CN106092921A - The detection method of hexavalent chromium content in a kind of passivating solution - Google Patents
The detection method of hexavalent chromium content in a kind of passivating solution Download PDFInfo
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- CN106092921A CN106092921A CN201610374713.3A CN201610374713A CN106092921A CN 106092921 A CN106092921 A CN 106092921A CN 201610374713 A CN201610374713 A CN 201610374713A CN 106092921 A CN106092921 A CN 106092921A
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- G—PHYSICS
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- 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
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- 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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Abstract
The invention discloses the detection method of hexavalent chromium content in a kind of passivating solution, comprise the following steps: (1) accurately measures passivating solution sample, in sample, add chelating agent and buffer solution, stirring reaction 10min～30min；(2) after reacting, solution imports separatory funnel, adds organic solvent extraction, isolates aqueous phase and organic facies, and the aqueous phase that will finally obtain is collected；(3) in aqueous phase, add acid solution, regulate pH to 1.5～2.5；(4) diphenylcarbazide acetone soln is added, colour developing, constant volume；(5) absorbance 540nm at, calculating sample Cr after ultraviolet-uisible spectrophotometer measures sample colour developing constant volume6+Content.The present invention uses 5 Br PADAP chelating agent and sodium carbonate sodium bicarbonate buffer solution that pH is 9, can separate various interfering ion, and interference colour is also removed simultaneously, can Accurate Determining hexavalent chromium content.
Description
Technical field
The present invention relates to metal ion inspection technical field, be specifically related to hexavalent chromium content in a kind of passivating solution
Detection method.
Background technology
On the one hand the development rapidly of new electronic technology allows product constantly update and regenerates, as only in more than 10 years
CPU by 386 Duo multinuclears up till now, dominant frequency by 386 8MHz to Duo i5 (four core) monokaryon 2.8GHz, similar one or two years
Just updating once: on the other hand, while enjoying technological progress, people are forced to the electronic waste in the face of pile up like a mountain
Thing, the environmental problem of electron wastes is also increasingly paid attention to.The process of electric garbage is substantially with landfill by various countries
Be main, the harmful substance such as Pb in these electron wastes, Cd, Hg etc. enter in water, soil and air, to human environment and from
So ecology causes greatly pollution.To this end, first European Union has made RoHS instruction on February 13rd, 2003, include China therewith,
The U.S. with Japan etc. state all formulated similar instruction, with the formal compulsion certification of decree, have to limit in electronic and electrical equipment
The use of pest matter.In RoHS instructs, Cr6+It is required to must not exceed 0.1wt%.
Cr6+Detection have different standards, such as IEC 62321:2008, SJ/T11365-2006, ISO 3613, EPA-
3060A and D1N53314 etc..These methods are all the spectrophotometrics using diphenylcarbazide chromogenic reaction in acid condition
Method.Its principle is the c utilizing and having strong oxidizing property in acid condition, and diphenylcarbazide redox reaction, Cr6+Reduction
Become Cr3+Oxidation product complexation with diphenylcarbazide forms mauve complex afterwards, can accurate quantification Cr by colorimetry6 +Concentration.Due to test is the single valence of Cr, and the operating procedure in test process will such as can cause variation of valence
Result accuracy is made to be affected, additionally since be to use colorimetry, if coloured word in solution, it will to test process
Produce the biggest interference.
For Cr6+Test for, electroplate liquid and passivating solution are class particular sample.As a example by passivating solution, it is by main one-tenth
Membrane (trivalent chromic ion), stabilizer (chelating agent has oxalic acid, citric acid and fluorion etc.), oxidant (nitrate anion etc.), and its
His ion (the regulation corrosion resistance of passivating film, wearability and the color of passivating film), color is the deepest.Such a to be detected contains
A large amount of Cr3+Sample in Cr6+, the operating procedure during its detection easily affects the accuracy of result, additionally since its face
Color is very deep, and its contrast color method interference is the biggest.The Cr of this kind of sample6+Test because above reason be difficult to obtain can be with the knot of confidence
Really, the relevant authentication of this series products is also hindered by this result.
Summary of the invention
For the deficiencies in the prior art, the present invention provides the detection method of hexavalent chromium content in a kind of passivating solution, accurate
Exactness is high, favorable reproducibility.
The technical solution used in the present invention is as follows:
The detection method of hexavalent chromium content in a kind of passivating solution, comprises the following steps:
(1) accurately measure passivating solution sample, in sample, add chelating agent and buffer solution, stirring reaction 10min～30min；
(2) after reacting, solution imports separatory funnel, adds organic solvent extraction, isolates aqueous phase and organic facies, collects aqueous phase；
(3) with acid regulation aqueous phase pH to 1.5～2.5；
(4) diphenylcarbazide acetone soln is added, colour developing, constant volume；
(5) absorbance 540nm at, calculating sample Cr after ultraviolet-uisible spectrophotometer measures sample colour developing constant volume6+'s
Content.
Preferably, described step (1) complexing agent is 5-Br-PADAP ethanol solution.
Preferably, in described step (1) buffer solution be pH be the soda-sodium bicarbonate solution of 9.
Preferably, described step (2) adds organic solvent extraction three times.
Preferably, in described step (2), organic solvent is chloroform.
Preferably, the described acid described in step (3) is sulphuric acid.
Beneficial effect: standard method IEC62321 and ASTM3060A for hexavalent chromium test analysis is blunt to plating
Change liquid etc. are containing a large amount of all kinds of metal ions and the difficulty of deep interference colour sample test, and selection pH is the sodium carbonate-carbonic acid of 9
Hydrogen sodium buffer solution, uses and can separate various interfering ion with 5-Br-PADAP solution before testing, simultaneously interference colour also by
Removing, the colorimetry of hexavalent chromium is the most smooth.
Detailed description of the invention
Below by specific embodiment, the present invention is further described in detail, but is not limited to this.
Embodiment 1
The detection method of hexavalent chromium content in a kind of passivating solution, comprises the following steps:
(1) accurately measuring 1mL sample 1, the 5-Br-PADAP ethanol solution and the 10mL pH that add 3mL 10wt% in sample 1 are
The soda-sodium bicarbonate solution of 9, stirring reaction 10min；
(2) after reacting, solution imports separatory funnel, adds 10mL chloroform every time and extracts three times, isolates aqueous phase and organic facies,
Collect aqueous phase；
(3) aqueous phase pH to 2.5 is regulated with sulphuric acid；
(4) diphenylcarbazide acetone soln is added, colour developing, constant volume 100mL；
(5) absorbance 540nm at, calculating sample Cr after ultraviolet-uisible spectrophotometer measures sample colour developing constant volume6+'s
Content.
Embodiment 2
The detection method of hexavalent chromium content in a kind of passivating solution, comprises the following steps:
(1) accurately measuring 1mL sample 2, the 5-Br-PADAP ethanol solution and the 10mL pH that add 3mL 10wt% in sample 2 are
The soda-sodium bicarbonate solution of 9, stirring reaction 30min；
(2) after reacting, solution imports separatory funnel, adds 10mL chloroform every time and extracts three times, isolates aqueous phase and organic facies,
Collect aqueous phase；
(3) aqueous phase pH to 1.5 is regulated with sulphuric acid；
(4) diphenylcarbazide acetone soln is added, colour developing, constant volume 100mL；
(5) absorbance 540nm at, calculating sample Cr after ultraviolet-uisible spectrophotometer measures sample colour developing constant volume6+'s
Content.
Embodiment 3
The detection method of hexavalent chromium content in a kind of passivating solution, comprises the following steps:
(1) accurately measuring 1mL sample 3, the 5-Br-PADAP ethanol solution and the 10mL pH that add 3mL 10wt% in sample 3 are
The soda-sodium bicarbonate solution of 9, stirring reaction 20min；
(2) after reacting, solution imports separatory funnel, adds 10mL chloroform every time and extracts three times, isolates aqueous phase and organic facies,
Collect aqueous phase；
(3) aqueous phase pH to 2 is regulated with sulphuric acid；
(4) diphenylcarbazide acetone soln is added, colour developing, constant volume 100mL；
(5) absorbance 540nm at, calculating sample Cr after ultraviolet-uisible spectrophotometer measures sample colour developing constant volume6+'s
Content.
Embodiment 4
The detection method of hexavalent chromium content in a kind of passivating solution, comprises the following steps:
(1) accurately measuring 1mL sample 4, the 5-Br-PADAP ethanol solution and the 10mL pH that add 3mL 10wt% in sample 4 are
The soda-sodium bicarbonate solution of 9, stirring reaction 25min；
(2) after reacting, solution imports separatory funnel, adds 10mL chloroform every time and extracts three times, isolates aqueous phase and organic facies,
Collect aqueous phase；
(3) aqueous phase pH to 2 is regulated with sulphuric acid；
(4) diphenylcarbazide acetone soln is added, colour developing, constant volume 100mL；
(5) absorbance 540nm at, calculating sample Cr after ultraviolet-uisible spectrophotometer measures sample colour developing constant volume6+'s
Content.
Embodiment 1 in 1 to 4 four kinds of sample different containing chromium passivating liquid, according to Cr6+Standard curve equation C=0.56
× A+0.04(R2=0.9986) the middle Cr of each sample is calculated6+Concentration, wherein, C is test sample concentration, and unit is that ppm, A are
Absorbance, raw sample concentration C0=100C, result is as shown in the table:
The present invention selects with 5-Br-PADAP as metal chelating agent, and the sodium carbonate-bicarbonate buffering selecting pH to be 9 is molten
Liquid, can make 5-Br-PADAP Zn optionally and in solution2+、Fe3+、Cu2+、Cd2+、Co2+、Ni2+And Mn2+Deng metal ion
Reaction, without with Cr6+Reaction, ion of can removing all kinds of obstacles, interference colour is also removed simultaneously, can detect molten accurately
Cr in liquid6+Content.
Claims (6)
1. the detection method of hexavalent chromium content in a passivating solution, it is characterised in that comprise the following steps:
(1) accurately measure passivating solution sample, in sample, add chelating agent and buffer solution, stirring reaction 10min～30min；
(2) reactant liquor is imported separatory funnel, add organic solvent extraction, isolate aqueous phase and organic facies, collect aqueous phase；
(3) with acid regulation aqueous phase pH to 1.5～2.5；
(4) diphenylcarbazide acetone soln is added, colour developing, constant volume；
(5) absorbance 540nm at, calculating sample Cr after ultraviolet-uisible spectrophotometer measures sample colour developing constant volume6+'s
Content.
The detection method of hexavalent chromium content in passivating solution the most according to claim 1, it is characterised in that described step
Suddenly (1) complexing agent is 5-Br-PADAP ethanol solution.
The detection method of hexavalent chromium content in passivating solution the most according to claim 1, it is characterised in that described step
Suddenly in (1) buffer solution be pH be the soda-sodium bicarbonate solution of 9.
The detection method of hexavalent chromium content in passivating solution the most according to claim 1, it is characterised in that described step
Suddenly (2) add organic solvent extraction three times.
The detection method of hexavalent chromium content in passivating solution the most according to claim 1, it is characterised in that described step
Suddenly in (2), organic solvent is chloroform.
The detection method of hexavalent chromium content in passivating solution the most according to claim 1, it is characterised in that described step
Suddenly the acid described in (3) is sulphuric acid.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107036989A (en) * | 2016-10-18 | 2017-08-11 | 四川大学 | A kind of method for determining chrome tanning agent active constituent content |
| CN108572235A (en) * | 2017-03-08 | 2018-09-25 | 上海梅山钢铁股份有限公司 | A kind of detection method of chromium passivating chromium from waste chromium content |
| CN110118869A (en) * | 2019-05-31 | 2019-08-13 | 安徽海螺建材设计研究院有限责任公司 | The test method of water soluble hexavalent chromium in a kind of cement or clinker |
| CN110632271A (en) * | 2019-10-17 | 2019-12-31 | 绍兴市三合检测技术有限公司 | Method for detecting heavy metal in soil |
| CN110658319A (en) * | 2019-10-17 | 2020-01-07 | 绍兴市三合检测技术有限公司 | Method for detecting heavy metals in water |
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| CN102721660A (en) * | 2011-09-02 | 2012-10-10 | 仲恺农业工程学院 | Novel determination method of Cr<6+> in electroplating passivation solution complex samples |
| CN103018183A (en) * | 2011-09-22 | 2013-04-03 | 江苏天瑞仪器股份有限公司 | Kit and method used for monitoring hexavalent chromium online |
| CN103822883A (en) * | 2012-12-25 | 2014-05-28 | 无锡点创科技有限公司 | Method for detecting total chromium in water |
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2016
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107036989A (en) * | 2016-10-18 | 2017-08-11 | 四川大学 | A kind of method for determining chrome tanning agent active constituent content |
| CN107036989B (en) * | 2016-10-18 | 2019-08-06 | 四川大学 | A method of measurement chrome tanning agent active constituent content |
| CN108572235A (en) * | 2017-03-08 | 2018-09-25 | 上海梅山钢铁股份有限公司 | A kind of detection method of chromium passivating chromium from waste chromium content |
| CN108572235B (en) * | 2017-03-08 | 2020-10-23 | 上海梅山钢铁股份有限公司 | Method for detecting chromium content in chromium passivation waste liquid |
| CN110118869A (en) * | 2019-05-31 | 2019-08-13 | 安徽海螺建材设计研究院有限责任公司 | The test method of water soluble hexavalent chromium in a kind of cement or clinker |
| CN110632271A (en) * | 2019-10-17 | 2019-12-31 | 绍兴市三合检测技术有限公司 | Method for detecting heavy metal in soil |
| CN110658319A (en) * | 2019-10-17 | 2020-01-07 | 绍兴市三合检测技术有限公司 | Method for detecting heavy metals in water |
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