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Letter 4072
Analysis of Sodium Sulphate in Nickel
Baths.
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Hello all,
Does anyone have the analytical procedure to analyze a
Watts Nickel plating bath for Sodium Sulphate content ?
Thanks in advance,
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Khozema
Vahanwala
Automaxx
Bangalore, Karnataka, India
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First of two simultaneous responses--
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What you really want to test for is sodium - the bath is
full of sulfate ion from the nickel sulfate.
There is a selective ion probe for sodium. Special
techniques may need to be used because the solution has a
lot of dissolved material and some of the components may be
interferences.
The other applicable method is flame photometry, where
the yellow sodium emission is measured and used to
quantitate the Na.
I'm sorry, but there's no simple titration or color
method, to the best of my knowledge.
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Dave Wichern
- Bronx, NY, USA
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Second of two simultaneous responses--
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Hello K Vahanwala,
To find the Sulfate: take a 10 ml sample of the bath and
(to be added in the order listed) about 100 ml DI water, 5
ml 50% HCl, 25 ml Ba(NO3)2 solution (about 15 grams of
reagent grade barium nitrate in about 70 ml of DI water)the
sulfate will precipitate continue adding drop wise more
barium nitrate until no more precipitate is formed, allow
solution to stand 4 hours, filter in tared Gooch crucible,
wash precipitate with DI water, dry in oven at 110 degrees
C., cooling in desiccator (dry to constant weight), and
weigh. SO4 (oz/gal) = (weight in grams of precipitate) X
5.488
Now, find the Nickel content and Chloride content. In
order to find the Nickel AS Chloride then Nickel AS Sulfate,
the balance of the Sulfate would be present as the Sodium
salt.
Regards,
Fred Mueller, CEF
- Royersford, PA
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Dear Mr Fred and Mr David.
Thanks for the immediate response. Much appreciated.
Pardon my ignorance but is it possible to briefly explain Flame
Photometry ? I am also lost as to " tared Gooch Crucible" . Is there
any other colloquial name or description for it?
Thanks again,
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Khozema
Vahanwala
Automaxx
Bangalore, Karnataka, India
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Flame photometry is done with a special instrument, a photometer.
The sample is sprayed into an oxygen/hydrogen flame, and the light
resulting from the emission of the sodium ions in the flame (in this
case yellow) is measured with a photosensor. The intensity of the
emission is proportional to the sodium concentration.
It's an expensive instrument - an outside lab would likely have
one though.
Dave Wichern
- Bronx, NY, USA
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Hey K. Vahanwala,
A Gooch Crucible is a small porcelain filter that (can be
used with a paper or glass filter disc) retains the
precipitate so that is can be weighed. It is used with a
vacuum flask (pulling a vacuum speeds the filtration) and
rubber gasket to make a seal. It can be reused after
cleaning with the right acids and bases (safety first, lots
of concerns, like were the vacuum pump exhausts). After
cleaning the Gooch Crucible is dried in an oven at 110
degrees C. (this drives off the water and brings the
crucible to its constant weight or lowest weight). Cooling
and storing the crucible in a desiccator prevents the
reabsorption of water moisture. We have weighed the crucible
(tared) and will subtract out the crucible to find the
weight of the precipitate. Lab products can be found
on-line.
Regards,
Fred Mueller, CEF
- Royersford, PA
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You are interested in Sodium and not in sulfate. Well the easiest
way to check sodium is by Atomic Absorption.
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Sara
Michaeli
chemical process supplier
Israel
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