CN108828052A - The method of tin amount in alkali fusion-inductively coupled plasma mass spectrometry measurement tin ore - Google Patents
The method of tin amount in alkali fusion-inductively coupled plasma mass spectrometry measurement tin ore Download PDFInfo
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Abstract
The invention discloses the methods of tin amount in a kind of alkali fusion-inductively coupled plasma mass spectrometry measurement tin ore, sample is through sodium peroxide fusion and decomposition, hot water leaching, hydrochloric acid acidification, solution moves on in volumetric flask, divide and takes clarified solution, after being diluted with nitric acid, sample enters radio frequency plasma by sampling system, and it is evaporated in high temperature quarter bend, dissociation, atomization and ionization, ion passes through bipyramid interface, ion mirror, level four bars mass analyzer, it is successively separated according to the size of mass/charge, finally detected by ion detector, and with the amount of calibration curve quantitative analysis tin, so as to quick, accurately, effectively measure the content of tin in tin ore.Meanwhile the method improves work efficiency, and reduces the labor intensity of operator, and will not cause damages to the body of operator, thus also there is significant social benefit.
Description
Technical field
The present invention relates to chemical substances to measure technical field processed, and in particular to one kind can be with alkali fusion-inductively coupled plasma
The method of body mass spectrometric determination tin amount.
Background technique
Tin, carbon group element, argenteous soft metal, specific gravity 7.3, atomic number 50, atomic weight 118.71, masurium come
Derived from Latin.Content of the tin in the earth's crust is 0.004%, is nearly all existed in the form of cassiterite (tin oxide), in addition there are
The sulfide mine of minimal amount of tin.Tin is famous " hardware " -- one of gold, silver, copper, iron, tin, and there is tin abundant in China
Mine, especially Area, Gejiu District, Yunnan Province city are world-famous " tin are all ".In addition, the provinces such as Guangxi, Guangdong, Jiangxi also all produce tin.Tin is on ground
Natural reserves in shell are 11,000,000 tons, 6,100,000 tons of workable reserves.
Currently, the analysis test method of tin element mainly has iodimetric titration, Solution by Phenylfluorone Spectrophotometry, polarography, emission spectrometry
Deng.The principle of iodimetric titration, which is sample, is reduced to divalent for tin with aluminium flake, iron powder etc. in hydrochloric acid medium by fusion and decomposition, with
The titration of Potassiumiodate standard solution, measures tin amount.The method have the shortcomings that one it is obvious, under normal circumstances, tin element and arsenic element
Accompanying element each other can generate the black precipitate of element arsenic, influence recognition of end-point when the content of arsenic in solution is greater than 3mg.This
Outside, the elements such as copper, tungsten, molybdenum, antimony, bismuth, germanium, chromium, vanadium, niobium, tantalum, fluorine are the interference elements of this method.Solution by Phenylfluorone Spectrophotometry
Principle is sample by decomposing, and with the iodide of benzene extraction of tin, separates interference element, then in sulfuric acid solution, tin and benzene fluorenes
Copper generates red precipitate, makes its dispersion in the solution with animal glue, is then measured with spectrophotometry.The method is a classics
Old chemical method, be widely applied in major geological laboratory at home, but shortcoming is that analysis process is long, expend analysis people
The time of member, in addition, this method is the process of extraction and back extraction that an organic matter participates in, to the health of analysis personnel
It will cause larger harm.Although polarography also occurs in books, with the appearance of large-scale precision instrument, each laboratory is not
Reuse the method analysis tin amount of this backwardness.Emission spectrometry is widely used in regional geochemistry prospecting sample analysis,
Tin usually only in geochemical sample can be analyzed with the method, and the analysis upper limit is 200ug/g, and for various reasons, essence
Density, stability etc. are not ideal.
Summary of the invention
The technical problem to be solved by the present invention is in view of the shortcomings of the prior art, provide, a kind of operating procedure is simple, sample
Handle alkali fusion-inductively coupled plasma mass spectrometry measurement tin ore that simple and quick, pollution is small, harm is small, measurement accuracy is high
The method of middle tin amount.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：A kind of alkali fusion-inductively coupled plasma constitution
The method that spectrometry measures tin amount in tin ore, it is characterised in that：Sample is through sodium peroxide fusion and decomposition, hot water leaching, hydrochloric acid acid
Change, solution moves on in volumetric flask, divides and takes clarified solution, and after nitric acid (2+98) dilution, sample enters radio frequency etc. by sampling system
Gas ions, and evaporation, dissociation, atomization and ionization in high temperature quarter bend, ion pass through bipyramid interface, ion mirror, level four bars matter
Contents analyzer is successively separated according to the size of mass/charge, is finally detected by ion detector, and use calibration curve method
The amount of quantitative analysis tin, instrument response inhibition or enhancement effect caused by sample matrices and instrumental shift are compensated using internal standard, are had
Body determination step is as follows,
1) sample is weighed；
2) blank test carries out duplicate blank test in company with sample, and agents useful for same is derived from same bottle, same amount is added；
3) verification test, in company with national standard substance similar in sample analysis same type, content；
4) sample decomposes
A, sample is placed in corundum crucible, 2g sodium peroxide is added, stirs evenly, covers one layer of sodium peroxide again above, put
Enter and melt 10min in 750 DEG C of high temperature furnaces, after taking out cooling, crucible is put into the beaker for filling 30mL boiling water, 0.2g wine is added
Stone acid, it is slightly cold, hydrochloric acid 15mL is added after fusant is completely fallen off, crucible is washed with water out, is cooled to room temperature, solution moves into
In 100mL volumetric flask, it is diluted with water to scale, is shaken up, clarification is placed；
B, 1.00mL supernatant is pipetted in 10mL polyethylene tube, is diluted to scale with nitric acid (2+98), is shaken up, to
It surveys；
5) configuration calibration solution, point take tin standard working solution that 0mL, 0.5mL, 5mL, 10mL concentration are 1ug/mL and 5mL,
10mL, 20mL concentration are 10ug/mL tin standard working solution in 100mL volumetric flask, and 10mL blank solution is added, is diluted with water to
Scale shakes up；
6) Specimen Determination
A, starting icp ms, selection analysis mass number and internal standard member are provided according to instrumentation
Element works out sample analysis method；
B, it tunes：Plasma flare stablizes 30min or so after working normally, with Li (lithium), Co containing 2ng/mL
(cobalt), In (indium), Ce (cerium), U (uranium) standard solution optimize instrument parameters, reach optimum sensitivity and best resolution
Rate introduces internal standard element mixed solution by threeway in continuous mode online；
C, it calibrates：To calibrate blank solution as zero point, the standard solution of several concentration levels establishes calibration curve, calibration
Data acquire at least 3 times, are averaged；
D, when every batch of sample measures, while measurement experiment room blank reagent solution；
E, the intermediate cleaning blank solution cleaning system of sample measurement；
8) calculated result
The amount of determinand in sample is calculated according to formula：
In formula：
ω (B) --- the mass fraction of determinand B in sample, unit are every gram of microgram (μ g/g)；
ρ --- the mass concentration of determinand in measurement solution, unit are nanograms per milliliter (ng/mL)；
ρ0--- the mass concentration of determinand in laboratory reagent blank solution, unit are nanograms per milliliter (ng/mL)；
V0--- preparation solution total volume, unit are milliliter (mL)；
V --- measurement liquor capacity, unit are milliliter (mL)；
M --- the quality of sample is weighed, unit is gram (g)；
V1--- point measurement liquid taken product, unit are milliliter (mL)；
Calculated result is expressed as：0.xx, x.xx, xx.x, xxx, unit are every gram of microgram (μ g/g).
Further, in step 5), tin standard that the tin standard working solution and concentration that concentration is 1ug/mL are 10ug/mL
Working solution is prepared according to the following steps respectively,
A, tin Standard Stock solutions are prepared：The 0.1000g metallic tin that purity is 99.99% is weighed, 250mL beaker is placed in
In, ρ 1.19g/mL, GR grades of hydrochloric acid 100mL is added overnight to being completely dissolved, 100mL water is added, stirs evenly, moves into 1000mL and holds
In measuring bottle and it is diluted to scale, is shaken up, tin mass concentration is 100ug/mL in the titer；
B, tin standard working solution is prepared：Tin Standard Stock solutions 10mL is in 100mL volumetric flask made from removing step A
In, it is diluted with water to scale, is shaken up, the concentration of this solution is 10ug/mL；Removing step A Plays stock solution 1mL in
In 100mL volumetric flask, it is diluted with water to scale, is shaken up, the concentration of this solution is 1ug/mL；
C, internal standard element standard solution is prepared
Rhodium Standard Stock solutions：The spectroscopic pure chlorine rhodium acid ammonium 3.5928g dried is weighed in 50mL beaker, 10mL is added
Hydrochloric acid and the dissolution of a small amount of sodium chloride, move into 1000mL volumetric flask, with hydrochloric acid (1+9) constant volume, shake up, rhodium matter in the standard solution
Amount concentration is 1mg/mL；
Rhodium internal standard element working solution：It is taken in the dilution certain multiple preparation of rhodium single element standard solution with ρ Rh=2ug/mL
Mark rhodium element solution, content 2ng/mL.
Further, the sample partial size in step 1) is less than 0.074mm, first in 105 DEG C of predrying 2h~4h, is placed in drying
It in device, is cooled to room temperature, is fitted into spare in ground glass stoppered bottle.
Preferably, in a step of step 4), sample higher for the content of organic matter is first placed in calcination in 650 DEG C of Muffle furnaces
1h。
Sample of the invention moves on in volumetric flask through sodium peroxide fusion and decomposition, hot water leaching, hydrochloric acid acidification, solution, point
Take clarified solution, after being diluted with nitric acid, sample enters radio frequency plasma by sampling system, and in high temperature quarter bend evaporation, from
Solution, atomization and ionization, ion is by bipyramid interface, ion mirror, level four bars mass analyzer, according to the size of mass/charge
It successively separates, is finally detected by ion detector, and with the amount of calibration curve quantitative analysis tin, so as to quick, smart
Really, the content of tin in tin ore is effectively measured.Meanwhile the method improves work efficiency, the labour for reducing operator is strong
Degree, and harm will not be generated to the body of operator, thus also there is significant social benefit.
Specific embodiment
It is described further With reference to embodiment：
In the present embodiment,
1, prepare reagent and material：
1.1 secondary deionized waters meet assay laboratory's second level water requirement of GB/T 6682.
The analysis of 1.2 sodium peroxides is pure
GR grades of 1.3 nitric acid (ρ 1.42g/mL)
1.4 nitric acid (2+98)
GR grades of 1.5 hydrochloric acid (ρ 1.19g/mL)
1.6 winestone acid analysis are pure
1.7 tin Standard Stock solutions (ρ Sn=100ug/mL) (or commercially available have card standard solution)
Tin Standard Stock solutions：0.1000g metallic tin (99.99%) is weighed, is placed in 250mL beaker, 100mL salt is added
Sour (1.5) are added 100mL water, stir evenly to being completely dissolved (overnight), move into 1000mL volumetric flask and are diluted to scale, shake up.
Tin mass concentration is 100ug/mL in the titer.
1.8 tin standard working solutions
a：1.7 Plays stock solution 10mL are pipetted in 100mL volumetric flask, scale is diluted with water to, shakes up, this solution
Concentration be 10ug/mL.
b：1.7 Plays stock solution 1mL are pipetted in 100mL volumetric flask, scale is diluted with water to, shakes up, this solution
Concentration be 1ug/mL.
1.9 internal standard element standard solution
a：Rhodium Standard Stock solutions：The spectroscopic pure chlorine rhodium acid ammonium 3.5928g dried is weighed in 50mL beaker, is added
10mL hydrochloric acid and the dissolution of a small amount of sodium chloride, move into 1000mL volumetric flask, with hydrochloric acid (1+9) constant volume, shake up.In the standard solution
Rhodium mass concentration is 1mg/mL.
b：Rhodium internal standard element working solution：(ρ Rh=2ug/mL) takes rhodium single element standard solution dilution certain multiple to prepare
Internal standard rhodium element solution, content 2ng/mL.
1.10 instruments tune solution
There is card mixture of multi-elements Standard Stock solutions (Li Co In Ce U) 10ug/mL nitric acid (1.4) dilution with commercially available
The mixed solution for being 2ng/mL at concentration, shakes up, for instrument tuning and mass calibration before analyzing.
1.11 blank solution
(a) blank solution is calibrated：Process white
(b) blank solution is cleaned：Nitric acid solution (2+98)
2, instrument and device
2.1 icp ms
(a) instrument quality scanning range 5u~250u, minimum resolution are 1u peak width, peristaltic pump threeway at 5% peak height
Sample introduction, the running parameter by taking quadrupole rod Inductively coupled plasma mass spectrometry as an example are shown in Table A.
(b) argon gas：High-purity grade (argon mass fraction >=99.99%).
2.2 argon gas：High-purity grade, purity are greater than 99.99%.
2.3 three-level electronic balances：Sensibility reciprocal 0.1mg.
3, sample
3.1 sample partial sizes should be less than 0.074mm.
3.2 samples should be placed in drier, be cooled to room temperature, be fitted into ground glass stoppered bottle in 105 DEG C of predrying 2h~4h
It is spare.
4 analytical procedures
4.1 accordings to the form below weigh sample, are accurate to 0.1mg.
| Sn amount (ug/g) | Sample weighting amount (g) |
| 10-1000 | 0.4 |
| 1000-10000 | 0.2 |
| 10000-30000 | 0.1 |
4.2 blank test
Duplicate blank test is carried out in company with sample, agents useful for same is derived from same bottle, same amount is added.
4.3 verification test
In company with national standard substance similar in sample analysis same type, content.
4.4 samples decompose
4.4.1 sample (4.1) is placed in corundum crucible, is added 2g sodium peroxide (1.2), stirs evenly, cover one again above
Layer sodium peroxide, is put into 750 DEG C of high temperature furnaces and melts 10min, and after taking out cooling, crucible is put into the beaker for filling 30mL boiling water
In, it is added 0.2g tartaric acid (1.6), it is slightly cold, hydrochloric acid (1.5) 15mL is added, after fusant is completely fallen off, crucible is washed with water out,
It is cooled to room temperature, solution moves into 100mL volumetric flask, is diluted with water to scale, shakes up, and places clarification.
If the content of organic matter is higher, the preparatory calcination 1h in 650 DEG C of Muffle furnaces is needed after claiming sample.
4.4.2 1.00mL (4.4.1) supernatant is pipetted in 10mL polyethylene tube, is diluted to scale with nitric acid (1.4),
It shakes up, it is to be measured.
4.5 calibration solution allocations
Divide and takes 0mL, 0.5mL, 5mL, 10mL tin standard working solution (1.8b), 5mL, 10mL, 20mL tin standard working solution
(1.8a) is added 10mL process white solution (1.11a) in 100mL volumetric flask, is diluted to scale with water (1.1), shakes up.
4.6 Specimen Determination
4.6.1 start instrument according to instrumentation specification rated condition.Selection analysis mass number and internal standard element, establishment
Sample analysis method.
4.6.2 tuning：Plasma flare stablizes 30min or so after working normally, with Li, Co containing 2ng/mL, In,
Ce, U standard solution (1.10) optimize instrument parameters, reach optimum sensitivity and optimum resolution.In continuous mode
In, introduce internal standard element mixed solution (1.9b) online by threeway.
4.6.3 calibration：To calibrate blank solution (1.11a) as zero point, the standard solution of multiple concentration levels establishes calibration
Curve.It calibration data acquisition at least 3 times, is averaged.
4.6.4 when every batch of sample measures, while measurement experiment room blank reagent solution.
4.6.5 intermediate cleaning blank solution (1.11b) cleaning system of sample measurement.
5, result calculates
5.1 Analysis result calculation
The amount of determinand in sample is calculated as follows：
In formula：
ω (B) --- the mass fraction of determinand B in sample, unit are every gram of microgram (μ g/g)；
ρ --- the mass concentration of determinand in measurement solution, unit are nanograms per milliliter (ng/mL)；
ρ0--- the mass concentration of determinand in laboratory reagent blank solution, unit are nanograms per milliliter (ng/mL)；
V0--- preparation solution total volume, unit are milliliter (mL)；
V --- measurement liquor capacity, unit are milliliter (mL)；
M --- the quality of sample is weighed, unit is gram (g)；
V1--- point measurement liquid taken product, unit are milliliter (mL).
Calculated result is expressed as：0.xx, x.xx, xx.x, xxx, unit are every gram of microgram (μ g/g).
5.2 precision and correctness
According to GB/T6392.2-2004, select standard substance 9 of different quality containing range, by 9 laboratories according to
This method carries out method precision experiment.Each horizontal sample is tested in each laboratory 5 times, and initial data is carried out statistical
Analysis, analysis method precision are shown in Table 1, and analysis method correctness is shown in Table 2.
1 analysis method precision of table
| Element | Horizontal extent m | Repeatability limit r | Reproducibility limits R |
| Sn | 12.5~12700 | R=0.0557m+0.1455 | R=0.081m-4.5379 |
2 analysis method correctness of table
6, quality assurance and control
6.1 control method
6.1.1 require analyst can skilled operation level four bars Inductively coupled plasma mass spectrometry, the interference of understanding mass spectrum and base
Principle that soma is disturbed simultaneously can be carried out interference correction.
6.1.2 when every batch of assaying, blank test, the methods of repeating sample analysis, standard substance verifying should be used simultaneously
Carry out quality assurance and control.
6.1.3 elemental standards stock solution should be checked to avoid the accuracy of impurity effect standard.
6.1.4 if analyte concentration is sufficiently high, it should be diluted that (Cmin after dilution should be at least 10 step by step
Times method detection limit).
6.1.5 analyst should monitor the response of the internal standard during entire sample analysis and internal standard and each analytical element signal
Ratio.80%~120% of interior target absolute response value deviation no more than initial response in calibration blank.If it exceeds this
Deviation should be analyzed and find out drift reason.
The quantity of 6.2 control samples
When every batch of sample analysis, repeated cryptanalysis is carried out by the sample that the total quantity of sample randomly selects 5%.
6.3 Con trolling index
6.3.1 correlation coefficient r >=0.999 of calibration curve
6.3.2 other Con trolling index are executed by DZ/T0130.3.
Running parameter of the Table A by taking certain quadrupole rod icp ms as an example
| Parameter | Setting value | Parameter | Setting value |
| ICP power | 1300w | Jump peak | 3 points/quality |
| Cooling gas flow | 14.0L/min | Residence time | 10ms/ point |
| Secondary air amount | 0.8L/min | Scanning times | 40 times |
| Atomization gas flow | 1.0L/min | Time of measuring | 60s |
| Sampling spiroid aperture | 1.2mm | Intercept taper hole diameter | 1.0mm |
The above has been described in detail, described above, is only a preferred embodiment of the present invention, when cannot
Limit practical range of the invention, i.e., it is all according to the made equivalent changes and modifications of the application range, it should still belong to the present invention and cover model
In enclosing.
Claims (4)
1. the method for tin amount in a kind of alkali fusion-inductively coupled plasma mass spectrometry measurement tin ore, it is characterised in that：Sample warp
Sodium peroxide decomposes, and hot water leaching, hydrochloric acid acidification, solution moves on in volumetric flask, divides and take clarified solution, dilute with nitric acid (2+98)
After releasing, sample enters radio frequency plasma by sampling system, and evaporation, dissociation, atomization and ionization in high temperature quarter bend, from
Son is successively separated by bipyramid interface, ion mirror, level four bars mass analyzer, according to the size of mass/charge, finally by ion
Detector is detected, and with the amount of calibration curve quantitative analysis tin, and instrument response caused by sample matrices inhibits or enhancing
Effect and instrumental shift are compensated using internal standard, and specific determination step is as follows,
1) sample is weighed；
2) blank test carries out duplicate blank test in company with sample, and agents useful for same is derived from same bottle, same amount is added；
3) verification test, in company with national standard substance similar in sample analysis same type, content；
4) sample decomposes
A, sample is placed in corundum crucible, 2g sodium peroxide is added, stirs evenly, covers one layer of sodium peroxide again above, be put into 750
10min is melted in DEG C high temperature furnace, take out it is cooling after, crucible is put into the beaker for filling 30mL boiling water, 0.2g tartaric acid is added,
It is slightly cold, hydrochloric acid 15mL is added after fusant is completely fallen off, crucible is washed with water out, is cooled to room temperature, solution moves into 100mL capacity
In bottle, it is diluted with water to scale, is shaken up, places clarification；
B, 1.00mL supernatant is pipetted in 10mL polyethylene tube, is diluted to scale with nitric acid (2+98), is shaken up, it is to be measured；
5) configuration calibration solution, point take tin standard working solution that 0mL, 0.5mL, 5mL, 10mL concentration are 1ug/mL and 5mL,
10mL, 20mL concentration are 10ug/mL tin standard working solution in 100mL volumetric flask, and 10mL blank solution is added, is diluted with water to
Scale shakes up；
6) Specimen Determination
A, starting icp ms, selection analysis mass number and internal standard element are provided according to instrumentation, compiled
Sample analysis method processed；
B, it tunes：Plasma flare stablizes 30min or so after working normally, and is marked with Li, Co, In, Ce, U containing 2ng/mL
Quasi- solution optimizes instrument parameters, reaches optimum sensitivity and optimum resolution, in continuous mode, is existed by threeway
Line introduces internal standard element mixed solution；
C, it calibrates：To calibrate blank solution as zero point, the standard solution of several concentration levels establishes calibration curve, calibration data
Acquisition at least 3 times, is averaged；
D, when every batch of sample measures, while measurement experiment room blank reagent solution；
E, the intermediate cleaning blank solution cleaning system of sample measurement；
8) calculated result
The amount of determinand in sample is calculated according to formula：
In formula：
ω (B) --- the mass fraction of determinand B in sample, unit are every gram of microgram；
ρ --- the mass concentration of determinand in measurement solution, unit is nanograms per milliliter；
ρ0--- the mass concentration of determinand in laboratory reagent blank solution, unit are nanograms per milliliter；
V0--- preparation solution total volume, unit are milliliter；
V --- measurement liquor capacity, unit is milliliter；
M --- the quality of sample is weighed, unit is gram；
V1--- point measurement liquid taken product, unit is milliliter；
Calculated result is expressed as：0.xx, x.xx, xx.x, xxx, unit are every gram of microgram.
2. the method for tin amount in alkali fusion according to claim 1-inductively coupled plasma mass spectrometry measurement tin ore,
It is characterized in that：In step 5), the tin standard working solution that the tin standard working solution and concentration that concentration is 1ug/mL are 10ug/mL divides
It does not prepare according to the following steps,
A, tin Standard Stock solutions are prepared：The 0.1000g metallic tin that purity is 99.99% is weighed, is placed in 250mL beaker, adds
The hydrochloric acid 100mL for entering ρ 1.19g/mL, GR grades is added 100mL water, stirs evenly, move into 1000mL volumetric flask overnight to being completely dissolved
And it is diluted to scale, it shakes up, tin mass concentration is 100ug/mL in the titer；
B, tin standard working solution is prepared：Tin Standard Stock solutions 10mL made from removing step A is used in 100mL volumetric flask
Water is diluted to scale, shakes up, and the concentration of this solution is 10ug/mL；Removing step A Plays stock solution 1mL is in 100mL capacity
In bottle, it is diluted with water to scale, is shaken up, the concentration of this solution is 1ug/mL；
C, internal standard element standard solution is prepared
Rhodium Standard Stock solutions：The spectroscopic pure chlorine rhodium acid ammonium 3.5928g dried is weighed in 50mL beaker, 10mL hydrochloric acid is added
It is dissolved with a small amount of sodium chloride, moves into 1000mL volumetric flask, with hydrochloric acid (1+9) constant volume, shake up, rhodium quality is dense in the standard solution
Degree is 1mg/mL；
Rhodium internal standard element working solution：Rhodium single element standard solution dilution certain multiple is taken to prepare internal standard rhodium with ρ Rh=2ug/mL
Element Solution, content 2ng/mL.
3. the method for tin amount in alkali fusion according to claim 1-inductively coupled plasma mass spectrometry measurement tin ore,
It is characterized in that：Sample partial size in step 1) is less than 0.074mm and is placed in drier first in 105 DEG C of predrying 2h~4h, cold
But it to room temperature, is fitted into spare in ground glass stoppered bottle.
4. the method for tin amount in alkali fusion according to claim 1-inductively coupled plasma mass spectrometry measurement tin ore,
It is characterized in that：In a step of step 4), sample higher for the content of organic matter is first placed in calcination 1h in 650 DEG C of Muffle furnaces.
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| CN201910308150.1A CN110031535A (en) | 2018-08-02 | 2019-04-17 | The method that sodium peroxide inductivity coupled plasma mass spectrometry measures tin amount in tin ore |
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| CN104807808A (en) * | 2015-05-11 | 2015-07-29 | 梧州市产品质量检验所 | Method for detecting tin in ore |
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2018
- 2018-08-02 CN CN201810868904.4A patent/CN108828052A/en not_active Withdrawn
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2019
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| CN111398400B (en) * | 2020-03-31 | 2022-11-15 | 广西壮族自治区地质矿产测试研究中心 | Method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry |
| CN112697871A (en) * | 2020-12-31 | 2021-04-23 | 华仁药业股份有限公司 | Detection method of glucose electrolyte beverage tin |
| CN113358735A (en) * | 2021-06-02 | 2021-09-07 | 河北省地质实验测试中心(国土资源部保定矿产资源监督检测中心、河北省金银宝玉饰品质量监督检验站) | Method for decomposing cassiterite-containing mineral suitable for measuring tin content and application thereof |
| CN113358735B (en) * | 2021-06-02 | 2022-10-28 | 河北省地质实验测试中心(国土资源部保定矿产资源监督检测中心、河北省金银宝玉饰品质量监督检验站) | Method for decomposing cassiterite-containing mineral suitable for measuring tin content and application thereof |
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