Transporting the Samples

The Joint Captured Material Exploitation Center (JCMEC), subordinate to the US Army 513th Military Intelligence Brigade, was responsible for assessing captured equipment and exploiting this knowledge by supplying tactical information useful to battlefield commanders. One of the unit’s missions was to acquire information of Iraqi chemical weapons.[70] On the evening of March 12, 1991, this unit dispatched a team to the 2d MARDIV headquarters to pick up the cement factory samples.[71] A 2d MARDIV NBC Gunnery Sergeant who was the senior NCO in charge of the 2d MARDIV Fox vehicles had custody of the seven soil samples. Each was packaged in individual snap-top canisters similar to 35mm film containers.[72]

The exchange of custody of the samples was made in the 2d MARDIV headquarters by the group leader, the 2d MARDIV NBC officer, the Gunnery Sergeant in charge of the Fox vehicles and several other Marines. They recall a US Army NCO, assigned to JCMEC, signing for the samples.[73] Additionally, several Marines involved in the exchange remembered that photocopied Fox tapes were included with the samples;[74] however, the tapes were not recorded on the Material Courier Receipt.[75] According to the Materiel Courier Receipt, the JCMEC NCO delivered the samples the following day, March 13, 1991, to an NCO of the technical escort unit (TEU[76] ) at the JCMEC facility in Dhahran, Saudi Arabia.[77]

During the war, suspected chemical warfare agent samples were analyzed at a field laboratory in Dhahran or at the Chemical Research Development and Engineering Center (CRDEC[78] ) in Edgewood, Maryland. According to the JCMEC commander, all samples that were thought to be positive for chemical warfare agent would be analyzed by the CRDEC. For this reason the Technical Escort Unit team took them to the CRDEC.[79] During transport, the TEU soldiers tested the outside container of the samples with an M18A1 Chemical Agent Detector kit. The results were negative for chemical warfare agent. The samples arrived at CRDEC on March 17, 1991.[80]

CRDEC Analysis

A team of CRDEC chemists performed a thorough chemical analysis on each of the samples.[81] None of the chemists remember receiving any Fox MM-1 tapes.[82] On March 27, 1991, the scientists at CRDEC sent a classified message reporting the findings to JCMEC. The message notes that testing proved negative for chemical warfare agent, but they also noted that the samples were improperly packaged and were not airtight.[83] An improperly sealed sample could have allowed agents to dissipate. The message clearly points out that improvements must be made in sample transportation.[84] At the time, the CRDEC determined that:

The conclusion can only be one of two things: Either there were no CW agents/by-products present to begin with, or the agents/by-products dissipated in the time between collection in field and lab analysis at CRDEC.[85]

The worksheets used during this analysis remain classified.[86] However, in 1996, at the request of the Persian Gulf Illnesses Investigation Team, the CRDEC chemists used these worksheets to prepare an unclassified Memorandum for the Record. The memorandum stated:

Conclusion: No evidence of any known CW [chemical warfare] agent or agent degradation product was found by any of the analyses performed. The predominant presence of aliphatic hydrocarbons in the extracts could indicate the presence of diesel exhaust or related residues in the areas sampled.[87]

In interviews, CRDEC chemists stated that a persistent agent like lewisite would have left traces of agent or the degradation product, lewisite oxide, even though the sample was improperly packaged. Neither of these compounds was found. The chemists did state that, after a week, non-persistent nerve agents might not be discernible. GB’s degradation product, isopropyl methylphosphonate, could be present, but it was not found in these samples. As the sample was improperly packaged and was not airtight, it is possible that a G-series agent might have vaporized and left no trace or byproduct.[88]

Reporting the Findings

CRDEC reported the negative findings to JCMEC on March 27th.[89] According to the group leader, this information was not passed to the 2d MARDIV.[90] Several days after the samples had been taken (date unknown but probably in the March 16-18 time frame), the Marine group leader called the JCMEC office and inquired about the samples. The group leader is unsure exactly who he talked to but believes it was an Army major. The group leader was told by someone at JCMEC that he did not have a "need to know" about the samples.[91]

The group leader felt he did have a need to know the testing results. Specifically, he wanted to know if the Fox vehicles and crews were correct in suspecting chemical warfare agents at the cement factory. He recalls asking the 2d MARDIV intelligence officer, or one of his assistants, to call the Army major. The group leader recalls that the intelligence officer was told the same thing, "You don’t have a need to know."[92][93] The I MEF NBC officer also recalls that he had a similar exchange with an officer at CENTCOM, in which the I MEF NBC officer was told he did not have a need to know.[94][95]

No records have been found that indicate that the 2d MARDIV sent any unit to inspect this area after the initial trip. The group leader and the rest of 2d MARDIV redeployed from the Persian Gulf to Camp Lejeune, North Carolina, on April 17, 1991.[96]

ANALYSIS

Given the information available to him at the time, the group leader reasonably assessed that this was a possible chemical mine filling station. Tests performed on the samples and analysis on the Fox tapes provides additional insights not available at the time to the group leader. Additionally, in the seven years since the end of Desert Storm, the US and the UN Special Commission (UNSCOM) on Iraq have learned a great deal about the Iraqi chemical weapons program. This knowledge provides additional data for assessing any Iraqi chemical operations at the cement factory.

Fox Tape and Sample Testing Results

Fox 1 Tapes

The Fox 1 tapes were not analyzed by any laboratory until 1998. Figure 7 is a representation of the Fox 1 MM-1 tape generated during the alert at the cement factory. The multiple alerts for "Fat, Oil, Wax" occurring between 15:08 (the local time) and 15:18 shows that there was some type of contamination in the area. It should be noted that contaminants from a variety of sources such as smoke, oil, or exhaust fumes will frequently trigger an MM-1 alert for "Fat, Oil, Wax."[97]

fig7s.gif (10657 bytes)

Figure 7.  Fox 1 Tape

The US Army Soldier and Biological Chemical Command[98] (SBCCOM) analyzed the Fox 1 tapes, including the spectrum that was performed and printed (Figure 8). The tapes show several alerts to cyclosarin (GF) at 15:25 through 15:28. These are just initial alerts and a spectrum must be performed to identify agent presence. According to the SBCCOM assessment, although the Fox identified the substance through the spectrum performed at 15:30 as xylyl bromide,[99] it is probably xylene. Xylene is not a chemical compound that is found in the Fox MM-1 library of 60 chemical substances but it is a component of and has some similar properties to xylyl bromide. The Fox MM-1 algorithm matched the sample with xylyl bromide implying the presence of this substance. The SBCCOM analysis states:

It is highly likely that the chemical present during this encounter was xylene. Xylene is used as a solvent in the production of dyes, insecticides, aviation fuels, polyester, and alkyl resins. It enters the atmosphere primarily from fuel emissions and exhausts linked with its use in gasoline.[100]

fig8s.gif (16399 bytes)

Figure 8.  Fox 1 Spectrum

It is unknown why xylene was present at the cement factory. Cement and concrete subject matter experts have stated that there are no known concrete or cement manufacturing processes that require this chemical.[101] Xylene is neither a CWA precursor chemical nor is it known to have been employed as a CWA by any nation.[102]

The National Institute of Standards and Technology (NIST) also analyzed the Fox 1 tape. The NIST analysis of the spectrum performed at 15:30 states:

The single mass spectrum reported on the tapes shows no evidence supporting the presence of chemical weapons or related compounds. Instead, the spectrum may be explained as arising from a mixture of conventional hydrocarbons. … These are very common compounds.[103]

In an interview the NIST chemist stated that the spectrum was consistent with a mix of xylene and trimethyl-benzenes. It is almost certainly not a chemical warfare agent or degradation byproducts of a chemical warfare agent.[104]

Fox 1 had several additional initial responses for phosgene between 15:47 and 15:49[105] (Figure 9). The tape shows that two spectra showing "Fat, Oil, Wax" were performed at 15:48 and 15:49. However, the operator did not print either of the spectra. According to the US Army SBCCOM analysis, "the spectrum denied the CWA responses by confirming the sample as Fat/Oil/Wax." [106] The NIST analysis states:

confirmation is not possible. However, two major phosgene peaks (m/z=63,65) are also present in many hydrocarbons and were present in the reported spectrum[the 15:30 spectrum], so a false alert for phosgene would not be surprising.[107]

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Figure 9.  Fox 1 Phosgene Alert

Analysis of Chemical Warfare Agents

Although prewar US intelligence reports place lewisite and phosgene as possibly in Iraq’s inventory,[108] UNSCOM has not found any lewisite or phosgene during any of their inspections.[109] Additionally, after Desert Storm, Fox vehicles were found to have a problem with the sampling wheel that could lead to a false alert for lewisite. Several years after the war, this problem was corrected by the introduction of a new sampling wheel.[110] Some Marines’ recollections and the Materiel Courier Receipt note a possible lewisite alert at the cement factory. There is no way of determining if the Fox design flaw could have been the cause of these lewisite alerts at the cement factory.

Without the Fox 2 tape, the G-series alert is also difficult to judge. UNSCOM destroyed large quantities of Iraqi GA, GB and GF nerve agents after the war.[111] The Fox 1 tapes show an initial alert for a G-series agent that a full spectrum failed to confirm and the Material Courier Receipt also notes G-series agents.[112] It is possible that a chemical compound that resembles a G-series agent in the Fox’s first look caused an alert, but that a full spectrum, the only way to have high confidence in agent presence, showed no agent present. G-series are volatile nerve agents that vaporize quickly.[113] The resultant vapor hazard is the primary casualty-causing mechanism, much like an aerosol insecticide.[114] However, no casualties occurred during the inspection and no Marines reported any symptoms.[115] The two laboratories, NIST and SBCCOM, presented analyses indicating that the initial responses of the MM-1 were probably false positives. The NIST analysis states:

The reporting of "false positives" is, in general, not surprising … an examination of the mass spectrum in the present tapes suggests that the corresponding alert was "false".[116]

The seven soil samples gave indications of diesel exhaust contamination. This is consistent with the SBCCOM analysis of the MM-1 tape that identified the compound as xylene. The samples provided no indications of G-series agent or lewisite, although lewisite is a persistent agent.[117]

Post-War Investigations

Iraq declared to UNSCOM that the Al Muthanna State Establishment, north of Baghdad, was the sole chemical weapons research, development, production, and filling facility, as well as a bulk agent storage site.[118] Although this does not exclude the possibility that filling of munitions could have taken place away from Al Muthanna, UNSCOM has no evidence that a chemical weapons filling area would be found in Kuwait.[119] Iraq declared no chemical mines in their inventory, and UNSCOM destruction records show no chemical mines being destroyed.[120][121] According to the US subject matter expert on foreign mines, of the 3.5 million mines that were cleared from Kuwait, none were assessed as being chemical-filled.[122] UNSCOM and the US intelligence agencies currently believe that Iraqi chemical munitions were not moved into Kuwait."[123][124] We have no information on what became of the area known as the cement factory, but we do know that between 1992 and 1994, contractors cleared all munitions from Kuwait. None of the contractors reported finding any chemical munitions or agents anywhere in Kuwait.[125]

ASSESSMENT

In the years since the end of the Gulf War, the UN and US have learned much about the Iraqi chemical weapons program. UNSCOM found evidence of only one Iraqi chemical munitions filling plant, Al Muthanna, which was located in Iraq. UNSCOM and Kuwaiti contractors found no evidence that Iraq had chemical warfare mines in their inventory. Neither UNSCOM nor US intelligence believes the Iraqis ever moved chemical munitions into Kuwait. Events at the cement factory do not contradict these findings. The Marines found no filled chemical warfare agent mines or other munitions during the March 12, 1991, inspection of the cement factory. For these reasons, an assessment of whether the cement factory was a chemical mine filling site is "Definitely Not."

It is more difficult to be definitive concerning the presence of chemical warfare agent at the cement factory. Evidence presented by the Fox 1 tape, the soil analysis, the lack of other evidence such as casualties caused by chemical warfare agent, and the lack of evidence of Iraq ever moving chemical munitions into Kuwait makes a very strong case that there was no chemical warfare agent at the cement factory. However, both the Fox vehicles alerted to some form of contamination: Fox 1 for xylene; unknown contamination for Fox 2. The soil analyses show no chemical warfare agent or by-products, but it is possible that improper packaging allowed a G-series nerve agent to dissipate prior to its arrival at the laboratory in Edgewood, Maryland. These issues preclude a "Definitely Not" assessment that CWA was present. For this reason, the assessment of chemical warfare agent presence at the cement factory is "Unlikely" and the exposure of US armed forces in the cement factory to chemical warfare agents must also be assessed as "Unlikely."

This case is still being investigated. As additional information becomes available, it will be incorporated. If you have records, photographs, recollections, or find errors in the details reported, please contact the DOD Persian Gulf Task Force Hot Line at

1-800-472-6719.


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