Injector, loop

Schematic diagram of a loop injector in the (a) load and (b) inject positions.

One advantage of an HPLC analysis is that a loop injector often eliminates the need for an internal standard. Why is an internal standard used in this analysis What assumption(s) must we make about the internal standard ... 

Kovat s retention index (p. 575) liquid-solid adsorption chromatography (p. 590) longitudinal diffusion (p. 560) loop injector (p. 584) mass spectrum (p. 571) mass transfer (p. 561) micellar electrokinetic capillary chromatography (p. 606) micelle (p. 606) mobile phase (p. 546) normal-phase chromatography (p. 580) on-column injection (p. 568) open tubular column (p. 564) packed column (p. 564) peak capacity (p. 554)... 

Injector The sample, typically 5-200 )J,L, is placed in the carrier stream by injection. Although syringe injections through a rubber septum are used, a more common means of injection is the rotary, or loop, injector used in ITPLC and shown in Figure 12.28 of Chapter 12. This type of injector provides reproducible injection volumes and is easily adaptable to automation, a feature that is particularly important when high sampling rates are desired. 

Loop injector Sample in Chromatographic Detector Recorder... 

For liquid chromatography, a sample of the mixture solution is injected through a loop injector which allows a quantity of the solution to be placed in a small tubular loop at atmospheric pressure. By manipulating a valve, the high-pressure flow of solvent to the column is diverted through the loop, carrying the sample with it (Figure 35.5). 

A typical loop injector showing the sampling position with pressurized solvent flowing through one loop onto the column and the sample solution placed in the other loop at atmospheric pressure. Rotation of the loop carrier through 180° puts the sample into the liquid flow at high pressure with only momentary change in pressure in the system. 

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... 

For better precision of quantitative determinations a loop injector may be incorporated. 

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). 

As mentioned previously, introducing the sample to the flowing mobile phase at the head of the column is a special problem in HPLC due to the high pressure of the system and the fact that the liquid mobile phase may chemically attack a rubber septum. For these reasons, the use of the so-called loop injector is the most common method for sample introduction. 

The loop injector is a two-position valve that directs the flow of the mobile phase along one of two different paths. One path is a sample loop, which when filled with the sample causes the sample to be swept into the column by the flowing mobile phase. The other path bypasses this loop while continuing on to the column, leaving the loop vented to the atmosphere and able to be loaded with the sample free of a pressure differential. Figure 13.7 is a diagram of this injector, showing both the load and inject positions and the path of the mobile phase in both positions. 

FIGURE 13.7 The loop injector for HPLC, (a) the load positon—the sample is loaded into the loop via a syringe at atmospheric pressure, and (b) the inject position—the mobile phase sweeps the contents of the loop onto the column. 

Automated injectors are often used when large numbers of samples are to be run. Most designs involve the use of the loop injector coupled to a robotic needle that draws the samples from vials arranged in a carousel-type auto-sampler. Some designs even allow sample preparation schemes such as extraction and derivatization (chemical reactions) to occur prior to injection. 

Describe in detail how the loop injector works and tell how it overcomes the problems that would be encountered with an injection port-septum system. 

What are some options that are available if an analyst wants to inject a volume that is smaller than the volume of a sample loop installed on an HPLC loop injector ... 

Non-Aqueous SEC Experiments. Non-aqueous SEC separations were carried out at ambient temperatures using two Varian MicroPak TSK GMH6 columns in series (7.5mm i.d. x 30cm each). This column is a mixed bed column containing pore sizes from 250 8 to 107 blended to ensure linearity of the molecular weight calibration curve. The mobile phase employed tetrahydrofuran at a flow rate of 1 ml/mln. Sample injection volumes were 50p)l using a Rheodyne 7126 manual loop Injector. 

Figure 3.5—The two positions of a loop injector, a) Load sample b) Inject sample. Schematic of the model 7125 valve from Rheodyne Inc. Injection valves can be manual, pneumatic or electrical (reproduced with...

Sample-loop injectors, although usually the most expensive, are generally applicable and give the best reproducibility. Their operation involves the introduction of die sample into a loop of a certain volume in a valve system. Hie valve system is then adjusted so that the sample in the loop is flushed on to the column by the mobile phase. The volume of sample loops varies from 1.0 jil to 2 ml. 

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