2581-34-2 Purity
98%
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Specification
The quantitative analysis of bis(sulfopropyl) disulfide (SPS), a brightener component in acidic copper plating baths, presents a real challenge due to the complex chemical matrix containing high amounts of Cu(II) ions and sulfuric acid as well as other organic additives and decomposition products. A new ion-pair chromatography method has been developed that allows the direct analysis of micromolar amounts of SPS in plating bath samples without the need for sample pretreatment. The addition of tetra-N-methylammonium cations as ion-pair agents in the methanol-sulfuric acid-water eluent increases the retention time of anionic SPS on the C column sufficiently to separate this compound from Cu(II) ions and additive byproducts.
SPS calibration was performed by ion-pair chromatography over a relevant concentration range between 1.4 × 10-5 and 1.41 × 10-4 M. However, it was determined that the linear response range of the calibration plot extends up to 1.7 × 10-3 M. Higher SPS levels were not evaluated in this study. The lowest SPS level observed in the bath was around 1.7 × 10-5M. Therefore, it was not necessary to extend the calibration plot below the 1.4 × 10-5 M level for this study, which is already well below the SPS concentration recommended for high-quality copper filling with the Shipley-Ronal Electraplate bath. The calibration study involved eight SPS concentration levels and nine replicates. The calibration design was chosen so that evenly distributed concentration levels existed in the range between 1.4 × 10-5 and 8.5 × 10-5 M. The design was completed for the 1.13 × 10-4 and 1.41 × 10-4M levels. For each replicate analysis of these calibration standards, a fresh stock solution of aqueous SPS was prepared to avoid any decomposition of the compound during the long time taken for this study and to include all possible sources of error in the preparation of the calibration solutions. The concentration of SPS was as close to the nominal value as possible, but due to the difficulty in weighing small amounts of SPS, the concentration for each replicate was not exact. For each calibration solution, two replicate injections were performed, and the average of the measured peak area values was used as the response for each concentration level and each replicate.
The interaction of the functional additive SPS (bis(sulfopropyl) disulfide) with polyethylene glycol (PEG) in the presence of chloride ions was investigated jointly by time-of-flight secondary ion mass spectrometry (TOF-SIMS) and cyclic voltammetry measurements (CV). The surface coverage of PEG, thiolates, and chlorides was evaluated and discussed in terms of their electrochemical inhibition/acceleration abilities. The effects of the conformations of the left/trans thiolate molecules and around CC and CO of PEG on the electrochemical performance were discussed. The contribution of the hydrophobic interaction of -CH-CH- of PEG with chloride ions was only slightly reduced after the addition of SPS, while the contribution of the Cu-PEG adduct was greatly weakened. SPS and PEG exhibited a remarkable synergistic effect through significant co-adsorption. The results showed that the inhibition ability of PEG, which depends on the formation of stable Cu-PEG adducts (determined as CHOCu and CHOCu), was significantly reduced after the addition of SPS. The major role of thiolate molecules adsorbed on the copper surface in reducing the inhibitory capacity of PEG relies on the effective capture of Cu ions, thereby reducing the available copper ions for the PEG ether oxygens.
TOF-SIMS data show that the addition of SPS leads to the co-adsorption of SPS and PEG, while the ratio of PEG surface coverage to thiolate surface coverage decreases as a function of SPS concentration. However, a significant deviation in the distribution of PEG/thiolate was observed for 0.5 ppm SPS. Moreover, the PEG/thiolate ratios were similar for 10 and 15 ppm SPS. Second, a significant reduction in the number of C2H4O2Cu+ and C3H6OCu+ adducts was observed after the injection of SPS. This implies that the thiolate molecules are able to effectively capture Cu2+ ions from the air oxygen environment of PEG. Since we did not observe a proportional reduction in CHCl+, this implies that the sparse conformation of PEG around C-C is significantly preserved. Based on this observation, we can conclude that the distance of O-O ether atoms also remains unchanged. For this reason, the competition between SPS and PEG for capturing Cu2+ ions relies on the higher affinity and flexibility of the sulfonate groups of the thiolate molecules.
The molecular formula is C6H12Na2O6S4.
The synonyms are 27206-35-5, 1-Propanesulfonic acid, 3,3'-dithiobis-, disodium salt, disodium;3-(3-sulfonatopropyldisulfanyl)propane-1-sulfonate, and Di(thiopropane sodium sulfonate).
The molecular weight is 354.4 g/mol.
The parent compound is 1-Propanesulfonic acid, 3,3'-dithiobis-.
The component compounds are 1-Propanesulfonic acid, 3,3'-dithiobis- and Sodium.
It was created on August 8, 2005.
It was last modified on October 21, 2023.
The IUPAC name is disodium;3-(3-sulfonatopropyldisulfanyl)propane-1-sulfonate.
The InChI is InChI=1S/C6H14O6S4.2Na/c7-15(8,9)5-1-3-13-14-4-2-6-16(10,11)12;;/h1-6H2,(H,7,8,9)(H,10,11,12);;/q;2*+1/p-2.
The CAS numbers are 27206-35-5 and 1437780-90-9.