CN103913452A - Method for measuring oxalate content in vanadyl oxalate product - Google Patents
Method for measuring oxalate content in vanadyl oxalate product Download PDFInfo
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Abstract
The invention provides a method for measuring oxalate content in a vanadyl oxalate product, comprising the following steps: mixing a to-be-measured sample with a calcium salt; dissolving the sample with hydrochloric acid and forming a first solution with the calcium salt, regulating the pH to be 6-7 with ammonia water, standing for ageing and precipitation; filtering to obtain a calcium oxalate precipitate, dissolving with nitric acid to form a second solution, adding ammonium persulfate, heating until large bubbles are generated, regulating pH to be greater than 12 with sodium hydroxide, then adding sodium carbonate, boiling, filtering to obtain a precipitate, dissolving with hydrochloric acid to form a third solution; regulating pH of the third solution to be 2.5-3.5 with potassium hydroxide or sodium hydroxide, adding an ammonia buffer solution to regulate pH to be 6-7, cooling, adding proper amount of a copper agent to form a fourth solution; measuring content of calcium in the fourth solution by using a complexometric titration, and thus calculating the oxalate content in the to-be-measured sample. According to the invention, the content of oxalate content in the vanadyl oxalate product can be accurately measured, and good precision degree and recovery rate are achieved.
Description
Technical field
The present invention relates to oxalate denominationby content analysis detection technique field, specifically, relate to a kind of method of measuring oxalic acid vanadyl product oxalate content.
Background technology
Conventionally, oxalic acid vanadyl is the precursor of multiple choices oxidation catalyst, can produce the barium oxide with catalytic activity by the thermal decomposition of oxalic acid vanadyl.This active matter usually generates vanadium oxides composite together with other oxide, industrial significant.The quality of oxalic acid vanadyl product and the method for inspection of grade are the research and development important support of oxalic acid vanadyl Product Process, purity and the quality of oxalic acid vanadyl product at present, and the mol ratio with oxalate according to vanadium (IV) conventionally, and the content of impurity element is determined.Do not find at present the open source literature of oxalic acid vanadyl oxalate content assaying method.
Mainly contain titrimetry, spectrophotometric method, high pressure lipuid chromatography (HPLC) and the chromatography of ions etc. about the assay method of oxalate.Conventionally the mensuration of high-load oxalate is take titrimetry as main, and wherein take potassium permanganate as titrant, the method for carrying out calculating oxalate radical content with the consumption of potassium permanganate is most widely used general.But these methods are not suitable for measuring the content of oxalic acid vanadyl product oxalate.
Therefore, need a kind of method of measuring oxalic acid vanadyl product oxalate content badly.
Summary of the invention
The object of the invention is to solve at least one in prior art above shortcomings.
For example, one of object of the present invention is to provide a kind of method of measuring oxalic acid vanadyl product oxalate content.
The invention provides a kind of method of measuring oxalic acid vanadyl product oxalate content.Described method comprises the following steps of carrying out successively: oxalic acid vanadyl sample to be measured is mixed with calcium salt; Form the first solution with dissolving with hydrochloric acid oxalic acid vanadyl to be measured sample and calcium salt, the pH of the first solution is adjusted to 6～7 with ammoniacal liquor, make oxalate and Ca
2+form calcium oxalate precipitation, leave standstill and precipitate with ageing; Filter, obtain calcium oxalate precipitation, form the second solution with nitric acid dissolve calcium oxalate precipitation, in the second solution, add ammonium persulfate, be heated to the second solution and emit air pocket, regulate the pH>12 of the second solution with NaOH, then, add sodium carbonate, boil, filter, be precipitated, with this precipitation formation the 3rd solution of dissolving with hydrochloric acid; The pH of the 3rd solution is adjusted to 2.5～3.5 with potassium hydroxide or NaOH, adds ammonia buffer that the pH of the 3rd solution is adjusted to 6～7, cooling, add amount of copper reagent, form the 4th solution; With the calcium element content in complexometric titration the 4th solution, thereby calculate the oxalate content in oxalic acid vanadyl sample to be measured.
Compared with prior art, beneficial effect of the present invention comprises: content that can Accurate Determining oxalic acid vanadyl product oxalate, and there is good precision and the recovery.
Embodiment
Hereinafter, describe the method for mensuration oxalic acid vanadyl product oxalate content of the present invention in detail in connection with exemplary embodiment.
Formed by the following steps of carrying out successively according to the method for mensuration oxalic acid vanadyl oxalate content of the present invention: oxalic acid vanadyl sample to be measured is mixed with calcium salt; Form the first solution with dissolving with hydrochloric acid oxalic acid vanadyl to be measured sample and calcium salt, the pH of the first solution is adjusted to 6～7 with ammoniacal liquor, make oxalate and Ca
2+form calcium oxalate precipitation, leave standstill and precipitate with ageing; Filter, obtain calcium oxalate precipitation, form the second solution with nitric acid dissolve calcium oxalate precipitation, in the second solution, add ammonium persulfate, be heated to the second solution and emit air pocket, regulate the pH>12 of the second solution with NaOH, then, add sodium carbonate, boil, filter, be precipitated, with this precipitation formation the 3rd solution of dissolving with hydrochloric acid; The pH of the 3rd solution is adjusted to 2.5～3.5 with potassium hydroxide or NaOH, adds ammonia buffer that the pH of the 3rd solution is adjusted to 6～7, cooling, add amount of copper reagent, form the 4th solution; With the calcium element content in complexometric titration the 4th solution, thereby calculate the oxalate content in oxalic acid vanadyl sample to be measured.
In one exemplary embodiment of the present invention, calcium salt can be one or more in calcium carbonate, lime chloride, calcium oxide.But, the invention is not restricted to this, can be also other calcium salt.The consumption of calcium salt wants to make all oxalates to generate precipitation.
In one exemplary embodiment of the present invention, in the step of ageing precipitation, the standing time is 4h～7h.But, the invention is not restricted to this, for example, the time of repose in the step of ageing precipitation also can be larger.
In one exemplary embodiment of the present invention, ammonia buffer can be ammonia spirit or hexamethylenetetramine solution.But, the invention is not restricted to this, for example, ammonia buffer also can other buffer solution that contains ammonium radical ion.
In one exemplary embodiment of the present invention, compleximetry can be EDTA titrimetry, EGTA or CyDTA titrimetry.
In one exemplary embodiment of the present invention, in the situation that in the step that oxalic acid vanadyl sample to be measured is mixed with calcium salt, the amount of measuring of oxalic acid vanadyl sample to be measured is 0.1～0.5g, the addition of described ammonium persulfate is 0.5～2g, the addition of described sodium carbonate is 2g～5g, and the addition of described cupferron is 0.1～1.0g.But, the invention is not restricted to this, the addition of ammonium persulfate, sodium carbonate, cupferron etc. also can be excessive, and the dosage having more for ammonium persulfate, sodium carbonate, cupferron etc. can be removed by modes such as heating.
In another exemplary embodiment of the present invention, the method for measuring oxalic acid vanadyl product oxalate content also can realize by following steps:
A, take testing sample in beaker, add calcium salt (calcium salt can be benchmark or high-purity), here, preferably, sample size taken amount is 0.1～0.5g, can avoid like this waste of calcium salt;
B, in testing sample, add water and hydrochloric acid, sample and calcium salt are dissolved completely, slowly add ammoniacal liquor, regulator solution pH, leaves standstill a few hours ageing precipitation;
C, with Filter paper filtering at a slow speed, with Warm Wash beaker and precipitate approximately 8～10 times.The acid-soluble solution of 10mL～20mL for precipitation, add 0.5g～2g ammonium persulfate, be heated to solution and emit air pocket, benefit adds water to 200mL left and right, uses sodium hydrate regulator solution pH>12, enters sodium carbonate, boil, with Filter paper filtering at a slow speed, with Warm Wash beaker and precipitate approximately 3～4 times, with hot hydrochloric acid (1+1) dissolution precipitation in 500mL beaker;
D, be about 3 with potassium hydroxide or sodium hydrate regulator solution pH, then add ammonia buffer regulator solution pH to be 6～7, cooling, add amount of copper reagent, stir;
E, solution is proceeded in 500mL volumetric flask, point get appropriate filtrate, by the calcium amount in complexometric titration test solution, according to the volume of the standard titration solution consuming, calculation sample oxalate content.
In the steps A of this exemplary embodiment, the calcium salt adding, can be calcium carbonate, lime chloride, calcium oxide etc., reagent purity is got over Gao Yuegao, for example, the purity of calcium salt can be greater than 99.5%, and it is excessive 10%～20% that the addition of calcium salt requires, and the addition of calcium salt can be carried out theory calculating by sample size when measuring.Add excessive calcium salt to make and oxalate denominationby oxalic calcium, the oxalate in sample is precipitated completely.
In the step B of this exemplary embodiment, adding ammoniacal liquor to regulate pH is 6～7, and under this pH, a large amount of tetravalence vanadium in sample are dissolved in ammoniacal liquor, and a small amount of pentavalent vanadium and calcium generate vanadic acid calcium, generates co-precipitation with calcium oxalate.Due to crystalline precipitate CaC
2o
4easily forming can be through the small crystallization of filter paper, so the condition that generates larger crystalline form is created in necessary ageing.Ageing not only can make to precipitate crystal grain and grow up, and makes precipitation more pure.For example, digestion time is preferably 4h～7h.
In the step C of this exemplary embodiment, the co-precipitation of calcium oxalate and vanadic acid calcium is after washing, and with excessive calcium ion, a large amount of tetravalence vanadium separates, and precipitation, after acid-soluble solution, must be carried out the separation of vanadium.Directly use complexometric titration calcium amount if do not separate vanadium, vanadium can seal calcon-carboxylic acid, causes analysis result on the low side.The present invention adopts following technology path to eliminate the interference of vanadium: utilize under strong alkaline condition, add sodium carbonate to make pentavalent vanadium be converted into solubility vanadic acid sodium, in order to guarantee the thorough separation of pentavalent vanadium, the dissolving acid of precipitation is chosen the nitric acid of oxidisability, add ammonium persulfate as oxygenant, vanadium oxide is all pentavalent vanadium simultaneously.The concentration of nitric acid is preferably the salpeter solution that is not less than (1+3), and the salpeter solution of described (1+3) is by the nitric acid of 1 part and the water of 3 parts form by volume.For example, in this exemplary embodiment, can adopt the salpeter solution of (1+3), its consumption can be controlled at 10mL～20mL.
In the step D of this exemplary embodiment, adding ammonia buffer to regulate test solution pH is 6～7, then adds amount of copper reagent to make calcium and a small amount of separation of metal ions that may cause interference.Ammonia buffer can be ammoniacal liquor, can be also six methine solution.The consumption of cupferron (for example, sodium diethyldithiocarbamate) is advisable with 0.2～1.0g.
In determination step E, point get appropriate test solution and carry out according to corresponding Standard of analytical methods titration operation step, the standard solution of complexometry can be selected EDTA, EGTA, Standard of analytical methods can be selected GB/T3286.1-2012 " lime stone and rauhkalk chemical analysis method part 1: the mensuration compleximetry of calcium oxide and content of magnesia ", GB/T6730.13-2007 " the mensuration EGTA-CyDTA titrimetry of iron ore calcium and content of magnesium " etc.
Describe exemplary embodiment of the present invention in detail below in conjunction with concrete example, but the present invention is not limited to following example.
Example 1: the EGTA titration measuring of oxalic acid vanadyl oxalate content
Accurately take oxalic acid vanadyl sample 0.250g in 400mL beaker, add 0.3000g calcium carbonate (benchmark, content 99.99), add 50mL distilled water, 5mL hydrochloric acid (1+1), is heated to dissolve completely, adds boiling water to liquor capacity 200mL left and right, slowly drip ammoniacal liquor and adjust pH value of solution 6～7, place 6h.With Filter paper filtering at a slow speed, with Warm Wash beaker and precipitate approximately 8～10 times.Precipitation is dissolved with the hot nitric acid of 10mL (1+1), add 0.5g ammonium persulfate, be heated to solution and emit air pocket, benefit adds water to about 200mL, is strong basicity (pH>12) with sodium hydrate regulator solution, adds 2g sodium carbonate, boil 2min, with Filter paper filtering at a slow speed, with Warm Wash beaker and precipitate approximately 3～4 times, rinse lower precipitation with hot hydrochloric acid (1+1); Benefit adds water to about 200mL, boils and takes off, and is adjusted to pH value of solution approximately 3 with potassium hydroxide (200g/L), it is 6～7 cooling adding the molten buffer solution of hexamethylenetetramine (400g/L) regulator solution pH, add about 0.5g cupferron, solution is proceeded in 500mL volumetric flask, dry filtration.Titration operation according to the 7.4.4 calcium of GB/T6730.13-2007 " the mensuration EGTA-CyDTA titrimetry of iron ore calcium and content of magnesium " carries out, be specially: divide and get 100.0mL filtrate in 300mL beaker, add 5mL triethanolamine solution (1+3), 5mL dextrin solution (50g/L), 20mL potassium hydroxide solution (200g/L) and appropriate calcon-carboxylic acid, be titrated to solution with EGTA standard titration solution (0.01mol/L) and become blueness from claret and be titration end-point.The computing formula of oxalate is as follows:
In formula: the concentration of C-EGTA standard titration solution, mol/L;
The molal weight of 88.02-oxalate, g/mol.
Same oxalate sample is carried out to independent mensuration according to the method described above 11 times, and the precision of statistical method, the results are shown in Table 1.
Table 1 EGTA titration measuring result
Good, reliable and stable by table 1 visual method precision.
Example 2: the EGTA titration measuring of oxalic acid vanadyl oxalate content
Accurately take oxalic acid vanadyl sample 0.300g in 400mL beaker, add 0.2500g calcium oxide (high-purity, 4N), add 50mL distilled water, 10mL hydrochloric acid (1+1), is heated to dissolve completely, adds boiling water to liquor capacity 200mL left and right, slowly drip ammoniacal liquor and adjust pH value of solution 6～7, place 6h.With Filter paper filtering at a slow speed, with Warm Wash beaker and precipitate approximately 8～10 times.Precipitation is dissolved with the hot nitric acid of 15mL (1+2), add 1.0g ammonium persulfate, be heated to solution and emit air pocket, benefit adds water to about 200mL, is strong basicity (pH>12) with sodium hydrate regulator solution, adds 3g sodium carbonate, boil 2min, with Filter paper filtering at a slow speed, with Warm Wash beaker and precipitate approximately 3～4 times, rinse lower precipitation with hot hydrochloric acid (1+1); Benefit adds water to about 200mL, boils and takes off, and is adjusted to pH value of solution approximately 3 with potassium hydroxide (200g/L), adds ammoniacal liquor (1+1) regulator solution pH and is 6～7, cooling, adds about 1.0g cupferron, solution is proceeded in 500mL volumetric flask to dry filtration.3.5.5.1.1 according to GB/T3286.1-2012 " lime stone and rauhkalk chemical analysis method part 1: the mensuration compleximetry of calcium oxide and content of magnesia " carries out titration, be specially: divide and get 100.0mL filtrate in 500mL conical flask, add 5mL triethanolamine (1+4), mix, add 20mL potassium hydroxide solution (200g/L) and about 0.1g calcon-carboxylic acid, mix.Being titrated to test solution with EDTA standard titration solution (0.01mol/L), to become sapphirine from redness be terminal.The computing formula of oxalate is as follows:
In formula: the concentration of C-EDTA standard titration solution, mol/L;
The molal weight of 88.02-oxalate, g/mol.
Table 2EDTA titration measuring result
Good, reliable and stable by table 2 visual method precision.Table 1 and table 2 data can find out, EDTA titrimetry and EGTA titrimetry data are basically identical, and the goodness of fit is very high.
Application Example 3: the determination of recovery rates of method
Take an oxalic acid vanadyl sample, add the benchmark sodium oxalate of different amounts, the recovery of assay method,
Carry out the accuracy of verification method.The results are shown in Table 3
Table 3 recovery test result
As can be seen from Table 3, the recovery of double methods of titration all can meet mensuration requirement.
In sum, the content that method of the present invention can Accurate Determining oxalic acid vanadyl product oxalate, and there is good precision and the recovery.
Although described the present invention in conjunction with exemplary embodiment above, those of ordinary skills should be clear, in the case of not departing from the spirit and scope of claim, can carry out various modifications to above-described embodiment.
Claims (6)
1. a method of measuring oxalic acid vanadyl product oxalate content, is characterized in that, described method comprises the following steps of carrying out successively:
Oxalic acid vanadyl sample to be measured is mixed with calcium salt;
Form the first solution with dissolving with hydrochloric acid oxalic acid vanadyl to be measured sample and calcium salt, the pH of the first solution is adjusted to 6～7 with ammoniacal liquor, make oxalate and Ca
2+form calcium oxalate precipitation, leave standstill and precipitate with ageing;
Filter, obtain calcium oxalate precipitation, form the second solution with nitric acid dissolve calcium oxalate precipitation, in the second solution, add ammonium persulfate, be heated to the second solution and emit air pocket, regulate the pH>12 of the second solution with NaOH, then, add sodium carbonate, boil, filter, be precipitated, with this precipitation formation the 3rd solution of dissolving with hydrochloric acid;
The pH of the 3rd solution is adjusted to 2.5～3.5 with potassium hydroxide or NaOH, adds ammonia buffer that the pH of the 3rd solution is adjusted to 6～7, cooling, add amount of copper reagent, form the 4th solution;
With the calcium element content in complexometric titration the 4th solution, thereby calculate the oxalate content in oxalic acid vanadyl sample to be measured.
2. the method for mensuration oxalic acid vanadyl product oxalate content according to claim 1, is characterized in that, described calcium salt is one or more in calcium carbonate, lime chloride, calcium oxide.
3. the method for mensuration oxalic acid vanadyl product oxalate content according to claim 1, is characterized in that, in the step of described ageing precipitation, the standing time is 4h～7h.
4. the method for mensuration oxalic acid vanadyl product oxalate content according to claim 1, is characterized in that, described ammonia buffer is ammonia spirit or hexamethylenetetramine solution.
5. the method for mensuration oxalic acid vanadyl product oxalate content according to claim 1, is characterized in that, described compleximetry is EDTA titrimetry, EGTA or CyDTA titrimetry.
6. the method for mensuration oxalic acid vanadyl product oxalate content according to claim 1, it is characterized in that, in the described step that oxalic acid vanadyl sample to be measured is mixed with calcium salt, the amount of measuring of oxalic acid vanadyl sample to be measured is 0.1～0.5g, the addition of described ammonium persulfate is 0.5～2g, the addition of described sodium carbonate is 2g～5g, and the addition of described cupferron is 0.1～1.0g.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104655610A (en) * | 2015-01-28 | 2015-05-27 | 攀钢集团研究院有限公司 | Analysis method and determination method of oxalate ion content in vanadyl oxalate |
| CN104880460A (en) * | 2015-05-19 | 2015-09-02 | 中国食品发酵工业研究院 | Method for identifying oxalate in portable spirit |
| CN112180030A (en) * | 2020-09-17 | 2021-01-05 | 大连博融新材料有限公司 | Method for measuring oxalate content in vanadyl oxalate solution through potentiometric titration and application |
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| CN102928421A (en) * | 2012-10-24 | 2013-02-13 | 山东农业大学 | Rapid determination method for content of calcium in limestone flour |
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| CN102928421A (en) * | 2012-10-24 | 2013-02-13 | 山东农业大学 | Rapid determination method for content of calcium in limestone flour |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104655610A (en) * | 2015-01-28 | 2015-05-27 | 攀钢集团研究院有限公司 | Analysis method and determination method of oxalate ion content in vanadyl oxalate |
| CN104655610B (en) * | 2015-01-28 | 2018-05-01 | 攀钢集团研究院有限公司 | The analysis method and assay method of vanadyl oxalate oxalate ion concentration |
| CN104880460A (en) * | 2015-05-19 | 2015-09-02 | 中国食品发酵工业研究院 | Method for identifying oxalate in portable spirit |
| CN112180030A (en) * | 2020-09-17 | 2021-01-05 | 大连博融新材料有限公司 | Method for measuring oxalate content in vanadyl oxalate solution through potentiometric titration and application |
| CN112180030B (en) * | 2020-09-17 | 2022-05-13 | 大连博融新材料有限公司 | Method for measuring oxalate content in vanadyl oxalate solution through potentiometric titration and application |
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Application publication date: 20140709 |