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 PDF

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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
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solution
content
ions
ferrous
zinc
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CN104155406A (en
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尚美洁
彭德柱
林贤杰
黄朝勇
覃枫
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Guangxi Electric Power Line Equipment Factory Co Ltd
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GUANGXI POWER LINE EQUIPMENT FACTORY
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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

Method for measuring content of ferrous ions and zinc chloride in hot-dip galvanizing plating assistant
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:
c ( Fe 2 + ) = 55.84 × 6 × c 1 × V 1 × 100 25 × 5 = 268.03 c 1 V 1
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:
c ( ZnCl 2 ) = 136.30 × ( c 2 g V 2 - 6 c 1 g V 1 ) × 100 25 × 5 = 109.04 ( c 2 V 2 - 6 c 1 V 1 )
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:
c ( Fe 2 + ) = 55.84 × 6 × c 1 × V 1 × 100 25 × 5 = 268.03 c 1 V 1
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:
c ( ZnCl 2 ) = 136.30 × ( c 2 g V 2 - 6 c 1 g V 1 ) × 100 25 × 5 = 109.04 ( c 2 V 2 - 6 c 1 V 1 )
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:
c ( Fe 2 + ) = 55.84 × 6 × c 1 × V 1 × 100 25 × 2 = 670.08 c 1 V 1
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:
c ( ZnCl 2 ) = 136.30 × ( c 2 V 2 - 6 c 1 V 1 ) × 100 25 × 2 = 272.6 ( c 2 V 2 - 6 c 1 V 1 )
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.
CN201410338545.3A 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 Active CN104155406B (en)

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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
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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 *
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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 *
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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

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Address after: No. 224-4, Yong'an East Road, Litang Town, Binyang County, Nanning City, Guangxi Zhuang Autonomous Region, 530409

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