOMA ,

, . SNH- 1174

• Docket'No. 70-1193

• RO Inspection Repo t No. 070-1193/73-03 SEC'1 *0N II I. INTRODUCTION

, An inspection of safcCuards contr over special .nucicar material at the Kerr-McGee Corporation, Cimari a Plutonium Facility was made by Region III, Materials and Plant.F Jtection Branch. The inspections -

, covered the period January 17, .>/2 through March -12,1973 for -

• SNH- 1174. The previous inspect ion of the plutonium facility did not

, include the provisions for the FFTF Contract initiated in May 1972.

. The field work was accomplished from February 21 through February 23

. , and March 12 through March 16, 1973. -

II. SCOPE .

The inspection was performed to determine the licensee's compliance with safeguards requirements of Title 10 CFR 70 and specific safe- -

guards requirements contained in license conditions of SNM-1174.

A separate inspection, RO 070-1193/73-01, dated February 16, 1973, was performed to determine compliance with requirer ents of Title 10 CFR Part 73.

. III. ,

SUMMARY

-PRELIMINARY REPORT OF FINDINGS .

• A. Items of Noncompliance .

,. 1. License Condition 3.4 - A report, dated February 15, 1973, -

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'was issued by the licer

- - - condition, but the repc calculation of limits,c

. 2. License Condition 3.7 -

on August 1, 1972. Ar measurement evaluation ope' rations on the FFTF Headquarters.

. 3 License Condition 6.5 Es1:nce crcund plutenit ,

exceed thirty days.

4. License Condition 7.1

• records are not being 2 ing period.

5. License condition 8.1 outlined the findings c and measurement and lir re' view of the remaining

• control system has not period. In fact, no si origination of the plut a this type of review wi' internal auditing deps B. Status of Prior Items of N:

McGee Corporation from C.D.

- 1. Contrary to Condition I the nuclear materials .

the overall system of :

not been conducted witl last review.

- Status: The licensee i this license .

portion of nu.

during the la

. is repeated.

2. It appears that certai compliance with the re '

i trary to 10 CFR 70.54 and distributing Form J. '

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- - - - - - - - - , - , , . - - _ _ . _ _ _ _ _ _ _ _ _ _ , . , , _ _ . - , - _ _ , . - . _ - - _ _ . _ _ _ _ , _ _ _ _ , - _ . - - , - - - - _ , , . ,.,,,m, _ , , - - . . - - , _ - - _ - . - . . . - - , , _ _ - - , - . -

I

.- I a.- Limits of error were not included on the forms documenting

, receipts; -

b. Limits of error for shipments were not reflected on the

• licensee's record copy of the form; and

c. All forms for receipts were not completed 'and distributed

. . within the time period specified.- - -

Status: nese noncompliance items were egrrected during the

, . inspection period, and therefore, were not repeated.

' 3. It was also noted that you had .not- followed the special

. instructions (le tter R. G. Page , NMS, to G. E. Wuller, Kerr-McGee

• dated February 2,1971) for maintaining records and reports under an assigned RIS (YUW) for nuclear material of Canadian origin.

Status: This situation was corrected prior to this inspection and therefore is not repeated. 'Ihe licensee has no Canadian owned nuclear materials at this time.

Licensee personnel furnishing information on the items of non-

. C.

compliance were: Ray Janka., Gavin Hallett, Bill Shelley, i Don Bristol, and Fred Welch. .. t

[V. DETAILS OF INSPECTION ,

• 1. 0 FACILITY ORGANIZATION ,

%e Cfmarron Facility Manager is responsible far clie management of the facilities activities including developing, revising, implementing, and enforcing nuclear material centrol procedures.

. he responsibility for the development and implementation of the

'- safeguards program has been delegated to the nuager, Administration and Accountability. ,

he current safeguards procedure manual and standard operating .

procedures issued by the Safeguards Group are aresently being

. revised. The licensee is planning further revisions when the .

l coatrols for the plutonium facility become conguterized, tenta- .

thely planned for May 1973. .

Cur.*ent plutonium safeguard procedures are prepared and signed by the Accountability Analyst and approved by Unager, Administration and Accountability., Manager Quality Assurance and Laboratory e

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, Operations, Plutonium Plant Superintendent, and Fa'cility Manager.

It,was noted during the inspection that some procedures, consid-cred pertinent to nuclear materials control, were not approved by the Manager, Administration and Ac' countability. It was suggested the document control officer formali::e the procedure to include the Manager, Administration and Accountability for. review and *

. approval of all procedures involving nuclear material:; control.

It is our co'nclusion that the overall management of the nucicar materials safeguards program is so.tisfactory. ,

/ 2.0 ThCILITY OPERATION . . ,- .

) ..

Four material ' balance areas ,(MBh's) had been estab1'ished* at the * '

Cimarron Plutonium Facility: ,

's. Ceramic Area *

b. Scrap and Laboratory .

. c. Fabrication .

. , d. Enriched Uranium (held in plutonium facility for laboratory services) -

o Effective with the tiarch 12, 1973 inventory the plutonium facility is incorporating the following additional fosr HBA's to increase

• the total to eight MBA's. , ,

' . a. Plutonium Vault

b. Pellet Manufact'. ring Ares ,

c. East Half of Pellet Storage Walls

d. West Half of Pellet Storage Walls

• All HBA's meet the license :ondition minimun' requirements and losses should be more casi)y localized by Mn with the inception

. of a computerized internal record system for the plutonium plant.

' Authorized liutts and actual possession of RIN under License No.' ,

. SNM 1174 are as follows: .-

Authorized Limits Possession SNM 1174 360 kgs. Fu

• 117.5 kas. Fu 1.1 kgs. U-235 0, Fossession and use of special nuclear materitt have been confined to the locations and purposes authorized in ::he license as req,uir-ed by 10 CFR 70s41. .

- 'the facility operations is considered satishctory by the inspec-

• tion team. .

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3.0 NEASUREMENTS AND STATISTICAL CONTROLS . .

• 'A . HEASUREMENT S STEM

1. Summary. ,

'. . %e licensee has developed a measurement system that is intended to comply with the requirements of Amendment .

. SG-2 ' to SNH- 1174. The system provides for the measure-ment of_ plutonium in all receipts,, shipments, discards, and inventories. In addition to these basic. require- ,

ments of SG-2, the licensee has a mass spectrometer for measurement of the p,1utonium isotopic composition '

of all receipts and product shipments. .

At the time of the inspection, the licensee was not yet in full production of plutonium-uranium oxide pellets for the FFTF program. . Measurement data were therefore limited in quantity, but measu ements of receipts, shipments, and discards completed to date appear satis-factory. However, on the basis of the physical inven-

, tory conducted during the inspection, it appears that the licensee will' be unable to meet the MUF requirements of license condition 3.2 under normal operating conditions.

ne reason is that under normal operating conditions, large quantities of plutonium are held up in the process; -

8 . these quantities are unmeasurable unless the system is

> completely flushed, a procedure that the licensee claims

)

• is not practicable except at the end of campaigns or jobs because it causes the loss of much produ'ction time and requires the addition of large volu=as of flush solutions *

. which then must be processed. .

%e licensee vac not in full compliance with condit' ion 3.4

- - since their measurement review dated February 15, 1973 did

• not include a quantitative calculation of the limits of ,

o error of measurement system, and in connection with Condition

- ' 3.7, the required measurement review report had not been Effective date of Condition 3.7 submitted to Headquarters.

. was August 1, 1972. .- . ,.

Receipts ** *

, i. ,

he licensee receives plutonium nitrate solution for the FFTP program in L-10 containers froc ARHC0 (HVA). . Each, Ir10 contains about ten liters of solution in a plastic bottle inside an interior stainless iteel container.

- Solutions are normally about 157 plu: onium by weight; each

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, ' full bottle contains about 1800 gr'ans of plutonium. ,

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he shipper groups the bottlesi into lots, a lot con-sisting of eight to twelve bottles, all of which . , .

, presumably contain solution of the same plutonium

, concentration. At the time of the inspecti.on, the licensee had received three shipments from ARHCO, e

.. each consisting of two lots of bottles. In the first two shipments there were 72,833 grams total of plutonium by shippers measurements; the third ship-

.- ment was in the process of being opened and, measured by the licensee. Each lot of containers is accompanied by two sealed ampoules containing plutonium nitrate -

solution which presumably has the same plutonium con-

. Sentration and composition as the solution in the ten-liter bottles. ,

~

, , Back-up data to the AEC-741, transfer documents provide ,*

the receiver with gros's, tare, and met weights of each ten-liter bottle and the concentratien of the solution in the sealed ampoules. Rese data are used by the receiver to confirm the shipper's spessurements. Each loaded bottle is removed from its container and weighed in a glovebox. ne solution is then wacuum transferred to a receiving

• tank and the empty bottle is rinsed, dried, and weighed. ne weights of de loaded and empty .

p bottle and the dif ference give the receiver a gross, tare, and net solution weight to compare with the corresponding shipper's quantities. He laboratory performs an assay analysis on the contents of the two sealed ampoules

, accompanying each lot of bottles. Thas the licensee ob-tains a comparison with the shipper's weight for each bottle and assay of the solution in each lot, he licensee has gone through an evolutionary process in arriving at his

• present method of arriving at the official quantities of

. plutonium in each lot of bottles received thus far. Al '

though shipper - receiver agreement based on ampoules

, measurements han not been unreasonabia, the licensee has varied the sampling procedure used to arrive at official quantities received as follows: ,

, . 1. On the first shipment, ampoule sanplesi two samples

• from each of two bottles in the ht, and a single sample from each of the other bocles in the lot were all analyzed. Only the results cf the ampoule samples were used to calculate, the Fu received and AEC-741' data.

He 'other data were regarded as hckup data and were

, , used for limit of error calculatians. .

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2. On the.second shipment, the licensee went through j

. the same analytical procedure. Later it was ,

decided to ese results~obtained on the duplicate -

samples froc. each c,f two bottles to calculate Pu received and AEC-741 data. Corrected AEC-741'c were accordingly issued on the first two shipments. ,

3. On -the third shipment, it has bee.n decided to use analytical results obtained on samples taken from the plutonium weigh tank downst' ream of the plutonium receiving station. The solution from all the bott1'es in a lot can, be collected in the weight tank,

., then weighed and sampled. Samples taken' in this way are considered to be more representative of the lot than either ampoule sampics or bottle samples. In ,

both theory and practice this is true, since the receiver is duplica_ ting in reverse the shipper's sampling ind analytical procedures. Ampoule and '

bottle samples will still be taken and bottles will be weighed, but the plan is to use these data only

, for backup and L. E. calculations.

The shipper-receiver agreement for the first two ship-

. . ments has been good, meaning that it is within limits -

that have been obtained in the past at other sites. -

[

, The licensee is interested in obtaining measurements that are as good as possible, since his financial l

interests under the FFTF contract are involved. 'Ihc contract states that shipper measurem.cnth of SNM are to be considered and the receiver is obligated to recover 99.57. of the SNM shipped. Recovery of less than 99.5%

.. in the form of finished product pins results in a

. monetary penalty to the licensee. Shiould the receiver disagree with the shipper's measurements, the parties , ,

resort to umpire measurements. ,

In Table 1 on the following page, shipper and receiver

. weight, analytical, and overall Pu me.asurements are com-

. pared for the first four lots of solution. 'Ihe data illustrate some peculiarities that seem to be common to .

- ,' shipper-receiver comparisons of plutonium solutions.

, , R ese are enumerated below: +

1. ne shipper's solution weights are larger than the ,

recef, vers by about 0.1'k. Inspection of the weights

. of individus1 bottles disclosen that this difference is not caused by a scale bias, bu- is the result of the receiver's inability to duplicate the shipper's

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weights of the empty botti,es. Receiver empty. *

, bottle weights are uniformly higher than corre-

, * 'sponding shipper's weights, because the receiver has ,

been unable to dry, the bottles completely' af ter" emptying them, despite reasonable efforts.

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2. The shipper and receiver ampoule assays exhibit a much wider range of variability than do the'veight

. measureme nt~s. The assay differences thus are responsible for the major portion of the S-R

. difference in the overall quantities of plutonium.

, '3. The receiver's assays of bottle sanples tend to

, agree with shipper assays more closely

• than do ampoule assays. When the receiver begins

• the

, , practice of combining the solution from all the bottles of a lot and sampling the entire lot, even better agr. cement should r ' esult, at least in theory.

1 FFTF Plutonium Nitrate. Shipper - Receiver Comparison

. LOT 1 LOT 2 LOT 3 . LOT 4

_(9 Bottles) _(8 Bottics) (11 Bottles) (12 Bottles)

Solution Wt(g) -

R 105,873 100,707 127,033 145,663 8' 106,050 100,772 127,173 145,837 S- R 177 65 140 174 (S-R)/S(%) 0.17 0.06 . 0.11 . 0.12 .

Pu Assay (g/g)

• R (Ampoules) 0.1612 0.1623 0.14 54 . 0.1456 8 . 0.1585 0.1602 0.1458 0.1463 .

S- R .

(0.0027) (0.'0021) 0.0004 0.0007 (Se R)/S(%) (1.70) (1.31) 0.27 0.48 .

R (2 Bottle. Av) 0.1609 0.1619 0.1458 0.1460

. S '

O.1585 0.1602 0.1458 0.1463 8- R (0.0024) (0.0017) 0.0000 0.0003 (8-R)/S(%) (1.51) (1.06) 0.00 0.20 .

_0verall Pu (m) . .

R(AEC-741) 17046 16302 18524 21267 .

8(AEC-741) 16808 16145

• 18543 21337 .

8- R (238) .

(157) 19 . 70 (8-R)/S(%) (1.42) (0.97) 0.10 0,33 S-Shipper *

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3. Discards 'l

, The licensee's plutonium plant,'like all other plutonium

' facilitic's, is designed for health and safety reasons to

• keep normal process lossds and accidental losses to a minimum. Plutonium is introduced into the process as a liquid and removed at the end of the process in pellet form. From beginning to end, the plutonium while in

. liquid form is kept within clo. sed stainless steel tanks which are within gloveboxes or built into concrete' walls.

The system of valves and piping does not pennit removal of solution, from the system in the course of normal operation. In solid form the plutonium is continuously contained within gloveboxes until the product fuel pins c6ntaining uranium - plutonium oxide pellets are removed

, at the end of the process. Removal fren the gloveboxes is possible only by bagging material ost through the bag ports with which, the boxes are equipped. .

Measured discards (FFTF and privately evned) during the

. inspection period (1/17/72 - 3/12/73) anounted to 584 This is 0.49% of the total plutonium

, grams of Pu.

roccipts for the period. Dvor half of this loss was I

', plutonium flushed .out of the process during an exten-sive cicanup campaign between the end of the ZPPR g

, campaign and the start of FFIT processirg. ,

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, The various forms of discards from the 7 1 utonium facility are described in the following paragraphs:

a. Solidified Liquid Wastes

• Since input to the process is an acidic plutonium nitrate solution and the product a solid, large volumes of solution from which the plutoniu4n has been removed must be removed from tha process and ,

discarded. Most of this liquid is in the form of solu, tion filtered from the slurry formed when blended plutonium - uranium nitrate solution reacts with ammonium hydroxide in the precipitation process. The filtrate is collected batchwise in tessels which are .

. sampled and analyzed. A concentratian of 0' .003 g/l or less permits the filtrate to be transferred to a SOOO-liter waste storage tank for ultimate disposal.

HIEher concentrations are transferrod to scrap re- .

covery for reproccasing of the plutonium.

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other sources of low concentration liquid waste in ,

l the scrap recovery process. These are raffinates

' froni the anion exchange and' solvent extraction - .

systems, solvent washes, degraded solvent, and evaporator condensate. E cse streams are.all sampled, analyzed, and transferred to the 5000-liter waste *

, storage tank if the concentration is less than 0.003 g/1,- or deemed to be uneconomical to recover.

De licensce's scrap recovery process has a large capacity so that large quantities of plutonium-containing liquids

• and solids may be accumulated for a lengthy period of time, i: hen the process is operated in a concentrated

, recovery campaign. Le licensee hopes to' opera,te the recovery system only once during the FFIT campaign.

. near the end. '

% e waste 1,iquids from all sources described in the precedf.ng paragraphs are collected in the 5000-liter i i

waste storage tank. When full, the tank is sampled from a drain line sampler and analyzed by alpha

', counting (radiochemical). The plutonium concentration thus determined times the volume of solution in the

' tank givec th,e quantity of plutonium discarded for accountability purposes ,

Contents of the waste storage tank is transferred into 55-gallon drums. Each drum is partially filled with

• a liquid uren formaldehyde resin prior to filling the drum with the waste solution. Af ter, dixing with the resin, called Tiger-loc, the mixture solidifies.

Normally several drums are filled in one operation, and each drum assigned a plutonium quantit'y in proportion to the total amount of Pu that was measured in the storage tank. This amount is normally not more than two grams per drum.

In October 1972 a total of 41 grams of plutonium was bur' led of f-site in 29 drums. This was about 167. of the losses for the month. Normally it is understood that

• solidified liqinid wastes constitute about 257. of operat- .

, ing, losses. ,

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b. Counted. Trash This category of wast accounts for the majo i

losses. Counted tras supplies, equipment, materials which have 2

of_the process and ma of plutonium which ar

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The measuring process the trash in standard count on an activated The ratio of the neut is a measure of the g licensee has guidelin item should be discar processing. For ex6m rubber gloves weighin grams of Pu by neutro ered worth further pr pound valve containin

. considered economical

,. In October 1972, 173

, neutron count, were s was 69% of the measur is about normal.

, c.. Laboratory Waste Plutonium - containin tributes a small but

, to the measured disca ability system, the 1 of the scrap MBA, sin laboratory is in the i

solution samples whic:

scrap recovery system

, sampics which.have no destructive analysis process, however.

Plutonium-bearing was

. laboratory consists o l have had laboratory ri sweepings, and contam

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No measurable S.NM is discarded in laundry waste water. *

. The licensee has a " hot" laundry system for clothing, '

. equip'm ent, and supplies that monitoring . tor health

• physics discloses to be c,ontaminated. There is also*

• a " cold" laundry for materials that monitoring has

' disclosed to be uncontaminated. The effluents from the hot laundry are collected in two 6000-gallon .

tanks. , Periodically the tanks are sampled and count-

. ed by health physics. If the radioactivity is less ,

than 1 HPC in accordance with 10 CFR P, art 20, the l

. water is discharged to a holding pond within the site perimeter. ,If the level is above 1 MPC, it is trans-ferred to the recovery process. Effluents from the

, cold laundry are collected in two 10,000-ga11on tank.s.

If the radioactivity is less than 0.1 MFC, the water is discharged to the sanitary lagoon. If above this limit, there are provisions for transfer of the water to recovery. ,

f. Stack Losses . .-

, No significant quantity of SNM is permitted to be lost ,

via the stack. l The single stack of the plutonium facility is continu-ously monitored isokinetically. The alpha radio-activity level is continuously recorded on a strip

. chart in the health physics office. An alarm sounds when the level exceeds 110% of normal background.

Assuming that all the alpha radioactivity. ih 1972 was from plutonium, which is not strictly true because of the presence of americium, the plutonium loss* via the

. stack was of the order of one gram. , ,

4. Product

• l The licensee's product under the FFTF contract with Westinghouse will consist of approximately 18,000 UO 2-Pu0 2 fuel pins. 'Esch aircaloy pin or rod will contain about

. 110 mixed oxide pellets, each weighing about two grams of '

which 0.5 grams will be' plutonium. The total quantity of .

plutonium to be processed during the campaign will*there-fore be about 1000 kilograms. .

Prior to full scale production the licensee is required to

• produce 500 qualification pins for acceptance by the.

cus t,ome r. At the time of the inspection, a full scale pro-

. duction had not yet started. Four pins had ,been shipped to the customer for experimental use, and finished pellets ,

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,- c:ntaining 10.7 ,kgs. of plut:nium wers star 2d in p211st

. storage wells in a glovebox. -

The ' accountability measurement system that the licensee will use for p'lutonium product will be a part, and ., .

arParently a minor part, of the. overall quality assurance that the licensee will be required to provide under the FFTF contract. What was learned of the measurement system for plutonium in the product during the inspection

• was obtained from discussions with licensee rep esenta-tives rather than from any extensive , study of acasurement

. records or procedures. There are some aspects of the measurement system,. including sampling requirements, that

. have not yet been< firmly agreed upon.

. Those aspects of the product measurement system tha't are -

of interest in plutonium accountability are described below: , ,

Blended uranium-plutonium nitrate is ' precipitated, dried, calcined, and milled to give a " lot" of mixed uranium oxide-plutonium oxide powder. Such a powder lot consists .

of about 200 kgs, of oxide and does not coincide with a receipt lot of plutonium nitrate solution bottles. A 4 powder lot is sampled and analyzed for plutonium assay, uranium assay, oxygen, O/M ratio, impurity content, homogeneity, and isotopic composition. Each powder lot must be certified by the customer before the licensee proceeds with pellet manufacture. The licensee has re-

. ported that difficulty in meeting homogeneity require-ments has been a major holdup in production thus far.

Each powder lot is an important produc' tion unit an'd lots must not be crossblended. For this reason the powder processing and pellet fabrication gloveboxes must be cleaned out between each lot. Residual quantities of powder and pellets are not added to the next lot, but go .

to recovery. .

Following certification of powder lot, pellets are manu-factured, sintered, arrayed on boats or trays, sampled, and weighed. It is reported that the sampling require- .

ment will be 15 pellets per lot (about 100,000 pellets). -

.This sampling requirement has apparently not been

. finalized; at one time the requirement was expected to be about 1000 pellets per lot (1%), which would appear tobeanunmanageableanalyticalwor;kload. Each pellet in .

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j the sample is analyzed for plutonium assay (g/g) and some pellets are subjected to isotopic analysis, -

impurities, O/M ratio, and physical tests. We -

i plutonium. assay' and isotopic analyses are those that are used to determine plutonium in product shipments. *

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Finished pellets are stored in small metal cans, .

. . about 1000 pellets or 2.5 kilograms to the can. The cans are stacked in storage wells in a glovebox. He weight of pellets in the cans as determined on a Hettler balance, combined with the ~ plutonium assay -

from the sample that was previously taken,' constitute the SNM measurement that will be used for accountability.

In the pin fabrication area, pe'11ets are stacked .iri a '

core stacking trough to the specified length. A stack will normally consist of 110 pellets but this. number can vary slightly depending on pellet length. From the stack the pellets are mechanically pushed into the open end of a pre-inspected and tested zircaloy pin or rod. After helium gas is forced into the pin, an end esp is welded over the open end and the finished rod is removed from the glovebox, inspected, radiographed, cleaned, and '

stored in wells.below the floor level until they are shipped. -

B. NEASUREMENT METHODS AND CONTROLS ,

1. Scales and Balances .

Dere are ~about ten scales and balances in the plutonium facility. All are used to weigh materials that .are inside

. gloveboxes at specific points in the process; the instru-ments all have fixed locations and all have a set of

, checkweights. .

. ' For measuring solutions at the beginning of the process

• there are three Toledo scales. The scales are cutside gloveboxes and mechanical linkages connect them to weigh

. tanks or a weighing platform inside the glowbox. One scale with a capacity of 25 kgs. is used to weigh plutonium nitrate bottles as received. he other two have capacities- '

of 500 kilograms and are used to weigh vessels containing blended plutonium nitrate solutions. De SCO kg. scales -

have precisions of 50 grams according to the licensee, an amazingly good precision for scales of this capacity and complex mechancial linkage. Usage, of these scales was -

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. t-

~

. observed during* the inventory' and a qualitative check.

made of their sensitivity and reproducibili~ty, both of ,

which were good. It was not possible to make any scale ' .

. calibrations during the inspection because of the con- l, taminated condition of the area., It was stated that the ,

l scales are checked and calibrated monthly by the vendor i and stickers on the instruments indicated a calibration in February. - -

/

' ' Downstream there are several smaller c'apacity balances in gloveboxes used for weighing powder and pellets. ,

There are three triple beam balances and four Mettler

" precision balances The Mettler balance designated ds the one used in accountability weight measurements of sintered pellets was checked over its entire range of

. , 0-250 grams with standard weights. The balance exhib-ited a bias of +0.01% against the standard weights over its entire range, an ins,ignificant amount.

To date the licensee has developed n?o limit of error data on his scales and balances. Plans for establish-ing such limits appear in a new ILnit of error manual .

and a recently revis,ed " pro forma" statement. Despite the lack of data, the important balances appear to be maintained in acceptable working order and standard weights are available and presumably used to verify t heir reliability. .

2. Analytical Measurements

a. Chemical Analysis ,

Amperometric titration is the single, basic a'ssay method used by the licensee to determine plutonium

. in solution and pellets. Prior to the FFIF c .

campaign, coulometric titration was used, but this method has been 'discontined because there were .

difficulties in maintaining the electronic equip- .

ment and the method is tLme consuming.' 1mperometric titration, is more dependable and quicker, and no accuracy is sacrificed. Other laboratories have

. discovered these same facts. .

. The assay procedure, as used by K-M is similar to that described in Selected Measurement P2thods. -

The ferrous ammonium sulfate titrant is fresulys-prepared by each shift that uses the metlod, an . j important consideration in obtaining accuracy.

e O e p

. . e

(- (~ )

%2 titrent is standardized 'against a mixed

' uranium-plutonium standard solution made from HBS ,

metal and U,38 0 . This same standard solution is .

analyz,e,d as a control standard when, analyzing

. samples.". ,, ,

Re laboratory proper'has no part in the determina-

- tion of limits of error. Data are analyzed and'LE's determined by an employee out::ide ,the laboratory.

The amperometric method has a precision of 0.287.

relative according to the procedure, but this is not

~

a working, current precision determined by routine analyses of standards or samples. %e licensee has

. . described the methods that will be used to determine

. . analytical limits of error in a recent manual

• but no data are yet available. -

Required ' limits of error,that the licensee has needed thus far to complete the receiver measurement section of the AEC-741 forms for the plutonium nitrate that has been received, have been calculated on an "ad hoc" basis from the replicate measurements that have been .

made on ampoule and bottle samples. On the first four 41ots of plutonium nitrate received, the following inconsistant limits of error were reported. The first

. two limits are smaller than could be expected to be routinely attainable, the second two limits are more representative of what can be routinely achieved. The data serve to illustrate the anomalies that are obtain-ed with limited data..

Lot No. Pu (grams) LE (grams). LE (7.)

~

1 17046 100 * . 0. 5'9

. 2 16302 89 0.55 .

. 3 18524 229 1.24 l

4 21267 262 1.23 .

1 .

! he customer of the licensee reportedly has established some strict controls over the licensee's assay measure-ments of powder and pellets. He customer has provided .

. a large number of blind powder and pellet standards . .

- which must be analyzed by the licensee slang with pro- -

. , duction samples. Results must be reported to the cus-toner and approved before the licensee's r.easurements '

are valid. The licensee is not told the true or l official assays and so cannot use the data for limit of .  :

error calculations.

1 . .. .

.w

.g , .

1. " 8* * '"* .._-.._.._.,_-_,,[_.y , ,m , , , , _ , , , , _ , , _ _ , . , , , , _ - " 4 -6 - - - - - - -

. v

- . s .

b. , Isotopic Analysis Isotopic measurements are made on a surface ionizations ma.ss spectrometer in the licensee's 4 '

own laboratory. Measurements are. Ifmitied to isotopic ratios of plutonium, and uranium; the instrument is not used for quantity toeasurements f-by isotopic dilution. Data from the mass spcc- -

trometer are all fed directly into a computer.

Recently the, licensee. lost the services of their mass spectroscopist, anfexperienced and qualified

- professional. The work is being continued by .

' te chnicians .

c. Radiochemical Analysis -

The only other type of analysis that enters into determination of plutonium , quantities is salvent extraction-alpha counting. This method is' used to determine plutonium in dilute so10 tion; in the accountability for plutonium it is the method used to analyze waste solutions before they are solidiff for burial. Single samples are analyzed. The plutonium is extracted with TOP solution; a solven' that is considered more specific for plutruium than the more common TTA.. The extracted samph is coun

' for total alpha, and alpha pulse height aialysis i used to subtract out the plutonium -238 artivity.

Precision of the method is stated to be diout 107..

- However, this limit of error does not apptar to be firmly established but it is typical for trhe metho

. The limit of error manual indicated that there is plan for determining the limit of error er the FFI program progresses.

d. Counting Methods ,

• The licensee has a neutron counting insernment th uses a plutonium -236 neutron source for determini plutonium. quantities in various forms of solid war l

. All wastes are packaged in standard fibemak cont 8" D x 10", for count;ing. Items containing econot

- cally recoverable amounts of plutonium am sent ti recovery; those containing less than ecotanically coverable amounts of plutonium are sent 6 scrap ery; those containing less than economically reco-quantities are sent to off-site burial. -

\

l - .

i l

\

e - -

(

3 . .

e I The measurement technigde consists of counting a

' ~

fiberpak containing no plutonium for 1000 seconds, .

then counting the fiber pak containing the con- -

taminated waste for 100 seconds 'in each of two positions 180 degr.ees apart. A ratio of the waste .

, container count versus background is calculated.

Plutonium content in grams is determined from a curve relating grams of plutonium to the ratio.

4 The curve was derived in 1971.using standards containing known amounts of plutonium. The standards

. are still in existance and are used oc~casionally to check

. operation of the instrument. These data are not recorded and no up-to-date information on limits of error are available. The overall limit of error is tho,ught to be

. "about 207.", and a study is planned as part of the limit of error program.

Gamma counting is employed to determine contamination

. levels of general waste before burial. The method is only for contamination control and the counting is not converted to plutonium quantities. Gamma-counted waste is thus not a part of plutonium accountability.

3. Sampling Procedures .

g i

The licensee has no recorded information on the inaccuracies that are introduced into the measurement system by his various sampling techniques; the proposed 1 Lait of er,ror *

. program includes procedures for determining these.

I

, The plutonium nitrate solutions are sampled as r.eceived by

. " grab sampling" from the 10 liter bottles. Thus far a sample has been taken from each bottle received,and bottle--

to-bottle assays have varies in about the range that is to be expected from non-agitated bottle solutions. Overall agreement for entire lots has agreed within 1.5% with -

shipper assays. Single grab samples from bottles do not, however, permit any assessment of sampling error, since the differences obtained result more from actual assay differences rather than sampling error.

After the contents of the b6ttles in a lot are blended, the

• plutonium nitrate is sampled at the plutonica nitrate blend-

. ing station. The sampling procedure is to agitate the vessel contents ten minutes for each 100 kgs. of solution, then take a single sample. The agitation process ensures that a sample .

as representative as possible is obtained, but no determination

, 19 I

-k - - . - - 9 , - -y.m , ,

, .. (* -

f-n s . .

of sampling error can be mede from data obtained on single samples. A procedure to determine sampling' error from ,

analysis of replicate samples is planne,d for the future.

The uranium o'xide-plutonium oxide powder is sampled on some. -

, basis ag ecd upon between the licensee and.his customer.

h is procedure was not investigated. Powder homogeneity is an important quality, therefore powder sampling must also

. . be important, but since powder is an intermediate form in ,

the process, the measurements do not figure in overall accountability unless the powder is on inventory. .

. . Product pellets are sampled on a . basis agreed upon with the customer. These ' sampling arrangements appear to be not completely resolved. Present ex'pectations seem to,be that *

. fifteen pellets will be sampled out of each lot of about 100,000 pellets.

He only waste stream of importance .that is sampled is the collected filtrate solutions in' the 5000-liter waste storage tank. Contents of the vessel are agitated, then a single l drain sample is taken. No calculation of sampling error is -

possible from single" samples, but sampling stror would be an insi*gnificant part of the overall measurement error, because of the relatively large error. inherent in the radiochemical analysis which is used.-

C. LIMITS OF ERROR-MATERIAL UNACCOUNTED FOR (MUF)

. During this inspection period the licensee conducted three' total plant physical inventories - March and July,1972 ~and March,1973.

. Between the January 17, 1972 physical inventory (beginning

inventory for this inspection period) and the March, .1972 physical,

' the major activity in the plutonium facility involved a cleanout of the system in preparation for the introduction of FFTF j ,

plutonium. In this three month period, approximately seven kilo- -

grams of holdup material was removed. Gamma measurements of -

equipment during the March,1972 inventory indicated 1,100 grams

, plutonium (privately owned-non FFTF) was still in the system

! adhered to processing equipment. De licensee stated that they l

don't expect to get this material out without tear down of equip-

!. ment. .

l .

Between March and July,1972, FFTF plutonium was introduc'ed into the system. In this period approximately 50 percent of the wall l

cells in the ceramic area and 10 percent of the scrap recovery -

system was wet down. he calcining furnace in the wet ceramic l

I e

1. ,

l

- - , we< ,-- _ _ -,,,,r-. -----,-----a-- --- , - - - - - - - - - , - - - - - - - - - - , - - - - - , - , , - , , ---s

y

• aran; pallet pressing and sintering furnaces had siso been

. utilized in the processing of FFTF matarisl. ,

. The licensee reported the following total facility balance

. and limit,s of error for the period January 17, 1972 through July 7, 1972: ,

Fu (Grams) LE (Grams Pu)

Beginning Inventory (1/17/7.2) 11,742 341 1 Receipts . 33,512 47 Shipments' 9,872 30 Discards ,

503 133

." Ending Inventory (7/7/72) 35,111 . 381 HUF ,

(232) 531,

~

. HUF - Privately Owned - (242) gms. Fu NUF - FFTF - 10 gms. Pu '

According to the licensee, there were 4,539 grams Pu holdup in the system du,e to processing FFTF material between March and July 7, 1972. The following July 7 physical inventory breakdown can be constructed:

. July 7, 1972 Physical Inventory Grams Pu Discrete Items 29,472 Holdup (P-O Material) 1,100 Holdup (FFTF Material) 4,539 35,111 ,

The limit of error of the ending inventor,y did not include

~

any calculations associated 'with holdup. -

. The licensee reported the following total facilty balance

. and ILmits of error for the period July 8,1972 through kbrch 12, 1973: .

~

. 152 (Grams). LE (Grams Pu) l 381 i Beginning Inventory (7/8/72) 35,111 Receip t's 83,181 51

. Shipments 176 2 Discards 586 174

- Ending Inventory (3/12/73) 117,530 -

671 ~

l ~

', HUF 0 . 793 l

l i.

i .

- em O'

. . . _._.____._m . _ . _ _ ..I

I. .

According to the licensee, 'there wara sn additions 15,827 grams Pu deposited in the system as holdup during the July 8,1972 -

March 12, 1973 period. 'Ihe following March 12 physical inven- *

. tory breakdown can be constructed:

March 12; 1973 -

' Physical Inventory i Crams Pu j Discrete Items 106,064

. Holdup (P-O material) . 1,100 Holdup (FFTF - previot s period) ,

4,539

• Holdup (FFTF - this pe.riod) 5,827 117,530 Again the ending inventory limit of error did no' t include uncertainties associated with the holdup quantity.

Since the March 12, 1973' physical inventory, there have been negotiations between the licensee and AEC resulting in changes to the safeguards amendment. The new licensee condition 6.2 states that a fixed value shall be established for the quantity and limit of error of equipment holdup of plutonium by

, June 30,1973. . At this time the inspection team will review the licensee's established fixed values.

Combination of the two inventory period calculations results in the following tota 7 inspection period baIance: -

Pu Grams) . LE (Grams Pu)

' 11,M2*

Beginning Inventory (1/17/72) 341 Receipts 116,593 - 69 Shipments 10,948 30

, . Discards -

1,989' 219 t' 106,364 Ending Inventory (3/13/73) 671 Holdup - 11,466 -

HUF (232) 787 * ,

These total inspection numbers differ s1Ightly from the attached j

inspecti~on period material balance totain for two reasons:

l 15 Inspection period balance includes 12ternal activity while

• the above totals do not.

2. 'Ihe above Receipts and Discards totals both include 11 grams

- Pu which we cannot reconcile, but the total MUF figura is not affected because the 11 grams Pu are offsetting in' the material balance equation.

i .

. =_

• Www - - _ - - - _ _ . - - _ . . . - _ .- _~ __ . __ , _ _ _ , . =_

.a Wra e I

End c appr ,

\

Qor tory sta daoximat ont n plans tic, ain ers of rds, pu sta n c re nundred i s da r ds

• a d. burnb n ad, ted impu rWe em tinghou was a le io tamin co a s s te re p be enoved e in n ider m d ms.

e spe ass ayed c ific by the labo os t.c ase to be SNMai c as a onte n 3

all n a ad n ratory.s, minu s ssigne 2.

eu tronnalyticaass l ray re Pelletswhatev

- Pelle,t . , co n u ted. equ et ssults wer ad n e .

S tor po m

All age Ar e nu ber .e trac el a store dSNM a w

s. The sc wa in - . .

s tra c e a me tals ca in.mthe fc 3 glov boxee s bles toc 'pns in of ,

othe j

, Pellet Ma rwis e e ificstorfinished appe a

age e

pe a enalytic a lw lls. .P llets, c

The glo nufa turing A rd clea. n requ luto n1 me was vebox es rea et s fo ad n ,

, in ntc whovisible se e equipm in th n spe tion ,inte rior glov boe n ad a of s c e xes t had 4 c lciners ou ld o be en m thent was o

inte r i ors be insper thos e pie a

cle ned.

Cera ic (We t) Area po s of ces No of et,

~

Plutoniu n s ible. all cted.

press How stored inm ad e,conv s ever

^ -

sa mple ur n eyot or w ll a iu a

o

. se lutio ns wwe igh storage'ta ksm n pluto ium .

w ighed er n

.A e train the s adn sa nitr ate o obseportio r e n of thismpled, nsferrd e n e ta ks. It is the nto po v d. thessslution

.O sa n m toe theDuring o ib s w mther tha mpling andov d cla ks lutio n ^inv nle to et e' pty of n wa e to w llw e ighte tory, re e w ighing a ta n

• c ivin SNM.The ll storage, the pr e storage. ks, prnitrate, g glove box are oc dure c area was of e ipitation the'v eigh , thea include was

• the sc we igh s the reported exc n the ept lic sixty a w tor ll ssystem, rbalen ta or n

ks m fxscale ta g ensee r the to be

\

that wasfor 33 of epor tedall age ta n kscalcitution le nded so pluto nitr ate e .

w ighed, sthe 4 a the system , lution,nium

. a 0 v ll egripm Forent invent adn ory pu forty the mpled, na dtadts that to be rpo s

. zatu r c e, s

\.

ned ontainedempty to the o a s lutio n e

w ll"tan ks

.~..... .

e

. N Y  %

'

• u. .a ma b=p,usqina ted This vz of the attempt v o so a sa Apr tectionging of s out re sul mai ome c s t difficul't of a bcertmi equipmc boxdditio wa n ecau e es nally, s r m ec n n

ad adn theequir e d, makio r 'e tta inated spills,thi a

lic ens

,ther eforis difficul equipm r etn to s isng in'pe

' ac ee 's t s c tiom cepted. ases impos s ible all to es , or wi u i e ho nd

.' Ther ertion that e.

h e thinsed wit e had In

'that es is,mu c h st conc e emptiedeffe c t, in the erv s to ainles s t pipe s syste . conn

. the s, an w m c et steel vaddition,d es e ould Pluto o n iuthevar iopiping in 'th .

s ls a plu_to niun t be mea o us ves e e c era plutoniu s hee ls m o msu's rde lution c u s ls ad i flu s hing,m c u o ld n o ld re n ei bea d'adhes lution a c du r ing thor r ould re main i nto oughne ss the am r e n inv in se to; n n inv m ake of ou t remov em d e ad mea wa main n to the entory.any flushthe flus is ov de su e lls. ome y 5 of being rd g pro e pr c

Su h unr La'bo a the ce c dur .oportioonly by a r tory ramic syste e nal c

wThe m The l ic to t er laboa prio ens ee c e inv rn tory c

- - r to th(

ontainers e toried.ontained infor 'he s about I

' n n e ite ms cthirty in'di me ts matio as ,wpellets, w po d

. tory ,u radioa ss nta me p rpo s o e,a r

e. ay, a ndvailable, nd onsisted n r ofvidu al asure s l iquiditems grams men ts u The inv gamma co w ight asta da ds. w e

of

• 6 n e tly nto n n o luWhere ass aste Scrap Re pluton ius m officie ry appeu ting w v

'd me ay ac cu rd ere a e u e cove ry n hand. a c sd mea su r- e

, The scrap r r te for thec implete for inve-n ad

~ n ecov the o ly 'atmaterials defi ery syste n approximate0 50 c n o tr at c infrequ ned as ,

ad n n i scrap s

or ca et mma ha a large solutiopipinE ls, yobec apac ity s tha mpaign.nterv a

n n s c c system, does theThe system In uhac slle ted ad n o that co s o lv n main c at the n proce nsistedpreparatio x cproce ontain s s ed of a ssed e t e tra ti of the tw entirely ofn entofor inv on sa, includin ed more ves s,els enty wa ll so lu ry, scr anio n e g a dis-xcha nge. ,

storage tions, wap ere :sterials

- ta ks n co o

.. which arns lidated, which

\

. e des ignatedin 14 e

• fo' r N..,

~

, '.N .

A

% * ~.

l l

l 9Y .

l . _ _ _ _ _ _ . _ _ _ . _ _ __

_y, __ _ _ _

scrsp recovery usa. These solutions,were transferred to

~

the recovery weigh scale tanks, weighed, sampled, and .

returned to.the wall storage tan.ks during the inventory.

• As in the ceramic area no flushout of the recovery system -

. was made prior to the inventory. .

, , All license conditons in Section 6.0 were complied with

. except 6.5. The lice.nsee ~had not closed a material ,

balance _around plutonium in process at intervals not to exceed thirty days. This was reported as en item.of noncomp11ance.

B. INVENTORY, KESULTS . -

. The. plutonium material balance on FFTF plutonium ca,lculated by the licensee at the conclusion of the inventory is tabulated below: . .

." Crams Pu

~

Beginning Inventory (1/17/72) Receipts 116,685 Shipments .

176 I

Discards . 282

.Ending Inventory (Book 3/12/73) . 116,227 Ending Inventory (Physical 3/12/73) 105,851 Holdup -

10,366 HUF 10 ,

. The balance shown is for the inspection period and includes only plutonium received under the FFTF program. Other

, plutonium totaling 11,742 grams 'was on hand at.the beginning

.of 'the inspection period but was all disposed of as shipments and discards except for 1,313 grams on inventory during the period and is not ine,1uded in the balance. Of the 1,313 grams, 1,100 grams is considered holdup.

The large holdup of 11,466 grams is,9.8% of the plutonium -

receips. The licensee maintains that this quantity is real plutonium in the process in unmeasurable places and therefore has decided to identify the 11,466 grams as h61 dup. This assumption is plausible because of the large amount of space

• in connecting pipelines and valves in the ceramic. process in which solution can accumulate. Such accumulation could also loccur on the walls of vessels and interior of equipment in the

' pellet manufacturing area. The licensee believes that the holdup quantity uill eventually stabilize, so that thereafter it will be possible to distinguish MUF from holdup. It is j believed (by the inspector) that the holdup will eyentually

. l

. e

-- - . ~ .._ . T

. n n -- ~ - . -- . .

,- _ _ _ _ _ _ , . _ . - - - , - . , -__ . - _._.--._._r. -.

,, - - , .- v ,% ,

s -

racch a maximum but that thi variability from this maximum gill be quite large, so that a large LE will have to be attached,to the holdup, ,thus obscuring accurate determination of FUF and LEMUF. .

C. . AEC INVENTORY SAMPLES , . . .

, , Five samples were I taken during the inventory by the licensee  !

. which were selected by AEC for analysis at Los Alamos. The l number of samples se.lectsd was small because th'e available 3L chi l shipping container would not accomodate a larger number. The

, sanples were ' selected to represent a significant amount of plutonium rathe.r than resorting to random selection because of the small number. A comparison of LASL and licensee assays. is

. tabulated below.

• Sample No. Material LASL (g/g) Lice nsee (g/g)

'l Pellets 0.2426 -

0.2440 2 Pellets 0.2392- 0.2440

. 3 Pellets 0.2420 0.2434

4. U-PuNitrate 0.0118 0.0118 5 U-PuNitrate 0.0262 0.0165 l fnspection of the data discoses that agreement is good for all except sample number 5. Here the difference is so large, 59%,

that is almost incon'ceivable that the two laboratories could have analyzed the same solution. There is s'uspicion therefore that there was some error in sampling or sample identification, resulting in the laboratories obtaining solutions that were not replicates. The sampling of the AEC sanple was witnessed.

The U-Pu nitrate was transferred from the vali storage tanks, agitated about twenty minutes, then the sample taken. Solution was allowed to flow through the sample line long enough to flush

. the line prior to filling the AEC sample bottle. Following an

, hour's delay, a sample was taken for the ' licensee laborato'ry,

• then solutions from other wall storage tanks were moved into the weigh tank in turn and sampled. The samples taken by the

• licensee for his own analyses were.not. witnessed. Non- repre sent- *

. stive sampling or incorrect identification could have occurred.

. The large difference between the analyses on sample number five represents approximately 4000 grams of plutonium. There is ,

l .

insufficient evidence to conclude that the licensee's analysis

! .is incorrect, but the probability exists. If the .itigher result is correct, then the holdup (or MUF) quantity would be only 7.5 i

kilograms.rather than 11.5 kilograms. .

l .

. -27 ' . .

e l

. -emmp*

. e o

• * - e sm es n

+ s No apparent loss of a discrete' item or container has been reported for the inspectibn period. ,

. g. -

J. A. Hind, Chie f -

Materials and Plant .

. Protection Branch

Attachment:

Material Balance Report'

• e t

O I

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1. . 8 O

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am - 2 9-essesp g

• **h + w w l

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~ . . .

Y KERR-HCCEE CORPORATION - FBN . JEC .

j

.HATERIAL BAIANCE RETORT FOR PIDTONIIM .

, ,l

. 1/17/72 - 3/12/73

_/'

• Beginning Hessured .

• c Inventory

• Inding

,i*

Receipts .. pigments Diecards M. Inventory 1/17/72 * ~

3/12/73 Pu Isotope Pu Isotope Pu Isotope Pu Isotope Fu Isotope g Isotore ITTF . 0 .0 116,685 102,657 176 154 282 247 10 9 116.217 102,247 STATION 1,886 1,662 8 6 1,543 1,367 351

• 301 0- 0 LIASE . 9,679 7,067* 0 0 9,536 6,962

• 143 105 . 0 . 0 5VREIGN On!VATE . 177 162 177 162 * -

, , g 0 0 .'

KM- PRIVATE O O' 1.373 1.044 . 302 ~ 250 (242) It00) 1.313 974 (

7nTALS 11.742 8.891' _118.066 103.707 11.432 8.645 1.078 0

'9_01 (232) (171) 117.530 103,221 1/

J/ Includes 11,466 grams Pu and 9,871 grams isotope as Holdup S

, =

I l'

Y