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Cobalt & nickel analysis -- A.A., ICAP/MS, or colorimetric
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A.A. = atomic absorption spectrometry
ICAP/MS = Inductively Coupled Plasma / Mass Spectrometry
CBN = cubic boron nitride
Current postings:
May 26, 2022Q. We have a small plating shop having anodizing as one of the processes. We are doing black electrolytic coloring using cobalt acetate, nickel sulphate, boric acid and 5 sulpho salicylic acid.
We are not able to analyze cobalt and nickel metal content separately in solution for replenishment purpose. Please suggest suitable analytical method.
- Gujarat India
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Closely related Q&A's, oldest first:
2000Q. Hey Everybody,
Wendt Dunnington makes Diamond and CBN tooling and we electroplate nickel (from Watts and Sulfamate baths) to hold the super abrasives in place. In a R&D mode we are adding Cobalt (1000 to 3000 ppm range)to the nickel chemistry. A low cost analysis for Cobalt in the presence of Nickel would be very helpful. Any ideas?
Thanks,
Fred Mueller, CEFWendt Dunnington - Royersford, Pennsylvania
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"Atomic Absorption Spectrophotometry"
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A. Nickel and cobalt are so close to identical That a cheap method is probably not possible. Atomic Absorption and possibly ICAP/MS may be necessary.
James Watts- Navarre, Florida
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2000
A. As long as the Ni/Co ratio is not more than a few hundreds, you should be able to do a colorimetric analysis based on formation of cobalt thiocyanate and its extraction into an organic phase. You will need a simple spectrophotometer (2K) and, preferably, a simple centrifuge (about 0.5K).
Another option I am aware of is potentiometric titration with potassium ferricyanide in the presence of ammonia. Worth trying if you have the equipment.
Emanuel I. CooperIBM - Yorktown Heights, New York
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2004
Q. I am working on a method to Analyze Cobalt in a nickel sulfamate bath I have tried linear, nonlinear, and matrix addition calibrations. I have also try matrix matching I have gotten good result however I am getting about 200 to 300 ppm less than the outside lab analysis. Can I get any suggestion on what to try next.
David MorrisonQC chemist - Titusville, Pennsylvania, USA
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"Atomic-Absorption Spectrophotometry" A. Are you using the same type of AA? Flame, Graphite Furnace or ICP-MS? It will make a difference. You might try using a standard from the same lot number as your outside contract lab does. All certified standards are not equal, despite certification. James Watts- Navarre, Florida ^ 2004 A. David, You may have to face the possibility that you're right! One error would be not diluting the sample & standard to the linear range for Cobalt, in which case any readings below the concentration of the standard (SOP) would read too high. Another error would be to choose a frequency for Cobalt measurement at which Nickel also has minor absorbance, again resulting in a high reading. Create a test sample of Nickel Sulfamate bath with a known measured quantity of Cobalt, have both machines test it. Craig HaseltineC&L Equipment Inc - St Charles, Illinois, USA ^ |
2004
Q. I am using nonlinear Direct addition on an AAnalist 200 with a wavelength of 240.73 nm I use a diluted Standard Nickel Sulfamate solution for the Blank and standards trying hard to eliminate any matrix effect. A have done a solution multiple times and had close numbers. I have even changed my dilutions and still came up pretty good. The only thing that I noticed is the higher the cobalt level the closer I get to them. I use a 1 ppm, 2.5 ppm, 5 ppm, and a 10 ppm. standards the Absorption of the 10 ppm is about .35 and 1 ppm is about .049 ppm I try to keep the sample as close to 5 ppm as possible. I guess I will track my number versus theirs and see what changes.
David Morrison [returning]- Titusville, Pennsylvania, USA
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