Method for determining content of dimethylformamide

A technology of dimethylformamide and content, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of inaccurate quantification, large amount of pretreatment reagents, unstable recovery rate, etc., and achieve the effect of easy promotion

Active Publication Date: 2013-10-02
广电计量检测(湖南)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The operation of the gas chromatography process is complicated, the amount of pretreatment reagents is large, the detection limit of the method is high, the recovery rate is unstable, and the quantification is not accurate

Method used

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  • Method for determining content of dimethylformamide
  • Method for determining content of dimethylformamide
  • Method for determining content of dimethylformamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Take a black bull head layer sofa leather sample produced by a certain enterprise, cut it into pieces of 5mm×5mm, and mix it evenly. Accurately weigh 2.1856g of the sample (accurate to 0.1mg) into a test tube and add 20mL of ethyl acetate, ultrasonically extract in a water bath at 40°C for 2h, add 20mL of ethyl acetate for ultrasonic extraction for 2h, combine the two extracts and evaporate in a rotary evaporator Concentrate on the instrument to 3mL, and finally dilute to 10mL with ethyl acetate as the sample extract.

[0048] The GC-MS conditions were set as follows:

[0049] Chromatographic column: DB-5MS column, 30m×0.25mm(i.d.)×0.25μm;

[0050] Column temperature: initial temperature of 60°C, keep for 1min, raise to 120°C at 10°C / min; keep for 2min, rise to 200°C at 20°C / min, keep for 5min;

[0051] Carrier gas: helium, purity ≥99.999%; control mode: constant flow; flow rate: 1.0mL / min;

[0052] Injection method: splitless injection, open the valve after 1min; inje...

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Abstract

The invention provides a method for determining the content of dimethylformamide, sequentially comprising the following steps of, firstly, pretreating a sample; secondly, preparing a sample extract and a standard working fluid; thirdly, carrying out gas phase chromatography-mass spectrometry (GC-MS) analysis; fourthly, drawing a standard curve; and fifthly, quantitatively determining the content of the dimethylformamide with an external standard method. The method is sensitive, accurate, exclusive, convenient, feasible and easy to popularize and is necessary to control residues of the dimethylformamide.

Description

technical field [0001] The invention relates to the field of product quality detection, in particular to a method for detecting the content of dimethylformamide in leather and textiles. Background technique [0002] Dimethylformamide (Dimethylformamide; DMF) is a colorless liquid with a light amine odor. Molecular formula C 3 h 7 NO, molecular weight 73.10, relative density 0.9445 (25°C), melting point -61°C, boiling point 152.8°C, flash point 57.78°C, vapor density 2.51, vapor pressure 0.49kpa (3.7mmHg25°C), autoignition point 445°C, mixture of steam and air The explosion limit is 2.2-15.2%, which can cause combustion and explosion when exposed to open flame and high heat. [0003] As an important chemical raw material and a solvent with excellent performance, dimethylformamide (DMF) is soluble in water, most organic solvents and inorganic liquids, and has a strong dissolving ability, so it is called a universal organic solvent. Dimethylformamide is a good solvent for v...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 王海鸣
Owner 广电计量检测(湖南)有限公司
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