CN102706875A - Method for determining chloride ions in copper-zinc-containing electrolyte sample - Google Patents
Method for determining chloride ions in copper-zinc-containing electrolyte sample Download PDFInfo
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- CN102706875A CN102706875A CN2012101730587A CN201210173058A CN102706875A CN 102706875 A CN102706875 A CN 102706875A CN 2012101730587 A CN2012101730587 A CN 2012101730587A CN 201210173058 A CN201210173058 A CN 201210173058A CN 102706875 A CN102706875 A CN 102706875A
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Abstract
A method for determining chloride ions in a copper-zinc-containing electrolyte sample comprises the following steps: taking 20-50ml of zinc electrolyte sample, adding 5ml of 50% sulfuric acid, adding 0.5-1.0 g of zinc powder with the purity of 99.999% or 0.2-0.5 g of aluminum powder with the purity of 99.999%, stirring until the reaction is finished, and fixing the volume to a 100ml volumetric flask; dry filtering, separating filtrate 20-50ml to 300ml beaker, adding 5-6ml nitric acid, adding known amount of excess silver nitrate (0.05 mol/L) until chloride ion precipitation is complete, heating and boiling to flocculate silver chloride precipitate, filtering, washing precipitate; adjusting the volume to 80ml-100ml, adding 1ml of saturated ferric sulfate solution acidified by nitric acid, and titrating by 0.01mol/L potassium thiocyanate solution until the solution is stable red, wherein the titration end point is obtained. The invention provides a method for rapidly and accurately measuring the chloride ion content in zinc electrolyte without using instruments.
Description
Technical field
The present invention relates to methods of chlorine ions in a kind of zinc electrolyte, specifically relate to a kind of method of measuring chlorion in the cupric zinc electrolyte sample.
Background technology
Chlorion is as important impurity element in the zinc electrolyte, and in the process of electrolytic zinc, the existence of chlorion can be corroded anode, therefore must remove, and Determination of chlorine ion content just seems particularly important in the zinc sulfate.At present, the Cl in China's working sample
-, adopting AAS, turbidimetry, the chromatography of ions, electrochemical methods, volumetric method etc. mostly, diverse ways has different usable range to different samples.1, AAS, 2, nephelometry, 3, the chromatography of ions, 4, atomic absorption method, 5, electrochemical analysis, 6, volumetric method etc.; Wherein preceding 5 kinds of methods can accurately be measured the concentration of chlorion; But only limit to trace or trace, chlorine ion concentration is high slightly to be no small burdens for instrument or operating personnel, mainly is argentometry for the 6th kind of volumetric method; It is judicial that argentometry can be divided into Moire technique, Fo Erhadefa and Fa Yang again; Moire technique is indicator to the reaction with silver nitrate standard solution direct titration with the chromate, measures Cl
-The maximum drawback of this method is that emphasis is difficult to judge; Fo Erhadefa is an indicator with the ferriammonium sulfate, uses SCN
-Direct titration Ag
+, FeSCN appears to solution
2+Red the time represent that emphasis arrives, perhaps in test solution, add known quantity and excessive silver nitrate standard solution, make Cl
-Or the thiocyanate ion quantitatively generates the silver salt post precipitation, adds the ferriammonium sulfate indicator again, with the remaining silver ion of thiocyanate standard solution back titration, adopts this method to measure Cl
-, its terminal colour changes fairly obvious, but strong oxidation and can be with SCN
-Oxidation, the low oxide of nitrogen and SCN
-Can form red NOSCN (sulphur cyanogen nitrosyl), possibly cause false judgment, mantoquita and mercury salt ability and SCN terminal point
-Reaction generates deposition, must eliminate.
The wherein most important interference element of determination of chloride ion is exactly a copper ion in zinc electrolyte; Volumetric determination for chlorion in the zinc electrolyte does not have effective and feasible way at present; The mensuration of the serious chlorion of influence of copper ion; The concentration of chlorion has a strong impact on the serviceable life of electrode, and the content of therefore accurately measuring chlorion in the zinc electrolyte seems particularly important.
Summary of the invention
The object of the invention is exactly deficiency and the shortcoming that will eliminate above-mentioned prior art, and the method for chloride ion content in a kind of volumetric determination zinc electrolyte is provided, and can measure chloride ion content easily and fast, accurately.
For reaching above-mentioned technique effect, the present invention adopts following technical scheme:
(1) get zinc electrolyte sample 20-50ml, add 50% sulfuric acid 5ml, adding purity is the 0.5g-1.0g of 99.999% zinc powder, and perhaps purity is 99.999% aluminium powder 0.2g-0.5g, is stirred to reaction and finishes, and is settled to the 100ml volumetric flask;
(2) do filtration, obtain in filtrating 20-50ml to the 300ml beaker, add nitric acid 5-6ml, excessive silver nitrate (0.05mol/L) to the chlorion deposition that adds known quantity is complete, and heated and boiled makes the silver nitride precipitation flocculation, filters washing precipitation;
(3) the adjustment volume adds the saturated ferrum sulfuricum oxydatum solutum 1ml of nitric acid acidifying at 80ml-100ml, and stable redness appears in potassium rhodanide solution titration to the solution of 0.01mol/L, is titration end-point.
Preferably, said step (1) moderate purity is that the addition of 99.999% zinc powder is 0.7g-1.0g, or purity is 99.999% aluminium powder 0.35g-0.5g.
Preferably, add nitric acid 5ml in the said step (2).
Beneficial effect of the present invention:
A kind of method of measuring chlorion in the cupric zinc electrolyte sample disclosed by the invention provides a kind of instrument that do not use just can fast, accurately measure Determination of chlorine ion content method in the zinc electrolyte; The present invention adopts highly purified zinc powder or aluminium powder to remove the interference metallic ion; And strict control have a try agent consumption and operation steps, can be at the scene, middle-size and small-size laboratory just can accurately measure.
Embodiment
Below in conjunction with embodiment the present invention is further described, but institute of the present invention protection domain is not limited thereto, zinc electrolyte selects for use the cupric zinc electrolyte of silver company for measuring solvent, and it is pure that sulfuric acid and nitric acid are analysis.
Embodiment 1:
1, gets cupric zinc electrolyte 20ml, add 50% sulfuric acid 5ml, add zinc powder (99.999%) 1g, be stirred to reaction and finish, be settled to the 100ml volumetric flask;
2, do filtration, obtain in filtrating 20ml to the 300ml beaker, add nitric acid (commercially available) 5ml, silver nitrate (0.05mol/L) to the chlorion deposition that adds 5ml is complete, and heated and boiled makes the silver nitride precipitation flocculation, filters washing precipitation;
3, the adjustment filtrate volume adds the saturated ferrum sulfuricum oxydatum solutum 1ml of nitric acid acidifying at 100ml, and stable redness appears in potassium rhodanide solution titration to the solution of 0.01mol/L, is titration end-point;
Table 1 adopts chlorion in the zinc determination by reduction sample
| Element | Measured value | Recovery of standard addition (%) | Standard deviation (S) |
| Cl | 3.24 | 99.2 | 0.034 |
Embodiment 2:
1, gets cupric zinc electrolyte 50ml, add 50% sulfuric acid (commercially available) 5ml, add zinc powder (99.999%) 0.5g, be stirred to reaction and finish, be settled to the 100ml volumetric flask;
2, do filtration, obtain filtrating, in 50ml to the 300ml beaker, add nitric acid (commercially available) 6ml, silver nitrate (0.05mol/L) to the chlorion that adds 2ml precipitates fully, and heated and boiled is flocculated silver nitride precipitation, filters washing precipitation;
3, the adjustment filtrate volume adds the saturated ferrum sulfuricum oxydatum solutum 1ml of nitric acid acidifying at 80ml, and stable redness appears in potassium rhodanide solution titration to the solution of 0.01mol/L, is titration end-point;
Table 2 adopts chlorion in the zinc determination by reduction sample
| Element | Measured value | Recovery of standard addition (%) | Standard deviation (S) |
| Cl | 0.080 | 100.4 | 0.0053 |
Embodiment 3:
1, gets cupric zinc electrolyte 30ml, add 50% sulfuric acid (commercially available) 5ml, add aluminium powder (99.999%) 0.2g, be stirred to reaction and finish, be settled to the 100ml volumetric flask;
2, do filtration, obtain in filtrating 20ml to the 300ml beaker, add nitric acid (commercially available) 5ml, silver nitrate (0.05mol/L) to the chlorion deposition that adds 5ml is complete, and heated and boiled makes the silver nitride precipitation flocculation, filters washing precipitation;
3, the adjustment filtrate volume adds the saturated ferrum sulfuricum oxydatum solutum 1ml of nitric acid acidifying at 90ml, and stable redness appears in potassium rhodanide solution titration to the solution of 0.01mol/L, is titration end-point;
Table 3 adopts chlorion in the aluminium reducing working sample
| Element | Measured value | Recovery of standard addition (%) | Standard deviation (S) |
| Cl | 3.27 | 99.6 | 0.030 |
Embodiment 4:
1, sample thief two 50ml, sulfuric acid (commercially available) 5ml of adding 50% adds aluminium powder (99.999%) 0.5g, is stirred to reaction and finishes, and is settled to the 100ml volumetric flask;
2, do filtration, obtain in filtrating 50ml to the 300ml beaker, add nitric acid (commercially available) 5ml, silver nitrate (0.05mol/L) to the chlorion deposition that adds 2ml is complete, and heated and boiled makes the silver nitride precipitation flocculation, filters washing precipitation;
3, the adjustment filtrate volume adds the saturated ferrum sulfuricum oxydatum solutum 1ml of nitric acid acidifying at 80ml, and stable redness appears in potassium rhodanide solution titration to the solution of 0.01mol/L, is titration end-point;
Table 4 adopts chlorion in the aluminium reducing working sample
| Element | Measured value | Recovery of standard addition (%) | Standard deviation (S) |
| Cl | 0.072 | 100.7 | 0.0052 |
Should be noted that control zinc powder dosage is when 0.7-1.0g or aluminium powder 0.35g-0.5g, titration results has better accuracy.A kind of method of measuring chlorion in the cupric zinc electrolyte sample disclosed by the invention provides a kind of instrument that do not use just can fast, accurately measure Determination of chlorine ion content method in the zinc electrolyte; The present invention adopts highly purified zinc powder or aluminium powder to remove the interference metallic ion; And strict control have a try agent consumption and operation steps, can be at the scene, middle-size and small-size laboratory just can accurately measure.
Above-described only is preferred embodiment of the present invention.Should be understood that for the person of ordinary skill of the art, under teachings provided by the present invention,, can also make other equivalent modifications and improvement, also should be regarded as protection scope of the present invention as the common practise of this area.
Claims (3)
1. method of measuring chlorion in the cupric zinc electrolyte sample, it is characterized in that: this method may further comprise the steps:
(1) get zinc electrolyte sample 20-50ml, add 50% sulfuric acid 5ml, adding purity is the 0.5g-1.0g of 99.999% zinc powder, and perhaps purity is 99.999% aluminium powder 0.2g-0.5g, is stirred to reaction and finishes, and is settled to the 100ml volumetric flask;
(2) do filtration, obtain in filtrating 20-50ml to the 300ml beaker, add nitric acid 5-6ml, excessive silver nitrate (0.05mol/L) to the chlorion deposition that adds known quantity is complete, and heated and boiled makes the silver nitride precipitation flocculation, filters washing precipitation;
(3) the adjustment volume adds the saturated ferrum sulfuricum oxydatum solutum 1ml of nitric acid acidifying at 80ml-100ml, and stable redness appears in potassium rhodanide solution titration to the solution of 0.01mol/L, is titration end-point.
2. according to the said a kind of method of measuring chlorion in the cupric zinc electrolyte sample of claim 1; It is characterized in that: said step (1) moderate purity is that the addition of 99.999% zinc powder is 0.7g-1.0g, or purity is 99.999% aluminium powder 0.35g-0.5g.
3. according to the said a kind of method of measuring chlorion in the cupric zinc electrolyte sample of claim 1, it is characterized in that: add nitric acid 5ml in the said step (2).
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105136894A (en) * | 2015-07-24 | 2015-12-09 | 铜陵有色金属集团股份有限公司金冠铜业分公司 | Determination method of chloride ion content of copper electrolyte |
| CN106124503A (en) * | 2016-07-18 | 2016-11-16 | 北京矿冶研究总院 | Method for detecting concentration of cyanide in ore pulp |
| CN108240984A (en) * | 2016-12-23 | 2018-07-03 | 九江天赐高新材料有限公司 | A kind of method with the double chlorine sulfimide purity of chemical determination |
| CN110220856A (en) * | 2019-06-05 | 2019-09-10 | 常州大学 | The method that Flow Injection Analysis detects chloride ion content in the electrodeposit liquid of electrolytic copper foil |
| CN110220964A (en) * | 2019-06-05 | 2019-09-10 | 常州大学 | The measurement method of chloride ion in the copper electrolyte of electrolytic copper foil |
| CN110726719A (en) * | 2019-10-17 | 2020-01-24 | 广西贺州市桂东电子科技有限责任公司 | Device and method for detecting content of chloride ions in anodic formed foil electrolyte |
| CN111678759A (en) * | 2020-06-19 | 2020-09-18 | 四川精创检测技术有限公司 | Sample pretreatment method for waste water chloride determination |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101614718A (en) * | 2009-07-27 | 2009-12-30 | 广西大学 | A kind of method of measuring chloride ion content in high-performance concrete |
| CN101865901A (en) * | 2009-04-17 | 2010-10-20 | 江苏苏杭电子有限公司 | Method for analyzing chloride ion content in acid copper plating bath |
-
2012
- 2012-05-30 CN CN2012101730587A patent/CN102706875A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101865901A (en) * | 2009-04-17 | 2010-10-20 | 江苏苏杭电子有限公司 | Method for analyzing chloride ion content in acid copper plating bath |
| CN101614718A (en) * | 2009-07-27 | 2009-12-30 | 广西大学 | A kind of method of measuring chloride ion content in high-performance concrete |
Non-Patent Citations (2)
| Title |
|---|
| 何久康: "伏尔哈德法测定氯离子的介质研究", 《化学世界》 * |
| 肖晓辉: "佛尔哈德法测定氯化除汞上清液中的氯量", 《湖南有色金属》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105136894A (en) * | 2015-07-24 | 2015-12-09 | 铜陵有色金属集团股份有限公司金冠铜业分公司 | Determination method of chloride ion content of copper electrolyte |
| CN105136894B (en) * | 2015-07-24 | 2017-10-17 | 铜陵有色金属集团股份有限公司金冠铜业分公司 | The assay method of chloride ion content in copper electrolyte |
| CN106124503A (en) * | 2016-07-18 | 2016-11-16 | 北京矿冶研究总院 | Method for detecting concentration of cyanide in ore pulp |
| CN108240984A (en) * | 2016-12-23 | 2018-07-03 | 九江天赐高新材料有限公司 | A kind of method with the double chlorine sulfimide purity of chemical determination |
| CN110220856A (en) * | 2019-06-05 | 2019-09-10 | 常州大学 | The method that Flow Injection Analysis detects chloride ion content in the electrodeposit liquid of electrolytic copper foil |
| CN110220964A (en) * | 2019-06-05 | 2019-09-10 | 常州大学 | The measurement method of chloride ion in the copper electrolyte of electrolytic copper foil |
| CN110220964B (en) * | 2019-06-05 | 2020-04-28 | 常州大学 | Method for measuring chloride ions in copper electrolyte of electrolytic copper foil |
| CN110220856B (en) * | 2019-06-05 | 2021-07-27 | 常州大学 | Method for detecting content of chloride ions in electrodeposition liquid of electrolytic copper foil by flow injection method |
| CN110726719A (en) * | 2019-10-17 | 2020-01-24 | 广西贺州市桂东电子科技有限责任公司 | Device and method for detecting content of chloride ions in anodic formed foil electrolyte |
| CN111678759A (en) * | 2020-06-19 | 2020-09-18 | 四川精创检测技术有限公司 | Sample pretreatment method for waste water chloride determination |
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Application publication date: 20121003 |