Method for measuring content of aminocaproic acid in caprolactam with high-performance liquid chromatography
A high-performance liquid chromatography and caprolactam technology, which is applied in the analysis field of aminocaproic acid content in amide oil, can solve problems such as complicated methods, and achieve the effects of good reproducibility, simple sample processing and analysis process, and high accuracy
Active Publication Date: 2015-12-23
HUBEI SANNING CHEM
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Problems solved by technology
[0005] At present, the determination of aminocaproic acid is concentrated in biomedicine, and its application in the caprolactam industry has not been reported; and the current determination methods of aminocaproic acid are mostly pre-column or post-column derivatization, and then the determination is relatively complicated.
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Embodiment 1
[0029] A method adopting high performance liquid chromatography to measure aminocaproic acid content in caprolactam, the specific steps are:
[0030] Analytical method for determination of aminocaproic acid content by liquid chromatography
[0031] 1. Mobile phase selection and detection wavelength selection:
[0032] 1) The experimental results of mobile phase selection show that: the buffer salt content increases, the mixed standard sample has a fast peak eluting time, but cannot be separated; the acetonitrile content increases, the mixed standard sample has a slow peak eluting time, but the peak shape is poor, taking into account the separation effect and analysis Time, using the following elution conditions: mixed solution: 10mmol / L buffer salt=98:2 (V / V); wherein the mixed solution adopts a volume concentration of 95% acetonitrile solution and 10mmol / L buffer salt in a volume ratio of 85: 15; 10mmol / L buffer salt is prepared by mixing potassium dihydrogen phosphate solut...
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The invention discloses a method for measuring the content of aminocaproic acid in caprolactam with high-performance liquid chromatography. The method is an analysis method for quantitatively analyzing the content of aminocaproic acid with an external standard method with the adoption of a mobile phase acetonitrile-buffer salt mixed solution system commonly used in reversion phase chromatography. Chromatographic conditions of the method are as follows: a chromatographic column is CAPCELL CORE PC S2.7 (2.1mml.d*150 mm); a mobile phase is prepared from a mixed solution and 10 mmol / L buffer salt through isocratic elution, and a volume ratio of the mixed solution to the 10 mmol / L buffer salt is 98:2; the flow velocity is 0.4 mL / min; the detection wavelength is 200 nm; the column temperature is 40 DEG C; the injection volume is 20 mu L. The method fills the technological blank of the aminocaproic acid measuring method in the field of caprolactam and has the advantages of simple sample processing and analyzing process, high accuracy of an analysis result, good reproducibility and the like.
Description
technical field [0001] The invention belongs to the technical field of analysis, and relates to a method for determining the content of aminocaproic acid, in particular to a method for analyzing the content of aminocaproic acid in amide oil by using high performance liquid chromatography in the production process of caprolactam. Background technique [0002] Aminocaproic acid (C 6 h 13 NO 2 ), in the production process of caprolactam, it is mainly obtained by hydrolysis and ring opening of caprolactam in the presence of water in acidic or alkaline medium. [0003] In the neutralization reactor, there are two streams of materials, namely the rearrangement liquid (containing concentrated sulfuric acid) and gaseous ammonia. If the two are mixed unevenly, it will inevitably cause local overacid or overalkaline, and a certain amount of Water makes the conditions for the hydrolysis of caprolactam mature, and a certain amount of by-product aminocaproic acid is produced. [0004...
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Inventor 李万清周学军陈志霞刘冬梅李芹芹张小兰张艳丽裴小英李焕张美丽
Owner HUBEI SANNING CHEM