CN107328762B - Method for measuring contents of lead and cadmium elements in silver ornaments - Google Patents
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Abstract
The invention relates to determination of lead and cadmium elements in silver ornaments, belonging to the field of noble metal analysis. A method for measuring the contents of lead and cadmium elements in a silver ornament comprises the following steps: dissolving a silver sample to be detected by using nitric acid to obtain a silver nitrate solution; then adding a thiocyanate solution into the silver nitrate solution to completely precipitate silver nitrate into silver thiocyanate; finally, filtering to remove the silver thiocyanate precipitate, and taking the filtrate to determine the content of the lead and the cadmium elements. The potassium thiocyanate is used as a precipitator, so that the problem that the lead and cadmium elements cannot be accurately detected due to the adsorption effect of silver chloride precipitates on the lead and cadmium elements can be well solved, and the accurate determination of the content of the two elements of the silver ornament can be realized.
Description
Technical Field
The invention relates to a method for detecting the element content of a silver ornament, in particular to a method for measuring the content of lead and cadmium elements in the silver ornament.
Background
The lead and cadmium are common impurity elements of pure silver ornaments, and lead is relatively common and can be introduced from the exploitation of silver ores to the processing of the silver ores into ornaments. Cadmium elements are often added to the solder to reduce its melting point and fluidity. Lead and cadmium are harmful elements, lead can cause disorder of blood and nervous system, and lead exceeding standard of blood lead of children can be caused by wearing the lead-containing children ornaments for a long time, so that hyperactivity, mania and the like are caused. Cadmium causes poisoning, resulting in bone damage. The lead content in the ornaments is regulated to be not more than 1000mg/kg, the cadmium content is not more than 100mg/kg in the national standard GB 28480-2012, and the lead content and the cadmium content in the ornaments for children are not more than 90mg/kg and 75mg/kg respectively. At present, in the field of noble metal analysis, hydrochloric acid precipitation is used for removing a silver matrix, and inductively coupled plasma atomic emission spectrometry (ICP-AES) which has the advantages of simultaneous determination of multiple elements and high analysis speed is selected for determining the content of lead and cadmium in the silver ornaments. However, the literature reports that the silver chloride precipitate has strong adsorption capacity to lead and cadmium elements, which results in inaccurate detection results. Especially, the content of lead and cadmium elements in the silver ornaments for children is very low originally, and accurate data cannot be obtained even after the silver ornaments are adsorbed by silver chloride precipitation.
Therefore, it is necessary to improve the existing method for measuring the content of lead and cadmium elements in the pure silver ornaments.
Disclosure of Invention
The invention aims to solve the technical problem of providing the method for measuring the contents of the lead and cadmium elements in the silver ornaments, the method can effectively avoid the adsorption effect of silver chloride precipitates on the lead and cadmium elements, the operation is simple, the precision is high, and the accuracy of the measurement result is effectively improved.
A method for measuring the contents of lead and cadmium elements in a silver ornament comprises the following steps:
weighing a certain mass of ornament to be detected as a silver sample, and dissolving the ornament to be detected by nitric acid to obtain a silver nitrate solution;
and (2) adding a thiocyanate solution into the silver nitrate solution obtained in the step (1) to fully precipitate silver ions into silver thiocyanate.
And (3) filtering the silver thiocyanide precipitate obtained in the step (2) to obtain a solution to be detected.
Weighing pure silver with the same mass as that in the step (1), and dissolving the silver with nitric acid to obtain a silver nitrate solution;
and (4) adding a thiocyanate solution into the silver nitrate solution obtained in the step (4) to fully precipitate silver ions into silver thiocyanate.
And (4) filtering the silver thiocyanide precipitate obtained in the step (5) to obtain a filtrate as a correction solution.
And (4) adopting the correction solution obtained in the step (6), selecting the working conditions of an inductively coupled plasma atomic emission spectrometer (ICP-AES), sequentially testing the standard solution, the correction solution and the solution to be tested, measuring the contents of lead and cadmium elements in the filtrate to be tested obtained in the step (3), and calculating the contents of lead and cadmium elements in the silver ornaments.
In the step (1), the mass of the silver ornament to be measured weighed in each measurement is 0.25-1.00 g, preferably 400-600 mg.
The concentration of the nitric acid in the step (1) is 5-98 wt%, preferably 30-68 wt%, and more preferably 65-68 wt%.
The molar ratio of the silver to the nitric acid in the step (1) is 1: 4-100, and preferably 1: 4-30. The molar ratio range of the silver to the nitric acid is excessive, and the aim is that after the silver is completely dissolved by the nitric acid, part of the nitric acid is remained, so that the detection accuracy is improved.
The molar ratio of the silver ions to the thiocyanate in the step (2) is 1: 1 to 1.1; the thiocyanate is selected from potassium thiocyanate and sodium thiocyanate, and preferably potassium thiocyanate; the concentration of the thiocyanate solution is 0.10-0.50 g/L, preferably 0.20-0.30 g/L.
When the inductively coupled plasma emission spectrometer is used for measuring the contents of lead and cadmium elements in the filtrate, the characteristic wavelength for detecting the lead element is 220.353nm, and the characteristic wavelength for detecting the cadmium element is 226.502 nm.
Has the advantages that:
the invention provides a method for measuring the contents of lead and cadmium elements in silver ornaments, and the method has the advantages that when Pb and Cd element samples with the concentrations of 1 mu g/mL, 5 mu g/mL and 10 mu g/mL are measured, the standard addition recovery rate is 90-104%, the recovery rate is high, and the stability is good. The potassium thiocyanate is used as a precipitator, so that the problem that the lead and cadmium cannot be accurately detected by the national standard GB/T21198.5-2007 due to the fact that the silver chloride adsorbs the Pb and Cd elements can be well solved, the potassium thiocyanate can be used as a supplementary detection for a silver analysis method in the national standard, and the accurate determination of the content of each element of the silver ornament can be realized.
Drawings
FIG. 1 is a curve of lead and cadmium element concentration-normalized recovery rate in filtrate obtained by silver chloride precipitation in national standard GB/T21198.5-2007;
FIG. 2 is a relative standard deviation-concentration curve of the normalized recovery rate of the lead and cadmium element concentration determination in the filtrate obtained by silver chloride precipitation in the national standard GB/T21198.5-2007;
FIG. 3 is a curve of lead and cadmium element concentration-normalized recovery rate in filtrate obtained by precipitating silver ions with potassium thiocyanate according to the operation steps of the national standard GB/T21198.5-2007.
Detailed Description
The invention will be further elucidated with reference to the specific embodiments and the accompanying drawings.
Laboratory instruments and parameters
In the following examples, the contents of lead and cadmium in the solution were measured by using a Thermo IRIS inductively coupled ii inductively coupled plasma emission spectrometer. The wavelength of element selective analysis is: pb 220.353nm and Cd 226.502 nm.
Working conditions of the Thermo IRIS inductively coupled II plasma emission spectrometer are as follows: argon is more than or equal to 99.995 percent; argon supply pressure is 0.6 MPa; the atomization gas pressure was 30 psi; radio frequency power 1150W; cooling air flow: 15L/min; the auxiliary gas flow is 1.0L/min; the pumping speed of the peristaltic pump is 100 r/min; sample introduction and washing time is 30 s; integration time: visible light region 10s, ultraviolet light region 8 s.
Example 1: the adsorption experiment of silver chloride on lead and cadmium elements in the test method of national standard GB/T21198.5-2007.
Preparing a mixed standard solution with lead and cadmium contents of 50 mu g/mL, preparing a lead and cadmium mixed series standard solution with the concentrations of 0, 1.0, 2.0, 3.0, 5.0 and 10.0 mu g/mL by using the lead and cadmium mixed standard solution, performing computer measurement, selecting a proper curve equation, and establishing a working curve.
Preparing 50 mu g/mL silver-containing matrix solution by using nitric acid and high-purity silver (the silver content is higher than 99.99 wt%), measuring 10.00mL of the 50 mu g/mL silver-containing matrix solution, putting the 50 mu g/mL silver-containing matrix solution into a 50mL beaker, respectively adding 1.00 mL, 5.00 mL and 10.00mL of lead and cadmium element mixed series standard solutions, adding 15mL of concentrated nitric acid, and slowly heating to remove nitrogen oxides. Then slowly dripping 2mL of 37 wt% hydrochloric acid solution, standing for 2h to completely precipitate silver nitrate into silver chloride precipitate, filtering with slow filter paper to remove the silver chloride precipitate, transferring the filtrate into a 50mL volumetric flask, adding 15mL of concentrated hydrochloric acid, and shaking up with water to constant volume. The theoretical concentrations of lead and cadmium elements (without considering the adsorption effect of silver chloride on each element) after constant volume are 1 mug/mL, 5 mug/mL and 10 mug/mL respectively. And (3) the solution is placed on a plasma emission spectrometer and is operated according to the working conditions of the instrument to measure the concentration of the lead and the cadmium elements.
And repeating the experiment operation for 11 times, recording related data, and calculating the standard recovery rate of the lead and cadmium elements by combining the working curve. Wherein, the detection results of lead and cadmium filter solutions with the concentration of 1 mu g/mL are shown in the table 1; the detection results of lead and cadmium filtrates with the concentration of 5 mu g/mL are shown in Table 2; the results of measuring lead and cadmium filtrates at a concentration of 10. mu.g/mL are shown in Table 3. The concentration-normalized recovery rate curves corresponding to tables 1-3 are shown in the attached figure 1; the relative standard deviation-concentration curves corresponding to tables 1-3 are shown in figure 2;
table 1: standard recovery rate of lead and cadmium elements of 1 mu g/mL
Table 2: standard recovery rate of lead and cadmium elements of 5 mu g/mL
Table 3: standard recovery rate of lead and cadmium element of 10 mu g/mL
As shown by combining tables 1-3 and attached figures 1 and 2, for Pb and Cd elements, the concentrations of the Pb and Cd elements are 1 mug/mL, 5 mug/mL and 10 mug/mL respectively, the labeling recovery rate is low and changes greatly along with the concentrations, and the AgCl precipitation is proved to have strong adsorption capacity on Pb and Cd. For Pb and Cd elements, the concentrations are respectively 1 mug/mL, 5 mug/mL and 10 mug/mL, the RSD is respectively 37.1, 12.9 and 10.7, the change is large, and the AgCl precipitation is proved to have strong adsorption capacity on Pb and Cd, and the AgCl precipitation has large change and small change along with the change of the concentrations and is related to the precipitation amount of silver chloride.
Example 2: and (3) an experiment for determining the contents of lead and cadmium elements in the silver solution by using the thiocyanate solution.
Preparing a mixed standard solution with lead and cadmium contents of 50 mu g/mL, preparing a lead and cadmium mixed series standard solution with the concentrations of 0, 1.0, 2.0, 3.0, 5.0 and 10.0 mu g/mL by using the lead and cadmium mixed standard solution, performing computer measurement, selecting a proper curve equation, and establishing a working curve.
Preparing 50 mu g/mL silver-containing matrix solution by using nitric acid and high-purity silver (the silver content is higher than 99.99 wt%), measuring 10.00mL of the 50 mu g/mL silver-containing matrix solution, putting the 50 mu g/mL silver-containing matrix solution into a 50mL beaker, respectively adding 1.00 mL, 5.00 mL and 10.00mL of two element mixed series standard solutions, adding 15mL of concentrated nitric acid, and slowly heating to remove nitrogen oxides. Then slowly dripping 2mL of 0.25g/mL potassium thiocyanate solution, standing to ensure that silver nitrate is completely precipitated to be silver thiocyanate precipitate, filtering the silver thiocyanate precipitate by using slow filter paper to remove the silver thiocyanate precipitate, transferring the filtrate to a 50mL volumetric flask, adding 5mL of concentrated nitric acid, and shaking uniformly with water to constant volume. The theoretical concentrations of lead and cadmium elements (without considering the adsorption effect of the silver thiocyanate on each element) after constant volume are respectively 1 mug/mL, 5 mug/mL and 10 mug/mL. And (3) the solution is placed on a plasma emission spectrometer and is operated according to the working conditions of the instrument to measure the concentration of the lead and the cadmium elements.
And repeating the experiment operation, recording related data, and calculating the standard recovery rate of the lead and cadmium elements by combining the working curve. Wherein, the detection results of lead and cadmium filter solutions with the concentration of 1 mu g/mL are shown in the table 1; the detection results of lead and cadmium filtrates with the concentration of 5 mu g/mL are shown in Table 2; the results of measuring lead and cadmium filtrates at a concentration of 10. mu.g/mL are shown in Table 3. The concentration-normalized recovery rate curves corresponding to tables 4-6 are shown in the attached figure 3;
table 4: standard recovery rate of lead and cadmium elements of 1 mu g/mL
Table 5: standard recovery rate of lead and cadmium elements of 5 mu g/mL
Table 6: standard recovery rate of lead and cadmium element of 10 mu g/mL
Combining the attached figure 3 and tables 4-6, the measured standard addition recovery rate of Pb and Cd solutions with the concentrations of 1 mug/mL, 5 mug/mL and 10 mug/mL is 96-107%, and the recovery rate is high and stable. Indicating that the silver thiocyanate precipitate has a weak and stable adsorption capacity for both elements. The potassium thiocyanate is used as a precipitator, so that the problem that the contents of lead and cadmium cannot be accurately detected due to the adsorption effect of silver chloride can be well solved, and the method can be used for supplementing the regulation of the national standard GB/T21198.5-2007 on the purity analysis method of the silver ornament.
Claims (9)
1. A method for measuring the contents of lead and cadmium elements in a silver ornament is characterized by comprising the following steps: the method comprises the following steps:
(1) dissolving a silver sample to be detected by using nitric acid to obtain a silver nitrate solution;
(2) adding a thiocyanate solution into a silver nitrate solution to completely precipitate silver ions into silver thiocyanate;
(3) filtering to remove silver thiocyanate precipitate, and taking the filtrate to determine the content of lead and cadmium elements.
2. The method for determining the content of lead and cadmium elements in the silver ornament according to claim 1, wherein the method comprises the following steps: and (3) measuring the contents of the lead and cadmium elements in the filtrate by using an inductively coupled plasma emission spectrometer.
3. The method for determining the content of lead and cadmium elements in the silver ornaments, as claimed in claim 2, wherein: before the content of lead and cadmium in the filtrate is determined, the step (3) further comprises the following steps: and (3) dissolving pure silver with the same mass as that in the step (1) by using nitric acid, then adding potassium thiocyanate, precipitating silver ions, filtering, and taking the filtrate as a correction solution for correcting the inductively coupled plasma emission spectrometer.
4. The method for determining the content of lead and cadmium elements in the silver ornament according to claim 1, wherein the method comprises the following steps: before the content of lead and cadmium in the filtrate is measured, the filtrate is acidified by nitric acid.
5. The method for determining the content of lead and cadmium elements in the silver ornament according to claim 1, wherein the method comprises the following steps: the concentration of the thiocyanate solution in the step (2) is 0.10-0.50 g/mL.
6. The method for determining the content of lead and cadmium elements in the silver ornament according to claim 1, wherein the method comprises the following steps: the thiocyanate in the step (2) is selected from sodium thiocyanate and potassium thiocyanate.
7. The method for determining the content of lead and cadmium elements in the silver ornaments, as claimed in claim 2, wherein: when the content of lead and cadmium in the filtrate is measured by adopting an inductively coupled plasma emission spectrometer, the characteristic wavelength for detecting the lead element is 220.353nm, and the characteristic wavelength for detecting the cadmium element is 226.502 nm.
8. The method for determining the content of lead and cadmium elements in the silver ornament according to claim 1, wherein the method comprises the following steps: the mass of the silver ornament sample in the step (1) is 0.25-1.00 g.
9. The method for determining the content of lead and cadmium elements in the silver ornament according to claim 1, wherein the method comprises the following steps: the molar ratio of the silver sample to the nitric acid in the step (1) is 1: 4-30.
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| CN102565029A (en) * | 2010-12-31 | 2012-07-11 | 北京有色金属与稀土应用研究所 | Method for measuring impurities in pure silver by electrical inductance-coupled plasma emission spectrometer |
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Inventor after: Li Guihua Inventor after: Liu Xuesong Inventor after: Liu Haibin Inventor after: Yu Chunhong Inventor after: Wang Ping Inventor after: Zhang Fengxia Inventor after: Bai Zhushuang Inventor before: Liu Haibin Inventor before: Li Guihua Inventor before: Liu Xuesong Inventor before: Yu Chunhong Inventor before: Wang Ping Inventor before: Zhang Fengxia Inventor before: Bai Zhushuang |
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