Column chromatography safety

The hypothesis that anions of BP A might be removed by column chromatography with Octolig was considered but not pursued because of the warnings in a MSDS (Material Safety Data Sheet) about hazards of BPA and because the pKa values of BPA were listed as 9.59 and 11.3. 

A 2-L four-necked round flask, a mechanical stirrer, a condenser, an addition funnel, a septum, a separatory funnel, a column for flash chromatography, safety glasses, and a laboratory coat. 

Column selection high performance liquid chromatography Electrical safety in the laboratory Flammable and explosive Instrumentation of HPLC (slide show and discussion)... 

Immunoaffinity columns are extremely versatile and have been used for the isolation and concentration of a diverse number of analytes from a wide array of matrices (2). Analytes may include macromolecules such as proteins and receptors or small molecules such as environmental toxins, antibiotics, or pesticides. Matrices may include animal tissues or excreta, plant extracts, cell culture medium, or virtually any milieu encountered in biological work. Because of its value as a research tool, immunoaffinity chromatography has found extensive use by the pharmaceutical industry to purify therapeutic proteins, the food safety community to purify small amounts of toxins from food and as a general tool for analytical chemists to purify analytes for subsequent instrumental analysis. 

The reaction solvent was diethyl ether (no other solvent produced a viable result). Therefore, safety considerations demanded that before the standard oxidative work-up the solvent had to be changed due to the possible presence of ether peroxides. After an aqueous quench, solvent evaporation and re-dissolution in methylene chloride, examination of the fate of 64a revealed that some 20% less was present in the mixture. Carrying out the oxidative work-up resulted in a further 20% loss. The product was not stable (in the reaction mixture) to the work-up conditions. To overcome this problem, we simply omitted these steps and after quenching the reaction mixture with water, it was diluted with the chromatography solvent and chromatographed directly on reverse phase silica gel. This led to a 60% yield of the desired alcohol 64a, epimer free The epimer 64b was isolated by further elution and recycled as described below. The summarized column conditions are outlined in Table 7. 

The PAN was isolated from the numerous side products by gas chromatography on preparatorysized columns and collected by cryogenic trapping. The PAN was then placed in large air canisters, diluted with zero air, and stored in a cold room for future use. Safety precautions are required with this method, because explosive accidents have been reported. The cause of the explosions is believed to be condensation of PANs in vacuum or pressure gauge systems. Like all nitrates, the peroxy nitrate PAN has explosive potential, and care must be taken when handling PAN on metal surfaces. The Stephens synthetic approach illustrated by Reaction 19.7 to Reaction 19.11 was quite successful, and a number of publications on the toxicity of PAN and its chemical and physical properties resulted from the use of the scheme. ... 

Safety devices such as air sensors and pressure transducers are built into preparative HPLC units, together with a series of valves. These devices create dead volume and contribute to the extra column volume. A large-scale chromatography unit is composed of valves for selection of buffers and feed solutions, at least two pumps, the separation column, and, in most cases, at least one detector. Instead of a fraction collector, a combination of valves is often used. These sources of dead volume create typical washout kinetics, which contribute exponentially to the band-broadening processes. For the industrial scale, the equipment is mainly customer designed. For medium scale, modular units are available [51]. Attention should be paid to extra column volume when systems are compared. Extra column effects are an important parameter of the quality of a system and should be considered when a system is purchased. 

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