Development Of Purification Process And Standard Specification Of Pesticide Residue Grade N-hexane And LC-MS Grade Acetonitrile

In the field of chemistry and chemical engineering, which needs high puritygrade solvents for chromatographic analysis, spectrum analysis, pesticideresidue detection, mass spectrometry analysis or organic synthesis. PesticideResidue grade solvent for pesticide residue analysis in food safety and LC-MSgrade solvent for LC-MS analysis. Pesticide Residue grade n-Hexane is one ofthe most widely used pesticide residue grade solvents, mainly applied in thepesticide residue analysis in food safety, environment detection, clinicalmedicine and other related fields, which playing a important role in thepesticide residue detection; while LC-MS grade acetonitrile is the mostcommon organic mobile phase for LC-MS, either for qualitative orquantitative purpose. As these two solvents develop too slowly in domestic,this study focused on the development of purification process and standardspecification of Pesticide Residue grade n-Hexane and LC-MS gradeacetonitrile. The main works are as follows: 1. Developing series of the standard specification and the research ofprocess of Pesticide Residue grade n-Hexane, with emphasis on the process:1)the total analysis methods were established, then the impurities of industrialn-Hexane are analyzed and qualitative by UV, GC and GC-MS;2) building thetechnology of Pesticide Residue grade n-Hexane: firstly building acombination process of decoloration, continuous distillation and filtration inlaboratory, on that basis, building a pilot scale process of double distillationwith capacity of30T/a which solved the technical challages from industrialgrade n-hexane to pesticide residue grade n-hexane directly and the productsproduced met the pesticide residue grade quality indexes, the products werechecked by National Research Center for Environmental Analysis andMeasurement (CNEAC), National Research Center for Geoanalysis, ChineseAcademy of Inspection and Quarantine (CAIQ), Chinese Academy ofAgricultural Sciences (CAAS) and were used to be compared with other fivemain brands of Pesticide Residue grade n-Hexane on market, the resultsshowed that they were equivalent to other foreign products and have good andsteady quality.2. Developing series of the standard specification and the research ofprocess of LC-MS grade acetonitrile, with emphasis on its standardspecification:1) the standard specification and detection methods of LC-MSgrade acetonitrile were researched by market investigation and literaturereview, the standard specification were made and six detection methods were set including LC-MS applicability, trace metal ion content, pesticide residuestest, fluorescence analysis, purity and UV value;2) the chromatographyprocess of from industrial acetonitrile to LC-MS grade acetonitrile was studiedpreliminaly, which was the foundation of process combination of distillationand adsorption in the later period, the experimental results showed that theadsorption effect of the chromatography column packing with the acidicalumina with the size of100-200mesh was the best by wet packing, the singleproductivity of chromatographic column was240mL, whose specification wasthat diameter is0.017m and height is0.3m, chromatography column couldrestore activity using three times the pure water to flush chromatographycolumn, regeneration for three times.