Method for detecting low-concentration methyl mercury

A methylmercury, low-concentration technology, applied in the field of heavy metal detection, can solve problems such as poor enrichment effect and content influence, achieve excellent selectivity and improve enrichment efficiency.

Active Publication Date: 2021-09-14
CHONGQING THREE GORGES UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The precipitation method is through the precipitant and Hg 2+ The reaction generates a precipitate to achieve the purpose of separating it from the sample liquid to be tested, but this method is effective in removing Hg 2+ At the same time, the CH 3 Hg + The content has a certain influence
Secondly, solid-phase microextraction (SPME) is a kind of sample pretreatment method that follows green chemical principle, as the solid-phase microextraction probe of the nano-gold modified wooden stick prepared in CN109187775A, is suitable for detecting the Hg in the water body 2+ , the detection limit of mercury is 0.06 μg / L, but the probe for CH 3 Hg + The enrichment effect is poor, so it is necessary to prepare a more suitable CH 3 Hg + Enrichment detection solid-phase microextraction sampler to improve detection efficiency

Method used

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  • Method for detecting low-concentration methyl mercury
  • Method for detecting low-concentration methyl mercury
  • Method for detecting low-concentration methyl mercury

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A method for detecting low-concentration methylmercury, carried out as follows:

[0045] Step 1. Preprocessing:

[0046] Take the ammonium sulfide solution with a concentration of 5mmol / L and add it to the water sample to be tested, let it stand for 20min, then centrifuge at 2000rpm for 20min, the volume ratio of the water sample to be tested and the ammonium sulfide solution is 1:0.02;

[0047] Step 2, preparation of Au-coated solid-phase microextraction sampler:

[0048] Take a birch wooden stick with a length of 2 cm and a tip diameter of 0.3 mm as a carrier in 0.5% KBH by volume fraction 4 Soak in the solution for 60 minutes, then immerse the wooden stick in the chloroauric acid solution with a concentration of 0.1mmol / L, let it stand for 50 minutes, and finally take it out and air-dry it at room temperature;

[0049] Step 3. Determination of methylmercury:

[0050] (1) Move the water sample to be tested after step 1 pretreatment to the headspace bottle, add 3.5%...

Embodiment 2

[0053] A method for detecting low-concentration methylmercury, carried out as follows:

[0054] Step 1. Preprocessing:

[0055] Take the ammonium sulfide solution with a concentration of 10mol / L and add it to the water sample to be tested, let it stand for 10min, then centrifuge at 20000rpm for 5min, the volume ratio of the water sample to be tested and the ammonium sulfide solution is 1:0.02;

[0056] Step 2, preparation of Au-coated solid-phase microextraction sampler:

[0057] Take a birch wooden stick with a length of 5 cm and a tip diameter of 0.5 mm as a carrier in a volume fraction of 5% KBH 4 Soak in the solution for 10 minutes, then immerse the wooden stick in the chloroauric acid solution with a concentration of 10mmol / L, let it stand for 20 minutes, and finally take it out and air-dry it at room temperature;

[0058] Step 3. Determination of methylmercury:

[0059] (1) Move the water sample to be tested after step 1 pretreatment to the headspace bottle, add 35% h...

Embodiment 3

[0062] A method for detecting low-concentration methylmercury, carried out as follows:

[0063] Step 1. Preprocessing:

[0064] Take the ammonium sulfide solution with a concentration of 1mol / L and add it to the water sample to be tested, let it stand for 15 minutes, and then centrifuge it at 12000rpm for 10 minutes. The volume ratio of the water sample to be tested and the ammonium sulfide solution is 1:0.02;

[0065] Step 2, preparation of Au-coated solid-phase microextraction sampler:

[0066] Take a birch wooden stick with a length of 3 cm and a tip diameter of 0.2 mm as a carrier in KBH with a volume fraction of 2%. 4 Soak in the solution for 40 minutes, then immerse the wooden stick in the chloroauric acid solution with a concentration of 2mmol / L, let it stand for 30 minutes, and finally take it out and air-dry it at room temperature;

[0067] Step 3. Determination of methylmercury:

[0068] (1) Move the water sample to be tested after step 1 pretreatment to the heads...

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Abstract

The invention relates to a method for detecting low-concentration methyl mercury. The method specifically comprises the following steps: firstly, adding an ammonium sulfide solution in the concentration of 5-10 mol/L into a water sample to be detected, sequentially carrying out static settlement and centrifugation according to the volume ratio of the water sample to the ammonium sulfide solution of 1: 0.02, then adding hydrochloric acid and potassium borohydride into the water sample to be detected, carrying out oscillation extraction at 45-70 DEG C by adopting an Au coated solid-phase microextraction sampler, and finally, transferring the extracted solid-phase micro-extraction sampler into a mercury measuring instrument, and measuring methyl mercury. According to the method disclosed by the invention, interference of mercury ions in detection is effectively removed, the enrichment efficiency of methyl mercury is improved, the detection of methyl mercury with lower concentration in a water body is realized, the detection limit is 0.02 mu g/L, a good linear relation is realized in a range of 0.2-10 mu g/L, and the detection method has excellent selectivity on methyl mercury.

Description

technical field [0001] The invention relates to the technical field of heavy metal detection, in particular to a method for detecting low-concentration methylmercury. Background technique [0002] Methylmercury (CH 3 Hg + ) is a highly lipophilic, highly neurotoxic organomercury compound with strong health and ecological risks. CH in water environment 3 Hg + Most of them are transformed from inorganic mercury under the action of microorganisms or chemical substances, and are amplified step by step along the food chain, eventually causing harm to human health. The "Minamata disease" in history is the human consumption of CH 3 Hg + A malignant disease caused by seafood polluting waters. Therefore, the detection of methylmercury has important practical significance for the protection of the ecological environment and human health. [0003] Existing CH 3 Hg + The detection means are separation instruments such as gas chromatography (GC), high performance liquid chromat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31G01N1/28G01N1/34G01N1/40
CPCG01N21/3103G01N1/28G01N1/34G01N1/40Y02A20/20
Inventor 马旭
Owner CHONGQING THREE GORGES UNIV
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