Method for simultaneous enrichment and analysis of heavy metal lead, cadmium and mercury ions

A technology of enrichment and mercury ions, which is applied in the direction of material analysis, analysis materials, and test sample preparation using wave/particle radiation, which can solve the inability to realize the detection and analysis of various heavy metals, limited detection sensitivity, and detection method equipment requirements advanced questions

Inactive Publication Date: 2015-01-14
ELECTROMECHANICAL PRODS DETECTING TECH CENT OF SHANGHAI ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The invention solves the defects of limited detection sensitivity in the detection method of the prior art, the detection method has high requirements on equipment, and cannot realize the d

Method used

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  • Method for simultaneous enrichment and analysis of heavy metal lead, cadmium and mercury ions
  • Method for simultaneous enrichment and analysis of heavy metal lead, cadmium and mercury ions
  • Method for simultaneous enrichment and analysis of heavy metal lead, cadmium and mercury ions

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Embodiment 1

[0030] The method of the present invention includes the following experimental steps, and the conditions are optimized results. The present invention uses two heavy metal complexing agents, namely dithizone (HDZ) and sodium diethyldithioformate (DDTC).

[0031] The experimental procedure that adopts dithizone to implement the method of the present invention is as follows: first, will contain the Pb of 1mg / L concentration 2+ , Cd 2+ , Hg 2+ After the pH value of the water sample was adjusted to 4.0, a 5 mL volume of water sample was taken out and added to a centrifuge tube (as shown in Figure 1a). Then, mix 50 μL dithizone solution of tetrachlorethylene (the concentration of dithizone is 0.1% mass fraction) and 500 μL acetone (as a dispersant, methanol, ethanol, etc. can also be used, which are easily soluble in water, and also mixed with tetrachloroethylene). Miscible reagents) after mixing, use a disposable syringe to quickly add the mixture to the water sample, and immedi...

Embodiment 2

[0038] The steps to create a standard curve are:

[0039] Add 5mL water samples with a pH value of 4.0 to six 25mL glass centrifuge tubes, in which Pb 2+ , Cd 2+ , Hg 2+ The concentrations are 0, 0.2, 0.5, 1.0, 1.5, 2.0mg / L respectively;

[0040] (1) Operate according to the steps of Example 1 to prepare two sets of standard solutions of tetrachlorethylene with HDZ and DDTC as complexing agents;

[0041] (2) Take 20 μL of the tetrachlorethylene phase, place it in the XRF sample cell, and perform a full-spectrum scan at a voltage of 1000 mV, and the scan time is 100 s. Read the Lα of Pb, Kα of Cd, and Kα of Hg spectrum peak response value, and make a standard curve, see image 3 , Figure 4 shown;

[0042] Among them, dithizone and DDTC were purchased from Sigma company, Pb(NO 3 ) 2 , Cd(NO 3 ) 2 The solid was also purchased from Sigma Company, prepared into a 1000mg / L stock solution with ultrapure water (18MΩ), and diluted when used. Hg 2+ The standard solution w...

Embodiment 3

[0047] Example 3: Soluble Pb in toy samples 2+ , Cd 2+ , Hg 2+ Determination of ions

[0048] Reference standard: EN71-3:1994+A1:2001

[0049] This embodiment shows the situation when the sample to be tested is a toy, and all accessible parts on the toy sample are tested.

[0050] sample

[0051] For toys such as textile fabrics, plastic or rubber, use scissors or pliers to cut the material into small pieces of 5mm×5mm as the samples to be tested.

[0052] For toys with paint, ink or similar coatings, use a clean razor blade to scrape off the part as the sample to be tested.

[0053] For toys that are liquid paint or ink, take a part of the paint and apply it on a clean glass plate, let it dry naturally at room temperature, and then scrape it off as the sample to be tested. If the sample to be tested cannot be dried at room temperature, it should be dried in an oven according to the temperature used, and scraped off to obtain the sample to be tested.

[...

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Abstract

The invention relates to the field of detection and analysis of heavy metal ions in water solution, and particularly discloses a method for simultaneous enrichment and analysis of heavy metal lead, cadmium and mercury ions, which adopts diethyl disulfide sodium formate or dithizone as a complexing agent, so as to realize complexation with the lead, cadmium and mercury ions to form metal complex, wherein the metal complex is extracted and enriched through the dispersive liquid phase micro-extraction technology, and qualitative and quantitative analysis is simultaneously performed on the lead, cadmium and mercury ions in the water solution through the X-ray fluorescence spectrum technology. The enrichment multiples of the lead, cadmium and mercury ions in the water solution are high, the enrichment is complete, the operation is simple and quick, and the simultaneous qualitative and quantitative analysis on the lead, cadmium and mercury ions is realized.

Description

technical field [0001] The invention relates to the field of detection and analysis of heavy metal ions in aqueous solution, in particular to a method for simultaneously enriching and analyzing heavy metal ions lead, cadmium and mercury. Background technique [0002] The hazards of heavy metal elements in articles and the environment are increasingly recognized by the whole society, and hot-spot hazard incidents emerge in endlessly, such as the incidents of blood lead exceeding the standard in many areas. Among the heavy metal elements in the environment, lead, cadmium and mercury are the most harmful, and they are also the most recognized by the society, and there are many detection methods and standards. Due to the close contact with children in children's products, the heavy metals contained in them can bring harmful elements into the human body through some children's behaviors such as sucking, touching, and swallowing. Heavy metals can accumulate in the body for a long ...

Claims

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Application Information

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IPC IPC(8): G01N23/223G01N1/40
Inventor 于文佳戴雪伟郑翊高欢林莉卫碧文
Owner ELECTROMECHANICAL PRODS DETECTING TECH CENT OF SHANGHAI ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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