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"Watts nickel analysis"



2005

Q. Watts nickel strike analysis? I have a watts nickel strike bath and would like to know how do I check my bath for chloride and sulfates. The PH in the bath is between 9 and 10 I was told to add a 10% sulfuric solution to my bath to lower the PH to 31/2 to 4. I am concerned this may raise the sulfate content too high can someone tell me how to check this and what equipment I need to do this..

John Pragar
plating shop - Statesville, North Carolina
^


2005

A. I'm a little confused. Watts bath is not normally used as a strike. Instead, a low pH high chloride bath known as Woods strike is very common or alternatively a sulfamate acidic bath. Both are used to preplate difficult metals. Please explain more what type of substrates you normally strike with this bath and why are you concerned about sulfate conc.

Guillermo Marrufo
Monterrey, NL, Mexico
^


2005

A. John,

I'm asking right now myself how could you plate with an pH of 9-10? Wasn't it a really rough deposit which you get?
Anyway, here is a procedure to determine the Chloride and sulphate content as Nickel sulphate and Nickel chloride. Depending the amount of chloride and sulphuric acid in your tank you might should choose which (diluted) acid will be necessary:

Determination of Nickel metal:

2 ml electrolyte sample into 300 ml Erlenmeyer flask
dilute with 100 ml DI-Water
then add 10 ml Ammonia 25% and 1-2 Spatulas Murexide Indicator (=>1 g Murexide mixed with 100 g NaCl)
Titrate with 0.1 M EDTA-Solution until color changes from golden yellow to violet.

Calculation:
Usage of EDTA-Solution in ml x 2.936 = content of Nickel metal in g/l.

Determination of Nickel chloride:
2 ml electrolyte sample into 300 ml Erlenmeyer flask
dilute with 100 ml DI-Water
Then add 3 ml 10% potassium chromate solution(=> 10 g potassium chromate dissolved in 100 ml DI-Water)
Titrate with 0.1 N silver nitrate solution from yellow to an onion reddish brown color.

Calculation:
Usage of silver nitrate x 5.945 = content of Nickel chloride in g/l

Calculation of nickel sulphate:
content of Nickel metal in g/l = "A"
content of Nickel chloride in g/l x 0,247 = "B"

(A-B) x 4.786 = g/l Nickel sulphate (NiSO4 x 7H2O)
(A-B) x 4.477 = g/l Nickel sulphate (NiSO4 x 6H2O)

Depending which salt you are using you should choose the factor.

Best regards from the alps and cows

Dominik Michalek
- Mexico City, Mexico
^

----
Ed. note: Thanks so much, Dominik!


2005

A. Like Guillermo, I too am totally confused. I have always believed a nickel strike is a chloride based system with hydrochloric acid (aka Woods Nickel). It operates at a low pH. I have never heard of a Watts strike that operates in the alkali range, although there is a sulphamate strike, but I have no experience of that. It sounds to me like the nickel strike is totally out of balance and needs remaking with nickel chloride (240 g/l) and hydrochloric acid (sg 1.11; 120 ml/l). Perhaps someone can enlighten me on the Watts strike system?

trevor crichton
Trevor Crichton
R&D practical scientist
Chesham, Bucks, UK
^


2005

A. I'm a little confused, too. At a pH of 9-10, almost all of the nickel metal should precipitate out as hydroxide! I'd lower the pH with sulfuric, too.

To check chloride, titrate with a standard silver nitrate solution to the dichromate endpoint. To determine sulfate (although I truly don't think it would be a problem with a Watts bath) you can precipitate the sulfate with excess of barium chloride solution and determine it gravimetrically.

James Totter
James Totter, CEF
- Tallahassee, Florida
^



To minimize search efforts and to offer multiple viewpoints, we combined previously separate threads onto this page. Please forgive any resultant repetition, failures of chronological order, or what may look like readers disrespecting previous responses -- those other responses may not have been on the page at the time :-)



How to do analysis of nickel bath

2005

Q. I want to test and measure the amount of nickel sulphate, nickel chloride and boric acid amount in my nickel plating bath.

Bilman
- Turkey
^


2005

A. Do you have a lab or any lab equipment? Are you a chemist or a lab tech or any plating solution analysis experience?
Most chemical suppliers will be happy to give you a test procedure for the chemical that they sell you. If you are buying proprietary plating bath chemicals, that company will give you an analyses method sheet and an operations sheet for the optimum level for each. Many will even have a sales or tech services person show you how to do it.
I imagine that you could even download it from the internet. There are many many plating analyses books on the market, most using low tech methods. High tech methods equipment would cost over $100,000 for state of the art equipment.
If you use the low tech methods, you will save a huge amount of learning curve time and possibly avoid results that are "off" if you have a qualified person show you how to do it.

James Watts
- Navarre, Florida
^


2005

A. Standard analytical procedures are available in most good electroplating books. Try The Canning Handbook.

trevor crichton
Trevor Crichton
R&D practical scientist
Chesham, Bucks, UK
^



October 8, 2009 -- this entry appended to this thread by editor in lieu of spawning a duplicative thread

Q. chloride in nickel sulfate solutions. need a quick and accurate method for determining chloride in nickel solutions

denise jones
lab personnel - nashville, Tennessee
^


June 3, 2013

Q. Hi. I just want to ask if there's any alternative analysis for Silver Nitrate standard solution? We've been using the said solution for a couple of years but our management would try to look for any replacement for it. Do you have any recommendations/suggestions? Actually, we're using the Silver Nitrate as a reagent in our copper analysis and nickel chloride analysis for a Nickel Sulfate-Chloride-Boric Bath. Any suggestions for an alternative for the said components are very much appreciated. Do you have any?

Mae Magallanes
- Lapu-Lapu City Cebu Philippines
^


August 27, 2014

A. Nickel Bath Analysis
Determination of Nickel metal:
1-take 2 ml electrolyte sample into 250 ml conical flask
2-dilute with 100 ml DI-Water
3- add 10 ml Ammonia 33% and 1-2 Spatulas Murexide Indicator (=1 g Murexide mixed with 100 g NaCl)
4-Titrate with 0.1 M EDTA-Solution until color changes from golden yellow to violet.
Calculation:
Usage of EDTA-Solution in ml x 2.936 = content of Nickel metal in g/l.

Determination of Nickel chloride:
1-take 2 ml electrolyte sample into 250 ml conical flask
2-dilute with 100 ml DI-Water
3- add 3 ml 10% potassium chromate solution(=10 g potassium chromate dissolved in 100 ml DI-Water)
4-Titrate with 0.1 N silver nitrate solution from yellow to an onion reddish brown color.

Calculation:
Usage of silver nitrate x 5.945 = content of Nickel chloride in g/l

Calculation of nickel sulphate:
content of Nickel metal in g/l = "A"
content of Nickel chloride in g/l x 0.247 = "B"
(A-B) x 4.786 = g/l Nickel sulphate (NiSO4 x 7H2O)
(A-B) x 4.477 = g/l Nickel sulphate (NiSO4 x 6H2O)
Depending which salt you are using you should choose the factor.
Determination of Boric Acid:
1-Take 1ml electrolyte sample into 250 ml conical flask
2-add it to 25 mls of "Indicator B".
3- titrate the aliquot against 0.1N NaOH

Calculation:
mls NaOH x 6.184 = Content of [H3BO3]g/l

Sherif Kamel
- Tanta,Egypt
^

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Ed. note: Thanks very much, Sherif!



July 25, 2018 -- this entry appended to this thread by editor in lieu of spawning a duplicative thread

Q. Sir,
How to check sulphate in nickel solution?

Ramkumar bisht
nickel - ludhiana punjab
^

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