CN104062252A - Method for measuring content of phosphorus pentoxide in glass - Google Patents
Method for measuring content of phosphorus pentoxide in glass Download PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- glass
- content
- phosphorus pentoxide
- sample
- phosphorus
- 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.)
- Pending
Links
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410300519.1A CN104062252A (en) | 2014-06-27 | 2014-06-27 | Method for measuring content of phosphorus pentoxide in glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410300519.1A CN104062252A (en) | 2014-06-27 | 2014-06-27 | Method for measuring content of phosphorus pentoxide in glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104062252A true CN104062252A (en) | 2014-09-24 |
Family
ID=51550067
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410300519.1A Pending CN104062252A (en) | 2014-06-27 | 2014-06-27 | Method for measuring content of phosphorus pentoxide in glass |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104062252A (en) |
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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003194683A (en) * | 2001-12-28 | 2003-07-09 | Japan Organo Co Ltd | Preparation method of analytical sample and quantitative analysis method of element |
| CN102854164A (en) * | 2011-07-01 | 2013-01-02 | 湖南晟通科技集团有限公司 | Method for measuring content of Ca in carbon material |
| CN103439313A (en) * | 2013-08-16 | 2013-12-11 | 成都光明光电股份有限公司 | Method for testing content of compound in glass |
-
2014
- 2014-06-27 CN CN201410300519.1A patent/CN104062252A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003194683A (en) * | 2001-12-28 | 2003-07-09 | Japan Organo Co Ltd | Preparation method of analytical sample and quantitative analysis method of element |
| CN102854164A (en) * | 2011-07-01 | 2013-01-02 | 湖南晟通科技集团有限公司 | Method for measuring content of Ca in carbon material |
| CN103439313A (en) * | 2013-08-16 | 2013-12-11 | 成都光明光电股份有限公司 | Method for testing content of compound in glass |
Non-Patent Citations (5)
| Title |
|---|
| 冯晓军等: "电感耦合等离子体发射光谱法快速测定磷矿石中主次量组分", 《岩矿测试》 * |
| 张静: "ICP-AES法测定硅铁中的铝钙铬锰磷", 《分析试验室》 * |
| 朱丽琴等: "电感耦合等离子体发射光谱法测定石灰性及中性土壤中的有效磷", 《广东化工》 * |
| 王虹等: "电感耦合等离子体发射光谱法同时测定玻璃中的硫和磷", 《分析试验室》 * |
| 马生凤等: "偏硼酸锂碱熔-电感耦合等离子体发射光谱法测定硫化物矿中硅酸盐相的主成分", 《岩矿测试》 * |
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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103267754B (en) | The method of macroelement and arsenic, tin, antimony trace element in quantitative measurement carbon steel or low alloy steel | |
| CN105259159A (en) | Analysis method for measuring content of phosphorus in ferro-molybdenum | |
| CN103048309B (en) | Method for determining content of vanadium | |
| CN104020157B (en) | Method for measuring elemental niobium content of titanium-niobium alloy | |
| CN104062252A (en) | Method for measuring content of phosphorus pentoxide in glass | |
| CN103604856A (en) | Potentiometric titration method of acid mixture solution | |
| CN103954617B (en) | Method for detecting content of lithium carbonate | |
| CN102207463A (en) | Method for measuring contents of phosphorus and copper in ferrotitanium | |
| CN101988884A (en) | Method for detecting phosphorus in organic fertilizer | |
| CN106248609B (en) | A kind of method that ultraviolet specrophotometer measures hexafluorophosphoric acid lithium content in lithium-ion battery electrolytes | |
| CN104111306B (en) | A kind of method measuring Tea Polyphenols in Tea content | |
| CN103969248A (en) | Method for determining content of phosphorus/phospholipid in grease through microwave digestion | |
| CN103048402B (en) | Method for detecting content of phosphate of different type in complex sodium phosphate product | |
| CN105044275B (en) | The method of testing of alumina content in aluminium metaphosphate | |
| CN105548115B (en) | The assay method of Mercury In Soil | |
| CN109406433A (en) | Method for detecting nitric acid content in aluminum etching solution | |
| CN101140242A (en) | Application of | |
| CN105806826A (en) | Method for determining content of elements in potassium-bearing ore by ICP (Inductively Coupled Plasma) internal standard method | |
| CN102042976A (en) | Method for measuring phosphorus and potassium content in fertilizer | |
| CN111323409A (en) | Method for detecting silicon content in high-temperature alloy | |
| CN114280221B (en) | Method for detecting phosphorus content | |
| CN103808791A (en) | Method for determining iron content in silicon nitride material | |
| CN106404870A (en) | Measuring method of trivalent and tetravalent vanadium ions in vanadium battery electrolyte | |
| CN105572120A (en) | Method for detecting phosphorus content of compound fertilizer | |
| CN104880454A (en) | Method for measuring metal element content in polycarbonate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140924 |
|
| RJ01 | Rejection of invention patent application after publication |