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Organochlorine content determination method

A determination method and organochlorine technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of large errors, complicated operation processes, low instrument sensitivity, etc., to improve production efficiency and economic benefits, eliminate test errors, and operate easy effect

Inactive Publication Date: 2015-07-08
SHANDONG DAMING FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the complex operation process, it is easy to cause operational errors, and the instrument has low sensitivity and large errors, which makes the reproducibility of test results poor.
Especially for non-flammable products, it is more difficult to obtain accurate test results

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The content of residual dichloroethane in water-soluble chemical products is determined according to the following steps:

[0023] a. Start the gas chromatograph:

[0024] Turn on the hydrogen generator (flow 0.3MPa), air cylinder (flow 0.5MPa), nitrogen cylinder (flow 0.5MPa), turn on the host computer, wait for the gas path to stabilize, turn on the headspace and gas chromatograph switch, and enter the LAB operation interface. Set the instrument operating parameters as follows:

[0025] Nitrogen flow rate: 26.2mL / min; hydrogen flow rate: 30 mL / min; air flow rate: 400 mL / min; column oven temperature: 80°C; injection port split ratio: 1:150; FID detector temperature: 300°C.

[0026] b. Standard solution preparation:

[0027] Weigh 0.1g (accurate to 0.001g) dichloroethane sample, dilute to 1L with distilled water, as the mother liquor, accurately pipette 1mL, 5 mL, 10 mL, 20 mL, 50 mL of mother liquor, and dilute to 100 mL as the standard solution, then pipette 5 mL o...

Embodiment 2

[0035] The residual dichloromethane content in water-soluble chemical products is carried out according to the following steps:

[0036] a. Start the gas chromatograph:

[0037] Turn on the hydrogen generator (flow 0.3MPa), air cylinder (flow 0.5MPa), nitrogen cylinder (flow 0.5MPa), turn on the host computer, wait for the gas path to stabilize, turn on the headspace and gas chromatograph switch, and enter the LAB operation interface. Set the operating parameters of the instrument as follows: nitrogen flow rate: 26.2mL / min; hydrogen flow rate: 30 mL / min; air flow rate: 400 mL / min; column oven temperature: 60°C; inlet split ratio: 1:150; FID detector Temperature: 300°C.

[0038] b. Standard solution preparation:

[0039] Weigh 0.1g (accurate to 0.001g) of dichloromethane sample, dilute to 1L with distilled water, as the mother liquor, accurately pipette 1mL, 5 mL, 10 mL, 20 mL, 50 mL mother liquor, and dilute to 100 mL with distilled water mL as the standard solution, pipett...

Embodiment 3

[0047] The content of residual dichloroethane in oil-soluble chemical products is determined according to the following steps:

[0048] a. Start the gas chromatograph:

[0049] Turn on the hydrogen generator (flow 0.3MPa), air cylinder (flow 0.5MPa), nitrogen cylinder (flow 0.5MPa), turn on the host computer, wait for the gas path to stabilize, turn on the headspace and gas chromatograph switch, and enter the LAB operation interface. Set the instrument operating parameters as follows:

[0050] Nitrogen flow rate: 26.2mL / min; hydrogen flow rate: 30 mL / min; air flow rate: 400 mL / min; column oven temperature: 80°C; injection port split ratio: 1:150; FID detector temperature: 300°C.

[0051] b. Standard solution preparation:

[0052] Weigh 0.1g (accurate to 0.001g) of dichloroethane sample, dilute to 1L with dimethyl sulfoxide, and use it as mother liquor, accurately pipette 1mL, 5 mL, 10 mL, 20 mL, 50 mL mother liquor respectively, and use Dimethyl sulfoxide was adjusted to 10...

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Abstract

The invention provides an organochlorine content determination method. The method comprises the following steps: weighing a pure chlorohydrocarbon compound contained in chemical engineering products, and diluting by using a solvent to form a certain concentration of a solution, wherein the solvent can be one or more of water, N,N-dimethyl formamide, dimethyl sulfoxide, 1,3-dimethyl-2-imidazolone and liquid paraffin; and respectively adding standard solutions into sample bottles, sealing by using a sealer, putting the sample bottles in a headspace sample cell, setting gas chromatographic operation parameters, and testing by adopting a gas chromatographic static headspace technology. The method for determining the content of organochlorine in the chemical engineering products by using gas chromatography has the advantages of high sensitivity, simple operation, and elimination of test errors brought by manual operation due to the adoption of the static headspace technology.

Description

Technical field: [0001] The invention relates to the technical field of chemical products, in particular to a method for measuring organic chlorine content. Background technique: [0002] In the crude oil refining process, the presence of chloride is an important factor causing equipment corrosion and catalyst poisoning. It is generally believed that organic chlorides in crude oil are mainly derived from chemicals added in the process of oil recovery and crude oil treatment. In order to better control the organic chloride content in crude oil, Shengli Oilfield further strengthened the detection of various oil recovery agents in 2013. The measuring method adopted is CN103389327A "Measurement Method of Organochlorine Content in Oil Recovery Auxiliaries", which is to convert the organic chlorine into inorganic chlorine after the sample is burned and decomposed, and after being absorbed by NaOH solution, measure the total chlorine content with a salt content measuring instrumen...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 杨明常李元新孟兆玲马丽红张翠苹杨丙飞
Owner SHANDONG DAMING FINE CHEM CO LTD
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