CN107037035B - Spectral analysis method for determining content of silver, boron and tin three-element in geochemical sample - Google Patents
Spectral analysis method for determining content of silver, boron and tin three-element in geochemical sample Download PDFInfo
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Abstract
The invention provides a spectral analysis method for determining the content of three elements of silver, boron and tin in a geochemical sample, which comprises the steps of firstly infiltrating the sample to be tested by adopting a liquid buffering agent to obtain an infiltrated sample; then putting the soaked sample into a sample electrode and compacting, dripping an alcohol sucrose solution, and drying to obtain a dried sample; and then, exciting and drying the sample by adopting an alternating current-direct current arc generator, performing spectrograph, calculating the contents of the silver, the boron and the tin by adopting CCD full-spectrum direct-reading test software, and deriving a result. The method is simple, convenient and quick to operate, effectively improves the working efficiency, and has accurate test result and good reproducibility.
Description
Technical Field
The invention belongs to the technical field of spectral analysis, and particularly relates to a spectral analysis method for determining the content of three elements of silver, boron and tin in a geochemical sample.
Background
The full-spectrum direct-reading alternating current and direct current arc emission spectrometry has the characteristics of high analysis speed, high accuracy, low detection limit and the like, and particularly can not be compared favorably with other technologies for analyzing insoluble (molten) solid samples. In the course of the analysis, it is generally necessary to add a spectral buffer to reduce matrix effects. Most of the existing buffer agents are solid, and although the matrix effect in the analysis process can be reduced to a certain extent, the problems of long test flow, low efficiency, easy pollution of part of elements and the like exist, and the existing solid buffer agents also easily contain part of elements to be tested to influence the test result. The selection of a proper buffering agent is very important for improving the accuracy of the analysis and test result of the full-spectrum direct-reading alternating current-direct current arc emission spectrometry.
Disclosure of Invention
In order to solve the technical problem, the invention provides a spectral analysis method for determining the content of three elements of silver, boron and tin in a geochemical sample, which comprises the following steps:
s1, infiltrating a sample to be tested by using a liquid buffer to obtain an infiltrated sample;
s2, placing the soaked sample into a sample electrode, compacting, dripping an alcohol sucrose solution, and drying to obtain a dried sample;
and S3, exciting and drying the sample by adopting an alternating current-direct current arc generator, performing spectrograph, calculating the contents of the silver, the boron and the tin by adopting CCD full-spectrum direct-reading test software, and deriving a result.
The invention adopts the liquid buffer to replace the common solid buffer, can be directly loaded after being mixed with the sample to be tested, omits the procedures of weighing, mixing, grinding and the like of the solid buffer, shortens the operation flow and improves the testing efficiency.
The liquid buffer in the invention can be prepared by dissolving one or more salt substances which do not contain silver, boron and tin into water. The salt can be selected from sodium chloride, potassium chloride, sodium sulfate, ammonium fluoride, potassium pyrosulfate, potassium iodate, ammonium chloride, aluminum chloride, etc.
The electrodes required by the invention comprise a counter electrode (an upper electrode) and a sample electrode (a lower electrode), wherein the counter electrode can be in a flat-head columnar structure, and the sample electrode (the lower electrode) is in a narrow-neck cup-shaped structure. The infiltrated sample is placed in the cup cavity of the sample electrode (lower electrode) and the infiltrated sample must be compacted.
The sample which can be detected by the spectral analysis method provided by the invention is a silicate-based sample, and can be any one of a water system precipitate, a soil sample and a rock sample which are silicate-based samples.
The alcoholic sucrose solution used in the present invention is prepared by dissolving 2g of sucrose in 100mL of an aqueous ethanol solution, wherein the volume ratio of ethanol to water in the aqueous ethanol solution is 1: 1.
Further, the liquid buffer is a potassium chloride solution.
Further, the potassium chloride solution is a saturated potassium chloride solution. The potassium chloride saturated solution is used as a buffer, so that the tested sample can be fully excited, the interference of the result derived from the test is less, and the test result is accurate.
Further, the operating conditions of the ac/dc arc generator are as follows: the precombustion 5A5S is exposed to 14A 30S. And placing the sample electrode filled with the infiltrated sample as a lower electrode and an upper electrode on a spectrograph electrode clamp to be vertically aligned, starting spectrograph when the interval between the upper electrode and the lower electrode is about 3mm, starting arcing when the current is 5A, rising to 14A after 5s, and keeping for 30 s.
When the working condition of the AC-DC arc generator is precombustion 5A5S exposure 14A 30S, the salt attached to the electrode clamp is reduced, the tested sample is fully excited, the interference of the result derived from the test is less, and the test result is accurate.
Further, step S1 specifically includes: placing a sample to be detected on parchment paper, transferring a proper amount of liquid buffer on one side of the sample to be detected, and slowly soaking until the sample to be detected is soaked completely.
The parchment paper is pure, hard in texture, not easy to deform and strong in anti-permeability, the buffering agent can be fully mixed with a sample to be measured on the parchment paper, the buffering effect of the buffering agent is fully exerted, and the measuring result is small in error and high in accuracy.
Further, the drying process comprises the following specific steps: baking at 70-90 deg.C for 1 hr.
Compared with the prior art, the invention has the beneficial effects that:
the spectral analysis method for determining the content of the silver, boron and tin three-element in the geochemical sample provided by the invention has the advantages of accurate test result, good reproducibility, simple, convenient and quick operation and effectively improved working efficiency.
Detailed Description
Example 1
A spectral analysis method for determining the content of three elements of silver, boron and tin in a geochemical sample comprises the following steps:
s1, soaking a sample to be detected by using a 20% ammonium fluoride solution to obtain a soaked sample;
s2, placing the soaked sample into a sample electrode, compacting, dripping an alcohol sucrose solution, and drying to obtain a dried sample;
and S3, exciting and drying the sample by adopting an alternating current-direct current arc generator under the excitation condition of pre-combustion 5A5S exposure for 14A 30S, performing spectrograph by adopting a spectrograph, calculating the contents of the silver, the boron and the tin by adopting CCD full-spectrum direct-reading test software, and deriving a result.
Example 2
A spectral analysis method for determining the content of three elements of silver, boron and tin in a geochemical sample comprises the following steps:
s1, preparing a potassium pyrosulfate saturated solution, adding potassium iodate into the potassium pyrosulfate saturated solution until the potassium iodate is saturated, and diluting the potassium pyrosulfate/potassium iodate solution by using deionized water for one time to obtain a potassium pyrosulfate/potassium iodate solution; preparing an ammonium chloride saturated solution and an aluminum chloride saturated solution; mixing an ammonium chloride saturated solution, an aluminum chloride saturated solution and a potassium pyrosulfate/potassium iodate solution according to the volume ratio of 1:1:2 to prepare a mixed solution; soaking a sample to be detected by adopting the mixed solution to obtain a soaked sample;
s2, placing the soaked sample into a sample electrode, compacting, dripping an alcohol sucrose solution, and drying to obtain a dried sample;
and S3, exciting and drying the sample by adopting an alternating current-direct current arc generator under the excitation condition of pre-combustion 5A5S exposure for 14A 30S, performing spectrograph by adopting a spectrograph, calculating the contents of the silver, the boron and the tin by adopting CCD full-spectrum direct-reading test software, and deriving a result.
Example 3
A spectral analysis method for determining the content of three elements of silver, boron and tin in a geochemical sample comprises the following steps:
s1, infiltrating a sample to be tested by using a potassium chloride saturated solution to obtain an infiltrated sample;
s2, placing the soaked sample into a sample electrode, compacting, dripping an alcohol sucrose solution, and drying to obtain a dried sample;
and S3, exciting and drying the sample by adopting an alternating current-direct current arc generator under the excitation condition of pre-combustion 5A5S exposure for 14A 30S, performing spectrograph by adopting a spectrograph, calculating the contents of the silver, the boron and the tin by adopting CCD full-spectrum direct-reading test software, and deriving a result.
Example 4
A spectral analysis method for determining the content of three elements of silver, boron and tin in a geochemical sample comprises the following steps:
s1, infiltrating a sample to be tested by adopting a potassium chloride solution with the mass fraction of 10% to obtain an infiltrated sample;
s2, placing the soaked sample into a sample electrode, compacting, dripping an alcohol sucrose solution, and drying to obtain a dried sample;
and S3, exciting and drying the sample by adopting an alternating current-direct current arc generator under the excitation condition of pre-combustion 5A5S exposure for 14A 30S, performing spectrograph by adopting a spectrograph, calculating the contents of the silver, the boron and the tin by adopting CCD full-spectrum direct-reading test software, and deriving a result.
Example 5
A spectral analysis method for determining the content of three elements of silver, boron and tin in a geochemical sample comprises the following steps:
s1, infiltrating a sample to be tested by adopting a potassium chloride solution with the mass fraction of 20% to obtain an infiltrated sample;
s2, placing the soaked sample into a sample electrode, compacting, dripping an alcohol sucrose solution, and drying to obtain a dried sample;
and S3, exciting and drying the sample by adopting an alternating current-direct current arc generator under the excitation condition of pre-combustion 5A5S exposure for 14A 30S, performing spectrograph by adopting a spectrograph, calculating the contents of the silver, the boron and the tin by adopting CCD full-spectrum direct-reading test software, and deriving a result.
Example 6
A spectral analysis method for determining the content of three elements of silver, boron and tin in a geochemical sample comprises the following steps:
s1, infiltrating a sample to be tested by using a potassium chloride saturated solution to obtain an infiltrated sample;
s2, placing the soaked sample into a sample electrode, compacting, dripping an alcohol sucrose solution, and drying to obtain a dried sample;
and S3, exciting and drying the sample by adopting an alternating current-direct current arc generator under the excitation condition of pre-combustion 5A5S exposure for 12A 20S, performing spectrograph by adopting a spectrograph, calculating the contents of the silver, the boron and the tin by adopting CCD full-spectrum direct-reading test software, and deriving a result.
Example 7
A spectral analysis method for determining the content of three elements of silver, boron and tin in a geochemical sample comprises the following steps:
s1, infiltrating a sample to be tested by using a potassium chloride saturated solution to obtain an infiltrated sample;
s2, placing the soaked sample into a sample electrode, compacting, dripping an alcohol sucrose solution, and drying to obtain a dried sample;
and S3, exciting and drying the sample by adopting an alternating current-direct current arc generator under the excitation condition of pre-combustion 5A5S exposure for 16.5A 40S, performing spectrograph by adopting a spectrograph, calculating the contents of the silver, the boron and the tin by adopting CCD full-spectrum direct-reading test software, and deriving a result.
Example 8
A spectral analysis method for determining the content of three elements of silver, boron and tin in a geochemical sample comprises the following steps:
s1, placing a sample to be detected on parchment paper, transferring a proper amount of saturated potassium chloride solution to one side of the sample to be detected, and slowly soaking until the sample to be detected is soaked completely;
s2, placing the soaked sample into a sample electrode, compacting, dripping an alcohol sucrose solution, and then drying for 1 hour at 70 ℃ to obtain a dried sample;
and S3, exciting and drying the sample by adopting an alternating current-direct current arc generator under the excitation condition of pre-combustion 5A5S exposure for 14A 30S, performing spectrograph by adopting a spectrograph, calculating the contents of the silver, the boron and the tin by adopting CCD full-spectrum direct-reading test software, and deriving a result.
Example 9
A spectral analysis method for determining the content of three elements of silver, boron and tin in a geochemical sample comprises the following steps:
s1, placing a sample to be detected on parchment paper, transferring a proper amount of saturated potassium chloride solution to one side of the sample to be detected, and slowly soaking until the sample to be detected is soaked completely;
s2, placing the soaked sample into a sample electrode, compacting, dripping an alcohol sucrose solution, and then drying for 1 hour at the temperature of 80 ℃ to obtain a dried sample;
and S3, exciting and drying the sample by adopting an alternating current-direct current arc generator under the excitation condition of pre-combustion 5A5S exposure for 14A 30S, performing spectrograph by adopting a spectrograph, calculating the contents of the silver, the boron and the tin by adopting CCD full-spectrum direct-reading test software, and deriving a result.
1. Instruments and working conditions:
the instrument used in the method provided by the invention comprises an AC/DC arc generator, a spectrograph and an electrode, wherein:
AC-DC arc generator: WPF type AC/DC arc generator;
spectrograph: WP1 type one-meter grating spectrograph, the inverse dispersion rate is 0.8nm/mm, the central wavelength is 280nm, three transparent lighting systems have the slit width of 12 mu m and the middle diaphragm of 3.2 mm;
an electrode: the device comprises a counter electrode (upper electrode) and a sample electrode (lower electrode), wherein the counter electrode (upper electrode) is of a phi 4mm multiplied by 10mm flat-head columnar structure, and the sample electrode (lower electrode) is of a phi 3.8 multiplied by 0.6 thin-neck cup-shaped structure.
The standard series adopts a mixed series of national first-grade standard substances and artificially synthesized silicate, and is specifically shown in table 1:
TABLE 1 elements of the Standard series (. mu.g/g)
| B | Sn | Ag | |
| S0 | 9.80 | 3.30 | 0.036 |
| S1 | 9.70 | 8.60 | 0.040 |
| S2 | 91.00 | 4.00 | 0.22 |
| S3 | 96.00 | 5.00 | 0.63 |
| S4 | 195.00 | 5.20 | 1.20 |
| S5 | 23.00 | 2.50 | 0.091 |
| S6 | 57.00 | 72.40 | 0.20 |
| S7 | 20.00 | 2.10 | 0.21 |
| S8 | 50.00 | -- | 0.51 |
| S9 | 100.00 | -- | 1.00 |
| SA | 200.00 | -- | 2.00 |
| SB | -- | -- | 5.00 |
| SC | -- | 200 | 10.00 |
2. Evaluation of detection limit of spectral analysis method
Using the method provided in example 3, 12 replicates were run using a standard substrate for spectroscopic analysis of synthetic silicate as a blank to obtain the method detection limits, the results of which are shown in table 2.
TABLE 2 evaluation of detection limits of the methods
| Element(s) | B | Sn | Ag |
| Analysis line (lambda/nm) | 249.7733 | 283.9351 | 328.068 |
| Detection limit (μ g/g) | 0.69 | 0.6 | 0.011 |
| Measurement Range (μ g/g) | 1-200 | 1.0-100 | 0.020-5.00 |
From the above results, it is found that the detection limit of B is 0.69. mu.g/g, the measurement range is 1 to 200. mu.g/g, and the requirement that the detection limit of B in the general survey Specification for geochemistry (1:50000) is 5. mu.g/g is satisfied;
the detection limit of Sn is 0.6 mug/g, the measuring range is 1.0-100 mug/g, and the requirement that the detection limit of Sn in the general survey specification (1:50000) of geochemistry is 1 mug/g is met;
the detection limit of Ag is 0.011 mu g/g, the measurement range is 0.020-5.00 mu g/g, and the requirement that the detection limit of Ag in the general survey specification of geochemistry (1:50000) is 0.03 mu g/g is met.
3. Evaluation of precision of spectral analysis method
Using the method provided in example 3, 12 parallel experiments were carried out using the national primary standard substance GBW07308a and the corresponding Relative Standard Deviation (RSD) was calculated and the results are shown in Table 3.
TABLE 3 evaluation of precision of method
| Element(s) | B | Sn | Ag |
| RSD(％) | 9.01 | 7.49 | 8.00 |
The test results show that the precision of the method provided by the invention can meet the requirement on the precision in the general geochemical survey specification (1:50000), and the test result of the method provided by the invention is accurate.
4. Accuracy evaluation of spectral analysis method
12 times of parallel tests were performed on 12 national primary geochemical standards (including rock components, water system sediments and soil components) by the method provided in example 3, and the results are shown in Table 4.
TABLE 4 evaluation of accuracy of spectral analysis method
Note: the units of the test element results in the table are ug/g.
According to the results, the results of B, Sn and Ag test and analysis by the method provided by the invention are consistent with the standard values, and the method has better test accuracy.
5. Evaluation of the Effect of buffer species on assay results
The same samples to be tested were analyzed and tested by the methods provided in example 1, example 2 and example 3, and the test results show that: when the ammonium fluoride solution is used as a buffering agent, the background of a spectral band is integrally improved, and the influence on the determination of a low-content sample is large; when the mixed solution of ammonium chloride, aluminum chloride, potassium iodate and potassium pyrosulfate is used as a buffer, 3-5 salts are attached to the electrode clamp per spectrograph due to the high salt content, so that the method is not suitable for large-scale detection tasks; and when the potassium chloride solution is used as a buffer, the background interference is obviously reduced, the salt attached to the electrode clamp is reduced, the excitation is sufficient and stable, and the test result is accurate.
6. Evaluation of influence of concentration of potassium chloride solution on analysis results
The same samples to be tested were analyzed and tested by the methods provided in examples 3, 4 and 5, and the test results show that: the potassium chloride saturated solution is used as a buffer, so that the tested sample can be fully excited, the interference of the result derived from the test is less, and the test result is accurate.
7. Evaluation of Effect of Current and Exposure time on analysis results
The same samples to be tested were analyzed and tested by the methods provided in examples 3, 6 and 7, and the test results show that: when the analysis method provided in embodiment 3 is used to analyze the sample to be tested, the salts attached to the electrode clamps are reduced, the sample to be tested is sufficiently excited, the interference of the result derived from the experiment is less, and the test result is accurate, so that the effect of the working condition of the alternating current/direct current arc generator adopting the pre-combustion 5A5S to expose 14A 30S is the best.
Finally, it should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered by the claims of the present invention.
Claims (2)
1. A spectral analysis method for measuring the content of three elements of silver, boron and tin in a geochemical sample is characterized in that,
s1, infiltrating a sample to be tested by using a potassium chloride saturated solution to obtain an infiltrated sample;
s2, placing the soaked sample into a sample electrode, compacting, dripping an alcohol sucrose solution, drying for 1 hour at 70-90 ℃, and drying to obtain a dried sample; the alcohol sucrose solution is prepared by dissolving 2g of sucrose in 100mL of ethanol water solution, wherein the volume ratio of ethanol to water in the ethanol water solution is 1: 1;
and S3, exciting and drying the sample by adopting an alternating current-direct current arc generator under the excitation condition of precombustion 5A5S exposure 14A 30S, performing spectrograph by adopting a spectrograph, calculating the contents of the silver, the boron and the tin by adopting CCD full-spectrum direct-reading test software, and deriving a result.
2. The method according to claim 1, wherein step S1 specifically comprises: placing a sample to be detected on parchment paper, transferring a proper amount of liquid buffer on one side of the sample to be detected, and slowly soaking until the sample to be detected is soaked completely.
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Inventor after: Yu Tian Inventor after: Wang Meng Inventor after: Zhang Junnan Inventor after: Li Junjie Inventor after: Yang Yamin Inventor after: Liu Yanting Inventor after: Xiao Zhibo Inventor after: Liu Liying Inventor after: Wang Jingxian Inventor after: Chen Huiyun Inventor after: Bo Surui Inventor after: Chen Xiaodi Inventor after: Fan Yufeng Inventor after: Mao Wei Inventor after: Lv Xiaohui Inventor after: Yang Xiuli Inventor after: Zhao Li Inventor after: Jia Chunfang Inventor after: Hao Hongyan Inventor after: Xiong Yubao Inventor after: Chen Yanan Inventor before: Yu Tian Inventor before: Hao Hongyan Inventor before: Xiong Yubao Inventor before: Qu Yunfei Inventor before: Chen Yanan Inventor before: Wang Meng Inventor before: Zhang Junnan Inventor before: Li Junjie Inventor before: Yang Yamin Inventor before: Liu Yanting Inventor before: Xiao Zhibo Inventor before: Zhang Jianqiang Inventor before: Liu Liying Inventor before: Wang Jingxian Inventor before: Chen Huiyun Inventor before: Bo Surui Inventor before: Fan Yufeng Inventor before: Mao Wei Inventor before: Zhang Lianqi Inventor before: Meng Dianchao Inventor before: Chen Xiaodi Inventor before: Yang Xiuli Inventor before: Lv Xiaohui Inventor before: Zhao Li Inventor before: Jia Chunfang |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: No.15, Yangao Road, Yanjiao Development Zone, Sanhe City, Langfang City, Hebei Province 065200 Patentee after: North China Nonferrous Metals (Sanhe) Yanjiao central laboratory Co.,Ltd. Address before: No.15, Yangao Road, Yanjiao Development Zone, Sanhe City, Langfang City, Hebei Province 065201 Patentee before: NORTH CHINA NONFERROUS METAL EXPLORATION BUREAU YANJIAO CENTRAL LABORATORY |