Trem Williams wrote:

> Hi Mike,
>
> Here's something else to throw us off.  I just had several samples measured
> for PPM by a lab using the atomic absorption process.  I asked them if they
> digested the CS before running the test.  Answer was "yes".  I asked them to
> run the test on each sample two times; once with and once without digestion.
> I did this because another lab had done the same tests for me without using
> digestion.  I was interested in seeing what differences would be uncovered.
> Well, the results were strikingly different.  With digestion (and by that I
> mean boiling in aqua regia) the PPM in 16 ounces of water using constant
> current production was about 3.5 PPM per hour.  The highest reading sample
> was 35 PPM after running the generator for 10 hours and the reading for 5
> hours was 18 PPM.  Pretty straightforward I thought but then the undigested
> samples threw me off.  They were 19 PPM for the 10 hour run and 11 PPM for
> the 5 hour run.  These readings were still proportionate to time but only
> about 54-58% of the digested readings.  The chemist told me that you cannot
> get accurate readings without complete digestion.  I wonder how many of
> those using spectrophotometers, such as "Ole Bob" digest their samples.  He
> told me once that he bleached the samples but didn't mention digestion.
>

We always digest our samples.

> Since I really don't know that much about the process, I can't speak with
> much authority but I suspect that those using spectrophotometers would also
> get much different readings between digesting and not digesting their
> samples.  I'd be interested in hearing reports from those who have them if
> they could run the tests both ways.
>
> As a side note, I tried a Hanna instrument silver colorimeter and was
> disappointed.  One used 4 different chemicals to react with the sample and
> the blank and then measured the color difference.  When I ran the unit to
> test undigested CS, the reading was always zero PPM.  In order to see if the
> unit was operable, I dissolved 1 mg silver in nitric acid by boiling and
> then added it to enough distilled water to get a 1 PPM standard solution.
> When I tested this sample, the unit did give a reading but it was very low
> (about 30% of the actual PPM).  I sent the unit back because it was not
> working accurately enough with my home made standard and didn't work at all
> with the undigested CS.
>

Yes, I bought a Hanna first also, and got results of about 20% to 30% of the
true ppm.  It is sitting on a shelf here somewhere, never to be used again.

> Afterward, I was told by the lab that did my last tests that digestion in
> nitric is not good enough.  One should use aqua regia for complete
> digestion.  So the upshot of all this to me was that you have to digest
> completely to get an accurate reading of the total amount of silver in the
> dispersion.  It is possible I could have gotten better results from the
> Hanna unit if I had used aqua regia but I didn't know it at the time.

Nitric should be good enough if you boil it dry, then add nitric a second time
and heat to boiling.  That is what I do.

Marshall


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