CN104062252A - Method for measuring content of phosphorus pentoxide in glass - Google Patents
Method for measuring content of phosphorus pentoxide in glass Download PDFInfo
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- CN104062252A CN104062252A CN201410300519.1A CN201410300519A CN104062252A CN 104062252 A CN104062252 A CN 104062252A CN 201410300519 A CN201410300519 A CN 201410300519A CN 104062252 A CN104062252 A CN 104062252A
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Abstract
The invention provides a method for easily, fast and accurately measuring the content of phosphorus pentoxide (P2O5) in glass. The method comprises the following steps: (1) adding perchloric acid and hydrofluoric acid into a glass sample, heating for dissolving, steaming to be dry nearly, cooling, adding nitric acid, heating for the dissolving, and diluting with water so as to obtain a sample solution; (2) preparing standard series of solutions of P; (3) determining the standard series of the solutions of P by using a plasma emission spectrometer, automatically establishing a calibration curve by using an instrument, then determining the sample solution, and automatically calculating the content of phosphorus in the sample solution by the instrument; and (4) calculating to obtain the content of the phosphorus pentoxide. The method provided by the invention has the advantages that as the plasma emission spectrometer is adopted to test the content of the P2O5 in the glass, the effects of being simple, fast and environmentally-friendly are achieved, the analytic procedures are omitted, the analytic efficiency is improved, the errors caused by artificial analysis are reduced, the repeatability and the accuracy of measurement can be obviously enhanced, and the interference of silicon, iron and titanium in phosphorus-vanadium-molybdenum-yellow spectrophotometry on testing is avoided.
Description
Technical field
The present invention relates to a kind of measuring method of glass content, particularly relate to the measuring method of phosphorus pentoxide content in a kind of glass.
Background technology
At present, the measuring method of the phosphorus pentoxide content in glass is mainly contained to the yellow photometry of phosphorus molybdenum acid ammonium capacity method, phosphomolybdic acid quinoline gravimetric method, phosphomolybdic acid quinoline volumetric method and phosphorus vanadium molybdenum etc.Wherein, phosphomolybdic acid quinoline gravimetric method and phosphomolybdic acid quinoline volumetric method because accuracy is high, good stability is by typing standard GB/T/T1871.1-1995.
Phosphomolybdic acid quinoline gravimetric method is in acid medium, and orthophosphoric acid root reacts with quinoline molybdenum lemon ketone precipitation agent and generates yellow phosphomolybdic acid quinoline precipitation, after filtration, washing, dry, weigh, can obtain the phosphorus pentoxide content in glass, the method is arbitration law.Phosphomolybdic acid quinoline volumetric method is in acid medium, orthophosphoric acid root reacts with quinoline molybdenum lemon ketone precipitation agent and generates yellow phosphomolybdic acid quinoline precipitation, after filtration, after washing, will be precipitated and dissolved in alkali standard solution, then use the alkali of sour standard solution overtitration, can obtain phosphorus pentoxide content.Although these two kinds of method measurement results are accurate, operation steps is more, and minute is long, obtain measurement result one time, needs 4 to 6 hours, is unfavorable for instructing producing.
The yellow photometry of phosphorus vanadium molybdenum is in acid solution, and phosphate radical and ammonium vanadate, ammonium molybdate effect generate yellow phosphovanadomolybdic acid complex compound, can be used for the colorimetric estimation of phosphorus.Acidity, temperature color speed and the color depth on phosphorus has impact, and when mensuration, reagent dosage is consistent as far as possible.When silicon, iron, Ti content are high, can cause interference, iron makes measurement result higher, should not use hydrochloric acid medium, must remove with nitric acid evaporate to dryness the yellow interference measurement of ferric trichloride in solution while having hydrochloric acid to exist.The method operation steps is more, and operating conditions harshness, and test result influence factor is many.
Summary of the invention
Technical matters to be solved by this invention be to provide a kind of can be easy, quick, the method for phosphorus pentoxide content in Measurement accuracy glass.
The technical scheme that technical solution problem of the present invention adopts is: the measuring method of phosphorus pentoxide content in glass, and the method comprises the following steps:
1) take 0.2～0.4g glass sample in beaker, add perchloric acid 5～10mL, hydrofluorite 5～10mL, heating for dissolving, steams near dry rear cooling, adds nitric acid 5～10mL heating for dissolving, and dilute with water, obtains sample solution;
2) standard solution (1000ug/mL) of getting P dilutes in right amount, the standard serial solution of preparation P;
3) wavelength of choosing P is that 213.617nm is as analytical line, with plasma emission spectrometer determination step 2) standard serial solution of P of preparation, instrument is set up calibration curve automatically, then determination step 1) sample solution that obtains, the content of P elements in the automatic calculation sample solution of instrument;
4) calculate phosphorus pentoxide content by following formula:
(P
2O
5)％＝2.2916*C*A*10
-6/m*100％
Wherein: C is the phosphorus content that plasma emission spectrometer is measured, (ug/mL)
A is the extension rate of sample
M is sample quality, g.
Further, step 1) concentration of described perchloric acid is 70～72%.
Further, step 1) concentration of described hydrofluorite is for being more than or equal to 40%.
Further, step 1) concentration of described nitric acid is 65.0～68.0%.
Further, step 1) described container employing polytetrafluoroethylene beaker or platinum crucible.
Further, step 1) described dilute with water is: is transferred in volumetric flask, is diluted with water to scale.
The invention has the beneficial effects as follows: adopt the P in plasma emission spectrometer tested glass
2o
5easy, quick, economy, environmental protection, reduce routine analyzer, improve analysis efficiency, reduce artificial analytical error, can significantly improve repeatability and the accuracy of measurement, simultaneously, adopt the inventive method and adopt the test result of phosphomolybdic acid quinoline gravimetric method consistent, having avoided silicon, iron, the interference of titanium to test in the yellow photometry of phosphorus vanadium molybdenum.
Embodiment
Measuring method of the present invention comprises the following steps:
1) take 0.2～0.4g glass sample in container, adding concentration is that 70～72% perchloric acid 5～10mL and concentration are more than or equal to hydrofluorite 5～10mL of 40%, heating for dissolving, steam near dry, cooling after, adding concentration is nitric acid 5～10mL of 65.0～68.0%, heating for dissolving, be transferred in volumetric flask, be diluted with water to scale and shake up, obtain sample solution;
2) standard solution (1000ug/mL, national standard GSB04-1741-2004 (a)) of getting P dilutes in right amount, the standard serial solution of preparation P;
3) wavelength of choosing P is that 213.617nm is as analytical line, with plasma emission spectrometer determination step 2) standard serial solution of P of preparation, instrument is set up calibration curve automatically, then determination step 1) sample solution that obtains, the content of P elements in the automatic calculation sample solution of instrument;
4) calculate phosphorus pentoxide content by following formula:
(P
2O
5)％＝2.2916*C*A*10
-6/m*100％
Wherein: C is the phosphorus content that plasma emission spectrometer is measured, (ug/mL);
A is the extension rate of sample;
M is glass sample quality, g.
Step 1 of the present invention) in container preferably adopt polytetrafluoroethylene beaker or platinum crucible.
With respect to the yellow photometry of phosphorus vanadium molybdenum, the present invention measures the content of phosphorus pentoxide in glass sample with plasma emission spectrometer, can effectively avoid silicon, iron, titanium test to disturb, reduce routine analyzer, improve analysis efficiency, reduce artificial analytical error, significantly improved repeatability and the accuracy of test; With respect to phosphomolybdic acid quinoline gravimetric method, the inventive method test is easy, quick, has reduced the process such as precipitation, suction filtration, and being dissolved sample is available instrument test.
Embodiment 1:
1) take 0.3g glass sample in polytetrafluoroethylene beaker, add perchloric acid 5mL, hydrofluorite 5mL, heating for dissolving on electric hot plate, evaporation, steams near dry, cooling after, add nitric acid 5mL, heating for dissolving, transfers in 100mL volumetric flask, is diluted with water to scale and shakes up, draw 10mL in 100mL volumetric flask, be diluted to scale mark, shake up, obtain sample solution;
2) standard solution (1000ug/mL, national standard GSB04-1741-2004 (a)) of getting P dilutes in right amount, the standard serial solution of preparation P;
3) wavelength of choosing P is that 213.617nm is as analytical line, with plasma emission spectrometer determination step 2) standard serial solution of P of preparation, instrument is set up calibration curve automatically, then determination step 1) sample solution that obtains, the content of P elements in the automatic calculation sample solution of instrument;
4) calculate phosphorus pentoxide content by following formula:
(P
2O
5)％＝2.2916*C*A*10
-6/m*100％
Wherein: C is the phosphorus content that plasma emission spectrometer is measured, (ug/mL);
A is the extension rate of sample;
M is sample quality, g.
By test result and the comparison of phosphomolybdic acid quinoline gravimetric method test result, as following table:
| The test result (%) of embodiment 1 | Phosphomolybdic acid quinoline gravimetric method test result (%) | |
| P in glass sample 2O 5Content | 48.69 | 48.64 |
Upper table data show that test result of the present invention is consistent with gravimetric method test result, and the inventive method test accurate and effective is described.
Embodiment 2:
1) take 0.2g sample in polytetrafluoroethylene beaker, add perchloric acid 8mL, hydrofluorite 10mL, heating for dissolving on electric hot plate, evaporation, steams near dry, cooling after, add nitric acid 10mL, heating for dissolving, transfers in 100mL volumetric flask, is diluted with water to scale and shakes up, draw 10mL in 100mL volumetric flask, be diluted to scale mark, shake up, obtain sample solution;
2) standard solution (1000ug/mL, national standard GSB04-1741-2004 (a)) of getting P dilutes in right amount, the standard serial solution of preparation P;
3) wavelength of choosing P is that 213.617nm is as analytical line, with plasma emission spectrometer determination step 2) standard serial solution of P of preparation, instrument is set up calibration curve automatically, then determination step 1) sample solution that obtains, the content of P elements in the automatic calculation sample solution of instrument;
4) calculate phosphorus pentoxide content by following formula:
(P
2O
5)％＝2.2916*C*A*10
-6/m*100％
Wherein: C is the phosphorus content that plasma emission spectrometer is measured, (ug/mL)
A is the extension rate of sample
M is sample quality, g.
By test result and the comparison of gravimetric method test result, as following table:
| The test result (%) of embodiment 2 | Phosphomolybdic acid quinoline gravimetric method test result (%) | |
| P in glass sample 2O 5Content | 64.07 | 64.12 |
Upper table data show that test result of the present invention is consistent with gravimetric method test result, and the inventive method test accurate and effective is described.
Embodiment 3:
1) take 0.4g glass sample in platinum crucible, add perchloric acid 5mL, hydrofluorite 10mL, heating for dissolving on electric hot plate, evaporation, steams near dry, cooling after, add nitric acid 8mL, heating for dissolving, transfers in 100mL volumetric flask, is diluted with water to scale and shakes up, draw 10mL in 100mL volumetric flask, be diluted to scale mark, shake up, obtain sample solution;
2) standard solution (1000ug/mL, national standard GSB04-1741-2004 (a)) of getting P dilutes in right amount, the standard serial solution of preparation P;
3) wavelength of choosing P is that 213.617nm is as analytical line, with plasma emission spectrometer determination step 2) standard serial solution of P of preparation, instrument is set up calibration curve automatically, then determination step 1) sample solution that obtains, the content of P elements in the automatic calculation sample solution of instrument;
4) calculate phosphorus pentoxide content by following formula:
(P
2O
5)％＝2.2916*C*A*10
-6/m*100％
Wherein: C is the phosphorus content that plasma emission spectrometer is measured, (ug/mL);
A is the extension rate of sample;
M is sample quality, g.
By test result and the comparison of gravimetric method test result, as following table:
| The test result (%) of embodiment 3 | Phosphomolybdic acid quinoline gravimetric method test result (%) | |
| P in glass sample 2O 5Content | 25.36 | 25.30 |
Upper table data show that test result of the present invention is consistent with gravimetric method test result, and the inventive method test accurate and effective is described.
The concentration of the perchloric acid that above-mentioned 3 embodiment adopt is 70～72%, and the concentration of hydrofluorite is for being more than or equal to 40%, and the concentration of nitric acid is 65.0～68.0%.
Claims (6)
1. the measuring method of phosphorus pentoxide content in glass, is characterized in that, the method comprises the following steps:
1) take 0.2～0.4g glass sample in container, add perchloric acid 5～10mL, hydrofluorite 5～10mL, heating for dissolving, steams near dry rear cooling, adds nitric acid 5～10mL heating for dissolving, and dilute with water, obtains sample solution;
2) standard solution (1000ug/mL) of getting P dilutes in right amount, the standard serial solution of preparation P;
3) wavelength of choosing P is that 213.617nm is as analytical line, with plasma emission spectrometer determination step 2) standard serial solution of P of preparation, instrument is set up calibration curve automatically, then determination step 1) sample solution that obtains, the content of P elements in the automatic calculation sample solution of instrument;
4) calculate phosphorus pentoxide content by following formula:
(P
2O
5)％＝2.2916*C*A*10
-6/m*100％
Wherein: C is the phosphorus content that plasma emission spectrometer is measured, (ug/mL)
A is the extension rate of sample
M is sample quality, g.
2. the measuring method of phosphorus pentoxide content in glass as claimed in claim 1, is characterized in that step 1) concentration of described perchloric acid is 70～72%.
3. the measuring method of phosphorus pentoxide content in glass as claimed in claim 1, is characterized in that step 1) concentration of described hydrofluorite is for being more than or equal to 40%.
4. the measuring method of phosphorus pentoxide content in glass as claimed in claim 1, is characterized in that step 1) concentration of described nitric acid is 65.0～68.0%.
5. the measuring method of phosphorus pentoxide content in glass as claimed in claim 1, is characterized in that step 1) described container employing polytetrafluoroethylene beaker or platinum crucible.
6. the measuring method of phosphorus pentoxide content in glass as claimed in claim 1, is characterized in that step 1) described dilute with water is: is transferred in volumetric flask, is diluted with water to scale.
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|---|---|---|---|
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Cited By (4)
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| CN106153819A (en) * | 2016-07-27 | 2016-11-23 | 湖北富邦科技股份有限公司 | Phosphorus pentoxide assay method in the phosphorus ore of a kind of improvement |
| CN106370510A (en) * | 2016-10-21 | 2017-02-01 | 天津大学 | Method for microwave digestion of glass body |
| CN107607522A (en) * | 2017-08-29 | 2018-01-19 | 东旭科技集团有限公司 | A kind of method of phosphorus content in measure glass |
| CN113884541A (en) * | 2021-09-30 | 2022-01-04 | 河南旭阳光电科技有限公司 | Method for measuring content of chloride ions and sulfate ions in glass and conductivity detection system |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106153819A (en) * | 2016-07-27 | 2016-11-23 | 湖北富邦科技股份有限公司 | Phosphorus pentoxide assay method in the phosphorus ore of a kind of improvement |
| CN106370510A (en) * | 2016-10-21 | 2017-02-01 | 天津大学 | Method for microwave digestion of glass body |
| CN107607522A (en) * | 2017-08-29 | 2018-01-19 | 东旭科技集团有限公司 | A kind of method of phosphorus content in measure glass |
| CN113884541A (en) * | 2021-09-30 | 2022-01-04 | 河南旭阳光电科技有限公司 | Method for measuring content of chloride ions and sulfate ions in glass and conductivity detection system |
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Application publication date: 20140924 |
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