Determination method for trace thallium in high-salt waste water

A technology of high-salt wastewater and determination method, which is applied in the field of heavy metal detection, can solve the problems of expensive equipment investment and operation cost, low detection limit, spray rate reduction, etc., and achieve the effect of low detection and operation cost

Active Publication Date: 2016-03-30
HUNAN BRUNP RECYCLING TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most of the spectrophotometric methods are determined by the means of separation and enrichment of organic solvents, which are mainly suitable for the analysis of constant and semi-trace thallium in water, but their sensitivity is low; electrochemical methods have many interference factors, poor stability and reproducibility; electrothermal atomic absorption Spectrometry (ETAAS) has high sensitivity, less sampling, and is easy to operate, but it is seriously interfered by the matrix; mass spectrometry ICP-MS is a plasma mass spectrometry test technology developed in the 1980s, which provides extremely low detection limited, extremely wide dynamic range, simple spectral lines, less interference, high analysis precision, fast analysis speed, strong anti-interference ability, and high sensitivity, it is widely used in the detection of thallium in geology and the environment, but when it is used When detecting thallium in high-salt wastewater: there is noise and background drift...

Method used

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  • Determination method for trace thallium in high-salt waste water
  • Determination method for trace thallium in high-salt waste water
  • Determination method for trace thallium in high-salt waste water

Examples

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Effect test

Embodiment 1

[0045] A method for detecting trace thallium in high-salt wastewater, comprising the following steps:

[0046] (1) Wastewater collection, transfer and storage: Take 200mL of wastewater from a factory in the hydrometallurgical industry (sodium content is 40g / L, thallium content is 8.10μg / L), seal it, and analyze it; if it cannot be analyzed in time, add nitric acid Acidify, adjust the pH to 1, and then store it below 4°C for no more than 5 days; when measuring, adjust the pH of the high-salt wastewater sample to 3.82 with ammonia water, and then extract; the mass fraction of the nitric acid is 65% ;

[0047] (2) Sample pretreatment:

[0048] ① Transfer the water sample from the sampling bottle to a 500mL beaker, and rinse the polyethylene bottle twice with 10mL of pure water each time, pour the rinsed water into the transferred water sample in turn, and mix well; The pH of the water sample adjusted by ammonia water is 3.82;

[0049]②Use 100mL of the saponified organic phase ...

Embodiment 2

[0062] A method for detecting trace thallium in high-salt wastewater, comprising the following steps:

[0063] (1) Wastewater collection, transfer and storage: Take 400mL of wastewater samples (sodium content is 5g / L, thallium content is 0.52μg / L) outside the sewage treatment station of a factory in the hydrometallurgical industry, seal it, and analyze it; The effluent waste water is the waste water after removing heavy metals from the raffinate waste water and adjusting the value through sand filtration; if it cannot be analyzed in time, add nitric acid to acidify, adjust the pH to 2, and then store it below 4°C for no more than 5 days; when measuring , adjusting the pH of the high-salt wastewater sample to 3.95 with ammonia water, and then extracting; the mass fraction of the nitric acid is 98%;

[0064] (2) Sample pretreatment:

[0065] ① Transfer the water sample from the sampling bottle to a 1000mL beaker, and rinse the polyethylene bottle 3 times with 10mL of pure water...

Embodiment 3

[0079] A method for detecting trace thallium in high-salt wastewater, comprising the following steps:

[0080] (1) Wastewater collection, transfer and storage: Take a 300mL sample of wastewater from a factory in the hydrometallurgical industry (with a sodium content of 0.5g / L and a thallium content of 0.1μg / L), seal it, and analyze it; if it cannot be analyzed in time, add Acidify with nitric acid, adjust the pH to 1.5, and then store at below 4°C for no more than 5 days; when measuring, adjust the pH of the high-salt wastewater sample to 3.5 with ammonia water, and then extract; the mass fraction of the nitric acid is 80 %;

[0081] (2) Sample pretreatment part:

[0082] ① Transfer the water sample from the sampling bottle to a 500mL beaker, and rinse the polyethylene bottle twice with 10mL of pure water each time, pour the rinsed water into the transferred water sample in turn, and mix well; The pH of the water sample adjusted by ammonia water is 3.5;

[0083] ②Use 100mL ...

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Abstract

The invention specifically relates to a determination method for trace thallium in high-salt waste water, which belongs to the technical field of heavy metal detection. The determination method for trace thallium in high-salt waste water comprises the following steps: (1) pretreating a waste water sample by using a continuous impurity removal and enrichment method consisting of procedures of extraction, washing, reverse extraction, pH value adjustment of an extraction solution, extraction, washing and reverse extraction; (2) drafting a standard work curve of thallium; (3) detecting the absorbance of the pretreated to-be-detected waste water sample through graphite furnace atomic absorption; and (4) calculating the concentration of the sample according to standard absorbance-concentration relation. According to the invention, extractant used in the method is regenerable and reusable; an added-standard recovery rate reaches 98 to 102%, and a detection limit value is up to 0.1 [mu]g/L, so emission standard detection requirements on thallium in industrial waste water are met; and a blank in determination methods for trace thallium in high-salt waste water is filled in.

Description

technical field [0001] The invention belongs to the technical field of heavy metal detection, and in particular relates to a method for determining trace thallium in high-salt wastewater. Background technique [0002] Thallium (Tl) is a typical, highly dispersed rare heavy metal element that is both lithophilic and sulfophilic in geochemistry and crystallography. According to reports, the annual production and use of thallium in the world is less than 15 tons, and the annual production of thallium by industry is about 2000-5000 tons, which is far greater than the demand, so there is no market condition for making products. At present, 56 kinds of thallium minerals have been reported in the world, and these minerals are mainly associated with other mines, especially sulfide ores. Besides iron oxide ore, the iron that we demand the most is pyrite; while non-ferrous metals such as copper, lead, zinc, antimony, nickel (associated in copper) and other non-ferrous metals that are...

Claims

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Application Information

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IPC IPC(8): G01N21/31
CPCG01N21/3103
Inventor 刘勇奇谭群英刘少葵唐红辉张敏孔水莲
Owner HUNAN BRUNP RECYCLING TECH
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