CN104849165A - Test method of content of high-purity barium fluoride - Google Patents
Test method of content of high-purity barium fluoride Download PDFInfo
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- CN104849165A CN104849165A CN201510246768.1A CN201510246768A CN104849165A CN 104849165 A CN104849165 A CN 104849165A CN 201510246768 A CN201510246768 A CN 201510246768A CN 104849165 A CN104849165 A CN 104849165A
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Abstract
The invention relates to a test method of the content of high-purity barium fluoride, which belongs to the technical field and mainly aims to solve the problems of complex test steps, long time and disadvantageousness in routine analysis of an existing test method. The test method is characterized by comprising the following steps of (1) placing m grams of a solid high-purity barium fluoride powder sample in a platinum crucible or a polytetrafluoroethylene beaker, adding concentrated perchloric acid, heating at low temperature until dense smoke occurs, cooling, and adding water to dissolve and dilute to 100 milliliters; (2) then heating at low temperature to boil, gradually adding dilute sulphuric acid precipitant when being hot, aging, filtering, performing washing precipitation, carbonization and ashing, precipitating barium sulfate at constant weight in a high-temperature furnace at 800 DEG C plus or minus 5 DEG C, wherein the precipitation mass is m1 grams after burning, and calculating to obtain the percent content of the barium fluoride. The test method has the characteristics of simplicity and convenience in test, short time and advantageousness in routine analysis and is mainly used for testing the content of the high-purity barium fluoride.
Description
Technical field
The invention belongs to barium fluoride content measuring technical field, be specifically related to a kind of method of testing of high-purity barium fluoride content.
Background technology
" in barium fluoride, fluorine, barium assay method are inquired into " (" inorganic chemicals industry ", 41st volume 4 phase in 2009) provide a kind of method of testing of barium fluoride content, namely use sal tartari melting barium fluoride sample, make barium fluoride component change into barium carbonate and potassium fluoride, leach and filter; Filter residue (barium carbonate) with dissolving with hydrochloric acid and add sulfuric acid generate barium sulfate precipitate, be deposited in hot solution and filter after ageing.Calcination ashing filter paper records barium content, converts as barium fluoride content.
The shortcoming of use the method is: testing procedure is loaded down with trivial details, and the time is long, unfavorable routine analysis.
Summary of the invention
The object of this invention is to provide a kind of method of testing of high-purity barium fluoride content, adopt simple effective method Removal of F-ion, then directly with the content of barium sulfate precipitate gravimetric method test barium fluoride.
Technical solution of the present invention is: a kind of method of testing of high-purity barium fluoride content, is characterized in that comprising the following steps:
1. solid-state high-purity m gram, barium dust sample of fluoridizing is placed in platinum crucible or tetrafluoro beaker, adds dense perchloric acid, low-temperature heat to smoke clogging near dry after, cooling, adds water and is diluted to 100 milliliters;
2. low-temperature heat is to boiling again, and gradation while hot adds 20% sulfuric acid precipitation agent 10mL, ageing, filtration, washing precipitation, and constant weight barium sulfate precipitate in carbonization, ashing, 800 DEG C ± 5 DEG C high temperature furnaces, calcination postprecipitation quality is m
1gram, the percentage composition of barium fluoride is calculated according to following formula:
In formula: m
1for calcination postprecipitation quality, g;
M is sample quality, g;
0.7514 is the coefficient that barium sulphate changes barium fluoride.
In above-mentioned steps, described solid-state high-purity barium fluoride is purity >=99%; The concentration of described perchloric acid is 70 ~ 72%.
In above-mentioned steps, be placed in tetrafluoro beaker by solid-state high-purity m gram, barium dust sample of fluoridizing, m is 0.2 ~ 0.3 gram (precisely to 0.0001g).
The method of testing of a kind of high-purity barium fluoride content described in technical solution of the present invention, is characterized in that comprising the following steps:
1. solid-state high-purity m gram, barium dust sample of fluoridizing is placed in platinum crucible or tetrafluoro beaker, m is 0.2 ~ 0.3 g (precisely to 0.0001g), adds dense perchloric acid 1 ~ 4ml after adding a small amount of water-wet, low-temperature heat to smoke clogging near dry after, cooling, adds water-soluble solution and is diluted to 100 milliliters;
2. low-temperature heat, to boiling, under agitation at the uniform velocity drips the sulfuric acid solution of 10 mL20%, builds beaker again, and at warm place, standing 3 h or placement are spent the night; With quantitative filter paper filtration at a slow speed, precipitation hot wash is no acidic only to filtrate; Precipitation is placed in calcination in the porcelain crucible of constant weight with filter paper, dry ashing, and in 800 DEG C ± 5 DEG C calcinations to constant weight in high temperature Muffle furnace, calcination postprecipitation quality is m
1gram, the percentage composition of barium fluoride is calculated according to following formula:
In formula: m1 is calcination postprecipitation quality, g;
M is sample quality, g;
0.7514 is the coefficient that barium sulphate changes barium fluoride.
The effect that the present invention is positive: 1) the inventive method adopts acid extracting dissolving directly to prepare barium solution, compared with the alkali solution technique of prior art, has the advantage that required reagent is less; 2), in the barium solution that prepared by this method, impurity content is low, the washing of favourable precipitation.
The present invention have test easy, the time is short, be beneficial to the feature of routine analysis.The present invention is mainly used in the test of high-purity barium fluoride content.
Embodiment
Embodiment one
Take at 110 DEG C of dry 0.3 gram, samples (precisely to 0.0001g), be placed in platinum crucible, a small amount of water-wet, 4ml perchloric acid, low-temperature furnace is heated to smoke clogging after after near doing, take off, move in beaker, be diluted to 100ml, be heated to boil, under agitation at the uniform velocity drip 10 mL sulfuric acid solutions (20%), build beaker, at warm place, standing 3 h or placement are spent the night.With quantitative filter paper filtration at a slow speed, precipitation hot wash is to filtrate is no acidic.Precipitation is placed in calcination in the porcelain crucible of constant weight with filter paper, dry ashing, and in 800 DEG C ± 5 DEG C calcinations to constant weight in high temperature Muffle furnace, calcination postprecipitation quality is m
1gram.The percentage composition of barium fluoride is calculated by formula.
In formula: m
1for calcination postprecipitation quality, g;
M is sample quality, g;
0.7514 is the coefficient that barium sulphate changes barium fluoride.
Duplicate measurements eight samples, test figure and test result see the following form:
It is consistent that embodiment one and ICP-OES method survey 99.76% result that minusing (100-Σ impurity %) that its calcium strontium fluoride burns the impurity such as decrement calculates.
Comparative example 1
Take at 110 DEG C of dry sample 0.4g (precisely to 0.0001g), be placed in platinum crucible, soak with water 50ml, 5ml red fuming nitric acid (RFNA) heating for dissolving, adds 1 gram of boric acid and moves in 250ml beaker, finally add 5 (1+1) hydrochloric acid, adjusting liquor capacity with water is 100 mL, is heated to boil by solution, under agitation at the uniform velocity drips 10 mL20% sulfuric acid solutions, build beaker, at warm place, standing 3 h or placement are spent the night.With quantitative filter paper filtration at a slow speed, precipitation hot wash is no acidic only to filtrate.Precipitation is placed in calcination in the porcelain crucible of constant weight with filter paper, dry ashing, and in 800 DEG C ± 5 DEG C calcinations to constant weight in high temperature Muffle furnace.Calcination postprecipitation quality is m
1gram.The percentage composition of barium fluoride is calculated by formula.
In formula: m
1for calcination postprecipitation quality, g;
M is sample quality, g;
0.7514 is the coefficient that barium sulphate changes barium fluoride.
Duplicate measurements 14 samples, test figure and test result see the following form
Comparative example 2
Take at 110 DEG C of dry 0.4 gram, samples (precisely to 0.0001g), be placed in tetrafluoro beaker, a small amount of water-wet, 4ml perchloric acid, after low-temperature furnace is heated to smoke clogging 5 minutes, take off, move in beaker, be diluted to 100ml, be heated to boil, under agitation at the uniform velocity drip 10 mL20% sulfuric acid solutions, build beaker, at warm place, standing 3 h or placement are spent the night.With quantitative filter paper filtration at a slow speed, precipitation hot wash is no acidic only to filtrate.Precipitation is placed in calcination in the porcelain crucible of constant weight with filter paper, dry ashing, and in 800 DEG C ± 5 DEG C calcinations to constant weight in high temperature Muffle furnace.Calcination postprecipitation quality is m
1gram.The percentage composition of barium fluoride is calculated by formula.
In formula: m
1for calcination postprecipitation quality, g;
M is sample quality, g;
0.7514 is the coefficient that barium sulphate changes barium fluoride.
Duplicate measurements eight samples, test figure and test result see the following form.
Above comparative example shows, comparative example 1 nitric acid dissolve does not drive fluorine test result instability, and precision is poor; Analyze its reason, find that nitrate method also has a small amount of residue after dissolving, and perchloric acid catches up with fluorine method not have residue.Therefore, this law adopts perchloric acid to catch up with fluorine, sulfuric acid precipitation gravimetric method.Comparative example 2 test result is higher, and the large impurity of this precipitation capacity is sandwiched relevant.
Embodiment two
Take at 110 DEG C of dry 0.2 gram, samples (precisely to 0.0001g), be placed in tetrafluoro beaker, a small amount of water-wet, 3ml perchloric acid, after low-temperature furnace is heated to smoke clogging near doing, take off, move in beaker, be diluted with water to 100ml, be heated to boil, under agitation at the uniform velocity drip 10 mL20% sulfuric acid solutions, build beaker, at warm place, standing 3 h or placement are spent the night.With quantitative filter paper filtration at a slow speed, precipitation hot wash is no acidic only to filtrate.Precipitation is placed in calcination in the porcelain crucible of constant weight with filter paper, dry ashing, and in 800 DEG C ± 5 DEG C calcinations to constant weight in high temperature Muffle furnace.Calcination postprecipitation quality is m
1gram.The percentage composition of barium fluoride is calculated by formula.
In formula: m
1for calcination postprecipitation quality, g;
M is sample quality, g;
0.7514 is the coefficient that barium sulphate changes barium fluoride.
Duplicate measurements six samples, test figure and test result see the following form:
Embodiment two and ICP-OES method are surveyed its calcium strontium fluoride and are coincide with the 99.28 % results that the minusing (100-Σ impurity %) burning the impurity such as decrement calculates.
Above embodiment shows, adopts the inventive method perchloric acid to catch up with fluorosulfuric acid precipitation gravimetry, and be conducive to reducing precipitation and sandwich impurity, be convenient to washing of precipitate, taking high-purity barium dust sample quality of fluoridizing is 0.2 ~ 0.3 gram (precisely to 0.0001g).
Claims (4)
1. a method of testing for high-purity barium fluoride content, is characterized in that comprising the following steps:
1. be placed in platinum crucible or tetrafluoro beaker by solid-state high-purity m gram, barium dust sample of fluoridizing, add dense perchloric acid, low-temperature heat is to smokeing clogging, and cooling, adds water and be diluted to 100 milliliters;
2. low-temperature heat is to boiling again, and gradation while hot adds dilute sulfuric acid precipitation agent, ageing, filtration, washing precipitation, and constant weight barium sulfate precipitate in carbonization, ashing, 800 DEG C ± 5 DEG C high temperature furnaces, calcination postprecipitation quality is m
1gram, the percentage composition of barium fluoride is calculated according to following formula:
In formula: m
1for calcination postprecipitation quality, g;
M is sample quality, g;
0.7514 is the coefficient that barium sulphate changes barium fluoride.
2. the method for testing of a kind of high-purity barium fluoride content according to claim 1, is characterized in that: described solid-state high-purity barium fluoride is purity >=99%; The concentration of described perchloric acid is 70 ~ 72%.
3. the method for testing of a kind of high-purity barium fluoride content according to claim 1 and 2, is characterized in that: be placed in tetrafluoro beaker by solid-state high-purity m gram, barium dust sample of fluoridizing, m is 0.2 ~ 0.3 gram, precisely to 0.0001g.
4. the method for testing of a kind of high-purity barium fluoride content according to claim 1 and 2, is characterized in that comprising the following steps:
1. be placed in platinum crucible or tetrafluoro beaker by solid-state high-purity m gram, barium dust sample of fluoridizing, m is 0.2 ~ 0.3, precisely to 0.0001g, dense perchloric acid 1 ~ 4ml is added after adding a small amount of water-wet, low-temperature heat to smoke clogging near dry after, cooling, adds water-soluble solution and is diluted to 100 milliliters;
2. low-temperature heat, to boiling, under agitation at the uniform velocity drips the sulfuric acid solution of 10 mL20%, builds beaker again, leaves standstill 3h or placement is spent the night at warm place; With quantitative filter paper filtration at a slow speed, precipitation hot wash is no acidic only to filtrate; Precipitation is placed in calcination in the porcelain crucible of constant weight with filter paper, dry ashing, and in 800 DEG C ± 5 DEG C calcinations to constant weight in high temperature Muffle furnace, calcination postprecipitation quality is m
1gram, the percentage composition of barium fluoride is calculated according to following formula:
In formula: m1 is calcination postprecipitation quality, g;
M is sample quality, g;
0.7514 is the coefficient that barium sulphate changes barium fluoride.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116411172A (en) * | 2022-11-18 | 2023-07-11 | 湖南理工学院 | Preparation method for recycling nano platinum from waste membrane electrode |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5877027A (en) * | 1996-03-18 | 1999-03-02 | Shin-Etsu Quartz Products Co., Ltd. | Method for the analysis of impurity contents in silicon dioxide |
| CN1687744A (en) * | 2005-05-18 | 2005-10-26 | 中国铝业股份有限公司 | Method for measuring alumina in aluminium fluoride |
| CN102336427A (en) * | 2011-09-07 | 2012-02-01 | 四川明晶光电科技有限公司 | Method for preparing electronic grade fine-crystalline barium fluoride |
| CN104142283A (en) * | 2014-08-04 | 2014-11-12 | 攀枝花学院 | Method for measuring barium titanate content |
-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5877027A (en) * | 1996-03-18 | 1999-03-02 | Shin-Etsu Quartz Products Co., Ltd. | Method for the analysis of impurity contents in silicon dioxide |
| CN1687744A (en) * | 2005-05-18 | 2005-10-26 | 中国铝业股份有限公司 | Method for measuring alumina in aluminium fluoride |
| CN102336427A (en) * | 2011-09-07 | 2012-02-01 | 四川明晶光电科技有限公司 | Method for preparing electronic grade fine-crystalline barium fluoride |
| CN104142283A (en) * | 2014-08-04 | 2014-11-12 | 攀枝花学院 | Method for measuring barium titanate content |
Non-Patent Citations (4)
| Title |
|---|
| 刘海霞,李震: "氟化钡中氟、钡测定方法探讨", 《无机盐工业》 * |
| 吴继尧: "高氯酸扩散_电位法测定氟化物", 《新疆医学院学报》 * |
| 李严吉: "钡盐生产工艺和应用开发近况", 《现代化工》 * |
| 梁树权: "高氯酸在分析化学中的应用", 《化学通报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116411172A (en) * | 2022-11-18 | 2023-07-11 | 湖南理工学院 | Preparation method for recycling nano platinum from waste membrane electrode |
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Application publication date: 20150819 |