Purge and trap instrumentation

Headspace analysis (EPA 3810, 5021) also works well for analyzing volatile petroleum constituents in soil. In the test method, the soil is placed in a headspace vial and heated to drive out the volatiles from the sample into the headspace of the sample container. Salts can be added for more efficient release of the volatile compounds into the headspace. Similar to water headspace analysis, the soil headspace technique is useful when heavy oils and high analyte concentrations are present, which can severely contaminate purge-and-trap instrumentation. Detection limits are generally higher for headspace analysis than for purge-and-trap analysis. 

Because the instrumentation requires the monitoring of several steps, valving, heating zones, and so on, purge-and-trap instrumentation is more complex, and may be more expensive to purchase, than other types of sample introduction. 

Some purge-and-trap instruments have trap injection ports that permit the injection of the internal standard solution onto the trap directly while the sample is being purged, which ensures that the whole injection is trapped but does not compensate for any loss due to purging efficiency, vessel leaking, and so on. With attention to sampling parameters and the selection of a compatible internal standard, purge-and-trap analyses can easily provide quantitative results with relative standard deviations for replicates below 5%. 

OIC Analytical Instrument supply the 4460A purge and trap concentrator. This is a microprocessor-based instrument with capillary column capability. It is supplied with an autosampler capable of handling 76 sample vials. Two automatic rinses of sample lines and vessel purge are carried out between sample analyses to minimize carry-over. 

All fuel methods analyze GRO with a purge and trap sample introduction technique, whereas semi volatile diesel fuel and heavy, non-volatile motor oil (DRO and RRO) are first extracted from soil or water samples, and the extracts are injected into the analytical instrument. This distinction in sample preparation gave rise to the terms of total purgeable petroleum hydrocarbons (TPPH) or total volatile petroleum hydrocarbons (TVPH) and total extractable petroleum hydrocarbons (TEPH). A group of petroleum fuels with the carbon range of C7 to Cig may be analyzed with either technique. Common petroleum fuels and other petroleum products fall into these three categories as shown in Table 2.3. 

Obviously, some procedures take less time than others. For example, sample concentration by the purge and trap technique that precedes VOC analyses takes only about 20 minutes. It is performed immediately prior to analysis on a multisample automated concentrator combined with an analytical instrument. The shortest of all sample preparation procedures is the waste dilution procedure, commonly known as dilute and shoot, which takes minutes. It consists of diluting a known volume of a concentrated waste sample in a known volume of a compatible solvent, followed by an injection into a gas chromatograph. 

There are many techniques available for the preparation of volatile analytes prior to instrumental analysis. In this chapter the major techniques, leading primarily to gas chromatographic analysis, have been explored. It is seen that the classical techniques purge and trap, static headspace extraction, and liquid-liquid extraction still have important roles in chemical analysis of all sample types. New techniques, such as SPME and membrane extraction, offer promise as the needs for automation, field sampling, and solvent reduction increase. For whatever problems may confront the analyst, there is an appropriate technique available the main analytical difficulty may lie in choosing the most appropriate one. 

Calibration is carried out using standard calibration curves. The simplicity, repeatability, and low cost of the method have allowed its use for routine determination of trihalomethanes in tap water. SOME has also been compared with solid phase microextraction (SPME), purge and trap (P T), and direct aqueous injection (DAI) [10]. This technique offers accuracy comparable with that obtained using P T and DAI. With respect to conventional LEE, the SDME method is more accurate. In contrast to DAI and P T, it requires no special equipment. SDME has been used for extraction of chlorophenols [II], pesticides [12, 13], warfare agents [14], and butanone derivatives [15], and for control of food products [16]. The low costs of the SDME method (typical GC syringe and 2-3 pL of solvent), simplicity, and short extraction time (approximately 15 min) make it particularly suitable for preliminary analyses of organic pollutants in water samples. It can also be an effective alternative to SPME, as it does not require the use of expensive instrumentation. 

Another configuration of MAP gas-phase extraction relates to dynamic headspace sampling, often referred to as purge and trap sampling. The container can be fitted with an aperture enclosing a trap, or a sorbent, cooled by some common means. This allows the application of a prolonged, low-power irradiation, or of a multi-pulse irradiation of the sample, thus providing a means to extract all of the volatile analytes from the matrix. The contents of the trap can then be transferred (by elution for a chemical or sorbent trap, or by thermal desorption for a cold trap) to an analytical instrument, such as a... 

Chloroethyl vinyl ether in potable and nonpotable waters and solid and hazardous wastes may be analyzed by EPA Methods based on GC and GC/MS instrumentation (U.S. EPA 1992 1997 Methods 611, 625, 8010, 8270) using a purge and trap or thermal desorption technique. Characteristic masses to identify this compound by GC/MS using electron-impact ionization are 106, 63, and 65. 

Figure 3.3a shows a schematic of a purge-and-trap system for the collection of volatiles contained in an aqueous sample. Clean air is bubbled through the water sample to purge the water of the volatiles and then carry the volatiles into the IMS. If the concentrations of the analytes are too low for direct detection, a trap (preconcentrator) device is inserted between the purged water sample and the IMS. Figure 3.3b is a schematic of an exponential dilution system used to calibrate IMS instruments for... 

Figure 2 shows a schematic diagram of a typical purge-and-trap system. It consists of two major components a purging device and a sorbent trap. The two parts are connected with each other and to the analytical instrument through transfer lines, with a six-port switching valve controlling the flow path. 

See also Activation Analysis Neutron Activation. Atomic Absorption Spectrometry Principles and Instrumentation. Atomic Emission Spectrometry Principles and Instrumentation. Chromatography Overview Principles. Gas Chromatography Pyrolysis Mass Spectrometry. Headspace Analysis Static Purge and Trap. Infrared Spectroscopy Near-Infrared Industrial Applications. Liquid Chromatography Normal Phase Reversed Phase Size-Exclusion. Microscopy Techniques Scanning Electron Microscopy. Polymers Natural Rubber Synthetic. Process Analysis Chromatography. Sample Dissolution for Elemental Analysis Dry... 

Gas chromatography (GC) instruments may be equipped with various detectors to accomplish different analytical tasks. Flame ionization and thermal conductivity detectors are the most widely used detectors for routine analyses, nitrogen-phosphorus detectors are used for the trace analysis of nitrogen-containing compounds, and electron-capture detectors are used for halogen-containing compounds. GCs may also be equipped with peripheral accessories such as autosamplers, purge and trap systems, headspace samplers, or pyrolyzer probes for special needs in sample introduction. 

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