CN102023190A - Method for detecting electronic-grade phosphoric acid trace impurity anions - Google Patents
Method for detecting electronic-grade phosphoric acid trace impurity anions Download PDFInfo
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- CN102023190A CN102023190A CN 201010501146 CN201010501146A CN102023190A CN 102023190 A CN102023190 A CN 102023190A CN 201010501146 CN201010501146 CN 201010501146 CN 201010501146 A CN201010501146 A CN 201010501146A CN 102023190 A CN102023190 A CN 102023190A
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Abstract
The invention relates to a method for detecting electronic-grade phosphoric acid trace impurity anions, in particular to an impurity anion separation method. The detection method comprises the following steps: a. a sample solution is prepared; b. the solution of standard series is prepared; c. separation is carried out; d. conversion is carried out; e. concentration is carried out; f. determination is carried out; and g. calculation is carried out. In the method for detecting electronic-grade phosphoric acid trace impurity anions in the invention, an ion exclusion column is adopted to separate trace chloride ions, nitrate ions and sulphate ions in electronic-grade phosphoric acid from concentrated phosphoric acid, thus the pre-treatment on a sample is simple, and the determination of impurity ions can not be influenced in the presence of high concentration phosphates.
Description
Technical field
The present invention relates to the anionic method of a kind of detected electrons level phosphoric acid trace impurity, the method that particularly a kind of impurity negative ion separates.
Background technology
Existing detection means mainly is a visual colorimetry, promptly by treating that the reaction of measured ion and corresponding reagent generates precipitation, carries out colorimetric with standard or than turbid, is difficult to accurately measure the content for the treatment of measured ion.
Summary of the invention
Purpose of the present invention is intended to overcome the defective of prior art, provides a kind of ion exclusion column that uses that the trace chloro ion in the electron-level phosphoric acid, nitrate ion and sulfate ion are separated from strong phosphoric acid, the method that detects with electric conductivity detector.
The anionic method of detected electrons level phosphoric acid trace impurity of the present invention, its detection step is:
A, sample solution: accurately take by weighing the electron-level phosphoric acid sample, add the deionized water dilution, mixing is mixed with 40%～60% sample solution;
The preparation of b, standard serial solution: according to the compound method of sample solution, prepare at least 4 parts of solution, in every part of solution, add and contain Cl
-, NO
3 -And SO
4 2-The negative ion mixed standard solution is mixed with and contains Cl
-, NO
3 -And SO
4 2-Standard serial solution, the concentration range of each ion is just prepared according to the content of testing sample in the standard serial solution, scope is 0.005～10 μ g/g;
C, separation: respectively sample solution and standard serial solution are entered ion exchange system, corresponding ion exchanges in the ion in the sample solution and the moving phase, and different ions is attached on the fixed charge in the stationary phase;
D, conversion: each negative ion that step c is separated converts the strong acid with high conductivity to through the rejector system, and the KOH leacheate then changes the carbonic acid of weak conductivity into, and is measured the conductivity of each anionic group by electric conductivity detector;
E, concentrated: the component of separated and collected is concentrated by the ion-exchange evaporating column;
F, mensuration: under selected chromatographic condition, adopt ion chromatograph that sample solution and standard serial solution are measured, instrument writes down the peak area value for the treatment of measured ion automatically;
G, calculating: with mixed standard solution concentration is horizontal ordinate, and peak area value is an ordinate, draws out the working curve of chlorion, nitrate ion, sulfate ion respectively, obtains anionic content to be measured in the phosphoric acid according to working curve.
The anionic method of detected electrons level phosphoric acid trace impurity of the present invention, use ion exclusion column with the trace chloro ion in the electron-level phosphoric acid, nitrate ion and sulfate ion are separated from strong phosphoric acid, component with separated and collected concentrates by the ion-exchange evaporating column again, negative ion to be measured enters ion exchange system with leacheate, through deionized water, potassium hydroxide, according to separating column each anionic different affinity is separated again, the negative ion that has separated converts the strong acid of the high conductivity of tool to through inhibition type detector system, and leacheate then changes the carbonic acid of weak conductivity into.Measure the conductivity of each anionic group by electric conductivity detector, quantitative with relative retention time and peak height or area.
Among the present invention, the chromatographic condition that is adopted is:
(1) chromatographic column
Guard column, 4 mm;
Analytical column, 4mm;
Evaporating column, 4 mm;
Catch post, 9 * 75mm;
Repel post, 9 * 250 mm.
(2) chromatographic condition
Ion exclusion: repel post, catch post
Leacheate: deionized water;
Flow velocity: 0.50 mL/min.
The condition of concentrating: evaporating column
Leacheate: potassium hydroxide (20 mM-60 mM);
Flow velocity: 1.00mL/min;
Sample size: 200 μ L;
Detecting device: inhibition type detecting device.
The anionic method of detected electrons level phosphoric acid trace impurity of the present invention, the method that is to use ion exclusion column that the trace chloro ion in the electron-level phosphoric acid, nitrate ion and sulfate ion are separated from strong phosphoric acid, this method is simple to sample pre-treatments, and the existence of high concentration phosphorus acid group does not influence the mensuration of foreign ion.
Embodiment
The present invention is described further below by embodiment, but be not limited to embodiment.
Embodiment 1
The anionic method of detected electrons level phosphoric acid trace impurity of the present invention, its detection step is:
A, sample: accurately take by weighing 5g phosphoric acid sample, add the deionized water dilution of equivalent, mixing, this solution are solution to be measured, accurately the quality of this solution of weighing;
The preparation of b, standard serial solution
Accurately take by weighing 4 parts in 5g phosphoric acid sample respectively, add the deionized water dilution of equivalent, behind the mixing, in every duplicate samples solution, add mixed standard solution respectively, be made into 1～4
#The hybrid standard working solution contains Cl respectively
-, NO
3 -And SO
4 2-Concentration be 1
#: Cl
-0.05 μ g/g, NO
3 -0.05 μ g/g, SO
4 2-0.50 μ g/g, 2
#: Cl
-0.10 μ g/g, NO
3 -0.10 μ g/g, SO
4 2-1.00 μ g/g, 3
#: Cl
-0.20 μ g/g, NO
3 -0.20 μ g/g, SO
4 2-2.00 μ g/g, 4
#: Cl
-0.40 μ g/g, NO
3 -0.40 μ g/g, SO
4 2-4.00 μ g/g;
C, separation: respectively sample solution and standard serial solution are entered ion exchange system, corresponding ion exchanges in the ion in the sample and the moving phase, and in the time of a weak point, sample ions can be attached on the fixed charge in the stationary phase.Because trace chloro ion, nitrate ion and sulfate ion in the phosphoric acid are different to stationary phase affinity, make that various ingredients is separated in the sample;
D, conversion: convert each negative ion that is separated of step c to strong acid through the rejector system with high conductivity, leacheate then changes the carbonic acid of weak conductivity into, and measure the conductivity of each anionic group by electric conductivity detector, quantitative with relative retention time and peak height or area;
E, concentrated: collect the sample that separates the 5-8min time period, the component of collection concentrates by the ion-exchange evaporating column;
F, mensuration: under selected chromatographic condition, solution to be measured and standard series are measured, instrument writes down the peak area value for the treatment of measured ion automatically, and chromatographic condition is:
(1) chromatographic column
Guard column, 4 mm;
Analytical column, 4mm;
Evaporating column, 4 mm;
Catch post, 9 * 75mm;
Repel post, 9 * 250 mm.
(2) chromatographic condition
Ion exclusion: repel post, catch post
Leacheate: deionized water;
Flow velocity: 0.50 mL/min.
The condition of concentrating: evaporating column
Leacheate: potassium hydroxide (20 mM-60 mM);
Flow velocity: 1.00mL/min;
Sample size: 200 μ L;
Detecting device: inhibition type detecting device
G, calculating: with the concentration of standard solution is horizontal ordinate, and peak area value is an ordinate, draws out the working curve of chlorion, nitrate ion, sulfate ion respectively, obtains anionic content to be measured in the phosphoric acid according to working curve.
Embodiment 2
The anionic method of detected electrons level phosphoric acid trace impurity of the present invention, its detection step is:
A, sample: accurately take by weighing 10g phosphoric acid sample, add the deionized water dilution of equivalent, mixing, this solution are solution to be measured, accurate this solution of weighing, and quality is m
1
The preparation of b, standard serial solution
Accurately take by weighing 4 parts in 10g phosphoric acid sample, add the deionized water dilution of equivalent, behind the mixing, in every duplicate samples solution, add mixed standard solution respectively, be made into 1～4
#The hybrid standard working solution contains Cl respectively
-, NO
3 -And SO
4 2-Concentration be 1
#: Cl
-0.01 μ g/g, NO
3 -0.01 μ g/g, SO
4 2-0.10 μ g/g, 2
#: Cl
-0.02 μ g/g, NO
3 -0.02 μ g/g, SO
4 2-0.20 μ g/g, 3
#: Cl
-0.04 μ g/g, NO
3 -0.04 μ g/g, SO
4 2-0.40 μ g/g, 4
#: Cl
-0.08 μ g/g, NO
3 -0.08 μ g/g, SO
4 2-0.80 μ g/g;
C, separation: respectively sample solution and standard serial solution are entered ion exchange system, corresponding ion exchanges in the ion in the sample and the moving phase, and in the time of a weak point, sample ions can be attached on the fixed charge in the stationary phase.Because trace chloro ion, nitrate ion and sulfate ion in the phosphoric acid are different to stationary phase affinity, make that various ingredients is separated in the sample;
D, conversion: convert each negative ion that is separated of step c to strong acid through the rejector system with high conductivity, leacheate then changes the carbonic acid of weak conductivity into, and measure the conductivity of each anionic group by electric conductivity detector, quantitative with relative retention time and peak height or area;
E, concentrated: the component of separated and collected is concentrated by the ion-exchange evaporating column, collect the sample of 5-8min time period, concentrate;
F, mensuration: under selected chromatographic condition, solution to be measured and standard series are measured, instrument writes down the peak area value for the treatment of measured ion automatically, and chromatographic condition is:
(1) chromatographic column
Guard column, 4 mm;
Analytical column, 4mm;
Evaporating column, 4 mm;
Catch post, 9 * 75mm;
Repel post, 9 * 250 mm.
(2) chromatographic condition
Ion exclusion: repel post, catch post
Leacheate: deionized water;
Flow velocity: 0.50 mL/min.
The condition of concentrating: evaporating column
Leacheate: potassium hydroxide (20 mM-60 mM);
Flow velocity: 1.00mL/min;
Sample size: 200 μ L;
Detecting device: inhibition type detecting device;
G, calculating: with the concentration of standard solution is horizontal ordinate, and peak area value is an ordinate, draws out the working curve of chlorion, nitrate ion, sulfate ion respectively, obtains anionic content to be measured in the phosphoric acid according to working curve.
Method detection limit and accuracy rate
1. detection limit
According to chromatography detection limit d computing formula d=3 * n * c/a, n is baseline noise (maximal value 0.003 μ s is got in this experiment) in the formula, and c is the mass concentration of standard substance, and a is the peak height of standard substance, obtains the detection limit of instrument.Consider the sample weighting amount and the dilution volume of this experimental technique, calculate the detection limit of method, see Table 1.
Table 1 detection limit test findings
2. precision
According to test method, repeatedly to measure with the electron-level phosphoric acid sample that two anion-contents differ bigger, test findings sees Table 2.Relative standard deviation (RSD) is Cl
-Less than 2.78%, NO
3 -Less than 1.59%, SO
4 2-Less than 6.15%.
Table 2 Precision test result
3. the recovery
The electron-level phosphoric acid sample is carried out the mark-on recovery test of variable concentrations, and test findings sees Table 3.The recovery of standard addition of each ion is respectively Cl 100
-%～108%, NO
3 -98%～111%, SO
4 2-99%～102%.
Table 3 recovery of standard addition test findings
Claims (3)
1. the anionic method of detected electrons level phosphoric acid trace impurity is characterized in that, its detection step is:
A, sample solution: accurately take by weighing the electron-level phosphoric acid sample, add the deionized water dilution, mixing is mixed with 40%～60% sample solution;
The preparation of b, standard serial solution: according to the compound method of sample solution, prepare at least 4 parts of solution, in every part of solution, add and contain Cl
-, NO
3 -And SO
4 2-The negative ion mixed standard solution is mixed with and contains Cl
-, NO
3 -And SO
4 2-Standard serial solution, the concentration range of each ion is just prepared according to the content of testing sample in the standard serial solution, scope is 0.005～10 μ g/g;
C, separation: respectively sample solution and standard serial solution are entered ion exchange system, corresponding ion exchanges in the ion in the sample solution and the moving phase, and different ions is attached on the fixed charge in the stationary phase;
D, conversion: each negative ion that step c is separated converts the strong acid with high conductivity to through the rejector system, and the KOH leacheate then changes the carbonic acid of weak conductivity into, and is measured the conductivity of each anionic group by electric conductivity detector;
E, concentrated: the component of separated and collected is concentrated by the ion-exchange evaporating column;
F, mensuration: under selected chromatographic condition, adopt ion chromatograph that sample solution and standard serial solution are measured, instrument writes down the peak area value for the treatment of measured ion automatically;
G, calculating: with mixed standard solution concentration is horizontal ordinate, and peak area value is an ordinate, draws out the working curve of chlorion, nitrate ion, sulfate ion respectively, obtains anionic content to be measured in the phosphoric acid according to working curve.
2. according to the anionic method of detected electrons level phosphoric acid trace impurity described in the claim 1, it is characterized in that it is the sample of collecting the 5-8min time period that the described collection of step g concentrates, and concentrates.
3. according to the anionic method of detected electrons level phosphoric acid trace impurity described in the claim 1, it is characterized in that the chromatographic condition that step h adopted is:
(1) chromatographic column
Guard column, 4 mm;
Analytical column, 4mm;
Evaporating column, 4 mm;
Catch post, 9 * 75mm;
Repel post, 9 * 250 mm;
(2) chromatographic condition
Ion exclusion: repel post, catch post
Leacheate: deionized water;
Flow velocity: 0.50 mL/min;
The condition of concentrating: evaporating column
Leacheate: potassium hydroxide (20 mM-60 mM);
Flow velocity: 1.00mL/min;
Sample size: 200 μ L;
Detecting device: inhibition type detecting device.
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|---|---|---|---|
| CN 201010501146 CN102023190A (en) | 2010-10-09 | 2010-10-09 | Method for detecting electronic-grade phosphoric acid trace impurity anions |
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|---|---|---|---|
| CN 201010501146 CN102023190A (en) | 2010-10-09 | 2010-10-09 | Method for detecting electronic-grade phosphoric acid trace impurity anions |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104483441A (en) * | 2014-11-20 | 2015-04-01 | 浙江大学 | System and method for separating fluorine ions and low-molecular-weight organic acids by ion-chromatographic-column switching method |
| CN111889083A (en) * | 2020-07-20 | 2020-11-06 | 中国科学院上海光学精密机械研究所 | Preparation of magnetic hydrotalcite and determination method of trace F, Cl anions in phosphorus-rich sample |
| CN113161152A (en) * | 2021-04-13 | 2021-07-23 | 新疆众和股份有限公司 | Method for leaching and detecting phosphate radical in anode foil of aluminum electrolytic capacitor |
| 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 |
| CN115494179A (en) * | 2022-09-30 | 2022-12-20 | 中国科学院大连化学物理研究所 | Analysis method for simultaneously detecting multiple anions in glycerol |
-
2010
- 2010-10-09 CN CN 201010501146 patent/CN102023190A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 《Journal of Chromatography A》 20021231 F.S. Stover Automated trace anion determinations in concentrated electronic grade phosphoric acid by ion chromatography 文章摘要、第2-3节 1-3 第956卷, * |
| 《分析测试学报》 20050531 史亚利等 直接进样离子色谱法测定磷酸试剂中痕量无机阴、阳离子 128-130 1-3 第24卷, 第3期 * |
| 《现代科学仪器》 20001231 顾海宁等 离子色谱法电导检测同时测定海水中硝酸盐、磷酸盐、硫酸盐等多种阴离子 40-42 1-3 , 第6期 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103454351B (en) * | 2013-03-02 | 2015-03-11 | 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 |
| CN104483441A (en) * | 2014-11-20 | 2015-04-01 | 浙江大学 | System and method for separating fluorine ions and low-molecular-weight organic acids by ion-chromatographic-column switching method |
| CN111889083A (en) * | 2020-07-20 | 2020-11-06 | 中国科学院上海光学精密机械研究所 | Preparation of magnetic hydrotalcite and determination method of trace F, Cl anions in phosphorus-rich sample |
| CN111889083B (en) * | 2020-07-20 | 2023-06-06 | 中国科学院上海光学精密机械研究所 | Preparation of magnetic hydrotalcite and determination method of trace F, cl anions in phosphorus-rich sample |
| CN113161152A (en) * | 2021-04-13 | 2021-07-23 | 新疆众和股份有限公司 | Method for leaching and detecting phosphate radical in anode foil of aluminum electrolytic capacitor |
| 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 |
| CN115494179A (en) * | 2022-09-30 | 2022-12-20 | 中国科学院大连化学物理研究所 | Analysis method for simultaneously detecting multiple anions in glycerol |
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Application publication date: 20110420 |