CN109030475A - The quantitative analysis method of trivalent chromium in a kind of passivating solution - Google Patents
The quantitative analysis method of trivalent chromium in a kind of passivating solution Download PDFInfo
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- CN109030475A CN109030475A CN201810618978.2A CN201810618978A CN109030475A CN 109030475 A CN109030475 A CN 109030475A CN 201810618978 A CN201810618978 A CN 201810618978A CN 109030475 A CN109030475 A CN 109030475A
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Abstract
The invention discloses a kind of quantitative analysis methods of trivalent chromium in passivating solution, it is respectively placed in conical flask the following steps are included: accurately pipetting two parts of prepare liquids, portion, which is added dilute sulfuric acid, ammonium persulfate aqueous solution and silver nitrate aqueous solution and heats, to be boiled to obtain sample to be tested one, another plus dilute sulfuric acid obtain sample to be tested two；It by resulting two parts of sample to be tested constant volumes and shakes up, measures the content of 6-valence Cr ions of two parts of samples to be tested respectively using oxidimetry, the content of 6-valence Cr ions that the content of 6-valence Cr ions of sample to be tested one subtracts sample to be tested two obtains the trivalent chromium content in prepare liquid.This method as replacement or can add generation influence to passivation effect of the foundation of passivating solution to reduce low price chromium with the content of trivalent chromium in Accurate Determining passivating solution；This method is not needed using analysis instrument, low in cost, and analysis speed is fast.
Description
Technical field
The present invention relates to elemental chromium determination techniques fields, it particularly relates to a kind of quantitative analysis method of trivalent chromium.
Background technique
The surface treatment procedure of copper foil is related to anti-oxidation processing, so that copper foil surface is generated one layer of passivating film, to guarantee copper
Oxidation does not occur in prolonged placement process and properties of product is caused to decline for foil.Currently, anti-oxidation processing work used in industry
Sequence is mostly sexavalence chromium passivating.This passivation technology can make copper foil surface form fine and close oxidation film, completely cut off empty gas and water to copper foil
The excellent of corrosion can meet the anti-oxidation purpose of copper foil well.
Passivating solution effective component is Cr VI, and Cr VI carries out lower continuous consumption, corresponding passivation effect in anti-oxidation technique
It can gradually decrease；It needs to carry out supplement replacement in time.In addition, the low price chromium ion generated in technique progress can play passivation effect
To interference, passivation layer is caused to be deteriorated, oxidation-protective effect reduces.Traditional handicraft pays close attention to influence of the high price chromium content to passivation effect,
And ignore influence of the generation to passivation effect of low price chromium.Therefore, measure passivating solution middle or low price chromium content, as replacement or
Add the foundation of passivating solution and highly important.
Summary of the invention
For above-mentioned technical problem in the related technology, the present invention proposes a kind of quantitative analysis side of trivalent chromium in passivating solution
Method can overcome the above-mentioned deficiency of the prior art.
To realize the above-mentioned technical purpose, the technical scheme of the present invention is realized as follows:
The quantitative analysis method of trivalent chromium in a kind of passivating solution, comprising the following steps:
(1) it accurately pipettes two parts of prepare liquids to be respectively placed in conical flask, a volume is V1, dilute sulfuric acid, persulfuric acid is added
Aqueous ammonium and silver nitrate aqueous solution and heat boil to obtain sample to be tested one, another volume be V2, only plus dilute sulfuric acid obtains
Sample to be tested two；
(2) it by the resulting two parts of sample to be tested constant volumes of step (1) and shakes up；
(3) content of 6-valence Cr ions that determination step (2) resulting two parts of samples to be tested are distinguished using oxidimetry, to
The content of 6-valence Cr ions that the content of 6-valence Cr ions of sample one subtracts sample to be tested two obtains the trivalent chromium content in prepare liquid.
Preferably, oxidimetry is permanganimetric method in step (3), method particularly includes: add in prepare liquid one
Entering excessive concentrations is CFeIron ammonium sulfate standard solution, addition volume be VFe1, it is C with concentrationMnPotassium permanganate standard it is molten
Drop determines remaining ferrous iron to terminal, becomes aubergine as terminal using solution colour, consumes the body of Standard Potassium Permanganate Solution
Product is VMn1；It is C that excessive concentrations are added in prepare liquid twoFeIron ammonium sulfate standard solution, addition volume be VFe2, use concentration
For CMnStandard Potassium Permanganate Solution titrate remaining ferrous iron to terminal, aubergine is become as terminal using solution colour, consumption
The volume of Standard Potassium Permanganate Solution is VMn2, the trivalent chromium concentration C that can be obtained in prepare liquid is calculated with following formula:
Preferably, oxidimetry is potassium dichromate method in step (3), method particularly includes: add in prepare liquid one
Entering excessive concentrations is CFeIron ammonium sulfate standard solution, addition volume be VFe1, using diphenylamine sulfonic acid sodium salt as indicator, use is dense
Degree is CCrPotassium bichromate standard solution titrate remaining ferrous iron to terminal, consumption potassium bichromate standard solution volume is VCr1；
It is C that excessive concentrations are added in prepare liquid twoFeIron ammonium sulfate standard solution, addition volume be VFe2, with diphenylamine sulfonic acid sodium salt
It is C with concentration for indicatorCrPotassium bichromate standard solution titrate remaining ferrous iron to terminal, consume potassium bichromate standard
Liquor capacity is VCr2；It is calculated with following formula and obtains the trivalent chromium concentration C in prepare liquid:
Preferably, V in step (1)1、V2It is 5mL.
Preferably, the concentration of dilute sulfuric acid is 10wt% in step (1), and dilute sulfuric acid additional amount is respectively 5- in two parts of prepare liquids
10mL。
Preferably, the concentration of ammonium persulfate aqueous solution is 2wt%, additional amount 5-6mL in step (1).
Preferably, the concentration of silver nitrate aqueous solution is 0.02mol/L, additional amount 0.2-1mL in step (1).
Preferably, boiling time is 1-3min in step (1).
Beneficial effects of the present invention: the quantitative analysis method of trivalent chromium can be passivated in passivating solution of the invention with Accurate Determining
The content of trivalent chromium in liquid, shadow of the generation to passivation effect as the foundation of replacement or addition passivating solution to reduce low price chromium
It rings；It does not need using expensive analysis instrument, low in cost, analysis speed is fast.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1
Take two parts of prepare liquids in conical flask, volume is 5mL, and 5.0mL concentration is added in a prepare liquid and is
The silver nitrate water that the ammonium persulfate aqueous solution and 1mL concentration that the dilute sulfuric acid of 10wt%, 5.0mL concentration are 2wt% are 0.02mol/L
Solution shakes up static 10min, then boils 3min, obtains sample to be tested one, by one constant volume of sample to be tested to 25.00mL.Another
The dilute sulfuric acid that 10.0mL concentration is 10wt% is added in a prepare liquid, by sample to be tested two, constant volume to 25.00mL.
The iron ammonium sulfate standard solution that excessive concentrations are 0.2mol/L, volume 20mL are added in sample to be tested one.
Remaining ferrous iron is titrated to terminal with the Standard Potassium Permanganate Solution that concentration is 0.05mol/L, and titration end-point solution colour becomes
For aubergine, consumption Standard Potassium Permanganate Solution volume is 10.60mL.
It is the iron ammonium sulfate standard solution of 0.2mol/L (with sample to be tested one that excessive concentrations are added in sample to be tested two
The solution used is identical), volume 20mL.Remaining divalent is titrated with the Standard Potassium Permanganate Solution that concentration is 0.05mol/L
To terminal, titration end-point solution colour becomes aubergine to iron, and consumption Standard Potassium Permanganate Solution volume is 12.70mL.
Trivalent chromium concentration C in prepare liquid are as follows: (0.035mol/L)
Embodiment 2
Take two parts of prepare liquids in conical flask, volume is 5mL, and 5.0mL concentration is added in a prepare liquid and is
The silver nitrate water that the ammonium persulfate aqueous solution and 0.2mL concentration that the dilute sulfuric acid of 10wt%, 6mL concentration are 2wt% are 0.02mol/L
Solution shakes up reaction 10min, then boils 1min, obtain sample to be tested one, by one constant volume of sample to be tested to 25.00mL.Another
The dilute sulfuric acid that 10.0mL concentration is 10wt% is added in a prepare liquid, sample to be tested two is shaken up, constant volume to 25.00mL.
The iron ammonium sulfate standard solution that excessive concentrations are 0.2mol/L, volume 20mL are added in sample to be tested one.
Using diphenylamine sulfonic acid sodium salt as indicator, remaining ferrous iron is titrated extremely with the potassium bichromate standard solution that concentration is 0.05mol/L
Terminal, consumption potassium bichromate standard solution volume are 8.85mL.
It is the iron ammonium sulfate standard solution of 0.2mol/L (with sample to be tested one that excessive concentrations are added in sample to be tested two
The solution used is identical), volume 20mL.Using diphenylamine sulfonic acid sodium salt as indicator, the potassium bichromate for being 0.05mol/L with concentration
Standard solution titrates remaining ferrous iron to terminal, and consumption potassium bichromate standard solution volume is 10.60mL.
Trivalent chromium concentration C in prepare liquid are as follows:
In conclusion by means of above-mentioned technical proposal of the invention, can with the content of trivalent chromium in Accurate Determining passivating solution,
As the foundation for replacing or adding passivating solution, influence of the generation of low price chromium to passivation effect is reduced；Quantitative analysis of the invention
Method is not needed using analysis instrument, low in cost, and analysis speed is fast.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. the quantitative analysis method of trivalent chromium in a kind of passivating solution, which comprises the following steps:
(1) it accurately pipettes two parts of prepare liquids to be respectively placed in conical flask, a volume is V1, it is water-soluble that dilute sulfuric acid, ammonium persulfate is added
Liquid and silver nitrate aqueous solution and heat boil to obtain sample to be tested one, another volume be V2, only plus dilute sulfuric acid is obtained to test sample
Product two；
(2) it by the resulting two parts of sample to be tested constant volumes of step (1) and shakes up；
(3) using the content of 6-valence Cr ions of oxidimetry difference determination step (2) resulting two parts of samples to be tested, to test sample
The content of 6-valence Cr ions that the content of 6-valence Cr ions of product one subtracts sample to be tested two obtains the trivalent chromium content in prepare liquid.
2. the quantitative analysis method of trivalent chromium in passivating solution according to claim 1, which is characterized in that step (3) is described
Oxidimetry is permanganimetric method: it is C that excessive concentrations are added in prepare liquid oneFeIron ammonium sulfate standard solution,
Addition volume is VFe1, it is C with concentrationMnStandard Potassium Permanganate Solution titrate remaining ferrous iron to terminal, become with solution colour
It is terminal for aubergine, the volume for consuming Standard Potassium Permanganate Solution is VMn1；It is C that excessive concentrations are added in prepare liquid twoFe's
Iron ammonium sulfate standard solution, addition volume are VFe2, it is C with concentrationMnStandard Potassium Permanganate Solution titrate remaining ferrous iron
To terminal, aubergine is become as terminal using solution colour, the volume for consuming Standard Potassium Permanganate Solution is VMn2, use following formula
Calculate the trivalent chromium concentration C that can be obtained in prepare liquid:
。
3. the quantitative analysis method of trivalent chromium in passivating solution according to claim 1, which is characterized in that step (3) is described
Oxidimetry is potassium dichromate method: it is C that excessive concentrations are added in prepare liquid oneFeIron ammonium sulfate standard solution,
Addition volume is VFe1, it is C with concentration using diphenylamine sulfonic acid sodium salt as indicatorCrPotassium bichromate standard solution titration remaining two
To terminal, consumption potassium bichromate standard solution volume is V to valence ironCr1；It is C that excessive concentrations are added in prepare liquid twoFeSulfuric acid it is sub-
Iron ammonium standard solution, addition volume are VFe2, it is C with concentration using diphenylamine sulfonic acid sodium salt as indicatorCrPotassium bichromate standard it is molten
Drop determines remaining ferrous iron to terminal, and consumption potassium bichromate standard solution volume is VCr2；With following formula calculate i.e. obtain to
Survey the trivalent chromium concentration C in liquid:
。
4. the quantitative analysis method of trivalent chromium in passivating solution according to claim 1, which is characterized in that step (1) is described
V1、V2It is 5mL.
5. the quantitative analysis method of trivalent chromium in passivating solution according to claim 1, which is characterized in that step (1) is described
The concentration of dilute sulfuric acid is 10wt%, and dilute sulfuric acid additional amount is respectively 5-10mL in two parts of prepare liquids.
6. the quantitative analysis method of trivalent chromium in passivating solution according to claim 1, which is characterized in that step (1) is described
The concentration of ammonium persulfate aqueous solution is 2wt%, additional amount 5-6mL.
7. the quantitative analysis method of trivalent chromium in passivating solution according to claim 1, which is characterized in that step (1) is described
The concentration of silver nitrate aqueous solution is 0.02mol/L, additional amount 0.2-1mL.
8. the quantitative analysis method of trivalent chromium in passivating solution according to claim 1, which is characterized in that step (1) is described
Boiling time is 1-3min.
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Cited By (3)
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| CN115613018A (en) * | 2022-09-26 | 2023-01-17 | 深圳惠科新材料有限公司 | Copper foil anti-oxidation treatment system and treatment method |
| JP2023034779A (en) * | 2021-08-31 | 2023-03-13 | 三菱重工業株式会社 | Sample analyzer and sample analysis method |
| CN116203189A (en) * | 2023-02-23 | 2023-06-02 | 武汉钢铁有限公司 | Method for measuring chromic acid point in galvanized passivation solution by using automatic potentiometric titrator |
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| CN116203189A (en) * | 2023-02-23 | 2023-06-02 | 武汉钢铁有限公司 | Method for measuring chromic acid point in galvanized passivation solution by using automatic potentiometric titrator |
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Application publication date: 20181218 |