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Ted Mooney, P.E. RET
Pine Beach, NJ
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for Metal Finishing 1989-2024
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Analysis of Pickling Bath
Q. We have to analyse a Pickling Bath solution, consisting of:
1. ~ 550 g/l Nitric Acid (53%) and
2. ~ 150 g/l Turco 4104 (a commercial product which consists of: ~ 10 to 20% acetic acid
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1. For the analysis of Nitric Acid, the analysis method given by the manufacturer is based (a)on the titration of the sample with 0.5N NaOH
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to pH 4 and (b) on the formula, which is extracted from the std equation N1XV1=N2XV2. Following this method we find concentration of Nitric Acid much higher than the actual one (for example, we prepared above pickling solution in lab and instead of 550 g/l Nitric Acid (53%), we found 503 g/l. Is there any other suggestion for an accurate and precise method for the Nitric acid evaluation?
2. We are waiting the detailed analysis method of the commercial product Turco 4104 from the manufacturer. Is there a chance that someone has used and analysed this product? It seems that it is based on the fluoride concentration of the solution.
aerospace - Tanagra, Viotiaw, GREECE
2005
A. A guess on the nitric acid is that you are using a slightly weaker makeup acid than was intended. If you look in a scientific supply catalogue, you will see that there are many different concentrations other than red fuming which very few people would use. Commercial nitric in the USA is always a couple of baumé weaker than analytic grade acid. Test a sample of your raw acid in the lab. Bet that you find it weaker than expected.
James Watts- Navarre, Florida
A. The method I use for analyzing nitric acid concentration is as follows:
1 mL of sample
Approx. 50-100 mL DI water
Add a few drops of phenolphthalein
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Titrate with 0.5 N sodium hydroxide
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to bright pink color
mLs x 2.258 = % nitric
I hope this helps.
- Colorado Springs, Colorado, USA
A. Personal opinion, phenolphthalein changes color at too high a pH and is not significantly higher than a pH4 indicator or meter in the titration. The higher pH end point is going to allow precipitation of metals which will indicate that the solution is much stronger than actual.
James Watts- Navarre, Florida
Q. Dear James and Barb,
Thanks a lot for your response.
1. I would like to make a correction on the quantities in my original text. The std solution we prepared in lab was 450 (and not 550) g/l Nitric Acid (53%) PLUS 150 g/l Turco Nitrad. Analyzing this std we found 503 g/l Nitric Acid (53%).
2. Just yesterday we got a letter from the manufacturer, whom we had asked the same questions. He said that Nitrad contains acid components and that is why the analysis based on the NaOH consumed ends up into a higher value for Nitric Acid. That is, the NaOH consumed gives the total acidity of the pickling solution.
3. We are still therefore waiting/searching for the method of analysis to calculate the only Nitric Acid in the pickling solution.
aerospace industry - Tanagra, Viotias, Greece
2005
A. The answer to this is to be practical.
If you want to analyse and control the "Free" nitric then find a pH indicator that changes somewhere down in the 3-3.5 pH range. Normally you would suggest using a pH meter but as you have acidic fluoride you would wreck your glass probe. If you use a high pH indicator like phenolphthalein you will titrate all your acids including the acetic.
Control analysis of processes like this are only guidelines and don't need to be absolutely accurate.
Make up your process with the amount of x% nitric and if it works well, analyse it by your method and then maintain it at that concentration.ie if you make it up at 20% nitric and this analyses with a titre of 25ml and it goes down to 20ml after use, you have used up 20% of what you put in in the first place and that needs to be replaced. When you add this of course it will never be the full amount because of dilution.
Geoffrey Whitelaw
- Port Melbourne, Australia
A. Try using Thymol Blue indicator. pH 1.2 Red to pH 2.8 Yellow. Nitradd test from the manufacturer is unreliable. It is only reliable for the initial makeup. Once the solution is introduced to metals (Ti, Al, etc.), the fluoride ions form complexities and detected through ISE procedures (which the manufacturer will recommend). Fluoride complexities are useless in the pickling, descaling of metals.
Let me know if the indicator helps.
Florida
Dear Mr. Whitelaw,
We prepared std solution of Nitric and Nitrad and we found out that the Nitric Acid is given at a pH of 3.2. We will use this pH point for the determination of Nitric in the production solutions, even though the last ones will have different matrix than the std.due to metals diluted, and other probable impurities. Do you think the difference will be important? Thanks a lot for your suggestions.
Dear Mr Yang,
We tried the Thymol Blue indicator on a std solution of Nitric and Nitrad, bu we do not have repeatable results due to non-clear end point. Working with pH 3.2 as end point gives much more repeatable and accurate results. Thanks a lot for your suggestions.
aerospace industry - Tanagra Viotias, GREECE
2005
Q. We are preparing the nitric acid and ammonium difluoride bath for pickling bath let me know how to analysis.
Prakash gemployee - India
October 27, 2010
Hi Prakesh.
Please try you best to frame your question in terms of what has already been offered. I'm afraid that starting over won't move us forward ... in fact, it is often the kiss of death, sealing the end of a thread :-) Thanks!
Regards,
Ted Mooney, P.E.
Striving to live Aloha
finishing.com - Pine Beach, New Jersey
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