HPLC (High Performance Liquid Chromatography) analysis method for sodium 3,3'-dithiodipropane sulfonate

Abstract

The invention discloses a HPLC (High Performance Liquid Chromatography) analysis method for sodium 3,3'-dithiodipropane sulfonate and belongs to the technical field of analysis. The HPLC analysis method is characterized in that a high performance liquid chromatograph with an ultraviolet detector is used for determining; octadecyl silane is taken as a filling column, the size of a chromatographic column is 250mm (length)*4.6mm (inner diameter) and the grain size is 5 microns; methyl alcohol and a buffer solution in volume ratio of (0-50):(100-50) is taken as a flowing phase; the detection wavelength is 190-330nm, and the column temperature is at 10-60 DEG C; the speed of the flowing phase is 0.3-1.2mL / min; the feeding size of a sample is 20 micro liter; the buffer solution contains 0.17mol / L acetic acid, 0.142mol / L triethylamine and ultrapure water. The content of sodium 3,3'-dithiodipropane sulfonate in a to-be-detected sample can be quickly and accurately measured according to a standard curve established via a standard solution; the determination result error is small; the repeated operability is strong; the precision is less than 2.8%; the recovery rate is 96.7%-99.3%; the HPLC analysis method can be widely applied to the production process detection and product quality detection for industrial sodium 3,3'-dithiodipropane sulfonate.

Description

technical field [0001] The invention relates to the technical field of analysis, in particular to a high-performance liquid chromatography analysis method for sodium polydithiodipropane sulfonate. Background technique [0002] Sodium polydisulfide dipropane sulfonate, the product code is SPS, mainly used in electroplating acid copper plating. As an acidic copper plating intermediate, it is the main additive in copper plating additives, which can refine the crystallization of the plating layer and effectively increase the current density. In the entire acid copper brightener market, this product is in great demand and has excellent application effects. In the copper plating additive formula, the amount of SPS added is related to the application effect of the formula, light output speed and stability, so the SPS content is an important indicator for product quality control, and it is very necessary to accurately determine its content. [0003] In the traditional methods for ...

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Problems solved by technology

[0003] In the traditional methods for detecting sulfur groups, most of them use strong oxidants to oxidize sulfur-containing compounds into sulfone compounds. This reaction method has strict requirements on reaction conditions, such as temperature, amount of reactants, and reaction time, and has poor selectivity. The results have large errors and cannot be used to accurately determine the concentration of compounds

[0004] Magazine " chromatography ", the article that the 17th volume, the 6th issue of 1999 publishes: " HPLC method is measured simultaneously the multiple organic additives in acidic copper-plating brightener ", has reported and selects phenyl chromatographic column, mobile phase is: V (methanol ): V (water)=30:70, flow velocity is 1.5mL / min, under the condition that detection wavelength is 210nm, 2-mercaptobenzimidazole, ethylenethiourea, sodium polydithiodipropanesulfonate are separated, and simultaneously Determination of their mass concentration, this method uses a phenyl chromatographic column, and the mobile phase is methanol and water. Although several substances are separated, the determination time is long and the content determination is not accurate enough

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