CN105372231A - Method for measuring content of calcium and magnesium in molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product - Google Patents

Method for measuring content of calcium and magnesium in molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product Download PDF

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CN105372231A
CN105372231A CN201510710905.2A CN201510710905A CN105372231A CN 105372231 A CN105372231 A CN 105372231A CN 201510710905 A CN201510710905 A CN 201510710905A CN 105372231 A CN105372231 A CN 105372231A
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calcium
magnesium
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molybdenum
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谢明明
杨红忠
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Jinduicheng Molybdenum Co Ltd
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Jinduicheng Molybdenum Co Ltd
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38—Diluting, dispersing or mixing samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44—Sample treatment involving radiation, e.g. heat

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Abstract

The invention discloses a method for measuring the content of calcium and magnesium in molybdenum trioxide, ammonium molybdate, molybdenum powder and a molybdenum product. The method comprises the steps of weighing out a sample, preparing a sample solution and a sample blank solution, preparing a working curve solution, drawing a working curve, measuring the content of calcium and magnesium in the sample solution and carrying out calculation. The method for measuring the content of calcium and magnesium in molybdenum trioxide, ammonium molybdate, molybdenum powder and the molybdenum product is easy and convenient to operate, high in efficiency and high in flexibility, the detecting limit of calcium is 0.65 mg/L, the detecting limit of magnesium is 0.43 mg/L, the recovery rate of calcium ranges from 91.25% to 101.2%, the recovery rate of magnesium ranges from 95.5% to 100.6%, the measuring range of calcium is 0.0001% to 0.0100%, and the measuring range of magnesium is 0.0001% to 0.0100%. The method is suitable for scientific research and industrial production, and is especially more suitable for industrial production requiring the fast sample measuring result.

Description

Content of calcium and magnesium assay method in molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product
Technical field
The invention belongs to trace impurity analysis technical field, be specifically related to content of calcium and magnesium assay method in a kind of molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product.
Background technology
Molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product are as the high purity product of molybdenum industry, more and more higher to the analysis testing requirement of the impurity content in these products.But in existing molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product, the analytical approach of content of calcium and magnesium is mostly more numerous and diverse, and analysis precision is lower, and the time is longer.
At present, molybdenum trioxide, ammonium molybdate, calcium in molybdenum powder and molybdenum product, the national standard analytical approach of content of magnesium is flame atomic absorption spectrometry (calcium: GB/T4325.13-2013, magnesium: GB/T4325.14-2013), the method uses peroxide decomposition sample, also need to add citric acid, in hydrochloric acid medium, adopt complexity and not easy-operating standard addition method, employ more reagent, sample processing steps is many, the Mo substrate coupling needing purity very high, lower limit for height (the calcium: 5mg/L measured, magnesium: 2mg/L), the precision of measurement result is lower, the requirement of Fast Measurement in suitability for industrialized production can not be met.
In sample pre-treatments, being alkali fusion or needing to add hydrofluorite of most employing, these methods operationally more complicated, mensuration process is difficult to control, and employs a large amount of chemicals reagent, need Mo substrate to mate in sample pretreating, the time of working sample is longer, Determination Limit is higher, and pollution is large and cost is high, can not meet the demand of suitability for industrialized production.
Summary of the invention
The object of this invention is to provide content of calcium and magnesium assay method in a kind of molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product, solve that the Determination Limit that existing assay method exists is high, measurement result precision is low, can not the problem of Fast Measurement.
The technical solution adopted in the present invention is, in molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product, content of calcium and magnesium assay method, comprises the steps:
The first step, sample takes
0.1000 ~ 1.000g sample is taken according to the massfraction of content of calcium and magnesium;
Second step, prepares sample solution and sample blank solution
Get two beakers, the sample that the first step takes is put in one of them beaker, then in two beakers, superoxol is added respectively, heat two beakers until sample dissolves completely, again respectively to adding salpeter solution A in two beakers and boiling, then two beaker coolings are taken off, after the solution in two beakers is cooled to room temperature, walls of beaker is rinsed with water, then the solution in two beakers is moved in two volumetric flasks respectively, finally be diluted with water to groove, and mix, respectively obtained sample solution and sample blank solution;
3rd step, preparation work curve solution
Get three volumetric flasks, add 0mL, 2.00mL, 4.00mL calcium, magnesium typical shelf solution respectively, then add salpeter solution B respectively, be diluted with water to scale, mix, obtained working curve solution;
4th step, drawing curve
The measurement parameter of inductive coupling plasma emission spectrograph is set, the intensity of three parts of working curve solution obtained in the 3rd step is measured respectively as ordinate with inductive coupling plasma emission spectrograph, using the concentration of calcium, magnesium standard solution as horizontal ordinate, draw out working curve;
5th step, the content of calcium and magnesium in working sample solution
Carrier gas is done, the intensity I of the sample solution obtained with inductance coupled plasma optical emission spectrophotometer second step with argon gas 1, and then measure the intensity I of sample blank solution obtained in second step 2; Then the working curve by drawing from the 4th step checks in I 1and I 2the concentration ρ of corresponding calcium, magnesium respectively 1and ρ 2;
6th step, calculates
Content of calcium and magnesium in sample is with the massfraction w of calcium, magnesium ca, w mgrepresent, numerical value represents with %, and according to following formulae discovery:
w C a , M g = ( ρ 1 - ρ 2 ) · V × 10 - 6 m × 100
Wherein V is the volume of sample solution, and m is the quality that the first step takes sample.
Feature of the present invention is also,
Carry out taking sample according to the massfraction of content of calcium and magnesium in the first step: when the mass fraction of calcium in sample, magnesium is 0.0001% ~ 0.005%, taking sample quality is 1g, is accurate to 0.0001g when taking; When the mass fraction of calcium in sample, magnesium is 0.0005% ~ 0.0050%, taking sample quality is 0.5g, is accurate to 0.0001g when taking; When the mass fraction of calcium in sample, magnesium is 0.0050% ~ 0.0100%, taking sample quality is 0.1g, is accurate to 0.0001g when taking.
In second step, the volume of two beakers is 100mL ~ 200mL, and the concentration of superoxol is 30%, and adding volume is 2mL ~ 20mL; The volume of salpeter solution A is 1mL ~ 5mL, and concentration is 15.32mol/L; The temperature of heating for dissolving is 150 DEG C ~ 500 DEG C; Two volumetric flask volumes are 50mL ~ 200mL.
Described in 3rd step preparation work curve solution, calcium, magnesium typical shelf solution are mixed standard solution, and concentration is that 1mL contains 10 μ g calcium, magnesium; The volume of salpeter solution B is 2mL ~ 3mL, and concentration is 15.32mol/L, and volumetric flask volume is 100mL.
The measurement parameter arranging inductive coupling plasma emission spectrograph in 4th step is specially: radio-frequency power 0.8kW ~ 1.5kW; Entrance slit 20 μm; Exit slit 15 μm; Cooling gas flow 12L/min ~ 15L/min; Sheath airshed 0.2L/min ~ 0.3L/min; Integral time 3s ~ 10s; Wavelength: calcium 393.366nm, magnesium 279.553nm.
5th step argon gas volume fraction is not less than 99.99%.
The invention has the beneficial effects as follows, content of calcium and magnesium assay method in molybdenum trioxide of the present invention, ammonium molybdate, molybdenum powder and molybdenum product, easy and simple to handle, efficiency is high, highly sensitive, detect and be limited to calcium 0.65mg/L, magnesium 0.43mg/L, the recovery is calcium 91.25% ~ 101.2%, magnesium 95.5% ~ 100.6%, and measurement range is calcium 0.0001% ~ 0.0100%, magnesium 0.0001% ~ 0.0100%; The present invention is applicable to scientific research and commercial production, especially more applicable to the suitability for industrialized production of Fast Measurement sample result.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
In molybdenum trioxide of the present invention, ammonium molybdate, molybdenum powder and molybdenum product, content of calcium and magnesium assay method, comprises the steps:
The first step, sample takes
0.1000 ~ 1.000g sample is taken according to the massfraction of content of calcium and magnesium;
Carry out taking sample according to the massfraction of content of calcium and magnesium, be accurate to 0.0001g when taking: when the mass fraction of calcium in sample, magnesium is 0.0001% ~ 0.005%, taking sample quality is 1g; When the mass fraction of calcium in sample, magnesium is 0.0005% ~ 0.0050%, taking sample quality is 0.5g; When the mass fraction of calcium in sample, magnesium is 0.0050% ~ 0.0100%, taking sample quality is 0.1g;
Second step, prepares sample solution and sample blank solution
Get two 100mL ~ 200mL beakers, the sample that the first step takes is put in one of them beaker, then in two beakers, 2mL ~ 20mL is added respectively, concentration is the superoxol of 30%, two beakers are heated until sample dissolves completely at 150 DEG C ~ 500 DEG C, 1mL ~ 5mL is added again respectively in two beakers, concentration is the salpeter solution A of 15.32mol/L and boils, then two beaker coolings are taken off, after the solution in two beakers is cooled to room temperature, walls of beaker is rinsed with water, then the solution in two beakers is moved in two 50mL ~ 200mL volumetric flasks respectively, finally be diluted with water to groove, and mix, obtained sample solution and sample blank solution respectively,
3rd step, preparation work curve solution
Get three 100mL volumetric flasks, add 0mL, 2.00mL, 4.00mL calcium, magnesium typical shelf solution respectively, then add 2mL ~ 3mL respectively, salpeter solution B that concentration is 15.32mol/L, be diluted with water to scale, mix, obtained working curve solution;
Calcium, magnesium typical shelf solution are mixed standard solution, and concentration is that 1mL contains 10 μ g calcium, magnesium;
4th step, drawing curve
The measurement parameter of inductive coupling plasma emission spectrograph is set: radio-frequency power 0.8kW ~ 1.5kW; Entrance slit 20 μm; Exit slit 15 μm; Cooling gas flow 12L/min ~ 15L/min; Sheath airshed 0.2L/min ~ 0.3L/min; Integral time 3s ~ 10s; Wavelength: calcium 393.366nm, magnesium 279.553nm;
Measure the intensity of three parts of working curve solution obtained in the 3rd step respectively as ordinate with inductive coupling plasma emission spectrograph, using the concentration of calcium, magnesium standard solution as horizontal ordinate, draw out working curve;
5th step, the content of calcium and magnesium in working sample solution
The argon gas being not less than 99.99% with volume fraction does carrier gas, the intensity I of the sample solution obtained with inductance coupled plasma optical emission spectrophotometer second step 1, and then measure the intensity I of sample blank solution obtained in second step 2; Then the working curve by drawing from the 4th step checks in I 1and I 2the concentration ρ of corresponding calcium, magnesium respectively 1and ρ 2;
6th step, calculates
Content of calcium and magnesium in sample is with the massfraction w of calcium, magnesium ca, w mgrepresent, numerical value represents with %, and according to following formulae discovery:
w C a , M g = ( ρ 1 - ρ 2 ) · V × 10 - 6 m × 100
Wherein V is the volume of sample solution, and m is the quality that the first step takes sample.
Embodiment 1
Measure the method for molybdenum trioxide calcium in sample, content of magnesium, concrete implementation step is:
The first step, sample takes
Take 0.75g molybdenum trioxide sample (being accurate to 0.0001g);
Second step, prepares sample solution and sample blank solution
Get two beakers, the molybdenum trioxide sample that the first step takes is put in one of them beaker, another beaker not setting-out product, then in two beakers, add concentration is 30% superoxol 20mL, in 500 DEG C of heating, two beakers until sample dissolves completely, again respectively to adding salpeter solution A5mL in two beakers and boiling, then two beaker coolings are taken off, after the solution in two beakers is cooled to room temperature, walls of beaker is rinsed with water, then the solution in two beakers is moved in two 100mL volumetric flasks respectively, finally be diluted with water to groove, and mix, obtained sample solution and sample blank solution respectively,
3rd step, preparation work curve solution
Get three 100mL volumetric flasks, add 0mL, 2.00mL, 4.00mL calcium, magnesium typical shelf solution respectively, then add 3mL salpeter solution B respectively, be diluted with water to scale, mix, obtained working curve solution;
4th step, setting apparatus measures condition of work
The measurement parameter arranging inductive coupling plasma emission spectrograph is; Radio-frequency power 0.8kW; Entrance slit 20 μm; Exit slit 15 μm; Cooling gas flow 15L/min; Sheath airshed 0.02L/min; Integral time 10s; Wavelength: calcium 393.366nm, magnesium 279.553nm;
5th step, drawing curve
Measure the intensity of three parts of working curve solution obtained in the 3rd step respectively as ordinate with inductive coupling plasma emission spectrograph, using the concentration of calcium, magnesium standard solution as horizontal ordinate, draw out working curve;
6th step, the content of calcium and magnesium in working sample solution
Carrier gas is done, the intensity I of the sample solution obtained with inductance coupled plasma optical emission spectrophotometer second step with argon gas 1, and then measure the intensity I of sample blank solution obtained in second step 2; Then the working curve by drawing from the 5th step checks in I 1and I 2the concentration ρ of corresponding calcium, magnesium respectively 1and ρ 2;
7th step, calculates
Content of calcium and magnesium in molybdenum trioxide sample is with the massfraction w of calcium, magnesium ca, w mgrepresent, numerical value represents with %, and according to following formulae discovery:
w C a , M g = ( ρ 1 - ρ 2 ) · V × 10 - 6 m × 100
Wherein V is the volume of sample solution, and m is the quality that the first step takes sample.
The content of calcium and magnesium that embodiment 1 records in molybdenum trioxide sample is: calcium 0.0002%, magnesium 0.0001%.
Embodiment 1 records content of calcium and magnesium in molybdenum trioxide sample and existing national standards GB/T4325.13-2013, GB/T4325.14-2013 method, and to record results contrast as shown in table 1.
The comparison of table 1 molybdenum trioxide sample determination result
Element The inventive method records result Existing national standards records result
Ca 0.0002％ 0.0003％
Mg 0.0001％ 0.0001％
Embodiment 2
Measure the method for ammonium molybdate calcium in sample, content of magnesium, concrete implementation step is:
The first step, sample takes
Take 1g ammonium molybdate sample (being accurate to 0.0001g);
Second step, prepares sample solution and sample blank solution
Get two beakers, the molybdenum trioxide sample that the first step takes is put in one of them beaker, another beaker not setting-out product, then in two beakers, add concentration is 30% superoxol 2mL, in 400 DEG C of heating, two beakers until sample dissolves completely, again respectively to adding salpeter solution A1mL in two beakers and boiling, then two beaker coolings are taken off, after the solution in two beakers is cooled to room temperature, walls of beaker is rinsed with water, then the solution in two beakers is moved in two 50mL volumetric flasks respectively, finally be diluted with water to groove, and mix, obtained sample solution and sample blank solution respectively,
3rd step, preparation work curve solution
Get three 100mL volumetric flasks, add 0mL, 2.00mL, 4.00mL calcium, magnesium typical shelf solution respectively, then add 2mL salpeter solution B respectively, be diluted with water to scale, mix, obtained working curve solution;
4th step, setting apparatus measures condition of work
The measurement parameter arranging inductive coupling plasma emission spectrograph is; Radio-frequency power 1kW; Entrance slit 20 μm; Exit slit 15 μm; Cooling gas flow 13L/min; Sheath airshed 0.25L/min; Integral time 8s; Wavelength: calcium 393.366nm, magnesium 279.553nm;
5th step, drawing curve
Measure the intensity of three parts of working curve solution obtained in the 3rd step respectively as ordinate with inductive coupling plasma emission spectrograph, using the concentration of calcium, magnesium standard solution as horizontal ordinate, draw out working curve;
6th step, the content of calcium and magnesium in working sample solution
Carrier gas is done, the intensity I of the sample solution obtained with inductance coupled plasma optical emission spectrophotometer second step with argon gas 1, and then measure the intensity I of sample blank solution obtained in second step 2; Then the working curve by drawing from the 5th step checks in I 1and I 2the concentration ρ of corresponding calcium, magnesium respectively 1and ρ 2;
7th step, calculates
Content of calcium and magnesium in ammonium molybdate sample is with the massfraction w of calcium, magnesium ca, w mgrepresent, numerical value represents with %, and according to following formulae discovery:
w C a , M g = ( ρ 1 - ρ 2 ) · V × 10 - 6 m × 100
Wherein V is the volume of sample solution, and m is the quality that the first step takes sample.
The content of calcium and magnesium recorded in ammonium molybdate sample is: calcium 0.0003%, magnesium 0.0002%.
Embodiment 2 records content of calcium and magnesium in ammonium molybdate sample and existing national standards GB/T4325.13-2013, GB/T4325.14-2013 method, and to record results contrast as shown in table 2.
The comparison of table 2 ammonium molybdate sample determination result
Element The inventive method records result Existing national standards records result
Ca 0.0003％ 0.0003％
Mg 0.0002％ 0.0002％
Embodiment 3
Measure the method for molybdenum powder calcium in sample, content of magnesium, concrete implementation step is:
The first step, sample takes
Take 0.5g molybdenum powder sample (being accurate to 0.0001g);
Second step, prepares sample solution and sample blank solution
Get two beakers, the molybdenum trioxide sample that the first step takes is put in one of them beaker, another beaker not setting-out product, then in two beakers, add concentration is 30% superoxol 5mL, in 300 DEG C of heating, two beakers until sample dissolves completely, again respectively to adding salpeter solution A2.5mL in two beakers and boiling, then two beaker coolings are taken off, after the solution in two beakers is cooled to room temperature, walls of beaker is rinsed with water, then the solution in two beakers is moved in two 100mL volumetric flasks respectively, finally be diluted with water to groove, and mix, obtained sample solution and sample blank solution respectively,
3rd step, preparation work curve solution
Get three 100mL volumetric flasks, add 0mL, 2.00mL, 4.00mL calcium, magnesium typical shelf solution respectively, then add 2.5mL salpeter solution B respectively, be diluted with water to scale, mix, obtained working curve solution;
4th step, setting apparatus measures condition of work
The measurement parameter arranging inductive coupling plasma emission spectrograph is; Radio-frequency power 1kW; Entrance slit 20 μm; Exit slit 15 μm; Cooling gas flow 12L/min; Sheath airshed 0.2L/min; Integral time 5s; Wavelength: calcium 393.366nm, magnesium 279.553nm;
5th step, drawing curve
Measure the intensity of three parts of working curve solution obtained in the 3rd step respectively as ordinate with inductive coupling plasma emission spectrograph, using the concentration of calcium, magnesium standard solution as horizontal ordinate, draw out working curve;
6th step, the content of calcium and magnesium in working sample solution
Carrier gas is done, the intensity I of the sample solution obtained with inductance coupled plasma optical emission spectrophotometer second step with argon gas 1, and then measure the intensity I of sample blank solution obtained in second step 2; Then the working curve by drawing from the 5th step checks in I 1and I 2the concentration ρ of corresponding calcium, magnesium respectively 1and ρ 2;
7th step, calculates
Content of calcium and magnesium in molybdenum powder sample is with the massfraction w of calcium, magnesium ca, w mgrepresent, numerical value represents with %, and according to following formulae discovery:
w C a , M g = ( ρ 1 - ρ 2 ) · V × 10 - 6 m × 100
Wherein V is the volume of sample solution, and m is the quality that the first step takes sample.
The content of calcium and magnesium recorded in molybdenum powder sample is: calcium 0.0012%, magnesium 0.0005%.
Embodiment 3 records content of calcium and magnesium in molybdenum powder sample and existing national standards GB/T4325.13-2013, GB/T4325.14-2013 method, and to record results contrast as shown in table 3.
The comparison of table 3 molybdenum powder sample determination result
Element The inventive method records result Existing national standards records result
Ca 0.0012％ 0.0012％
Mg 0.0005％ 0.0006％
Embodiment 4
Measure the method for molybdenum product calcium in sample, content of magnesium, concrete implementation step is:
The first step, sample takes
Take 0.1g molybdenum product sample (being accurate to 0.0001g);
Second step, prepares sample solution and sample blank solution
Get two beakers, the molybdenum trioxide sample that the first step takes is put in one of them beaker, another beaker not setting-out product, then in two beakers, add concentration is 30% superoxol 10mL, in 150 DEG C of heating, two beakers until sample dissolves completely, again respectively to adding salpeter solution A2.5mL in two beakers and boiling, then two beaker coolings are taken off, after the solution in two beakers is cooled to room temperature, walls of beaker is rinsed with water, then the solution in two beakers is moved in two 200mL volumetric flasks respectively, finally be diluted with water to groove, and mix, obtained sample solution and sample blank solution respectively,
3rd step, preparation work curve solution
Get three 100mL volumetric flasks, add 0mL, 2.00mL, 4.00mL calcium, magnesium typical shelf solution respectively, then add 2mL salpeter solution B respectively, be diluted with water to scale, mix, obtained working curve solution;
4th step, setting apparatus measures condition of work
The measurement parameter arranging inductive coupling plasma emission spectrograph is; Radio-frequency power 1.5kW; Entrance slit 20 μm; Exit slit 15 μm; Cooling gas flow 12L/min; Sheath airshed 0.3L/min; Integral time 3s; Wavelength: calcium 393.366nm, magnesium 279.553nm;
5th step, drawing curve
Measure the intensity of three parts of working curve solution obtained in the 3rd step respectively as ordinate with inductive coupling plasma emission spectrograph, using the concentration of calcium, magnesium standard solution as horizontal ordinate, draw out working curve;
6th step, the content of calcium and magnesium in working sample solution
Carrier gas is done, the intensity I of the sample solution obtained with inductance coupled plasma optical emission spectrophotometer second step with argon gas 1, and then measure the intensity I of sample blank solution obtained in second step 2; Then the working curve by drawing from the 5th step checks in I 1and I 2the concentration ρ of corresponding calcium, magnesium respectively 1and ρ 2;
7th step, calculates
Content of calcium and magnesium in molybdenum product sample is with the massfraction w of calcium, magnesium ca, w mgrepresent, numerical value represents with %, and according to following formulae discovery:
w C a , M g = ( ρ 1 - ρ 2 ) · V × 10 - 6 m × 100
Wherein V is the volume of sample solution, and m is the quality that the first step takes sample.
The content of calcium and magnesium recorded in molybdenum product sample is: calcium 0.0062%, magnesium 0.0055%.
Embodiment 4 records content of calcium and magnesium in molybdenum product sample and existing national standards GB/T4325.13-2013, GB/T4325.14-2013 method, and to record results contrast as shown in table 4.
The comparison of table 4 molybdenum product sample determination result
Element The inventive method records result Existing national standards records result
Ca 0.0062％ 0.0061％
Mg 0.0055％ 0.0056％

Claims (6)

1. content of calcium and magnesium assay method in molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product, is characterized in that, comprise the steps:
The first step, sample takes
0.1000 ~ 1.000g sample is taken according to the massfraction of content of calcium and magnesium;
Second step, prepares sample solution and sample blank solution
Get two beakers, the sample that the first step takes is put in one of them beaker, then in two beakers, superoxol is added respectively, heat two beakers until sample dissolves completely, again respectively to adding salpeter solution A in two beakers and boiling, then two beaker coolings are taken off, after the solution in two beakers is cooled to room temperature, walls of beaker is rinsed with water, then the solution in two beakers is moved in two volumetric flasks respectively, finally be diluted with water to groove, and mix, respectively obtained sample solution and sample blank solution;
3rd step, preparation work curve solution
Get three volumetric flasks, add 0mL, 2.00mL, 4.00mL calcium, magnesium typical shelf solution respectively, then add salpeter solution B respectively, be diluted with water to scale, mix, obtained working curve solution;
4th step, drawing curve
The measurement parameter of inductive coupling plasma emission spectrograph is set, the intensity of three parts of working curve solution obtained in the 3rd step is measured respectively as ordinate with inductive coupling plasma emission spectrograph, using the concentration of calcium, magnesium standard solution as horizontal ordinate, draw out working curve;
5th step, the content of calcium and magnesium in working sample solution
Carrier gas is done, the intensity I of the sample solution obtained with inductance coupled plasma optical emission spectrophotometer second step with argon gas 1, and then measure the intensity I of sample blank solution obtained in second step 2; Then the working curve by drawing from the 4th step checks in I 1and I 2the concentration ρ of corresponding calcium, magnesium respectively 1and ρ 2;
6th step, calculates
Content of calcium and magnesium in sample is with the massfraction w of calcium, magnesium ca, w mgrepresent, numerical value represents with %, and according to following formulae discovery:
w C a , M g = ( ρ 1 - ρ 2 ) · V × 10 - 6 m × 100
Wherein V is the volume of sample solution, and m is the quality that the first step takes sample.
2. content of calcium and magnesium assay method in molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product as claimed in claim 1, it is characterized in that, carry out taking sample according to the massfraction of content of calcium and magnesium in the first step, be accurate to 0.0001g when taking: when the mass fraction of calcium in sample, magnesium is 0.0001% ~ 0.005%, taking sample quality is 1g; When the mass fraction of calcium in sample, magnesium is 0.0005% ~ 0.0050%, taking sample quality is 0.5g; When the mass fraction of calcium in sample, magnesium is 0.0050% ~ 0.0100%, taking sample quality is 0.1g.
3. content of calcium and magnesium assay method in molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product as claimed in claim 1, it is characterized in that, in second step, the volume of two beakers is 100mL ~ 200mL, and the concentration of described superoxol is 30%, and adding volume is 2mL ~ 20mL; The volume of described salpeter solution A is 1mL ~ 5mL, and concentration is 15.32mol/L; The temperature of described heating for dissolving is 150 DEG C ~ 500 DEG C; Described two volumetric flask volumes are 50mL ~ 200mL.
4. content of calcium and magnesium assay method in molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product as claimed in claim 1, it is characterized in that, described in 3rd step preparation work curve solution, calcium, magnesium typical shelf solution are mixed standard solution, and concentration is that 1mL contains 10 μ g calcium, magnesium; The volume of described salpeter solution B is 2mL ~ 3mL, and concentration is 15.32mol/L, and described volumetric flask volume is 100mL.
5. content of calcium and magnesium assay method in molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product as claimed in claim 1, it is characterized in that, the measurement parameter arranging inductive coupling plasma emission spectrograph in the 4th step is specially: radio-frequency power 0.8kW ~ 1.5kW; Entrance slit 20 μm; Exit slit 15 μm; Cooling gas flow 12L/min ~ 15L/min; Sheath airshed 0.2L/min ~ 0.3L/min; Integral time 3s ~ 10s; Wavelength: calcium 393.366nm, magnesium 279.553nm.
6. content of calcium and magnesium assay method in molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product as claimed in claim 1, it is characterized in that, the 5th step argon gas volume fraction is not less than 99.99%.
CN201510710905.2A 2015-10-28 2015-10-28 Method for measuring content of calcium and magnesium in molybdenum trioxide, ammonium molybdate, molybdenum powder and molybdenum product Pending CN105372231A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103645165A (en) * 2013-11-26 2014-03-19 金堆城钼业股份有限公司 Method for measuring content of selenium in molybdenum and molybdenum product

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103645165A (en) * 2013-11-26 2014-03-19 金堆城钼业股份有限公司 Method for measuring content of selenium in molybdenum and molybdenum product

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
张俊峰等: "ICP-AES法测定钼钇合金中钇的质量分数", 《宁夏工程技术》 *
郑洪涛等: "ICP-AES测定纯三氧化钼和钼酸铵中痕量元素", 《中国钼业》 *
马琪 李正明: "电感耦合等离子体发射光谱法测定钼铜合金中镍、钙、镁、铝", 《装备制造》 *

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