High-performance liquid chromatography phase experiment

B. Waiczak, L. Morin-Allory, M. Chrdtien, M. Lafosse and M. Dreux, Factor analysis and experiment design in high-performance liquid chromatography. III. Influence of mobile phase modifications on the selectivity of chalcones on a diol stationary phase. Chemom. Intell. Lab. Syst., I (1986) 79-90. 

Walczak, B., Chretien, J.R., Dreux, M., Morin-Allory, L., and Lafosse, M. (1987), Factor Analysis and Experiment Design in High-performance Liquid Chromatography. IV. Influence of Mobile Phase Modifications of the Selectivity of Chalcones on an ODS Stationary Phase, Chemom. Intel. Lab. Sys., 1, 177-189. 

Another widely used method for qualitative and quantitative analysis of amino acid mixtures is high-performance liquid chromatography (HPLC) (see Experiments 2 and 6). The mixture of amino acids is first subjected to reaction with phenylisothiocyanate (PITC) to convert them to the phenylthiocarbamyl-amino acid derivatives, which are then subjected to chromatographic separation. The derivativatization of the amino acids serves two purposes it attaches a UV-absorbing tag, which makes their quantitative determination easy, and it converts them to a more hydrophobic form, which is necessary for good separation on the reverse-phase system commonly used with this technique. This method of amino acid analysis will be used in Experiment 6. 

Abstract A protocol has been developed illustrating the link between validation experiments and measurement uncertainty evaluation. The application of the protocol is illustrated with reference to a method for the determination of three markers (Cl solvent red 24, quinizarin and Cl solvent yellow 124) in fuel oil samples. The method requires the extraction of the markers from the sample matrix by solid phase extraction followed by quantification by high performance liquid chromatography (HPLC)... 

The steady-state partial oxidation reaction experiments were carried out in a quartz fixed-bed, flow reactor with 10 mm I.D. and a length of 50 mm. The analytical system consisted of two parts. Gas Chromatography (GC) and High Performance Liquid Chromatography (HPLC). GC was used to analyze on-line the reaction products that were in the gas phase. The GC (HP-5890) was equipped with a Chromosorb PAW 23% SP-1700 column (30 ft. 1/8") for FID, a Hayesep D column (15 ft. 1/8") and a Molecular Sieve 5A column (10 ft. 1/8") connected serially to TCD. Reverse-phase HPLC with a Spherisorb 5 ODS-2 (1 ft. 1/4") column was used off-line to analyze the products that were solid or liquid at room temperature. The details of the experimental procedures have been described elsewhere [12,13]. 

The experiments within the frame of the REHE project were performed in the aqueous phase in a discontinuous, batch-wise manner. It was necessary, in order to get a statistically significant result, to repeat the same experiment several hundred or even several thousand times with a cycle time of typically 45 s. These studies were performed with the Automatic Rapid Chemistry Apparatus (ARCA) II (SchSdel et al, 1989), a computer-controlled apparatus for fast, repetitive high-performance liquid chromatography (HPLC) separations. A schematic of the ARCA II components is shown in Figure 6.2. 

Deng, 1. F., C. C. Yang, W. 1. Tsai, J. Ger, and M. L. Wu. 2001. Acute ethylene chlorohydrin poisoning experience of a poison control center. 7. Toxicol, Clin. Toxicol, 79(6) 587-93. Dunn, D. L., W. 1. lones, andE. D. Dorsey. 1983. Analysis of chlorobutanol in ophthalmic ointments and aqueous solutions by reverse-phase high-performance liquid chromatography. 7. Pharm. Scl 72(3) 277-80. 

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