CN104155406B - The assay method of ferrous ion and zinc chloride content in a kind of Plating Auxiliary of Hot Dip Galvanizing - Google Patents
The assay method of ferrous ion and zinc chloride content in a kind of Plating Auxiliary of Hot Dip Galvanizing Download PDFInfo
- Publication number
- CN104155406B CN104155406B CN201410338545.3A CN201410338545A CN104155406B CN 104155406 B CN104155406 B CN 104155406B CN 201410338545 A CN201410338545 A CN 201410338545A CN 104155406 B CN104155406 B CN 104155406B
- Authority
- CN
- China
- Prior art keywords
- solution
- content
- ions
- ferrous
- zinc
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910001448 ferrous ion Inorganic materials 0.000 title claims abstract description 48
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 title claims abstract description 41
- 238000007747 plating Methods 0.000 title claims abstract description 29
- 239000011592 zinc chloride Substances 0.000 title claims abstract description 22
- 235000005074 zinc chloride Nutrition 0.000 title claims abstract description 19
- 238000005246 galvanizing Methods 0.000 title claims abstract description 14
- 238000003556 assay Methods 0.000 title abstract 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 22
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000004448 titration Methods 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 40
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 33
- 239000012086 standard solution Substances 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- RYYWUUFWQRZTIU-UHFFFAOYSA-N Thiophosphoric acid Chemical compound OP(O)(S)=O RYYWUUFWQRZTIU-UHFFFAOYSA-N 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- DGXTZMPQSMIFEC-UHFFFAOYSA-M sodium;4-anilinobenzenesulfonate Chemical compound [Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=CC=C1 DGXTZMPQSMIFEC-UHFFFAOYSA-M 0.000 claims description 5
- 239000010981 turquoise Substances 0.000 claims description 4
- 244000025254 Cannabis sativa Species 0.000 claims description 3
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 3
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims 1
- 238000010790 dilution Methods 0.000 claims 1
- 230000000873 masking effect Effects 0.000 claims 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 abstract 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- -1 iron ions Chemical class 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003926 complexometric titration Methods 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
An assay method for ferrous ion and zinc chloride content in Plating Auxiliary of Hot Dip Galvanizing, wherein, the mensuration of ferrous ion content comprises the steps: (1) fluxing agent solution-treated; (2) dichromate titration; (3) ferrous ion cubage; Zinc ion content is measured the preparation that comprises the steps: (1) Cu-PAN mixed indicator; (2) EDTA titration; (3) zinc ion content is calculated. The method is simple and quick, and the degree of accuracy is high.
Description
Technical Field
The invention relates to a method for measuring the content of ferrous ions and zinc chloride in a hot-dip galvanizing plating assistant, belongs to the technical field of a solution analysis method of the hot-dip galvanizing assistant, and is particularly suitable for measuring the content of ferrous ions and zinc ions in a hot-dip galvanizing solution taking zinc chloride and ammonium chloride as the plating assistant.
Background
The hot-dip galvanizing technology is used for corrosion prevention of steel products and is widely applied to the fields of electric power, traffic, buildings and the like. The hot-dip galvanizing assistant is the most widely used assistant at present, which is a mixed aqueous solution of ammonium chloride and zinc chloride. The method for determining the contents of ferrous ions and zinc ions in a hot-dip galvanizing plating assistant solution published in China at present mainly comprises the steps of firstly, using sodium diphenylamine sulfonate as a color developing agent, preparing a series of standard solutions, and measuring the content of the ferrous ions by using a spectrophotometer method; second, a complexometric titration method in which PAN is used as an indicator and zinc ions are titrated with EDTA. The first method is highly demanding for production shop analysts and is often difficult to achieve in practice; in the second method, the phenomenon that the end point color development is not sharp and the judgment is unclear occurs when the hot-dip galvanizing plating assistant solution is measured. In order to find a simple and effective method, a method for measuring the content of ferrous ions and zinc ions in the plating assistant is researched.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for measuring the content of ferrous ions and zinc chloride in a hot-dip galvanizing plating assistant, sodium diphenylamine sulfonate is added into a solution to be measured, potassium dichromate is used for redox titration until the solution turns purple, and the content of ferrous ions is measured; then, taking a part of solution, adding thiophosphoric acid to mask iron ions, adjusting the pH value of the solution to be about 5-6, using Cu-PAN as an indicator, titrating the solution by EDTA until the solution becomes turquoise, measuring the total content of the ferrous ions and the zinc ions, and subtracting the measured content of the ferrous ions to obtain the content of the zinc ions in the solution. The method is simple and rapid and has high accuracy.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for measuring the content of ferrous ions and zinc chloride in a hot-dip galvanizing plating assistant comprises the following steps:
determination of ferrous ion content
(1) Plating assistant solution treatment
2.00mL of plating assistant solution is sucked, diluted and fixed to 100 mL; sucking 25.00mL of diluent into a 250mL conical flask, adding 10mL of sulfuric-phosphoric acid, 10mL of water and a few drops of sodium diphenylamine sulfonate;
(2) titration of potassium dichromate
Titrating with a potassium dichromate standard solution with the concentration of 0.010M until the solution changes from light green to purple;
(3) ferrous ion content calculation
The ferrous ion content is calculated as follows:
wherein,
c(Fe2+) The content of ferrous ions in the plating assistant solution is g/L;
55.84 is ferrous ion molar mass;
6 is the reaction molar coefficient ratio of ferrous ions to potassium dichromate;
c1the concentration of the standard solution of potassium dichromate is shown in mol/L;
V1the volume of a potassium dichromate standard solution consumed for titrating ferrous ions is mL;
determination of the Zinc ion content
(1) Preparation of Cu-PAN Mixed indicator
1.2610g of blue vitriol is weighed, dissolved by deionized water to be 100 mL; measuring 10mL of copper sulfate solution, adding 10mL of ethanol, adding 3-4 drops of 1% PAN indicator, and shaking up; titrating with EDTA solution with the concentration of 0.05M until the solution turns into grass green;
(2) EDTA titration
Adding 25.00mL of diluted plating assistant agent into a 250mL conical flask, adding 10mL of thiophosphoric acid, adding 7mLCu-PAN indicator, adding 3-4 drops of PAN indicator, and titrating with EDTA standard solution until the solution turns into turquoise;
(3) calculation of Zinc ion content
The zinc ion content is calculated according to the following formula:
wherein,
c(ZnCl2) The zinc chloride content in the plating assistant solution is g/L;
136.30 is the molar mass of zinc chloride;
c2the concentration of the EDTA standard solution is shown in mol/L;
V2the volume of the EDTA standard solution consumed for titrating ferrous ions and zinc ions is mL;
6c1V1amount of a substance that is ferrous ions;
compared with the prior art, the invention has the beneficial results that:
1. the titration method of potassium dichromate ferrous oxide ions is adopted, so that the cost is low, technicians can easily master the titration method, the endpoint judgment is accurate, and the content of ferrous ions in the plating assistant can be monitored in time.
2. The zinc chloride content is measured by adopting a differential method, the end point judgment is accurate, and the accuracy is high.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
A method for measuring the content of ferrous ions and zinc chloride in a hot-dip galvanizing plating assistant comprises the following steps:
determination of ferrous ion content
(1) Plating assistant solution treatment
2.00mL of plating assistant solution is sucked, diluted and fixed to 100 mL; sucking 25.00mL of diluent into a 250mL conical flask, adding 10mL of sulfuric-phosphoric acid, 10mL of water and a few drops of sodium diphenylamine sulfonate;
(2) titration of potassium dichromate
Titrating with a potassium dichromate standard solution with the concentration of 0.010M until the solution changes from light green to purple;
(3) ferrous ion content calculation
The ferrous ion content is calculated as follows:
wherein,
c(Fe2+) The content of ferrous ions in the plating assistant solution is g/L;
55.84 is ferrous ion molar mass;
6 is the reaction molar coefficient ratio of ferrous ions to potassium dichromate;
c1the concentration of the standard solution of potassium dichromate is shown in mol/L;
V1the volume of a potassium dichromate standard solution consumed for titrating ferrous ions is mL;
determination of zinc chloride content
(1) Preparation of Cu-PAN Mixed indicator
1.2610g of blue vitriol is weighed, dissolved by deionized water to be 100 mL; measuring 10mL of copper sulfate solution, adding 10mL of ethanol, adding 3-4 drops of 1% PAN indicator, and shaking up; titrating with EDTA solution with the concentration of 0.05M until the solution turns into grass green;
(2) EDTA titration
Adding 25.00mL of diluted plating assistant agent into a 250mL conical flask, adding 10mL of thiophosphoric acid, adding 7mLCu-PAN indicator, adding 3-4 drops of PAN indicator, and titrating with EDTA standard solution until the solution turns into turquoise;
(3) calculation of Zinc chloride content
The zinc ion content is calculated according to the following formula:
wherein,
c(ZnCl2) The zinc chloride content in the plating assistant solution is g/L;
136.30 is the molar mass of zinc chloride;
c2the concentration of the EDTA standard solution is shown in mol/L;
V2the volume of the EDTA standard solution consumed for titrating ferrous ions and zinc ions is mL;
6c1V1amount of species that are ferrous ions.
Claims (1)
1. A method for measuring the content of ferrous ions and zinc chloride in a hot-dip galvanizing plating assistant comprises the following steps:
determination of ferrous ion content
(1) Plating assistant solution treatment
2.00mL of plating assistant solution is sucked, diluted and fixed to 100 mL; 25.00mL of the dilution was aspirated into a 250mL Erlenmeyer flask,
(2) titration of potassium dichromate
Titrating with a potassium dichromate standard solution with the concentration of 0.010M until the solution changes from light green to purple;
(3) ferrous ion content calculation
The ferrous ion content is calculated as follows:
wherein,
c(Fe2+) The content of ferrous ions in the plating assistant solution is g/L;
55.84 is ferrous ion molar mass;
6 is the reaction molar coefficient ratio of ferrous ions to potassium dichromate;
c1the concentration of the standard solution of potassium dichromate is shown in mol/L;
V1the volume of a potassium dichromate standard solution consumed for titrating ferrous ions is mL;
determination of the Zinc ion content
(1) Preparation of Cu-PAN Mixed indicator
1.2610g of blue vitriol is weighed, dissolved by deionized water to be 100 mL; measuring 10mL of copper sulfate solution, adding 10mL of ethanol, adding 3-4 drops of 1% PAN indicator, and shaking up; titrating with EDTA solution with the concentration of 0.05M until the solution turns into grass green;
(2) EDTA titration
Adding 25.00mL of diluted plating assistant agent into a 250mL conical flask, adding 10mL of thiophosphoric acid, adding 7mLCu-PAN indicator, adding 3-4 drops of PAN indicator, and titrating with EDTA standard solution until the solution turns into turquoise;
(3) calculation of Zinc ion content
The zinc ion content is calculated according to the following formula:
wherein,
c(ZnCl2) The zinc chloride content in the plating assistant solution is g/L;
136.30 is the molar mass of zinc chloride;
c2the concentration of the EDTA standard solution is shown in mol/L;
V2the volume of the EDTA standard solution consumed for titrating ferrous ions and zinc ions is mL;
6c1V1the amount of a substance that is ferrous ions,
the method is characterized in that the plating assistant agent solution treatment (1) further comprises the steps of adding 10mL of thiophosphoric acid, 10mL of water and a few drops of sodium diphenylamine sulfonate; when the contents of ferrous ions and zinc ions are measured, thiophosphoric acid is added as a masking agent, and the pH is adjusted to 5-6; when the content of zinc ions is measured, the content of ferrous ions is firstly measured, then the total amount of the ferrous ions and the zinc ions is measured by a titration method, and the content of the zinc ions is obtained by a difference method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410338545.3A CN104155406B (en) | 2014-07-16 | 2014-07-16 | The assay method of ferrous ion and zinc chloride content in a kind of Plating Auxiliary of Hot Dip Galvanizing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410338545.3A CN104155406B (en) | 2014-07-16 | 2014-07-16 | The assay method of ferrous ion and zinc chloride content in a kind of Plating Auxiliary of Hot Dip Galvanizing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104155406A CN104155406A (en) | 2014-11-19 |
| CN104155406B true CN104155406B (en) | 2016-05-04 |
Family
ID=51880962
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410338545.3A Active CN104155406B (en) | 2014-07-16 | 2014-07-16 | The assay method of ferrous ion and zinc chloride content in a kind of Plating Auxiliary of Hot Dip Galvanizing |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104155406B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108037238A (en) * | 2018-02-11 | 2018-05-15 | 中国科学院海洋研究所 | A kind of dichromate titration for measuring silicate rock divalence iron content |
| CN109580872A (en) * | 2018-12-11 | 2019-04-05 | 天津冶金集团中兴盛达钢业有限公司 | Bivalent cupric ion rapid assay methods in a kind of copper plating bath |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1264041A (en) * | 2000-01-25 | 2000-08-23 | 纪胜 | Method for eliminating Fe2+ interference in detection of Zn content |
-
2014
- 2014-07-16 CN CN201410338545.3A patent/CN104155406B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1264041A (en) * | 2000-01-25 | 2000-08-23 | 纪胜 | Method for eliminating Fe2+ interference in detection of Zn content |
Non-Patent Citations (6)
| Title |
|---|
| EDTA容量法直接测定酸铜镀液中的锌杂质;董荟文，郭崇武;《电镀与环保》;20140531;第34卷(第3期);前言第5~8行、摘要第1~2行、第1.2节第7~11行和第1.4~1.5节 * |
| 热浸镀锌物料中铁离子分析测定方法研究;徐杰等;《江西科学》;20101231;第28卷(第6期);全文 * |
| 用Cu-PAN系统作EDTA对钙、钡、镁、铝、铬、锌、铁、铅、铋、铜等化合物的测定;陆明廉等;《药学学报》;19630731;第10卷(第7期);全文 * |
| 采用新型指示剂的EDTA络合滴定法测定镀锌液中锌离子浓度的研究;卞明辉;《电镀与环保》;19870731;第7卷(第4期);全文 * |
| 锌-铁合金镀液中锌、铁的测定;章江洪等;《电镀与精饰》;20040531;第26卷(第3期);全文 * |
| 镀锌废酸中铁、锌含量的测定方法;叶素妹;《化学分析计量》;20090228;第18卷(第1期);摘要第一行、第52页左栏第2段和倒数第1段、第52页右栏第1~17和倒数第1~2行和第53页左栏第1~28行 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104155406A (en) | 2014-11-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101349648B (en) | Method for measuring trace elements in high titanium high boiler slag | |
| CN101995383A (en) | Method for measuring copper ion content of solution | |
| CN103439454B (en) | Method for measuring vanadium pentoxide content by potentiometric titration | |
| CN104155406B (en) | The assay method of ferrous ion and zinc chloride content in a kind of Plating Auxiliary of Hot Dip Galvanizing | |
| CN105158406A (en) | Method for measuring silica content in ferromanganese iron by utilizing potassium fluosilicate volumetric method | |
| CN103471889A (en) | Method for detecting trivalent chromic ions by using gamma-polyglutamic acid stabilized gold nanoparticles | |
| CN103487550A (en) | Method for determining content of nitric acid in titanium plate pickling solution | |
| CN102866145A (en) | Method for measuring total vanadium concentration in all vanadium redox flow battery electrolyte | |
| CN110726802B (en) | Method for accurately analyzing nickel sulfate in citrate nickel plating solution | |
| CN102313771B (en) | Method for measuring metallic iron in iron-containing material | |
| CN105548147B (en) | A kind of method of manganese element content in measurement Mn-rich slag | |
| CN107037036B (en) | Method for measuring phosphorus content in lithium iron phosphate | |
| CN103954574A (en) | Method for testing content of tungsten in ferroniobium | |
| CN103604804A (en) | Method for measuring content of iron in iron raw materials | |
| CN104034726A (en) | Method for determining bismuth content and vanadium content of bismuth vanadate | |
| CN103823017A (en) | Method for accurate measurement on nitric acid content of chemical corrosion solution for titanium alloy | |
| CN104655610B (en) | The analysis method and assay method of vanadyl oxalate oxalate ion concentration | |
| CN105223200B (en) | A kind of method of content of hydrochloric acid in Accurate Determining iron chloride etchant solution | |
| CN103091320A (en) | Method for testing content of titanium dioxide by complexometric titration-back titration method | |
| CN103940763A (en) | Method for detection of lead ions in water | |
| CN113607722A (en) | Method for detecting concrete chloride ion erosion depth | |
| CN113418910A (en) | Method for measuring iron ion content | |
| CN105067605A (en) | Method for continuously determining calcium content and iron content in limestone powder | |
| CN110794084A (en) | Method for measuring calcium chlorate content | |
| CN105067754A (en) | Method for analyzing content of iron in hot-dip galvanized alloyed steel plate by oxidimetry |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: No. 9 West nine road, Keyuan Avenue, Nanning, the Guangxi Zhuang Autonomous Region Patentee after: Guangxi electric power line equipment factory Co., Ltd. Address before: No. 224 Yongan East Road, Litang Town, Binyang County, Nanning, the Guangxi Zhuang Autonomous Region Patentee before: Guangxi Power Line Equipment Factory |
|
| CP03 | Change of name, title or address | ||
| CP02 | Change in the address of a patent holder |
Address after: No. 224-4, Yong'an East Road, Litang Town, Binyang County, Nanning City, Guangxi Zhuang Autonomous Region, 530409 Patentee after: GUANGXI POWER LINE EQUIPMENT AND FITTING FACTORY Co.,Ltd. Address before: 530007 No.9, Xijiu Road, Keyuan Avenue, Nanning, Guangxi Zhuang Autonomous Region Patentee before: GUANGXI POWER LINE EQUIPMENT AND FITTING FACTORY Co.,Ltd. |
|
| CP02 | Change in the address of a patent holder |