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A pretreatment method for oil in carbon residue for detection

A technology of carbon residue and oil content, applied in the field of chemical detection, can solve the problems of low carbon residue density, difficult separation of carbon tetrachloride, slow filtration speed, etc., achieve high accuracy and reliability, shorten filtration time, and improve accuracy sexual effect

Active Publication Date: 2021-04-13
SHANGHAI INST OF MEASUREMENT & TESTING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to conveniently and accurately detect the oil in the carbon residue, refer to the determination method in HJ 637-2012 "Determination of Water Quality Petroleum and Animal Oil", and choose carbon tetrachloride as the extraction reagent. However, the carbon residue has a small density and is very easy to float or Suspended in carbon tetrachloride, and it is difficult to separate from carbon tetrachloride, which affects the accuracy of oil content detection
In order to remove carbon residue, filter paper or absorbent cotton is currently used for filtration, but the filtration speed of filter paper or absorbent cotton is slow, which may also affect the accurate detection of oil content
On the one hand, the filtration speed of filter paper or absorbent cotton is slow, which may cause the volatilization of oil and carbon tetrachloride, and prolong the contact time between filter paper or absorbent cotton and oil and carbon tetrachloride, affecting the accurate detection of oil content; On the one hand, the filter paper is easily damaged, and the absorbent cotton will also leak, which is difficult to meet the separation and purification requirements, or repeated operations to meet the separation and purification requirements also affect the accurate detection of oil content
[0004] Therefore, in order to overcome the problem that the oil content in the carbon residue cannot be measured accurately due to the difficulty of separating the small density substances such as carbon residue and organic extractants such as carbon tetrachloride, it is very important to provide a new pretreatment method for the oil content in the carbon residue. It is necessary that the method does not affect oil and organic solvent (carbon tetrachloride) (such as adsorption, chemical reaction), and can quickly separate carbon residue from oil and organic solvent (carbon tetrachloride) Improve the accuracy and reliability of oil content determination in carbon residue

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1 The influence of different filter materials on oil recovery rate

[0021] According to different filter materials (absorbent cotton, filter paper and solid-phase extraction column), it was divided into three test groups: absorbent cotton group, filter paper group and solid-phase extraction column group. Each group was carried out in parallel in 3 parts. The operation of each group was as follows:

[0022] Absorbent cotton group: take the infrared oil standard substance solution with a concentration of 1000mg / L, dilute it with carbon tetrachloride to a concentration of 100mg / L, filter through a funnel with absorbent cotton, and measure the oil value of the obtained solution with an infrared oil meter. 110.3 mg / L (average of 3 copies), the recovery rate was 110%.

[0023] Filter paper group: Take the infrared oil standard substance solution with a concentration of 1000mg / L, dilute it with carbon tetrachloride to a concentration of 100mg / L, filter through a fu...

Embodiment 2

[0026] The influence of embodiment 2 carbon slag on the recovery rate of oil under different filter materials

[0027] According to different filter materials (absorbent cotton, filter paper and solid-phase extraction column), it was divided into three test groups: absorbent cotton group, filter paper group and solid-phase extraction column group, and each group carried out two experimental operations in parallel. The specific operations were as follows:

[0028] Absorbent cotton group:

[0029] Operation 1: After mixing 1g of carbon residue with 50mL of carbon tetrachloride, filter through a funnel placed with absorbent cotton, and measure the oil value of the obtained solution with an infrared oil meter to 232.02mg / L (average value of 3 copies).

[0030] Operation 2: Add 5mL, 1000mg / L standard substance solution for infrared oil to 1g of carbon residue, and use carbon tetrachloride to make the volume to 50mL, filter through a funnel with absorbent cotton, and measure the oil...

Embodiment 3

[0042] Embodiment 3 Filtration time investigation

[0043]According to different filter materials (absorbent cotton, filter paper and solid phase extraction column), it is divided into three test groups: absorbent cotton group, filter paper group and solid phase extraction column group. The operation of each group is as follows:

[0044] Absorbent cotton group: After mixing 1g of carbon residue with 20mL of carbon tetrachloride, filter through a funnel with absorbent cotton for 1.5min, and measure the oil content of the solution with an infrared oil detector to 574.4mg / L.

[0045] Filter paper group: After mixing 1g of carbon residue with 20mL of carbon tetrachloride, filter through a funnel with filter paper for 0.5min, and measure the oil content of the resulting solution to 505mg / L with an infrared oil detector.

[0046] Solid-phase extraction column group: After mixing 1g of carbon residue and 20mL of carbon tetrachloride, add a C18 silica gel solid-phase extraction column...

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Abstract

The invention belongs to the field of chemical detection, and specifically relates to a pretreatment method for oil in carbon residues for detection. After mixing the carbon residues and carbon tetrachloride, they are pressure-filtered from a solid-phase extraction column or a solid-phase extraction membrane. A carbon tetrachloride solution in which oil is dissolved is obtained. This pretreatment method overcomes the difficult problem of separation between small-density substances such as carbon residue and organic solvents such as carbon tetrachloride, ensures effective separation between carbon residue and the carbon tetrachloride solution that is dissolved with oil, and avoids carbon residue on the carbon tetrachloride solution. The influence of subsequent oil content determination; at the same time, the solid-phase extraction column and solid-phase extraction membrane itself will not affect the oil and carbon tetrachloride, and can enrich and purify the oil in carbon tetrachloride to improve the carbon residue The accuracy and reliability of the oil content test results.

Description

technical field [0001] The invention belongs to the field of chemical detection, and in particular relates to a pretreatment method for oil in carbon residues for detection. Background technique [0002] With the development of environmental protection, more and more enterprises pay attention to the utilization of waste. Some industrial waste and domestic waste are treated with multi-stage large-scale industrial equipment to obtain carbon residue. If the detected value of the carbon residue is within the emission standard limit If it is within the limit, it can be discharged or used for secondary utilization such as making handicrafts and returning to farmland. Oil, one of the components of carbon residue, is a difficult pollutant to clean up. [0003] In order to conveniently and accurately detect the oil in the carbon residue, refer to the determination method in HJ 637-2012 "Determination of Water Quality Petroleum and Animal Oil", and choose carbon tetrachloride as the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/34G01N1/40
CPCG01N1/34G01N1/4077G01N2001/4088
Inventor 李学辉陈希尧钟义林唐巍飚刘悦丁臻敏
Owner SHANGHAI INST OF MEASUREMENT & TESTING TECH
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