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2025

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11

Determination of ferric iron content in etching solution by fully automated potentiometric titration method


I. Introduction

Etching solutions are liquids that carve materials by eroding them. Currently, there are six main types of etching solutions in use: acidic copper chloride, alkaline copper chloride, ferric chloride, ammonium persulfate, sulfuric acid/chromic acid, and sulfuric acid/hydrogen peroxide etching solutions. The etching rate of ferric chloride etching solutions is mainly affected by etching temperature, hydrochloric acid content, and iron ion content. The Fe content in the etching solution primarily affects the etching rate; as the concentration gradually increases, the etching rate for copper increases accordingly. However, when the Fe content exceeds a certain concentration, the etching rate decreases due to increased solution viscosity. This experiment used a JH-T6 fully automatic potentiometric titrator from Shanghai Jiahang to determine the endpoint based on the potential jump point, measured the trivalent iron content, and verified the feasibility of the experimental scheme.

II. Instruments and Reagents

2.1 Instruments

JH-T6 fully automatic potentiometric titrator, composite platinum electrode, analytical balance, etc.

2.2 Reagents

Potassium iodide, hydrochloric acid (1+3) solution, 0.1 mol/L sodium thiosulfate standard titrant

III. Experimental Methods

3.1 Experimental Procedure:

Accurately weigh 0.5 g (accurate to 0.0001 g) of the sample to be tested into a titration vessel. Add 30 mL of deionized water, 3 g of potassium iodide, and 20 mL of (1+3) hydrochloric acid solution sequentially. Shake well, seal the vessel, and place it in the dark for 30 min. After standing, place the titration vessel on the titration stage, turn on the stirrer, and titrate with a known concentration of c=0.1017 mol/L sodium thiosulfate standard titrant until the potential jump endpoint. Record the titration volume. Repeat 3 sets, and simultaneously perform a blank experiment under the same conditions.

3.2 Instrument Parameters

Instrument parameters are shown in Table 1:

Table 1 Titrator Parameter Settings

Titration type: Dynamic titration; Method name: Determination of ferric iron in etching solution
Burette volume:

10mL

Sample measurement

g

Working electrode: Composite platinum electrode; eference electrode: None
Stirring speed:

7

Pre-stirring time:

5s

Electrode equilibration time:

4s

Electrode equilibration potential:

1mv

Titration speed: Standard; Pre-titration equilibration potential:

6mv

Display unit:

mv

Finished volume:

20mL

Pre-titration addition volume: 0 (can be set appropriately); Minimum addition volume:

0.02mL

Potential jump: 500mV

500mV

Pre-control mV value:

0

Pre-control mV value: 0

16.219

Result unit:

%

Titrant name:

Na2S2O6

Theoretical concentration:

0.1017

 

IV. Results and Discussion

4.1 Experimental Results

The samples were tested, and the experimental results are shown in Table 2:

Table 2 Content Test Results

Sample Name c(Na2S2O6) Sample Amount (g)

Blank Volume V0 (mL)

Titration Volume V1

(mL)

Content (%) Average Content (%)

RSD(%)

 

Ferric chloride solution

 

0.1017

0.4734

 

 

0.03

12.502

43.456

 

43.421

 

0.2563

0.4329

11.449

43.510

0.4741

12.475

43.296

 4.2 Titration Spectrum

4.3 Conclusion

This test used a fully automated potentiometric titration method to determine the content of ferric iron in the etching solution. Instrumental judgment reduced human error and greatly improved the accuracy of the experiment. Therefore, potentiometric titration is a good choice for detecting this type of sample.

Keyword:

automated potentiometric titration