Sulphur detector

Adlard and Matthews [16] applied the flame photometric sulphur detector to pollution identification. A sample of the oil pollutant was submitted to gas chromatography on a stainless steel column lm><3mm packed with 3% of OV-1 on AW-DMCS Chromosorb G (85-100 mesh). Helium was used as carrier gas (35rnLmin ) and the column temperature was programmed from 60 to 295°C and 5°C per minute. The column effluent was split between a flame ionisation and a flame photometric detector. Adlard and Matthews [16] claim that the origin of oil pollutants can be deduced from the two chromatograms. The method can also be used to measure the degree of weathering of oil samples. 

Further, mention should be made of solid-cell coulometric detectors for halogens and halogen compounds121 and for sulphur compounds122, where for example in the latter instance a solid cell of Pt Ag Agl Ag2S Pt interacts with passing gaseous sulphur compounds. 

For less well defined incidents however, these detection systems may be inadequate. Portable chemical detectors may not be able to be deployed to the site, not detect the agen, or give inconclusive results. Clinical findings may be non-specific, present in an atypical manner, or for example in the case of sulphur mustard, have a latency period that delays firm pattern recognition. Due to the physico-chemical properties of the agent or the time between release and collection, environmental samples may have low agent levels or sufficiently high contaminants to prevent adequate results. 

This is a selective detector for phosphorus and sulphur-containing compounds which makes use of the... 

Tan [71] devised a rapid simple sample preparation technique for analysing polyaromatic hydrocarbons in sediments. Polyaromatic hydrocarbons are removed from the sediment by ultrasonic extraction and isolated by solvent partition and silica gel column chromatography. The sulphur removal step is combined into the ultrasonic extraction procedure. Identification of polyaromatic hydrocarbon is carried by gas chromatography alone and in conjunction with mass spectrometry. Quantitative determination is achieved by addition of known amounts of standard compounds using flame ionization and multiple ion detectors. 

The analysis of organosulphur compounds has been greatly facilitated by the flame photometric detector [2], Volatile compounds can be separated by a glass capillary chromatographic column and the effluent split to a flame ionization detector and a flame photometric detector. The flame photometric detector response is proportional to [S2] [3-6]. The selectivity and enhanced sensitivity of the flame photometric detector for sulphur permits quantitation of organosulphur compounds at relatively low concentrations in complex organic mixtures. The flame ionization detector trace allows the organosulphur compounds to be referenced to the more abundant aliphatic and/or polynuclear aromatic hydrocarbons. 

Reliable flame photometric detector quantification of organosulphur compounds requires careful optimization of the gas chromatograph parameters. Although the relative response of the flame photometric detector to various sulphur compounds remains somewhat controversial [7], analysis of organosulphur compounds by flame photometric detector is now relatively straightforward. 

In a method described by Bates and Carpenter [8] for the characterization of organosulphur compounds in the lipophilic extracts of marine sediments these workers showed that the main interference is elemental sulphur (S8). Techniques for its elimination are discussed. Saponification of the initial extract is shown to create organosulphur compounds. Activated copper removes S8 from an extract and appears neither to create nor to alter organosulphur compounds. However, mercaptans and most disulphides are removed by the copper column. The extraction efficiency of several other classes of sulphur compounds is 80-90%. Extracts are analyzed with a glass capillary gas chromatograph equipped with a flame photometric detector. Detection limit is lg S and precision 10%. 

The sample is extracted with a mixture of hexane, acetone and water. After separation, the hexane phase is reduced in volume and divided into two aliquots, one of which is first shaken with 7% fuming sulphuric acid to remove lipids, and then with cyanide to eliminate interference by elemental sulphur. The other aliquot is evaporated to dryness and heated with ethanolic potassium hydroxide. The two aliquots are injected into a gas chromatograph fitted with a glass capillary column and an electron capture detector. Hexabromobenzene is used as an internal standard. Polychlorinated biphenyls are determined quantitatively by comparing the peaks of the sample with those of Clophen A... 

The Oxamyl in this extract is then determined by gas chromatography using on-column reaction with trimethylphenyl ammonium hydroxide, the derivative so formed being determined by a flame photometric detector operated in the sulphur mode. Both Oxamyl and Oxamyl oxime in the soil react with trimethylphenyl ammonium hydroxide to form the same methoxime derivative (CH3)2NCOC(SCH3) -NOCH3. 

The main analytical technique for pesticides is gas chromatography using a variety of detectors such as electron capture for halogenated compounds, thermionic for compounds containing either phosphorus or nitrogen, and flame photometric for compounds containing sulphur or phosphorus. 

The flame photometry detector is specific for compounds containing sulphur or phosphorous. Compounds eluting from the column are burned in a flame hot enough to excite these elements and induce photonic emission, which is detected by a photomultiplier (see Fig. 2.12). Optical filters are used in the detection system to... 

In most cases, the separation of alcohols, usually methanol, ethanol, and glycerol, is carried out contemporaneously with the separation of sugars and organic acids, and almost always the desire is to quantify all these analytes. It is seen, therefore, that the mobile phase is often an aqueous acid solution, even though only water may be used (5,9). Sulphuric acid is the one most frequently used, although phosphoric acid is preferred by some, since it is less corrosive on the components of the HPLC system (10). The concentration of sulphuric acid normally varies between 0.004 N and 0.01 N or more. The choice of acid may, however, be dictated by other considerations. This is the case, for example, with the use of a conductivity detector, which requires an appropriate conductivity suppressor system. If such a device is not available for a particular... 

---