CN102879385A - Method for measuring content of trace element calcium in pure molybdenum - Google Patents
Method for measuring content of trace element calcium in pure molybdenum Download PDFInfo
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- CN102879385A CN102879385A CN2012100961090A CN201210096109A CN102879385A CN 102879385 A CN102879385 A CN 102879385A CN 2012100961090 A CN2012100961090 A CN 2012100961090A CN 201210096109 A CN201210096109 A CN 201210096109A CN 102879385 A CN102879385 A CN 102879385A
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Abstract
The invention belongs to the technology of analytical chemistry, and relates to a method for measuring the content of trace element calcium in pure molybdenum. The method comprises the following steps of: preparing a pure molybdenum test sample solution; preparing calcium working curve standard solutions at different concentrations; drawing the working curves of the calcium working curve standard solutions; and calculating the content of the element calcium in the pure molybdenum. The invention provides the method for measuring the content of the trace element calcium in the pure molybdenum; and the requirements on accurately measuring the content of the trace element calcium in the pure molybdenum are met.
Description
Technical field
The invention belongs to technique of analytical chemistry, relate to a kind of method of measuring trace element calcium in the pure molybdenum.
Background technology
Pure molybdenum has good thermal conductivity and electric conductivity, low thermal expansivity, and excellent corrosion resistivity is widely used in Aero-Space, electricity power, the fields such as microelectronics.The content of calcium in pure molybdenum is very little, but the content of calcium constituent has important impact to the performance of pure molybdenum.Growing along with industries such as automobile, electronics, Aeronautics and Astronautics, more and more higher to the quality requirements of molybdenum powder metallurgical product, to having higher requirement of the content of calcium constituent in the molybdenum powder, need to accurately measure the content of calcium constituent in the molybdenum powder.Do not retrieve the open source literature of trace element calcium content in the pure molybdenum of domestic and international mensuration.
Summary of the invention
The objective of the invention is: provide a kind of method of measuring trace element calcium content in the pure molybdenum, in order to satisfy the demand of trace element calcium content in the pure molybdenum of Measurement accuracy.
Technical scheme of the present invention is: a kind of method of measuring trace element calcium content in the pure molybdenum, and adopt inductively coupled plasma atomic emission spectrometer to measure, it is characterized in that, the step of mensuration is as follows:
1, the pure molybdenum sample solution of preparation: accurately take by weighing the pure molybdenum sample of 0.2000g～1.0000g in beaker, dissolve pure molybdenum sample with the sour mixed liquor of 15ml～50ml hydrochloric acid and nitric acid and form pure molybdenum solution, the percent by volume that nitric acid accounts for mixed liquor is 20%～30%, surplus is hydrochloric acid, it is pure that hydrochloric acid and nitric acid are top grade, is heated to pure molybdenum sample and dissolves fully, after the cooling pure molybdenum solution is transferred in the 100mL volumetric flask, use the secondary deionized water constant volume, shake up the pure molybdenum sample solution of rear formation;
2, the calcium working curve standard solution of preparation variable concentrations: from 5 commercially available μ g/mL calcium standard solutions, accurately pipette 0.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL calcium standard solution place respectively 6 beakers, the sour mixed liquor that adds respectively hydrochloric acid and nitric acid in each beaker forms the mixed liquor of calcium standard solution, the composition of added sour mixed liquor and the sour blended liquid phase of the hydrochloric acid in quantity and the step 1.1 and nitric acid are same, be transferred to respectively in 6 100mL volumetric flasks, use the secondary deionized water constant volume, shake up the calcium working curve standard solution of rear formation variable concentrations;
3, draw the working curve of calcium working curve standard solution: line strength of measuring respectively 6 calcium working curve standard solution calcium in the volumetric flask with JY 170 ULTRACE inductively coupled plasma atomic emission spectrometers, select the 393.366nm spectral line as measuring spectral line, take the concentration of calcium constituent as horizontal ordinate, line strength is ordinate, draws out the working curve of calcium working curve standard solution;
4, calculate the content of calcium constituent in the pure molybdenum: line strength of measuring calcium in the pure molybdenum sample solution with JY 170 ULTRACE inductively coupled plasma atomic emission spectrometers, calculate the volumetric concentration c of calcium constituent in the pure molybdenum sample solution according to the working curve of calcium working curve standard solution, every milliliter of unit milligram is calculated as follows the quality percentage composition x of calcium in the pure molybdenum:
In the formula: v: the volume of pure molybdenum sample solution, unit milliliter; M: the pure molybdenum sample quality that takes by weighing when preparing pure molybdenum sample solution, unit gram.
Advantage of the present invention is: a kind of method of measuring trace element calcium content in the pure molybdenum is provided, has satisfied the demand of trace element calcium content in the pure molybdenum of Measurement accuracy.
Embodiment
The below is described in further details the present invention.A kind of method of measuring trace element calcium content in the pure molybdenum adopts inductively coupled plasma atomic emission spectrometer to measure, and it is characterized in that, the step of mensuration is as follows:
1, the pure molybdenum sample solution of preparation: accurately take by weighing the pure molybdenum sample of 0.2000g～1.0000g in beaker, dissolve pure molybdenum sample with the sour mixed liquor of 15ml～50ml hydrochloric acid and nitric acid and form pure molybdenum solution, the percent by volume that nitric acid accounts for mixed liquor is 20%～30%, surplus is hydrochloric acid, it is pure that hydrochloric acid and nitric acid are top grade, is heated to pure molybdenum sample and dissolves fully, after the cooling pure molybdenum solution is transferred in the 100mL volumetric flask, use the secondary deionized water constant volume, shake up the pure molybdenum sample solution of rear formation;
2, the calcium working curve standard solution of preparation variable concentrations: from 5 commercially available μ g/mL calcium standard solutions, accurately pipette 0.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL calcium standard solution place respectively 6 beakers, the sour mixed liquor that adds respectively hydrochloric acid and nitric acid in each beaker forms the mixed liquor of calcium standard solution, the composition of added sour mixed liquor and the sour blended liquid phase of the hydrochloric acid in quantity and the step 1.1 and nitric acid are same, be transferred to respectively in 6 100mL volumetric flasks, use the secondary deionized water constant volume, shake up the calcium working curve standard solution of rear formation variable concentrations;
3, draw the working curve of calcium working curve standard solution: line strength of measuring respectively 6 calcium working curve standard solution calcium in the volumetric flask with JY 170 ULTRACE inductively coupled plasma atomic emission spectrometers, select the 393.366nm spectral line as measuring spectral line, take the concentration of calcium constituent as horizontal ordinate, line strength is ordinate, draws out the working curve of calcium working curve standard solution;
4, calculate the content of calcium constituent in the pure molybdenum: line strength of measuring calcium in the pure molybdenum sample solution with JY 170 ULTRACE inductively coupled plasma atomic emission spectrometers, calculate the volumetric concentration c of calcium constituent in the pure molybdenum sample solution according to the working curve of calcium working curve standard solution, every milliliter of unit milligram is calculated as follows the quality percentage composition x of calcium in the pure molybdenum:
In the formula: v: the volume of pure molybdenum sample solution, unit milliliter; M: the pure molybdenum sample quality that takes by weighing when preparing pure molybdenum sample solution, unit gram.
Principle of work of the present invention is: test portion is diluted to certain volume with hydrochloric acid, nitric acid dissolve.On inductively coupled plasma atomic emission spectrometer, under selected condition, measure the content of calcium in the test solution.
Embodiment 1, measures calcium element content in certain pure molybdenum sample.The step of measuring is as follows:
1, the pure molybdenum sample solution of preparation: accurately take by weighing the pure molybdenum sample of 0.5000g in beaker, dissolve pure molybdenum sample with the sour mixed liquor of 30ml hydrochloric acid and nitric acid and form pure molybdenum solution, the percent by volume that nitric acid accounts for mixed liquor is 20%～30%, surplus is hydrochloric acid, it is pure that hydrochloric acid and nitric acid are top grade, is heated to pure molybdenum sample and dissolves fully, after the cooling pure molybdenum solution is transferred in the 100mL volumetric flask, use the secondary deionized water constant volume, shake up the pure molybdenum sample solution of rear formation;
2, the calcium working curve standard solution of preparation variable concentrations: from 5 commercially available μ g/mL calcium standard solutions, accurately pipette 0.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL calcium standard solution place respectively 6 beakers, the sour mixed liquor that adds respectively hydrochloric acid and nitric acid in each beaker forms the mixed liquor of calcium standard solution, the composition of added sour mixed liquor and the sour blended liquid phase of the hydrochloric acid in quantity and the step 1.1 and nitric acid are same, be transferred to respectively in 6 100mL volumetric flasks, use the secondary deionized water constant volume, shake up the calcium working curve standard solution of rear formation variable concentrations;
3, draw the working curve of calcium working curve standard solution: line strength of measuring respectively 6 calcium working curve standard solution calcium in the volumetric flask with JY 170 ULTRACE inductively coupled plasma atomic emission spectrometers, select the 393.366nm spectral line as measuring spectral line, take the concentration of calcium constituent as horizontal ordinate, line strength is ordinate, draws out the working curve of calcium working curve standard solution;
4, calculate the content of calcium constituent in the pure molybdenum: line strength of measuring calcium in the pure molybdenum sample solution with JY 170 ULTRACE inductively coupled plasma atomic emission spectrometers, calculate the volumetric concentration c of calcium constituent in the pure molybdenum sample solution according to the working curve of calcium working curve standard solution, every milliliter of unit milligram is calculated as follows the quality percentage composition x of calcium in the pure molybdenum:
In the formula: v: the volume of pure molybdenum sample solution, unit milliliter; M: the pure molybdenum sample quality that takes by weighing when preparing pure molybdenum sample solution, unit gram.
5, test findings: in plasma-speetrometer, measure according to the condition of work of table 1, measurement result is as follows:
Embodiment 2, measure calcium element content in certain pure molybdenum sample.The step of measuring is as follows:
1, the pure molybdenum sample solution of preparation: accurately take by weighing the pure molybdenum sample of 1.0000g in beaker, dissolve pure molybdenum sample with the sour mixed liquor of 50ml hydrochloric acid and nitric acid and form pure molybdenum solution, the percent by volume that nitric acid accounts for mixed liquor is 20%～30%, surplus is hydrochloric acid, it is pure that hydrochloric acid and nitric acid are top grade, is heated to pure molybdenum sample and dissolves fully, after the cooling pure molybdenum solution is transferred in the 100mL volumetric flask, use the secondary deionized water constant volume, shake up the pure molybdenum sample solution of rear formation;
2, the calcium working curve standard solution of preparation variable concentrations: from 5 commercially available μ g/mL calcium standard solutions, accurately pipette 0.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL calcium standard solution place respectively 6 beakers, the sour mixed liquor that adds respectively hydrochloric acid and nitric acid in each beaker forms the mixed liquor of calcium standard solution, the composition of added sour mixed liquor and the sour blended liquid phase of the hydrochloric acid in quantity and the step 1.1 and nitric acid are same, be transferred to respectively in 6 100mL volumetric flasks, use the secondary deionized water constant volume, shake up the calcium working curve standard solution of rear formation variable concentrations;
3, draw the working curve of calcium working curve standard solution: line strength of measuring respectively 6 calcium working curve standard solution calcium in the volumetric flask with JY 170 ULTRACE inductively coupled plasma atomic emission spectrometers, select the 393.366nm spectral line as measuring spectral line, take the concentration of calcium constituent as horizontal ordinate, line strength is ordinate, draws out the working curve of calcium working curve standard solution;
4, calculate the content of calcium constituent in the pure molybdenum: line strength of measuring calcium in the pure molybdenum sample solution with JY 170 ULTRACE inductively coupled plasma atomic emission spectrometers, calculate the volumetric concentration c of calcium constituent in the pure molybdenum sample solution according to the working curve of calcium working curve standard solution, every milliliter of unit milligram is calculated as follows the quality percentage composition x of calcium in the pure molybdenum:
In the formula: v: the volume of pure molybdenum sample solution, unit milliliter; M: the pure molybdenum sample quality that takes by weighing when preparing pure molybdenum sample solution, unit gram.
5, test findings: in plasma-speetrometer, measure according to the condition of work of table 1, measurement result is as follows:
Claims (1)
1. a method of measuring trace element calcium content in the pure molybdenum adopts inductively coupled plasma atomic emission spectrometer to measure, and it is characterized in that, the step of mensuration is as follows:
1.1, the preparation pure molybdenum sample solution: accurately take by weighing the pure molybdenum sample of 0.2000g～1.0000g in beaker, dissolve pure molybdenum sample with the sour mixed liquor of 15ml～50ml hydrochloric acid and nitric acid and form pure molybdenum solution, the percent by volume that nitric acid accounts for mixed liquor is 20%～30%, surplus is hydrochloric acid, it is pure that hydrochloric acid and nitric acid are top grade, is heated to pure molybdenum sample and dissolves fully, after the cooling pure molybdenum solution is transferred in the 100mL volumetric flask, use the secondary deionized water constant volume, shake up the pure molybdenum sample solution of rear formation;
1.2, the calcium working curve standard solution of preparation variable concentrations: from 5 commercially available μ g/mL calcium standard solutions, accurately pipette 0.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL calcium standard solution place respectively 6 beakers, the sour mixed liquor that adds respectively hydrochloric acid and nitric acid in each beaker forms the mixed liquor of calcium standard solution, the composition of added sour mixed liquor and the sour blended liquid phase of the hydrochloric acid in quantity and the step 1.1 and nitric acid are same, be transferred to respectively in 6 100mL volumetric flasks, use the secondary deionized water constant volume, shake up the calcium working curve standard solution of rear formation variable concentrations;
1.3, draw the working curve of calcium working curve standard solution: line strength of measuring respectively 6 calcium working curve standard solution calcium in the volumetric flask with JY 170 ULTRACE inductively coupled plasma atomic emission spectrometers, select the 393.366nm spectral line as measuring spectral line, take the concentration of calcium constituent as horizontal ordinate, line strength is ordinate, draws out the working curve of calcium working curve standard solution;
1.4, calculate the content of calcium constituent in the pure molybdenum: line strength of measuring calcium in the pure molybdenum sample solution with JY 170 ULTRACE inductively coupled plasma atomic emission spectrometers, calculate the volumetric concentration c of calcium constituent in the pure molybdenum sample solution according to the working curve of calcium working curve standard solution, every milliliter of unit milligram is calculated as follows the quality percentage composition x of calcium in the pure molybdenum:
In the formula: v: the volume of pure molybdenum sample solution, unit milliliter; M: the pure molybdenum sample quality that takes by weighing when preparing pure molybdenum sample solution, unit gram.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103267754A (en) * | 2013-05-09 | 2013-08-28 | 二重集团（德阳）重型装备股份有限公司 | Method for quantitative determination of macroelements and trace elements comprising arsenic, tin and antimony in carbon steel or low alloy steel |
| CN112362639A (en) * | 2020-11-26 | 2021-02-12 | 三门核电有限公司 | Method for measuring content of trace elements in boron matrix sample |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103267754A (en) * | 2013-05-09 | 2013-08-28 | 二重集团（德阳）重型装备股份有限公司 | Method for quantitative determination of macroelements and trace elements comprising arsenic, tin and antimony in carbon steel or low alloy steel |
| CN112362639A (en) * | 2020-11-26 | 2021-02-12 | 三门核电有限公司 | Method for measuring content of trace elements in boron matrix sample |
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