Replenishing Nickel in solution

[woodjames]

My dopey self let the ph of Nickel get a little too high again. I started noticing a haze on pieces, and rather than realize that it was a ph problem, I just kept adding a little more birghtener, and a little hydrogen peroxide. Finally I checked it with papers and it was much higher than the recommended, I was surprised that it was even plating at all. Oops. I cooked off any of the hydrogen peroxide, and got lucky adding the correct amount of brightener, so now I'm guessing I'm back in spec, and pieces are plating better than ever. I know that anode depletion into solution is not very efficient at higher ph's, so I'm positive that I lost some nickel in solution. It's plating well, but what is the test of the nickel content in the solution? I don't want this to be a problem down the road, if it happens again. Lance? Obviously it's time for a digital ph tester, now that I know how important that part of it is. Thanks in advance!

-Jimmy

[lcaswell]

Here's the procedure - probably more trouble than it's worth.

NICKEL BATH ANALYSIS

A. Determination of Nickel Metal
1. Pipette 2 ml bath sample into a 250 ml Erlenmeyer flask.
2. Add 20 ml of 50% Ammonium Hydroxide and about 1/2 gram of Murexide Indicator and swirl to dissolve.


3. Titrate with 0.1 M EDTA until the color changes from yellowish-green or brown to deep
blue-purple at the end point.

ml of EDTA x 0.39 = oz/gal Nickel Metal
[A-(B x 0.25)] x 4.5 = oz/gal of Nickel Sulfate, 6H2O
A = oz/gal of Nickel Metal B = oz/gal NiCl2.6H20

[woodjames]

Beautiful, thanks much. Seems a little involved, but I'm sure it'll be worth it as I plan on sticking with this. What temperature is the procedure done at?

Thanks again.
Jimmy.

Originally Posted by lcaswell

Here's the procedure - probably more trouble than it's worth.

NICKEL BATH ANALYSIS

A. Determination of Nickel Metal
1. Pipette 2 ml bath sample into a 250 ml Erlenmeyer flask.
2. Add 20 ml of 50% Ammonium Hydroxide and about 1/2 gram of Murexide Indicator and swirl to dissolve.


3. Titrate with 0.1 M EDTA until the color changes from yellowish-green or brown to deep
blue-purple at the end point.

ml of EDTA x 0.39 = oz/gal Nickel Metal
[A-(B x 0.25)] x 4.5 = oz/gal of Nickel Sulfate, 6H2O
A = oz/gal of Nickel Metal B = oz/gal NiCl2.6H20

[almasih86]

sorry for interupting,but ive done your prosedure last time but the color doesnt change at all after add murexide indicator (purple blue)..we used 30% ammonium hydroxide..plz give a feed back..

[NOL4154]

Jimmy,
First, you mention high pH?? 3.8, 4.0, 4.5, 5.0 ? Two, have you ever thought about carbon treatment to your nickel solution? If you kept adding brightner to your nickel solution, add H-peroxide and then boil off the nickle solution. Brightners breakdown and need to be removed with activated carbon. Excess brightner breakdown can cause big headache by making deposit to brittle, spotting, etc... Be very careful in adding excessive brightners to your nickel solution. If you need a procedure for carbon treatment of nickel solution write back

When analyzing a nickel bath you must analyze the following:
1. Total Nickle
2. Nickle sulfate
3. Nickle chloride
4. Boric acid
5. pH

NOL4154



My dopey self let the ph of Nickel get a little too high again. I started noticing a haze on pieces, and rather than realize that it was a ph problem, I just kept adding a little more birghtener, and a little hydrogen peroxide. Finally I checked it with papers and it was much higher than the recommended, I was surprised that it was even plating at all. Oops. I cooked off any of the hydrogen peroxide, and got lucky adding the correct amount of brightener, so now I'm guessing I'm back in spec, and pieces are plating better than ever. I know that anode depletion into solution is not very efficient at higher ph's, so I'm positive that I lost some nickel in solution. It's plating well, but what is the test of the nickel content in the solution? I don't want this to be a problem down the road, if it happens again. Lance? Obviously it's time for a digital ph tester, now that I know how important that part of it is. Thanks in advance!

-Jimmy

[woodjames]

The ph got up over 5 in that particular instance, and the plating looked terrible. Soon after that I did do a carbon treatment, using powdered carbon, I stirred the solution at 170, then let it sit overnight. Then I filtered it back in after cleaning the sludge out of the bottom of the tank. Then I replaced the brighteners at the suggested amount, everything was great. I still get a little bit of pitting-like stardust, so I'll need to add a wetting agent. What do you recommend? Caswell calls for hydrogen peroxide, but does not mention the percentage of concentration.

Originally Posted by NOL4154

Jimmy,
First, you mention high pH?? 3.8, 4.0, 4.5, 5.0 ? Two, have you ever thought about carbon treatment to your nickel solution? If you kept adding brightner to your nickel solution, add H-peroxide and then boil off the nickle solution. Brightners breakdown and need to be removed with activated carbon. Excess brightner breakdown can cause big headache by making deposit to brittle, spotting, etc... Be very careful in adding excessive brightners to your nickel solution. If you need a procedure for carbon treatment of nickel solution write back

When analyzing a nickel bath you must analyze the following:
1. Total Nickle
2. Nickle sulfate
3. Nickle chloride
4. Boric acid
5. pH

NOL4154



My dopey self let the ph of Nickel get a little too high again. I started noticing a haze on pieces, and rather than realize that it was a ph problem, I just kept adding a little more birghtener, and a little hydrogen peroxide. Finally I checked it with papers and it was much higher than the recommended, I was surprised that it was even plating at all. Oops. I cooked off any of the hydrogen peroxide, and got lucky adding the correct amount of brightener, so now I'm guessing I'm back in spec, and pieces are plating better than ever. I know that anode depletion into solution is not very efficient at higher ph's, so I'm positive that I lost some nickel in solution. It's plating well, but what is the test of the nickel content in the solution? I don't want this to be a problem down the road, if it happens again. Lance? Obviously it's time for a digital ph tester, now that I know how important that part of it is. Thanks in advance!

-Jimmy

[NOL4154]

Hello,
Now, after carbon treatment, etc... and added back some brighnters. Did you do some low current dumbing and then increase to high current for a short period of time? This helps the nickle bath to stablize. The peroxide I use is 35% which is the industrial grade (strong oxidizer and handle with care), but you need to add to your nickle bath before heating and adding peroxide. Do some research on the following testing using "Hull cells" for plating. It is a method used through out the plating industrial to trouble-shoot electrolytic plating solutions (copper, brass, nickle, chrome zinc., etc...)
Write back to my e-mail.
nol4154


The ph got up over 5 in that particular instance, and the plating looked terrible. Soon after that I did do a carbon treatment, using powdered carbon, I stirred the solution at 170, then let it sit overnight. Then I filtered it back in after cleaning the sludge out of the bottom of the tank. Then I replaced the brighteners at the suggested amount, everything was great. I still get a little bit of pitting-like stardust, so I'll need to add a wetting agent. What do you recommend? Caswell calls for hydrogen peroxide, but does not mention the percentage of concentration.