Method of determining content of methanol, isobutanol, isoamylol of alcohol

A technology of n-propanol and isobutanol, which is applied in the field of determination of alcohol, can solve the problems of quantitative result deviation, large calibration factor deviation, deviation, etc., and achieve the effect of simple operation

Inactive Publication Date: 2013-06-05
CHINA TOBACCO JIANGXI IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The chemical components in alcohol are diverse and very complex. Methanol, n-propanol, isobutanol, and isoamyl alcohol are harmful components in alcohol. At present, most of their determination methods are gas chromatography, and they all use single-stage The method of calculating the calibration factor of the standard sample and then quantifying it requires that the solvent used does not contain any methanol, n-propanol, isobutanol, and isoamyl alcohol, and the requirements for the solvent are particularly high. For propanol, isobutanol, and isoamyl alcohol, there will be deviations in the calculated amounts of samples and blank samples, resulting in large deviations in the final quantitative results
In addition, since the calibration factor is calculated by a single-level standard sample, it is very easy to cause a large deviation in the calibration factor, resulting in a large deviation in the final quantitative result.
In addition, the detector used in gas chromatography is an FID detector. Compared with mass spectrometry detectors, there is a gap in terms of detection sensitivity and locking target compounds.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] a. Accurately pipette 5ml of alcohol samples produced from sugarcane, corn, potatoes, molasses, etc. as raw materials into a 10ml volumetric flask, then add 2ml of internal standard solution, dilute with absolute ethanol and set the volume to the mark, mix well, and use as Liquid to be tested.

[0016] b. GC-MS analysis is performed on the obtained sample. The analysis results are as follows:

[0017] raw material Methanol n-propanol Isobutanol Isoamyl alcohol Sugarcane 1 35.4 31.1 not detected not detected Sugarcane 2 42.9 46.5 2.0 not detected Sugarcane 3 30.6 282.7 20.8 not detected Yams 1 271.2 180.6 10.3 not detected Yams 2 77.1 109.6 11.7 not detected Yams 3 19.2 24.5 not detected not detected Corn 1 87.6 126.5 8.8 3.6 Corn 2 22.6 5.9 not detected not detected Corn 3 253.9 13.8 not detected not detected Molasses 1 25.3 168.5 3.5 not detected ...

Embodiment 2

[0019] a. Accurately pipette 5ml of alcohol samples used by different industrial enterprises into a 10ml volumetric flask, then add 2ml of internal standard solution, dilute with absolute ethanol and adjust the volume to the mark, mix well, and use it as the test solution.

[0020] b. GC-MS analysis is performed on the obtained sample. The analysis results are as follows:

[0021] use enterprise Methanol n-propanol Isobutanol Isoamyl alcohol Enterprise 1 32.1 59.4 not detected not detected Enterprise 2 22.6 5.9 not detected not detected Enterprise 3 74.3 143.4 not detected not detected Enterprise 4 130.2 75.6 31.2 41.5 Enterprise 5 75.5 194.3 not detected not detected Enterprise 6 272.7 243.3 28.0 not detected Enterprise 7 77.1 109.6 11.7 not detected Enterprise 8 243.3 12.7 not detected not detected Enterprise 9 16514.8 191.2 36.9 46.5 Enterprise 10 36.8 47.6 ...

Embodiment 3

[0023] a. Accurately pipette 5ml of alcohol samples produced by different alcohol manufacturers into a 10ml volumetric flask, then add 2ml of internal standard solution, dilute with absolute ethanol and adjust the volume to the mark, mix well, and use it as the solution to be tested.

[0024] b. GC-MS analysis is performed on the obtained sample. The analysis results are as follows:

[0025] manufacturer Methanol n-propanol Isobutanol Isoamyl alcohol Enterprise 1 8.7 20.5 not detected not detected Enterprise 2 44.6 97.5 10.6 17.4 Enterprise 3 96.0 190.4 20.1 29.7 Enterprise 4 154.3 78.9 5.7 4.1 Enterprise 5 14.9 101.2 not detected not detected

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PUM

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Abstract

The invention discloses a method of determining content of methanol, isobutanol, and isoamylol of alcohol, and relates to methods of determining alcohols. The method of determining the content of the methanol, the isobutanol and the isoamyol of the alcohol comprises steps as below sequentially: (1) alcohol sample pretreatment processing steps: moving sample alcohol into a volumetric flask, adding interior label solution into the volumetric flask, using absolute ethanol to dilute the solution to a constant volume measured by scales, blending the solution to be used as the solution to be tested; (2) blank experiment: adding no samples, and repeating the step (1); (3) carrying out combination analysis of gas chromatography-mass spectra analysis of the samples and the blank sample. The method of determining the content of the methanol, the isobutanol, and the isomylol of the alcohol achieves accurate precise quantification analysis of the content of the methanol, the normal propyl alcohol, the isobutanol and the isoamylol of the alcohol through method improvement and replacing of detectors. The method of determining the content of the methanol, the isobutanol and the isoamylol of the alcohol is simple to operate and fast and accurate.

Description

technical field [0001] The invention relates to a method for measuring alcohol, in particular to a method for measuring the contents of methanol, n-propanol, isobutanol and isoamyl alcohol in alcohol. Background technique [0002] The chemical components in alcohol are various and very complicated. Methanol, n-propanol, isobutanol, and isoamyl alcohol are harmful components in alcohol. At present, most of their determination methods are gas chromatography, and they all use single-stage The method of calculating the calibration factor of the standard sample and then quantifying it requires that the solvent used does not contain any methanol, n-propanol, isobutanol, and isoamyl alcohol, and the requirements for the solvent are particularly high. For propanol, isobutanol, and isoamyl alcohol, there will be deviations in the calculated amounts of samples and blank samples, resulting in large deviations in the final quantitative results. In addition, since the calibration factor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72
Inventor 彭春鸣方茶华余静张翼柳维
Owner CHINA TOBACCO JIANGXI IND CO LTD
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