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Gas chromatography packed columns for fluorine-containing small molecule compound and preparation method and application thereof
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A gas chromatography and packed column technology, which is applied in the field of chromatographic analysis, can solve problems such as unsatisfactory analysis requirements and chromatographic column failure, and achieve the effects of protection from oxidation, clear separation peaks, and convenient use
Active Publication Date: 2019-08-02
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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However, in the production of fluorine-containing chemicals, there are quite a few intermediates and reaction by-products with strong polarity, strong oxidation, acidity and corrosion, such as F 2 、COF 2 、CF 3 COF, etc., these components are easy to react with the carrier and fixative, F 2 The gas can even quickly carbonize the column packing, making the column invalid, so capillary columns and conventional polar packed columns cannot meet the analysis needs of industrial processes
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Embodiment 1
[0030] This embodiment provides a method for preparing a gas chromatography packed column, specifically:
[0031] (a) Purchase a stainless steel column with a length of 3m and 5m, an outer diameter of 3mm, and an inner diameter of 1.5mm, wash with 5% hot KOH solution and 3% HCl solution, and then rinse continuously with 500ml deionized water , dry the column for later use;
[0032] (b) Take the specific surface area≧250m 2 The microspheresilica gel of / g is processed 24h under 200 ℃ in oven, standby;
[0034] (d) Accurately weigh 0.42g of the fixative perfluoropolyether oil in beaker B, add 11ml of trifluoroethyltetrafluoroethyl ether and stir until ...
Embodiment 2
[0039] This embodiment applies the gas chromatography packed column that embodiment 1 provides, to prove its application effect.
[0050] Take 1ml mixed gas sample, the known components of the mixed gas: CO, F 2 , CF 4 , CF 3 OF, COF 2 , C 2 f 6 o 2 , Determine the chromatographic peak component assignment by the internal standard method, and the evaluation results are shown in Table 1.
[0051] Table 1: Quantitative results of...
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Abstract
The invention relates to gas chromatography packed columns for fluorine-containing small molecules. The packed column comprises a first packed column and a second packed column connected in series, wherein the first packed column is filled with a carrier with the surface coated with polychlorotrifluoroethylene, and the second packed column is filled with a carrier with the surface coated with perfluoropolyether. The packed columns provided by the invention adopt polychlorotrifluoroethylene and perfluoropolyether as fixing liquid coating carriers, which can not only protect the carriers from being oxidized and greatly prolong the use time of the chromatographic columns, but also form different partition coefficients with most fluorine-containing compounds and improve the separation efficiency. The chromatographic packed columns provided by the invention can ensure clearer separation peaks and higher column efficiency. The preparation method of the packed columns provided by the invention is simple, convenient to use and good in reproducibility, and can be generally used for detecting fluorine-containing small molecular compounds.
Description
technical field [0001] The invention belongs to the technical field of chromatographic analysis, and in particular relates to a gas-phase filled chromatographic column for analyzing fluorine-containing small molecule compounds and a preparation method thereof. Background technique [0002] In the production process of fluorine-containing fine chemicals, the monitoring and analysis of raw materials, intermediates and by-products are mostly carried out by chemical analysis and chromatographic analysis. Chemical analysis methods mostly use gravimetric analysis and titration analysis to calculate the substance content by means of color change, precipitation change, weight increase or decrease, enrichment, masking and other means. An important means of detection of constant reactions in industrial production. However, the production process of fluorine-containing fine chemicals is precisely controlled, and trace impurities can affect the yield of the final product, and there are...
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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02B01D15/20
CPCB01D15/206G01N30/02
Inventor 宋亦兰李慧汪仲权王雯霞
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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