Sample loop

In the load position the sampling loop is isolated from the mobile phase and is open to the atmosphere. A syringe with a capacity several times that of the sampling loop is used to place the sample in the loop. Any extra sample beyond that needed to fill the sample loop exits through the waste line. After loading the sample, the injector is turned to the inject position. In this position the mobile phase is directed through the sampling loop, and the sample is swept onto the column. 

The basic difference between this type of valve and the normal external loop sample valve is the incorporation of an extra port at the front of the valve. This port allows the injection of a sample by a syringe directly into the front of the sample loop. Position (A) shows the load position. Injection in the front port causes the sample to flow into the sample loop. The tip of the needle passes through the rotor seal and, on... 

Figure 2.20 Schematic representation of the set-up used for on-line exti action-GC VI and V2, valves PI and P2, syringe pumps L, sample loop CC flow, countercunent flow CT, cold ti ap. Reprinted from Journal of High Resolution Chromatography, 16, H. G. J. Mol et ai, Use of open-tubular tapping columns for on-line exti action-capillary gas cluomatography of aqueous samples , pp. 413-418, 1993, with permission from Wiley-VCH.

Figure 14.2 Schematic diagram of the cliromatographic system used for the analysis of low concenti ations of sulfur compounds in ethene and propene VI, injection valve V2, column switcliing valve SL, sample loop R, restriction to replace the column SCD, sulfur chemiluminescence detector.

A five-column configuration of Such an analyser system is depicted in Figure 14.6. The first event in the process is the analysis of Hj by injection of the contents of sample loop 2 (SL2) onto column 5 (a packed molecular sieve column). Hydrogen is separated from the other compounds and detected by TCD 2, where nitrogen is used as a carrier gas. The next event is the injection of the contents of sample loop 1 (SLl), which is in series with SL2, onto column 1. After the separation of compounds up to and including C5, and backflushing the contents of column 1, all compounds above C5 (Q+) are detected by TCDl. The fraction up to and including C5 is directed to column 2, where air, CO, COj, Cj, and 2= (ethene) are separated from... 

Figure 14.6 Schematic diagram of a five-column cliromatographic refinery analyser system SL, sample loop V1, two-way valve to block the sample line V2 and V5, ten-port valves V3 and V4, six-way valves Cl C5, packed columns R, restriction TCD, thermal conductivity detector-.

Figure 14.8 shows a detailed schematic representation of a natural gas analysis System, which fully complies with GPA standardization (8). This set-up utilizes four packed columns in connection with a TCD and one capillary column in connection with an FID. The contents of both sample loops, which are connected in series, are used to perform two separate analyses, one on the capillary column and one on the packed columns. The resulting chromatograms are depicted in Figure 14.9. 

Figure 14.8 Schematic diagram of the natural gas analyser system SL, sample loop VI, two-way valve to block the sample lines V2, ten-port valve V3, V4 and V5, six-port valves R, restriction TCD, themial-conductivity detector FID, flame-ionization detector.

It should be stressed that only those surfaces that actually come in contact with the sample need to be bio-compatible and the major parts of the valve can still be manufactured from stainless steel. The actual structure of the valve varies a little from one manufacturer to another but all are modifications of the basic sample valve shown in figure 13. The valve usually consists of five parts. Firstly there is the control knob or handle that allows the valve selector to be rotated and thus determines the load and sample positions. Secondly, a connecting device that communicates the rotary movement to the rotor. Thirdly the valve body that contains the different ports necessary to provide connections to the mobile phase supply, the column, the sample loop if one is available, the sample injection port and finally a port to waste. Then there is the rotor that actually selects the mode of operation of the valve and contains slots that can connect the alternate ports in the valve body to provide loading and sampling functions. Finally there is a pre-load assembly that furnishes an adequate pressure between the faces of the rotor and the valve body to ensure a leak tight seal. 

Where peak dispersion has not been constrained to very small volumes the external sample loop injector can be used and the external loop sample system, which employs six ports, is depicted in figure 15. In the external loop sample valve, three slots are cut in the rotor so that any adjacent pair of ports can be connected. In the loading position shown on the left, the mobile phase supply is connected by a rotor slot to port (4) and the column to port (5) thus allowing mobile phase to flow directly through the column. In this position the sample loop is connected to ports (3) and (6). Sample flows from a syringe into port (1) through the rotor slot to the sample loop at port (6). At the same... 

The second valve controls a sample loop, 5 cm long and 1 mm in diameter, packed with dimethyloctadecyl reverse phase comprising of fairly coarse particles 100-120 im in diameter to reduce flow impedance. The sample pump is supplied via a two-way tap from either of two reservoirs, one containing pure water and the other, normal saline. The output of the pump can be used to either force the contents of the open loop sample tube through the packed loop, or to permit washing with an appropriate solvent. The separate pump is necessary to overcome the impedance of the packed loop. 

A sample loop, having a capacity of 400 pi, was filled with the serum which was displaced by 2 ml of normal saline onto the packed sample loop. The loop was then washed with a further 2 ml of saline followed by 2 ml of water and the placed in line with the solvent flow and the program initiated. The chromatogram obtained is shown in figure 6. 

We are first concentrating on commercially-available instrument technologies providing in situ measurements in polymer reactors, as opposed to those requiring new instrument development or external sampling loops. 

Successful use of modern liquid chromatography in the clinical laboratory requires an appreciation of the method s analytical characteristics. The quantitative reproducibility with respect to peak height or peak area is quite good. With a sample loop injector relative standard deviations better than 1% are to be expected. The variability of syringe injection (3-4% relative standard deviation) requires the use of an internal standard to reach the 1% level (2,27). 

The apparatus employed for chromatographing particle suspensions in this laboratory has been reported in detail elsewhere (ll). A sample loop of approximately O.U ml was used. The detector was a Pharmacia UV-spectrophotometer with a cell of 1 cm path length and an operating wavelength of either 25, 280 or 350 nm. The volume counter had a capacity of 1 ml. 

The apparatus employed for this study was a Waters Associates Model ALC/GPC 300 with a differential refractometer as mass detector operated at room temperature. A 2 ml sample loop with polymer concentrations of 0.01-0.1 wt.% cUid a 5 ml siphon were employed with mobile phase flowrates in the reuige 1-8 ml/min. 

Figure4.62 Experimental set-up for liquid/liquid experiments (a) reservoir for the substrate in n-heptane (b) water reservoir (c, d) high-pressure liquid pumps (e) HPLC injection valve with sample loop for catalyst injection (f) micro mixer ...

Figure 5.28 Schematic of the experimental set-up. Water/ethylene glycol/SDS reservoir (a) high-pressure liquid pumps (b) catalyst/ substrate HPLC injection valve with 200 pi sample loop (c) hydrogen supply, equipped with mass flow controller (d) micro mixer (e) heating jacket (f) tubular glass or quartz reactor (g) back-pressure regulator (h) [64],...

Cleanup of crude extracts. Inject ca 10 mL of the filtered extract derived from one of the Modules E into the 5-mL sample loop (5.0 mL = Vga). 

The sample is loaded at atmospheric pressure into an external or internal loop, or groove in the valve core and introduced into the mobile phase stream by a short rotation of the valve. The volume of sample injected is normally V2u ied by changing Ute volume of the sample loop or by partially filling a sample loop with a fraction of its nominal volume. External sample loops have volumes from about 5 microliters up to about 1 ml. 

Figure 8.26(A) is an example of a valve type interface [329]. Helium carrier gas is provided to the headspace saiq)ler and is split into two flow paths. One path is flow-controlled and provides a constant flow of carrier gas which passes from the headspace unit through the heated transfer line to the gas chromatograph. The second flow path is pressure-regulated and, in the standby mode, the seunple loop and seuapling needle are flushed continuously by the helium flow. At a time determined by the operator, the sampling needle pierces the septum and helium pressurizes the headspace vial to any desired pressure. The headspace gas is then allowed to vent through the sample loop. Once filled, the sample loop is placed in series with the normal carrier gas flow and its contents are driv Bbhrough the heated...

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