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Method for detecting relative mass correction factor of impurity derivative chromatogram response of sample with not high purity

A technology of correction factor and relative mass, which is used in measuring devices, instruments, scientific instruments, etc. to ensure the accuracy

Inactive Publication Date: 2019-09-20
NANTONG BAICHUAN NEW MATERIAL CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The purpose of the present invention is to overcome the chromatographic purity of the currently used indirect method to measure the product, especially when measuring the chromatographic purity of organic chemical products with low purity, in the preparation steps of adding nominal amount and diluting, the derivation of certain known impurities is calculated. To provide a well-considered calculation and determination method to more accurately determine the relative mass correction factor of the chromatographic response of the corresponding impurity derivatives

Method used

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  • Method for detecting relative mass correction factor of impurity derivative chromatogram response of sample with not high purity
  • Method for detecting relative mass correction factor of impurity derivative chromatogram response of sample with not high purity
  • Method for detecting relative mass correction factor of impurity derivative chromatogram response of sample with not high purity

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Embodiment 1

[0055] Step 1. The boiling point of ditrimethylolpropane under normal pressure is 435.6°C, which cannot be directly measured by gas chromatography. Accurately weigh 2.4956g of ditrimethylolpropane which has been refined and whose mass fraction of the main component is higher than 95%. Put propane in a 50mL flat-bottomed glass tube with a ground mouth, transfer 25mL (calculated excess) acetic anhydride selected as a derivatization reagent, put the glass tube into a matching electric heating aluminum bath reactor, and select 142°C for derivatization Chemical reaction, the upper part of the reactor is equipped with an air condenser tube, so that the volatile matter can be condensed and recovered. After the reaction is complete for 1 hour, the glass tube is taken out. Cool to room temperature, and open the ground plug on the top of the condenser tube every five minutes to ensure that the liquid droplets condensed on the wall of the condenser tube can flow back to the reactor under ...

Embodiment 2

[0104] Step 1, the known industrialized production of trimethylolpropane contains impurities with higher boiling points under normal pressure such as ditrimethylolpropane (Di-TMP), TMF, etc., so it is necessary to accurately measure trimethylolpropane with a gas chromatograph propane, also need to use indirect method, use acetic anhydride to esterify trimethylolpropane and its impurities into substances with lower boiling point, and accurately weigh 1.9795g of refined and the mass fraction of the main component is higher than 99%. In a 50mL flat-bottomed glass tube with ground mouth, transfer trimethylolpropane to 25mL (calculated excess) acetic anhydride as a derivatization reagent, put the glass tube into a matching electric heating aluminum bath reactor, select The derivatization reaction is carried out at 142°C. The upper part of the reactor is equipped with an air condenser, so that the volatiles can be condensed and recovered. After 1 hour of complete reaction, the glass ...

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Abstract

The invention relates to a method for detecting a relative mass correction factor of impurity derivative chromatogram response of a sample with not high purity. When derivative reaction is carried out, the total weight loss before and after derivatization of a substance is controlled within 0.1% by measures including condensation recovery; the relative error of each step is controlled within 0.1% in the labeled weighing and dilution step; namely, when a theoretical mass score is calculated, contribution of an added impurity sample derivative to the theoretical mass score of the impurity derivative as well as contribution of existing impurity derivative in the sample derivative to the theoretical mass score of the impurity derivative is taken into consideration, the area normalized appearance mass score, measured by a chromatogram, of the impurity derivative serves as the abscissa, a fit straight line is drawn, and the gradient of the fit straight line serves as the relative mass correction factor of chromatogram response of the derivative with known impurity, and thus, the relative mass correction factor of chromatogram response of the corresponding impurity derivative can be determined more accurately.

Description

technical field [0001] The invention belongs to the technical field of analysis of organic chemical products, and relates to a method for determining the chromatographic response relative mass correction factor of impurity derivatives in organic matter with low purity after derivatization and transformation. Background technique [0002] The purity of organic chemical products, especially the purity expressed by mass fraction, is a particularly important item in the standards of organic chemical products, and it is also an item that users are particularly concerned about. Using chromatographic technology to separate and measure the mass fraction of organic chemical products is a method that analysts are increasingly fond of because of its intuitiveness and reliability. [0003] The purity of industrially produced products is difficult to reach 100%, and there must be impurities, some of which directly affect the downstream application of organic chemical products. [0004] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/86
CPCG01N30/8675
Inventor 薛建军张海兵俞晔虎马俊华吕坚陈明雷周国君高芳姜伟伟
Owner NANTONG BAICHUAN NEW MATERIAL CO LTD
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