Sample preparation method and detection method for water-soluble heavy metal elements in solid waste

A detection method and solid waste technology, applied in the field of analytical chemistry, can solve the problems of high technical requirements, high reagent consumption, and long cycle of using cost inspection conditions, and achieve low requirements for analytical equipment performance and experimental conditions, and the lower limit of quantitative determination The effect of low cost and low measurement cost

Inactive Publication Date: 2016-09-07
PANGANG GROUP RESEARCH INSTITUTE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The main technical shortcomings of the existing detection methods include: Although the technical performance indicators such as sensitivity and detection limit of the ICP-MS method are superior to the conventional ICP-OES method, the purchase price of the detection instrument is much higher than that of the ICP-OES method. , and its use cost and technical requirements for inspection conditions are relatively high, and it usually needs to be equipped with expensive special clean laboratories, as well as the maintenance of equipment and clean rooms, and the cost of parts such as sampling cones and consumables is very high. This has led to an increase in the cost of detection and analysis, which has affected the popularization of analytical methods
Ordinary laboratories that are not equipped with high-end instruments such as ICP-MS usually use the HG-AFS detection method to conduct Hg, Cd, Pb, As, Se, Zn and other harmful heavy metal elements that can produce hydride reactions with reducing agents such as potassium bor...

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  • Sample preparation method and detection method for water-soluble heavy metal elements in solid waste
  • Sample preparation method and detection method for water-soluble heavy metal elements in solid waste

Examples

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preparation example Construction

[0024] The preparation method of the water-soluble heavy metal element sample in the solid waste of the present invention comprises the following steps:

[0025] a. Add water-soluble heavy metal element extractant pure water to the solid waste to be tested; according to the solid-liquid ratio, the solid waste to be tested: pure water=1:2~2.5g / mL;

[0026] b. Add a neutral oxidizing atmosphere protective agent, and continuously oscillate and extract on an oscillator for 4-6 hours;

[0027] c, filter, take the filtrate, remove the insoluble solids in the solution, add an oxidizing strong acid solution to the filtrate, supplement and add a neutral oxidizing atmosphere protective agent, to obtain a mixed solution;

[0028] d. Put the mixed solution on a low-temperature electric heating plate or a hot water bath, let it evaporate and concentrate in a sub-boiling state, cool to room temperature, dilute it with water, and set the volume in a small-volume container to obtain water-sol...

Embodiment 1

[0054] 1. Preparation of sample solution for titanium chloride extraction tailings

[0055] Weigh 50g of titanium chloride extraction tailings sample (Sample No. 1) into a conical flask, add 100g (or mL) of water and 5mL of hydrogen peroxide, place on a shaker and continuously vibrate for extraction for 4 hours; filter and discard the solution Medium-insoluble solid, the filtrate is collected in a wide-mouth container, add 5mL concentrated nitric acid and 3mL hydrogen peroxide respectively, place it in a hot water bath and keep it in a sub-boiling heating state at 80°C, continue to evaporate and concentrate the solution to about 3mL, and cool to room temperature Afterwards, dilute with water to a constant volume in a 5mL colorimetric tube and mix well.

[0056] 2. Use ICP-OES to determine the content of heavy metal elements in the sample solution of titanium chloride extraction tailings

[0057] Using Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-OES) as a dete...

Embodiment 2

[0061] Weigh 100g of titanium chloride extraction tailings sample (Sample No. 2), add 250g (or mL) of water and 10mL of hydrogen peroxide, shake and extract for 6 hours; add 10mL of concentrated nitric acid and 6mL of hydrogen peroxide to the filtrate collected by filtration , sub-boiling evaporation to concentrate the solution to about 5mL, after cooling, dilute with water to volume and mix in a 10mL colorimetric tube.

[0062] In addition, the sample solution of the titanium chloride extraction tailings was prepared according to the same method as that of Example 1, and the content of heavy metal elements contained in the solution was determined by ICP-OES.

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Abstract

The invention specifically relates to a sample preparation method and detection method for water-soluble heavy metal elements in solid waste, belonging to the technical field of analytical chemistry. The method comprises the following steps: a, adding pure water into to-be-detected solid waste; b, adding a neutral oxidizing atmosphere protective agent and carrying out vibrating extraction for 4 to 6 h; c, carrying out filtering, taking filtrate and adding an oxidizing strong acid solution and the neutral oxidizing atmosphere protective agent into the filtrate so as to obtain a mixed solution; and d, maintaining the mixed solution in a sub-boiling state and then successively carrying out evaporative concentration, cooling to room temperature, dilution and volume fixation. The methods provided by the invention have the characteristics of easy operation, a few steps, low requirements on the performance of analysis equipment and experimental condition, small usage amounts of reagents, capacity of simultaneous determination of multiple elements, low quantitative determination lower limit, high precision, etc. and totally meet technical needs for accurate determination of water-soluble heavy metal elements like Hg, Cd, Pb, As, Se, Be, Cr, Cu, Zn and Ni in antimony titanium chloride tailings in an analysis laboratory with common equipment and conditions.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a sample preparation method and detection method of trace or trace elements in solid waste, in particular to a sample preparation method and detection method of water-soluble heavy metal elements in tailings of titanium chloride extraction method. Background technique [0002] The titanium extraction process by the chloride method is the main technology for the production of titanium products. The key is to firstly mix the raw materials such as titanium concentrate and titanium slag with a carbon-containing reducing agent, and then carry out high-temperature smelting to reduce iron oxides to achieve separation of iron and titanium, and then through boiling chlorine Crude titanium tetrachloride is obtained by chemical and other treatment processes, and the refined titanium tetrachloride after purification and removal of impurities is used to manufacture sp...

Claims

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Application Information

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IPC IPC(8): G01N21/71G01N1/38G01N1/40
CPCG01N1/38G01N1/4022G01N21/71G01N2001/4027
Inventor 成勇
Owner PANGANG GROUP RESEARCH INSTITUTE CO LTD
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