CN105548149A - Method for measuring purity of barium sulfate for lead-acid storage battery - Google Patents
Method for measuring purity of barium sulfate for lead-acid storage battery Download PDFInfo
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- CN105548149A CN105548149A CN201511016838.0A CN201511016838A CN105548149A CN 105548149 A CN105548149 A CN 105548149A CN 201511016838 A CN201511016838 A CN 201511016838A CN 105548149 A CN105548149 A CN 105548149A
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a method for measuring the purity of barium sulfate for a lead-acid storage battery. The amount of barium ions is invariant, and the purity of barium sulfate is calculated steadily. The measurement method is simple, and has high accuracy and good measurement result consistency.
Description
Technical field
The present invention relates to lead-acid storage battery production technical field, particularly a kind of assay method of lead-acid accumulator barium sulphate purity.
Background technology
Barium sulphate is colourless orthorhombic system crystals or white amorphous powder, easily lumps time dry.Relative density 4.50 (15 DEG C), fusing point 1580 DEG C.Water-soluble, ethanol and acid hardly.Be dissolved in hot concentrated sulfuric acid.Polymorphic transformation is there is at about 1150 DEG C.Start significantly to decompose at about 1400 DEG C.Stable chemical nature.Barium sulphate is as a kind of adjuvant of acid accumulator negative pole lead, and self difficulty is dissolved in acidity and alkaline solution.In existing chemical analysis technology, be mainly two kinds of methods and content detection is carried out to barium sulphate in lead plaster.The first uses nitric acid dissolve method, and dissolve the material of solubility, filtration washing, the solution obtained carries out inductively coupled plasma test.Barium sulphate can not be dissolved in solution by the method completely, and most barium sulphate is present in filter residue, very low to the test accuracy of barium.Second method is then the GB GB/T2899-2008 detection method with reference to barium sulphate, natrium carbonicum calcinatum and sal tartari is used to mix by quality 4:1 with barium sulphate, roasting under 800 DEG C of conditions, be translated into barium carbonate, washing, after filter residue is carried out acid dissolve, inductively coupled plasma test is carried out to solution.Material, to the test of barium sulphate, relatively better, but need be carried out pyroprocessing by the method, and treatment conditions are harsh.And carry out at material in the process shifted, the loss of barium ion is more, collimation and the consistance of front and back experiment are poor.Its accuracy is also poor, and front and back otherness is larger.Many problems are still existed to the test of barium sulphate.
The barium sulphate purity of existing lead-acid accumulator, when being greater than 98%, thinks qualified, and purity is not up to standard can affect performances of the lead-acid battery.But because existing detection method exists some problems, cause barium sulphate purity detecting consistance poor, data difference is detected comparatively greatly to the different batches that a producer provides, cannot accurately judge barium sulphate purity.
Summary of the invention
The object of the present invention is to provide a kind of assay method of lead-acid accumulator barium sulphate purity, take barium ion as invariant, the purity of constant calculating barium sulphate, and method of testing is simple, and accuracy is high, and check result consistance is better.
The technical solution adopted for the present invention to solve the technical problems is:
An assay method for lead-acid accumulator barium sulphate purity, comprises the following steps:
(1) the barium sulphate sample taking mass M adds in clean beaker, add the sodium carbonate liquor of excessive mass concentration 15-30%, be heated to boiling, maintain boiling 15-20min, after having reacted, while hot filter and the hot sodium carbonate liquor of service property (quality) concentration 2-5% fully wash filter residue to sulfate radical-free ion intermediate A, discard filtrate;
This step selects the hot sodium carbonate liquor washing of mass concentration 2-5% to take away barium ion, the detection method of abundant washing filter residue to sulfate radical-free ion is: get 1mL filtrate, add the barium chloride solution that 2 are analyzed pure 1+1 hydrochloric acid solution and 0.5mL mass concentration 5-20% successively, after leaving standstill 5min, filtrate still keeps transparent.
(2) in intermediate A, the pure 1+1 hydrochloric acid solution of quantitative analysis was added, be heated to boiling, maintain boiling 15-20min, filter while hot and use pure water to carry out washing to without barium ion, collect filtrate, be settled to volume V, use ICP inductively-coupled plasma spectrometer to measure barium ion content m, calculate the purity X obtaining barium sulphate sample.
This step uses pure water to carry out washing to without the detection method barium ion: get 1mL filtrate, add 2 mass concentration 20% sulfuric acid solutions, and after standing 5min, filtrate still keeps transparent.
The present invention improves existing method, also contrasts the accuracy of barium sulphate test and the consistance of experiment, draws one method more accurately.The present invention is relatively simple to the method for testing of barium sulphate, and accuracy is high, and through repeatedly contrast experiment, the consistance of front and back is better.
As preferably, in step (1), the consumption of the sodium carbonate liquor of mass concentration 15-30% adds 100-300mL meter according to 0.01g barium sulphate sample.
As preferably, in step (1), the temperature of hot sodium carbonate liquor controls as 40-70 DEG C.
As preferably, the consumption analyzing pure 1+1 hydrochloric acid solution in step (2) adds 20-25mL meter according to 0.01g barium sulphate sample.
As preferably, analyze the pure concentrated hydrochloric acid of analysis that pure 1+1 hydrochloric acid solution is mass concentration 36-38% and distilled water mixes according to the volume ratio of 1:1.
As preferably, the computing formula that step (2) calculates barium sulphate sample purity is: X=[(m × V × 233)/(137 × M)] × 100%.M: inductively-coupled plasma spectrometer measures barium content (μ g/ml); V: the volume of constant volume solution, unit is milliliter (mL).M: take sample mass (g).233: barium sulphate molal weight (g/mol).137: the molal weight (g/mol) of barium.
The invention has the beneficial effects as follows:
1, existing detection method uses natrium carbonicum calcinatum and sal tartari to carry out 1:1-3 with sample to mix, at the temperature of about 800 DEG C, carry out melting 40-100min.And the present invention this be use the sodium carbonate liquor of high concentration to transform a small amount of barium sulphate solid, experiment condition is comparatively gentle, does not need harsh reaction conditions, and simple to operate, do not need to carry out high-temperature fusion, energy consumption is little, more economical, meets green production requirement.
2, the product of existing detection method to melting washs, and the solid obtained is carrying out gravimetric determination etc., and sample will there will be loss in the process of transfer, cause test value less than normal.And the present invention only needs the transfer of twice material, the time will greatly reduce.
3, existing detection method (GB GB/T2899-2008 detection method), needs the hot hydrochloric acid of 30ml to carry out repeatedly washing precipitation, more loaded down with trivial details, and the present invention then only needs to wash for twice, simplifies step, reduces the loss of barium ion.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.
In the present invention, if not refer in particular to, the raw material adopted and equipment etc. all can be buied from market or this area is conventional.Method in following embodiment, if no special instructions, is the conventional method of this area.
Preparation of reagents:
Analyze pure 1+1 hydrochloric acid solution: the pure concentrated hydrochloric acid of analysis of mass concentration 36-38% and distilled water mix according to the volume ratio of 1:4.
Embodiment 1:
An assay method for lead-acid accumulator barium sulphate purity, comprises the following steps:
(1) take mass M to be about 0.01g and (to be accurate to 0.0001g, drying, and keep constant weight) barium sulphate sample add in clean beaker, add the sodium carbonate liquor of the excessive mass concentration of 100mL 30%, be heated to boiling, maintain boiling 15min, during boiling suitable supplementary pure water (general 10-20mL), prevent the too high generation bumping of fluid temperature, produce loss of liquid, cause test inaccurate.After having reacted, filter (use at a slow speed quantitative filter paper filter) while hot and the hot sodium carbonate liquor of service property (quality) concentration 2% (70 DEG C) fully washing filter residue to sulfate radical-free ion intermediate A, discard filtrate.
This step fully washs the detection method of filter residue to sulfate radical-free ion: get 1mL filtrate, and add the barium chloride solution that 2 are analyzed pure 1+1 hydrochloric acid solution and 0.5mL mass concentration 5-20% successively, after leaving standstill 5min, filtrate still keeps transparent.
(2) in intermediate A, add 20mL and cross the pure 1+1 hydrochloric acid solution of quantitative analysis, be heated to boiling, maintain boiling 15min, filter while hot and use pure water to carry out washing to without barium ion, collect filtrate, be settled to volume V (250mL), use ICP inductively-coupled plasma spectrometer to measure barium ion content m (0.0284g/L), calculate the purity X obtaining barium sulphate sample.
This step uses pure water to carry out washing to without the detection method barium ion: get 1mL filtrate, add 2 mass concentration 20% sulfuric acid solutions, and after standing 5min, filtrate still keeps transparent.
The computing formula calculating barium sulphate sample purity is: X=[(m × V × 233)/(137 × M)] × 100%=[(0.0284 × 0.25 × 233)/(137 × 0.0123)] × 100%, in lead plaster, barium sulfate content is 98.2% as calculated.
Embodiment 2:
An assay method for lead-acid accumulator barium sulphate purity, comprises the following steps:
(1) take mass M to be about 0.02g and (to be accurate to 0.0001g, drying, and keep constant weight) barium sulphate sample add in clean beaker, add the sodium carbonate liquor of the excessive mass concentration of 600mL 15%, be heated to boiling, maintain boiling 20min, during boiling suitable supplementary pure water (general 10-20mL), prevent the too high generation bumping of fluid temperature, produce loss of liquid, cause test inaccurate.After having reacted, filter (use at a slow speed quantitative filter paper filter) while hot and the hot sodium carbonate liquor of service property (quality) concentration 5% (40 DEG C) fully washing filter residue to sulfate radical-free ion intermediate A, discard filtrate.
This step fully washs the detection method of filter residue to sulfate radical-free ion: get 1mL filtrate, and add the barium chloride solution that 2 are analyzed pure 1+1 hydrochloric acid solution and 0.5mL mass concentration 5-20% successively, after leaving standstill 5min, filtrate still keeps transparent.
(2) in intermediate A, add 25mL and cross the pure 1+1 hydrochloric acid solution of quantitative analysis, be heated to boiling, maintain boiling 20min, filter while hot and use pure water to carry out washing to without barium ion, collect filtrate, be settled to volume V (250mL), use ICP inductively-coupled plasma spectrometer to measure barium ion content m (0.0549g/L), calculate the purity X obtaining barium sulphate sample.
This step uses pure water to carry out washing to without the detection method barium ion: get 1mL filtrate, add 2 mass concentration 20% sulfuric acid solutions, and after standing 5min, filtrate still keeps transparent.
The computing formula calculating barium sulphate sample purity is: X=[(m × V × 233)/(137 × M)] × 100%=[(0.0549 × 0.25 × 233)/(137 × 0.0237)] × 100%, in lead plaster, barium sulfate content is 98.5% as calculated.
Embodiment 3:
An assay method for lead-acid accumulator barium sulphate purity, comprises the following steps:
(1) take mass M to be about 0.01g and (to be accurate to 0.0001g, drying, and keep constant weight) barium sulphate sample add in clean beaker, add the sodium carbonate liquor of the excessive mass concentration of 200mL 20%, be heated to boiling, maintain boiling 18min, during boiling suitable supplementary pure water (general 10-20mL), prevent the too high generation bumping of fluid temperature, produce loss of liquid, cause test inaccurate.After having reacted, filter (use at a slow speed quantitative filter paper filter) while hot and the hot sodium carbonate liquor of service property (quality) concentration 3% (50 DEG C) fully washing filter residue to sulfate radical-free ion intermediate A, discard filtrate.
This step fully washs the detection method of filter residue to sulfate radical-free ion: get 1mL filtrate, and add the barium chloride solution that 2 are analyzed pure 1+1 hydrochloric acid solution and 0.5mL mass concentration 5-20% successively, after leaving standstill 5min, filtrate still keeps transparent.
(2) in intermediate A, add 25mL and cross the pure 1+1 hydrochloric acid solution of quantitative analysis, be heated to boiling, maintain boiling 18min, filter while hot and use pure water to carry out washing to without barium ion, collect filtrate, be settled to volume V (250mL), use ICP inductively-coupled plasma spectrometer to measure barium ion content m (0.0259g/L), calculate the purity X obtaining barium sulphate sample.
This step uses pure water to carry out washing to without the detection method barium ion: get 1mL filtrate, add 2 mass concentration 20% sulfuric acid solutions, and after standing 5min, filtrate still keeps transparent.
The computing formula calculating barium sulphate sample purity is: X=[(m × V × 233)/(137 × M)] × 100%=[(0.0259 × 0.25 × 233)/(137 × 0.0112)] × 100%, in lead plaster, barium sulfate content is 98.3% as calculated.
Identical sample adopts GB GB/T2899-2008 detection method to detect, and barium sulphate purity figure is all less than detection method of the present invention, and testing result differs greatly, and visible detection method of the present invention is simple, and accuracy is high, and the consistance of front and back is better.
Described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (6)
1. a lead-acid accumulator assay method for barium sulphate purity, is characterized in that, comprise the following steps:
(1) the barium sulphate sample taking mass M adds in clean beaker, add the sodium carbonate liquor of excessive mass concentration 15-30%, be heated to boiling, maintain boiling 15-20min, after having reacted, while hot filter and the hot sodium carbonate liquor of service property (quality) concentration 2-5% fully wash filter residue to sulfate radical-free ion intermediate A, discard filtrate;
(2) in intermediate A, the pure 1+1 hydrochloric acid solution of quantitative analysis was added, be heated to boiling, maintain boiling 15-20min, filter while hot and use pure water to carry out washing to without barium ion, collect filtrate, be settled to volume V, use ICP inductively-coupled plasma spectrometer to measure barium ion content m, calculate the purity X obtaining barium sulphate sample.
2. assay method according to claim 1, is characterized in that: in step (1), the consumption of the sodium carbonate liquor of mass concentration 15-30% adds 100-300mL meter according to 0.01g barium sulphate sample.
3. assay method according to claim 1 and 2, is characterized in that: in step (1), the temperature of hot sodium carbonate liquor controls as 40-70 DEG C.
4. assay method according to claim 1 and 2, is characterized in that: the consumption analyzing pure 1+1 hydrochloric acid solution in step (2) adds 20-25mL meter according to 0.01g barium sulphate sample.
5. assay method according to claim 4, is characterized in that: analyze the pure concentrated hydrochloric acid of analysis that pure 1+1 hydrochloric acid solution is mass concentration 36-38% and distilled water mixes according to the volume ratio of 1:1.
6. assay method according to claim 1 and 2, is characterized in that: the computing formula that step (2) calculates barium sulphate sample purity is: X=[(m × V × 233)/(137 × M)] × 100%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106596517A (en) * | 2016-11-18 | 2017-04-26 | 超威电源有限公司 | Detection method for content of barium sulfate in recovered lead powder |
| CN108816065A (en) * | 2018-04-24 | 2018-11-16 | 中国科学技术大学 | A method of being completely dissolved barite |
| CN109632768A (en) * | 2018-10-25 | 2019-04-16 | 超威电源有限公司 | A kind of measuring method of antimony oxide purity |
| CN113970541A (en) * | 2020-07-24 | 2022-01-25 | 中国石油天然气股份有限公司 | Method for detecting barium content in chelating agent solution |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106596517A (en) * | 2016-11-18 | 2017-04-26 | 超威电源有限公司 | Detection method for content of barium sulfate in recovered lead powder |
| CN108816065A (en) * | 2018-04-24 | 2018-11-16 | 中国科学技术大学 | A method of being completely dissolved barite |
| CN109632768A (en) * | 2018-10-25 | 2019-04-16 | 超威电源有限公司 | A kind of measuring method of antimony oxide purity |
| CN113970541A (en) * | 2020-07-24 | 2022-01-25 | 中国石油天然气股份有限公司 | Method for detecting barium content in chelating agent solution |
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