CN111579714A - Method for measuring content of copper oxide in copper metaphosphate - Google Patents
Method for measuring content of copper oxide in copper metaphosphate Download PDFInfo
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- CN111579714A CN111579714A CN202010597442.4A CN202010597442A CN111579714A CN 111579714 A CN111579714 A CN 111579714A CN 202010597442 A CN202010597442 A CN 202010597442A CN 111579714 A CN111579714 A CN 111579714A
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- copper
- metaphosphate
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
- G01N31/164—Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The invention belongs to the field of chemical analysis and test, and particularly discloses a determination method capable of rapidly and accurately determining the content of copper oxide in copper metaphosphate. The method for measuring the content of copper oxide in copper metaphosphate comprises a sample weighing step, a melting step, a frit transferring step, a potentiometric titration step and a calculating step. Weighing a proper amount of copper metaphosphate sample, adding a corresponding amount of fluxing agent to melt the copper metaphosphate sample at high temperature, and preparing Cu2+And testing the solution by adopting a potentiometric titration method, and finally calculating to obtain the content of the copper oxide in the copper metaphosphate. The determination method has the advantages of refining, simple and convenient operation, short test time, less types and usage of reagents required to be used, less pollution to the environment, accurate and reliable determination result, good reproducibility and high precision.
Description
Technical Field
The invention belongs to the field of chemical analysis and test, and particularly relates to a method for determining the content of copper oxide in copper metaphosphate.
Background
Copper metaphosphate is a raw material for manufacturing optical glass, and the purity thereof directly affects the optical properties of the optical glass. How to evaluate the purity of the copper metaphosphate is that no corresponding national standard test method is found so far, and no test method can be used for reference in the industry. For soluble metaphosphate salts, the purity is usually evaluated by testing the content of phosphorus pentoxide or the content of metal oxide therein. However, the conventional characterization method has the following disadvantages:
the method has the advantages that the method adopts a phosphomolybdic acid quinoline gravimetric method, the precision and the accuracy are good, the defects are that the analysis steps are complicated, the analysis period is long, and the preparation of the precipitator uses two toxic organic matters, namely acetone and quinoline, so that great harm is brought to analysis and test personnel, and meanwhile, the environment is polluted.
The test of the copper oxide generally adopts an indirect iodometry method, and comprises the following specific steps: after a sample is dissolved, adjusting the pH value of the solution to 3.5-4.0 by using ammonia water and acetic acid, adding a proper amount of potassium iodide to react with divalent copper ions to separate out equivalent iodine, and dripping the equivalent iodine by using standard sodium thiosulfate titration liquid to separate out iodine; starch is used as an indicator, and the end point is judged by the change of color. The method has the advantages of long and complicated process flow, long analysis period, large variety and dosage of used reagents, and easy influence on the judgment of the end point color of the indicator by the acidity of the solution and human factors, which all influence the accuracy of a test result and have poor parallelism.
Disclosure of Invention
The invention aims to provide a method for rapidly and accurately measuring the content of copper oxide in copper metaphosphate.
The technical scheme adopted by the invention for solving the technical problems is as follows: the method for measuring the content of copper oxide in copper metaphosphate comprises the following steps:
a sample weighing step: weighing 0.2-0.45 g of dried copper metaphosphate sample;
a melting step: putting the weighed copper metaphosphate sample into a melting container, adding 3-5 g of fluxing agent into the melting container, and putting the melting container into a heating device to melt the substances in the melting container at high temperature;
a frit transferring step: taking out the melting container from the heating device, and transferring the melted material into a solution container by using hot water and acid liquor after the melted material in the melting container is cooled into a fusion cake;
a potentiometric titration step: firstly, ammonia water is used for adjusting the pH value of a solution in a solution container to 8-9, and 10-20 mL of buffer solution with the pH value of 10 is added; then, a Cu electrode is used as an indicating electrode, an Ag/AgCl electrode is used as a reference electrode, and the EDTA standard solution is used for titrating the Cu in the solution container under the continuous stirring action2+Drawing a U-V curve and a delta U/delta V-V curve to indicate a titration end point;
a calculation step: calculating the content w of copper oxide in the copper metaphosphate sample according to the following formula;
in the formula:
v represents the volume of EDTA standard solution consumed;
c represents the concentration of the EDTA standard solution;
m represents the value of the molar mass of copper oxide;
and m is the mass of the copper metaphosphate sample.
Further, in the step of weighing, the copper metaphosphate sample is dried at 105-110 ℃ and then weighed, and the weighing value is accurate to 0.00001 g.
Furthermore, in the melting step, the mass ratio of the adopted fluxing agent is Na2CO3:K2CO3:Na2B4O7·10H2O＝1:1:2。
Further, in the melting step, the temperature of high-temperature melting is 900-950 ℃ and the time is 10-15 min.
Further, in the frit transfer step, the acid solution used is 1+1 hydrochloric acid or 1+3 sulfuric acid.
Further, the melting container is a corundum crucible, the heating device is a muffle furnace, and the solution container is a beaker.
Further, in the potentiometric titration step, the stirring rate at the time of titration is 40r/min to 50 r/min.
Further, in the potentiometric titration step, the EDTA standard solution was used at a concentration of 0.05mol/L and an initial volume of 80 mL.
The invention has the beneficial effects that: weighing a proper amount of copper metaphosphate sample, adding a corresponding amount of fluxing agent to melt the copper metaphosphate sample at high temperature, and preparing Cu2+Testing the solution by adopting a potentiometric titration method, and finally calculating to obtain the content of copper oxide in the copper metaphosphate; the determination method has the advantages of refining, simple and convenient operation, short test, less types and usage of reagents required to be used, less pollution to the environment, accurate and reliable determination result, good reproducibility and high precision.
Detailed Description
The present invention will be further described with reference to the following examples.
The method for measuring the content of copper oxide in copper metaphosphate comprises the following steps:
a sample weighing step: weighing 0.2-0.45 g of dried copper metaphosphate sample; in the step, a copper metaphosphate sample is dried at 105-110 ℃ and then weighed, and the weighing value is preferably accurate to 0.00001 g;
a melting step: putting the weighed copper metaphosphate sample into a melting container, adding 3-5 g of fluxing agent into the melting container, and putting the melting container into a heating device to melt the substances in the melting container at high temperature; the melting container is generally a crucible, preferably a corundum crucible; the heating device can be various, and is preferably a muffle furnace; the fluxing agent is a substance capable of reducing the softening, melting or liquefaction temperature of the copper metaphosphate; the flux is preferably Na2CO3、K2CO3And Na2B4O7·10H2A mixture of O;
a frit transferring step: taking out the melting container from the heating device, and transferring the melted material into a solution container by using hot water and acid liquor after the melted material in the melting container is cooled into a fusion cake; in the step, the adopted acid solution is preferably 1+1 hydrochloric acid or 1+3 sulfuric acid; the 1+1 hydrochloric acid is a mixed solution of 1 volume of concentrated hydrochloric acid and 1 volume of distilled water; the 1+3 sulfuric acid is a mixed solution of 1 volume of concentrated sulfuric acid and 3 volumes of distilled water; the solution container can be various, and is preferably a beaker;
a potentiometric titration step: firstly, ammonia water is used for adjusting the pH value of a solution in a solution container to 8-9, and 10-20 mL of buffer solution with the pH value of 10 is added; then, a Cu electrode is used as an indicating electrode, an Ag/AgCl electrode is used as a reference electrode, and the EDTA standard solution is used for titrating the Cu in the solution container under the continuous stirring action2+Drawing a U-V curve and a delta U/delta V-V curve to indicate a titration end point; the buffer solution is a mixed solution composed of weak base and salt thereof, and can offset and lighten the influence of the added ammonia water on the pH value of the solution in the solution container to a certain extent, thereby keeping the pH value of the solution relatively stable; the concentration of the adopted EDTA standard solution is preferably 0.05mol/L, and the initial volume is preferably 80 mL;
a calculation step: calculating the content w of copper oxide in the copper metaphosphate sample according to the following formula;
in the formula:
v represents the volume of EDTA standard solution consumed;
c represents the concentration of the EDTA standard solution;
m represents the value of the molar mass of copper oxide;
and m is the mass of the copper metaphosphate sample.
In order to enable the copper metaphosphate sample to be rapidly and effectively melted so as to be prepared into Cu2+In the step of melting the solution, the mass ratio of the adopted fluxing agent is Na2CO3:K2CO3:Na2B4O7·10H2O is 1:1:2, the temperature of high-temperature melting is 900-950 ℃, and the time is 10-15 min.
In order to ensure the titration effect and further shorten the test period, the stirring speed during titration is 40r/min to 50r/min in the potentiometric titration step. Automated mechanical agitation is typically performed using equipment embodied as magnets or paddles.
Example 1
The method comprises the following specific steps of measuring the content of copper oxide in copper metaphosphate at a certain time:
a sample weighing step: weighing a 105-110 ℃ dried copper metaphosphate sample, and accurately weighing the sample to 0.00001 g;
a melting step: putting the weighed copper metaphosphate sample into a corundum crucible, adding 3g of fluxing agent into the corundum crucible, and then placing the corundum crucible into a muffle furnace to melt the substances in the corundum crucible at the high temperature of 900 ℃ for 10 min;
a frit transferring step: taking the corundum crucible out of the muffle furnace, and transferring the corundum crucible into a 200mL beaker by using hot water and 1+1 hydrochloric acid after the molten material in the corundum crucible is cooled to be a clinker;
a potentiometric titration step: firstly, ammonia water is used for adjusting the pH value of a solution in a beaker to 8.5, and 10mL of buffer solution with the pH value of 10 is added; then, a Cu electrode is used as an indicating electrode, an Ag/AgCl electrode is used as a reference electrode, and the Cu in the solution in the beaker is titrated by EDTA standard solution under the stirring action of the stirring speed of 40r/min2+Drawing a U-V curve and a delta U/delta V-V curve to indicate a titration end point;
a calculation step: calculating the content w of copper oxide in the copper metaphosphate sample according to the following formula;
in the formula:
v represents the volume of EDTA standard solution consumed in mL;
c represents the concentration of the EDTA standard solution, and is 0.04805 mol/L;
m represents the number of the molar mass of the copper oxide and the unit is g/mol;
and m is the mass of the weighed copper metaphosphate sample and the unit is g.
Six repeated measurements were performed, and the relevant parameters and the measurement results are shown in table 1 below;
table 1:
the standard average deviation of six repeated measurements is 0.39% by calculation, so that the determination method has accurate and reliable determination result, good reproducibility and high precision.
Example 2
The method comprises the following specific steps of measuring the content of copper oxide in copper metaphosphate at a certain time:
a sample weighing step: weighing a 105-110 ℃ dried copper metaphosphate sample, and accurately weighing the sample to 0.00001 g;
a melting step: putting the weighed copper metaphosphate sample into a corundum crucible, and adding 5g of fluxing agent into the corundum crucible, wherein the mass ratio of the fluxing agent is Na2CO3:K2CO3:Na2B4O7·10H2O1: 1: 2; then placing the corundum crucible in a muffle furnace to melt the substances in the corundum crucible at the high temperature of 950 ℃ for 15 min;
a frit transferring step: taking the corundum crucible out of the muffle furnace, and transferring the corundum crucible into a 200mL beaker by using hot water and 1+3 sulfuric acid after the molten material in the corundum crucible is cooled to be a clinker;
a potentiometric titration step: firstly, ammonia water is used for adjusting the pH value of a solution in a beaker to 9, and 20mL of buffer solution with the pH value of 10 is added; then, a Cu electrode is used as an indicating electrode, an Ag/AgCl electrode is used as a reference electrode, and the Cu in the solution in the beaker is titrated by EDTA standard solution under the stirring action of 50r/min of stirring speed2+Drawing a U-V curve and a delta U/delta V-V curve to indicate a titration end point;
a calculation step: calculating the content w of copper oxide in the copper metaphosphate sample according to the following formula;
in the formula:
v represents the volume of EDTA standard solution consumed in mL;
c represents the concentration of the EDTA standard solution, and is 0.04809 mol/L;
m represents the number of the molar mass of the copper oxide and the unit is g/mol;
and m is the mass of the weighed copper metaphosphate sample and the unit is g.
Six repeated measurements were performed, and the relevant parameters and the measurement results are shown in table 2 below;
table 2:
the standard average deviation of six repeated measurements is 0.27 percent by calculation, so that the measurement method has accurate and reliable measurement result, good reproducibility and high precision.
Claims (8)
1. The method for measuring the content of copper oxide in copper metaphosphate is characterized by comprising the following steps of:
a sample weighing step: weighing 0.2-0.45 g of dried copper metaphosphate sample;
a melting step: putting the weighed copper metaphosphate sample into a melting container, adding 3-5 g of fluxing agent into the melting container, and putting the melting container into a heating device to melt the substances in the melting container at high temperature;
a frit transferring step: taking out the melting container from the heating device, and transferring the melted material into a solution container by using hot water and acid liquor after the melted material in the melting container is cooled into a fusion cake;
a potentiometric titration step: firstly, ammonia water is used for adjusting the pH value of a solution in a solution container to 8-9, and 10-20 mL of buffer solution with the pH value of 10 is added; then, a Cu electrode is used as an indicating electrode, an Ag/AgCl electrode is used as a reference electrode, and the EDTA standard solution is used for titrating the Cu in the solution container under the continuous stirring action2+Drawing a U-V curve and a delta U/delta V-V curve to indicate a titration end point;
a calculation step: calculating the content w of copper oxide in the copper metaphosphate sample according to the following formula;
in the formula:
v represents the volume of EDTA standard solution consumed;
c represents the concentration of the EDTA standard solution;
m represents the value of the molar mass of copper oxide;
and m is the mass of the copper metaphosphate sample.
2. The method for determining the content of copper oxide in copper metaphosphate according to claim 1, wherein: in the sample weighing step, a copper metaphosphate sample is dried at 105-110 ℃ and then weighed, and the weighing value is accurate to 0.00001 g.
3. The method for determining the content of copper oxide in copper metaphosphate according to claim 1, wherein: in the melting step, the mass ratio of the adopted fluxing agent is Na2CO3:K2CO3:Na2B4O7·10H2O＝1:1:2。
4. The method for determining the content of copper oxide in copper metaphosphate according to claim 3, wherein: in the melting step, the temperature of high-temperature melting is 900-950 ℃ and the time is 10-15 min.
5. The method for determining the content of copper oxide in copper metaphosphate according to claim 1, wherein: in the frit transfer step, the acid solution used is 1+1 hydrochloric acid or 1+3 sulfuric acid.
6. The method for determining the content of copper oxide in copper metaphosphate according to claim 1, wherein: the melting container is a corundum crucible, the heating device is a muffle furnace, and the solution container is a beaker.
7. The method for determining the content of copper oxide in copper metaphosphate according to any one of claims 1 to 6, wherein: in the step of potentiometric titration, the stirring speed during titration is 40r/min to 50 r/min.
8. The method for determining the content of copper oxide in copper metaphosphate according to claim 7, wherein: in the potentiometric titration step, the EDTA standard solution was used at a concentration of 0.05mol/L and an initial volume of 80 mL.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4407786A (en) * | 1978-12-21 | 1983-10-04 | International Standard Electric Corporation | Glass composition |
| SU1346598A1 (en) * | 1986-02-27 | 1987-10-23 | Государственный научно-исследовательский институт стекла | Glass |
| CN103353453A (en) * | 2013-06-25 | 2013-10-16 | 彩虹集团电子股份有限公司 | Inductively coupled plasma-atomic emission spectrometry (ICP-AES) method for testing chemical components of blue phosphors of plasma display panel (PDP) |
| CN105044275A (en) * | 2015-08-12 | 2015-11-11 | 成都光明光电股份有限公司 | Method for testing content of aluminum oxide in aluminum metaphosphate |
| WO2016171255A1 (en) * | 2015-04-24 | 2016-10-27 | 旭硝子株式会社 | Near infrared cut-off filter glass |
| CN107132222A (en) * | 2017-06-29 | 2017-09-05 | 成都光明光电股份有限公司 | The assay method of zinc oxide content in metaphosphoric acid zinc |
| CN107202831A (en) * | 2017-06-05 | 2017-09-26 | 深圳市华星光电技术有限公司 | The assay method of copper ion concentration in a kind of copper acid etch liquid |
| CN108982749A (en) * | 2018-06-25 | 2018-12-11 | 河钢股份有限公司 | The method for measuring Main elements nickel and copper content in monel |
| CN110040707A (en) * | 2019-05-13 | 2019-07-23 | 刘鹏 | A kind of preparation method of high-purity optical glass additive metaphosphoric acid copper |
-
2020
- 2020-06-28 CN CN202010597442.4A patent/CN111579714A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4407786A (en) * | 1978-12-21 | 1983-10-04 | International Standard Electric Corporation | Glass composition |
| SU1346598A1 (en) * | 1986-02-27 | 1987-10-23 | Государственный научно-исследовательский институт стекла | Glass |
| CN103353453A (en) * | 2013-06-25 | 2013-10-16 | 彩虹集团电子股份有限公司 | Inductively coupled plasma-atomic emission spectrometry (ICP-AES) method for testing chemical components of blue phosphors of plasma display panel (PDP) |
| WO2016171255A1 (en) * | 2015-04-24 | 2016-10-27 | 旭硝子株式会社 | Near infrared cut-off filter glass |
| CN105044275A (en) * | 2015-08-12 | 2015-11-11 | 成都光明光电股份有限公司 | Method for testing content of aluminum oxide in aluminum metaphosphate |
| CN107202831A (en) * | 2017-06-05 | 2017-09-26 | 深圳市华星光电技术有限公司 | The assay method of copper ion concentration in a kind of copper acid etch liquid |
| CN107132222A (en) * | 2017-06-29 | 2017-09-05 | 成都光明光电股份有限公司 | The assay method of zinc oxide content in metaphosphoric acid zinc |
| CN108982749A (en) * | 2018-06-25 | 2018-12-11 | 河钢股份有限公司 | The method for measuring Main elements nickel and copper content in monel |
| CN110040707A (en) * | 2019-05-13 | 2019-07-23 | 刘鹏 | A kind of preparation method of high-purity optical glass additive metaphosphoric acid copper |
Non-Patent Citations (4)
| Title |
|---|
| XIE,KP 等: "Insight into hydrothermal aging of phosphorus-poisoned Cu-SSZ-13 for NH3-SCR", 《APPLIED CATALYSISI B-ENVIRONMENTAL》 * |
| 杨倩倩 等: "电感耦合等离子体原子发射光谱法测定高纯石墨中9种元素", 《冶金分析》 * |
| 胡建华 等: "添加聚磷酸盐防止工业用碳的氧化", 《新型碳材料》 * |
| 陈治清: "《口腔材料学》", 31 July 2000 * |
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Application publication date: 20200825 |