CN101344488A - Analytical method and special reagent for zinc chloride content in acidic zincing solution - Google Patents
Analytical method and special reagent for zinc chloride content in acidic zincing solution Download PDFInfo
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- CN101344488A CN101344488A CN 200810016537 CN200810016537A CN101344488A CN 101344488 A CN101344488 A CN 101344488A CN 200810016537 CN200810016537 CN 200810016537 CN 200810016537 A CN200810016537 A CN 200810016537A CN 101344488 A CN101344488 A CN 101344488A
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- special agent
- zinc chloride
- ammonium fluoride
- dihydrogen phosphate
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Abstract
The invention discloses an analyzing method of the zinc butter content in an acid galvanized solution and a specialized reagent, and the analyzing method adds the specialized WH177 reagent, an ammoniac buffer solution with pH equal to 10, a chrome black T into the measured solution, implements titration with an EDTA standard solution until an end point that the measured solution changes from red to blue, and finally computes the mass concentration of the zinc butter in the measured solution; the specialized WH177 reagent is prepared by mixing ammonium fluoride and monopotassium phosphate according to a certain proportion. The analyzing method solves the problem that traditional analyzing methods have bad accuracy in the content measurement of a main raw material in the galvanized solution when the galvanized solution has heavy impurity interference, and is characterized by practicability, quickness and accuracy, etc.
Description
Affiliated technical field
The invention belongs to the chemical analysis technology field, specifically, is zinc chloride analysis on Content method and special agent in a kind of acid zinc plating solution.
Background technology
Zinc-plated is a kind of important method of Treatment of Metal Surface.Traditional zincincation such as cyaniding is zinc-plated, alkaline zinc plating etc., safeguard simple relatively, but serious environment pollution all, thereby mostly progressively eliminated, the substitute is the electroplating technology of some environmental protections, wherein acid chlorization potassium zincincation is the zinc-plated main technique of environmental protection, and extremely people praise highly always.This implementation of processes need be to ZnCl in the galvanizing flux
2, KCl, H
3BO
4Content analyze so that in time adjust the concentration of each raw material in the plating bath, can obtain electroplating effect preferably.Yet because the quality of industrial chemicals is uneven, the more phenomenon of impurity in the plating bath often appears.Under the situation that serious impurity disturbs, traditional analytical approach can't correct analysis goes out in the plating bath especially ZnCl of each raw material
2Accurate content, also just can't play directive function to the conventional maintenance of zincincation, cause the enforcement of this green zincincation technical blind area to occur, thereby also make some enterprises this technology of having to abandon adopting, readopt the zincincation of some other high pollution then.
Summary of the invention
The purpose of this invention is to provide a kind of ZnCl in the acid zinc plating solution that analyzes
2The method of content makes in this way to exist under the situation of serious impurity interference at plating bath, can accurately analyze ZnCl in the plating bath
2Content, thereby also can accurately analyze the content of other raw materials in the plating bath.
Another object of the present invention provides a kind of acid zinc plating solution ZnCl that is used for analyzing
2The special agent of content.
For achieving the above object, the technical scheme of analytical approach of the present invention is ammonia buffer solution and the eriochrome black T that adds WH177 special agent, PH=10 in detected solution, becoming blueness to solution by redness with the EDTA standard solution titration then is terminal point, calculates the mass concentration of zinc chloride in the detected solution at last; Said WH177 special agent is formulated by a certain percentage by ammonium fluoride and potassium dihydrogen phosphate.
The said WH177 special agent of the present invention is formulated by the mass ratio of 0.5-1.5: 2.5-3.5 by ammonium fluoride and potassium dihydrogen phosphate, and ratio is 1: 3 preferably; The minimum flow of every milliliter of detected solution adding WH177 special agent is 1g.Before the mensuration, should add the dilution of a certain amount of water in the detected solution earlier, drip triethanolamine number droplet after, add other reagent again.The mass concentration of zinc chloride can be calculated as follows in the detected solution:
ρ＝c×v×136.3
ρ is the mass concentration (g/l) of zinc chloride in the detected solution in the formula, and c is the volumetric molar concentration (mol/l) of EDTA standard solution, and v is the milliliter number that consumes the EDTA standard solution, the 136.3rd, and the molecular weight of zinc chloride.
The feature of special agent WH177 technical scheme of the present invention is to contain ammonium fluoride and potassium dihydrogen phosphate in this special agent, and the mass ratio of ammonium fluoride and potassium dihydrogen phosphate is 0.5-1.5: 2.5-3.5, and ratio is 1: 3 preferably.
The present invention is particularly suitable for existing under the situation of serious impurity interference at electrogalvanizing solution, and the content of main salt such as its contained zinc chloride, potassium chloride is analyzed.In general, dispose in the used raw material of galvanizing solution and often contain impurity such as magnesium salts, calcium salt easily, if impurity content is higher, when using classic method that the zinc chloride content in the plating bath is measured, be difficult to find exactly reaction end, also just can't measure exactly, also can't accurately analyze thus the content of potassium chloride.Specific complex reagent WH177 used in the present invention, have shelter, the effect of complexing impurity element, have beyond thought effect for the content of zinc chloride in the accurate mensuration galvanizing flux.Specific complex reagent among the present invention is the molecular structure according to selected compounds, the result who draws through repetition test.According to test, use ammonium fluoride separately or use potassium dihydrogen phosphate all undesirable separately the masking effect of impurity in the plating bath, when the two made complex reagent, its effect was but obvious especially.
The invention solves the problem of traditional analysis method assay poor accuracy of primary raw material in galvanizing solution exists under the situation that serious impurity disturbs galvanizing solution.Use the present invention, even under the situation that serious impurity disturbs, also can measure the content of zinc chloride in the galvanizing flux accurately and rapidly, make also thus that the accurate mensuration of KCE content is achieved in the plating bath, have practicality, characteristics such as quick, accurate, through test, each links such as the plating solution maintenance in potassium chloride zinc plating process, adjustment, control have all obtained promising result, play very important regulating and controlling effect.Appearance of the present invention can make zinc-plated this environmental protection technology of potassium chloride be able to smooth implementation, thereby not contaminated type technology replaces, and therefore, the present invention also has the good social benefit.
Embodiment
Embodiment 1, in a certain amount of NH of the accurate weighing of 1: 3 ratio of mass ratio
4F and KH
2PO
3, mix, make the WH177 special agent.With analytical balance weighing ZnCl
260g, KCl180g, H
3BO
420g and MgCl
220g is mixed with 1 liter of simulation plating bath.Get 1ml simulation plating bath in the 250ml conical flask, add water 75ml dilution, drip triethanolamine number droplet, add again WH177 special agent 1g, PH=10 buffer solution 10ml, eriochrome black T a little, becoming blueness to solution by redness with the 0.05mol/lEDTA standard solution titration is terminal point, consumes EDTA standard solution 8.84ml altogether.The mass concentration of zinc chloride can be calculated as follows in the detected solution:
ρ＝c×v×136.3
ρ is the mass concentration (g/l) of zinc chloride in the detected solution in the formula, and c is the volumetric molar concentration (mol/l) of EDTA standard solution, and v is the milliliter number that consumes the EDTA standard solution, the 136.3rd, and the molecular weight of zinc chloride.Get ZnCl as calculated
2Mass concentration be 60.24g/l.Get the above-mentioned simulation plating bath of 1ml and carry out assay determination, get ZnCl with classic method
2Mass concentration be 106.04g/l.Compare with numerical value that analytical approach of the present invention is surveyed and numerical value that classic method is surveyed, can obviously find out advantage of the present invention place.Its comparing result sees the following form:
Embodiment 2, in a certain amount of NH of the accurate weighing of 1.5: 3.5 ratio of mass ratio
4F and KH
2PO
3, mix, make the WH177 special agent.With the accurate weighing ZnCl of analytical balance
270g, KCl190g, H
3BO
425g and MgCl
220g, CaCl
210g is mixed with 1 liter of simulation plating bath.Get 1ml simulation plating bath in the 250ml conical flask, add water 75ml dilution, drip triethanolamine number droplet, add again WH177 special agent 1.2g, PH=10 buffer solution 10ml, eriochrome black T a little, becoming blueness to solution by redness with the 0.05mol/lEDTA standard solution titration is terminal point, consumes EDTA standard solution 8.91ml altogether.Get ZnCl as calculated
2Mass concentration be 60.72g/l.Get the above-mentioned simulation plating bath of 1ml and carry out assay determination, get ZnCl with classic method
2Mass concentration be 128.33g/l.Contrast situation with analytical approach of the present invention and traditional analysis method measured result sees the following form:
Embodiment 3, in a certain amount of NH of the accurate weighing of 0.8: 2.8 ratio of mass ratio
4F and KH
2PO
3, mix, make the WH177 special agent.With the accurate weighing ZnCl of analytical balance
280g, KCl200g, H
3BO
430g and MgCl
220g, CaCl
210g, FeSO
45g is mixed with 1 liter of simulation plating bath.Get 1ml simulation plating bath in the 250ml conical flask, add water 75ml dilution, drip triethanolamine number droplet, add again WH177 special agent 1.2g, PH=10 buffer solution 10ml, eriochrome black T a little, becoming blueness to solution by redness with the 0.05mol/lEDTA standard solution titration is terminal point, consumes EDTA standard solution 11.7ml altogether.Get ZnCl as calculated
2Mass concentration be 79.74g/l.Get the above-mentioned simulation plating bath of 1ml and carry out assay determination, get ZnCl with classic method
2Mass concentration be 137.46g/l.Contrast situation with analytical approach of the present invention and traditional analysis method measured result sees the following form:
Claims (9)
1, zinc chloride analysis on Content method in a kind of acid zinc plating solution, it is characterized in that in detected solution, adding ammonia buffer solution and the eriochrome black T of WH177 special agent, PH=10, becoming blueness to solution by redness with the EDTA standard solution titration then is terminal point, calculates the mass concentration of zinc chloride in the detected solution at last; Said WH177 special agent is formulated by a certain percentage by ammonium fluoride and potassium dihydrogen phosphate.
2, analytical approach as claimed in claim 1 is characterized in that said WH177 special agent is formulated by the mass ratio of 0.5-1.5: 2.5-3.5 by ammonium fluoride and potassium dihydrogen phosphate.
3, analytical approach as claimed in claim 1 is characterized in that said WH177 special agent is formulated by 1: 3 mass ratio by ammonium fluoride and potassium dihydrogen phosphate.
4, analytical approach as claimed in claim 1 is characterized in that the minimum flow of every milliliter of detected solution adding WH177 special agent is 1g.
5, analytical approach as claimed in claim 1 is characterized in that in detected solution adding earlier a certain amount of water dilution, drip triethanolamine number droplet after, add other reagent again.
6, analytical approach as claimed in claim 1 is characterized in that the mass concentration of zinc chloride in the detected solution can be calculated as follows:
ρ＝c×v×136.3
ρ is the mass concentration (g/l) of zinc chloride in the detected solution in the formula, and c is the volumetric molar concentration (mol/l) of EDTA standard solution, and v is the milliliter number that consumes the EDTA standard solution, the 136.3rd, and the molecular weight of zinc chloride.
7, a kind of special agent WH177 that is used for analyzing acid zinc plating solution zinc chloride content is characterized in that containing in this special agent ammonium fluoride and potassium dihydrogen phosphate.
8, special agent WH177 as claimed in claim 7, the mass ratio that it is characterized in that ammonium fluoride and potassium dihydrogen phosphate is 0.5-1.5: 2.5-3.5.
9, special agent WH177 as claimed in claim 7, the mass ratio that it is characterized in that ammonium fluoride and potassium dihydrogen phosphate is 1: 3.
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|---|---|---|---|
| CN 200810016537 CN101344488A (en) | 2008-05-31 | 2008-05-31 | Analytical method and special reagent for zinc chloride content in acidic zincing solution |
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|---|---|---|---|
| CN 200810016537 CN101344488A (en) | 2008-05-31 | 2008-05-31 | Analytical method and special reagent for zinc chloride content in acidic zincing solution |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103063671A (en) * | 2011-10-19 | 2013-04-24 | 沈阳理工大学 | Rapid online analysis method for main component in acidic galvanization electroplate liquid |
| CN103913457A (en) * | 2012-12-31 | 2014-07-09 | 北京有色金属与稀土应用研究所 | Method for titration of zinc content in silver-copper-zinc alloy by ethylenediamine tetraacetic acid |
| CN103954730A (en) * | 2014-05-22 | 2014-07-30 | 山东安能输送带橡胶有限公司 | Method for detecting barium and zinc in zinc-barium liquid compound stabilizer |
| CN104749318A (en) * | 2013-12-30 | 2015-07-01 | 北京有色金属与稀土应用研究所 | Method for volumetric method determination of zinc content in silver copper zinc cadmium nickel solder |
| CN105891408A (en) * | 2016-04-01 | 2016-08-24 | 中国科学院青海盐湖研究所 | Method for measuring magnesium and zinc content in alloy at same time and application thereof |
| CN108845073A (en) * | 2018-06-08 | 2018-11-20 | 广州超邦化工有限公司 | Measure the new method of Potassium Chloride Zinc Plating Chlorine in Solution zinc |
| CN112505034A (en) * | 2020-11-23 | 2021-03-16 | 山西北方机械制造有限责任公司 | Non-toxic and environment-friendly chemical analysis method for zinc ions in galvanizing solution |
-
2008
- 2008-05-31 CN CN 200810016537 patent/CN101344488A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103063671A (en) * | 2011-10-19 | 2013-04-24 | 沈阳理工大学 | Rapid online analysis method for main component in acidic galvanization electroplate liquid |
| CN103913457A (en) * | 2012-12-31 | 2014-07-09 | 北京有色金属与稀土应用研究所 | Method for titration of zinc content in silver-copper-zinc alloy by ethylenediamine tetraacetic acid |
| CN104749318A (en) * | 2013-12-30 | 2015-07-01 | 北京有色金属与稀土应用研究所 | Method for volumetric method determination of zinc content in silver copper zinc cadmium nickel solder |
| CN103954730A (en) * | 2014-05-22 | 2014-07-30 | 山东安能输送带橡胶有限公司 | Method for detecting barium and zinc in zinc-barium liquid compound stabilizer |
| CN103954730B (en) * | 2014-05-22 | 2015-08-05 | 山东康迪泰克工程橡胶有限公司 | The detection method of barium and zinc in liquid barium zinc compound stabilizer |
| CN105891408A (en) * | 2016-04-01 | 2016-08-24 | 中国科学院青海盐湖研究所 | Method for measuring magnesium and zinc content in alloy at same time and application thereof |
| CN108845073A (en) * | 2018-06-08 | 2018-11-20 | 广州超邦化工有限公司 | Measure the new method of Potassium Chloride Zinc Plating Chlorine in Solution zinc |
| CN112505034A (en) * | 2020-11-23 | 2021-03-16 | 山西北方机械制造有限责任公司 | Non-toxic and environment-friendly chemical analysis method for zinc ions in galvanizing solution |
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Open date: 20090114 |