Chromatography sample collection

Average of five composite samples analyzed by electron capture gas chromatography. Samples collected from drip zone of tree. 

Although comprehensive two-dimensional gas chromatography has not been applied to any great extent in forensic analysis, the technique shows great promise when samples or sample matrices are complex. For example, when oil is spilled into waterways, assigning responsibility for the economic and environmental damage is often difficult. Gaines et al. employed comprehensive two-dimensional GC in the forensic analysis of samples collected at oil-spill sites and were able to obtain results which were comparable to those obtained by classical methods (39). This article also... 

Discontinuous chemical-detection systems do not provide a signal that is continuous in time, but rather cycle rapidly through a series of phases such as sample collection, preconcentration, separation, and detection in such a way that the overall system is capable of providing a detection report every minute or so. Examples of such systems include ion mobility spectrometers, mass spectrometers, and chromatography-based systems. Many technologies are possible candidates for each of the different phases.2... 

Analysis of this product by gas liquid chromatography (QF-1 coated column, 130°) showed it to be >98.5% pure. The boiling point of a sample collected by chromatography was 169-171°. 

Organotin compounds enriched from a diethylether extract of a snow sample collected from the city of Gdansk, Poland and analyzed are shown in Fig. 22 b, c [286]. Gas chromatography with atomic emission detection (GC-AED) run in the chlorine and tin channels, respectively, revealed the presence of tributyltin chloride and this was subsequently confirmed by GC-MS and GC-AED analyses of an internal standard solution (e.g., 1-chlorooctane) of that compound. Quantification was based on the response to chlorine (wavelength 479 nm) in the AED system, and a detection limit of 0.5-1 ng/1 was achieved for all the reference substances. 

Zero-headspace procedures involve the collection of a soil sample with immediate transfer to a container into which the sample fits exactly. The only space for gases is that within the soil pores. The volume of sample collected depends on the concentration of volatiles in the soil. It is imperative that the container employed can be interfaced directly with the gas chromatograph. Several commercial versions of zero-headspace sampling devices are available. The sample is transported to the laboratory at 4°C, where it is analyzed directly by purge-and-trap gas chromatography (EPA 5035) or other appropriate techniques, such as vacuum distillation (EPA 5032) or headspace (EPA 5021). 

Errors in trace analyses are usually hidden to all except those intimately involved in the sample collection and, later, in the bench analysis. In chromatography, especially, it is too easy to hide behind uncertain work because published research does not concern itself with exactly how the chromatographer makes his quantitative decisions. Today, with the advent of the microprocessor and with the use of black box instruments, the chromatographer knows even less about his calibration graph or line, or the error associated with it. In these instruments, a single point and the origin may determine the calibration graph. Similar problems exist in other modern instrumental analysis techniques. 

The various fractions of the forerun were analyzed employing a gas chromatography column packed with silicone gum, No. XE-60, suspended on Chromosorb P and heated to 248°. The components found (with the retention times indicated) were benzyl bromide (9.0 minutes), 2-methylcyclohexanone (5.3 minutes), and, in some cases, bibenzyl (22.6 minutes). The bibenzyl, formed by reaction of the benzyl bromide with the excess methyllithium, was identified from the infrared spectrum of a sample collected from the gas chromatograph. 

Decabrom, Tetrabrom, and Firemaster 680. All of these compounds are amenable to analysis by selected ion monitor glc/ms/comp. However, substantially lower detection limits for TRIS were attained using glc/ecd. Thin-layer chromatography was used for the analysis of Decabrom in some air samples collected during a preliminary study. 

Filters. HN03 is efficiently trapped out on nylon filters. Typically, two or more filters are connected in series. A schematic of such a filter pack was shown in Fig. 11.22 (Anlauf et al., 1988). A Teflon filter first removes particles from the airstream and a nylon filter then removes gaseous HNO,. In this particular system, a third filter (Whatman 41 impregnated with an aqueous solution of glycerol and citric acid) was used to trap NH3. After sample collection, each of the filters is extracted separately and nitrate, ammonium, and additional particle components collected on the Teflon filter are measured by ion chromatography. The sensitivity of this method for nitric acid and the other species is determined in part by filter blank values (i.e., nitrate on unexposed filters) and by the total amount collected and hence the sampling time used. Times of... 

In order to preclude this problem and the necessary frequent regeneration of the anion system s suppressor column, an ion chromatography exclusion scheme was utilized. Samples collected in a mine environment were reliably concentrated by freeze-drying and then analyzed on an ICE system with dilute hydrochloric acid eluent. The precision of the ICE method was experimentally determined to be 2.5% in a concentration range of 1 to 10 yg/mL. The accuracy was not independently determined but good precision and recovery yield confidence that measured values are within 5% of the true value. No interferences were observed in the ICE system due to strong acids, carbonic acid or other water soluble species present in mine air subject to diesel emissions. 

The chemical properties of HVA, 5HIAA and 3-MD make them amenable to reverse-phase high-performance liquid chromatography (HPLC) with electrochemical detection. Furthermore, the composition of CSF means that little, if any, sample preparation is required prior to analysis. However, the susceptibility of these metabolites to oxidation means that careful sample collection and storage is required in order to minimise analyte degradation. 

---