ITWG CMX-4 Exercise - LLNL s Experience RMCC XI Workshop

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ITWG CMX-4 Exercise - LLNL s Experience RMCC XI Workshop Michael Kristo Group Leader, Chemical & Isotopic Signatures Group December 12, 2016 This

Lawrence Livermore National Security, LLC To deter illicit nuclear trafficking, nuclear forensics laboratories have been cooperating on common

was chartered by the G-8 in 1996 The ITWG s objective is to provide cooperative and effective technical solutions to governments who request

1 ITWG CMX-4 Exercise - LLNL s Experience RMCC XI Workshop Michael Kristo Group Leader, Chemical & Isotopic Signatures Group December 12, 2016 This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under contract DE-AC52-07NA Lawrence Livermore National Security, LLC To deter illicit nuclear trafficking, nuclear forensics laboratories have been cooperating on common technical strategies and databases The initial organizational meeting for the ITWG (ITWG-0) was held at LLNL in 1995 The Nuclear Smuggling ITWG was chartered by the G-8 in 1996 The ITWG s objective is to provide cooperative and effective technical solutions to governments who request assistance 22 Meetings, 30+ countries The ITWG works closely with the IAEA to provide requesting states with assistance as well as with logistical support 2 2 1

Exercises and round robins have been a key ITWG activity from its

Robin 2; HEU oxide powder 2010: Round Robin 3; HEU metal 2014:

Devised as learning experiences not performance tests 3 3 a)

confidential informant, a passenger scheduled to fly out of Country

2 Exercises and round robins have been a key ITWG activity from its beginning 1999: Round Robin 1; plutonium oxide powder 2003: Round Robin 2; HEU oxide powder 2010: Round Robin 3; HEU metal 2014: CMX-4; LEU oxide powder & pellets Poster from 2 nd ITWG Round Robin Devised as learning experiences not performance tests 3 3 a) Country A International Airport Sample ES1 On a tip from a confidential informant, a passenger scheduled to fly out of Country A International Airport to Frankfurt, Germany is targeted for questioning/interdiction. 4 2

Suspect apprehended Leads investigators to residence The

alleged simple possession of a radioactive substance

ES2 In a separate search of the subject s residence in

dense radioactive object, suspected to be a nuclear fuel

3 Suspect apprehended Leads investigators to residence The suspect passenger is stopped by airport authorities for alleged simple possession of a radioactive substance without proper documentation LLNL-PRES Sample ES2 In a separate search of the subject s residence in Country A, authorities located and took into evidence a dense radioactive object, suspected to be a nuclear fuel pellet, such as one that would be used for nuclear power generation 6 3

4 Are these pellets similar to what was found in country A? Sample ES3 Uranium pellets have previously been seized by authorities 5 years prior at an abandoned warehouse in Frankfurt, Germany 7 Sample Opening at LLNL - Establish chain-of-custody - Photo documentation - Initial physical measurements (mass, dimensions) 8 4

5 Sample number Form A Interdiction location ES1 Powder Country A International Airport ES2 Fuel pellet Suspect s Residence, Country A B ES3 Fuel pellet Frankfurt, Germany Metal canister with exercise samples ES-1 powder sample ES-2 pellet sample C 9 Questions to be answered... ANALYTICAL PLAN DEVELOPMENT 1. Do the seized materials contain uranium? Yes No 2. What is the mass & enrichment level? Outside scope of exercise 3. Do they originate from the same facility/process/batch? 10 5

Physical Dimensions Figure 1. Diameter A. Figure 2. Diameter B (rotated 90 degrees azimuthal relative to A).

358 ± Diameter A, Bottom (in) 0.360 ± 0.359 ± Figure 3.

359 ± ES-1 ES-2 ES-3 ITEM Powder Pellet Pellet MASS 2.9867 2.3813 2.3794 UNCERTA INTY (k=2) ± 0.0001 ± 0.

142 ± - Physical dimensions of ES-2 and ES-3 were found to be the same within uncertainty.

6 Physical Dimensions Figure 1. Diameter A. Figure 2. Diameter B (rotated 90 degrees azimuthal relative to A). Sample ID Diameter A, Top (in) ES ± ES ± Diameter B, Top (in) ± ± Diameter A, Bottom (in) ± ± Figure 3. Diameter measurements were made at top and bottom of each pellet. Diameter B, Bottom (in) ± ± ES-1 ES-2 ES-3 ITEM Powder Pellet Pellet MASS UNCERTA INTY (k=2) ± ± ± UNITS grams grams grams Length (in) ± ± - Physical dimensions of ES-2 and ES-3 were found to be the same within uncertainty. - Both pellets seemed slightly tapered. Available within 24 hours 11 Optical Microscopy ES-2 Fuel Pellet TOP BASE SIDE This pellet seemed more distressed than the other- more chips, cracks, oxidation, etc. Both pellets had this vertical line on the side. Possible artifact from the pellet mold? Available within 24 hours 12 6

Optical Microscopy ES-3 Fuel Pellet TOP BASE SIDE Available within 24 hours 13 U

were determined to be (0.88±0.04) g/g (2σ) for the pellets and (0.85± 0.

) There was no evidence of 237 Np, 241 Am, Pu, or residual fission products in the

7 Optical Microscopy ES-3 Fuel Pellet TOP BASE SIDE Available within 24 hours 13 U Assay by Gamma spectrometry Preliminary values for the mass of U per mass of sample were determined to be (0.88±0.04) g/g (2σ) for the pellets and (0.85± 0.06) g/g (2σ) for the powder. (UO 2 is 0.88 g/g.) There was no evidence of 237 Np, 241 Am, Pu, or residual fission products in the preliminary spectra. Longer counting would be conducted later to place better limits on undetected species. Available within 24 hours 14 7

8 U Isotopics using Gamma Spectrometry What s the samples enrichment? U/ 238 U (atom ratio) Pellet Frankfurt Pellet Country A Powder Country A U/ 238 U (atom ratio) Available within 24 hours Do the seized materials contain U? 16 8

Can we determine the enrichment more precisely? Sample ID 234 U/ 238 U +/- 2σ 235 U/ 238 U +/- 2σ 236 U/ 238 U +/- 2σ ES1 0.0002527 0.0000009 0.02981 0.00003 0.00001862 0.00000017 ES2 0.0002526 0.

9 Can we determine the enrichment more precisely? Sample ID 234 U/ 238 U +/- 2σ 235 U/ 238 U +/- 2σ 236 U/ 238 U +/- 2σ ES ES ES U/ 238 U (atom ratio) ES1 ES2 ES3 ES1 and ES2 overlapping U/ 238 U (atom ratio) 236 U/ 238 U (atom ratio) ES1 ES2 ES3 ES1 and ES2 overlapping U/ 238 U (atom ratio) Available within a few days. LLNL-PRES What is the enrichment level? 18 9

10 Intensity (cps) Model date 12/18/2016 Radiochronometry Radiochronometry Are they from the same batch? 17-Feb U-Th U- model 230 Th model date date 235 U-Pa 231 model Pa model date date 1-Aug Jan Jun Dec May-02 5-Nov Apr-01 ES1 1 ES2 2 ES3 3 Sample ID Number Available within 1-2 weeks. 19 ES1 Black powder intercepted in Texas Phases identified α-u 3 O 8 46% Uraninite (UO 2 ) 54 % ES2 Pellet intercepted in Texas Phases identified Uraninite (UO 2 ) 100 % ES3 Pellet intercepted in Frankfurt Phases identified Uraninite (UO 2 ) 100 % Example spectrum from ES θ angle 20 10

11 Fe (ppm) Re (ppm) Mo (ppm) Ni (ppm) 12/18/ ES1 ES2 ES ES1 ES2 ES W (ppm) Mn (ppm) ES1 ES2 ES ES1 ES2 ES Cr (ppm) Ba (ppm) Do they originate from the same facility/process/batch? not 22 11

In summary Country A Pellet ES2 Samples from Batch B (2.

2% U 235 ) Similar process as Batch B Frankfurt Pellet

Consisted of two separate batches of high-fired, low

(A) was enriched 12 February 2002 (2.2% 235U).

9% 235U - produced sometime between 2002 and 2007.

12 In summary Country A Pellet ES2 Samples from Batch B (2.9% U 235 ) Sample from Batch A (2.2% U 235 ) Similar process as Batch B Frankfurt Pellet ES3 Country A Powder ES1 23 Materials origin The Reveal Consisted of two separate batches of high-fired, low enriched uranium oxide (LEU UO 2 ) pellets: One Batch (A) was enriched 12 February 2002 (2.2% 235U). Another Batch (B) was enriched to 2.9% 235U - produced sometime between 2002 and Pellets were originally produced as targets in the production of medical radioisotopes. ES1 (powder) came from Batch B - crushed and partially oxidized in a tube furnace. ES2 (pellet) came from Batch B. ES3 (pellet) came from Batch A

13 Materials preparation: powder sample (ES2) The Reveal Enrichment: 2.9% Mass: ~ 2.4g Pellet was first ground in a bench top mill, then 25 Powder preparation, continued The Reveal heated in a tube furnace to oxidize

14 14

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