Liquid samples, automatic analysis

Figure 12.6 illustrates the outline of such an analysis. An automatic pipette extracts a preset volume of the liquid sample (or solution) from a cup presented to it on a turntable. The measured sample is mixed with the reagents in the appropriate proportions, and propelled through the instrument by the peristaltic proportioning pump. This pump operates by means of moving bars, attached to a chain drive, which sequentially compress the plastic sample and reagent tubes to drive the liquids forward through the instrument. The incorporation of a succession of air bubbles at... 

The whole atomizer may be water cooled to improve precision and increase the speed of analysis. The tube is positioned in place of the burner in an atomic absorption spectrometer, so that the light passes through it. Liquid samples (5-100 mm ) are placed in the furnace, via the injection hole in the centre, often using an autosampler but occasionally using a micro-pipette with a disposable, dart-like tip. Solid samples may also be introduced in some designs, this may be achieved using special graphite boats. The sample introduction step is usually the main source of imprecision and may also be a source of contamination. The precision is improved if an autosampler is used. These samplers have been of two types automatic injectors and a type in which the sample was nebulized into the furnace prior to atomization. This latter type was far less common. 

The ability to inject 100 or more microliters of a liquid sample rapidly and automatically into a capillary gas chromatograph necessitates another look at liquid-liquid extraction. Sensitivity of the analysis is a common problem... 

Figure 12.7 illustrates the outline of such an analysis. An automatic pipette extracts a preset volume of the liquid sample (or solution) from a cup presented to it on a turntable. The measured sample is mixed with the reagents in the... 

Synchroton radiation has been employed as a spectral source for a study of the absorption of HCN and DCN in the wavelength range 80—120nm. A vacuum-u.v. spectrophotometer for absorptions in the region 105—200 nm has been described. Solid-, liquid-, and gas-phase samples could be analysed at temperatures from —200 to 100 °C and at pressures between 0 and 150 atmospheres. The absorption spectrum of tra j-di-imide in the vacuum-u.v. has been measured. First-derivative u.v. spectroscopy has been employed in the analysis of Watts nickel plating solutions for trace amounts of saccharin. Impurity levels of 0.1 p.p.m. have been recorded. A wavelength modulated derivative spectrophotometer with a multi-pass absorption cell has been developed for the automatic analysis of atmospheric pollutants. Traces of SOj, NO, and NO2 were detected with limits of 15, 13, and Sp.p.b., respectively. A double-beam single-detector absorption spectrometer has been constructed. Independence... 

From the physical point of view, the most important considerations are temperature, pressure, and sample cleanness. Suspended solids in liquid samples and dust in gas samples often interfere with transducers in continuous-sampling instruments and with the volumetric sampling techniques used in batch-sampling instruments. Automated systems that filter out solids should be amenable to automatic cleaning. In continuous instnunents, data output must be interrupted while the filters are cleaned in batch-sampling systems, filters can be cleaned during the deadtime after a sample has been injected for analysis. 

P T-GC). This technique is now frequently used to detect residues of volatile organic compounds in the environment and in the analysis of liquid and solid foodstuffs. In particular, the coupling with GC-MS systems allows its use as a multi-component process for the automatic analysis of a large series of samples. 

Analytical Methods. Liquid scintillation counting (LSC) was done using Packard Models 3375 and 3380 Liquid Scintillation Spectrometers equipped with automatic external standards. Solid samples were combusted in a Packard model 306 Sample Oxidizer prior to LSC analysis. 

Two variations on the analysis of PCR products by ESI mass spectrometry have emerged (1) direct-injection MS and tandem mass spectrometry (MS-MS) and (2) liquid chromatography-mass spectrometry (LC-MS) and tandem mass spectrometry (LC-MS/MS). In the former approach, the sample is cleaned manually, and as noted above, the cleanup is performed as simply and rapidly as possible. In the latter approach, the cleanup is done automatically... 

The analysis takes place in a circular disc called the transfer disc or rotor (Figure 6.1) made of an inert material such as Teflon or acrylic whose surface properties allow minimal adhesion of liquid. It contains radially arranged sets of cavities, each set composed of two or more interconnected cavities, one for the sample and the others for the reagents (Figure 6.2). Small measured volumes of sample and reagent, e.g. 5 - 200/rl, are automatically pipetted into the appropriate wells so that each set contains a different sample but the same... 

In our development studies, Endeavor (5 mL) and Buchi (IL) reactor systems were used to screen catalysts and to evaluate the impurity profile under various process conditions. Elydrogenation kinetic studies were carried out using a 100 mL EZ-seal autoclave with an automatic data acquisition system to monitor the hydrogen uptake and to collect samples for HPLC analysis. Standard conditions of 5 g of aldehyde in 25 mL ethyl acetate and 25 mL methanol with 0.5 g of 5%Pd/C Engelhard Escat 142 were used in this investigation. For the Schiff s base formation and subsequent hydrogenation, inline FTTR was used to follow the kinetics of the Schiff s base formation under different conditions. Tables 1 and 2 show the changes in the substrate concentration under different conditions. Both experiments were carried without any limitations of gas-liquid mass transfer. 

Automatic headspace samplers are available from manufacturers of gas chromatographs. These devices are based on the technique of sampling an amount of vapor above the sample itself. Samples are sealed, neat or in a suitable solvent, in containers, and hold at a preset temperature in a thermostatted liquid bath. The headspace vapor results as a partition equilibrium is established between the liquid or solid and the gaseous phase of the volatiles. As each sample is presented to the analyzer, the vessel is punctured and a portion of the headspace gas is withdrawn by a pneumatic injection technique and forced into the column. The main application for those samplers is in the routine analysis of low-boiling fractions in samples containing nonvolatile solids or high-boiling components. Some of the more popular applications today are ... 

The aliquots of the solution-state chemical synthesis samples were directly injected into a standard HPLC-NMR probe by using a robotic liquid handler. The NMR software was used to automatically find and suppress the intense NMR signals from any non-deuterated solvents used, typically using the WET sequence [5]. Unlike the characterisation of impurities in organic compounds (see the next section) or drug metabolites (see the appropriate chapter in this volume) where the proportions of the analytes can be very different, combinatorial chemistry samples tend to be all of similar quantity and this simplifies the analysis in that it is not usually necessary to worry overly about carry-over of material from sample to sample, nor it is necessary to readjust the NMR spectrometer receiver gain after every sample, thus saving considerable machine time. 

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