CN101397145A - Method for preparing primary standard reagent sodium chloride - Google Patents
Method for preparing primary standard reagent sodium chloride Download PDFInfo
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- CN101397145A CN101397145A CNA2007100612879A CN200710061287A CN101397145A CN 101397145 A CN101397145 A CN 101397145A CN A2007100612879 A CNA2007100612879 A CN A2007100612879A CN 200710061287 A CN200710061287 A CN 200710061287A CN 101397145 A CN101397145 A CN 101397145A
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- Prior art keywords
- filtration
- sodium chloride
- standard reagent
- filtration solution
- primary standard
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for preparing standard reagent of sodium chloride, comprising the steps as follows: (1) industrial salt is dissolved in deioned water and filtrated statically; (2) the filtration solution is acidified by hydrochloric acid; chlorizated salt is added in the filtration solution to remove sulfate; the filtration solution is filtrated statically; (3) the pH value of the filtration solution is adjusted by sodium hydroxide and is adjusted subsequently by adding sodium carbonate; sodium polyacrylate is added in the filtration solution; the filtration solution is filtrated statically; (4) hydrogen peroxide is added in the filtration solution which is statically filtrated; (5) the filtration solution is counteracted by hydrochloric acid; the filtration solution is evaporated, crystallized, dried by throwing method and dried in vacuum so as to form the standard reagent of sodium chloride product. The metal carbonates separated out are provided with positive charges which exclude each other and obstacle agglomeration and settlement; furthermore, the sodium polyacrylate with negative charges can be combined with the metal ion deposition with the positive charges, thus leading the metal ion to be agglomerated and settled rapidly and leading the clarity to achieve the best effect by the filtration.
Description
Technical field
The invention belongs to the chemical reagent field, especially a kind of preparation method of primary standard reagent sodium chloride.
Background technology
Primary standard reagent sodium chloride transmits as the amount matter of the chemical analytical standard solution of all trades and professions, and it is chemical analytical standard solution " ruler ", is requisite operating variable standard substance in the analyzing and testing.Sodium-chlor as standard reagent is preparation so at present: in industrial crude salt, at first add yellow soda ash, and then hydro-oxidation sodium, its objective is and remove contained metal ion in the crude salt.Because solution is to be tart, H
++ CO
3 2+→ CO
2↑+H
2O, its CO
3 2+Root has all run, and GOLD FROM PLATING SOLUTION belongs to ion can not form carbonate deposition, and metal ion removes not fall, and has greatly influenced the clarity of sodium-chlor; And clarity is defective, has also influenced the standard of operating variable standard substance in the analyzing and testing.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, the preparation method of the higher primary standard reagent sodium chloride of a kind of clarity is provided.
The technical scheme that the present invention takes is:
A kind of preparation method of primary standard reagent sodium chloride, the step of its preparation method is:
(1). industrial crude salt is dissolved in the deionized water static 0.5～1.5 hour after-filtration;
(2). filtrate is used hcl acidifying, add barium salt and remove sulfate radical, static 1～3 hour after-filtration;
(3). filtrate is transferred Ph9～11 with sodium hydroxide solution, add yellow soda ash again and will transfer Ph to 12～13, add sodium polyacrylate again, static 1～3 hour after-filtration;
(4). in filtrate, add hydrogen peroxide ferrous ion be oxidized to high ferro and be precipitated out, static 0.5～1.5 hour after-filtration by hydrolysis reaction;
(5). transferring the Ph of filtrate with hydrochloric acid is 3～5, and this filtrate by evaporation, crystallization, drying, vacuum-drying, is promptly obtained the primary standard reagent sodium chloride finished product.
And, described be dissolved in industrial crude salt in the deionized water after, need to adopt ammonium sulfide to remove beavy metal impurity contained in the industrial crude salt.
And described barium salt is a bariumchloride.
And described industrial crude salt is 375:1 with the weight ratio of the sodium polyacrylate that is added.
Advantage of the present invention and positively effect are:
The carbonic acid metal salt that preparation method of the present invention separated out all has positive charge, mutually exclusive and hinder agglomerate and sink, and adopt sodium polyacrylate electronegative, can combine with positively charged precipitation by metallic ion thing, thereby can make the rapid agglomerate and sink of metal ion, through filtering, can make clarity reach best effect again.
Embodiment
Below in conjunction with embodiment technology contents of the present invention is described further; Following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
The preparation method of this primary standard reagent sodium chloride, the step of its preparation method is:
(1). 75 kilograms of industrial crude salt are dissolved in 200 kilograms of deionized waters, add the 100g ammonium sulfide and remove beavy metal impurity, as Pb, Cu etc., chemical equation is as follows:
Pb
2++S
2-→PbS↓ Cu
2++S
2-→CuS↓
Static 1 hour after-filtration.
(2). is 4 with filtrate with hcl acidifying Ph, adds the 500g bariumchloride and removes sulfate radical, and chemical equation is as follows:
Ba
2++SO
4 2-→BaSO
4↓
Static 2 hours after-filtration.
(3). filtrate is transferred Ph to 10 with sodium hydroxide solution, add yellow soda ash again and will transfer Ph to 12, add sodium polyacrylate 200g again.
Static 2 hours after-filtration.
(4). add the 100ml hydrogen peroxide again in filtrate ferrous ion is oxidized to high ferro, promptly hydrolysis reaction takes place and be precipitated out, chemical equation is as follows:
Fe
3++3H
2O→Fe(OH)
3↓+3H
+
Static 1 hour after-filtration;
(5). making Ph with the hydrochloric acid neutralization solution is 4, evaporating solns then, crystallization is separated out, and dries, and vacuum-drying promptly gets 30 kilograms of primary standard reagent sodium chloride finished products.
Claims (4)
1. the preparation method of a primary standard reagent sodium chloride is characterized in that:
The step of its preparation method is:
(1). industrial crude salt is dissolved in the deionized water static 0.5～1.5 hour after-filtration;
(2). filtrate is used hcl acidifying, add barium salt and remove sulfate radical, static 1～3 hour after-filtration;
(3). filtrate is transferred Ph9～11 with sodium hydroxide solution, add yellow soda ash again and will transfer Ph to 12～13, add sodium polyacrylate again, static 1～3 hour after-filtration;
(4). in filtrate, add hydrogen peroxide ferrous ion be oxidized to high ferro and be precipitated out, static 0.5～1.5 hour after-filtration by hydrolysis reaction;
(5). transferring the Ph of filtrate with hydrochloric acid is 3～5, and this filtrate by evaporation, crystallization, drying, vacuum-drying, is promptly obtained the primary standard reagent sodium chloride finished product.
2. the preparation method of primary standard reagent sodium chloride according to claim 1 is characterized in that: described be dissolved in industrial crude salt in the deionized water after, need to adopt ammonium sulfide to remove beavy metal impurity contained in the industrial crude salt.
3. the preparation method of primary standard reagent sodium chloride according to claim 1, it is characterized in that: described barium salt is a bariumchloride.
4. the preparation method of primary standard reagent sodium chloride according to claim 1 is characterized in that: described industrial crude salt is 375:1 with the weight ratio of the sodium polyacrylate that is added.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100612879A CN101397145A (en) | 2007-09-28 | 2007-09-28 | Method for preparing primary standard reagent sodium chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100612879A CN101397145A (en) | 2007-09-28 | 2007-09-28 | Method for preparing primary standard reagent sodium chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101397145A true CN101397145A (en) | 2009-04-01 |
Family
ID=40516018
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007100612879A Pending CN101397145A (en) | 2007-09-28 | 2007-09-28 | Method for preparing primary standard reagent sodium chloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101397145A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275954A (en) * | 2011-06-28 | 2011-12-14 | 广东广试试剂科技有限公司 | Method for purifying potassium iodide and use thereof |
| CN108423692A (en) * | 2018-03-22 | 2018-08-21 | 安徽泰格生物技术股份有限公司 | With the method for production of vitamin C abraum salt purification sodium chloride |
-
2007
- 2007-09-28 CN CNA2007100612879A patent/CN101397145A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275954A (en) * | 2011-06-28 | 2011-12-14 | 广东广试试剂科技有限公司 | Method for purifying potassium iodide and use thereof |
| CN108423692A (en) * | 2018-03-22 | 2018-08-21 | 安徽泰格生物技术股份有限公司 | With the method for production of vitamin C abraum salt purification sodium chloride |
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Legal Events
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090401 |