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Old 11-13-2013, 02:28 AM   #11
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Originally Posted by mjc1024
Hey, I'm interested in getting some of the ASBC methods of analysis. Do you still have them available?
We do still have them. They are kept online and protected by a password and ASBC.org asks for our IP address to allow it through their firewall. There are hundreds and hundreds, maybe thousands of methods. You'll have to know the specific method you'd like to perform and I'll happily discuss how we perform the method in our lab and how you might want to achieve the same things in yours.

I feel like I should warn you, we have one of the most capable labs as any microbrewery in the USA and as good as some of the larger craft breweries. We have GC/MS and LC/MS, spectrophotometers, gradient pumps, rotovap, microscopes, incubators and cryogenics and cell storage. We have DNA electrophoresis and PCR capabilities, extensive access to Ohio State University researchers and faculty. We employee chemists, biologists, and molecular geneticists and the ASBC methods are pretty serious stuff.

There are chemicals and apparatus that we cannot justify or afford for many of these methods. Even our simplest method, measuring the IBU in a beer, it's just not gonna happen reliably in someone's kitchen, unless you have an ultraviolet spectrophotometer, fused quartz cuvettes, centrifuge, shaker, and 99.99% pure 2,2,4 trimethlypentane. Not to mention craploads of disposable tubes, pipettes, wipes, parafilm and all the other crap you need to keep a lab going. Then lots of education, practice, notes, good habits, scientific integrity and lots and lots of patience.

I realized before I became a professional brewer, my thinking was that I wanted to see the methods just to see them, for information sake. Here's some screen shots. I strongly believe this falls within 'fair use' of copyrighted material.
screen-shot-2013-11-13-12.58.30-am.jpg   screen-shot-2013-11-13-1.15.45-am.jpg   screen-shot-2013-11-13-1.17.10-am.jpg  
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Reason: The words better. and correction 2,2,4 trimethypentane.
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Old 11-13-2013, 05:15 AM   #12
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Don't discourage people! The MOAs are not 'way serious' by any means. Any tech should be able to carry them out with simple training. GS/MS is definitely not needed (though it certainly would be nice to have). One can do many of the analyses with nothing more than a $5K UV/VIS spectrophotometer (and basic supporting lab gear). Hach was showing their latest spec at the MBAA conference. It has many of the MOA's built in so you don't even really need a subscription to the MOAs to carry out those. You do not need a large centrifuge to do IBU. I have been doing this with a used doctor's office centrifuge (and in fact, did it in my kitchen for many years). You just have to know the trick to separating the phases with modest centrifuge power. And you do not need a shaker. I know a guy who makes his living doing analysis for small breweries who does not have one. He shakes the tubes manually. I wouldn't want to do it that way but he seems to have no problem with it (you should see his wrists).

I have to say that the last post reads a little funny. MS is mentioned (which would hardly be justified for any microbrewery to my way of thinking) but the one instrument that any working brewery would want to have (and middle sized ones often do) is not mentioned and that is an Anton Paar Density meter preferably equipped with Alcolyzer and gas measurement modules. Squirt in the beer (or have it taken up by an autosampler) and out comes ABV, OG, FG, ADF, RDF, TE, pH and CO2. The basic instrument is about $22K (you have to feed it distillate to get the ABV). All tricked out with the Alcolyzer, autosampler, and gas analyzer it's more like $60K. Is this some sort of pilot brewery attached to a brewing school or Uni?

So yes, you need some gear to do many of the MOAs but it doesn't have to be terribly expensive gear as there are often multiple methods available for the same assay. Diacetyl, for example, can be assayed by GC (or GC/MS) or by wet chemistry and spectrophotometry. All the basic finished beer properties can be obtained very easily via the most expensive option (fully equipped Alcolyzer), with more labor with the much less expensive densitometer and with more labor still using a pycnometer and lab balance.

2,2,4 - that's three methyl groups.

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Old 11-13-2013, 06:26 AM   #13
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You're right, I shouldn't be discouraging. I may have been. I originally started this lab far before we were brewing and I had purchased a lot of used stuff on ebay, and most of it is in production today. A GC can be had for under $2k, UV/VIS under $500, and a wrist action shaker for about a hundred bucks (we used to shake our vials by hand). Chinese glassware might be had for $1000 or less and a good microscope from ebay for less than $300. We had a $200 ebay centrifuge, it only held 15ml vials, and repeatability was below useful. The Anton Paars are $30-$60k our density/alcohol meter is made by Mettler Toledo and saved us $20k. Most of the instruments aren't inheriently expensive. We have expensive and cheap instruments and that's not where the trouble lies. Your dude, shaking his vials might be an expert, but he's just not going to shake that stuff the same every time. The IBU method already has problems with dissolved particulates without standardized shaking.

The diacetyl method you mention, to be fair, only measures total vicinal
diketones, you really need a GC to measure diacetyl. The method for Diacetyl UV/VIS (from 1964) was archived in 1992. I'm not sure why they archive the methods, but it's accuracy is questionable, given the requirements for tenths of a milligram weights and internal standards and all that. Not saying it can't be done, it will take loads of discipline to accomplish accurately.

I don't want to be discouraging and I'm willing to discuss how we adopt an asbc method into an actual method (which I'm absolutely willing to share with anyone, they are our methods). I'm even willing to help transcribe them. I'm just saying, I don't think people should get their hopes up about being able to these analysis with accuracy. I'd say ±10 IBU, ±2% abv and just completing any method quantifying gluten, lipids or proteins would be pretty impressive. And you're right - it's 2,2,4 Trimethylpentane - isooctane for short.

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Old 11-13-2013, 01:06 PM   #14
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Originally Posted by Cryptochronolite View Post
You're right, I shouldn't be discouraging. I may have been. I originally started this lab far before we were brewing and I had purchased a lot of used stuff on ebay, and most of it is in production today. A GC can be had for under $2k, UV/VIS under $500, and a wrist action shaker for about a hundred bucks (we used to shake our vials by hand). Chinese glassware might be had for $1000 or less and a good microscope from ebay for less than $300. We had a $200 ebay centrifuge, it only held 15ml vials, and repeatability was below useful. The Anton Paars are $30-$60k our density/alcohol meter is made by Mettler Toledo and saved us $20k. Most of the instruments aren't inheriently expensive. We have expensive and cheap instruments and that's not where the trouble lies.
That's more like it.

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Your dude, shaking his vials might be an expert, but he's just not going to shake that stuff the same every time.
No disagreement there. In my experience if you do a couple by hand you'll be happy to shell out for the shaker and repeatability is frosting on the cake.

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Originally Posted by Cryptochronolite View Post
The IBU method already has problems with dissolved particulates without standardized shaking.
Not sure what you mean here but the IBU method is really kind of shaky anyway. The fact that it is International Bitterness Units rather than mg/L isohumulone is a clue. I always remind people that, per the MOA (older version) IBU "... express the bitter flavor of beer satisfactorily ..." and that, therefore, one can't put too much reliance on IBU. One could, for example, take a two glasses of a Bohemian Pilsner, stir some gypsum into one and leave the other alone. The bitterness qualities of the two will be quite different though both will clearly have the same IBU rating. The value in measuring IBU is as a way of indicating that something is out of whack. For a particular beer one knows what to expect and if he gets a deviant value knows he needs to check his process, the batch of hops he is using...

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Originally Posted by Cryptochronolite View Post
The diacetyl method you mention, to be fair, only measures total vicinal
diketones, you really need a GC to measure diacetyl. The method for Diacetyl UV/VIS (from 1964) was archived in 1992. I'm not sure why they archive the methods, but it's accuracy is questionable, given the requirements for tenths of a milligram weights and internal standards and all that. Not saying it can't be done, it will take loads of discipline to accomplish accurately.
Yes, the wet chemistry methods that detect the vicininal carbonyl groups react to both diacetyl and pentane dione and give a 'total VDK' result but this is adequate for most purposes. It certainly is if the goal is the detection of 'sarcina sickness' and is even so for determining whether 'diacetyl rests' have been adequately carried out. A GC will separate the two but even GC analysis has its pitfalls as one has to worry about treatment of the sample in order to avoid conversion of acetolactate to diacetyl. Some labs intentionally promote that reaction (by incubation of samples) in order to measure a total diacetyl potential as acetolactate is indeed potential diacetyl in a beer on the shelf.

The main problem with the hydroxylamine method is that it is not sensitive enough given that taste threshold is at the tenths of mg/L level. One cannot typically measure that low without going to cuvets of path longer than 1 cm. Plus a time consuming distillation is involved.

Seems to be a lot if interest in diacetyl these days. I noted from the images in the earlier post that diacetyl is the molecule ASBC chose to illustrate the MOA home page.

Quote:
Originally Posted by Cryptochronolite View Post
I'm just saying, I don't think people should get their hopes up about being able to these analysis with accuracy. I'd say ±10 IBU, ±2% abv
Wow. You don't mean that. An ABV report of 5 ± 2% would be pretty useless data almost 2 orders of magnitude worse than I can do as a 'kitchen chemist'. I've done error analysis on my ethanol recovery and have a total error budget of 0.03% for a beer with 10% ABV. I think you must have meant 2% CV e.g if the beer were 10% the error would be 0.02*10 = ±0.2% ABV.

The error analysis is at
http://www.wetnewf.org/pdfs/Brewing_...illation__.pdf
What may be of more interest in this article to the guys originally looking for data on what is involved in running the MOAs are details on how I implement the MOA including a picture of the glassware setup.

If you are trying to make the points that one must be cognizant of error sources, must run standards, must know how to detect interferences etc. then yes indeed, those are all valid points. I said in an earlier post that any tech should be able to run these procedures if trained but you do need someone who knows something about analysis and knows his way around a lab to do the training.

To me the biggest discouragement to a home brewer contemplating doing some of these measurements would be that no one will sell chemicals anymore. Even Cynmar which used to be so friendly to home brewers wouldn't sell me sodium bicarbonate without registration as a business and won't ship to home addresses.
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Old 12-09-2013, 11:00 PM   #15
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I'm looking for a sample of the ICE-3 calibration standard for HPLC analysis. I just want to do a single AA analysis on the hops I picked this fall but I can't justify buying the whole sample for $150 for only 3 analyses.

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Old 01-25-2014, 07:55 PM   #16
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I'm looking for a sample of the ICE-3 calibration standard for HPLC analysis. I just want to do a single AA analysis on the hops I picked this fall but I can't justify buying the whole sample for $150 for only 3 analyses.
"Stocks of ICE-3 are being divided between ASBC (in USA) and EBC (distribution through Labor Veritas in Switzerland), from which sources analysts can purchase the new standard in the usual vials.*
ICE-2 will now be available only while stocks last. ICE-3 is valid from September 1st, 2010.
* Purchasers in the USA, Canada, Central and South America should contact ASBC headquarters (email: asbc@scisoc.org; tel: +1 (651) 454-7250), while those in Europe and Africa should direct enquiries to Labor Veritas, Zürich, Switzerland (email: admin@laborveritas.ch; tel: +41 (0) 44 283 29 30). Persons ordering from other parts of the world may make their approach to either party."

The price is $160, unfortunately, they have a monopoly.
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Old 05-08-2014, 04:09 PM   #17
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Hi,
i'm trying to bring the vdk analysis in the brewery i'm working in using the ASBC Methods of Analysis Beer-25B (broad spectrum).
My question is do I have to do the standard curve for every analysis or can I do it only one time and pretend it's gonna be the same everytime I do it?
I already have all the equipment since i'm doing the IBU, SRM and %alcool for them.

Thank's for your help and sorry for my bad english

Charles
Quebec, Canada

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Old 05-08-2014, 04:38 PM   #18
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The curve calibrates your reagents and procedures. You can use the same calibration curve for as long as your procedures and reagents stay the same. As reagents lose potency over time it is best to check on things by running standards from time to time. Of course running a complete set of standards is effectively recreating the calibration curve. You may wish to run one or two standards at about the levels at which you typically measure diacetyl which will, we hope, be less than 0.5 mg/L i.e. at the 0.5 mg/L level and if the numbers start to drift repeat the calibration or make up fresh reagents.

The problems I had with 25A when I used it was that there just wasn't enough diacetyl in my beers to give a good response to the test.

The English is perfect except for the French spelling of alcohol.

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Old 05-24-2014, 04:31 PM   #19
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We do still have them. They are kept online and protected by a password and ASBC.org asks for our IP address to allow it through their firewall. There are hundreds and hundreds, maybe thousands of methods. You'll have to know the specific method you'd like to perform and I'll happily discuss how we perform the method in our lab and how you might want to achieve the same things in yours.
Hey Crypto,
Are you still on this forum? I had posted on the forum about a year ago asking about access to ASBC MOAs. You mentioned that you had access to them and something about a password and an IP address for authentication. I was wondering if I could get access to them and how? Is that something I can get from you? I have a biochem degree and have worked in the pharmaceutical industry for several years so I'm very comfortable with the subject matter. I would like to get some methods for analytical analysis of beer (IBUs, diacetyl, calories, etc.) I've got my lab pretty much stocked, still need a uv/vis spec and gc or hplc, but that'll come soon hopefully. I appreciate any help you can give. Cheers!
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Old 10-14-2014, 08:46 PM   #20
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The diacetyl method you mention, to be fair, only measures total vicinal
diketones, you really need a GC to measure diacetyl.
90% of this thread is over my head, but VDK is what I'd need to measure anyway. I can TASTE for diactyl with my tongue and it's a "free" test.

The AMOUNT of VDK isn't necessarily super important in brewery Q&A; what I need to know is if there IS VDK, so some old, only marginally accurate test is actually "good enough".

The first rule in quality control (ISO 9001, anyway) is to define your spec and your tolerance to that spec. The diacetyl spec that's required is pretty low. -Have I taken up all / most VDK? Does my test reveal any VDK? -Then "can I taste diacetyl?" -If no, empty the fermenter / brite tank...

I think the diminishing returns curve for VDK testing is insanely sharp beyond this point; the cost to get higher accuracy explodes with very little benefit to your finished beer or consistency.

Adam
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