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Method for rapidly determining trace quantity of thallium in drinking water

A technology for rapid determination and drinking water, applied in the measurement of color/spectral characteristics, etc., can solve the problems of expensive equipment, many interference factors of electrochemical methods, low detection limit, etc., to shorten the detection time, shorten the detection time, and reduce the number of chemical reagents. Effect

Active Publication Date: 2013-08-07
CHONGQING UNIV +1
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  • Abstract
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Problems solved by technology

The principle of spectrophotometric measurement of thallium is to use azo dye color reagent, chlorpromazine hydrochloride and other amine color reagents to complex with thallium ions to form colored substances, and then colorimetrically quantify. This method has high accuracy in determining thallium. Wide range, suitable for constant and semi-micro analysis of thallium, while the determination of trace thallium requires a large amount of organic reagent extraction, which is easy to endanger operators and the environment, and the method interferes seriously; the electrochemical method has many interference factors, poor reproducibility, and stability Inductively coupled plasma mass spectrometry (ICP-MS) is a new testing technology developed in the 1980s, because of its extremely low detection limit, extremely wide dynamic linear range, multi-element It has been widely used due to its analytical and isotope analysis capabilities. Using inductively coupled plasma mass spectrometry, it is possible to easily measure thallium without any enrichment technology. This method has fast detection, high sensitivity, and strong anti-interference ability, and is widely used in geology and the environment. The detection of thallium in medium, but ICP-MS itself is expensive in equipment, high in operation and maintenance costs, and has high requirements for operators, so it is difficult to popularize
The atomic absorption method has become the recommended determination method in the national standard (GB / T 5750.6-2006) due to its advantages of rapidity, sensitivity, good anti-interference, good selectivity, less sampling volume, and low instrument cost. However, the national standard recommends "no "Flame atomic absorption spectrophotometry" still has certain defects, such as the large sample demand of at least 500ml, and the determination of water samples requires pretreatment such as coprecipitation and enrichment, which is not only complicated to operate, but also takes a long time for pretreatment (overnight) , and the sample repeatability is poor, the standard addition recovery rate is low, especially at low concentrations, and the use of a large amount of chemicals is likely to cause secondary pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: A method for rapid determination of trace thallium in drinking water, comprising the steps of:

[0029] (1) Water sample collection, transportation and storage: Take 100 ml of factory water from a waterworks, add 0.1 ml of high-grade pure concentrated nitric acid to make the pH value <2, and then add a certain amount of thallium standard solution to make the The concentration of thallium in the water sample is 0.0001 mg / L, and this solution is used as the target water sample to be tested. The target water sample to be tested should be stored at 4°C for no more than 7 days;

[0030](2) Draw the standard curve of thallium absorbance: quantify by external standard method, dilute the thallium standard stock solution purchased from the National Standard Material Center from 100 mg / L to 0.02 mg / L as the standard solution, and then use the standard solution to prepare The concentrations of thallium are: 0 mg / L, 0.0005 mg / L, 0.001 mg / L, 0.002 mg / L, 0.004 mg / L, 0.008...

Embodiment 2

[0039] Example 2: A method for rapid determination of trace thallium in drinking water, comprising the steps of:

[0040] (1) Water sample collection, transportation and storage: Take 100 ml of factory water from a waterworks, add 0.1 ml of high-grade pure concentrated nitric acid to make the pH value <2, and then add a certain amount of thallium standard solution to make the The concentration of thallium in the water sample is 0.0002 mg / L, and this solution is used as the target water sample to be tested. The target water sample to be tested should be stored at 4°C for no more than 7 days;

[0041] (2) Draw the standard curve of thallium absorbance: quantify by external standard method, dilute the thallium standard stock solution purchased from the National Standard Material Center from 100 mg / L to 0.02 mg / L as the standard solution, and then use the standard solution to prepare The concentrations of thallium are: 0 mg / L, 0.0005 mg / L, 0.001 mg / L, 0.002 mg / L, 0.004 mg / L, 0.0...

Embodiment 3

[0050] Example 3: A method for rapid determination of trace thallium in drinking water, comprising the steps of:

[0051] (1) Water sample collection, transportation and storage: Take 100 ml of factory water from a waterworks, add 0.1 ml of high-grade pure concentrated nitric acid to make the pH value <2, and then add a certain amount of thallium standard solution to make the The concentration of thallium in the water sample is 0.0005 mg / L, and this solution is used as the target water sample to be tested. The target water sample to be tested should be stored at 4°C for no more than 7 days;

[0052] (2) Draw the standard curve of thallium absorbance: quantify by external standard method, dilute the thallium standard stock solution purchased from the National Standard Material Center from 100 mg / L to 0.02 mg / L as the standard solution, and then use the standard solution to prepare The concentrations of thallium are: 0 mg / L, 0.0005 mg / L, 0.001 mg / L, 0.002 mg / L, 0.004 mg / L, 0.0...

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Abstract

The invention relates to a method for rapidly determining trace quantity of thallium in drinking water, which comprises the following steps: (1) acquiring, transporting and storing water sample; (2) drafting thallium absorbance standard curves: preparing standard series solutions, and then detecting absorbance of each solution of the standard series solutions by a graphite oven, and drafting thallium absorbance standard curves; (3) continuously enriching-determining the object sample to be detected on-line, condensing the object sample to be detected, and detecting the absorbance by a graphite oven; (4) calculating the thallium quality concentration of the object sample to be detected. The used reagent and operation process does not produce secondary pollution, and the detection limit can reach 0.00005 mg / L, and the detection reappearance is controlled within 5%, and the recovery rate reaches to 75-110%, and satisfies the thallium content limit value detection in drinking water GB / T5749-2006.

Description

technical field [0001] The invention relates to a method for determining trace thallium in water, in particular to a method for rapidly determining trace thallium in drinking water. [0002] Background technique [0003] Thallium (Tl) is a typical dispersed element, which is widely used in superconducting materials, high-energy physics, aerospace, military industry and other fields, but it is also a typical toxic element, and its toxicity is far higher than that of Cd, Pb, Hg, etc. Thallium is mainly distributed in potassium minerals and minerals, such as mica, showing lithophilic characteristics; at the same time, thallium is also widely distributed in sulfides, forming symbiotic combinations with Zn, Fe, As, etc., showing sulfophilic characteristics. The continuous development and utilization of mineral resources by humans and natural mineralization have exposed these minerals to the surface. Under epigenetic geological processes, Tl in them is easily released, enters the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31
Inventor 刘力维郑怀礼叱干勇唐晓旻肖浪许志楠车飞
Owner CHONGQING UNIV
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