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Method for detecting and pretreating polycyclic aromatic hydrocarbon in oily sludge

A polycyclic aromatic hydrocarbon and pretreatment technology, which is applied in the field of oily sludge treatment, can solve the problems of long time consumption, complicated operation, large amount of extraction solvent, etc., and achieve the effect of simple operation, less usage and short pretreatment time

Inactive Publication Date: 2015-02-25
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Therefore, it is necessary to carry out detection and control of PAHs in oily sludge. Before detection, PAHs in oily sludge should be pretreated to facilitate detection and make detection accuracy and sensitivity higher; however, currently There is no specific pretreatment method for PAHs in oily sludge
In the prior art, the pretreatment methods of polycyclic aromatic hydrocarbons in soil are mainly Soxhlet extraction and chromatographic purification. This pretreatment method has problems such as complicated operation, large amount of extraction solvent, and long time consumption, and this method is aimed at PAHs in soil should be pretreated instead of oily sludge, a substance with high organic matter content and complexity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] This embodiment provides a detection pretreatment method for polycyclic aromatic hydrocarbons in oily sludge, comprising the following steps:

[0042] Sample preparation:

[0043] Get the oily sludge with an oil content of 28.35% (tank cleaning sludge), remove stones and other sundries, add 100 g of diatomaceous earth to 100 grams of the oily sludge, put it in a mortar and grind it, and pass through a 100-mesh sieve after grinding to make it The components are evenly distributed, and an oily sludge sample is obtained.

[0044] Rapid extraction of PAHs:

[0045] Weigh 0.2 g of oily sludge sample, add 0.1 mg of substitute (naphthalene-D8) to the oily sludge sample, and mix to obtain the oily sludge mixture;

[0046] Put the oily sludge mixture into the stainless steel extraction tank of the ASE350 accelerated solvent extractor, and extract it with dichloromethane, the extraction temperature is 100°C, the pressure is 1500psi, and the extraction is 3 times, each time with...

Embodiment 2

[0057] This embodiment provides a detection pretreatment method for polycyclic aromatic hydrocarbons in oily sludge, comprising the following steps:

[0058] Sample preparation:

[0059] Get the oily sludge with an oil content of 18.68% (ground oily sludge), remove stones and other sundries, add 100 g of diatomaceous earth to 100 grams of oily sludge, place it in a mortar and grind it, pass through a 100-mesh sieve after grinding, and make it assembled Evenly distributed, the oily sludge sample was obtained.

[0060] Rapid extraction of PAHs:

[0061] Take 0.5g oily sludge sample by weighing, add (naphthalene-D8) 0.5mg to the oily sludge sample, and mix to obtain the oily sludge mixture;

[0062] Put the oily sludge mixture into the stainless steel extraction tank of the ASE350 accelerated solvent extractor, and extract it with acetone, the extraction temperature is 100°C, the pressure is 1500psi, and the extraction is performed twice, with a static cycle of 5 minutes each t...

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Abstract

The invention provides a method for detecting and pretreating polycyclic aromatic hydrocarbon in oily sludge. The method comprises the steps of taking the oily sludge, feeding kieselguhr into the oily sludge, grinding, sieving, adding a substitute, evenly mixing and then extracting with extract liquor; collecting the extract liquor, and concentrating to obtain extract concentrated solution; filling a chromatographic column; after the chromatographic column is balanced, feeding the extract concentrated solution sample onto the chromatographic column, eluting the chromatographic column with n-hexane after the chromatographic column comes into full contact with the extract concentrated solution; eluting the chromatographic column with a mixed eluant of dichloromethane and n-hexane; collecting the eluant until the mixed eluant of dichloromethane and n-hexane completely flows outside, thus obtaining the mixed liquid of the polycyclic aromatic hydrocarbon; concentrating the mixed liquid of the polycyclic aromatic hydrocarbon, and carrying out nitrogen purging concentration to obtain the polycyclic aromatic hydrocarbon sample. With adoption of the rapid extraction method, the use amount of an organic solvent is small, the pretreatment time is short and operation is simple.

Description

technical field [0001] The invention relates to a detection and pretreatment method for polycyclic aromatic hydrocarbons in oily sludge, belonging to the technical field of oily sludge treatment. Background technique [0002] Oily sludge is the main solid waste discharged from oil fields and refining and chemical enterprises. It is mainly composed of crude oil, water, clay minerals, biological organic matter and chemical additives. The general oil content is about 10%, and the highest can reach 20%. -30%, has always been an environmental protection problem in the petroleum and petrochemical industry. Oily sludge has been included in the "National List of Hazardous Wastes". Domestic and foreign government agencies, non-governmental organizations, scientific research institutions, and production enterprises and institutions all attach great importance to the environmental management and pollution control of oily sludge. [0003] Polycyclic aromatic hydrocarbons (PAHs) are the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/40G01N1/34
Inventor 任雯刘光全王蓉沙张明栋岳勇谢水祥
Owner PETROCHINA CO LTD
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