Sulfur Content in Nickel Plating

A. I have analyzed the S contents in electroplated Ni alloy by EPMA and Elemental Analyzer(CHNS). I think it was satisfactory. The S contents was about 0.1 wt%.

A. I would think that your best bet is to plate a foil, being careful to maintain the same current density and plating parameters, then get the foil assayed for sulfur. Our lab uses a Leco low sulfur analyser to determine the sulfur level in nickel.

A. Alan,

We have our Sulfamate nickel bath analyzed monthly for "P". The method that works for us is EDX. I'm assuming you could do the same for "S". The report out will have a graph of your deposit.

Good Luck,

A. Hello Mr. Mahalingam,

I ran an ICP-OES for AGES looking for metals in water and sediment, never Sulfur, but a quick internet search led me to this article where it was successfully quantified in Stainless steel. Perhaps this will be a good place to begin your search:

http://chemetal-journal.org/ejournal5/CMA0105.pdf

Note in particular that there is a section about sample preparation by dissolving in mixed high-purity acids. At our lab, we always purchased our digestion acids in the form of "Trace Metals Analysis Grade", which is cleaner than ACS Reagent Grade.
Don't forget that any time you are setting up quality control for something that has been digested, you must run a digestion blank consisting of the exact digestion solution processed at the same time and under the same conditions as your samples, plus a matrix interference sample which is a duplicate of a sample that has had a known quantity of your element of interest added to it. It is perhaps overcautious, but still wise, to run fortified samples where a standard has been added before, and another one where it has been added after, digestion.
Hope that helps even a little to get you pointed in the right direction!

A. Hi Vignesh. Are you using sulfurized anodes? Are you adding organic brighteners to the bath? Is zero stress critical, or is stress level not critical? Are you trying to do high speed plating (significantly greater than 40 ASF)? Thanks! I think topic 18596 will be interesting to you, but I don't know, and we have dozens of threads about sulfur and sulphamate nickel plating :-)

Regards,

A. Hi Rupali. Please tell us what you do and why you want to know. Try to make this an interesting discussion, which will attract readers, by telling us what issues you are having that are motivate you to ask readers to supply you with such data. Thanks!

Regards,

Hi Rupali,

May I know the reason you want to analyze sulfur content in nickel bath? If you aim to know whether sulfur is co-deposited with nickel then you shall apply instrumental analysis (e.g. XPS) on nickel deposit directly as bath solution contains sulfur element in compound form such as sulphate, sulphamate or sulfur containing additive which unlikely co-deposit with nickel.

Regards,
David

A. Yes to the sulfur concentration in the nickel deposit. No, as David says, to the sulfur concentration in the bath. No abstract questions please :-)

Regards,