CN103645165B - Measure the method for Se content in molybdenum and molybdenum product - Google Patents
Measure the method for Se content in molybdenum and molybdenum product Download PDFInfo
- Publication number
- CN103645165B CN103645165B CN201310619007.7A CN201310619007A CN103645165B CN 103645165 B CN103645165 B CN 103645165B CN 201310619007 A CN201310619007 A CN 201310619007A CN 103645165 B CN103645165 B CN 103645165B
- Authority
- CN
- China
- Prior art keywords
- solution
- molybdenum
- sample
- concentration
- selenium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The method of Se content in mensuration molybdenum disclosed by the invention and molybdenum product, comprise sampling, prepare sample solution and sample blank solution, Se content in preparation work curve solution, drawing curve, working sample solution and calculate six steps, the method of Se content in mensuration molybdenum of the present invention and molybdenum product, solves the problem that Se content that existing By Hydride Generation-atomic Fluorescence Spectrometry cannot be applied to molybdenum and molybdenum product because the selenium hydride of molybdenum is difficult to be formed is measured.Assay method of the present invention, easy and simple to handle, efficiency is high, highly sensitive, detect and be limited to 0.13ng/mL, the recovery is 90.23% ~ 105.1%, and the measurement range of Se content is 0.0001% ~ 0.0050%.
Description
Technical field
The invention belongs to trace impurity analysis technical field, a kind of concrete method measuring Se content in molybdenum and molybdenum product.
Background technology
Along with industrial expansion, new material is constantly released, and various excellent performance material is further strict to the requirement of its composition, and in metal, the impact of content on material property of impurity element is most important.Molybdenum and molybdenum product, as highly purified starting material, first must control raw-material impurity component, only have highly purified starting material, could smelt highly purified quality matetrial.As requested, in molybdenum and molybdenum product, the content of selenium must not more than 10/1000000ths (10ppm).
According to the difference of measured Se content, the conventional method measuring Se content in metal has: inductively coupled plasma spectrometry method (ICP-AES), Inductively coupled plasma-mass spectrometry (ICP-MS), atomic absorption spectrography (AAS) (AAS), By Hydride Generation-atomic Fluorescence Spectrometry (HG-AFS), spectrophotometric method and oscilloscopic polarography.
Atomic fluorescence spectrometry proposes middle 1960s and the novel spectral analysis technique grown up, and being one of three large branches (AES, AAS, AFS) in atomic spectroscopy, is a kind of new trace, extreme trace analysis technology.It has Atomic absorption and atomic emission spectrum two kinds of technical advantages, and overcome the shortcoming of their some aspects, there is sensitivity for analysis high, interference less, the range of linearity is wide, can the feature of Simultaneous multi element analysis, be a kind of excellent trace, extreme trace analysis technology.
Inductively coupled plasma spectrometry method (ICP-AES), Inductively coupled plasma-mass spectrometry (ICP-MS), when measuring elemental selenium, due to serious interference, cause measurement to detect limit for height.
Atomic absorption spectrography (AAS) (AAS) complex disposal process, sensitivity is relatively low.
Spectrophotometric method detects limit for height, pollution is large and cost is high.
By Hydride Generation-atomic Fluorescence Spectrometry (HG-AFS) is that develop out on existing atomic fluorescence spectrometry basis a kind of up-to-date carries out method for measuring to Se content.It combines the advantage of atomic absorption spectroscopy and Atomic Emission Spectral Analysis method two kinds of technology, and overcome their respective shortcomings, there is very high sensitivity for analysis, interference less, the range of linearity is wide, instrument price is cheap, processing procedure is simple, at present, this technology oneself be more and more subject to people's attention.But existing By Hydride Generation-atomic Fluorescence Spectrometry is applied to the aspect such as food, biology more, it is applied to the analysis of Se content in molybdenum and molybdenum product, there is following difficulty: in molybdenum and molybdenum product, selenium hydride is difficult to be formed, and therefore follow-up test cannot launch; And adopt other method existing also cannot carry out Accurate Determining for Determination of Trace Selenium in molybdenum and molybdenum product.
Summary of the invention
The object of the present invention is to provide a kind of method measuring Se content in molybdenum and molybdenum product, solve the problem that Se content that existing By Hydride Generation-atomic Fluorescence Spectrometry cannot be applied to molybdenum and molybdenum product because the selenium hydride of molybdenum is difficult to be formed is measured.
The technical solution adopted in the present invention is: the method measuring Se content in molybdenum and molybdenum product, comprises the steps:
The first step, sampling
Get molybdenum powder to be determined, carry out at least twice division according to inquartation, obtain sample; Or get molybdenum bar to be determined, first molybdenum bar is pulverized, and sieve with the standard screen cloth that mesh diameter is 0.75mm, obtain sample;
Second step, prepares sample solution and sample blank solution
Get two beakers, the sample that the first step is obtained is put in one of them beaker, and add water and carry out moistening to sample, then in two beakers, hydrochloric acid solution A and salpeter solution is added respectively, cover surface plate, heat two beakers respectively until sample dissolves completely, again respectively to adding citric acid solution in two beakers and boiling, surface plate and walls of beaker is rinsed with water after cooling, add urea liquid respectively again, then the solution in two beakers is moved in two volumetric flasks respectively, hydrochloric acid solution B is added again respectively in two volumetric flasks, last dilute with water, and mix, obtained sample solution and sample blank solution respectively,
3rd step, preparation work curve solution
Get Mo substrate, and described Mo substrate is divided into six equal portions, six parts of Mo substrate are dropped into respectively in six beakers, add water moistening, add hydrochloric acid solution C respectively again, salpeter solution, cover surface plate, heating makes Mo substrate dissolve completely, add citric acid solution respectively and boil, surface plate and walls of beaker is rinsed with water after cooling, add urea liquid respectively again, then the solution of six beakers is moved to respectively in six volumetric flasks, add hydrochloric acid solution D respectively again, then in six beakers, 0.00mL is added respectively, 0.10mL, 0.50mL, 1.00mL, 2.00mL, the selenium standard solution of 5.00mL, last dilute with water, mix, obtained working curve solution,
4th step, drawing curve
Set the instrumentation and testing parameter of atomic fluorescence spectrometer, the fluorescence intensity of six parts of working curve solution obtained in the 3rd step is measured respectively by atomic fluorescence spectrometer, the fluorescence intensity that a working curve solution wherein adding 0.00mL selenium standard solution records is counted " zero intensity ", the fluorescence intensity recorded using other five parts of working curve solution deducts fluorescence intensity level after " zero intensity " respectively as ordinate, using the concentration of selenium standard solution as horizontal ordinate, draw out working curve;
5th step, the Se content in working sample solution
Using sodium borohydride solution as reductive agent, using argon gas as carrier gas with shielding gas, using the extraordinary hollow cathode lamp of selenium as excitation source, measure the fluorescence intensity I of the sample solution that second step obtains by atomic fluorescence spectrometer
1, and then measure the fluorescence intensity I of sample blank solution obtained in second step
2; Then the working curve drawn by the 4th step checks in I
1and I
2the concentration ρ of selenium corresponding respectively
1and ρ
2;
6th step, calculates
Se content in sample is with the mass fraction w of selenium
serepresent, and according to following formulae discovery:
Wherein V is the volume of second step sample solution, and m is the quality of sample.
Feature of the present invention is also,
The quality of sample described in the first step is got according to following rule: when the mass fraction of Selenium In Some Selenium-rich Biological Samples is between 0.0001% ~ 0.0010%, and taking sample quality is 0.50g; When the mass fraction of Selenium In Some Selenium-rich Biological Samples is between 0.0010% ~ 0.0050%, taking sample quality is 0.10g; 0.0001g is accurate to when taking.
The capacity of two beakers described in second step is 150mL, and the volume of hydrochloric acid solution A is 15mL, and concentration is 11.65 ~ 12.40mol/L; The volume of salpeter solution is 5mL, and concentration is 14.32 ~ 15.32mol/L; The volume of citric acid solution is 5mL, and concentration is 800g/L; The volume of urea liquid is 5mL, and concentration is 7mol/L, and the volume of hydrochloric acid solution B is 10mL, and concentration is 11.65 ~ 12.40mol/L, and the temperature of heating beaker is 150 DEG C ~ 180 DEG C, and the capacity of two volumetric flasks is 100mL.
In 3rd step, the capacity of six beakers is 150mL, and the volume of hydrochloric acid solution C is 15mL, and concentration is 11.65 ~ 12.40mol/L; The volume of salpeter solution is 5mL, and concentration is 14.32 ~ 15.32mol/L; The volume of citric acid solution is 5mL, and concentration is 800g/L; The volume of urea liquid is 5mL, and concentration is 7mol/L, and the volume of hydrochloric acid solution D is 10mL, and concentration is 11.65 ~ 12.40mol/L, and the temperature of heating beaker is 150 DEG C ~ 180 DEG C, and the capacity of six volumetric flasks is 100mL.
In selenium standard solution in 3rd step, every 1mL solution contains 1 μ g selenium.
The instrumentation and testing parameter of the 4th step Atom fluorescence spectrophotometer is specially: hollow cathode lamp negative high voltage: 350V; Lamp current: 100mA; Atomizer height: 8mm; Carrier gas flux: 400mL/min; Shield gas flow amount: 800mL/min; Reading duration: 10s; Metering system: calibration curve method; Time delay: 2.5s; Reading mode: integrating peak areas; Multiplicity: 2 times.
In 5th step, the concentration of sodium borohydride solution is 20g/L.
The invention has the beneficial effects as follows: the method for Se content in mensuration molybdenum of the present invention and molybdenum product, easy and simple to handle, efficiency is high, highly sensitive, detect and be limited to 0.13ng/mL, the recovery is 90.23% ~ 105.1%, and the measurement range of Se content is 0.0001% ~ 0.0050%.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The method of Se content in mensuration molybdenum of the present invention and molybdenum product, the Se content in the molybdenum of Accurate Measurement two kinds of specifications or molybdenum product: one is through Preliminary Determination, the molybdenum of Se content between 0.0001% ~ 0.0010% and molybdenum product; Another kind is through Preliminary Determination, the molybdenum of Se content between 0.0010% ~ 0.0050% and molybdenum product.
Embodiment 1
In mensuration molybdenum of the present invention and molybdenum product, the method for Se content, comprises the steps:
The first step, sampling
Get molybdenum bar to be determined, through Preliminary Determination, in this molybdenum bar, the mass fraction of selenium is between 0.0001% ~ 0.0010%, pulverizes this molybdenum bar, then sieves with the standard screen cloth that mesh diameter is 0.75mm, obtains sample;
Second step, prepares sample solution and sample blank solution
Getting two capacity is the beaker of 150mL, the sample 0.5g that the first step is obtained is put in one of them beaker, and add water and carry out moistening to sample, then in two beakers, hydrochloric acid solution A that 15mL concentration is 12.40mol/L is added respectively and 5mL concentration is the salpeter solution of 15.32mol/L, cover surface plate, heat two beakers to 150 DEG C respectively, until sample dissolves completely, again respectively to adding citric acid solution that 5mL concentration is 800g/L in two beakers and boiling, surface plate and walls of beaker is rinsed with water after cooling, add the urea liquid that 5mL concentration is 7mol/L more respectively, then the solution in two beakers being moved into two capacity is respectively in the volumetric flask of 100mL, be 12.40mol/L hydrochloric acid solution B respectively to adding 10mL concentration in two volumetric flasks again, last dilute with water, and mix, obtained sample solution and sample blank solution respectively,
3rd step, preparation work curve solution
Get Mo substrate, and described Mo substrate is divided into six equal portions, it is in the beaker of 150mL that six parts of Mo substrate are dropped into six capacity respectively, add water moistening, adding 15mL concentration is more respectively 12.40mol/L hydrochloric acid solution C, 5mL concentration is 15.32mol/L salpeter solution, cover surface plate, heat two beakers to 150 DEG C respectively, Mo substrate is made to dissolve completely, again respectively to adding citric acid solution that 5mL concentration is 800g/L in two beakers and boiling, surface plate and walls of beaker is rinsed with water after cooling, add the urea liquid that 5mL concentration is 7mol/L more respectively, then the solution of six beakers being moved to respectively six capacity is in the volumetric flask of 100mL, adding 10mL concentration is more respectively 12.40mol/L hydrochloric acid solution D, then in six volumetric flasks, 0.00mL is added respectively, 0.10mL, 0.50mL, 1.00mL, 2.00mL, the selenium standard solution of 5.00mL, last dilute with water, mix, obtained working curve solution, in selenium standard solution, every 1mL solution contains 1 μ g selenium,
4th step, drawing curve
Set the instrumentation and testing parameter of atomic fluorescence spectrometer, hollow cathode lamp negative high voltage: 350V; Lamp current: 100mA; Atomizer height: 8mm; Carrier gas flux: 400mL/min; Shield gas flow amount: 800mL/min; Reading duration: 10s; Metering system: calibration curve method; Time delay: 2.5s; Reading mode: integrating peak areas; Multiplicity: 2 times; The fluorescence intensity of six parts of working curve solution obtained in the 3rd step is measured respectively by atomic fluorescence spectrometer, the fluorescence intensity that a working curve solution wherein adding 0.00mL selenium standard solution records is counted " zero intensity ", the fluorescence intensity recorded using other five parts of working curve solution deducts fluorescence intensity level after " zero intensity " respectively as ordinate, using the concentration of selenium standard solution as horizontal ordinate, draw out working curve;
5th step, the Se content in working sample solution
With concentration be the sodium borohydride solution of 20g/L as reductive agent, using argon gas as carrier gas with shielding gas, using the extraordinary hollow cathode lamp of selenium as excitation source, measure the fluorescence intensity I of the sample solution that second step obtains by atomic fluorescence spectrometer
1, and then measure the fluorescence intensity I of sample blank solution obtained in second step
2; Then the working curve drawn by the 4th step checks in I
1and I
2the concentration ρ of selenium corresponding respectively
1and ρ
2;
6th step, calculates
Se content in sample is with the mass fraction w of selenium
serepresent, and according to following formulae discovery:
Wherein V is the volume of second step sample solution, and m is the quality of sample.
Through calculating, in the molybdenum bar in the present embodiment, selenium content is 0.0002%.
Embodiment 2
In mensuration molybdenum of the present invention and molybdenum product, the method for Se content, comprises the steps:
The first step, sampling
Get molybdenum powder to be determined, through Preliminary Determination, in this molybdenum powder, the mass fraction of selenium is between 0.0010% ~ 0.0020%, carries out three divisions according to inquartation to this molybdenum powder, obtains sample;
Second step, prepares sample solution and sample blank solution
Getting two capacity is the beaker of 150mL, the sample 0.10g that the first step is obtained is put in one of them beaker, and add water and carry out moistening to sample, then in two beakers, hydrochloric acid solution A that 15mL concentration is 11.65mol/L is added respectively and 5mL concentration is the salpeter solution of 14.32mol/L, cover surface plate, heat two beakers to 180 DEG C respectively, until sample dissolves completely, again respectively to adding citric acid solution that 5mL concentration is 800g/L in two beakers and boiling, surface plate and walls of beaker is rinsed with water after cooling, add the urea liquid that 5mL concentration is 7mol/L more respectively, then the solution in two beakers being moved into two capacity is respectively in the volumetric flask of 100mL, be 11.65mol/L hydrochloric acid solution B respectively to adding 10mL concentration in two volumetric flasks again, last dilute with water, and mix, obtained sample solution and sample blank solution respectively,
3rd step, preparation work curve solution
Get Mo substrate, and described Mo substrate is divided into six equal portions, it is in the beaker of 150mL that six parts of Mo substrate are dropped into six capacity respectively, add water moistening, adding 15mL concentration is more respectively 11.65mol/L hydrochloric acid solution C, 5mL concentration is 14.32mol/L salpeter solution, cover surface plate, heat two beakers to 180 DEG C respectively, Mo substrate is made to dissolve completely, again respectively to adding citric acid solution that 5mL concentration is 800g/L in two beakers and boiling, surface plate and walls of beaker is rinsed with water after cooling, add the urea liquid that 5mL concentration is 7mol/L more respectively, then the solution of six beakers being moved to respectively six capacity is in the volumetric flask of 100mL, adding 10mL concentration is more respectively 11.65mol/L hydrochloric acid solution D, then in six volumetric flasks, 0.00mL is added respectively, 0.10mL, 0.50mL, 1.00mL, 2.00mL, the selenium standard solution of 5.00mL, last dilute with water, mix, obtained working curve solution, in selenium standard solution, every 1mL solution contains 1 μ g selenium,
4th step, drawing curve
Set the instrumentation and testing parameter of atomic fluorescence spectrometer, hollow cathode lamp negative high voltage: 350V; Lamp current: 100mA; Atomizer height: 8mm; Carrier gas flux: 400mL/min; Shield gas flow amount: 800mL/min; Reading duration: 10s; Metering system: calibration curve method; Time delay: 2.5s; Reading mode: integrating peak areas; Multiplicity: 2 times; The fluorescence intensity of six parts of working curve solution obtained in the 3rd step is measured respectively by atomic fluorescence spectrometer, the fluorescence intensity that a working curve solution wherein adding 0.00mL selenium standard solution records is counted " zero intensity ", the fluorescence intensity recorded using other five parts of working curve solution deducts fluorescence intensity level after " zero intensity " respectively as ordinate, using the concentration of selenium standard solution as horizontal ordinate, draw out working curve;
5th step, the Se content in working sample solution
With concentration be the sodium borohydride solution of 20g/L as reductive agent, using argon gas as carrier gas with shielding gas, using the extraordinary hollow cathode lamp of selenium as excitation source, measure the fluorescence intensity I of the sample solution that second step obtains by atomic fluorescence spectrometer
1, and then measure the fluorescence intensity I of sample blank solution obtained in second step
2; Then the working curve drawn by the 4th step checks in I
1and I
2the concentration ρ of selenium corresponding respectively
1and ρ
2;
6th step, calculates
Se content in sample is with the mass fraction w of selenium
serepresent, and according to following formulae discovery:
Wherein V is the volume of second step sample solution, and m is the quality of sample.
Through calculating, in the molybdenum powder in the present embodiment, selenium content is 0.0013%.
Embodiment 3
In mensuration molybdenum of the present invention and molybdenum product, the method for Se content, comprises the steps:
The first step, sampling
Get molybdenum powder to be determined, through Preliminary Determination, in this molybdenum powder, the mass fraction of selenium is between 0.0030% ~ 0.0050%, carries out three divisions according to inquartation to this molybdenum powder, obtains sample;
Second step, prepares sample solution and sample blank solution
Getting two capacity is the beaker of 150mL, the sample 0.10g that the first step is obtained is put in one of them beaker, , and add water and carry out moistening to sample, then in two beakers, hydrochloric acid solution A that 15mL concentration is 12mol/L is added respectively and 5mL concentration is the salpeter solution of 15mol/L, cover surface plate, heat two beakers to 170 DEG C respectively, until sample dissolves completely, again respectively to adding citric acid solution that 5mL concentration is 800g/L in two beakers and boiling, surface plate and walls of beaker is rinsed with water after cooling, add the urea liquid that 5mL concentration is 7mol/L more respectively, then the solution in two beakers being moved into two capacity is respectively in the volumetric flask of 100mL, be 12mol/L hydrochloric acid solution B respectively to adding 10mL concentration in two volumetric flasks again, last dilute with water, and mix, obtained sample solution and sample blank solution respectively,
3rd step, preparation work curve solution
Get Mo substrate, and described Mo substrate is divided into six equal portions, it is in the beaker of 150mL that six parts of Mo substrate are dropped into six capacity respectively, add water moistening, adding 15mL concentration is more respectively 12mol/L hydrochloric acid solution C, 5mL concentration is 15mol/L salpeter solution, cover surface plate, heat two beakers to 170 DEG C respectively, Mo substrate is made to dissolve completely, again respectively to adding citric acid solution that 5mL concentration is 800g/L in two beakers and boiling, surface plate and walls of beaker is rinsed with water after cooling, add the urea liquid that 5mL concentration is 7mol/L more respectively, then the solution of six beakers being moved to respectively six capacity is in the volumetric flask of 100mL, adding 10mL concentration is more respectively 12mol/L hydrochloric acid solution D, then in six volumetric flasks, 0.00mL is added respectively, 0.10mL, 0.50mL, 1.00mL, 2.00mL, the selenium standard solution of 5.00mL, last dilute with water, mix, obtained working curve solution, in selenium standard solution, every 1mL solution contains 1 μ g selenium,
4th step, drawing curve
Set the instrumentation and testing parameter of atomic fluorescence spectrometer, hollow cathode lamp negative high voltage: 350V; Lamp current: 100mA; Atomizer height: 8mm; Carrier gas flux: 400mL/min; Shield gas flow amount: 800mL/min; Reading duration: 10s; Metering system: calibration curve method; Time delay: 2.5s; Reading mode: integrating peak areas; Multiplicity: 2 times; The fluorescence intensity of six parts of working curve solution obtained in the 3rd step is measured respectively by atomic fluorescence spectrometer, the fluorescence intensity that a working curve solution wherein adding 0.00mL selenium standard solution records is counted " zero intensity ", the fluorescence intensity recorded using other five parts of working curve solution deducts fluorescence intensity level after " zero intensity " respectively as ordinate, using the concentration of selenium standard solution as horizontal ordinate, draw out working curve;
5th step, the Se content in working sample solution
With concentration be the sodium borohydride solution of 20g/L as reductive agent, using argon gas as carrier gas with shielding gas, using the extraordinary hollow cathode lamp of selenium as excitation source, measure the fluorescence intensity I of the sample solution that second step obtains by atomic fluorescence spectrometer
1, and then measure the fluorescence intensity I of sample blank solution obtained in second step
2; Then the working curve drawn by the 4th step checks in I
1and I
2the concentration ρ of selenium corresponding respectively
1and ρ
2;
6th step, calculates
Se content in sample is with the mass fraction w of selenium
serepresent, and according to following formulae discovery:
Wherein V is the volume of second step sample solution, and m is the quality of sample.
Through calculating, in the molybdenum powder in the present embodiment, selenium content is 0.0042%.
By the way, the method for Se content in mensuration molybdenum of the present invention and molybdenum product, solves the problem that Se content that existing By Hydride Generation-atomic Fluorescence Spectrometry cannot be applied to molybdenum and molybdenum product because the selenium hydride of molybdenum is difficult to be formed is measured.Assay method of the present invention, easy and simple to handle, efficiency is high, highly sensitive, detect and be limited to 0.13ng/mL, the recovery is 90.23% ~ 105.1%, and the measurement range of Se content is 0.0001% ~ 0.050%.
Claims (5)
1. measure the method for Se content in molybdenum and molybdenum product, it is characterized in that, comprise the steps:
The first step, sampling
Get molybdenum powder to be determined, carry out at least twice division according to inquartation, obtain sample; Or get molybdenum bar to be determined, first molybdenum bar is pulverized, and sieve with the standard screen cloth that mesh diameter is 0.75mm, obtain sample;
Second step, prepares sample solution and sample blank solution
Get two beakers, the sample that the first step is obtained is put in one of them beaker, and add water and carry out moistening to sample, then in two beakers, hydrochloric acid solution A and salpeter solution is added respectively, cover surface plate, heat two beakers respectively until sample dissolves completely, again respectively to adding citric acid solution in two beakers and boiling, surface plate and walls of beaker is rinsed with water after cooling, add urea liquid respectively again, then the solution in two beakers is moved in two volumetric flasks respectively, hydrochloric acid solution B is added again respectively in two volumetric flasks, last dilute with water, and mix, obtained sample solution and sample blank solution respectively,
3rd step, preparation work curve solution
Get Mo substrate, and described Mo substrate is divided into six equal portions, six parts of Mo substrate are dropped into respectively in six beakers, add water moistening, add hydrochloric acid solution C respectively again, salpeter solution, cover surface plate, heating makes Mo substrate dissolve completely, add citric acid solution respectively and boil, surface plate and walls of beaker is rinsed with water after cooling, add urea liquid respectively again, then the solution of six beakers is moved to respectively in six volumetric flasks, add hydrochloric acid solution D respectively again, then in six beakers, 0.00mL is added respectively, 0.10mL, 0.50mL, 1.00mL, 2.00mL, the selenium standard solution of 5.00mL, last dilute with water, mix, obtained working curve solution,
4th step, drawing curve
Set the instrumentation and testing parameter of atomic fluorescence spectrometer, the fluorescence intensity of six parts of working curve solution obtained in the 3rd step is measured respectively by atomic fluorescence spectrometer, the fluorescence intensity that a working curve solution wherein adding 0.00mL selenium standard solution records is counted " zero intensity ", the fluorescence intensity recorded using other five parts of working curve solution deducts fluorescence intensity level after " zero intensity " respectively as ordinate, using the concentration of selenium standard solution as horizontal ordinate, draw out working curve;
5th step, the Se content in working sample solution
Using sodium borohydride solution as reductive agent, using argon gas as carrier gas with shielding gas, using the extraordinary hollow cathode lamp of selenium as excitation source, measure the fluorescence intensity I of the sample solution that second step obtains by atomic fluorescence spectrometer
1, and then measure the fluorescence intensity I of sample blank solution obtained in second step
2; Then the working curve drawn by the 4th step checks in I
1and I
2the concentration ρ of selenium corresponding respectively
1and ρ
2;
6th step, calculates
Se content in sample is with the mass fraction w of selenium
serepresent, and according to following formulae discovery:
Wherein V is the volume of second step sample solution, and m is the quality of sample;
The capacity of two beakers described in second step is 150mL, and the volume of described hydrochloric acid solution A is 15mL, and concentration is 11.65 ~ 12.40mol/L; The volume of described salpeter solution is 5mL, and concentration is 14.32 ~ 15.32mol/L; The volume of citric acid solution is 5mL, and concentration is 800g/L; The volume of urea liquid is 5mL, and concentration is 7mol/L, and the volume of described hydrochloric acid solution B is 10mL, and concentration is 11.65 ~ 12.40mol/L, and the temperature of heating beaker is 150 DEG C ~ 180 DEG C, and the capacity of described two volumetric flasks is 100mL;
The instrumentation and testing parameter of the 4th step Atom fluorescence spectrophotometer is specially: hollow cathode lamp negative high voltage: 350V; Lamp current: 100mA; Atomizer height: 8mm; Carrier gas flux: 400mL/min; Shield gas flow amount: 800mL/min; Reading duration: 10s; Metering system: calibration curve method; Time delay: 2.5s; Reading mode: integrating peak areas; Multiplicity: 2 times.
2. the method measuring Se content in molybdenum and molybdenum product as claimed in claim 1, it is characterized in that, the quality of sample described in the first step is got according to following rule: when the mass fraction of Selenium In Some Selenium-rich Biological Samples is between 0.0001% ~ 0.0010%, and taking sample quality is 0.50g; When the mass fraction of Selenium In Some Selenium-rich Biological Samples is between 0.0010% ~ 0.0050%, taking sample quality is 0.10g; 0.0001g is accurate to when taking.
3. the method measuring Se content in molybdenum and molybdenum product as claimed in claim 1, it is characterized in that, described in the 3rd step, the capacity of six beakers is 150mL, and the volume of described hydrochloric acid solution C is 15mL, and concentration is 11.65 ~ 12.40mol/L; The volume of described salpeter solution is 5mL, and concentration is 14.32 ~ 15.32mol/L; The volume of citric acid solution is 5mL, and concentration is 800g/L; The volume of urea liquid is 5mL, and concentration is 7mol/L, and the volume of described hydrochloric acid solution D is 10mL, and concentration is 11.65 ~ 12.40mol/L, and the temperature of heating beaker is 150 DEG C ~ 180 DEG C, and the capacity of described six volumetric flasks is 100mL.
4. the method measuring Se content in molybdenum and molybdenum product as claimed in claim 1, it is characterized in that, in the selenium standard solution described in the 3rd step, every 1mL solution contains 1 μ g selenium.
5. the method measuring Se content in molybdenum and molybdenum product as claimed in claim 1, it is characterized in that, in the 5th step, the concentration of sodium borohydride solution is 20g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310619007.7A CN103645165B (en) | 2013-11-26 | 2013-11-26 | Measure the method for Se content in molybdenum and molybdenum product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310619007.7A CN103645165B (en) | 2013-11-26 | 2013-11-26 | Measure the method for Se content in molybdenum and molybdenum product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103645165A CN103645165A (en) | 2014-03-19 |
| CN103645165B true CN103645165B (en) | 2016-04-06 |
Family
ID=50250416
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310619007.7A Active CN103645165B (en) | 2013-11-26 | 2013-11-26 | Measure the method for Se content in molybdenum and molybdenum product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103645165B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107462567B (en) * | 2015-03-30 | 2019-04-09 | 国核宝钛锆业股份公司 | A method of lithium content in measurement zirconium and zircaloy |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105372231A (en) * | 2015-10-28 | 2016-03-02 | 金堆城钼业股份有限公司 | Method for measuring content of calcium and magnesium in molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product |
| CN105548150A (en) * | 2015-12-30 | 2016-05-04 | 东旭科技集团有限公司 | Method for determining zirconium content in glass |
| CN106770117A (en) * | 2016-12-28 | 2017-05-31 | 许昌学院 | A kind of assay method of Selenium in Food |
| CN107101905B (en) * | 2017-04-24 | 2020-03-24 | 阳谷祥光铜业有限公司 | Method for measuring selenium content in crude selenium |
| CN108732161A (en) * | 2018-06-04 | 2018-11-02 | 金堆城钼业股份有限公司 | A kind of method of molybdenum content in quick measurement molybdenum raw ore |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102879373A (en) * | 2012-10-12 | 2013-01-16 | 中国航空工业集团公司北京航空材料研究院 | Method for determining selenium and tellurium content of pure chromium by using atomic fluorescence spectrometry |
-
2013
- 2013-11-26 CN CN201310619007.7A patent/CN103645165B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102879373A (en) * | 2012-10-12 | 2013-01-16 | 中国航空工业集团公司北京航空材料研究院 | Method for determining selenium and tellurium content of pure chromium by using atomic fluorescence spectrometry |
Non-Patent Citations (4)
| Title |
|---|
| Redox speciation analysis of antimony in soil extracts by hydride generation atomic fluorescence spectrometry;Edwar Fuentes.etc;《Spectrochimica Acta Part B》;20030731;page 1279-1289 * |
| 微波消解-氢化物发生原子吸收光谱法测定还原染料中的硒;李艳丽等;《染料与染色》;20091231;第49-51页 * |
| 氢化物发生-原子荧光光谱法测定钼粉及钼制品中铋和碲;谢明明等;《理化检验-化学分册》;20111031;第1186-1188页 * |
| 连续流动氢化物发生-原子吸收光谱法测定镍合金中硒及碲;童开源等;《冶金分析》;19961231;第4-6页 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107462567B (en) * | 2015-03-30 | 2019-04-09 | 国核宝钛锆业股份公司 | A method of lithium content in measurement zirconium and zircaloy |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103645165A (en) | 2014-03-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103645165B (en) | Measure the method for Se content in molybdenum and molybdenum product | |
| CN103196880B (en) | Method for determining content of arsenic in iron ore by using hydride generation-atomic fluorescence spectroscopy | |
| CN102998303B (en) | Applied microwave clears up the detection method that-ICP-AES measures Niobium in Steel, tantalum content | |
| CN103604800B (en) | A kind of analytical approach measuring titanium vanadium tungsten manganese silicon in K25 refractory Cr-base alloy | |
| CN102735678A (en) | Method for determining chromium content and aluminum content in nickel-chromium-aluminum coated diatomite | |
| CN103454131B (en) | The efficient assay method of cobalt, nickel, aluminium content in a kind of natural micro alloy iron powder | |
| CN103411960B (en) | By the method for multielement content in ICP spectrophotometer height silicon low-alloy steel | |
| CN107976481B (en) | Method for detecting scandium content in traditional Chinese medicinal materials | |
| CN103293216A (en) | Method for quickly and accurately determining 4 heavy metals in cigarette smoke | |
| CN103575707B (en) | Photo-electric direct reading spectrometer is used to measure the method for nickel base superalloy composition of steel | |
| CN103543133A (en) | Method for determining content of bismuth in iron ores by hydride generation-atomic fluorescence spectrometry method | |
| CN103149183A (en) | Method for swiftly detecting Leersia hexandra middlechro (VI) ion concentration | |
| CN102879373A (en) | Method for determining selenium and tellurium content of pure chromium by using atomic fluorescence spectrometry | |
| CN102207464A (en) | Analytical method of trace elements of Ni, Cr and Cu in low and medium alloy steels | |
| CN102830111A (en) | Method for rapidly analyzing SiO2 and BN content in aluminum silicon boron nitride powder | |
| CN103698176A (en) | Determination method of total aluminum content in steel and alloy | |
| CN105445208A (en) | Determination method for trace thallium in high-salt waste water | |
| CN110308196B (en) | Method for measuring 19 elements such as germanium, boron, tin, iodine, fluorine, arsenic, strontium, barium and the like in geochemical sample | |
| CN102004098A (en) | Method for measuring trace elements in fertilizer | |
| CN103543134A (en) | Method for determining lead content in iron ore through hydride generation-atomic fluorescence spectrometry | |
| CN109470689A (en) | The measuring method of slowly available potassium and available potassium in a kind of soil | |
| CN103543141B (en) | The analytical approach of tin oxide electrode micro impurity element Fe and Cu | |
| CN106093012A (en) | The assay method of potassium oxide in a kind of compound fertilizer | |
| CN105021692A (en) | Method for simultaneously determining multiple inorganic elements in cigarette liquid of electronic cigarette | |
| CN105021591B (en) | A kind of method of silicomanganese phosphorus molybdenum copper titanium magnesium lanthanum cerium yttrium content in measurement cast iron |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |