Analytical tool to measure saccharin and butynediol concentrations in Nickel sulfamate electroforming bath

The best way is probably to use HPLC; I got saccharin analysis down to about 10 ppb detection limit and 1,4-butyne diol down to about 100 ppb. I cannot recall if I used a conductivity or UV detector, but I used acetyl nitrile as a solvent and the equipment was made by Dionex. The problem is that the concentrations are very low in the electroforming bath, but the nickel levels are very high, so high dilutions need to be used. I know you can use solvent extraction (chloroform) for saccharine, but do not know for butyne diol, so perhaps a technique could be developed around that methodology...

The method that I use is based upon proprietary reagents so I won't give it to you. It is, however, based upon information available from the suppliers of sodium saccharine and 1,4 butynediol. I would suggest you get the information from them for relatively simple wet titrations.

Julio,
I have a procedure that will work for you. You need to determine the "factor". This you do by analyzing a known quantity of the sodium saccharin in solution.

1. Pipet a 50 ml sample of the nickel solution and pour into a pear shaped separatory funnel.
2. Add 2 ml concentrated Hydrochloric Acid. Shake well for 1 to 2 minutes. Then add 25 ml Ethyl Acetate. Shake well again for 2 to 3 minutes and allow to settle
3. Run lower nickel layer off into a beaker [beakers on eBay or Amazon [affil links] . (retain for further use). Wash ethyl acetate layer with DI water by running the water down the side of the separatory funnel. Allow to separate (do not shake) and run off and discard lower layer.
4. Repeat washing a second time. Check the ph of the wash water being drawn off (should be about 4.5) Transfer ethyl acetate to a 250 ml Ehrlenmeyer flask
5. Put retained nickel layer into separatory funnel. Extract and wash as before.
6. Combine both extractions in the same flask. Add 10 ml methyl alcohol and 1 ml bromocresol purple ⇦this on eBay or Amazon [affil links] Indicator. Titrate to a blue endpoint with 0.1N Sodium Hydroxide ⇦this on eBay or Amazon [affil links] .
7. Using you standard calculate the sodium saccharin concentration.

(This procedure adapted from that used to measure some nickel stress relievers/carriers).

Thanks Dave,

Indeed there are analytical techniques and even standards for saccharine in the food industry but the ones I found use HPLC, as suggested by Trevor.
I look for something less expensive, in terms of equipment investment.
The bromine lead for butynediol can be investigated...
Potentiometric titration is another lead that we investigate...but most likely we won't be able to measure both compounds at the same time, we will need to extract one of them.
We have contacted our product suppliers as suggested by Gene, but so far no relevant answer from them...
So we keep on searching...