CN107037035A - Determine the spectroscopic analysis methods of silver-colored boron tin three constituent content in geochemical sample - Google Patents
Determine the spectroscopic analysis methods of silver-colored boron tin three constituent content in geochemical sample Download PDFInfo
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- CN107037035A CN107037035A CN201710364331.7A CN201710364331A CN107037035A CN 107037035 A CN107037035 A CN 107037035A CN 201710364331 A CN201710364331 A CN 201710364331A CN 107037035 A CN107037035 A CN 107037035A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Abstract
Obtain infiltrating sample using liquid buffer infiltration testing sample the invention provides a kind of spectroscopic analysis methods for determining silver-colored boron tin three constituent content in geochemical sample, including first；Then infiltration sample is fitted into sample electrode and is compacted, instill alcohol sucrose solution, drying obtains drying sample；Drying sample is excited using alternating current-direct current arc generator again, and spectrum is taken the photograph using spectrograph progress, direct reading test software calculating silver, boron, the content of the element of tin three are then composed using CCD entirely and result is exported.The present invention is simple to operate, convenient, quick, effectively increases operating efficiency, and test result is accurate, favorable reproducibility.
Description
Technical field
The invention belongs to the silver-colored element of boron tin three in field of spectral analysis technology, more particularly to a kind of measure geochemical sample
The spectroscopic analysis methods of content.
Background technology
Full spectrum direct-reading alternating current-direct current electric arc emission spectrometry has that analyze speed is fast, the degree of accuracy is high, the low feature of detection limit, especially
It is the analysis to indissoluble (molten) class solid sample, what even more other technologies can not match in excellence or beauty.During analysis, generally require and add
Enter spectroscopic buffer to reduce matrix effect.Existing buffer is generally solid, although can to a certain extent reduce and analyze
Matrix effect in journey, but there are problems that testing process length, efficiency are low, easily cause Partial Elements, and it is existing
Solid buffer agents in itself also easily containing part element to be measured and influence test result.Suitable buffer is selected to improving full spectrum
The accuracy of the analysis test result of direct-reading alternating current-direct current electric arc emission spectrometry is particularly significant.
The content of the invention
In order to solve the above-mentioned technical problem, the present invention provides silver-colored boron tin three constituent content in a kind of measure geochemical sample
Spectroscopic analysis methods, including：
S1. obtain infiltrating sample using liquid buffer infiltration testing sample；
S2. infiltration sample is fitted into sample electrode and is compacted, instill alcohol sucrose solution, then drying obtains drying sample
Product；
S3. drying sample is excited using alternating current-direct current arc generator, and spectrum is taken the photograph using spectrograph progress, then using CCD
Full spectrum direct reading test software calculates silver, boron, the content of the element of tin three and exports result.
The present invention substitutes conventional solid buffer agents using liquid buffer, is directly filled after being mixed with testing sample
Sample, removes from using processes such as weighing, mixing, the grindings of solid buffer agents, shortens operating process, improve testing efficiency.
Liquid buffer in the present invention can not contain silver, boron, the salts substances of the element of tin three using one or more
It is dissolved in water and is prepared from.Salts substances can select sodium chloride, potassium chloride, sodium sulphate, ammonium fluoride, potassium pyrosulfate, acid iodide
Potassium, ammonium chloride, aluminium chloride etc..
The electrode needed in the present invention is included to electrode (Top electrode) and sample electrode (bottom electrode), and electrode can be selected
Tack column structure, sample electrode (bottom electrode) selects thin neck cup-like structure.Infiltrate sample and load sample electrode (bottom electrode)
Cup intracavitary, infiltration sample must compress compacting.
The sample that the spectroscopic analysis methods that the present invention is provided can be detected is sample based on silicate, can be with
Silicate is any one in water system sediment, pedotheque and the rock sample of main body.
The alcohol sucrose solution used in the present invention is that 2g sucrose is dissolved in 100mL ethanol waters to be prepared from, second
The volume ratio of second alcohol and water is 1 in alcohol solution:1.
Further, the liquid buffer is Klorvess Liquid.
Further, the Klorvess Liquid is saturated potassium chloride solution.Buffer is used as using saturated potassium chloride solution
Sample can be made to excite fully, the derived result interference of experiment is few, and test result is accurate.
Further, the condition of work of the alternating current-direct current arc generator is：Pre-burning 5A 5S exposure 14A 30S.It is loaded into
The sample electrode of infiltration sample is placed on vertical alignment on spectrograph electrode holder as bottom electrode and Top electrode, and upper/lower electrode interval is about
3mm or so starts to rise to 14A after taking the photograph spectrum, starting the arc when electric current is 5A, 5s, keeps 30s.
When the condition of work of alternating current-direct current arc generator is that pre-burning 5A 5S expose 14A 30S, the salt adhered on electrode holder
Reduce, sample is excited fully, the derived result interference of experiment is few, and test result is accurate.
Further, step S1 is specifically included：Testing sample is placed on template, pipette appropriate amount of fluid buffer in
The side of testing sample, slowly infiltrates to testing sample is immersed and runs through.
The papery of template is pure, quality is hard, be unlikely to deform, permeability resistance is strong, can make buffer thereon with treating
Test sample product are sufficiently mixed, and give full play to the buffering effect of buffer, make that measuring result error is small, the degree of accuracy is high.
Further, the concrete technology of the drying is：Dried 1 hour under conditions of 70-90 DEG C.
Compared with prior art, the beneficial effects of the present invention are：
What the present invention was provided determines the spectroscopic analysis methods test result of silver-colored boron tin three constituent content in geochemical sample
Accurately, favorable reproducibility, it is simple to operate, convenient, quick, effectively increase operating efficiency.
Embodiment
Embodiment 1
The spectroscopic analysis methods of silver-colored boron tin three constituent content in a kind of measure geochemical sample, including：
S1. obtain infiltrating sample using 20% ammonium fluoride solution infiltration testing sample；
S2. infiltration sample is fitted into sample electrode and is compacted, instill alcohol sucrose solution, then drying obtains drying sample
Product；
S3. drying sample is excited using alternating current-direct current arc generator, shooting condition is that pre-burning 5A5S exposes 14A 30S, and
Carry out taking the photograph spectrum using spectrograph, then composing direct reading test software entirely using CCD calculates silver, boron, the content of the element of tin three and export
As a result.
Embodiment 2
The spectroscopic analysis methods of silver-colored boron tin three constituent content in a kind of measure geochemical sample, including：
S1. potassium pyrosulfate saturated solution is prepared, then Potassiumiodate is added in potassium pyrosulfate saturated solution until Potassiumiodate is satisfied
With, then using one times of acquisition potassium pyrosulfate/potassium iodate solution of deionized water dilution；Ammonium chloride saturated solution, aluminium chloride is prepared to satisfy
And solution；By ammonium chloride saturated solution, aluminium chloride saturated solution, potassium pyrosulfate/potassium iodate solution according to 1:1:2 volume ratio
It is hybridly prepared into mixed solution；Obtain infiltrating sample using mixed solution infiltration testing sample；
S2. infiltration sample is fitted into sample electrode and is compacted, instill alcohol sucrose solution, then drying obtains drying sample
Product；
S3. drying sample is excited using alternating current-direct current arc generator, shooting condition is that pre-burning 5A5S exposes 14A 30S, and
Carry out taking the photograph spectrum using spectrograph, then composing direct reading test software entirely using CCD calculates silver, boron, the content of the element of tin three and export
As a result.
Embodiment 3
The spectroscopic analysis methods of silver-colored boron tin three constituent content in a kind of measure geochemical sample, including：
S1. obtain infiltrating sample using saturated potassium chloride solution infiltration testing sample；
S2. infiltration sample is fitted into sample electrode and is compacted, instill alcohol sucrose solution, then drying obtains drying sample
Product；
S3. drying sample is excited using alternating current-direct current arc generator, shooting condition is that pre-burning 5A5S exposes 14A 30S, and
Carry out taking the photograph spectrum using spectrograph, then composing direct reading test software entirely using CCD calculates silver, boron, the content of the element of tin three and export
As a result.
Embodiment 4
The spectroscopic analysis methods of silver-colored boron tin three constituent content in a kind of measure geochemical sample, including：
S1. mass fraction is used to obtain infiltrating sample for 10% Klorvess Liquid infiltration testing sample；
S2. infiltration sample is fitted into sample electrode and is compacted, instill alcohol sucrose solution, then drying obtains drying sample
Product；
S3. drying sample is excited using alternating current-direct current arc generator, shooting condition is that pre-burning 5A5S exposes 14A 30S, and
Carry out taking the photograph spectrum using spectrograph, then composing direct reading test software entirely using CCD calculates silver, boron, the content of the element of tin three and export
As a result.
Embodiment 5
The spectroscopic analysis methods of silver-colored boron tin three constituent content in a kind of measure geochemical sample, including：
S1. mass fraction is used to obtain infiltrating sample for 20% Klorvess Liquid infiltration testing sample；
S2. infiltration sample is fitted into sample electrode and is compacted, instill alcohol sucrose solution, then drying obtains drying sample
Product；
S3. drying sample is excited using alternating current-direct current arc generator, shooting condition is that pre-burning 5A5S exposes 14A 30S, and
Carry out taking the photograph spectrum using spectrograph, then composing direct reading test software entirely using CCD calculates silver, boron, the content of the element of tin three and export
As a result.
Embodiment 6
The spectroscopic analysis methods of silver-colored boron tin three constituent content in a kind of measure geochemical sample, including：
S1. obtain infiltrating sample using saturated potassium chloride solution infiltration testing sample；
S2. infiltration sample is fitted into sample electrode and is compacted, instill alcohol sucrose solution, then drying obtains drying sample
Product；
S3. drying sample is excited using alternating current-direct current arc generator, shooting condition is that pre-burning 5A5S exposes 12A 20S, and
Carry out taking the photograph spectrum using spectrograph, then composing direct reading test software entirely using CCD calculates silver, boron, the content of the element of tin three and export
As a result.
Embodiment 7
The spectroscopic analysis methods of silver-colored boron tin three constituent content in a kind of measure geochemical sample, including：
S1. obtain infiltrating sample using saturated potassium chloride solution infiltration testing sample；
S2. infiltration sample is fitted into sample electrode and is compacted, instill alcohol sucrose solution, then drying obtains drying sample
Product；
S3. drying sample is excited using alternating current-direct current arc generator, shooting condition is that pre-burning 5A5S exposes 16.5A 40S,
And carry out taking the photograph spectrum using spectrograph, direct reading test software calculating silver, boron, the content of the element of tin three are then composed using CCD entirely and led
Go out result.
Embodiment 8
The spectroscopic analysis methods of silver-colored boron tin three constituent content in a kind of measure geochemical sample, including：
S1. testing sample is placed on template, pipettes appropriate saturated potassium chloride solution in the side of testing sample, slowly
Slow infiltration is run through to testing sample is immersed；
S2. infiltration sample is fitted into sample electrode and is compacted, alcohol sucrose solution is instilled, then under conditions of 70 DEG C
Dry and obtain within 1 hour drying sample；
S3. drying sample is excited using alternating current-direct current arc generator, shooting condition is that pre-burning 5A5S exposes 14A 30S, and
Carry out taking the photograph spectrum using spectrograph, then composing direct reading test software entirely using CCD calculates silver, boron, the content of the element of tin three and export
As a result.
Embodiment 9
The spectroscopic analysis methods of silver-colored boron tin three constituent content in a kind of measure geochemical sample, including：
S1. testing sample is placed on template, pipettes appropriate saturated potassium chloride solution in the side of testing sample, slowly
Slow infiltration is run through to testing sample is immersed；
S2. infiltration sample is fitted into sample electrode and is compacted, alcohol sucrose solution is instilled, then under conditions of 80 DEG C
Dry and obtain within 1 hour drying sample；
S3. drying sample is excited using alternating current-direct current arc generator, shooting condition is that pre-burning 5A5S exposes 14A 30S, and
Carry out taking the photograph spectrum using spectrograph, then composing direct reading test software entirely using CCD calculates silver, boron, the content of the element of tin three and export
As a result.
1. instrument and condition of work：
Instrument includes alternating current-direct current arc generator, spectrograph and electrode in method provided by the present invention, wherein：
Alternating current-direct current arc generator：WPF type alternating current-direct current arc generators；
Spectrograph：One meter of grating spectrograph of WP1 types, constrigence 0.8nm/mm, centre wavelength 280nm, three transparent illuminations
System, a width of 12 μm of slit, middle light bar 3.2mm；
Electrode：Including being Ф 4mm × 10mm to electrode (Top electrode) to electrode (Top electrode) and sample electrode (bottom electrode)
Tack column structure, sample electrode (bottom electrode) is the thin neck cup-like structures of Ф 3.8 × 3.8 × 0.6.
Standard series is specifically shown in Table 1 using national standard reference material and artificial synthesized silicate mixing series：
The element (μ g/g) of the standard series of table 1
| 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. spectroscopic analysis methods detection limit is evaluated
The method provided using embodiment 3, is entered using the spectrum analysis standard substratess of synthetic silicate as blank sample
12 parallel laboratory tests of row, draw method detection limit, as a result as shown in table 2.
The method detection limit of table 2 is evaluated
| Element | B | Sn | Ag |
| Analytical line (λ/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, B detection is limited to 0.69 μ g/g, and measurement range is 1-200 μ g/g, meets geochemistry general
Look into specification (1:50000) B detection is limited to 5 μ g/g requirement in；
Sn detection is limited to 0.6 μ g/g, and measurement range is 1.0-100 μ g/g, meets geochemical reconnaisance specification (1:
50000) Sn detection is limited to 1 μ g/g requirement in；
Ag detection is limited to 0.011 μ g/g, and measurement range is 0.020-5.00 μ g/g, meets geochemical reconnaisance specification
(1:50000) Ag detection is limited to 0.03 μ g/g requirement in.
3. spectroscopic analysis methods precision is evaluated
The method provided using embodiment 3,12 parallel laboratory tests are carried out using national standard reference material GBW07308a,
Corresponding relative standard deviation (RSD) is calculated, as a result as shown in table 3.
The method precision evaluation of table 3
| Element | B | Sn | Ag |
| RSD (%) | 9.01 | 7.49 | 8.00 |
The precision for the method that the present invention is provided can meet geochemical reconnaisance rule it can be seen from above-mentioned result of the test
Model (1:50000) to the requirement of precision in, the method testing result that the present invention is provided is accurate.
4. spectroscopic analysis methods accuracy estimating
The method provided using embodiment 3, the country-level Geochemical Certified Reference Materials of selection 12 (including rock composition,
Sediments and soil constituent) 12 parallel testings are carried out respectively, its result is as shown in table 4.
The spectroscopic analysis methods accuracy estimating of table 4
Note：Test elements result unit is ug/g in table.
From the above results, method test analysis B, Sn, Ag that the present invention is provided result are consistent with standard value, have
There is preferably test accuracy.
5. influence evaluation of the buffer species to analysis result
The method analysis test identical testing sample provided using embodiment 1, embodiment 2 and embodiment 3, is tied by test
Fruit understands：During using ammonium fluoride solution as buffer, the background of bands of a spectrum is integrally improved, to determine low content sample effects compared with
Greatly；Using ammonium chloride, aluminium chloride, Potassiumiodate, potassium pyrosulfate mixed solution as buffer when, due to its esters content too
Height, often takes the photograph on spectrum 3-5 bars, electrode holder and just adheres to many salts, be not suitable for mass detection task；And use Klorvess Liquid
Substantially reduced as ambient interferences during buffer, the salt that adheres on electrode holder is reduced, excite abundant, stably, test result is accurate
Really.
6. influence evaluation of the concentration of Klorvess Liquid to analysis result
The method analysis test identical testing sample provided using embodiment 3, embodiment 4 and embodiment 5, is tied by test
Fruit understands：As buffer sample can be made to excite fully using saturated potassium chloride solution, the derived result interference of experiment
Few, test result is accurate.
7. the influence evaluation of electric current and time for exposure to analysis result
The method analysis test identical testing sample provided using embodiment 3, embodiment 6 and embodiment 7, is tied by test
Fruit understands：The analytical testing sample provided using embodiment 3, the salt of electrode holder attachment is reduced, and sample swashs
Hair is abundant, and the derived result interference of experiment is few, and result of the test is accurate, therefore alternating current-direct current arc generator is exposed using pre-burning 5A 5S
Light 14A 30S condition of work best results.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although reference
The present invention is described in detail for preferred embodiment, it will be understood by those within the art that, can be to the present invention's
Technical scheme is modified or equivalent substitution, and without departing from the spirit and scope of technical solution of the present invention, it all should cover
Among scope of the presently claimed invention.
Claims (6)
1. a kind of spectroscopic analysis methods for determining silver-colored boron tin three constituent content in geochemical sample, it is characterised in that the side
Method includes：
S1. obtain infiltrating sample using liquid buffer infiltration testing sample；
S2. infiltration sample is fitted into sample electrode and is compacted, instill alcohol sucrose solution, then drying obtains drying sample；
S3. drying sample is excited using alternating current-direct current arc generator, and spectrum is taken the photograph using spectrograph progress, then composed entirely using CCD
Direct reading test software calculates silver, boron, the content of the element of tin three and exports result.
2. according to the method described in claim 1, it is characterised in that the liquid buffer is Klorvess Liquid.
3. method according to claim 2, it is characterised in that the Klorvess Liquid is saturated potassium chloride solution.
4. according to the method described in claim 1, it is characterised in that the condition of work of the alternating current-direct current arc generator is：In advance
Fire 5A 5S exposure 14A 30S.
5. according to the method described in claim 1, it is characterised in that step S1 is specifically included：Testing sample is placed on sulfuric acid
On paper, appropriate amount of fluid buffer is pipetted in the side of testing sample, is slowly infiltrated to testing sample is immersed and is run through.
6. according to the method described in claim 1, it is characterised in that the concrete technology of the drying is：In 70-90 DEG C of condition
It is lower to dry 1 hour.
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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 |