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DMA OGs vs Brewhouse Hydrometer

  • 1.  DMA OGs vs Brewhouse Hydrometer

    Posted 07-25-2017 17:20

    Is anyone else using a DMA 4500 M Alcolyzer Beer ME? We've been using ours for almost 2 years now, and we use it every day to check our final product. It works beautifully for alcohol and final gravity, with a very high level of reproducibility. We've noticed, however, that the calculated OGs it spits out are off by about 0.5 Plato from what the brewers were reading on our calibrated hydrometers. Certain brands seem to be a bit further off than others as well.

    We weren't sure where in the process the misstep was, so we began running every single hydrometer sample run by the brewers through the DMA. We ran over 200 samples and the majority of the time got a higher reading on our hydrometers, with most of them being over 0.1P off. The German calibrated hydrometers were definitely closer than the cheaper ones, but we were seeing differences upwards of 0.5P between the readings, which is beyond human error. Meanwhile, some samples were exactly the same, to the hundredths place. We would occasionally see numbers in the ABV section during this, which was strange, as they were pre-yeast. 

    The beers we ran these tests on are finishing up in the fermenters, and I've been able to compare the calculated OGs from the DMA from the OG it read itself out of the HX, and the calculated is higher than the original read. We have a bit longer to wait for more data though. 

    All of our FGs match, alcohol is on point, but for some reason this OG calculation isn't working out. We've also struggled with any beer that has appreciable haze, and find that filtering/centrifuging will give us different alcohol levels. I'm assuming this is because the alcohol module in the DMA is based in spectrophotometry the haze is interfering? 

    Has anyone else had trouble with any of these issues? We're not sure which numbers to trust anymore, as the further we look into this, the less sense it makes. This has happened despite all checks and calibrations being passed, proper daily cleaning regimens being followed, and extensive conversations with Anton-Paar. I'm out of ideas and would love any input fellow QC folks have. We're trying to dial in our recipes further and it's difficult when you can't trust your OGs.



    ------------------------------
    Kate Steblenko
    Quality Scientist
    Jack's Abby Craft Lagers
    Framingham MA
    (508) 872-9000
    kates@jacksabby.com
    ------------------------------


  • 2.  RE: DMA OGs vs Brewhouse Hydrometer

    Posted 07-25-2017 20:21

    Hi Katherine 

    I suggest that you take a look at Alex Speer's discussion on Extract below.  You can also contact him at IBD.  He is smart and helpful.  

    There are correction factors required for Yeast and CO2 when one calculates OG.  Having said that I must warn you that math is not my forte.  

    Back in the 80's the large breweries used a primitive DMA method to calculate Alcohol.  We had a DMA reading plus AE from a calibrated hydrometer or pycnometer plus SG from an ABBE refrac.  Different beers required different correction factors.  Three points would determine OG and Alcohol

    The OG as determined by calibrated hydrometer or pycnometer is your OG ...as long as the sample is filtered to remove particles and the measurement is taken at exactly 20C.  See ASBC methodology.

    Should you wish to go backwards in time to the real measurement of SG, ....thereby the measurement of Calc. OG, RE, Alc by Wt, and Alc by Vol....gravimetricly using a pycnometer... be prepared for a learning experience with the ASBC tables.  This requires pycnometers and an analytical balance good to the 4th decimal, and distillation equipment.  Remove the Alcohol from the beer by distillation and determine its SG by pyc.  Determine the RE of the beer minus alcohol, by pyc.  Then hit the ASBC tables.  If its done properly with great technique the process results in true SG.

    Anton Parr has been measuring SG for decades so I would strongly suggest that you have a good discussion with their technical people.  Perhaps they can suggest appropriate corrections.

    Thanks for allowing me to regurgitate my QC technicians work from the dark ages of 73'. 

     

    http://www.asbcnet.org/membership/buzz/Documents/PDFs/2015/FeatAug15.pdf

    ------------------------------
    James Holden
    Brewing Consultant
    Retired but Busy
    jholden007@hotmail.com
    Canada/US/Mexico
    ------------------------------



  • 3.  RE: DMA OGs vs Brewhouse Hydrometer

    Posted 07-27-2017 13:09

    Hi Katherine,

    We have been using the Anton Paar Alcolyzer for a couple years now, and have run up against the same issues.  However, we also love the instrument, and would rather struggle with its problems than all the problems I used to have getting accurate readings from hydrometers, pycnometers & etc.  For all its faults and intricacies, the Anton-Paar instrument gives marvelously precise and repeatable measurements, and we are delighted to have it in our QA lab.

     

    I too have casually noticed that the alcohol readings can change for hazy samples depending on the degree to which you clarify them before measurement.  I think your theory makes sense: the Alcolyzer module measures alcohol by long-wave-length spectroscopy.  This is similar to how the method Beer-10 checks for haze in samples to validate color measurements.  So it makes sense that hazy samples would throw off the alcohol measurement.

     

    I trust the DMA4500 to measure density more accurately than hydrometers.  When checking the accuracy of hydrometers in standard sucrose solutions, at various temperatures, I find that they are rarely very accurate.  I find that they are also affected by the presence of cold-break.  I have tested the DMA4500 with standard sucrose solutions and found it to be perfectly accurate.  My daily water density checks give me confidence that the density module stays precise and accurate.  If you use the Brix method (not the beer method) I believe it is only using the DMA4500 density module to calculate Brix, so it is very accurate and reliable.  If you use the Beer method, the instrument is trying to figure out how much alcohol is in your unfermented sample, and will sometimes give you slightly positive or negative numbers.  So, it's not perfect, but IMHI the Brix method is your "gold standard" for Original Extract measurements of unfermented wort.

     

    The real extract is calculated from the measurements of both the density module and the Alcolyzer, so that any inaccuracy in either/both modules will be multiplied in the real extract module.  These inaccuracies could be due to limitations of the instrument and/or introduced by your sample prep methods.  Moreover, the Original Extract calculation is based on certain assumptions about the amount of extract consumed in fermentation for yeast growth and CO2 production.  I trust this measurement least of all.  When I have used the Alcolyzer Beer method to track fermentations in progress on a daily basis, I find the calculated Original Extract values bounce around wildly.

     

    Cullen Dwyer, Q.A. Manager

    Wachusett Brewing Co.

    Westminster, MA

    Office: (978) 874-9965 x160

    Fax: (978) 874-0784

     






  • 4.  RE: DMA OGs vs Brewhouse Hydrometer

    Posted 07-27-2017 15:36
    The following response from Alex White was received personally by Cullen Dwyer, and forwarded to "Ask the Brewmasters" at Mr. White's request:​


    Hello All, Great discussion.  Feedback is always appreciated.  I just wanted to add and hopefully clarify that some of the parameters available in the instrument configuration of an Alcolyzer + DMA are the result of inputs from both units, while others are solely measured and/or calculated from either instrument.  The Alcolyzer measures ethanol concentration directly using the NIR absorption method at a specific wavelength, and the density meter only, of course, measures density using the oscillating u-tube method.  The back of the Alcolyzer manual lists the formulas for all of the calculated parameters and so can assist in determining where and how the values are calculated.  Customers often find that the original extract (OE) of the finished beer (if calculated using our Beer Analyzing System) is different than the OE measured in the lab prior to fermentation. The true OE, pre fermentation, is the correct OE.  There are several explanations for this:

    • The Balling formula is not perfect (140 year old formula).
    • Other ingredients can be metabolized differently than malt and may affect the OE calculation.
    • Further deviations in OE may depend on yeast strain and fermentation variations.

    We do not recommend using the Alcolyzer parameter "OE" for measuring wort, as the OE calculation is based on density and alcohol.  If wort is measured with an Alcolyzer, be sure to use the parameter "apparent extract (Ea)". This parameter uses density only.

    As for alcohol concentration variations in hazy beer, these can be cleared up (sorry) using diatomaceous earth (approx. 1g/100 ml) and filtering with 4-7 micrometer pore size paper.

    Best regards, Alexander White Technical Sales Representative Business Unit Measurement Anton Paar USA, Inc. 10215 Timber Ridge Drive Ashland, VA  23005 USA T: +1 - 804 - 550 - 1051 - X377 M: +1 - 804 - 334 - 4977 F: +1 - 804 - 550-1057 www.anton-paar.com



    ------------------------------
    Cullen Dwyer
    QA Manager
    Wachusett Brewing Co
    Westminster MA
    (978) 874-9965x160
    ------------------------------



  • 5.  RE: DMA OGs vs Brewhouse Hydrometer

    Posted 07-30-2017 07:37
    Dear Katherine,
    I always thought the future of the ASBC would be to create User Groups to answer your post.  We need an Anton Paar Group.  There's enough of us, already.
    I waited for some ASBC 'A-lister' like Greg Casey or Gary Spedding or the aforementioned Alex Speers to reply; but in their absence, I'll weigh in as a journeyman analytical technician working in the greatest industry on earth.  I'm never going back to hazardous waste characterization.  God Bless that Cullen Dwyer, but I'll push you where you need to go.

    The Anton Paar suite of instrumentation is my ATM machine.  My kids are going to Oregon State on its reproducibility and resolution.   It's your job to master the idiosyncracies of the Austrian mindset. 

    Understand what you bought- a Near InfraRed measurement/exquisite algorithm of ethanol in malted beverages (for the Beer Analyzer.)  Although, note that methanol and isopropanol will positively interfere with the algorithm.  Really, what you've bought is a fine temperature control of density with the DMA4500.

    Rely on density.  It will never let you down, but you need to build robust datasets to tame the inevitable random error.  Remember, you are working with a tripartite solution in finished beer;  ethanol, water and everything left behind.

    1) Do a Gage Reproducibility and Reliability with everyone who relies on these data to make decisions:  brewers, cellar staff, managers, you.  It is absolutely critical to get buy-in by your team to master the investment and create a culture where folks want the instrument to work.   Have everyone run 10 samples- Anton Paar and hydrometer.
    Those knuckle-draggin' brewers who swear by their hydrometers, can they control temp to  0.1°C?  Get the data: run 10 Anton Paar  samples and 10 with their hydrometer.  Chart the results with coefficients of variance.  Let the chips fall where they may. 

    2) Run pre-pitch wort samples the same way.  You may need to centrifuge to finish the hot trub precipitation.  Get everyone to run the instrument.  You all have to make that instrument your own and make it pay.

    3) You:  distill samples until you have confidence that you can sell the NIR results to your team.  We distilled alcohols until the power company thought we were drawing so much power that we HAD to be doing something illegal. 
    Distilling is the reference method and can tell you if/when an interference from turbidity is significant.  I don't filter, except under duress.  I will centrifuge, as needed.

    4) Never give in.  We all use Anton Paar, and/or Kyoto and/or whatever Chinese upstart is on the horizon.  The fundamentals are well observed- control temperature, get some way to measure density and ethanol and you will rule the world. 
    Beat those who claim that a hydrometer is superior with a stick.
    Scott

    ------------------------------
    Scott Bruslind
    Laboratory Manager
    Analysis Laboratory
    Lebanon OR
    (541) 451-8571
    ------------------------------



  • 6.  RE: DMA OGs vs Brewhouse Hydrometer

    Posted 08-01-2017 11:39
    Greetings All,

    I couldn't agree with Scott more.  

    These comments are for others out there having similar issues with generally measuring wort and beer parameters:

    As an analytical chemist and engineer by training I can tell you that there are three critical aspects of measurement: Be Consistent, Compare to Standards, and Know Your Equipment.  

    Be Consistent -  Whatever method you choose to use, be consistent in how you use it.  Always take the time to adjust temperatures, let equipment warm up to operating stability, and make multiple measurements of each sample.  In our own lab, we always split the samples and do any preparations on the duplicate samples, then each duplicated sample is split again prior to being measured.  If the protocol calls for a temperature of 20.0 C but you find it is better to run it at 25 C, that is fine, but always run your tests at 25 C to develop a consistent data set.  If you are reading the hydrometers at the top of the meniscus, always read it at the top of the meniscus (and always clean the hydrometer!).  If you are going to compare your measurements with someone else, be sure that both sets of measurements are following the same protocols.

    Compare to Standards -  This follows from the last statement.  If you are going to compare your measurements to anyone else's measurements, you need to follow the same protocol.  Standards have been developed to provide a common "page" for all comparisons between labs.  To ensure that you are getting the values you think you are, run the protocol with a known, accepted standard.  Spike a sample with a known amount of alcohol to confirm that you are able to correctly determine the amount.  For those using hydrometers or refractometers, prepare known samples of sucrose (sugar) in water, adjust the temperature and test your equipment...  and keep them CLEAN!  If your values are different, use the difference to calibrate your equipment.

    Know Your Equipment -  Every piece of measurement equipment and every device has its own limitations.  Extract in degrees Plato assumes your sample is a pure sucrose in distilled water solution.  We all know thats not true, but we accept it as a common comparison scale, and that's okay ("Be Consistent").  Hydrometers are designed to be read at the bottom of the meniscus (that is the true surface level of the liquid), however, its not possible to read the hydrometer properly in a dark Baltic Porter.  You could read the hydrometer at both the top and bottom of the meniscus for lighter colored beers, find the average difference between them and then use the difference with that troublesome Baltic Porter. 

    I spend a lot of my time working with brewers to help them understand ("Know") their brewing and measuring equipment, both new and old.  The various automated systems are great time savers (Only an analytical chemist would be crazy enough to work with picnometers, constant temperature baths and distillation equipment!), but they are expensive, have their own set of quirks and need a bit of understanding at a different level.

    Hope this helps!

    ------------------------------
    Rick Cole
    Manager
    Midwest Hop and Beer Analysis, LLC
    Evansville, WI
    608 882 4677
    ------------------------------



  • 7.  RE: DMA OGs vs Brewhouse Hydrometer

    Posted 07-05-2018 11:28
    Scott mentioned my name and I have been busy and traveling. I am not sure I have much to add except a reference:

    Cutaia, A.J., Reid, A-J. and R.A. Speers,  2009. Examination of the relationships between Original, Real and Apparent Extracts, and Alcohol in Pilot Plant and Commercially Produced Beers. J. Inst. Brew. 115:318-327.


    It provides a background and equations to relate OE, AE, RE OH etc etc. I have a pretty amateur (but accurate) spreadsheet with those equations embedded in them if people want a copy.

    Cheers,

    Alex.Speers@dal.ca



    ------------------------------
    Alex Speers B.Sc. (Agr.), Ph.D.,FIBD
    Canadian Institute of Fermentation Technology
    Dalhousie University,
    Halifax, NS
    ------------------------------



  • 8.  RE: DMA OGs vs Brewhouse Hydrometer

    Posted 07-31-2017 19:13
    We use an AP DMA 35 for SG readings on the brewfloor and an ALEX500 for final product ABV and Density results.

    We also had an issue where they two sets of numbers weren't agreeing, but it was because at some point the DMA35 was set to show SG as Denisty (SG 20/00 as opposed the correct setting of SG 20/20) and this caused quite a bit of confusion until it was corrected.

    I agree with some of the earlier comments that a thorough and rigorous self-check of your procedures is a great way to ensure that your SOPs are working as expected. It's a pain to do, but well worth the effort.


    ------------------------------
    Christopher Mills
    Kereru Brewing Company Limited
    Upper Hutt
    64 4 9746343
    ------------------------------



  • 9.  RE: DMA OGs vs Brewhouse Hydrometer

    Posted 08-01-2017 16:31
    Rick hit the nail on the head: Always know what you are measuring and the limitations of your instrument. Utilize known standards to calibrate your equipment, and verify calibrations with internal standard additions.

    The main target of the measurements discussed in this thread appears to be accurate %ABV.
    None of the techniques described above measure the amount of ethanol molecules in the volume of beer (or other beverages) directly (even the distillation step evaporates not just ethanol...).

    Our quantitative method of choice in our lab to directly measure ethanol contents in a mixture (like beer, wine, or kombucha), is by capillary gaschromatography (preferably headspace GC) coupled with a suitable detector. My preference is a mass spectrometer detector that measures the ethanol molecule directly via its molecular mass, possibly against an isotope labeled internal ethanol standard.

    Expensive (you can find used once for less than a new alcolizer though), and also not " fool proof", but als not easily thrown off by turbidity, other alcohols, phenols, sugars, turbidity, color, etc. The only other molecule that shares the same molecular mass as ethanol is dimethylether, which is easily separated from ethanol in the gaschromatograph.

    Don't get me wrong, the modern day density meters and near-infrared (NIR) detectors and combinations thereof are marvelous instruments, and can help you to obtain very reliable and accurate data in your brewery very quickly, if properly used, maintained, calibrated, and understood... We have tested pretty much all techniques side-by-side and in most "normal" cases found excellent correlation of measurements. However, most of our craft brewing clients like to deviate from "normal"  on occasion, and find some surprising situations, e.g., certain IPAs on the East Coast are known to have high turbidity and can fool the most expensive alcolizers, some "heavy" beers have more ABVs than expected, as do some of the "non-alcoholic" kombuchas...

    In most instances the differences are small and probably negligible for practical purposes. However, when these differences exceed several %ABV or get near or exceed legal thresholds, then there may be cause for pause. In case of question, you might want to back up your density and NIR based results with a properly calibrated GC/MS based measurement. Most service labs for alcoholic beverages can provide this as a service for you for a marginal fee and great peace of mind.

    ------------------------------
    Volker Bornemann
    President
    Avazyme, Inc.
    Research Triangle Park, NC
    avazyme.com
    ------------------------------



  • 10.  RE: DMA OGs vs Brewhouse Hydrometer

    Posted 08-04-2017 16:36
    Thanks everyone for all the responses! 

    Moving forward, we've decided to trust our Brewhouse hydrometer for our pre-fermentation OGs, but still run our heat exchanger samples through the DMA for comparison. We'll also start using a 1g DE/ 100 mL turbid sample prep method as recommended by Anton Paar. 

    The only troublesome thing left is that the same exact samples sometimes run differently on hydrometers vs DMA, but hopefully playing around with the DE will help to clear some of that up (it's really hard to not use that pun). 

    We're looking into the DMA 35 for our brewhouse / fermentation gravities in the future, to eliminate any differences between reads and operator errors. If anyone has any experience with mid fermentation samples and that piece of equipment I'd be interested in hearing it. 

    I'll update this thread in a few weeks with any significant findings. Thanks also to everyone who sent me an email with assistance! I really appreciate the helpfulness of our community.

    ------------------------------
    Kate Steblenko
    Quality Scientist
    Jack's Abby Craft Lagers
    Framingham MA
    (508) 872-9000
    kates@jacksabby.com
    ------------------------------



  • 11.  RE: DMA OGs vs Brewhouse Hydrometer

    Posted 06-25-2018 06:18
    Hello everyone,
    We have run across this issue before and it is not new. Here is the official explanation form our FAQs. The article referenced is from the Scandinavian School of Brewing and I highly recommend it (a simple google search will find it): 

    Original Extract Calculation in mPDS 5 and Beer Analyzer System
    Customers often find that the original extract (OE) of the finished beer calculated in the mPDS 5 and Beer
    Analyzing System is different than the OE measured in the lab prior to fermentation. There are several
    explanations for this:
    • As described in the article above, the Balling formula is not perfect and modern production practices do not always agree with the 140 year old formula.
    • Other ingredients may also be added to the wort. Instead of barley or wheat malt, rice, corn or raw sugar may be added. These are metabolized differently than malt and may affect the OE calculation as described in the article above.
    • Further deviations in OE may depend on feedstock fluctuations, yeast strain and fermentation variation. The true OE, pre fermentation, is the correct OE. A brewery or feedstock specific adjustment may be needed or desired, depending on the breweries needs.

    Can I use the Alcolyzer Beer Analyzing System to measure wort from the brewhouse?

    Yes, you can use the Alcolyzer Analyzing System for wort analysis, but be careful!

    If the Alcolyzer Analyzing System is used to measure wort (no alcohol present) you must use the parameter
    "Ea (app. Extract) (%w/w)" and not "p (original extract)(%w/w)". The "Ea (app. Extract)(%w/w)" parameter
    uses density only and is the correct value for wort analysis!

    The original extract calculation is based on the measured density and alcohol values. It is designed to
    measure the Extract content of finished beer. So in case the Alcolyzer Beer determines any alcohol the
    calculated original extract value on wort might be incorrect.

    The alcohol deviation in OE is approximately double the alcohol concentration. A wort alcohol value of 0.05% v/v results in a deviation of 0.1° Plato OE.

    Note: The Beer Analyzing System must be thoroughly cleaned after measuring wort samples. Due to the
    high extract content and hop oils it is very sticky and often difficult to clean! Mind the cleaning
    recommendations for wort (instruction manual for Alcolyzer Analyzing Systems)!

    Hope that helps shed some light on the subject!
    Cheers,

    ------------------------------
    Daniel Gore
    Key Account Manager Beverages
    Anton Paar GmbH
    Graz
    +43 316 257 1165
    ------------------------------



  • 12.  RE: DMA OGs vs Brewhouse Hydrometer

    This message was posted by a user wishing to remain anonymous
    Posted 07-05-2018 11:29
    This message was posted by a user wishing to remain anonymous

    For a more up to date reference:

    Cutaia, A.J., Reid, A-J. and R.A. Speers,  2009. Examination of the relationships between Original, Real and Apparent Extracts, and Alcohol in Pilot Plant and Commercially Produced Beers. J. Inst. Brew. 115:318-327.