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Method for quick determination of zinc content in alkaline zinc-nickel alloy plating solution

A zinc-nickel alloy and rapid determination technology, which is applied in the direction of material analysis by observing the influence of chemical indicators, and analysis by making materials undergo chemical reactions, can solve the difficulty of judging the end point and the influence of dimethylglyoxime and nickel. Color reaction speed, nickel titration, etc.

Active Publication Date: 2019-10-11
宁波优优希新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Coordinating agents such as diethylenetriamine in the alkaline zinc-nickel alloy plating solution seriously affect the color reaction speed of dimethylglyoxime and nickel, and the color cannot be completely developed after 2 hours of reaction, and the result of the determination of nickel is obviously low [2] , leading to significantly higher zinc determination results
When adopting said method to measure the total amount of zinc and nickel in the alkaline zinc-nickel alloy plating solution, because nickel has generated a relatively stable complex with diethylenetriamine, nickel cannot be completely titrated by EDTA, and the total amount of zinc and nickel cannot be obtained. quantity
In addition, using the method to determine the total amount of zinc and nickel, nickel ions interfere with the discoloration of the CuY-PAN indicator, making it difficult to judge the end point

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Prepare the following reagents:

[0036] Polyethylene polyamine solution: 50 g / L polyethylene polyamine aqueous solution;

[0037] Dilute hydrochloric acid: the volume ratio of concentrated hydrochloric acid to water is 1: 1;

[0038] Acetic acid-sodium acetate buffer solution: dissolve 160 g of anhydrous sodium acetate in water, add 60 mL of glacial acetic acid, and add water to 1 L;

[0039] Ascorbic acid: solid;

[0040]Sodium fluoride: solid;

[0041] m-nitrophenol indicator: 0.1% ethanol solution of m-nitrophenol.

[0042] Xylenol orange indicator: 0.2% xylenol orange aqueous solution.

[0043] EDTA standard solution: 0.05 mol / L disodium edetate aqueous solution.

[0044] Draw 2 mL of alkaline zinc-nickel alloy plating solution into a 300 mL conical flask, add 100 mL of water to dilute, add 2-3 drops of m-nitrophenol indicator, add dropwise dilute hydrochloric acid until the test solution changes from yellow to colorless, add Acetic acid-sodium acetate buffer...

Embodiment 2

[0076] Prepare the following reagents:

[0077] Polyethylene polyamine solution: 40 g / L polyethylene polyamine aqueous solution;

[0078] Dilute hydrochloric acid: the volume ratio of concentrated hydrochloric acid to water is 1: 1.2;

[0079] Acetic acid-sodium acetate buffer solution: dissolve 160 g of anhydrous sodium acetate in water, add 60 mL of glacial acetic acid, and add water to 1 L;

[0080] Ascorbic acid: solid;

[0081] Sodium fluoride: solid;

[0082] m-nitrophenol indicator: 0.05% ethanol solution of m-nitrophenol.

[0083] Xylenol orange indicator: 0.15% xylenol orange aqueous solution.

[0084] EDTA standard solution: 0.05 mol / L disodium edetate aqueous solution.

[0085] Take the alkaline zinc-nickel alloy plating solution from the production line of the electroplating factory as the solution to be tested:

[0086] Draw 2 mL of alkaline zinc-nickel alloy plating solution into a 300 mL conical flask, add 100 mL of water to dilute, add 2-3 drops of m-nitr...

Embodiment 3

[0097] Prepare the following reagents:

[0098] Polyethylene polyamine solution: 60 g / L polyethylene polyamine aqueous solution;

[0099] Dilute hydrochloric acid: the volume ratio of concentrated hydrochloric acid to water is 1: 2;

[0100]Acetic acid-sodium acetate buffer solution: dissolve 160 g of anhydrous sodium acetate in water, add 60 mL of glacial acetic acid, and add water to 1 L;

[0101] Ascorbic acid: solid;

[0102] Sodium fluoride: solid;

[0103] m-nitrophenol indicator: 0.08% ethanol solution of m-nitrophenol.

[0104] Xylenol orange indicator: 0.25% xylenol orange aqueous solution.

[0105] EDTA standard solution: 0.05 mol / L disodium edetate aqueous solution.

[0106] Determining the precision of an analytical method

[0107] Take the alkaline zinc-nickel alloy plating solution from the production line of the electroplating factory as the solution to be tested.

[0108] Draw 2 mL of alkaline zinc-nickel alloy plating solution to be tested into a 300 mL...

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Abstract

The invention discloses a method for rapidly determining the content of zinc in an alkaline zinc-nickel alloy plating solution, which adopts polyethylene polyamine to conceal nickel ions and copper impurities, solves the technical difficulty that no method for concealing the nickel ions under an acid condition is provided in the past, and also creates a novel method for concealing the copper impurities under the acid condition. According to the method provided by the invention, ascorbic acid is adopted to conceal iron impurities, sodium fluoride is used to conceal aluminum impurities, xylenolorange is used as an indicator under the condition that pH is 5.0 to 5.3, and an EDTA standard solution is used for titrating zinc. By adopting the method for determining the content of the zinc in the alkaline zinc-nickel alloy plating solution, the relative average deviation is 0.35 percent, the recovery rate is 99.4 percent, and the method is simple, rapid, accurate and environmentally friendly.

Description

technical field [0001] The invention relates to an analysis method for zinc in an alkaline zinc-nickel alloy plating solution, in particular to an analysis method for zinc in an alkaline zinc-nickel alloy plating solution containing various aliphatic polyamine complexing agents. Background technique [0002] For the analysis of alkaline zinc-nickel alloy plating solution, potassium cyanide was used to mask nickel in the past, and the content of zinc was determined by EDTA volumetric method [1] . Cyanide is one of the highly toxic compounds strictly prohibited by the state, and this method has been banned. Relevant literature reports the determination method of zinc and nickel content in acidic zinc-nickel alloy plating solution [2] , Use EDTA spectrophotometry to measure the nickel content, use the EDTA volumetric method to measure the total amount of zinc and nickel, and then use the subtraction method to calculate the zinc content. Because the alkaline zinc-nickel alloy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/78
Inventor 郭崇武赖奂汶黎小阳
Owner 宁波优优希新材料科技有限公司