Guide-sample-free GC-FID (Gas Chromatograph-Flame Ionization Detector) accurate quantifying method for organic impurities in an organic ester

A GC-FID and organic impurity technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of large quantitative errors of organic impurities, and achieve the effect of simple method, improved detection sensitivity, and high purity

Inactive Publication Date: 2012-08-15
XIAN MODERN CHEM RES INST
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Problems solved by technology

[0009] Due to the above three reasons, in this case, the area percentag

Method used

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  • Guide-sample-free GC-FID (Gas Chromatograph-Flame Ionization Detector) accurate quantifying method for organic impurities in an organic ester
  • Guide-sample-free GC-FID (Gas Chromatograph-Flame Ionization Detector) accurate quantifying method for organic impurities in an organic ester
  • Guide-sample-free GC-FID (Gas Chromatograph-Flame Ionization Detector) accurate quantifying method for organic impurities in an organic ester

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Embodiment 1

[0044] Embodiment 1: Impurity determination of organic ester analog sample DBP

[0045] In this embodiment, a simulated sample DBP (the impurities are 0.24% DEP and 0.27% DOP) is prepared with known impurity amount, and the impurity is determined by the method of the present invention. It is assumed that there is no corresponding standard sample for the impurity and cannot be valued by external standard method or internal standard method. At the same time, use the area percentage method to determine the value. The detection data of the present invention and the detection data of the area percentage method are compared with the real value.

[0046] 1. Preparation of simulated sample DBP

[0047] Accurately weigh 0.05096g of analytically pure diethyl phthalate (DEP), 0.05564g of dioctyl phthalate (DOP), and 20.72382g of dibutyl phthalate (DBP) and mix them together to prepare DBP The simulated sample, ie the DBP simulated sample contained "impurities" 0.24% DEP and 0.27% DOP....

Embodiment 2

[0068] Embodiment 2: Determination of organic impurities in DBS standard substance candidate

[0069] A certain batch of DBS (dibutyl n-sebacate) samples was purified by vacuum distillation, and the DBS samples with high purity were obtained as standard substance candidates. The impurities in it are detected by GC-MS and combined with the process, they are characterized as butanol, ethyl butyl sebacate, dibutyl azelate, propyl sebacate butyl, stereoisomers of main substances, Butyl amyl sebacate, dibutyl C11 acid, dibutyl C12 acid, a total of 8 impurities. Among them, butanol can be found as a reference substance, which is detected by the conventional GC-FID external standard method. There are no corresponding commercially available reagents or standard samples for the remaining 7 impurities. If these 7 impurities are also valued by external standards, 7 products with a purity ≥ 95% must be specially synthesized, and the cost is too high to be adopted. Because the impurities...

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Abstract

The invention discloses a guide-sample-free GC-FID (Gas Chromatograph-Flame Ionization Detector) accurate quantifying method for organic impurities in an organic ester sample. A solvent is added into the sample to prepare a sample solution; fewer samples are used and prepared into a reference solution; two solutions are respectively injected to the GC for separation; the FID is used for detecting; a relative quality response value is calculated according to a main substrate correction instrument response signal in the reference solution; and the relative quality response value is considered to be equal to the relative quality response value of each impurity, thereby calculating the accurate content of each organic impurity in the sample. Through adoption of the guide-sample-free GC-FID accurate quantifying method, the problem that no corresponding guide sample for the organic impurities exists in the sample is effectively solved. Reliable data is provided for controlling the product quality of the organic ester substrate.

Description

technical field [0001] The invention belongs to the field of analysis and detection of organic impurities, and mainly relates to accurate quantification of organic impurities, in particular to a standard-free accurate quantification method for organic impurities in organic esters. Background technique [0002] During the synthesis and preparation of organic chemical products, due to the many impurities in the raw materials used, the many side reactions in the synthesis process, and the use of organic solvents in the synthesis, there will be many impurities in the prepared crude product, which needs to be purified by rectification, recrystallization and other purification processes in the later stage. Reduce impurities and improve product purity. Through the purification process, the inorganic impurities, solvents, physical and chemical properties in the crude product and the organic impurities that are quite different from the main substance are easy to remove, but the organ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 贾林胡岚张皋严蕊陈曼王婧娜刘红妮张婷温晓燕梁忆陈智群
Owner XIAN MODERN CHEM RES INST
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