Analytical method for determining micro moisture in cyclopropyl amine by gas phase chromatography
An analysis method, a technology of trace moisture, applied in the field of chromatographic analysis, can solve the problems of large difference and difficulty in accurately determining the moisture content of cyclopropylamine, etc., and achieve the effect of offsetting the poor stability of the instrument
Inactive Publication Date: 2007-08-29
INNER MONGOLIA NORMAL UNIVERSITY
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Problems solved by technology
Due to the great difference between the content of cyclopropylamine and moisture in cyclopropylamine products, it is difficult to accurately determine the content of trace moisture in cyclopropylamine by normalization method
Method used
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[0007] 1 Instruments, reagents, samples
[0008] Gas chromatograph, thermal conductivity detector, data processing workstation; GDX-201 (80-100 mesh); distilled water as standard; absolute ethanol (A·R) as internal standard; 5A molecular sieve; cyclopropylamine sample.
[0009] 2 Chromatographic operating conditions
[0010] Chromatographic column: Ф3×2000mm stainless steel packed column, filled with GDX-201 (80-100 mesh); column temperature 100°C; detection temperature 150°C; gasification temperature 200°C; carrier gas: high-purity hydrogen, flow rate 25-30ml min -1 ; Pre-column pressure 0.02Mpa; Bridge current 150mA; Injection volume 2μl.
[0011] 3 Experimental methods
[0012] Absolute ethanol treated by 5A molecular sieve water absorption is internal standard, distilled water is standard substance, and cyclopropylamine treated by 5A molecular sieve water absorption is solvent, and the cyclopropylamine solution containing water and ethanol ratio of 1:4~4:1 is made as De...
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Abstract
The invention discloses a analyze method of measuring micro wet of cycle propyl amine, its chief process is that On a 5A molecular sieve suction treated with cycle propyl amine as the solvent, the 5A molecular sieve suction treated with anhydrous ethanol as internal standard substance, distilled water as the standard, water and ethanol made from different ratio to manufacture cycle propyl amine solution, in accordance with the measurement of the selected chromatogram conditions, it can reckon up the correction factor. When the invention measure sample, in a certain amount of cycle propyl amine, accurate enter a certain amount dehydrated alcohol internal standard substance by the dehydrated treatment, measure according to the selected chromatography conditions, by calculating it can obtain the analysis results of water in cycle propyl amine. The chromatographic analysis condition is: phi3*2000mm stainless steel packed column, inner filled GDX-201(80-100order); the column temperature is 100- 110deg.C; detecting temperature is 140-150deg.C; aerification temperature is 180-200deg.C; carrier gas: high pure hydrogen, flow rate is 25-30ml.min-1; former press of column is 0.02-0.03MPa; bridge current is 140-150mA; enter sample quantity is 1-3mul. The method is simple, applicable, rapid, accurate and can be used for product quality cycle propyl amine Detection.
Description
technical field [0001] The invention belongs to a chromatographic analysis method, in particular to an analysis method for measuring trace moisture in cyclopropylamine products by gas chromatography. Background technique [0002] Cyclopropylamine is an aliphatic amine containing a three-membered ring and is an important fine chemical intermediate. Widely used in medicine, pesticide, organic synthesis and other fields. In medicine, it is mainly used to synthesize new antibiotics ciprofloxacin, ciprofloxacin, sparfloxacin, enrofloxacin, etc.; in the pesticide industry, it is used to synthesize cyprofloxacin, ciprozine, and cyprocyanil Chemical herbicides such as Zine and Propylmethylcyclopropylamine. In addition, the application prospect in organic synthesis is also very broad. Cyclopropylamine products require that the content of cyclopropylamine be above 99.0%, and the moisture content be below 0.1%. Analysis and determination of trace moisture content in cyclopropylamin...
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IPC IPC(8): G01N30/02G01N30/88G01N30/60G01N30/38
Inventor 李景峰
Owner INNER MONGOLIA NORMAL UNIVERSITY