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Method and system for measuring chlorine content of chlorinated paraffin

A technology of chlorinated paraffin and determination method, applied in the field of analysis and detection, can solve the problems of easy generation of errors, errors, complicated detection and the like, and achieve the effect of less sample consumption

Pending Publication Date: 2021-02-02
ZHEJIANG SCI-TECH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among these methods, the mercury measurement method requires human judgment on the titration end point, which is prone to certain errors, and waste acid and waste mercury need to be specially treated to avoid polluting the surrounding environment and endangering human health; Both require cumbersome sample pretreatment on chlorinated paraffins, which complicates the detection and is prone to errors

Method used

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  • Method and system for measuring chlorine content of chlorinated paraffin
  • Method and system for measuring chlorine content of chlorinated paraffin
  • Method and system for measuring chlorine content of chlorinated paraffin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] 1. Instruments and reagents

[0050] Instruments: Agilent 7890B-5977A gas chromatography-mass spectrometer, Frontier PY-3030D micro-furnace cracker.

[0051] Reagent: n-hexane (chromatographic grade), using chlorinated paraffin standard products with chlorine content N=41.95%, 70.12% to prepare chlorinated paraffin standard series (chlorine content N=41.95%, 44.78%, 47.58%, 50.40%), chlorine Paraffin wax test sample (chlorine content N=42.06%, executive standard: HG / T 3017-1988 mercury measurement method).

[0052] 2. Methods and Results

[0053] 2.1 Measurement conditions

[0054]Chromatographic conditions: initial column temperature of 50°C, hold for 1min, increase temperature at 10°C / min to 280°C, hold for 2min; inlet temperature 280°C; mass spectrometry conditions: quadrupole temperature 150°C, ion source temperature 230°C, interface temperature 250°C, selected ion mode monitoring. Cracking conditions: cracking temperature 850°C, cracking time 30s. Injection vo...

Embodiment 2

[0062] 1. Instruments and reagents

[0063] Instrument: Agilent 7890B-5977A gas chromatography-mass spectrometer, Frontier PY-3030D micro-furnace cracker;

[0064] Reagent: cyclohexane (chromatographic grade), using chlorinated paraffin standard products with chlorine content N=41.95%, 70.12% to prepare chlorinated paraffin standard series (chlorine content N=47.58%, 50.40%, 53.22%, 56.04%), Chlorinated paraffin test sample (chlorine content N=52.18%, executive standard: HG / T 3017-1988 mercury measurement method).

[0065] 2. Methods and results

[0066] 2.1 Measurement conditions

[0067] Chromatographic conditions: initial column temperature 50°C, keep for 1min, increase temperature to 280°C at 15°C / min, keep for 2min; inlet temperature 250°C; mass spectrometry conditions: quadrupole temperature 150°C, ion source temperature 230°C, interface temperature 250°C, selected ion mode monitoring. Cracking conditions: cracking temperature 850°C, cracking time 36s. Injection vol...

Embodiment 3

[0075] 1. Instruments and reagents

[0076] Instrument: Agilent 7890B-5977A gas chromatography-mass spectrometer, Frontier PY-3030D micro-furnace cracker;

[0077] Reagent: cyclohexane (chromatographic grade), using chlorinated paraffin standard products with chlorine content N=41.95%, 70.12% to prepare chlorinated paraffin standard series (chlorine content N=58.85%, 61.67%, 64.49%, 67.30%), Chlorinated paraffin test sample (chlorine content N=63.14%, executive standard: HG / T 3017-1988 mercury measurement method).

[0078] 2. Methods and results

[0079] 2.1 Measurement conditions

[0080] Chromatographic conditions: initial column temperature of 50°C, hold for 1min, increase temperature at 10°C / min to 280°C, hold for 2min; inlet temperature 280°C; mass spectrometry conditions: quadrupole temperature 150°C, ion source temperature 230°C, interface temperature 250°C, selected ion mode monitoring. Cracking conditions: cracking temperature 800°C, cracking time 60s. Injection ...

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Abstract

The invention discloses a method and a system for measuring chlorine content of chlorinated paraffin, which are characterized in that cracking chromatography-mass spectrometry is utilized to measure chlorine content in chlorinated paraffin, anaerobic cracking temperature is 350-1050 DEG C, peak area or peak height signals of a hydrogen chloride component in a cracking product are taken as two groups of variables, and the standard curve equation is measured by using a chlorinated paraffin standard substance with known chlorine content so as to obtain the chlorine content of the chlorinated paraffin test sample. The system comprises a sample injection unit, a cracking unit, a separation unit, a detection unit and a calculation module. The method and the system have the advantages of less sample consumption, simplicity, high efficiency and environmental protection.

Description

technical field [0001] The invention relates to the technical field of analysis and detection, in particular to a method and system for determining the chlorine content of chlorinated paraffin. Background technique [0002] Chlorine content is the main indicator of chlorinated paraffin product quality, which determines the performance of the product. Chlorinated paraffin products can be divided into chlorinated paraffin-42, chlorinated paraffin-52 and chlorinated paraffin-70 according to the chlorine content. [0003] Due to the difference in the number and substitution position of chlorine atoms in chlorinated paraffin, its composition is complex and its physical and chemical properties are quite different. At present, the measuring method of chlorine content in chlorinated paraffin mainly contains mercury method (HG / T 3017-1988), turbidimetry, ion chromatography, flame atomic absorption spectrometry etc. (as Liu Jiping, " in chlorinated paraffin Review of the Determinati...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/12G01N30/30G01N30/72G01N30/16
CPCG01N30/02G01N30/06G01N30/12G01N30/30G01N30/72G01N30/16G01N2030/067G01N2030/126G01N2030/3076
Inventor 陈海相魏凯佳戴宏翔李楠陈麟杰姚若兰
Owner ZHEJIANG SCI-TECH UNIV
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