Extraction and detection methods for mercury compounds in sediments

An extraction method and technology of mercury compounds, applied in the field of environmental analytical chemistry, can solve the problems of cumbersome extraction process, easy conversion of mercury forms, long extraction time, etc., and achieve high enrichment multiples, environmental friendliness, and good extraction effect

Active Publication Date: 2015-06-03
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the problems of poor extraction effect, insufficient sensitivity, cumbersome extraction process, long extraction time, easy conversion, loss, contamination of mercury form, and high toxicity of the extractant in the prior art, the present invention aims to provide a method with good extraction effect, High enrichment multiple, simple, fast, and environmentally friendly extraction method for mercury compounds in sediments, and provides a stable and sensitive detection method for mercury compounds in sediments

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  • Extraction and detection methods for mercury compounds in sediments
  • Extraction and detection methods for mercury compounds in sediments
  • Extraction and detection methods for mercury compounds in sediments

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Experimental program
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Effect test

Embodiment 1

[0029] Embodiment 1 Screening of various process parameters in the extraction method of the present invention

[0030] The method of the screening experiment of this embodiment is carried out according to the following steps: a, take the sediment sample spiked, add complexing agent, shake, carry out complexation reaction, obtain complex compound, centrifuge, remove supernatant; b, take The supernatant in step a is added to the ionic liquid, shaken, centrifuged, and the sedimentary phase at the bottom is taken as the extract enriched in mercury compounds.

[0031]After that, it is detected by high performance liquid chromatography-cold atomic fluorescence spectrometry system, and the recovery rate of standard addition is calculated to obtain the extraction effect under different process parameters. The specific detection conditions are:

[0032] The chromatographic column of high performance liquid chromatography is a C18 chromatographic column, and the flow rate is 2.0mL min ...

Embodiment 2

[0059] Embodiment 2 The extraction method of mercury compound in the deposit of the present invention

[0060] Accurately weigh 0.2g of the sediment sample in a 25mL conical test tube, add 5mL of 0.004% (m / v) complexing agent dithizone, after mixing, add 0.05mol L -1 nitric acid and sodium hydroxide to adjust the pH to 4.5. Then the sample is placed on a vortex shaker and shaken at a rate of 2800rpm for 1min. At this time, methylmercury, ethylmercury and inorganic mercury in the sample undergo a complexation reaction with dithizone to generate corresponding complexes. The samples were then placed in a centrifuge and centrifuged at 3000 rpm for 5 min. After centrifugation, take 4 mL of supernatant to a 25 mL conical test tube, slowly add 60 μL of ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate, then place the sample on a vortex shaker and shake at 2800 rpm 1min, after the extraction is complete, the sample is placed in a centrifuge and centrifuged at 3000rpm for ...

Embodiment 3

[0061] Embodiment 3 The detection method of mercury compound in sediment of the present invention

[0062] (1) Preparation of mercury compound standard solution:

[0063] Methylmercury and ethylmercury standard solution: Accurately weigh 0.1g of methylmercury chloride standard and 0.1g of ethylmercury chloride standard in a 250mL beaker, then add methanol to dissolve it, and finally transfer to a 100mL brown volume Store in the bottle for later use, the concentration of methylmercury and ethylmercury standard solution is 10mg / L (calculated as methylmercury chloride and ethylmercury chloride).

[0064] Inorganic mercury standard solution: Accurately pipette 1mL of 1000mg / L Hg(II) stock solution into a 100mL brown volumetric flask for later use, and use 2% (v / v) nitric acid to make up the volume, the concentration of inorganic mercury standard solution is 10mg / L (with mercury meter).

[0065] Take 1mL of the methylmercury, ethylmercury and inorganic mercury standard solutions ob...

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Abstract

The invention provides an extraction method for mercury compounds in sediments. The extraction method comprises the following steps: adding a complexing agent into the sediments, and carrying out complexing reaction, thereby obtaining complex; and centrifuging, taking out supernatant liquor, adding ion liquid, oscillating, centrifuging, and taking sedimentary facies at the bottom, i.e., extracts containing rich mercury compounds. The extraction method utilizes the ion liquid to extract the mercury compounds in the sediments, so that the extraction effect is good, the enrichment multiple is high, and the extraction method is simple, fast and environmental-friendly. The invention also provides a detection method for the mercury compounds in the sediments. According to the detection method, pretreatment is carried out on the sediments according to the extraction method provided by the invention, and then the obtained extracts are detected by combined use of high-performance liquid chromatography and cold atomic fluorescence spectrometry. The detection method has the advantages of fastness, accuracy, stability, sensitivity and the like and is applicable to daily environmental monitoring.

Description

technical field [0001] The invention belongs to the technical field of environmental analysis chemistry, in particular to a method for extracting and detecting mercury compounds in sediments. Background technique [0002] The toxicity, bioavailability, migration and re-migration of mercury are closely related to its chemical form. Therefore, the rapid and accurate acquisition of mercury chemical form information has become a research focus and hot spot in many fields. Water system sediments are the ultimate receptors of mercury pollutants, and are considered to be excellent indicators of environmental pollution, and different forms of mercury can be transformed into each other under the action of microorganisms. Therefore, the accurate and efficient analysis of mercury species in water system sediments is of great significance. [0003] Mercury exists mainly in the form of inorganic mercury and organic mercury in sediments. Inorganic mercury is mainly in the form of divale...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/14G01N30/02
Inventor 冷庚
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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