CN107132222A - The assay method of zinc oxide content in metaphosphoric acid zinc - Google Patents
The assay method of zinc oxide content in metaphosphoric acid zinc Download PDFInfo
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- CN107132222A CN107132222A CN201710515573.1A CN201710515573A CN107132222A CN 107132222 A CN107132222 A CN 107132222A CN 201710515573 A CN201710515573 A CN 201710515573A CN 107132222 A CN107132222 A CN 107132222A
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- oxide content
- metaphosphoric acid
- zinc oxide
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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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
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Abstract
The invention belongs to chemical analysis test field, and in particular to the assay method of optical glass zinc oxide content in raw material metaphosphoric acid zinc.The technical problems to be solved by the invention are to provide a kind of assay method of zinc oxide content in metaphosphoric acid zinc, comprise the following steps：Metaphosphoric acid zinc is decomposed, using xylenol orange solution as indicator, regulation pH is 5~6, and titration end-point is titrated to disodium ethylene diamine tetraacetate standard liquid.This method has the advantages that simple to operate, accuracy is high.
Description
Technical field
The invention belongs to chemical analysis test field, and in particular to optical glass zinc oxide content in raw material metaphosphoric acid zinc
Assay method.
Background technology
Metaphosphoric acid zinc Zn (PO3)2, it is that vitreousness powder is slightly soluble in water, is mainly used in special optical glass and special type protection
Addition in glass and radiation resistant glass material, phosphate glass, fluorphosphate glass, laser glass, can make in glass
Setting rate is slack-off when glass is molded, and reduces the tendency towards devitrification of glass, improves the chemical stability and mechanical strength of glass.In phosphorus
Introduction volume is 5~20% in hydrochlorate and fluorphosphate glass system.
All it is difficult to inquire related data in the current data of metaphosphoric acid zinc, also without associated test standards.The titration of zinc is current
Tradition is given instruction agent using eriochrome black T, and Zn content is obtained with disodium ethylene diamine tetraacetate titration.But in metaphosphate system
During middle use this method, the discoloration of indicator terminal can be caused unobvious, it is impossible to judge titration end-point and cause result error very
Greatly.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of assay method of zinc oxide content in metaphosphoric acid zinc.The survey
The method of determining comprises the following steps：Metaphosphoric acid zinc is decomposed, using xylenol orange solution as indicator, regulation pH value of solution is 5~6, uses second
Edetate disodium standard liquid volumetric soiutions pass through the disodium ethylene diamine tetraacetate standard liquid of consumption to titration end-point
Amount, which is calculated, can obtain zinc oxide content.
Specifically, said determination method, comprises the following steps：Concentrated hydrochloric acid is added in testing sample metaphosphoric acid zinc, is heated
It is completely dissolved sample；After sample cooling, add water, plus xylenol orange indicator, solution is adjusted to aubergine with ammoniacal liquor, then use salt
Solution is adjusted to yellow by acid, and it is 5~6 to add hexamethylenetetramine cushioning liquid adjustment system pH；Ethylenediamine tetra-acetic acid two is used again
Sodium standard solution is titrated to titration end-point, is calculated by the amount of the disodium ethylene diamine tetraacetate standard liquid of consumption and can obtain oxygen
Change Zn content.
It is preferred that, in said determination method, the testing sample metaphosphoric acid zinc is in 105~110 DEG C of drying to constant weight.
It is preferred that, in said determination method, the xylenol orange concentration of indicator is 2~5g/L.Weigh 0.2~0.5g
Xylenol orange, is dissolved in water, is diluted to 100mL.
It is preferred that, in said determination method, the mass concentration of the concentrated hydrochloric acid is 36~38%.
It is preferred that, in said determination method, the hexamethylenetetramine cushioning liquid pH is 5.5~6.0.Weigh 200g six
Methine tetramine is dissolved in 1000mL water, and addition mass concentration is 38% hydrochloric acid, is adjusted to pH5.5~6.0.
It is preferred that, in said determination method, the concentration of the disodium ethylene diamine tetraacetate standard liquid for 0.02~
0.05mol/L。
It is preferred that, in said determination method, the ammoniacal liquor is the aqueous solution and 1 of 1 volume mass concentration containing ammonia 25~28%
~3 volume of water mixed preparings are formed.
It is preferred that, in said determination method, the hydrochloric acid is that 1 volume concentrated hydrochloric acid is formed with 1~3 volume of water mixed preparing,
The mass concentration of the concentrated hydrochloric acid is 36~38%.
The inventive method solves the problems, such as zinc oxide content Accurate Determining in optical glass raw material metaphosphoric acid zinc, experiment knot
Fruit shows that accurately and reliably, favorable reproducibility, precision is high, is conducive to utilization and extention for this method.
Embodiment
Due to there is phosphate anion in solution to be measured of the invention, when using eriochrome black T as indicator, terminal can be produced
Raw interference, causes without obvious color change, so that terminal can not be determined, it is impossible to accurately test Zn content.Being found through inventor can
Using xylenol orange as indicator, xylenol orange indicator can only be used in an acidic solution, as pH ＞ 6.3 in purplish red
Color, pH ＜ 6.3 are in yellow, so pH value of solution must be made to be 5~6, then to ensure Acidity Range, must add hexamethylenetetramine
Cushioning liquid, to ensure that disodium ethylene diamine tetraacetate accurately titrates zinc ion, improves test accuracy.So, to ensure solution
PH in OK range, solution is first adjusted to lucky aubergine with ammoniacal liquor, solution is then adjusted to lucky yellow with hydrochloric acid again.
The assay method of zinc oxide content, comprises the following steps in metaphosphoric acid zinc：
1) the sample metaphosphoric acid zinc of 0.1g~0.30g dryings is weighed in conical flask, adds 3~5mL concentrated hydrochloric acids, plus it is few
Ultrapure water is measured, sample dissolving is heated to completely, is now transparent colourless solution；
2) after sample cooling, plus ultra-pure water, the drop xylenol orange solution of 2 drop~3, now solution presentation yellow；Ammonia is used again
Solution is adjusted to aubergine by water, and solution then is adjusted into yellow with watery hydrochloric acid, is in after adding 5mL hexamethylenetetramine cushioning liquid
Existing aubergine；
3) it is terminal to be titrated to color with disodium ethylene diamine tetraacetate standard liquid to be changed into yellow from aubergine；
4) result is calculated：
In formula：V --- the numerical value of disodium ethylene diamine tetraacetate standard titration solution volume, unit is milliliter (mL)；
C --- the exact value of disodium ethylene diamine tetraacetate standard titration solution concentration, unit is mole every liter of (mol/
L)；
The numerical value of m --- sample quality, unit is gram (g)；
M --- the numerical value of zinc oxide molal weight, unit is gram every mole (g/mol).
Embodiment 1
1) samples of the 0.15g (being accurate to 0.0001g) through 105 DEG C of drying is weighed in conical flask, adds 5mL hydrochloric acid molten
It is complete that sample dissolving is heated on liquid, plus a small amount of ultrapure water, electric furnace；
2) after sample cooling, plus 50mL ultra-pure waters, the drop xylenol orange solution of 2 drop~3, solution is adjusted to ammoniacal liquor purplish red
Color, then yellow is adjusted to hydrochloric acid, add 5mL hexamethylenetetramine cushioning liquid.
3) it is eventually to be titrated to color with 0.02mol/L disodium ethylene diamine tetraacetate standard liquids to be changed into yellow from aubergine
Point；
4) result is calculated.
Using the inventive method to same sample retest 6 times, its result such as table 1 below：
Table 1
| 1 | 2 | 3 | 4 | 5 | 6 | |
| ZnO (%) | 36.23 | 36.22 | 36.30 | 36.25 | 36.31 | 36.27 |
As can be seen from Table 1, standard deviation=0.036, the ＜ 2% of relative standard deviation=0.10%.
Embodiment 2
1) samples of the 0.30g (being accurate to 0.0001g) through 105 DEG C of drying is weighed in conical flask, adds 5mL hydrochloric acid molten
It is complete that sample dissolving is heated on liquid, plus a small amount of ultrapure water, electric furnace；
2) after sample cooling, plus 50mL ultra-pure waters, the drop xylenol orange solution of 2 drop~3, solution is adjusted to ammoniacal liquor purplish red
Color, then yellow is adjusted to hydrochloric acid, add 5mL hexamethylenetetramine cushioning liquid.
3) it is eventually to be titrated to color with 0.05mol/L disodium ethylene diamine tetraacetate standard liquids to be changed into yellow from aubergine
Point；
4) result is calculated.
Using the inventive method to same sample retest 6 times, its result such as table 2 below：
Table 2
| 1 | 2 | 3 | 4 | 5 | 6 | |
| ZnO (%) | 36.37 | 36.32 | 36.22 | 36.28 | 36.29 | 36.3 |
As can be seen from Table 2, standard deviation=0.049, the ＜ 2% of relative standard deviation=0.14%.
It in summary it can be seen that the inventive method precision is good, accuracy is high, method is feasible, suitable for promoting.
Claims (9)
1. the assay method of zinc oxide content in metaphosphoric acid zinc, it is characterised in that：Comprise the following steps：Metaphosphoric acid zinc is decomposed, with
Xylenol orange solution is indicator, and regulation pH value of solution is 5~6, with disodium ethylene diamine tetraacetate standard liquid volumetric soiutions to drop
Determine terminal, calculated by the amount of the disodium ethylene diamine tetraacetate standard liquid of consumption and can obtain zinc oxide content.
2. the assay method of zinc oxide content in metaphosphoric acid zinc according to claim 1, it is characterised in that：Including following step
Suddenly：Concentrated hydrochloric acid is added in testing sample metaphosphoric acid zinc, heating is completely dissolved sample；After sample cooling, add water, plus xylenol
Orange indicator, aubergine is adjusted to ammoniacal liquor by solution, then solution is adjusted into yellow with hydrochloric acid, adds hexamethylenetetramine buffering molten
Liquid adjustment system pH is 5~6；Pass through consumption to titration end-point with disodium ethylene diamine tetraacetate standard liquid volumetric soiutions again
The amount of disodium ethylene diamine tetraacetate standard liquid, which is calculated, can obtain zinc oxide content.
3. the assay method of zinc oxide content in metaphosphoric acid zinc according to claim 1 or 2, it is characterised in that：It is described to treat
Test sample product metaphosphoric acid zinc is in 105~110 DEG C of drying to constant weight.
4. the assay method of zinc oxide content in metaphosphoric acid zinc according to claim 1 or 2, it is characterised in that：Described two
Cresols orange concentration of indicator is 2~5g/L.
5. the assay method of zinc oxide content in metaphosphoric acid zinc according to claim 1 or 2, it is characterised in that：It is described dense
The mass concentration of hydrochloric acid is 36~38%.
6. the assay method of zinc oxide content in metaphosphoric acid zinc according to claim 1 or 2, it is characterised in that：Described six
Methine tetramine cushioning liquid pH is 5.5~6.0.
7. the assay method of zinc oxide content in metaphosphoric acid zinc according to claim 1 or 2, it is characterised in that：The second
The concentration of edetate disodium standard liquid is 0.02~0.05mol/L.
8. the assay method of zinc oxide content in metaphosphoric acid zinc according to claim 1 or 2, it is characterised in that：The ammonia
Water forms for the aqueous solution of 1 volume mass concentration containing ammonia 25~28% with 1~3 volume of water mixed preparing.
9. the assay method of zinc oxide content in metaphosphoric acid zinc according to claim 1 or 2, it is characterised in that：The salt
Acid forms for 1 volume concentrated hydrochloric acid with 1~3 volume of water mixed preparing, and the mass concentration of the concentrated hydrochloric acid is 36~38%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107656008A (en) * | 2017-09-29 | 2018-02-02 | 安徽沙丰新材料有限公司 | The assay method of calcium oxide content in a kind of calcium stearate |
| CN111579714A (en) * | 2020-06-28 | 2020-08-25 | 成都光明光电股份有限公司 | Method for measuring content of copper oxide in copper metaphosphate |
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| CN103913457A (en) * | 2012-12-31 | 2014-07-09 | 北京有色金属与稀土应用研究所 | Method for titration of zinc content in silver-copper-zinc alloy by ethylenediamine tetraacetic acid |
| CN105445414A (en) * | 2015-12-17 | 2016-03-30 | 天津神能科技有限公司 | Chemical analysis determination method of zinc content of molecular sieve |
| CN105738561A (en) * | 2016-04-21 | 2016-07-06 | 武汉理工大学 | Rapid detection method for activity of metakaolin |
| CN105891407A (en) * | 2016-04-01 | 2016-08-24 | 中国科学院青海盐湖研究所 | Method for determining content of magnesium, zinc and rare earth in alloy and application of method |
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2017
- 2017-06-29 CN CN201710515573.1A patent/CN107132222A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103913457A (en) * | 2012-12-31 | 2014-07-09 | 北京有色金属与稀土应用研究所 | Method for titration of zinc content in silver-copper-zinc alloy by ethylenediamine tetraacetic acid |
| CN105445414A (en) * | 2015-12-17 | 2016-03-30 | 天津神能科技有限公司 | Chemical analysis determination method of zinc content of molecular sieve |
| CN105891407A (en) * | 2016-04-01 | 2016-08-24 | 中国科学院青海盐湖研究所 | Method for determining content of magnesium, zinc and rare earth in alloy and application of method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107656008A (en) * | 2017-09-29 | 2018-02-02 | 安徽沙丰新材料有限公司 | The assay method of calcium oxide content in a kind of calcium stearate |
| CN111579714A (en) * | 2020-06-28 | 2020-08-25 | 成都光明光电股份有限公司 | Method for measuring content of copper oxide in copper metaphosphate |
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