Quantitative detection reagent and detection method for sodium polydithiodipropane sulfonate in acid copper electroplating liquid

The technology of sodium polydithiodipropane sulfonate and detection reagent is applied in the field of analysis and detection of sodium polydithiodipropane sulfonate, which can solve the problems of cumbersome operation process, increased detection cost, corrosion and the like, and achieves good repeatability, Accurate, easy-to-use effects

Active Publication Date: 2020-05-15
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the methods for measuring sodium polydithiodipropane sulfonate include HPLC detection method and ion chromatography pulse amperometry, but these methods cannot be aimed at the detection of acid copper liquids such as electrolytic copper foil, and the required instruments and equipment are expensive, and the operation process It is cumbersome, and most of them can only measure the total amount of sulfonate. At the same time, copper acid solution entering the chromatographic column will cause corrosion, wear out the chromatographic column, and increase the detection cost

Method used

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  • Quantitative detection reagent and detection method for sodium polydithiodipropane sulfonate in acid copper electroplating liquid
  • Quantitative detection reagent and detection method for sodium polydithiodipropane sulfonate in acid copper electroplating liquid
  • Quantitative detection reagent and detection method for sodium polydithiodipropane sulfonate in acid copper electroplating liquid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Step 1, drawing of L-cysteine ​​standard curve:

[0037] (1) Accurately weigh 1.0g of L-cysteine ​​and dissolve it in a 1000mL volumetric flask, and use H 2 PO 4 - -HPO 4 2- Dilute the buffer solution to the mark, and make 1.0g / L L-cysteine ​​stock solution.

[0038] (2) Add the L-cysteine ​​stock solution in 0mL, 1mL, 2mL, 3mL, 4mL, 5mL, 6mL, 7mL (1) to eight 100mL volumetric flasks respectively, and use H 2 PO 4 - -HPO 4 2- Dilute the buffer solution to the scale line, and make 8 kinds of L-cysteine ​​standard solutions, the concentrations of L-cysteine ​​are 0 μmol / L, 82.5 μmol / L, 165.1 μmol / L, 247.6 μmol / L , 330.1 μmol / L, 412.7 μmol / L, 495.2 μmol / L, 577.7 μmol / L.

[0039] (3) Use a pipette to pipette 1 mL of L-cysteine ​​standard solution into a 10 mL colorimetric tube, add 100 μL of chromogenic reagent, dilute to the mark with deionized water, and develop color for 15 min.

[0040] (4) Take the concentration of the standard substance as the abscissa, and...

Embodiment 2

[0055] Embodiment two differs from embodiment one in that:

[0056] Pipette the sodium polydithiodipropanesulfonate electroplating solution to be tested in 1mL embodiment 1 step 2 (c), add 1000 μ L 80 μ mol / L mercaptoacetic acid, 5 mL buffer solution and 150 μ L chromogen, after it fully reacts, measure its The absorbance is calibrated with the L-cysteine ​​standard curve to obtain the content of the total sulfhydryl group and substitute it into the sodium polydisulfide dipropane sulfonate-mercapto group relational formula to indirectly obtain the sodium polydisulfide dipropane sulfonate in the electroplating solution to be measured. content.

Embodiment 3

[0058] Embodiment three differs from embodiment two in that:

[0059] Pipette the sodium polydithiodipropanesulfonate electroplating solution to be tested in 1mL embodiment 1 step 2 (c), add 1500 μ L 80 μ mol / L mercaptoacetic acid, 5 mL buffer solution and 200 μ L chromogen, after it fully reacts, measure its The absorbance is calibrated with the L-cysteine ​​standard curve to obtain the content of the total sulfhydryl group and substitute it into the sodium polydisulfide dipropane sulfonate-mercapto group relational formula to indirectly obtain the sodium polydisulfide dipropane sulfonate in the electroplating solution to be measured. content.

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Abstract

The invention provides a detection reagent and a detection method for detecting the content of sodium polydithiodipropane sulfonate in an acid copper electroplating solution. The used detection reagent comprises a reducing agent, a buffer solution and a color developing agent, and the reducing agent is a reducing reagent for reducing disulfide bonds in the sodium polydithiodipropane sulfonate intosulfydryl. The buffer solution is a buffer solution with the pH value of 8-10. The color developing agent is 5,5'-dithiobis (2-nitrobenzoic acid). The method has the advantages of simple operation, rapidness, convenience, good repeatability and high accuracy. The relative error is about 0.8%-4%, the detection limit is as low as 2[mu]mol / L, and the detection reagent is suitable for real-time monitoring of plating solution components of acid copper electroplating factories and electrolytic copper foil enterprises and stabilizes the product quality.

Description

technical field [0001] The invention relates to the technical field of organic matter detection, in particular to an analysis and detection method of sodium polydithiodipropane sulfonate in an acid copper electroplating solution. Background technique [0002] Due to its excellent electrical conductivity, thermal conductivity, and plasticity, copper is widely used in the surface of materials, counterbore electroplating, and electrolytic copper foil preparation, especially the current negative electrode current collector copper foil for lithium-ion batteries, which requires a thickness of less than 8 μm. Copper electroplating solution has developed into a mainstream production method. The key to the quality of copper plating lies in the selection of additives in acid copper solution and the formulation of components. An appropriate amount of additives can significantly adjust the growth and performance of the coating, and improve the structure and performance of the coating. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/78G01N21/31
CPCG01N21/78G01N21/31G01N2021/775
Inventor 唐云志师慧娟樊小伟谭育慧刘耀
Owner JIANGXI UNIV OF SCI & TECH
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