Method for determination of antimony in water sample
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A determination method and technology for water samples, which are applied in the direction of material excitation analysis, fluorescence/phosphorescence, etc., to achieve the effects of simple and easy method, high reproducibility and accurate measurement results.
Inactive Publication Date: 2013-06-05
SHANXI DATONG UNIV
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[0004] The present invention provides a new method for the determination of antimony in water samples in order to solve the problem that various methods used for the determination of antimony in existing water samples have their own shortcomings.
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Embodiment 1
[0008] Embodiment 1: use antimony potassium tartrate and potassium pyroantimonate to be mixed with trivalent antimony and pentavalent antimony mixed solutions containing different concentrations, adopt the method of the present invention to measure, and the steps are as follows:
[0009] (1) Solution preparation:
[0010] A, preparation concentration is the citric acid solution of 40 g / l; B, preparation concentration is the sodium fluoride solution of 2 g / l; C, preparation concentration is the thiourea and ascorbic acid mixed solution of 100 g / l; D, preparation A mixed solution of 0.5% oxygen-containing potassium oxide and 2% potassium borohydride is used as a reactant for generating hydrides in an atomic fluorescence instrument;
[0011] (2) Drawing of standard curve: Accurately add 20, 40, 80, 100, 200, 400 μl of antimony standard solution to six 10 ml volumetric flasks, respectively add 1 ml of the mixture of thiourea and ascorbic acid in step (1) Solution, 1.7 ml concentr...
Embodiment 2
[0017] Example 2: Add a series of interfering ions, Mn(II), Cu(II), Fe to the mixed solution of trivalent antimony (10 μg / l) and pentavalent antimony (10 μg / l) in Example 1 (Ⅲ), Co(II), then measure according to the method described in Example 1, and the assay results are as follows:
[0018] Table 2 Effect of interfering ions on the determination of trivalent antimony and pentavalent antimony
[0019]
Embodiment 3
[0020] Embodiment 3: In order to determine the optimal reaction condition of masking agent, the final concentration of masking agent in the water sample and the concentration of hydrochloric acid have been done the selection of optimum condition when measuring, and concentration described in embodiment 1 is 10 μ g / l In the solutions of trivalent antimony and pentavalent antimony, masking agents of different concentrations were added respectively, and then concentrated hydrochloric acid was added to make the final concentration of hydrochloric acid 2 M. Coordinates, taking the absorbance as the ordinate, draw a curve, add the result of citric acid masking agent, add the result of sodium fluoride masking agent, it can be seen that the optimal use concentration range of the two combined as masking agent should be 0.03 in citric acid ~0.09% (mass volume concentration), sodium fluoride is 0.04% ~ 0.08% (mass volume concentration), respectively corresponding to the initial concentrat...
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Abstract
The invention relates to a method for measuring trace chemicals in water, particularly provides a method for determination of antimony in a water sample, and aims at solving the problems that existing methods for the determination of the antimony have respective shortcomings. The method for the determination of the antimony in the water sample includes that a solution of citric acid, a solution of sodium fluoride, a mixed solution of thiourea and ascorbic acid and a mixed solution containing oxygen hydroxide and potassium borohydride are prepared; the concentration of the antimony in a standard solution is used as a horizontal coordinate, and the fluorescence intensity is used as a vertical coordinate so that a standard curve can be drawn; the mixed solution of the thiourea and the ascorbic acid, and a solution of concentrated hydrochloric acid are sequentially added into the water sample containing the antimony, and an atomic fluorescence spectrometer (ASF) is used for measuring the concentration of total antimony in the water sample; the solution of citric acid, the solution of sodium fluoride, and the solution of concentrated hydrochloric acid are sequentially added into the water sample containing the antimony, and the ASF is used for measuring the concentration of trivalent antimony in the water sample; and the concentration of pentavalent antimony is obtained by subtracting the measured concentration of the trivalent antimony from the measured concentration of the total antimony. The solution of citric acid and the solution of sodium fluoride are utilized as combined masking agents, the pentavalent antimony and other interfering ions in the water sample can be well masked, the determination result of the trivalent antimony is enabled to be very accurate, and therefore the method for the determination of the antimony in the water sample is simple, easy to implement, accurate in determination result, and high in reproducibility.
Description
technical field [0001] The invention relates to a method for measuring trace chemical substances in water quality, in particular to a method for measuring antimony in water samples. Background technique [0002] Antimony (Sb) is a toxic element widely distributed in nature. Antimony and its compounds are widely used in modern industry, mainly for the production of ceramics, glass, batteries, paints, pyrotechnic materials and flame retardants. , where the main use of antimony is to make flame retardants. The pure metal antimony is commonly used in the manufacture of semiconductors, infrared detectors and diodes. The common antimony trivalent compound potassium oxystimony tartrate and the pentavalent antimony compound sodium antimony gluconate are widely used as insect repellants. At present, there are about 14,000 tons of antimony products in the world every year. These antimony-containing products are eventually discarded into the environment after losing their use value, ...
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