CN102879452A - Method for determining content of micro chlorine ions in surface treatment solution - Google Patents
Method for determining content of micro chlorine ions in surface treatment solution Download PDFInfo
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- CN102879452A CN102879452A CN201210352457XA CN201210352457A CN102879452A CN 102879452 A CN102879452 A CN 102879452A CN 201210352457X A CN201210352457X A CN 201210352457XA CN 201210352457 A CN201210352457 A CN 201210352457A CN 102879452 A CN102879452 A CN 102879452A
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Abstract
The invention provides a method for determining the content of micro chlorine ions in a surface treatment solution. According to the method, the concentration of chlorine ions to be measured in the solution is improved by means of adding a certain amount of standard solution, so that the content of the micro chlorine ions in the surface treatment solution can be determined rapidly and accurately, and the content of the detected micro chlorine ions is enabled to achieve n ppm level. The method can be applied to the determination of the content of the micro chlorine ions in the surface treatment solutions such as chrome plated, aluminium alloy sulfuric acid anodization, aluminium alloy hard anodization, aluminium alloy chromic acid anodization, aluminium alloy chromic oxalate anodization, various aluminium alloy anodization dichromate sealing, various aluminium alloy anodization nickel acetate sealing and the like.
Description
Technical field
The present invention relates to a kind of method of measuring trace chlorine content in the surface processing solution, belong to the technical field of electrochemical analysis.
Background technology
At present, the assay method of chloride ion content mainly contains three major types: 1. classical macro-analysis method, namely judge the indicator titration method of titration end-point according to the indicator change color; 2. trace and trace analysis method, the i.e. chromatography of ions; 3. determine the potentiometric titration of titration end-point according to the hop of current potential, it detects and is limited to 10
-1～10
-5Mol/L both had been applicable to macro-analysis, also was applicable to the detection of microcomponent.In addition, the assay of chlorion can also adopt ion selective electrode method and turbidimetry.
And for surface processing solution, because trace chlorine content wherein is seldom, adopt classical macro-analysis method, can't detect terminal point at all.Secondly, because the comparison of ingredients of surface processing solution is complicated, high salt, peracid all can cause damage to pillar and the rejector of chromatography of ions, and cost is too high.Adopt the chromatography of ions, if pre-treatment is done well, not only instrument is caused damage, detected data are also inaccurate.
According to the physical condition of factory, we have at first adopted ion selective electrode method.By the test of a large amount of the method, its result shows: adopt ion-selective electrode, relative method to measure the content of the trace chlorine in the surface processing solution, method is quick and easy, does not need the effects on surface Treatment Solution to carry out special processing procedure.Not enough is that the ion-selective electrode relative method can not provide the definite data of trace chlorine content in the surface processing solution.Use turbidimetry, carry out the mensuration of trace chlorine in the surface processing solution, light and heat easily decomposes, unsettled character owing to silver chloride is subjected to, so that unstable result, test condition is wayward, and the experimenter is had relatively high expectations.Therefore invent a kind of simple and easyly, easy to operate, the method for trace chlorine content has great importance in the mensuration surface processing solution of good stability.
Summary of the invention
Technical matters to be solved by this invention is a kind of method of measuring chloride ion content in the surface processing solution of invention, is specially adapted to the mensuration of the trace chlorine content of n ppm in the surface processing solution, and described method is simple, quick, accurate, and good stability.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme to realize:
A kind of method of measuring trace chlorine content in the surface processing solution, adopt following steps:
1. adopt autopotentiometric titrator
Material and utensil: crosspoint 5ml; Electrode: silver electrode 6.0430.100;
2. reagent:
AgN03 standard solution: 0.01mol/L;
NaCl standard solution 500ppm: take by weighing benchmark NaCl reagent, descended dry 1 hour at 600 ℃ first, accurately take by weighing 0.5000g, use deionized water dissolving, and be diluted to 1000ml, shake up;
3. parameter setting:
DET pH
＞beginning condition
＞stop condition
4. determination method: A. pipette 500ppm the NaCl standard solution in beaker in tall form, add the deionized water that 40-60 doubly measures, stir; AgNO with 0.01mol/L
3Standard solution, the potentiometric titrimeter titration is designated as V with the terminal point volume
1B. get surface processing solution with the deionized water equal volume in beaker in tall form, pipette again with A in the NaCl standard solution of 500ppm of equal volume, stir, with the AgNO of 0.01mol/L
3Standard solution, the potentiometric titrimeter titration, the terminal point volume is designated as V
2C. the following formula of substitution calculates the content of trace chlorine in the surface processing solution;
NaCl=C (AgNO
3) * (V
2-V
1) * 58.45/ surface processing solution sample volume (g/L).
Specifically, described step determination method 4. is: pipette the NaCl standard solution 1.0ml of 500ppm in the 100ml beaker in tall form, add deionized water 50ml, stir; AgNO with 0.01mol/L
3Standard solution, the potentiometric titrimeter titration is designated as V with the terminal point volume
1, get surface processing solution 50.0ml in the 100ml beaker in tall form, pipette again the NaCl standard solution 1.0ml of 500ppm, stir, with the AgNO of 0.01mol/L
3Standard solution, the potentiometric titrimeter titration, the terminal point volume is designated as V
2, the following formula of substitution calculates the content of trace chlorine in the surface processing solution;
NaCl=C (AgNO
3) * (V
2-V
1) * 58.45/ surface processing solution sample volume (g/L).
The content assaying method of chlorion adopts following steps in described chrome-plated surface Treatment Solution, the aluminium alloy chromium oxalic acid anodized surface Treatment Solution:
1. adopt autopotentiometric titrator
Material and utensil: crosspoint 5ml; Electrode: silver electrode 6.0430.100;
2. reagent:
AgNO3 standard solution: 0.01mol/L;
NaCl standard solution 500ppm: take by weighing benchmark NaCl reagent, descended dry 1 hour at 600 ℃ first, accurately take by weighing 0.5000g, use deionized water dissolving, and be diluted to 1000ml, shake up;
3. parameter setting:
DET pH
＞beginning condition
＞stop condition
4. determination method: get surface processing solution 50.0ml to be measured in the 300ml beaker, add 20g solid BaCO
3, it is colourless fully reacting rear filtrate, dried Filter paper filtering is got filtrate in the 100ml beaker in tall form, pipettes NaCl standard solution 1.0ml again, stirs, and the titration parameter is set, with the AgNO of 0.01mol/L
3Standard solution, the potentiometric titrimeter titration, the terminal point volume is designated as V
2Pipette the NaCl standard solution 1.0ml of 500ppm in the 100ml beaker in tall form, add deionized water 50ml, stir, with the AgNO of 0.01mol/L
3Standard solution, the potentiometric titrimeter titration, its terminal point volume is designated as V
1The following formula of substitution calculates the content of trace chlorine in the surface processing solution;
NaCl=C (AgNO
3) * (V
2-V
1) * 58.45/ surface processing solution sample volume (g/L).
The present invention is the potentiometric titration of determining titration end-point according to the hop of current potential, and it detects and is limited to 10
-1～10
-5Mol/L both had been applicable to macro-analysis, also was applicable to the detection of microcomponent.Potentiometric titration be in titration process by measuring potential change to determine the method for titration end-point, it does not need exactly potential electrode potential value, thereby the impact of temperature, liquid junction potential seems and is not very important.Potentiometric titration is indicated titration end-point by the hop of electrode potential: before and after titration is reached home, ion concentration to be measured in the dropping liquid often changes n the order of magnitude continuously, cause the hop of current potential, the content of tested composition still calculates by the amount that consumes titrant.This specific character of potentiometric titration is highly suitable for the assay of each component in the surface processing solution.
But, because the content of trace chlorine is too low in the surface processing solution, directly measure wherein contained trace chlorine with potentiometric titration, can not find terminal point at all.In addition, the surface processing solution complicated component not only has the principal ingredient of obtain solution, the various impurity of bringing in addition when piece surface is processed.The composition of all existence, all the mensuration of trace chlorine exerts an influence in the possibility effects on surface Treatment Solution.Because content is extremely low and solution in the existence of interference component, measure according to the method for routine, can't go out the trace chlorine content that only has n ppm in the surface processing solution by Accurate Determining at all.
Therefore the applicant is through a large amount of experimental studies have found that, on autopotentiometric titrator, add a certain amount of standard solution by crossing, by improving the way of chlorine ion concentration to be measured in the solution, can determine accurately the trace chlorine content that only has n ppm in the surface processing solution.
We find again under study for action, other compositions are treated micrometer amount chlorion in the surface processing solution system interference, research is found: relatively simple for lock solution compositions such as sodium bichromate sealing, potassium dichromate sealing, Nickel acetate sealings, nickel acetate is on the not impact of mensuration of chlorion, the content of sodium bichromate and potassium dichromate is lower, can ignore the impact of determination of chloride ion.Other compositions that may bring into are less, can not produce large impact to determination of chloride ion, also can ignore.But chromate participant silver nitrate reacts, and produces the siliver chromate precipitation, so the chromate ion in the chromium plating, chromium oxalic acid anodization solution can produce certain impact to the mensuration of chlorion.Through research, the present invention adopts barium carbonate to remove the interference of chromate, can make the accuracy of testing result reach best.
The applicant has carried out a large amount of experimental studies, and is as follows:
Experimental example 1: the micro-Cl in the potentiometric determination confining surface Treatment Solution
-Ion
Material and utensil: crosspoint 5ml; Electrode silver electrode 6.0430.100
Main agents: AgN0
3Standard solution 0.01mol/L;
NaCl standard solution (500ppm): accurately take by weighing benchmark NaCl reagent (600 ℃ lower dry 1 hour) 0.5000g, use deionized water dissolving, and be diluted to 1000ml, shake up.
Analytical procedure:
Pipette NaCl standard solution (500ppm) 1.0ml in the 100ml beaker in tall form, add deionized water 50ml.Stir.AgN0 with 0.01mol/L
3Standard solution, the potentiometric titrimeter titration.The terminal point volume is designated as V
1(Cl).
The following setting of titration parameter:
DET pH
＞beginning condition
＞stop condition
Get surface processing solution 50.0ml in the 100ml beaker in tall form, pipette again NaCl standard solution (500ppm) 1.0ml, stir.AgNO with 0.01mol/L
3Standard solution, the potentiometric titrimeter titration.
The titration parameter arranges the same.
Calculate:
Micro-Cl in the gauging surface Treatment Solution
-Content (conversion for NaCl):
NaCl＝C(AgN0
3)×[EP(1)-V
1(Cl)]×58.45/V (g/L)
Wherein, C (AgNO
3)-----AgNO
3The concentration of standard solution, mol/L
EP (1)---consume AgNO during-Di 1 equivalent point
3The volume of standard solution, ml
V
1(Cl)----titration is blank, sees 2.5.1, ml
The V-----sample volume, ml
With above-mentioned Formula Input Technology titrator.
1) the micro-Cl in potentiometric determination chrome-plating bath, the chromium oxalic acid anodization rooved face Treatment Solution
-Ionic material, utensil, reagent are with 1).
2) analytical procedure:
The blank volume of titration is designated as V
1(Cl).Method is with 1).
Get surface processing solution 50.0ml in the 300ml beaker, add 20g solid BaC0
3, fully react rear filtrate and should be colourless.Dried Filter paper filtering.Get above-mentioned filtrate 30ml in the 100ml beaker in tall form, pipette again NaCl standard solution (500ppm) 1.0ml, stir.AgNO with 0.01mol/L
3Standard solution, the potentiometric titrimeter titration.
The titration parameter arranges with 1).
Computing formula is with 1).
3) verification experimental verification
Choose at random three surface processing solutions to be measured, carry out the recovery of standard addition test.Add Cl
-Ion standard solution 4ppm.It the results are shown in Table 1;
Fig. 1, Fig. 2 are seen in test data sheet for example.
Fig. 1 is the test findings that adopts the present invention that trace chlorine in the hard anodized surface processing solution is measured, and the result shows that the NaCl content in its solution is 0.05mg/L;
Fig. 2 adopts the present invention that Fig. 1 is adopted demonstration test result's (mark-on recovery test) that trace chlorine is measured in the hard anodized surface processing solution, it adds scalar 4.00mg/L, NaCl content behind the actual measurement mark-on is 4.46mg/L, and the recovery is 110%;
Table 1 recovery of standard addition test findings
By the result as seen, automatic potentiometric titration is measured the recovery of standard addition of trace chlorine content in the surface processing solution between 95%～110%, and accuracy is high, can meet the demands.
Compared with prior art, assay method of the present invention has following beneficial effect:
1, can measure fast and accurately trace chlorine content in the surface processing solution, make the trace chlorine content that detects reach n ppm level, develop new analytical approach.
2, the present invention adopts and once to add the target way, i.e. a certain amount of standard solution of disposable adding in surface processing solution to be measured has enlarged the concentration of chlorion to be measured, increased the volume that silver nitrate consumes, reduced the error of reading, precision is higher, is fit to microanalysis.
4, make that the mensuration of trace chlorine becomes simply in the surface processing solution, easy row, and the result is accurate, precision is high, makes our analytical technology, analysis level that further raising arranged.
5, the thinking that the effects on surface Treatment Solution is analyzed has been expanded in the removal of interfering ion.
6, the present invention can be applicable to the assay of trace chlorine in the surface processing solutions such as chromium plating, aluminium alloy sulfur acid anodizing, aluminum alloy hard anodization, aluminium alloy chromic acid anodizing, the anodization of aluminium alloy chromium oxalic acid, the sealing of all kinds of aluminium alloy anodization dichromate, all kinds of aluminium alloy anodization Nickel acetate sealings.
Description of drawings
Fig. 1 is trace chlorine assay figure as a result in the hard anodized surface processing solution;
Fig. 2 is as a result figure of trace chlorine is measured in the hard anodized surface processing solution demonstration test (mark-on recovery test);
Fig. 3 is chlorine ion content determination figure as a result in the chromic acid anodizing Nickel acetate sealing surface processing solution;
Fig. 4 is trace chlorine assay figure as a result in the chromium oxalic acid anodized surface Treatment Solution.
Embodiment:
Embodiment 1.Cl in the chromic acid anodizing Nickel acetate sealing surface processing solution
-Assay
1. adopt autopotentiometric titrator
Instrument model: Switzerland's ten thousand logical full-automatic current potential titration instruments of 809 types;
Material and utensil: crosspoint 5ml; Electrode: silver electrode 6.0430.100;
2. reagent:
AgN03 standard solution: 0.01mol/L;
NaCl standard solution 500ppm: take by weighing benchmark NaCl reagent, descended dry 1 hour at 600 ℃ first, accurately take by weighing 0.5000g, use deionized water dissolving, and be diluted to 1000ml, shake up;
3. parameter setting:
DET pH
＞beginning condition
＞stop condition
4. determination method: pipette the NaCl standard solution 1.0ml of 500ppm in the 100ml beaker in tall form, add deionized water 50ml, stir; AgNO with 0.01mol/L
3Standard solution, the potentiometric titrimeter titration is designated as V with the terminal point volume
1, get surface processing solution 50.0ml in the 100ml beaker in tall form, pipette again the NaCl standard solution 1.0ml of 500ppm, stir, with the AgNO of 0.01mol/L
3Standard solution, the potentiometric titrimeter titration, the terminal point volume is designated as V
2, the following formula of substitution calculates the content of trace chlorine in the surface processing solution, and test findings is seen Fig. 3;
NaCl=C (AgNO
3) * (V
2-V
1) * 58.45/ surface processing solution sample volume (g/L).
Embodiment 2.Micro-C1 in the chromium oxalic acid anodized surface Treatment Solution
-Assay
1. adopt autopotentiometric titrator
Instrument model: Switzerland's ten thousand logical full-automatic current potential titration instruments of 809 types;
Material and utensil: crosspoint 5ml; Electrode: silver electrode 6.0430.100;
2. reagent:
AgN03 standard solution: 0.01mol/L;
NaCl standard solution 500ppm: take by weighing benchmark NaCl reagent, descended dry 1 hour at 600 ℃ first, accurately take by weighing 0.5000g, use deionized water dissolving, and be diluted to 1000ml, shake up;
3. parameter setting:
DET pH
＞beginning condition
＞stop condition
4. determination method: get surface processing solution 50.0ml to be measured in the 300ml beaker, add 20g solid BaCO
3, it is colourless fully reacting rear filtrate, dried Filter paper filtering is got filtrate in the 100ml beaker in tall form, pipettes NaCl standard solution 1.0ml again, stirs, and the titration parameter is set, with the AgNO of 0.01mol/L
3Standard solution, the potentiometric titrimeter titration, the terminal point volume is designated as V
2Pipette the NaCl standard solution 1.0ml of 500ppm in the 100ml beaker in tall form, add deionized water 50ml, stir, with the AgNO of 0.01mol/L
3Standard solution, the potentiometric titrimeter titration, its terminal point volume is designated as V
1The following formula of substitution calculates the content of trace chlorine in the surface processing solution; Test findings is seen Fig. 4.
NaCl=C (AgNO
3) * (V
2-V
1) * 58.45/ surface processing solution sample volume (g/L).
Claims (4)
1. method of measuring trace chlorine content in the surface processing solution is characterized in that: adopt following steps:
1. adopt autopotentiometric titrator
Material and utensil: crosspoint 5ml; Electrode: silver electrode 6.0430.100;
2. reagent:
AgNO3 standard solution: 0.01mol/L;
NaCl standard solution 500ppm: take by weighing benchmark NaCl reagent, descended dry 1 hour at 600 ℃ first, accurately take by weighing 0.5000g, use deionized water dissolving, and be diluted to 1000ml, shake up;
3. parameter setting:
DET pH
＞beginning condition
＞stop condition
4. determination method: A. pipette 500ppm the NaCl standard solution in beaker in tall form, add the deionized water that 40-60 doubly measures, stir; AgNO with 0.01mol/L
3Standard solution, the potentiometric titrimeter titration is designated as V with the terminal point volume
1B. get surface processing solution with the deionized water equal volume in beaker in tall form, pipette again with A in the NaCl standard solution of 500ppm of equal volume, stir, with the AgNO of 0.01mol/L
3Standard solution, the potentiometric titrimeter titration, the terminal point volume is designated as V
2C. the following formula of substitution calculates the content of trace chlorine in the surface processing solution;
NaCl=C (AgNO
3) * (V
2-V
1) * 58.45/ surface processing solution sample volume (g/L).
2. measure as claimed in claim 1 the method for trace chlorine content in the surface processing solution, it is characterized in that:
Described step determination method 4. is: pipette the NaCl standard solution 1.0ml of 500ppm in the 100ml beaker in tall form, add deionized water 50ml, stir; AgNO with 0.01mol/L
3Standard solution, the potentiometric titrimeter titration is designated as V with the terminal point volume
1, get surface processing solution 50.0ml in the 100ml beaker in tall form, pipette again the NaCl standard solution 1.0ml of 500ppm, stir, with the AgNO of 0.01mol/L
3Standard solution, the potentiometric titrimeter titration, the terminal point volume is designated as V
2, the following formula of substitution calculates the content of trace chlorine in the surface processing solution;
NaCl=C (AgNO
3) * (V
2-V
1) * 58.45/ surface processing solution sample volume (g/L).
3. measure as claimed in claim 1 or 2 the method for trace chlorine content in the surface processing solution, it is characterized in that: described surface processing solution comprises chrome-plated surface Treatment Solution, aluminium alloy sulfur acid anodizing surface processing solution, Lv Hejin hard anodizing surface processing solution, aluminium alloy chromic acid anodizing surface processing solution, aluminium alloy chromium oxalic acid anodized surface Treatment Solution, aluminium alloy anodization dichromate confining surface Treatment Solution, aluminium alloy anodization Nickel acetate sealing surface processing solution.
4. measure as claimed in claim 3 the method for trace chlorine content in the surface processing solution, it is characterized in that:
The content assaying method of chlorion adopts following steps in described chrome-plated surface Treatment Solution, the aluminium alloy chromium oxalic acid anodized surface Treatment Solution:
1. adopt autopotentiometric titrator
Material and utensil: crosspoint 5ml; Electrode: silver electrode 6.0430.100;
2. reagent:
AgNO3 standard solution: 0.01mol/L;
NaCl standard solution 500ppm: take by weighing benchmark NaCl reagent, descended dry 1 hour at 600 ℃ first, accurately take by weighing 0.5000g, use deionized water dissolving, and be diluted to 1000ml, shake up;
3. parameter setting:
DET pH
＞beginning condition
＞stop condition
4. determination method: get surface processing solution 50.0ml to be measured in the 300ml beaker, add 20g solid BaCO
3, it is colourless fully reacting rear filtrate, dried Filter paper filtering is got filtrate in the 100ml beaker in tall form, pipettes NaCl standard solution 1.0ml again, stirs, and the titration parameter is set, with the AgNO of 0.01mol/L
3Standard solution, the potentiometric titrimeter titration, the terminal point volume is designated as V
2Pipette the NaCl standard solution 1.0ml of 500ppm in the 100ml beaker in tall form, add deionized water 50ml, stir, with the AgNO of 0.01mol/L
3Standard solution, the potentiometric titrimeter titration, its terminal point volume is designated as V
1The following formula of substitution calculates the content of trace chlorine in the surface processing solution;
NaCl=C (AgNO
3) * (V
2-V
1) * 58.45/ surface processing solution sample volume (g/L).
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| CN105675831A (en) * | 2015-11-08 | 2016-06-15 | 张开航 | Apparatus and method for measuring chlorine ion and total organic carbon in water |
| CN105806993A (en) * | 2016-04-08 | 2016-07-27 | 天津中水有限公司 | Method for detecting chloride in reclaimed water and titration apparatus |
| CN107727791A (en) * | 2017-10-17 | 2018-02-23 | 广西金川有色金属有限公司 | The determination method of chlorion in a kind of quartz sand |
| CN111879891A (en) * | 2020-06-30 | 2020-11-03 | 武汉钢铁有限公司 | Method for rapidly determining content of sulfite in industrial sulfuric acid |
| CN112326889A (en) * | 2020-11-04 | 2021-02-05 | 中国计量科学研究院 | Device and method for measuring content of volatile organic compounds in atmosphere |
| CN114705794A (en) * | 2022-04-15 | 2022-07-05 | 西湖大学 | Proteomics analysis method for biological sample |
| CN115508502A (en) * | 2022-09-21 | 2022-12-23 | 湖北兴瑞硅材料有限公司 | Method for detecting content of chloride ions in dimethyl dimethoxy silane hydrolysate |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105675831A (en) * | 2015-11-08 | 2016-06-15 | 张开航 | Apparatus and method for measuring chlorine ion and total organic carbon in water |
| CN105806993A (en) * | 2016-04-08 | 2016-07-27 | 天津中水有限公司 | Method for detecting chloride in reclaimed water and titration apparatus |
| CN105806993B (en) * | 2016-04-08 | 2018-08-21 | 天津中水有限公司 | Detect the detection method and titration outfit of chloride in recycled water water |
| CN107727791A (en) * | 2017-10-17 | 2018-02-23 | 广西金川有色金属有限公司 | The determination method of chlorion in a kind of quartz sand |
| CN111879891A (en) * | 2020-06-30 | 2020-11-03 | 武汉钢铁有限公司 | Method for rapidly determining content of sulfite in industrial sulfuric acid |
| CN112326889A (en) * | 2020-11-04 | 2021-02-05 | 中国计量科学研究院 | Device and method for measuring content of volatile organic compounds in atmosphere |
| CN114705794A (en) * | 2022-04-15 | 2022-07-05 | 西湖大学 | Proteomics analysis method for biological sample |
| CN115508502A (en) * | 2022-09-21 | 2022-12-23 | 湖北兴瑞硅材料有限公司 | Method for detecting content of chloride ions in dimethyl dimethoxy silane hydrolysate |
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Application publication date: 20130116 |