Lead testing in bourbon, step by step

[michaelturtle1]

Thought this might interest some other members. With all the talk of lead leaching from ceramic decanters and the fact that I have a Graphite Furnace Auto Analyzer at my lab which is utilized to run leads weekly, I figured I would get off my lazy ass and actually prep a few samples and shoot them through the machine. I have 3 samples from my collection a 1968 Beam, 1970 old Fitz decanter and a 1971 old Fitz figural decanter also there is a 1986 Weller decanter member sent me a sample out of.

[michaelturtle1]

Step #1 is sample prep which consists of an acid digestion of the sample. Basically you add concentrated nitric acid and then cook the sample until most of the water boils off. For this step I started with 10mls of bourbon and then added acid and a bit of DI water to the sample to make it easier to digest without loss from spattering. Once cooked I will adjust the volume to 10mls as to not have any dilution factor.

[michaelturtle1]

Step #2. After digesting the samples are brought back to the original 10ml volume and then centrifuged to remove any particles. Which there was a fair amount of in the older samples..

The rest will follow this evening after the AA run is complete

[ChainWhip]

Subscribed! Fascinating stuff Michael!

[jtgraves]

This is exciting. After so much theorizing around here, I'm really excited to see what your results are from some legitimate testing.

[devillighter]

Very cool - I am extremely excited to see the results!

[michaelturtle1]

Start of step#3 the determination step involves a ton of calibration and calibration checks then throw in a few method blanks and you have 2 hrs into setting up the machine. The basic premise of how the graphite furnace AA works is a small aliquot of sample is heated at 2600°, every metal gives off a specific wave length of light when it burns so the machine has a detector to determine how much of a given wave length of light is emitted..

[Zeke]

Howdy!

Wicked cool! Looking forward to seeing (and reading) about the results. I don't know whether to be thankful or annoyed that we never got any decanters up here in Quebec... This might help me make up my mind.

[michaelturtle1]

The finale, to start lets keep in mind the drinking water limit for lead is 15 ppb. I think that is a fair comparison in a way as you are consuming it in the same way but not nearly consuming as much..

The 1968 Beam 18 ppb, 1970 Old Fitz 21 ppb, 1971 Old Fitz figural 103 ppb and the 1986 Weller 59 ppb.. For shits and giggles I ran a 2012 FrSBLE through and lead was not detected.

[smknjoe]

Thanks a million Mike! All of the levels are much lower than anticipated. Clearly it's safe to drink any of those in moderation. I think I'll be drinking a little Weller this weekend.

[michaelturtle1]

To summarize what I have found, All 4 decanters tested above the federal limit for lead in drinking water. The figural decanter obviously was much higher than the other style decanters, that is the only one I have so a single sample does not make a trend so I would like to do a few more tests to see if that style is generally higher in lead than the others. The newer decanter was 2x's higher than the older decanters, I find this interesting but again I would need to do more analysis to see if this is a trend. In the future I would also like to test a few older bourbons that were not from decanters to see what contribution the distillery itself makes to lead in the samples. Given the amount of piping and copper work in the distilleries it is a fair assumption to say some lead came from the workings of the distillery itself as lead was used in solder flux just as it was used in the glaze flux for ceramic wear.

So in total, the figural decanter will be sparingly consumed but I dont' see much of an issue with the other 3 especially given that these decanters usually contain "special" bourbon that really would never be a daily pour.

[ChainWhip]

Next project for Michael: write a protocol for the teleporter to beam out the lead content whilst leaving the whiskey unmolested ;-)

Seriously cool work Michael!

[MyOldKyDram]

Indeed it was. Very cool and informative experimenting there sir.

[smknjoe]

His findings are also contrary to what others have said about porcelain vs ceramic (although not conclusive.) In the other lead thread many stated that the porcelain was okay but steer clear of the ceramic decanters.

[michaelturtle1]

My next step is to do a leach test on the decanters themselves. Every piece of ceramic wear that is to be used in a food contact situation needs to be tested for lead. I will use the same methods to test the decanters.

What is interesting about the porcelain vs ceramic is that the 2 decanters contained 86 proof Old Fitz Prime. That eliminates a lot of factors and points towards the porcelain being the source of the elevated lead levels

[sku]

Great work! Thanks for doing this.

[GaryT]

Wow - that is awesome work Mike!!! Thanks for not only doing all of that, but sharing it! We're tremendously lucky to not only have someone who knows how to do all that AND has access to the stuff to do it, but also has some dusty decanters laying around

[MauiSon]

Very interesting, but I wonder about the solids. What are the detection parameters on your equipment?

Edited August 9, 2013 by MauiSon

[c2walker]

Current frontrunner for thread of the year. Thanks for sharing, Mike!

[Richnimrod]

Wow, Mike; I am in complete and total awe of your skills, abilities, and dedication to serve your fellow Boubonitos. :bigeyes:

Besides all that, I must say, as did Gary, how lucky we all are to have you (and the access you have to this equipment) on our side.

I wish I'd saved a few of my old decanters from the 60's, 70's and 80's. We could refill 'em all with 'something' and let you test how long it takes for lead to leach into the juice.

I truly look forward to your next experiment Dr. Jekyll.

[michaelturtle1]

Very interesting, but I wonder about the solids. What are the detection parameters on your equipment?

I have been racking my brain to figure out what was in the bottom of the centrifuge tubes. My biggest guess would be something to do with tannins but the odd part was the newer bourbon had about half the solids..

The lowest calibration standard we use is 5ppb so that is what is known as our PQL or practical quantificatation limit.. the actual detection limit of the machine is much lower than that but is not really relevant as compared to the drinking water limit.

[HighInTheMtns]

This is really interesting, Mike. Definitely would be cool to see more decanters/other old whiskies tested to see what trends you would discover.

[tylermke]

Thanks for sharing, Mike! A great experiment to be sure!

[smknjoe]

I have been racking my brain to figure out what was in the bottom of the centrifuge tubes. My biggest guess would be something to do with tannins but the odd part was the newer bourbon had about half the solids..

The lowest calibration standard we use is 5ppb so that is what is known as our PQL or practical quantificatation limit.. the actual detection limit of the machine is much lower than that but is not really relevant as compared to the drinking water limit.

Mike, I strained the Weller through a "natural" coffee filter to remove some of the small pieces of cork that fell in when it broke.

Edited August 10, 2013 by smknjoe

[whiskeyagonzo]

Wow. Just fantastic work. Can't wait for more testing. Great job!!