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Measurement method of content of short-chain chlorinated paraffin

A technology for short-chain chlorinated paraffins and determination methods, applied in the field of analysis and detection, can solve problems such as interference, difficulty in short-chain chlorinated paraffins, and inaccurate quantitative results, and achieve high accuracy, high sensitivity, and accurate and reliable results

Pending Publication Date: 2018-05-11
INST OF ANALYSIS GUANGDONG ACAD OF SCI (CHINA NAT ANALYTICAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the difference in the length of the carbon chain, the number of substituted chlorine atoms and the substitution position, and the two stable isotopes of chlorine ( 35 Cl and 37 Cl) leads to tens of thousands of homologues, isomers and isotopomers in chlorinated paraffins, which causes great difficulties in the separation, identification and determination of short-chain chlorinated paraffins , how to accurately determine the content of short-chain chlorinated paraffins has always been a difficult problem in the world
Since some of the medium-chain low-chlorine substitutions and short-chain high-chlorination substitutions in CPs have similar molecular weights, the chromatographic separation technology cannot completely separate the compounds, and the chromatographic peaks are in the form of "bulges", and the peaks of a certain retention time period are combined during quantification Calculation, short-chain chlorinated paraffins are interfered by medium-chain chlorinated paraffins, and the quantitative results are inaccurate
The current chromatographic separation technology cannot separate the various compounds in CPs, and the accurate determination of the content of short-chain chlorinated paraffins has become a worldwide problem

Method used

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  • Measurement method of content of short-chain chlorinated paraffin
  • Measurement method of content of short-chain chlorinated paraffin
  • Measurement method of content of short-chain chlorinated paraffin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Determine the content of short-chain chlorinated paraffins in samples with known content:

[0025] 1) Instruments and reagents

[0026] Agilent1290HPLC-6540-Q-TOF-MS (Agilent Corporation of the United States), equipped with dual-jet electrospray ion source; KQ2200 desktop mechanical ultrasonic cleaner (Dongguan Ultrasonic Equipment Co., Ltd.), Sartorius TP-114 electronic balance ( American Sartorious company). Methanol, ethanol and acetonitrile are chromatographically pure reagents (Merck, Germany), water is double distilled water, and ammonium acetate (Aladdin reagent). Standard: chlorparaffin C 10 -C 13 , 51.5% Cl (Dr. Ehrenstorfer GmbH).

[0027] 2) Sample pretreatment

[0028] Accurately weigh 0.1g of the sample into a 10mL volumetric flask, ultrasonically dissolve it in 2mL of n-hexane, make up to volume with ethanol, and pass through a 0.20μm microporous membrane for LC-QTOF-MS detection.

[0029] 3) Liquid chromatography conditions

[0030] Chromatographic...

Embodiment 2

[0037] Determination of short-chain chlorinated paraffins in actual industrial chlorinated paraffin products:

[0038] 1) Instruments and reagents

[0039] Agilent1290HPLC-6540-Q-TOF-MS (Agilent Corporation of the United States), equipped with dual-jet electrospray ion source; KQ2200 desktop mechanical ultrasonic cleaner (Dongguan Ultrasonic Equipment Co., Ltd.), Sartorius TP-114 electronic balance ( American Sartorious company). Methanol, ethanol and acetonitrile are chromatographically pure reagents (Merck, Germany), water is double distilled water, and ammonium acetate (Aladdin reagent). Standard: Chlorparaffin C 10 -C 13 , 51.5% Cl (Dr. Ehrenstorfer GmbH).

[0040] 2) Sample pretreatment

[0041] Accurately weigh 0.1g of the sample into a 10mL volumetric flask, ultrasonically dissolve it in 2mL of n-hexane, constant volume with ethanol, pass through a 0.20μm microporous membrane, and detect by LC-QTOF-MS. .

[0042] 3) Liquid chromatography conditions

[0043] Chro...

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Abstract

The invention discloses a measurement method of the content of short-chain chlorinated paraffin. According to the method, an ultra-performance liquid chromatography-serially-connected quadrupole time-of-flight mass spectrometry instrument is adopted for measuring a chlorinated paraffin sample and a short-chain chlorinated paraffin standard substance, and an anion full-scanning mode is adopted formeasuring mass spectrometric data of 24 compounds in the short-chain chlorinated paraffin in which the carbon number is 10-13 and the number of chlorine substituents is 5-10; two isotope ion peaks high in abundance and accurate in mass are selected from each molecular formula to serve as feature ions, 48 isotope feature ions accurate in mass number are extracted from a total ion flow chromatogram,with the abundance of two feature ion peaks in each kind of molecular formula short-chain chlorinated paraffin compounds as qualitative reference, the total peak area of the 48 isotope feature ions is adopted for quantification, a quantification result is contrasted with the short-chain chlorinated paraffin standard substance at last, and the content of the short-chain chlorinated paraffin is calculated. The measurement method solves the problems that the measurement of the short-chain chlorinated paraffin is interfered by medium-chain chlorinated paraffin, and the short-chain chlorinated paraffin is difficult to separate from the medium-chain chlorinated paraffin; the method has the advantages of being accurate and reliable in result and high in sensitivity.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection. More specifically, the invention relates to a chemical detection method for the content of short-chain chlorinated paraffins (SCCPs) in chlorinated paraffins (CPs) products. Background technique [0002] Short-chain chlorinated paraffins have attracted widespread attention due to their persistent pollutant properties. In November 2015, the EU law stipulated that the mass fraction of SCCPs in products should be less than 0.15%. The implementation of this bill has caused a strong impact on my country's chlorinated paraffin-related industries. [0003] Chlorinated paraffins can be divided into short-chain chlorinated paraffins (C10-13, SCCPs), medium-chain chlorinated paraffins (C14-17, MCCPs) and long-chain chlorinated paraffins (greater than C18, LCCPs) according to the length of the carbon chain. Among them, LCCPs and MCCPs are less toxic, while SCCPs are more toxic, and have been...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88G01N30/86
CPCG01N30/06G01N30/8634G01N30/88
Inventor 吴惠勤黄芳黄晓兰罗辉泰
Owner INST OF ANALYSIS GUANGDONG ACAD OF SCI (CHINA NAT ANALYTICAL
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