CN107632011A - The assay method of impurity content in a kind of high purity bismuth - Google Patents
The assay method of impurity content in a kind of high purity bismuth Download PDFInfo
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- CN107632011A CN107632011A CN201710641690.2A CN201710641690A CN107632011A CN 107632011 A CN107632011 A CN 107632011A CN 201710641690 A CN201710641690 A CN 201710641690A CN 107632011 A CN107632011 A CN 107632011A
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Abstract
The invention discloses a kind of assay method of impurity content in high purity bismuth, it removes bismuth main body using HCl gaseous volatilizations, solve main body interference and main body removes cumbersome difficult point, using bismuth and hydrogen chloride gas precursor reactant generation bismuth trichloride and then the method for removal of volatilizing again, bismuthino body can be effectively removed, new impurity element will not be introduced, it effectively prevent the ambient interferences of main element, make element main peak to be measured more notable, sensitivity improves, and reappearance is high.The analysis method that the present invention uses, can be with multielement simultaneous determination, and easy to operate, analyze speed is fast, shortens analytical cycle, improves analysis efficiency, alleviates the labor intensity of analysis operation personnel.The content of impurity element in high purity bismuth is determined using the inventive method, its measurement result has good stability, reappearance and accuracy.Experiment proves that the inventive method is reliable, practical, can meet the requirement that the impurity content of production and scientific research high purity bismuth detects.
Description
Technical field
The invention belongs to test chemical technical field, and in particular to the measure side of impurity content in a kind of high purity bismuth
Method.
Background technology
Bismuth metal is more than 99.999% mainly for the manufacture of low-melting alloy, nuclear reactor coolant, bismuth salt etc., bismuth-containing
Pure bismuth is high pure metal bismuth, is widely used in prepare compound semiconductor, high purity alloys, electronic cooling element, thermoelectric conversion element
And liquid cooled carrier etc. in the nuclear reactor, research and development high purity bismuth have broad prospects.As high purity bismuth is each
The extensive use and further investigation in individual field, in high purity bismuth the detection of impurity content be increasingly taken seriously.Standard GB/T/
Impurity in the methods of GFAAS is used in T 91521995 measure bismuth metal, but the method must carry out Matrix Match, and analysis process is grown,
Precision is poor.Also someone uses strong-base anion-exchange resin separation of Bismuth matrix, inductively coupled plasma mass spectrometry measure
Impurity in bismuth metal, but in the method bismuthino body minimizing technology it is cumbersome, easily error.
The content of the invention
In view of this, the invention provides a kind of assay method of impurity content in high purity bismuth, this method operation letter
It is single, conveniently, can effectively remove bismuthino body, measurement result has good stability, reappearance and accuracy, meet production and
The requirement of the impurity content detection of scientific research high purity bismuth.
To solve above technical problem, the technical scheme is that the survey using impurity content in a kind of high purity bismuth
Determine method, it comprises the following steps：
(1) standard curve is established：
Using the spectral intensity of impurity element in spectrographic determination impurity element standard solution, standard curve is established, institute
It is silver element, cadmium element, copper, nickel element, lead element, magnesium elements or gold element to state impurity element；
(2) high purity bismuth testing sample is handled：
Weigh a certain amount of high purity bismuth testing sample and be dissolved in salpeter solution and evaporate, add appropriate hydrochloric acid solution to dissolve, then
2~3h of hydrogen chloride gas is passed through under conditions of 280 DEG C to obtain separating the sample after main body, the sample hydrochloric acid solution that will be obtained
Solution to be measured is obtained after dissolving；
(3) test comparison is analyzed：
It is bent according to spectral intensity and the standard of foundation using the spectral intensity of impurity element in spectrographic determination solution to be measured
Line, the content of impurity element in high purity bismuth is calculated.
Further, the preparation method of impurity element standard solution is in the step (1)：By impurity element standard female
Liquid is placed in volumetric flask, is 1 with volume ratio：9 salpeter solution constant volume, shake up and produce；The impurity element standard mother liquor is silver
Elemental standards liquid, cadmium element titer, copper titer, nickel element titer, lead element titer, magnesium elements titer or
Gold element titer.
Preferably, above-mentioned spectroscopic methodology is inductively coupled plasma emission spectrography (ICP-OES), have it is quantitative accurate,
Analyze speed is fast, the range of linearity is wide, high sensitivity, can analyze the characteristics of multiple element simultaneously.
Preferably, the accuracy of above-mentioned steps (2) high purity bismuth amount of weighing is 0.001g, and the amount of weighing is with 3.000g ± 1.000g
It is advisable.
Preferably, the volume by volume concentration of salpeter solution is 1 in above-mentioned steps (2):9.
Preferably, the volume by volume concentration of hydrochloric acid solution is 1 in above-mentioned steps (2):9.
Preferably, the purity of high purity bismuth is Bi-05 or Bi-06 in above-mentioned steps (2).The trade mark of high purity bismuth is according to coloured row
Industry standard (YS/T 818-2012) is divided into Bi-05, Bi-06 etc. by purity, bismuth-containing amount more than 99.999% for Bi-05, bismuth-containing
Amount is Bi-06 more than 99.9999%.
Preferably, the measurement range of the inventive method impurity content is following mass ratioes：
Copper, silver, gold：1.2×10-4~1 × 10-6%
Cadmium, nickel, lead, magnesium：1×10-4~5 × 10-6%.
The impurity element in high purity bismuth is determined using inductively coupled plasma emission spectrography, due to miscellaneous in high purity bismuth
The content of prime element is extremely low, and the presence of bismuth main body, its main body background easily covers the main peak of impurity element to be measured, causes member to be measured
Cellulose content it is relatively low, it is therefore desirable to will bismuth main body remove after detected again.Compared with prior art, the present invention uses HCl gas
Body volatilization removes bismuth main body, solves main body interference and main body removes cumbersome difficult point, this method is simple, convenient, can have
Effect removes bismuthino body, the method for generating bismuth trichloride and then removal of volatilizing again using bismuth and hydrogen chloride gas precursor reactant, will not introduce
New impurity element, the background influence of main element is effectively prevent, make element main peak to be measured more notable, sensitivity improves, weight
Existing property is high.The analysis method that the present invention uses, can be with multielement simultaneous determination, and easy to operate, analyze speed is fast, shortens analysis
In the cycle, analysis efficiency is improved, alleviate the labor intensity of analysis operation personnel.Determined using the inventive method miscellaneous in high purity bismuth
The content of prime element, its measurement result have good stability, reappearance and accuracy.Experiment proves that the inventive method can
Lean on, be practical, the requirement that the impurity content of production and scientific research high purity bismuth detects can be met.
Embodiment
In order that those skilled in the art more fully understands technical scheme, the present invention is made below further
Detailed description.
The invention provides a kind of assay method of impurity content in high purity bismuth, it comprises the following steps：
(1) standard curve is established：
Using the spectral intensity of impurity element in spectrographic determination impurity element standard solution, standard curve is established, institute
It is silver element, cadmium element, copper, nickel element, lead element, magnesium elements or gold element to state impurity element；
(2) high purity bismuth testing sample is handled：
Weigh a certain amount of high purity bismuth testing sample and be dissolved in salpeter solution and evaporate, add appropriate hydrochloric acid solution to dissolve, then
Hydrogen chloride gas is passed through under conditions of 280 DEG C, 2~3h obtains separating the sample after main body, and obtained sample hydrochloric acid is molten
Solution to be measured is obtained after liquid dissolving；
(3) test comparison is analyzed：
It is bent according to spectral intensity and the standard of foundation using the spectral intensity of impurity element in spectrographic determination solution to be measured
Line, the content of impurity element in high purity bismuth is calculated.
Preferably, above-mentioned spectroscopic methodology is inductively coupled plasma emission spectrography (ICP-OES), have it is quantitative accurate,
Analyze speed is fast, the range of linearity is wide, high sensitivity, can analyze the characteristics of multiple element simultaneously.In the present invention, the inductance coupling
Close plasma emlssion spectrometry test process be：Argon gas produces plasma in the presence of high frequency magnetic field, will be a series of
Impurity element standard solution sample introduction successively, the negative pressure formed is flowed by argon gas sample solution is sucked into capillary, via mist
Change device formed aerosol simultaneously enter torch pipe, in thermal-flame plasma concurrently project characteristic spectral line, test impurity element
Spectral intensity, its spectral intensity are directly proportional to corresponding impurity content.
In the present invention, the preparation method of impurity element standard solution is in the step (1)：By impurity element standard
Mother liquor is placed in volumetric flask, is 1 with volume ratio：9 salpeter solution constant volume, shake up and produce；The impurity element standard mother liquor is
Silver element titer, cadmium element titer, copper titer, nickel element titer, lead element titer, magnesium elements titer
Or gold element titer.Described impurity element standard mother liquor is the commercially available impurity list mark prepared by china institute of metrology
Elemental standard solution, its mass concentration are 10 μ g/ml.
Preferably, the accuracy of the high purity bismuth amount of weighing is 0.001g in above-mentioned steps (2), the amount of weighing with 3.000 ±
1.000g it is advisable；The volume by volume concentration of salpeter solution is 1：9；The volume by volume concentration of hydrochloric acid solution is 1：9；The purity of high purity bismuth is
Bi-05 or Bi-06.
Preferably, the measurement range of the inventive method impurity content is following mass ratioes：
Copper, silver, gold：1.2×10-4~1 × 10-6%
Cadmium, nickel, lead, magnesium：1×10-4~5 × 10-6%.
The inventive method is described further with reference to specific embodiment, in following embodiments, inductive
Plasma emission spectrometer (ICP-OES) sets pre- spray time as 30s, and it is 20s to clean the time, ICP-OES running parameters
It see the table below：
The present invention does not have special limitation to the method for establishing spectral intensity-mass fraction standard curve, using this area
The technical scheme of standard curve is established known to technical staff.The foundation of the standard curve is preferred in the following embodiments
Following technical scheme：
A series of impurity element standard solution of various concentrations is surveyed using inductively coupled plasma emission spectrography
Examination, the spectral intensity of impurity element in impurity element standard solution is tested, according to the impurity element mark of obtained various concentrations
Standard draws the function curve of impurity element concentration and spectral intensity corresponding relation, as standard curve using the spectral intensity of liquid.
In the present invention, the concentration of impurity element is in a series of impurity element standard solution of various concentrations
Know.The present invention is using above-mentioned specific impurity element titer salpeter solution (1：9) a series of impurity element mark is prepared
Standard uses liquid.
In a particular embodiment of the present invention, a series of silver element standard solution, cadmium element standard solution, copper coin
Plain standard solution, nickel element standard solution, lead element standard solution, magnesium elements standard solution, gold element standard make
It is respectively 0.0 μ g/ml, 0.2 μ g/ml, 0.4 μ g/ml, 0.8 μ g/ml and 1.6 μ g/ml with the mass concentration of liquid.
Embodiment 1：
It is miscellaneous in high purity bismuth product Bi-05 using being detected after HCl gaseous volatilizations of the present invention removal bismuth main body with ICP-OES methods
Prime element content, it is specially：
3.000 grams of samples are weighed, are accurate to 0.001 gram.In company with the blank amount of sample measurement impurity element.Sample is placed in
In silica crucible, heating, the dissolving of 4-6ml nitric acid is added dropwise, heating evaporation, dissolving with hydrochloric acid is added dropwise and obtains testing liquid.By containing, experiment is molten
It is indoor that the crucible of liquid is placed in volatilization, connects device and starts water-jet pump, electrified regulation, rotates dropping funel piston at about 200 DEG C, to
Hydrochloric acid is added dropwise in the sulfuric acid of boiling flask, hydrogen chloride gas is occurred with the continuous countably speed of bubble, acts on, protects with testing liquid
Hold 280 ± 30 DEG C of volatilizations and eliminate bismuth trichloride (about needing 2.5h), stop heating and continue ventilation 10 minutes.Stop ventilation, take out stone
English crucible, add 10% dissolving with hydrochloric acid residue and obtain prepare liquid, be settled to 3ml, it is measured in ICP-OES.
Obtained spectral intensity result will be determined compared with standard curve, be calculated using the Return Law in sample respectively
The content of impurity element.
According to above-mentioned test method, same high purity bismuth product Bi-05 replications are no less than 6 times, analysis result is seen below
Shown in table：
Embodiment 2：
It is miscellaneous in high purity bismuth product Bi-06 using being detected after HCl gaseous volatilizations of the present invention removal bismuth main body with ICP-OES methods
Prime element content, it is specially：
3.000 grams of samples are weighed, are accurate to 0.001 gram.In company with the blank amount of sample measurement impurity element.Sample is placed in
In silica crucible, low-temperature heat, the dissolving of 4-6ml nitric acid is added dropwise, heating evaporation, dissolving with hydrochloric acid is added dropwise and obtains testing liquid.Tried containing
Testing the crucible of solution, to be placed in volatilization indoor, connects device and starts water-jet pump, electrified regulation, and rotating dropping funel at about 200 DEG C lives
Plug, hydrochloric acid is added dropwise into the sulfuric acid of boiling flask, and hydrogen chloride gas occurs with the continuous countably speed of bubble, makees with testing liquid
With 280 ± 30 DEG C of volatilizations of holding eliminate bismuth trichloride (about needing 2.5h), stop heating and continue ventilation 10 minutes.Stop ventilation, take
Go out silica crucible, add 10% dissolving with hydrochloric acid residue and obtain prepare liquid, be settled to 3ml, it is measured in ICP-OES.
Obtained spectral intensity result will be determined compared with standard curve, be calculated using the Return Law in sample respectively
The content of impurity element.
According to above-mentioned test method, same high purity bismuth product Bi-06 replications are no less than 6 times, analysis result is seen below
Shown in table：
As can be seen that each impurity element contains in the inventive method detection high purity bismuth sample from the table of Examples 1 and 2
Amount, each testing result are more or less the same, and its measurement result has good stability, reappearance and accuracy, its relative standard
Deviation (RSD) is respectively less than 1%, meets analysis measure and requires.
In summary, the inventive method simply, conveniently, effectively eliminates bismuth main body, solves main body interference and main body is gone
Except cumbersome difficult point, the method for generating bismuth trichloride and then removal of volatilizing again using bismuth and hydrogen chloride gas precursor reactant, will not introduce
New impurity element, the background influence of main element is effectively prevent, make element main peak to be measured more notable, sensitivity improves, weight
Existing property is high.
It the above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
The limitation of the present invention, protection scope of the present invention should be defined by claim limited range.For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, some improvements and modifications can also be made, these change
Enter and retouch and also should be regarded as protection scope of the present invention.
Claims (10)
- A kind of 1. assay method of impurity content in high purity bismuth, it is characterised in that：Comprise the following steps：(1) standard curve is established：Using the spectral intensity of impurity element in spectrographic determination impurity element standard solution, standard curve is established, it is described miscellaneous Prime element is silver element, cadmium element, copper, nickel element, lead element, magnesium elements or gold element；(2) high purity bismuth testing sample is handled：Weigh a certain amount of high purity bismuth testing sample and be dissolved in salpeter solution and evaporate, dissolved with appropriate hydrochloric acid solution, then 280 Hydrogen chloride gas is passed through under conditions of ± 15 DEG C, 2~3h obtains separating the sample after main body, the sample hydrochloric acid solution that will be obtained Solution to be measured is obtained after dissolving；(3) test comparison is analyzed：Using the spectral intensity of impurity element in spectrographic determination solution to be measured, according to spectral intensity and the standard curve of foundation, The content of impurity element in high purity bismuth is calculated.
- 2. the assay method of impurity content in a kind of high purity bismuth according to claim 1, it is characterised in that：Described Spectroscopic methodology is inductively coupled plasma emission spectrography.
- 3. the assay method of impurity content in a kind of high purity bismuth according to claim 1, it is characterised in that：The step Suddenly the preparation method of impurity element standard solution is in (1)：Impurity element standard mother liquor is placed in volumetric flask, it is molten with nitric acid Liquid constant volume, shake up and produce；The impurity element standard mother liquor be silver element titer, cadmium element titer, copper titer, Nickel element titer, lead element titer, magnesium elements titer or gold element titer.
- 4. the assay method of impurity content in a kind of high purity bismuth according to claim 3, it is characterised in that：It is described fixed The salpeter solution volume by volume concentration of appearance is 1：9.
- 5. the assay method of impurity content in a kind of high purity bismuth according to claim 1, it is characterised in that：The step Suddenly the accuracy of the high purity bismuth amount of weighing is 0.001g in (2).
- 6. the assay method of impurity content in a kind of high purity bismuth according to claim 1, it is characterised in that：The step Suddenly the amount of weighing of high purity bismuth is 3.000g ± 1.000g in (2).
- 7. the assay method of impurity content in a kind of high purity bismuth according to claim 1, it is characterised in that：The step Suddenly the volume by volume concentration of salpeter solution is 1 in (2)：9.
- 8. the assay method of impurity content in a kind of high purity bismuth according to claim 1, it is characterised in that：The step Suddenly the volume by volume concentration of hydrochloric acid solution is 1 in (2)：9.
- 9. the assay method of impurity content in a kind of high purity bismuth according to claim 1, it is characterised in that：The step Suddenly the purity of high purity bismuth is Bi-05 or Bi-06 in (2).
- 10. the assay method of impurity content in a kind of high purity bismuth according to claim 1, it is characterised in that：This hair The measurement range of bright method impurity content is following mass ratioes：Copper, silver, gold：1.2×10-4~1 × 10-6%Cadmium, nickel, lead, magnesium：1×10-4~5 × 10-6%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108572213A (en) * | 2018-04-24 | 2018-09-25 | 株洲科能新材料有限责任公司 | A kind of high purity tellurium impurity enriched device and its method for 5N grades of tellurium analysis detections |
| KR20200039144A (en) * | 2018-10-05 | 2020-04-16 | 주식회사 엘지화학 | Method for analyzing contents of bi in inorganic materials |
| CN111999154A (en) * | 2020-08-28 | 2020-11-27 | 戚紫宣 | Method for detecting element content in alloy raw material |
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| CN103926372A (en) * | 2014-03-26 | 2014-07-16 | 湖南水口山有色金属集团有限公司 | Method for measuring content of silver in high-bismuth material |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103926372A (en) * | 2014-03-26 | 2014-07-16 | 湖南水口山有色金属集团有限公司 | Method for measuring content of silver in high-bismuth material |
Non-Patent Citations (1)
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| 胡汉祥等: "电感耦合等离子体原子发射光谱法测定铋及氧化铋中5种杂质元素", 《冶金分析》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108572213A (en) * | 2018-04-24 | 2018-09-25 | 株洲科能新材料有限责任公司 | A kind of high purity tellurium impurity enriched device and its method for 5N grades of tellurium analysis detections |
| KR20200039144A (en) * | 2018-10-05 | 2020-04-16 | 주식회사 엘지화학 | Method for analyzing contents of bi in inorganic materials |
| KR102431337B1 (en) | 2018-10-05 | 2022-08-09 | 주식회사 엘지화학 | Method for analyzing contents of bi in inorganic materials |
| CN111999154A (en) * | 2020-08-28 | 2020-11-27 | 戚紫宣 | Method for detecting element content in alloy raw material |
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