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Pretreatment method for rapidly extracting ten nitro aromatic compounds in soil

A technology of nitroaromatics and compounds, applied in the field of speech, to achieve rapid and efficient extraction analysis, increase extraction efficiency, and save manpower and material resources

Inactive Publication Date: 2014-09-10
NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] Aiming at the pretreatment problems existing in the quantitative analysis of nitroaromatic compounds in soil environmental samples, the present invention provides a pretreatment method for rapidly extracting 10 kinds of nitroaromatic compounds in soil, using organic solvents with different mixed polarities System, the use of mechanical shaking and crushing methods, the use of high-speed centrifugation to achieve solid-liquid separation, so as to quickly and efficiently extract the pretreatment analysis technology of nitroaromatic compounds in the soil. It has obvious advantages in manpower consumption and environmental friendliness, which can greatly save the time and cost of pretreatment analysis of traditional soil, sediment, and sediment samples, save solvent consumption, and reduce the environmental risk of toxic solvents

Method used

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  • Pretreatment method for rapidly extracting ten nitro aromatic compounds in soil
  • Pretreatment method for rapidly extracting ten nitro aromatic compounds in soil
  • Pretreatment method for rapidly extracting ten nitro aromatic compounds in soil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment 1: (the pretreatment method of nitrobenzene compound in soil)

[0051] (1) The target compound is a nitrobenzene compound, and a nitrobenzene standard solution with a concentration of 1000ug / mL is prepared.

[0052] (2) Sample preparation: Weigh the blank soil (blank soil is prepared by purifying and extracting the blank soil from the natural environment as a substitute), and add 1.0ml of the nitrobenzene standard solution prepared in step (1) to prepare the soil For 5g of sample, add 5g of activated diatomaceous earth (baked at 400°C for 6h to remove organic matter), and put the mixed sample into a 40ml clean glass bottle.

[0053] (3) Sample extraction: add 10ml of acetone solvent (chromatographic grade), shake quickly for about 3 minutes, break the soil into a homogenous slurry, then add 10ml of n-hexane solvent (chromatographic grade), tighten the bottle cap, and put it into the shaker Medium and rapid shaking extraction for 40min, the speed is 200r / min....

Embodiment 2

[0059] Embodiment 2: (the pretreatment method of o-dinitrobenzene compound in soil)

[0060] (1) Select o-dinitrobenzene compound as the target compound, and prepare o-dinitrobenzene standard solution with a concentration of 1000ug / mL.

[0061] (2) Sample preparation: Weigh blank soil and add 1.0ml of the solution prepared in step (1) to obtain 5g of soil sample, add 5g of activated diatomite (baked at 400°C for 6h to remove organic matter), mix The final sample was packed into a 40ml clean glass bottle.

[0062] (3) Sample extraction: add 10ml of acetone solvent (chromatographic grade), shake quickly for about 3 minutes, break the soil into a homogenous slurry, then add 10ml of dichloromethane solvent (chromatographic grade), tighten the bottle cap, and put in the shaker Quickly shake and extract in the container for 40min at a speed of 200r / min.

[0063] (4) Centrifugation and concentration of the sample: the sample extracted by shaking in the previous step was placed in a...

Embodiment 3

[0068] Embodiment 3: (the pretreatment method of dinitrobenzene compound in the middle of soil)

[0069] (1) Select the m-dinitrobenzene compound as the target compound, and prepare m-dinitrobenzene standard solution with a concentration of 1000ug / mL.

[0070] (2) Sample preparation: Weigh blank soil and add 1.0ml of the standard solution prepared in step (1) to prepare 5g of soil sample, add 5g of activated diatomite (baked at 400°C for 6h to remove organic matter), The mixed samples were packed into 40ml clean glass bottles.

[0071] (3) Sample extraction: Add 10ml of ethyl acetate solvent (chromatographic grade), shake quickly for about 3min, break the soil into a homogenous slurry, then add 10ml of cyclohexane solvent (chromatographic grade), tighten the bottle cap, put Put it into the shaker and shake it rapidly for 40min, the speed is 200r / min.

[0072] (4) Centrifugation and concentration of the sample: the sample extracted by shaking in the previous step was placed i...

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Abstract

The invention provides a pretreatment method for rapidly extracting ten nitro aromatic compounds in soil. The method comprises the steps of soil sample preparation, oscillation extraction and centrifugal separation. Specifically, soil and purified anhydrous sodium sulfate and diatomite are mixed to achieve the effects of removing water and dispersing a matrix; an effect of dissolving active ingredients contained in soil media such as a soil solution and soil organic matter by an extraction solvent is guaranteed through extraction with hydrophobic and hydrophilic mixed solvents; a soil breaking effect is achieved by a mechanical shaking mode, and the extraction efficiency is improved; solid-liquid separation between a soil sample and the extraction solvent is finished through low-temperature high-speed centrifuging, so that an extracting solution is rapidly extracted. Compared with traditional methods for extracting nitro aromatic compounds in soil, such as Soxhlet extraction, ultrasonic extraction and accelerated solvent extraction, the pretreatment method has the obvious advantages of high one-step sample treatment capacity, small amount of organic solvents, simple steps, high extraction efficiency, low-price and simple equipment and the like.

Description

technical field [0001] The invention relates to a pretreatment extraction technology for 10 kinds of nitroaromatic compounds in polluted soil, specifically, a pretreatment method for rapidly extracting 10 kinds of nitroaromatic compounds in soil, which is a multiphase mixing electrode A pretreatment method for rapidly extracting 10 kinds of nitroaromatic compounds from soil samples using a non-toxic organic solvent as an extractant, mechanical shaking, and high-speed low-temperature centrifugation. Background technique [0002] Nitroaromatics is the general term for nitroaromatic compounds, and they are intermediates in the synthesis of dyes, paints, plastics, explosives, pharmaceuticals and pesticides. Nitroaromatic pollutants in the environment mainly include nitrobenzene, chloronitrobenzene, nitrotoluene and other substances. [0003] Most nitroaromatic compounds have the characteristics of stable chemical properties, high toxicity and bioaccumulation. They are highly to...

Claims

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Application Information

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IPC IPC(8): G01N1/28
Inventor 赵欣丁宝国单艳红冯艳红应蓉蓉孔令雅林玉锁郑丽萍李群周艳
Owner NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA
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