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Method for determining sulfide in spirit

A sulfide and liquor technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of time-consuming and labor-intensive sensitivity, poor selectivity, and limited sensitivity, so as to improve the quality of liquor, avoid decomposition, and improve accuracy. sexual effect

Inactive Publication Date: 2007-08-15
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although traditional solvent extraction and traditional static headspace extraction are widely used, they are time-consuming and laborious and have poor sensitivity. In addition, some sulfides are extremely volatile and chemically active, so traditional methods cannot be used to enrich liquor Sulfide in
At present, flame photometric detectors, chemiluminescence detectors and atomic emission detectors are mostly used for the detection of sulfides, but the selectivity and sensitivity of these detectors are still limited.

Method used

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  • Method for determining sulfide in spirit
  • Method for determining sulfide in spirit
  • Method for determining sulfide in spirit

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Dilute 53% (v / v) Moutai liquor with deionized water to 14% alcohol (v / v), draw 5mL liquor sample into a 20mL headspace bottle, add 100μL internal standard solution, and saturate with sodium chloride , screw on the cap. Stir and balance in a water bath at 30°C at a speed of 500rpm for 30min, insert a 85μm Carboxen-PDMS fiber head, and extract at 30°C and 250rpm for 15min. Then insert the extraction head into the gas phase inlet, and desorb at 300 °C for 7 min in splitless mode. Using DB-FFAP, the column temperature was maintained at 35°C for 3 minutes, raised to 150°C at a rate of 10°C / min, maintained for 5 minutes, then raised to 220°C at a rate of 20°C / min, and maintained for 3 minutes. Nitrogen was used as the carrier gas with a constant flow of 2 mL / min. The temperature of the detector is 300°C, and it is supplied with 14mL / min of hydrogen, 17mL / min of air 1 and 10mL / min of air 2. The detector voltage is 500V, the gate delay is 6ms, and the gate width is 20ms.

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Embodiment 2

[0031] The 52% (v / v) Wuliangye was detected, and the detection conditions were the same as in Example 1. Fig. 2 is the gas chromatogram of this wine sample, and the sulfide that detects has hydrogen sulfide (H 2 S) 176.17μg / L, methyl mercaptan (MeSH) 28.93μg / L, dimethyl sulfide (DMS) 6.30μg / L, methyl thioacetate (MeSOAc) 39.60μg / L, dimethyl disulfide (DMDS) 1.68μg / L, ethyl thioacetate (EtSOAc) 19.73μg / L, diethyl disulfide (DEDS) 0.05μg / L, dimethyl trisulfide (DMTS) 21.45μg / L, 3 - methionol 0.36 mg / L.

Embodiment 3

[0033] 46% (v / v) of Yanghe Daqu was detected, and the detection conditions were the same as in Example 1. Fig. 3 is the gas chromatogram of this wine sample, and the sulfide detected has hydrogen sulfide (H 2 S) 17.50μg / L, methyl mercaptan (MeSH) 14.46μg / L, dimethyl sulfide (DMS) 2.52μg / L, methyl thioacetate (MeSOAc) 1.60μg / L, dimethyl disulfide (DMDS) 1.52μg / L, ethyl thioacetate (EtSOAc) 5.33μg / L, diethyl disulfide (DEDS) 0.04μg / L, dimethyl trisulfide (DMTS) 14.56μg / L, 3 - methionol 0.81 mg / L.

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Abstract

This invention relates to one method to test sulfur compound in the analysis technique, which uses top fix phase micro extraction and gas phase and color spectrum and impulse flare light tester cross technique for quantitative analysis. This invention establishes one sulfur compound test with rapid speed with limit to 0.01 mu g / L, linear relative parameter R2 less than 0.98 and with relative standard error less than 20 percent and alcohol recycle rate as 80 to 100 percent.

Description

technical field [0001] The invention discloses a method for determining sulfide in liquor, which belongs to the technical field of liquor flavor analysis, and specifically relates to the combined technology of headspace solid-phase microextraction and gas chromatography-pulse flame photometric detector. Background technique [0002] Liquor has a long history of production in China, with an annual output of 8 million tons at its peak. Liquor is very rich in trace components, including alcohols, aldehydes, acids, esters, sulfides, and aromatic compounds. The sulfide has a strong characteristic odor, which is beneficial to the flavor when it exists in the liquor at a very low concentration, but damages the overall flavor of the liquor when its concentration is slightly higher, so controlling the content of the sulfide in the liquor is very important. Improving the quality of wine is very important. However, the formation mechanism of these sulfides has not been thoroughly stu...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08G01N30/86G01N30/68
Inventor 范文来徐岩
Owner JIANGNAN UNIV
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