Role of analytical chemistry in support of demilitarisation

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1 Role of analytical chemistry in support of demilitarisation James Riches and Chris Timperley 17 th International Chemical Weapons Demilitarisation Conference 4-6 June June 14

2 Content Designated Laboratory Role of analysis Case studies Conclusions 17 June 14

3 UK Designated Laboratory Designated by the Director-General of the OPCW Rigorous quality system and nationally accredited Successful performance in official Proficiency Tests One of 21 OPCW designated laboratories worldwide

4 Role in demilitarisation Investigations of suspected or alleged use of chemicals Analysis to support stockpile destruction and verification Analysis to evaluate chemical destruction technologies Analysis to support assistance and protection activities Occupational health monitoring (environmental/personnel)

5 Case studies Allegations of CW use in Iraq in 19s Moscow Theatre Siege in 2 Development of a biomedical sample analysis capability Effects of fire and decontamination on VX in field study Agent fate/evaporation studies Allegations of CW use in Syria in 13

6 Allegations of CW use in Iraq (19s) Sarin degradation product identified in soil Sarin nerve agent identified in paint from munition fragment R M Black, R J Clarke, R W Read and M T J Reid, J. Chromatogr (1994) 17 June 14

7 Moscow theatre siege (2) Alleged use of incapacitant chemicals Clothing obtained for analysis from surviving British casualties 17 June 14

8 Moscow theatre siege Identification of carfentanil by trace analysis RT: 2.6 MA: m/z = NL: 3.16E4 RT: 2.6 MA: 2986 m/z = NL: 4.31E RT: 2.6 MA: NL: 1.31E RT: 2.6 MA: NL: 1.57E4 Relative Abundance m/z = RT: 2.6 NL: 1.E4 MA: m/z = RT: 2.1 NL: 1.17E4 MA: 738 m/z = Time (min) Sample Relative Abundance m/z = RT: 2.6 MA: m/z = RT: 2.6 MA: m/z = Time (min) Standard NL: 2.28E4 NL: 1.58E4 17 June 14

Moscow theatre siege Carfentanil metabolite confirmed in urine sample RT:. - 25. 9 Blank urine 7 5 3 1 9 8.52 7 5 Victim (<.1 ng/ml) 3 1 8.

9 Moscow theatre siege Carfentanil metabolite confirmed in urine sample RT: Blank urine Victim (<.1 ng/ml) Standard (norcarfentanil in urine at.1 ng/ml) Time (min) J Riches et al. J. Anal. Toxicol (12) 17 June 14

and nerve agents Capability pivotal in confirming exposure to sarin nerve

10 A capability to analyse biomedical samples 25+ publications on the development of methods for chemical exposure monitoring for sulfur mustard and nerve agents Capability pivotal in confirming exposure to sarin nerve agent in Syrian conflict 13 More recently capability extended to riot control agents 17 June 14

11 A capability to analyse biomedical samples Future priorities and directions Emerging threat chemicals : chemical incapacitants (e.g. fentanyls) Toxic industrial chemicals: chlorine, ammonia, hydrogen cyanide Chemical precursors Analysis of hair Use of high resolution mass spectrometry 17 June 14

12 Fire Trial Effects on CW of fire and liquid decontaminants Accelerant based fire could be used to mask the signature from illegal testing of chemical warfare agents (CWAs) Little knowledge on the effect of fire or liquid decontamination on soil contaminated with CWAs No published analytical methods on CWAs and degradation products extracted from burnt/charred/decontaminated soil 17 June 14

13 Fire Trial Effects on VX of fire and liquid decontaminants 17 June 14

14 Fire Trial Outcomes Sample preparation required to remove unburnt fuel residue prior to GC-MS analysis VX and its degradation products were detected in all samples One or two degradation products of VX appear to result from the effects of the fire (potential unique markers of a fire event) Submitted for publication in Analytical Bioanalytical Chemistry 17 June 14

Agent fate/evaporation studies Evaporation Test Facility commissioned and validated 1 m Used to obtain accurate evaporative emissions for sulfur mustard and sarin from building materials Data

15 Agent fate/evaporation studies Evaporation Test Facility commissioned and validated 1 m Used to obtain accurate evaporative emissions for sulfur mustard and sarin from building materials Data exploited to underpin hazard mitigation strategies for buildings Concentration / µg/m Evaporation profiles for sulfur mustard from building materials Plasterboard upvc Glass Concrete Deliberate heating event Elapsed Time / Days 17 June 14

16 Proof of chemical use in Syria

17 Allegations of CW use in Syria (13) Blood based biomarker (sarin from fluoride reactivation) Blank Sample Standard 17 June 14

18 Allegations of CW use in Syria 13 Blood based biomarker of sarin : sarin-tyrosine adduct RT: SM: 5G NL: 5.6E4 m/z= F: + c ESI SRM ms2 32. [ , , , ] MS CR4BLK NL: 4.2E3 m/z= F: + c ESI SRM ms2 32. [ , , , ] MS CR4BLK NL: 2.5E4 m/z= F: + c ESI SRM ms2 Serum from casualty [ , , , ] MS cr NL: 1.8E4 m/z= F: + c ESI SRM ms2 32. [ , , , ] MS cr NL: 5.72E4 m/z= F: + c ESI SRM ms2 Plasma + 5 nm GB-Tyr 32. [ , , , ] MS plsstd NL: 4.73E4 m/z= F: + c ESI SRM ms2 32. [ , , , ] MS plsstd Time (min) Williams NH et al. Arch. Toxicol (7) 17 June 14

19 Allegations of CW use Syria 13 Analysis of environmental samples confirms all UN findings UKAS accredited methods OPCW identification criteria 17 June 14

20 Conclusions Chemical agent evidence cannot escape detection Analysis of biomedical samples is important Use of analytical techniques in combination provides high level of confidence Classical and emerging CW agent use can be proved

21 Perspective The role of chemical analysis will not diminish It will play an essential part in future CW demilitarisation The methods presented here will underpin chemical analysis used in demilitarisation

22 Acknowledgements All members of the CB Analytical and Attribution Capability Robin Black, Jim McGilly, Dean Payne Environmental Sciences Range staff ACP and MoD Chief Scientific Advisor 17 June 14

Weapons of Mass Destruction. Lesson Goal. Lesson Objectives 9/10/2012

Weapons of Mass Destruction. Lesson Goal. Lesson Objectives 9/10/2012 Weapons of Mass Destruction Lesson Goal To become familiarize with the concept of weapons of mass destruction (WMD), how these weapons might be used, and the type of treatment that would be appropriate