CN103852468A - Method for detecting content of cerous sulfate in tin-cerium alloy electroplating solution - Google Patents

Abstract

The invention relates to a method for detecting a content of cerous sulfate in a tin-cerium alloy electroplating solution and belongs to the field of electroplating solution analysis technologies. The method is mainly characterized by comprising the following steps: oxidizing the electroplating solution to be detected by using perchloric acid, phosphoric acid and nitric acid with a certain concentration; with N-phenyl o-aminobenzoic acid as an indicator, detecting the content of the cerous sulfate in the tin-cerium alloy electroplating solution in a way of titrating tetravalent cerium into trivalent cerium by using an ammonium ferrous sulfate standard titration solution. The detection method has the characteristics that the detection is simple, the detection process is convenient, quick and environment-friendly and low in cost, and the detection results are accurate and coincident.

Description

A kind of assay method of tin-cerium alloy electroplating solution cerous sulfate content

Technical field

The present invention relates to a kind of assay method of tin-cerium alloy electroplating solution cerous sulfate content, belong to Plating Solution for Analysis technical field, it is specially adapted to the content of cerous sulfate composition in bright tin plating cerium alloy electroplating solution to measure.

Background technology

Bright tin plating cerium alloy is applied at home, the alloy of cerium and tin co-precipitation can prevent that matrix copper from forming the alloy diffusion layer that can not weld, and this Alloy Anti oxidability is strong, and chemical stability and weldability are good, cerium ion prevents the function of sub-tin oxidation and hydrolysis, process stabilizing in addition simultaneously.In background technology, in domestic disclosed mensuration tin-cerium alloy electroplating solution, the method for cerous sulfate content has four kinds at present: the first is to adopt highly basic precipitate and separate-EDTA volumetric method; The second is to adopt cupferron precipitate and separate-azo III photometry; The third is to adopt the direct photometry of chlorophosphonazo-ma; The 4th kind is at " HCl-HNO by tin-cerium alloy electroplating solution ₃" heated oxide, to emitting white cigarette, makes the Ce in plating solution in nitration mixture ³⁺, Sn ²⁺and organism is all oxidized, cooling after, take phenyl for ortho-aminobenzoic acid as indicator, measure with iron ammonium sulfate standard titration solution.In above four kinds of methods, the operating process of the first, the second, the third method is more complicated, and sense cycle is long, and testing result exists certain error; The 4th kind of method, owing to using HCl-HNO ₃nitration mixture heated oxide, generates insoluble jelly, adds 1+3 hydrochloric acid 30mL and is heated to boiling, and jelly does not dissolve, and adds indicator after cooling, and solution colour, without significant change, exists the inaccurate defect of titration.For overcoming above-mentioned deficiency, realize to cerous sulfate content in tin-cerium alloy electroplating solution fast, accurately detect, the assay method of tin-cerium alloy electroplating solution cerous sulfate content is studied.

Summary of the invention

Technical matters to be solved by this invention is the assay method that a kind of tin-cerium alloy electroplating solution cerous sulfate content will be provided, it adopts certain density perchloric acid, phosphoric acid, nitric acid to carry out oxidation processes to electroplating solution to be measured, take N-phenylanthranilic acid as indicator, with iron ammonium sulfate standard titration solution titration quadrivalent cerium be the content that cerous method is measured cerous sulfate in tin-cerium alloy electroplating solution, this detection method fast and easy, testing result accuracy is high.

The technical scheme that the present invention solves its technical matters employing is that it comprises the following steps:

(1) reagent is prepared

A, perchloric acid (ρ=1.75g/mL);

B, phosphoric acid (ρ=1.69g/mL);

C, nitric acid (ρ=1.46g/mL);

D, iron ammonium sulfate standard titration solution { c[(NH ₄) ₂fe (SO ₄) ₂]=0.02mol/L}, uses front demarcation;

E, N-phenylanthranilic acid indicator solution (1g/L): get N-phenylanthranilic acid 0.10g and be dissolved in the sodium carbonate liquor that 100mL concentration is 2g/L,

(2) draw 5.00mL electroplating solution to be measured, be placed in 250mL conical flask,

(3), in exhausting cabinet, in the 250mL conical flask that electroplating solution to be measured is housed, adding successively density is perchloric acid 5mL, the phosphatase 11 0mL that density is 1.69g/mL, the nitric acid 5mL that density is 1.46g/mL of 1.75g/mL, shake up,

(4) in exhausting cabinet, 250mL conical flask is carefully heated, in the time being full of the dense white cigarette of perchloric acid in conical flask, continue heating, while being back to the bottle end of conical flask to the dense white cigarette of perchloric acid, stop heating, take off conical flask and be cooled to room temperature,

(5) add 50mL water in cooled 250mL conical flask, shake up,

(6) in 250mL conical flask, add the N-phenylanthranilic acid indicator solution that 3 concentration are 1g/L, the iron ammonium sulfate standard titration solution that is simultaneously 0.02mol/L by concentration immediately carries out titration to the solution in conical flask, disappear for terminal to solution in conical flask is red

Cerous sulfate content is calculated as follows:

$\mathrm{Ce}{\left({\mathrm{SO}}_4\right)}_2(g/L)=\frac{c\×v\×332.24}{5}$

In formula:

The actual concentrations of c-iron ammonium sulfate standard titration solution, unit is mol/L;

V-titration consumes the volume of iron ammonium sulfate standard titration solution, and unit is mL;

Molal weight { M[Ce (the SO of 332.24-cerous sulfate ₄) ₂], unit is g/mol.

The present invention compares produced beneficial effect with background technology

1, the present invention adopts certain density perchloric acid, phosphoric acid, nitric acid to carry out oxidation processes to electroplating solution to be measured, take N-phenylanthranilic acid as indicator, measure the content of cerous sulfate in tin-cerium alloy electroplating solution by the method for iron ammonium sulfate standard titration solution titration, can avoid traditional detection method operating process complexity, sense cycle is long, oxidation does not reach the deficiency of requirement, while guaranteeing titration, the variable color of solution terminal is sensitive, make technician's adjustment tank formula of liquid in time, effective guarantee tin-cerium alloy quality of coating.

2, this assay method is simple, and testing process is convenient, fast, environmental protection, and completing one-time detection only needed about 30 minutes, and testing result is accurately consistent, and expense cost is low.

Embodiment

With regard to specific embodiment, the invention will be further described below.

An assay method for tin-cerium alloy electroplating solution cerous sulfate content, it comprises the following steps:

(1) reagent is prepared

A, perchloric acid (ρ=1.75g/mL);

B, phosphoric acid (ρ=1.69g/mL);

C, nitric acid (ρ=1.46g/mL);

D, iron ammonium sulfate standard titration solution { c[(NH ₄) ₂fe (SO ₄) ₂]=0.02mol/L}, uses front demarcation;

E, N-phenylanthranilic acid indicator solution (1g/L): get N-phenylanthranilic acid 0.10g and be dissolved in the sodium carbonate liquor that 100mL concentration is 2g/L.

(2) draw 5.00mL electroplating solution to be measured, be placed in 250mL conical flask.

(3), in exhausting cabinet, in the 250mL conical flask that electroplating solution to be measured is housed, adding successively density is perchloric acid 5mL, the phosphatase 11 0mL that density is 1.69g/mL, the nitric acid 5mL that density is 1.46g/mL of 1.75g/mL, shakes up.

(4) in exhausting cabinet, 250mL conical flask is carefully heated, in the time being full of the dense white cigarette of perchloric acid in conical flask, continue heating, while being back to the bottle end of conical flask to the dense white cigarette of perchloric acid, stop heating, take off conical flask and be cooled to room temperature.

(5) add 50mL water in cooled 250mL conical flask, shake up.

(6) in 250mL conical flask, add the N-phenylanthranilic acid indicator solution that 3 concentration are 1g/L, the iron ammonium sulfate standard titration solution that is simultaneously 0.02mol/L with concentration immediately carries out titration to the solution in conical flask, to red disappearance of solution in conical flask be terminal.

Cerous sulfate content is calculated as follows:

$\mathrm{Ce}{\left({\mathrm{SO}}_4\right)}_2(g/L)=\frac{c\×v\×332.24}{5}$

In formula:

The actual concentrations of c-iron ammonium sulfate standard titration solution, unit is mol/L;

V-titration consumes the volume of iron ammonium sulfate standard titration solution, and unit is mL;

The molal weight of 332.24-cerous sulfate M[Ce (SO4) 2] }, unit is g/mol.

Claims (3)

1. an assay method for tin-cerium alloy electroplating solution cerous sulfate content, is characterized in that it comprises the following steps:

(1) reagent is prepared

A, perchloric acid (ρ=1.75g/mL);

B, phosphoric acid (ρ=1.69g/mL);

C, nitric acid (ρ=1.46g/mL);

D, iron ammonium sulfate standard titration solution, use front demarcation;

E, N-phenylanthranilic acid indicator solution: get N-phenylanthranilic acid and be dissolved in sodium carbonate liquor;

(2) draw 5.00mL electroplating solution to be measured, be placed in 250mL conical flask;

(3), in exhausting cabinet, in the 250mL conical flask that electroplating solution to be measured is housed, adding successively density is perchloric acid 5mL, the phosphatase 11 0mL that density is 1.69g/mL, the nitric acid 5mL that density is 1.46g/mL of 1.75g/mL, shakes up;

(4) in exhausting cabinet, 250mL conical flask is carefully heated, in the time being full of the dense white cigarette of perchloric acid in conical flask, continue heating, while being back to the bottle end of conical flask to the dense white cigarette of perchloric acid, stop heating, take off conical flask and be cooled to room temperature;

(5) add 50mL water in cooled 250mL conical flask, shake up;

(6) in 250mL conical flask, add 3 N-phenylanthranilic acid indicator solutions, simultaneously with iron ammonium sulfate standard titration solution, the solution in conical flask carried out to titration immediately, to red disappearance of solution in conical flask be terminal;

Cerous sulfate content is calculated as follows:

$\mathrm{Ce}{\left({\mathrm{SO}}_4\right)}_2(g/L)=\frac{c\×v\×332.24}{5}$

In formula:

The actual concentrations of c-iron ammonium sulfate standard titration solution, unit is mol/L;

V-titration consumes the volume of iron ammonium sulfate standard titration solution, and unit is mL;

Molal weight { M[Ce (the SO of 332.24-cerous sulfate ₄) ₂], unit is g/mol.

2. the assay method of tin-cerium alloy electroplating solution cerous sulfate content according to claim 1, the concentration that it is characterized in that N-phenylanthranilic acid indicator solution is 1g/L.

3. the assay method of tin-cerium alloy electroplating solution cerous sulfate content according to claim 1, the concentration that it is characterized in that iron ammonium sulfate standard titration solution is 0.02mol/L.