Development and evaluation of a standard method for the quantitative determination of elements in float glass samples by LA-ICP-MS

Forensic analysis of glass samples was performed in different laboratories within the NITE-CRIME (Natural Isotopes and Trace Elements in Criminalistics and Environmental Forensics) European Network, using a variety of Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) systems. The main objective of the interlaboratory tests was to cross-validate the different combinations of laser ablation systems with different ICP-MS instruments. A first study using widely available samples, such as the NIST SRM 610 and NIST SRM 612 reference glasses, led to deviations in the determined concentrations for trace elements amongst the laboratories up to 60%. Extensive discussion among the laboratories and the production of new glass reference standards (FGS 1 and FGS 2) established an improved analytical protocol, which was tested on a well-characterized float glass sample (FG 10-1 from the BKA Wiesbaden collection). Subsequently, interlaboratory tests produced improved results for nearly all elements with a deviation of < 10%, demonstrating that LA-ICP-MS can deliver absolute quantitative measurements on major, minor and trace elements in float glass samples for forensic and other purposes.     

Carbon monoxide-related deaths in a metropolitan county in the USA: an 11-year study

Carbon monoxide (CO) poisoning as a cause of death is well documented in industrialized countries. The objective of this study was to compare demographic data in deaths due to accidents (in fires) and suicides in the same population between 1988 and 1998. Furthermore, the potential effect of a community wide education effort regarding safety in the home was assessed. Postmortem reports were reviewed for all deaths examined at the Office of the Cuyahoga County Coroner in Cleveland, OH, USA. During the study period, there were 209 accidental deaths due to fires in the home (6.5% of all accidents in the home) and 182 CO deaths by suicide (9.8% of all suicides). Demographic characteristics of the two groups differed: while males represented the majority of cases in both groups (55% of accidents, 70% suicides), race specific death rates were higher for whites than blacks (18/100,000 white, 3/100,000 black) in suicides compared with 29/100,000 deaths for blacks and 11/100,000 for whites in accidental cases. Fire deaths were prevalent in the young (0-9 years) and old (>60) whereas in the suicide group the age specific death rate was highest for those over 70 years. The majority of fire deaths occurred in the city of Cleveland but suicides were prevalent in the suburbs. More fire deaths occurred in December than any other month whereas more suicides occurred in April. In 1992, there was a community wide effort to provide free smoke detectors to residents in Cleveland. In 1992, there were 4.2/100,000 fire deaths in the city. This decreased to 0.6/100,000 in 1996, increased to 1.2/100,000 in 1997 followed by a decrease to 0.8/100,000 in 1998. This suggested that the program may have aided in decreasing these types of deaths. Deaths due to fires in the suburbs were <1/100,000 throughout the study period.     

Trace analysis of peroxide explosives by high performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry (HPLC-APCI-MS/MS) for forensic applications

An HPLC-APCI-MS(/MS) method for the (trace) analysis of the most commonly encountered peroxide explosives, hexamethylenetriperoxidediamine (HMTD) and triacetonetriperoxide (TATP), has been developed. With this method, HMTD and TATP have been analyzed in the same run. (Pseudo-)molecular ions of these peroxides have been obtained as base peak under the same condition. A series of product ions was produced from these pseudo-molecular ions ([HMTD - 1]+ and [TATP + NH4]+) in the MS/MS analysis. We also pioneered in showing that a TATP molecular ion [TATP + H]+ can be observed with HPLC-MS/MS. The limit of detection for HMTD and TATP was 0.26 and 3.3 ng, respectively, on column by HPLC-MS in the Full Scan mode and 0.08 and 0.8, respectively, by HPLC-APCI-MS/MS in Selected Reaction Monitoring (single mass unit) mode. The method presented has been applied successfully for the identification of peroxides in the bulk solid state (powder sample), as well as in post-blast extracts originating from a forensic case. For the post-blast extracts, the use of tandem MS has been shown clearly to be of crucial importance for the identification and detection of the peroxide explosives.