ML20209D202

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RO SNM Insp Rept 70-1193/73-08 on 731203-07.Noncompliance Noted:Limit of Error Associated W/Muf Exceeded 1.5 Kg Pu. Supporting Documentation Encl.Portions of Rept Details Illegible
ML20209D202
Person / Time
Site: 07001193
Issue date: 02/13/1974
From: Hind J, Peck C
NRC OFFICE OF INSPECTION & ENFORCEMENT (IE REGION III)
To:
Shared Package
ML20209D148 List:
References
FOIA-86-281 70-1193-73-08, 70-1193-73-8, NUDOCS 8609090234
Download: ML20209D202 (15)
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6 U. S. ATOMIC ENERGY C010iISSION

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DIRECTORATE OF REGULATORY OPERATIONS REGION III RO Inspection Report No. 070-1193/73-08

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Licensee: Kerr-McGee Corporation Kerr-McGee Building Oklahoma City, Oklahoma 73102 ,

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Cimarron Facility Plutonium Plant License No. SNM-1174 f k Crescent, Oklahoma 73028 Priority: I j Category.: A(1) ,

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Type of Licensee: Plutonium Fuel Fabricator Type of Inspection: Special Nuclear Materials, Announced Observation of Plutonium Inventory 4

Dates of Inspection: ' December ^ 3-7,'1973'-

Dates of Previous Inspection: October 19, 25, 26 and November'2, 1973

/3 Y Lead Inspector: -C. C. Peck Other Accompanying Personnel: None Reviewe By: d ief c /3!7[

(Date) terials and Plant Protection Branch

Attachment:

Findings (Exempt from Disclosure) ,

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8609090234 860815 PDR FOIA -

CANTREL86-281 PDR t

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SUMMARY

OF FINDINGS ,

Enfercement Action The following item of noncompliance was identified

The licer.see's limit of error of material unaccounted for (LEMUF) for the

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30-day material balance period ending December 5,1973, was 6.802 kilograms,-

and the LEMUF quantities for the four previous material balance periods vere as follows:

Period Ending LEMUF (kgs)_

8/10/73 6.299 9/11/73 6.127 10/10/73 6.337 l ~

i 11/9/73- 6.542* .

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~ License Condition 3.2 states': "The frequency and quality of the measurements

' made to comply with the license conditions shall be controlled so that the

. limit of error associated with the material unaccounted for (LEMUF) for the 30-day material balance period does not exceed one and one half (1.5) kilograms of plutonium."

Licensee Action on Previousiv ' Identified Enforcement Items Items of noncompliance identified in the previous inspection (February The 21-23 and March 12-16, 1973) were not within the scope of this inspection.

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status of these items will be investigated in a future, inspection.

Unusual Occurrences: None ,

Other Significant Findings: None Management Interview

  • A closcout meeting was held December 7,1973, by C. C. Peck withSafeguards R. A. Janka, Manager of Administration and Accountability and G. R. Mallett, Specialist.

The discussion centered on the physical plutonium inventoryThe conducted by the licensee December 3-6 and witnessed by the inspector. .

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licensee representatives were advised that in the opinion of the inspector the observed portions of inventory had been conducted in accordance with the licensee's established inventory procedures. Instances were discussed in which minor violations of the' procedures had occurred. It tas concluded that these were occasioned by inadequate understanding cf the inventory procedures on the part of individuals involved in conducting the inventory and could be corrected in the future,by continued emphasis on personnel training.

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_ REPORT DETAILS

_ Persons Contacted W. J. Shelley, Director, Regul cci Contro C. R. Mallett, Safeguards Specialist J. V. Marler, Plutonium Plant Superintend ent T. Clanton, Auditor - Kerr-Mc P. Carst, Safeguards Analyst.

um on D. Osvald, Safeguards Clerk i C. Cender, Safeguards Clerk

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J. V. Smith, Process Supervisor

, Plutonium R. J. Adkisson, Contract entativ mRela R. Marshall, Manager - Laboratory

_ Scope of Inspection 3

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, I by the licensee from December u onium intervals not exceeding thirty days bySuch Li in cense Co i and Plant Protection observing the particular inventory ofo.Decem Amendment SNM- to had been unable in previous inventoriesr 3-t to comply which for (LEMUF) states for 'the that the inventory 30-day limit of error period e vi s shall from the caterial balance for nvento orth was 6.0 high.

unusually kgs; although within the LEMUFgs, .

of 6 t

  • appraisal of the licensee's inventory ance.

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The process of conducting the inventory c consi wh weighing, sampling, from December 3 through 6. and listing all plutonium

- onta prior to the inspection. areas were also es pri o

been in an unchanged conditio ems t current the measurements inspection period. only on new items or tho v ous ir se that An attempt to perform curren E

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Thus, inventory items, normally numbering over 2000, would be made at an earlier date.

Results of the inventory, that is, the construction of the material balance and. calculation of the FNF and LEMUF quantities were not determined until several days after the end of the actual inventory process and were not witnessed as part of the inspection.

. C'ompliance with license conditions other than 6.0, Inventory only to the extent and could be evaluated.

The following sections, whose titles correspond to license conditions, present the details of the inspection.

Facility Operation (License condition 2.0)

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As required by the license condition, the plutonium facility uses the materi Seven MBA's have been balance area (MBA) concept in controlling SNM. establishe

. instances the supervisor of tihe area. Move =ent of SNM between MBA's is controlled, bility for more than one MBA.and the various points at which losses can occ by the license condition.

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MBA's and their custodians are listed below:

1 Number Custodian MBA Chem Process Supervisor 11 Scrap

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Lab Manager Laboratory 11 Chem Process Supervisor 13 Ceramic 12 Records Clerk Vault 21

  • Fabrication Supervisor Pellet Manufacture ,

Fabrication Supervisor l Pellet Storage, East 22 ,

23 Fabrication Supervisor Pellet Storage,5 test

  • Fabrication Supervisor 31 Fabrication , ,

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_ Measurements and Statistical

. Sufficient information was acquired du:

fact that the licensee is making all tl determine the quantities of plutonium with receipts, shipments, discards, and License condition 3.2 requires the lice i

. quality of his measurements so that the material unaccounted for (LEMUF) does not exceed 1.5 kilograms of pluto plutonium nitrate received measured by weighing and assay of samp measured by radioassay and neutron count items are measured by an appropriate e. m prior to the inventory.

i detail during this inspection. Quality of the t 1 Previous and balance accuracy to be acceptabic a samples formixing sufficient and blending are perfor analysis.

of inaccu ate weighing wa when weighing errors of more than a hun 2100 grams each.while reweighing fo by'100 grams. The corrected weights it The errors in the original insufficient understanding of the weighin

" incorrect use of tare weights. g Although t in the plutonium inventory, it was not of the licensee has experienced. erro 1

were detected during the inventory.No other w

! Laboratory analyses of samples are th i

that inherently produces the largest limit s i amperometric titration as his basic method i

with high plutonium concent used in industry for such materials and has be made for the presence of chromium a licensee does make these correction A sec radioassay, or alpha counting, an acceptab B

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- and/or dilute and do not represent a large amount of plutonium. The accuracy

- of the method is not high; claims of 10% to 20% cccuracy expressed as the coefficient of variation of a single analysis are common. This level of accuracy is acceptable, provided the samples analyzed do not represent major

? portions,of the material balance.

To ' test the quality of licensee's analytical measurements, three solution samples were taken during the inspection for analysis by Los Alamos Scientific Laboratory. The samples chosen were from scrap area vall tanks containing several kilograms of plutonium. Two samples were' solvent extrac-tion feed, the other solvent extraction product. Scrap area sampics were

. selected because this area has the largest variability of any of the MBA's and the wr.11 tanks in the area contain large amounts of plutonium. The AEC samples were taken at the same time the licensee took replicate samples for his own analyses for inventory purposes.

The licensee stated during the inspection that the product sample would probably be analyzed by amperometric titration, and the feed samples by .

- radioassay, because the large impurity content would make the more accurate amperometric method unreliable. Instead all three samples were analyzed g

by radioassay. .

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Arrangements were made with Los' Alamos to analyze the AEC samples by isotopic l dilution, with additional verification by amperometric analysis and/or radioassay.

Results of the AEC analyses were received February 5, 197'4. A comparison

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. of AEC and licensee results is tabulated below:

Sample Wt Solution (g) Cone (g/g) Pli (g)

L AEC L AEC O.00675 0.006719 2905 2892

. 6,7,8,9; Product 430400 296450 0.01926 0.008405 5710 2492 16,18,20; Feed 0.00905 0.008430 2771 2581 It,17,19; Feed 306150 7965 11386 Difference: 3421 grams The licensee stated that the limit of' error for each sample was 0.0034 g/g.

Application of this limit of each of the three solution weights produces limits of 1463g, 1008g, and 1041g. These limits produce a combined limit

. cf 2059g .

on the en, tire material balanceogram ments made. 91thwhich limit of e out regard to any other inv gp Agreement poor. between licensee and AEC differences between AEC and licCollectively 21 grams represented by error that replicate could samples thatbe w established ensee resultshas exceeds rea The licensee agreed to a resolve are the differe,nce. ere taken during the inspection correct,

, . the licensee cculd be considcIf it can n aneven c:

condition 3.2 on the basis of thered to be in violation e that After the physical inventory was poor quality of his measuremen

Condition 3.5. error associated with the MUF wer  !

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, of the material balance necesssry tThe period bet I This that items is thewerenormal sarpled amount me required for inve of ti to o determine the MUF was i

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each item, and establish limits of ntory, calculate plutonium  !

T sidered necessary because error fortheaccomplished each item. Calculati m time and is concidered not yet computer program hasn ,- b reliable.

' Results of the inventory are pre n.

i Storage _ and Internal Transfers (Lisented in detail v The Safeguards group has continuo cense Condition 5 MBA's throughIT's serially numbered theto theusevariofransferinternal forms tus knowledg (IT's).

The group use them for each material transferous MBA custo ferred and initials the of thefor custodi information to complete Type and quantity of material ms. ans Safeguards group to prepare theThemof the areas involved are req around each MBA.

observed inventory It wastonoted accountaterial that balance forthe all i as ablefor licensee w the inv used during the inventory period during the forms to acccunt for. .

- There were over two i

Inventory (License Condition 6 0)_ .

As required by License Condition 6 been closing material balances arou.1, the licensee sinc u y 1, 1973, nd the facility by material balance e

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i at intervals not exceeding thirty days. On the one occasion in which the

- interval exceeded thirty days, a request for an extension was approved by Licensing. Limits of error have been calculated for all components of these material balances, that is, receipts, shipments, and invantories as required, and these limits have been used to calculate the limit of error

of the material unaccounted for (LEMUF). In none of the five material balance periods to date has the licensee's calculated LEMUF been within the 1.5 kilogram limit imposed by License Condition 3.2. The variability of the inventory component of the material balance has been too large to permit attainment of this limit. Since the licensee has an " inventory -

dominated" system, since the inventory is of a much larger magnitude than I the receipt or shipment components of the material balance, there is small

' probability that the 1.5 kilogram limit can be attained. The measurement

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methods for in-process materials do not have the precisions thct would be i required to achieve a 1.5 kg LEMUF.

In addition to receipts, shipments, and measurable materials in inventory, the licensee has a large quantity of unmeasurable plutonium in his system.

This " holdup" is required to be a fixed quantity by License Condition 6.2

and accordingly has been , set at 18.7 kilograms. A fixed limit of error is ij also required to be associated with this holdup. The limit of error that has been established is about five kgs. This quantity by itself is much
- larger than the 1.5 kg limit of License condition 3.2. Combining this LE associated with the unmeasurable materials with the LE of the measurables, the overall LE of material unaccounted for has consistently exceeded six j  ;

kilograms.

In the attachment to this report, the licensee's material balances for all five inventory periods are summarized in tabular form.

License Condition 6.3 sets forth requirements for inventory procedures.

The licensee has such written procedures, approved by the responsible heads

'of the groups involved in the inventory. These are the facility manager, accountability manager, plutonium plant superintendent, and laboratory manager. The procedures meet the requirements of the license conditicas and observations during the inspection disclosed that the inventory and inventory preparations were conducted in accordance with the precedures.

In the ceramic area (MBA 13) all scrap powder had been swept up and removed to the vault. The precipitation equipment had been rinsed. There was no evidence of any unmeasurable solutions in glovebox sumps. In the pellet l

manufacturing area (MBA 21) the equipment appeared clean and all scrap i

powder and contaminated waste had been removed to the vault. In the pellet storage areas (MBA's 22 and 23), all pellets were in storage containers and gloveboxes appeared clean. To aid in the preparat' ion of the MBA's for

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the inventory, a series of checksheets, one for each of the MBA's, are The

- completed by the MBA custodians and approved by the Safeguards group.

checksheets require the custodians to affirm that the plutonium in each area is in a location and form amenable to inventory, that equipment has been cleaned, that logs and other paperwork are up to date, and that trans-fer forms have all been accounted for. Af ter all areas have been prepared in' accordance with the checksheets and have been approved by the Safeguards group, the inventory is conducted. HBA custodians in each area identify each inventory item observed by members of the safeguards group who prepare the inventory lists, one for each area.

L, l Summary of Inspection Status k The tabulation below summarizes the status of the licensee with respect to

' each license condition and regulation at the conclusion of the inspection of December 3-7, 1973.

Inspection (Note 1)

Previous Present 12/73 Future License Coadition 3/73 I

1.0 Organization 0'K Inspect-OK Routine Check 1.1 Routine Check 1.2 Unsatisfactory Inspect-OK OK Inspect-OK Routine Check 1.3 Routine Check

- 1.4 OK Inspect-OK 2.0 Operation -

OK Inspect-OK Routine Check

-2.1 Inspect-OK Routine Check 2.2, OK

~0K Inspect-OK Routine Check 2.3 Routine Check 2.4 OK Inspect-OK OK Inspect-OK Routine Check 2.5 3.0 Measurements and Statistical controls Routine Check Inspect 3.1 OK OK Noncompliance (Note 2) Inspect 3.2 Inspect 3.3 Unsatisfactory Routine Check (Note 3)

Omitted Inspect 3.4 Noncompliance (Note 4)

OK Inspect-OK Routine Check 3.5 Inspect 3.6 NA (Note 5) (Note 6)

NA Inspect 3.7 NA NA NA 3.8 ~ NA

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- Inspection (Note 1) cont. .

Previous Present 3/73 12/73 Future Liecase Condition 4.'O Shipping and Receiving

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OK Omitted Inspect 4.1 NA 4.2 OK NA 5.0 Storage and Internal controls .

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l OK Inspect-OK Omit

  • 5.1 Routine Check 5.2 OK Inspect-OK

', Routine Check 5.3 OK Inspect-OK 6.0 Inventory OK Inspect-OK Routine Check 6.1 6.2 NA Inspect-OK (Note 7) Inspect OK Inspect-OK Routine Check 6.3 Routine Check 6.4 OK Inspect-OK.

? 6.5 . OK Inspect-OK Inspect NA NA NA 6.6 7.0 Records and Reports

' Inspect

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7.1 Noncompliance (Note 8) Routine Check-OK OK Omitted Inspect 7.2 Routine Check 7.3 OK' Inspect-OK

. 8.0 Management of Materials control System Noncompliance (Note 9) Omitted Inspect 8.1 Inspect 8.2 OK Omitted OK Omitted Routine Check 8.3 9.0 Physical Protection Omitted Inspect 9.1 - 9.6 OK (1/73) .

l Part 70 omitted Inspect 70.54 OK

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Note 1. Definitions of terms used in table: "OK" or " Inspect-OK."

Item was inspected and licensee found to be in compliance.

" Routine check." A g'eneral investigation to deterr.ine compliance with no effort to collect detailed information or data.

" Inspect." A complete investigation, consisting of examination of all data and procedures.

" Unsatisfactory." Indicates that licensee was in' compliance,

.but that quality of ef fort was less than desirable. ,

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"NA." Not applicable.

Note 2. Licensee has consistently been unable to meet 1.5 kg LDCF limit, f

Note 3. Standardization and calibration data were in early phase of development in 3/73. A general check 12/73 indicated that

efforts were patisfactory.

Note 4. No measurement review had been made as of 3/73. Measurement 1

review must be made by 3/74 to avoid repeat item of noncompliance.

i Licensee was in process of Vote 5. No NUF or LDWF data as of 3/73.

determining holdup quantity.

f Note 6. Licensee's notifications of corrective actions to reduce LDSF l

considered insufficient duiing period prior to inspection.

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  • Licensee response considered satisfactory in December 1973.

Note 7. LE for holdup varies slightly around 5 kgs Pu.

Note 8. Material balance and plant record's were not being reconciled prior to 3/73.

Note 9. No review of the SNM control system was made prior to 3/73.

Review required prior to 3/74 to avoid repeat noncompliance iten.

Attachment:

Plutonium Plant Inventory Summary j -

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j ATTACHMENT

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i PLUTONIUM PLANT INVENTORY

SUMMARY

i : ' NET FOR

'g 9/11/73 10/10/73 11/9/73 12/5/73 8/10/73 i INVENTORY DATE -

5 PERIODS INVENTORY DATE (GRAMS) 97072 120694 140813" 77449 98804 BEGINNING INVENTORY 77449 .

122740 j ! 7 24478 39918 39114 RECEIPTS 19223 403 18266 I t 187 3864 49 13763 l

  • SHIPMENTS
  • 120694 140813 186171 186171 ENDING INVENTORY 98804 97072 18700 I

18700 '18700

- 18700 18700 18700

!. HOLDUP '

\  : * (2319) (2125) . 806 603'6 (6648) (4238)

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LIMIT OF ERROR DATA (GRAMS) .

1618 714 324 2469 2453 -

BE:; INNING INVENTORY 1618

  • 441 197 272 282 RECEIPTS 43 0 , ,

208 22 11 205 20 -

SHIPMENTS 15 ,

2825 ll l 324 2469 2453 2825

' ENDING INVENTORY 714 ,

249C 3497 3752 3292 ,

e 1769 784 j LEMUF (hXCLUDING HOLDUP)

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6337 6542 6802 6299 6127 l LEMUF (INCLUDING HOLDUP) 3372 4612 6016 6016 LE 4399 5094 j

. (HOLDUP ONLY)

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  • SHIPMENTS INCLUDE MEASURED LOSSES ~

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.T F 9j-DIRECTORATE OF REGULATORY OPE TIONS

. NOTIFICATION OF AN INCIDENT OR OCCURRENCE Facility: Kerr-McGee NucJear Corporation , ,

Cimarron Facility - Plutonium Plant Crescent, Oklahoma -

Problem: SIGNIFICANT MATERIAL UNACCOUNTED FOR (FUF) QUANTITY .

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_, a ~..n On; February;28, 1974, RO Region III was notified 3y Kerr-McGee by telephone that the February monthly plutonium physical investory indicates a MUF loss quantity o 1.5 ilograms Pu with limits of errar of .4 ilograms Pu.

(The limits of error quantity exceeds the technicz1' specification of ,

'1.5 kilograms Pu.) The MUF quantity is significart because (1) it exceeds the ' associated limits of error, and (2) the January 1974 inventory MUF quantity was also a loss 6.5 ilograms Pu). Invastigation by the licensee, has failed to rev.eal exact causes of the significznt MUF quantity.

In a telephone conversation," being confirmed in w2iting, by Region III, the licensee is taking the following actions:

i Fabrication of fuel has been stopped and a ner invent'ory is being l

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conducted,- inventory started on March 1, 19M. .

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, 2. Fabrication of fuel will not be , resumed until the MUF is resolved to the satisfaction of the licensee and RO:III. .

' Action'by Regulatory Operations: . .

1. RO is following the actions being taken by the' licensee. An inspector is at the site. ,
2. No press release has been made; however, the AEC-CH Fublic Information Offic isEwareoftheproblem.
3. Chairman Ray's Special Assistant, Commissioner'Doub's Technical Assistant, Commissioner Larson's Technical Assistant, Commissioner Anders' Temporary Assistant, Commissioner ,Kriegsman's As'sistant, and the Office of

- Information Services have been informed by telephone.

Contact:

Further information concerning this occurrence can be obta,ined from: . .

S. Bryan - Ext 7353

( H. D. Thornburg - Ex't 7353 ,

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. J. G. Davis - 7541 l .-.- --. . ..-

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