Valve switching

The regenerative nature of the Wulff operation permits the recovery of most of the sensible heat in the cracked gas. The gases leave the furnace at temperatures below 425°C, thus obviating the need for special high temperature alloys in the switch valve and piping system. 

The small volumes of the feed line from the switching valve to the reactor and the discharge line to the analyzer can be corrected for, since they will have plug flow. This will only displace the zero time on the recorder and it can be easily corrected. 

Piping, manifolds, switching valves and controls to direct and control the flow of gases according to the process requirements. 

A switching valve (low pressure) may be used to divert the eluent from the detector to the fraction collector as soon as the polymer is detected. Another switching valve can be used to select the polymer solution or the solvent for introduction into the pump. 

In this way, the liquid can be transferred at a speed corresponding to the evaporation speed. The fraction to be analysed is contained in a loop (see Eigure 2.5), connected to a switching valve. By opening the valve, the sample in the loop is driven by the carrier gas into the GC unit (8), instead of the LC pump. An early vapour exit is usually placed after a few metres of the deactivated precolumn (9) and a short piece (3-4 m) of the main column (retaining precolumn). This valve is opened during solvent evaporation in order to reduce the amount of solvent that would reach the detector, and at the same time, to increase the solvent evaporation rate (6). 

Figure 2.12 Schematic representation of an on-line SPE-GC system consisting of three switching valves (VI-V3), two pumps (a solvent-delivery unit (SDU) pump and a syringe pump) and a GC system equipped with a solvent-vapour exit (SVE), an MS instrument detector, a retention gap, a retaining precolumn and an analytical column. Reprinted from Journal of Chromatography, AIIS, A. J. H. Eouter et al, Analysis of microcontaminants in aqueous samples hy fully automated on-line solid-phase extraction-gas chromatography-mass selective detection , pp. 67-83, copyright 1996, with permission from Elsevier Science.

Overall, the technical complexity of the Deans switch system is considerably greater than that of a mechanical switching valve and it is accepted that reliability and ease of use is reduced as the system complexity increases. For many compound types, however, the completely non-intrusive nature of the Deans method offers sufficient advantages to justify its application. However, the use of modern electronic pressure and flow controls integrated into the overall computer control of the chromatographic system does now make the operation of Deans switches significantly easier or more reliable than has been reported in its earlier applications. 

S. T. Adam, Quality test of a mechanical switching valve for two-dimensional open tubular gas cliromatography , 7. High Resolut. Chromatogr. Chromatogr. Commun. 11 85-89(1988). 

Sotolon (4,5-dimethyl-3-hydroxy-2(5H)-furanone) and solerone (4-acetyl- y-butirrolactone) were claimed to be responsible for some aroma characteristic of flor sherries wines. These compounds are present only as traces, and are chemically unstable. A system of two gas chromatographs coupled with a four-port switching valve was used to quantitate these components without previous fractionation. The first chromatograph was equipped with an on-column injector, in order to avoid thermal degradation of sotolon in the heated injector, a DB-5 column and an FID. The second chromatograph was equipped with an on-column injector, a DB-1701 column and an FID. The method allowed quantification of solerone and sotolon at concentrations as low as a few ppb (29). 

Figure 11.3 Typical configuration for the on-line coupling of an achiral and chiral cliro-matograpliic system by means of a switching valve. The non-enantio-resolved solute is isolated on the achiral phase and then stereochemically separated on the chiral phase. Reprinted from G. Subramanian, A Practical Approach to Chiral Separation by Liquid Chromatography, 1994, pp. 357-396, with permission from Wiley-VCH.

Zebiihr et al. (29) developed an automated system for determining PAHs, PCBs and PCDD/Fs by using an aminopropyl silica column coupled to a porous graphitic carbon column. This method gives five fractions, i.e. aliphatic and monoaromatic hydrocarbons, polycyclic aromatic hydrocarbons, PCBs with two or more ortho-chlorines, mono-ort/io PCBs, and non-ortho PCBs and PCDD/Fs. This method employed five switching valves and was successfully used with extracts of sediments, biological samples and electrostatic filter precipitates. 

A commonly used system in environmental analysis is the heart-cutting technique which uses the separation power of the first column to obtain a higher selectivity than with the previously described precolumn enrichment. The two columns are coupled via a switching valve, as shown in Figure 13.5. 

Different approaches utilizing multidimensional EC or SEC systems have been reported for the analysis of middle distillates in diesel fuel. A method, based on the EC separation of paraffins and naphthenes by means of a micro-particulate, organic gel column has been described (23, 24). The complete system contained up to four different EC columns, a number of column-switching valves and a dielectric constant detector. However, the EC column for the separation of paraffins and naphthenes, which is an essential part of the system, is no longer commercially available. 

Multidimensional LC has also been used to determine ursodeoxycholic acid and its conjugates in serum (14). These compounds are used in the treatment of cholesterol gallstones, hepatitis and bilary cirrhosis. These authors employed a traditional (10 X 4 mm) pre-column and a micro-bore (35 X 2 mm) analytical column that were interfaced by using a six-port switching valve. 

Recently, multidimensional GC has been employed in enantioselective analysis by placing a chiral stationary phase such as a cyclodextrin in the second column. Typically, switching valves are used to heart-cut the appropriate portion of the separation from a non-chiral column into a chiral column. Heil et al. used a dual column system consisting of a non-chiral pre-column (30 m X 0.25 mm X 0.38 p.m, PS-268) and a chiral (30 m X 0.32 mm X 0.64 p.m, heptakis(2,3-di-(9-methyl-6-(9-tert-butyldimethylsilyl)-(3-cyclodextrin) (TBDM-CD) analytical column to separate derivatized urinary organic acids that are indicative of metabolic diseases such as short bowel syndrome, phenylketonuria, tyrosinaemia, and others. They used a FID following the pre-column and an ion trap mass-selective detector following the... 

Valeo Instruments, six-port switching valve Spherisorb Cl, 100 x 4.6-mm i.d., 5-p.m particle size (Fisher, Cat. No. 05-692-547)... 

Perkin-Elmer Model lSS-100 automatic sampler Kratos ABI Spectroflow Model 783 UV/VIS detector, VlCl EQ60 LC switching valve Supelcosil LC-CN, 33 x 4.6-mm i.d., 5-pm particle size... 

The equipment used in this application included two Waters M-45 pumps, a Waters 481 UV detector with microbore cell, an air-actuated Rheodyne 7413 injection valve with a 1-pl injection loop, an air-actuated Valeo four-port sampling valve (A2CI4UW2) with no groove in the injection entry ports, an air-actuated Valeo three-port switching valve (AC3W), and a Digital Equipment LSI-11/23 microcomputer. The LC system was located in a purged cabinet suitable for use in Class I, division 2 areas. The cabinet was in a heated room about 40 feet from the reactor column. The two Valeo valves were mounted next to the reactor column, while the microcomputer was located in the control room. 

To obtain a sample, the reactor was manually pressurized with nitrogen to 10 to 12 psi, and the four-port switching valve was activated to divert the flow of reactor solvent to recycle. The pressure forced about 4 ml of sample through the 5-pl slot of the tantalum valve. The valve was then switched to transfer the sample to the HPLC located about 15 feet away. The solvent for transfer and dynamic dilution was ethoxyethanol, with a boiling point of... 

B - Switching Valve, Valeo 1/8" Fittings E - Shut-Off Valve, Teflon... 

Fig. 11. Schematic of a research flow-reversal reactor showing switching valves and instrumentation. Heavy insulation was used to tty to obtain adiabatic operation. (Figure adapted from Xiao and Yuan, 1996, with permission of the authors.)...

The collected sample at -196°C was isolated from the flow of the GC s helium gas stream and then the loop was warmed to ambient temperature for GC-mass spectroscopic analyses. The gas cell, which contained the isotopic CO2 and the C2Hg standard in helium at one atmosphere, was placed in the injection helium flow of the GC-mass spectrometer for ten minutes, before the mini-switching valve was turned to inject the vapor contents into the instrument. After three minutes, the CO2 peak eluted. The superimposed peaks were sampled ten times during their elution and the relative isotopic quantities of - C02 C02 and C02 were determined. 

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