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Method for detecting short-chain chlorinated paraffins (SCCPs)

A technology of short-chain chlorinated paraffins and detection methods, which is applied in measuring devices, instruments, and material analysis through electromagnetic means, and can solve problems such as poor anti-interference ability, cumbersome operation, and long processing time, and achieve strong anti-interference ability , convenient operation, and sufficient and convenient extraction effects

Inactive Publication Date: 2012-06-20
深圳天祥质量技术服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention proposes a simple, rapid, and accurate qualitative and quantitative detection method for short-chain chlorinated paraffins in products using gas chromatography-mass spectrometry to solve the problems of long pretreatment time, cumbersome operation, and poor anti-interference ability. technical problem

Method used

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  • Method for detecting short-chain chlorinated paraffins (SCCPs)
  • Method for detecting short-chain chlorinated paraffins (SCCPs)
  • Method for detecting short-chain chlorinated paraffins (SCCPs)

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Using toluene as a solvent, a series of standard solutions of short-chain chlorinated paraffins were prepared, and analyzed and detected by gas chromatography and mass spectrometry according to the experimental conditions. figure 1 Chromatogram of short-chain chlorinated paraffins. The total target peak response value is plotted against the concentration, and the standard curve of short-chain chlorinated paraffins is established according to the three parallel measurement results of the standard solution, such as figure 2 As shown, the abscissa represents the concentration of the short-chain chlorinated paraffin standard solution, and the ordinate represents the gas chromatography peak area response value, and the functional relationship of the resulting standard curve is Y=7373X+24232, where X represents the concentration of the short-chain chlorinated paraffin, Y represents the response value of the gas chromatography peak area, and its linear correlation coefficient...

Embodiment 2

[0034] Accurately weigh 1.0 g of the prepared sample into a container, add 20 mL of toluene, and place it in an ultrasonic water bath at 23°C (room temperature) for ultrasonic extraction at 100% power for 1 hour. After the extraction is completed, take out the container and wait for cooling, then filter it through a 0.45 micron filter head into a chromatographic bottle for instrumental analysis. Three parallel samples were made for the sample, the test numbers were a1, a2 and a3, the analysis results were shown in Table 1, and the first parallel sample (test number a1) was measured 4 times, the analysis results were shown in Table 2. From Table 1, the relative standard deviation (RSD) of parallel samples was 2.37%. Known from Table 2, the relative standard deviation of the repeatability test is 1.01%.

[0035] Table 1 Test content of short-chain chlorinated paraffins in samples

[0036]

[0037] Table 2 Test repeatability of short-chain chlorinated paraffins in samples

...

Embodiment 3

[0040] The standard solution was added to the sample respectively, and the experiment was carried out according to the above-mentioned sample pretreatment method and instrument analysis and detection method. Each sample was measured 3 times in parallel to get the average value, and the recovery rate of the sample was calculated according to the actual amount added and the measured results. The experimental results are shown in Table 3. It can be seen from Table 3 that the recovery rate of the sample is above 92.8%, indicating that the test method used is suitable for the test of short-chain chlorinated paraffins.

[0041] Table 3 Recovery rate of samples

[0042]

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Abstract

The invention discloses a method for detecting short-chain chlorinated paraffins (SCCPs). The method comprises the following steps of: pretreating a sample by an ultrasonic extraction method; filtering extract liquor in a chromatograph bottle, and performing instrumental analysis; detecting the SCCPs by a gas chromatography-mass spectrometry technology; allowing the pretreated sample to enter a chromatographic column from a sample inlet of a gas chromatograph-mass spectrometer, and performing programmed heating; and allowing sample components which are separated by the chromatographic column to enter a mass spectrum detection part of the gas chromatograph-mass spectrometer through a port, and bombarding an ion source which is subjected to mass spectrum detection by using electrons. According to the method, an instrument is low in price and safe; an analysis method is accurate and quick and low in interference; and the SCCPs can be separated optimally.

Description

technical field [0001] The invention relates to a method for detecting chlorinated paraffins, in particular to a method for detecting short-chain chlorinated paraffins by gas chromatography-mass spectrometry. Background technique [0002] Chlorinated paraffin is a polychlorinated long-chain n-alkane, the chain length can vary from C10 to C30, and the chlorine content is between 30 wt% and 70 wt%. According to the different chain lengths, chlorinated paraffins can be divided into short-chain (C10-C13), medium-chain (C14-C17) and long-chain (C18-C30) chlorinated paraffins. Chlorinated paraffins are obtained by reacting normal alkanes in petroleum fractions with chlorine molecules, and are a mixture of a series of isomers. Due to its good chemical stability, suitable viscosity, good flame retardancy, low vapor pressure and other properties, it is mainly used as an additive for cutting fluids, a lubricant for metal processing, and in plastics, paints and Used as a flame retard...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/60G01N27/68
Inventor 邓湘辉舒文利
Owner 深圳天祥质量技术服务有限公司
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