CN106290699B - Free fluorine and the method for single fluorophosphoric acid radical content in a kind of quick measure sodium monofluorophosphate - Google Patents
Free fluorine and the method for single fluorophosphoric acid radical content in a kind of quick measure sodium monofluorophosphate Download PDFInfo
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- CN106290699B CN106290699B CN201610783729.XA CN201610783729A CN106290699B CN 106290699 B CN106290699 B CN 106290699B CN 201610783729 A CN201610783729 A CN 201610783729A CN 106290699 B CN106290699 B CN 106290699B
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- sodium monofluorophosphate
- fluorophosphoric acid
- single fluorophosphoric
- ions
- chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention belongs to chemical industry measurement analysis field, more particularly to free fluorine and the method for single fluorophosphoric acid root in a kind of quick measure sodium monofluorophosphate, leacheate using chromatography of ions is the alkalescent leacheate such as strong basicity KOH solution, Na2CO3, NaHCO3 different from the past.Sodium monofluorophosphate sample is diluted into certain multiple with pure water, solution is injected into ion chromatograph, carries out gradient elution, rapidly and accurately separates and measures free fluorine and single fluorophosphoric acid radical content.By the present invention, substitute the detection method in national standard with the chromatography of ions, the detection time of single fluorophosphoric acid root in sodium monofluorophosphate can be shorten to 20min by the 26h in national standard.
Description
Technical field
The present invention relates to chemical industry measurement analysis field, free fluorine and list in more particularly to a kind of quick measure sodium monofluorophosphate
The method of fluorophosphoric acid radical content.
Background technology
Sodium monofluorophosphate is a kind of new chemical products, national standard (the single fluorophosphoric acid of GB 24567-2009 toothpaste industries
Sodium) in the detection method that uses of free fluorine and single fluorophosphoric acid root it is extremely complex, took and be about 26h, and process is cumbersome, asks
Inscribe not easy-to-search reason.
The content of the invention
The present invention provides free fluorine and the method for single fluorophosphoric acid radical content in a kind of quick measure sodium monofluorophosphate, Ke Yizhun
Really, free fluorine and the content of single fluorophosphoric acid root in quick detection sodium monofluorophosphate.
The technical solution adopted in the present invention is：
Free fluorine and the method for single fluorophosphoric acid radical content in a kind of quick measure sodium monofluorophosphate, are comprised the steps of：
1) standard liquid of fluorine ion and single fluorophosphoric acid root is respectively configured；
2) standard liquid is implanted sequentially chromatography of ions, sample introduction, carries out gradient elution；
3) after treating standard liquid operation, sodium monofluorophosphate sample is prepared, chromatography of ions is injected, sample introduction, carries out gradient
Sample introduction is eluted, is tested.
Preferably, the concentration of fluorine ion standard liquid is that fluorinion concentration is 0.1-10ug/ml in the step 1), single fluorine
Phosphate radical normal concentration is 10-500ug/ml.
Preferably, the step 2), the leacheate of step 3) gradient elution are KOH.
Preferably, the concentration of step 2) the gradient elution liquid is 25-50-99-50mmol/L.
Preferably, step 3) the sodium monofluorophosphate sample is diluted to 100-5000 times.
Preferably, step 3) the chromatography of ions condition is as follows：
Splitter：AS11-HC, specification 4mm；
Suppressor：ASRS-II, specification 4mm；
Leacheate：KOH；
Flow velocity：1.00mL/min；
Pressure：1600-1800psi.
Beneficial effects of the present invention：
1st, the use of the leacheate of chromatography of ions is strong basicity KOH solution in the present invention, Na different from the past2CO3、
NaHCO3It is very fast using strong basicity KOH solution, appearance etc. faintly acid leacheate, and peak type is agile does not trail.
2nd, sodium monofluorophosphate sample is diluted into certain multiple with pure water, solution is injected into ion chromatograph, carries out gradient
Elution, then it can rapidly and accurately be separated in 20min and measure free fluorine and single fluorophosphoric acid radical content.Substituted with the chromatography of ions
Detection method in national standard, test can be completed in 20min, detection time is substantially reduced, improves operating efficiency.
3rd, this method is simple and easy to do, and the degree of accuracy and precision are higher.
Brief description of the drawings
Fig. 1 fluorine ions and single fluorophosphoric acid root spectrogram.
Embodiment
The present invention is further illustrated with reference to embodiment, but the scope of protection of present invention is not limited to implement
The scope of example statement.
Embodiment 1
Using INSTRUMENT MODEL：ICS-2000 ion chromatographs (Dionex companies), Millipore A10 ultra-pure water instrument；
Free fluorine and the method for single fluorophosphoric acid radical content in a kind of quick measure sodium monofluorophosphate, it comprises the following steps：
1) start shooting, using KOH leacheates, setting flow velocity is 1.00mL/min, method for building up；
2) a series of fluorine ion standard liquids, fluorinion concentration 0.1,0.5,1,5,10ug/ml are prepared；Prepare a series of
Single fluorophosphoric acid root standard liquid, single fluorophosphoric acid root concentration are 50,100,150,200,300,400,500ug/ml；
3) standard liquid is implanted sequentially in chromatography of ions, progress gradient elution, eluent concentration 25,50,99,
50mmol/L, wherein the testing time of a sample needle is 20min；
4) a certain amount of sodium monofluorophosphate sample is weighed, about 3000 times is diluted with pure water, sample introduction, is tested, its is linear
Equation, precision and test result see the table below.
The linear equation of table 1. and coefficient correlation
| Ion | The range of linearity/ppm | Linear equation | Coefficient correlation |
| F- | 0.25-10.0 | Y=0.4215x+0.9311 | 0.9999 |
| PO3F- | 1.0-100.0 | Y=0.1106x-0.1806 | 0.9991 |
The precision of the analysis result of table 2
| Project | F-Retention time | PO3F-Retention time | F-Peak area | PO3F- peak areas |
| 3.050 | 6.187 | 0.9220 | 3.5364 | |
| 3.050 | 6.187 | 0.9352 | 3.5402 | |
| 3.053 | 6.180 | 0.9265 | 3.5366 | |
| 3.050 | 6.180 | 0.9552 | 3.5402 | |
| 3.047 | 6.173 | 0.9410 | 3.5325 | |
| 3.040 | 6.18 | 0.9223 | 3.5378 | |
| 3.047 | 6.177 | 0.9154 | 3.5322 | |
| 3.050 | 6.173 | 0.9156 | 3.5439 | |
| 3.050 | 6.180 | 0.9230 | 3.5468 | |
| 3.053 | 6.173 | 0.9225 | 3.5398 | |
| Average | 3.049 | 6.179 | 0.9279 | 3.5386 |
| RSD/% | 0.12 | 0.08 | 1.34 | 0.13 |
The sample detection result of table 3
From above table, the chromatography of ions can rapidly and accurately simultaneously separation and quantitative fluorine and single fluorophosphoric acid radical content,
Its degree of accuracy determined and precision are all preferable.Using the inventive method, national standard method can be substituted.
The above embodiments are only the preferred technical solution of the present invention, and are not construed as the limitation for the present invention, this Shen
Please in embodiment and embodiment in feature in the case where not conflicting, can mutually be combined.The protection model of the present invention
Enclose the equivalent substitution side of technical characteristic in the technical scheme that should be recorded with claim, including the technical scheme of claim record
Case is protection domain.Equivalent substitution i.e. within this range is improved, also within protection scope of the present invention.
Claims (3)
1. free fluorine and the method for single fluorophosphoric acid root in a kind of quick measure sodium monofluorophosphate, it is characterised in that include following step
Suddenly：
1）The standard liquid of fluorine ion and single fluorophosphoric acid root is respectively configured；
2）Standard liquid is implanted sequentially chromatography of ions, sample introduction, carries out gradient elution；
3）After treating standard liquid operation, sodium monofluorophosphate sample is prepared, chromatography of ions is injected, sample introduction, carries out gradient elution,
Tested
The step 2）, step 3）The leacheate of gradient elution is KOH；
The step 2）The concentration of gradient elution liquid is 25-50-99-50 mmol/L；
The step 3）Chromatography of ions condition is as follows：
Splitter：AS11-HC, specification 4mm；
Suppressor：ASRS-II, specification 4mm；
Leacheate：KOH；
Flow velocity：1.00mL/min；
Pressure：1600-1800psi.
2. according to the method for claim 1, it is characterised in that：The step 1）The concentration of middle fluorine ion standard liquid is
0.1-10 μ g/ml, single fluorophosphoric acid root concentration of standard solution are 10-500 μ g/ml.
3. according to the method for claim 1, it is characterised in that：The step 3）Sodium monofluorophosphate sample is diluted to 100-
5000 times.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101327923A (en) * | 2007-06-19 | 2008-12-24 | 云南江磷集团股份有限公司 | Preparation of sodium monofluorophosphate |
| CN103454351A (en) * | 2013-03-02 | 2013-12-18 | 安徽皖仪科技股份有限公司 | Ion chromatographic method for simultaneously measuring trace amount of anions in high-purity phosphoric acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6582682B2 (en) * | 2000-10-30 | 2003-06-24 | Noville, Inc. | Oral care compositions comprising stabilized chlorine dioxide |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101327923A (en) * | 2007-06-19 | 2008-12-24 | 云南江磷集团股份有限公司 | Preparation of sodium monofluorophosphate |
| CN103454351A (en) * | 2013-03-02 | 2013-12-18 | 安徽皖仪科技股份有限公司 | Ion chromatographic method for simultaneously measuring trace amount of anions in high-purity phosphoric acid |
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| 单氟磷酸钠产品主要指标的测定;只秉文 等;《食品研究与开发》;19981231;第20卷;57-58页 * |
| 离子色谱法测定单氟磷酸钠;只秉文 等;《现代仪器》;20031231(第3期);第14页"摘要"，第3段，第1节，第14-16页2-3节 * |
| 离子色谱法测定牙膏中可溶性氟含量;陈锦玲 等;《化学分析计量》;20141231;第23卷(第Z1期);第60页"摘要"，第二段，第60-62页1-2节 * |
| 离子色谱测定口腔含漱剂中的多种成分;章燕珍 等;《分析化学》;20070731;第35卷;1032-1034页 * |
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