Brewery Quality Crash Course Ben Bailey Quality Assurance Manager - - PowerPoint PPT Presentation

Brewery Quality Crash Course

Ben Bailey Quality Assurance Manager Troegs Brewing Company bbailey@troegs.com

Outline of Discussion

• Process Measurements vs. Quality Control vs. Quality

Assurance vs. Quality System

• Defining the role of the lab in your brewery’s Quality

Program

• Process Measurements (Choosing what to measure)
• Individual Tests
• Yeast Propagation
• Sanitation / Microbiological Testing
• Sensory / Taste Testing
• Setting Up Limits for Beer Parameters / Control Charts
• Example of Small Brewery Quality Lab

What does QA / QC mean?

Process Measurements / Quality Control / Quality Assurance

• Process Measurements are the first step to Quality Control.
• Volume of wort collected in the kettle
• Weight of specialty malts added to the grist
• Temperature of the Hot Liquor Tank
• Quality Control is measuring the results of a process. REACTIVE
• IBU of beer at the end of fermentation
• Go / No-Go Tastes prior to packaging
• ATP Swabs on Packaging Line prior to production
• Quality Assurance is making sure QC results are good the first time. PROACTIVE
• Validation / Calibration of temperature probes in the mash tun
• Assurance that the temperature measurements are correct
• Hygienic Design of Packaging Line
• Assurance that the equipment is cleanable
• Quality System is a set of rules and procedures that ensure that a quality

product is being produced. The Book / Binder / Bible

• List of specifications to be met for a brand in a Brite Tank prior to release for packaging
• Frequency that a DO meter needs to be validated / calibrated.
• Requirements for each supplier to meet during qualification/audits.
• Actions to take when any requirement results in a deviation or Out Of Spec (OOS) result.

Quality Assurance Example

DIN 11851 Connection “Tri-Clamp” Connection DIN 32676 / ISO 2852 Does not conform to EHEDG guidelines! Hygienic Design

Choosing which tests to perform

Test? Legally Required?

Perform Test

Would OOS result cause rework, hold or refusal of batch being tested? Would OOS result cause change in processing for current or future batches?

Perform Test Perform Test

Parameter is probably not worth testing. Is there a cost to OOS result? Consider testing if response to OOS result is available CoA? Perform Test N Y Y Y Y Y N N N N

Ranking testing by importance / ability to react

• In order of importance
• Legally required
• Rinse water testing (FDA)
• ABV Testing (TTB) (some states)
• Fill Level verification (TTB)
• Process Inputs (Inputs can be corrected prior to start of process step)
• Temperatures of HLT & CLT
• Yeast Counting
• Measuring Concentration of Cleaning Chemicals
• Measuring Malt Weights
• ATP Swabs (High RLU results)
• Micro Plating with dependent release
• Beer is held in warehouse after packaging until results show beer is ok to ship. Out of spec beer would likely be

destroyed, but should protect the brewery from micro based recalls.

• Process Outputs
• Correction on same batch (beer tested can be brought in spec)
• CO2 in BBT
• DO in BBT
• Conversion in Mash Tun
• ABV% (if high, dilution still possible)
• Correction on subsequent batches (beer or process tested can’t be brought into spec without blending)
• Mill Sieve Testing
• Color
• IBUs
• Traditional Micro Plating (beer shipped before results are available)

Prioritizing Supplier Audits

Test?

Perform Test

Would OOS result cause change in processing for current or future batches?

Perform Test Perform Test

Parameter is probably not worth testing. Is OOS result likely? Consider testing if response to OOS result is available CoA? Y Y Y Y N N N Slide from 2015 MBAA Presentation by Brad Rush

Individual Tests

Density

Density measurement is one

• f the most important

parameters to measure. Density is a simple way to measure concentrations of binary mixtures (sugar/water, ethanol/water, caustic/water) Hydrometer is cheapest, but least accurate Pycnometer is very accurate, but is also very time consuming Digital Density meter is fast and accurate. No operator differences in results. Pycnometer Hydrometer Digital Density meters

pH

pH is another measurement that every brewery should be performing. Required for proper enzyme control in the mash, and to meet FDA requirements. Invest in a good pH meter with ATC and a quality all-in-one probe. Need to be calibrated daily.

• Microscope capable of 100x

magnification (400x for bacteria)

• Hemacytometer
• Methylene Blue (White Labs)
• Pipettes or beakers to dilute slurry
• Tally Counter or Hemacytometer

iPhone App

Yeast Viability Equipment

Carbonation

• Every brewery should be

checking carbonation levels.

• Zahm & Nagel tester is relatively

inexpensive.

• Digital meters that work on

various principles.

• Some can measure other

dissolved gasses like Nitrogen or Oxygen simultaneously.

• Digital Meters are pricey, but
• ffer repeatable results.
• All instruments require proper

care and calibration.

• Carbonation meters are often

abused by brewers in the cellar

Oxygen Measurement

• Wort DO measurement is

important for every brewery

• Oxygen measurement is very

important for all packaging breweries

• Air testing using the Zahm

equipment can give a decent idea of oxygen levels, and is not too expensive

• Testing with an optical DO

meter can give more information (DO and TPO) and can be used elsewhere in the process to troubleshoot

• Package Analyzers are also

available which can directly measure headspace O2 and DO, or calculate TPO.

Alcohol Measurement

• Distillation of beer creates a “binary

mixture” of ethanol and water. The concentration of this mixture can be determined by density (digital density meter or pycnometer)

• Takes about 12-15 minutes per sample
• TTB accepted method for verifying label

claim of alcohol

• When coupled with the measurement
• f the AE prior to distillation, most

relevant parameters can be calculated. AE, ABV, ABW, OG, RE, E/A, kCal.

• Alternative to purchase of Alcolyzer.

Alcolyzer can complete the same analysis in less than 3 minutes. Density meter coupled with NIR measurement

• f ethanol.

Color

• Most easily measured by UV-Spec
• Can also be measured with a

comparator

• ASBC Beer-10
• Simple quick measurement that can

show deviations in the brewhouse such as; recipe, hot time, hot side oxidation.

• Samples need to be filtered prior to

measurement

• Dark beers will need to be diluted or

measured with a smaller cuvette (1mm

• vs. 1cm)

IBUs

• Need a UV-Spec that can measure in

accurately at 275 nm (UV Range)

• Can help a great deal when

determining hop addition times or rates during recipe development

• Consistent bitterness is key to

maintaining a consistent flavor profile

• Uses Iso-Octane which is an organic

solvent, and needs to be properly disposed of or regenerated

• DO NOT PUT DOWN DRAIN!!
• Iso-Octane regeneration saves on both

consumable use and hazardous waste disposal costs

• Equipment shown on right
• 2013 MBAA Poster describing method
• Upcoming MBAA TQ Article

Other Tests done with a UV-Spec

• Iron concentration
• Thiobarbituric Acid Index
• FAN
• Total Polyphenols
• SO2
• Testing for Glycol contamination
• Many other methods available,

such as HSI, however most of these have limited use in monitoring brewery production.

Optimization of Mill Settings

• Sieves to optimize mill settings for

maximum brewhouse extract efficiency are a good investment even for small breweries

• Van Havig’s MBAA presentation

showed 70 lb. of malt savings per brew

• n a 10 bbl system
• Sieves are about $50 a piece, need 6

(plus pan) for ASBC method, 4 for method described by Van Havig

• Shaker is great for repeatability of sieve
• testing. Start around $850
• Sieve results need to be compared with

Brewhouse Extract Efficiency numbers and lauter times to determine

• ptimum settings for your system.

Turbidity and Stability Testing

• Tyndall Light box can be built

inexpensively and when used with Formazin standards for comparison, can give pretty good results.

• Beer Turbidity meters give readings at

two different angles and can measure accurately at near 0 deg. C. Water turbidity meters will not work due to condensation!

• Turbidity is a way to measure shelf

stability and validate the effectiveness

• f stabilization. Hazy beers can also be

measured to ensure that they are consistently hazy.

• The ratio of 90⁰/11⁰ or 90⁰/25⁰ can give

you an indication of how stable your hazy beer is. For German style Wheat Beers, a ratio of 0.9 is a good target.

Yeast Propagation

Yeast Propagation

• Yeast propagation can be a good way to begin a

microbiological program

• It is one of the only tasks that a quality department

typically undertakes that produces something of tangible value to the brewery.

• Media needed for yeast growth is simple to make
• Wort Agar, Wort
• A brewery with 20 bbl fermentations, producing 3000 bbl a

year, using yeast up to 5 generations and pitching a single fermenter from each yeast harvest would spend $15,000 a year on WLP001 from White Labs. That comes to $5.00 per bbl for yeast alone.

• That same brewery making 300 bbl of a slower selling

specialty beer with a secondary yeast strain which can’t be re-pitched due to the frequency of brews would spend $7,500 on yeast. That is $25.00 per bbl for yeast!

• The equipment needed to ensure good yeast quality can be

used for a microbiological QC program as well.

• Autoclave, Laminar Flow Hood, Fridge, Incubator, etc.

Yeast Propagation Equipment

Yeast Handling

Sanitation

ATP Meter

• Cost around $2000, and about $1/test
• Give rapid results (<15 seconds)
• Indication of cleanliness
• Very useful for surface testing of fillers
• Can also be used to test rinse water on

tanks, filters, pipes, or other equipment post-CIP

• Does not specify what kind of growth is

present

• Does not differentiate between beer-spoilers and

non beer-spoilers

Microbiological Filtration

• Filtration is necessary to

concentrate microbiological samples

• nto agar plates
• For bright beers, you can

filter an entire 12 oz can

• r bottle to get a total CFU

per package

• For labs without a decent

sized autoclave, single use funnels or flame-able stainless funnels don’t require autoclaving

Yeast Lysine Agar Copper Sulfate Agar (Lin) Crystal Violet Agar Lin’s Wild Yeast Medium Schwarz Differential Medium Copper Sulfate Agar (Taylor and Marsh)

Brewing Culture Yeast

• Saccharomyces Wild Yeast
• +

+ +/- +

Non-Saccharomyces Wild Yeast +

+

• +

+

Bacteria Risk Group NBB Beer Wort Agar / MRS* UBA HLP (Hsu’s Lacto/Pedio) LMDA/SDA

Obligatory Beer Spoilers

+ +

• /+

+ +/- +

Potential Beer Spoilers

+ w/- +/- +

• /+

+

Indirect Beer Spoilers

+

• +

+

• /+

+/-

Indicator Bacteria

+/w

• +

+/-

• Latent Bacteria
• +
• Note: Information taken from Farbatlas und Handbuch der Getränkebiologie, Bd.1, Kultivierung, Methoden, Brauerei, Winzerei, W. Back.

UBA, HLP and LMDA results are of the author‘s personal experience.

Selectivity of traditional detection media

Anaerobic Incubation

• Anaerobic Incubation is

necessary to detect beer spoiling micro-organisms

• Anaerobic Environments

can be achieved using GasPak boxes, pouches, or dedicated anaerobic incubators

• Boxes or Pouches still

need to be incubated at a controlled temperature

Process Sample Valves

• Proper sample valves are needed in
• rder to take samples in process.

These are needed to take microbiological samples, as well as validate processes such as filtration.

• Sample valves are also needed to verify

and adjust inline measurements.

• Sample valves should be of a

construction that allows them to be CIP’d and also flamed for microbiological sampling

• Without sample valves, a process can

become a “black box”, even with inline measurements.

“Step Control” Troubleshooting

• “Step Control” is the method of testing beer after every process, and on every

process input in order to confirm that the process did not cause an unwanted

• utcome.
• Was usually used for microbiological control in order to determine the point of

infection.

• Can be used for other issues, like DO troubleshooting.
• When designing a brewery or an expansion, make sure to include proper sample

valves after every process. You can’t take a sample without a valve!

• Do not expect every supplier to automatically include these. Even on a skid mounted system

Microbiological Control points In Filtration.

Sanitation Management

• The Quality Department typically fulfills the role of plant sanitarian
• Inspection of brewery to ensure GMP compliance
• Develop Master Cleaning Plans for Packaging Equipment, or other areas
• Approve new equipment to ensure clean-ability ,chemical compatibility, AND

SAMPLE PORTS

Sensory

Sensory Lab

• A place that is free from odors and

distractions can be used to taste samples

• The sensory panelists should fill out

sheets (no discussion) in order to avoid influences due to seniority or position

• Training on off-flavors is recommended
• A dedicated sensory lab is not

necessary, but regular tastings are.

Aging Testing

• Retains should be kept until at

least the expiration date

• Should be tasted on some

frequency to monitor shelf life

• Turbidity testing can be a good

indicator of shelf life

• Non-destructive
• Needed in case of complaints
• Example of every batch / lot

should be kept

• Should be kept at room temp. to

more accurately represent storage in trade/retail

• Forced Testing can provide

insight into process changes, but do not accurately represent the flavors in normally aged beer.

Metrology

Quality Assurance and Metrology

• All measurement equipment needs to

have its accuracy verified.

• Equipment that is not measuring

properly will need to be re-calibrated

• Many inline meters can be checked

without removing by analyzing beer from a sample valve with another instrument

• Lab equipment can be checked with

beer from the same run. Purchased beer can also be used for this, but make sure to get beer produced at the same time.

• The accuracy of your data is directly

related to how well your equipment is maintained and calibrated

Statistics

A very short introduction to

Using Control Charts (Turbidity Mystery)

Using Control Charts (Turbidity Mystery cont.)

Using Control Charts (Turbidity Mystery cont.)

Using Control Charts (Happy Ending)

Some notes to Setting Limits

• Some limits might be set by law
• ABV must be +/- 0.3% label claim
• SO2 must be below 10 ppm (to avoid sulfite labelling requirements)
• Control Limits and Specification Limits may have different values or reactions
• A brewery might have a 2x IPA with a control limit of +/-5 IBU, but the Spec Limit might be +/- 10 IBU
• Put another way, you might have to blend a beer that is out of spec (reaction limit), but you would take a

look at your recipe and brewhouse parameters when you have IBUs that are out of control.

• Control Limits should be set based on process capability
• The ASQ Control Charts can give you an idea of where to start
• Spec Limits should be set based on product perception
• Can a trained taster or a customer differentiate between a 5 IBU difference in a particular beer?
• If control limits are set tighter than process capability, you will probably increase variation

by reacting to overly tight control limits

• Remember that you can’t set limits (control or specification) tighter than your measurement

precision.

Brewery Example

Table Stakes:

Process Measurements for every Brewery

• Every brewery has to make decisions on which tests to perform and processes to

monitor

• The responsible person for each measurement needs to be determined
• Prioritize measurements that result in information that you can react to
• Checking carbonation in the Brite Tank prior to packaging
• Checking pH and temperature during mash
• Titration and Tasting of process water
• Extract Efficiency in Brewhouse
• Validate measurements
• Getting false information is not helpful
• Dial Thermometers need to be checked (boiling water / ice bath)
• Record measurements
• A simple paper notebook can be sufficient in a small brewery, if it is well kept.
• Excel spreadsheets are great, plenty of online resources to help figure out functions.

However, Excel will also become cumbersome when trying to keep or process large amounts

• f data.
• Database systems are the best, but unless you are a programmer you will likely want to find

a company to provide that solution. Be wary of “all-in-one” packages that have a quality database rolled into an ERP, or process control software. R is a free database program.

• Every Brewery should be able to measure/test:
• pH
• Important parameter in brewhouse performance (enzyme optimums, extract efficiency, hop utilization rate)
• Needed to help verify that residual cleaner did not contaminate wort or beer. Verification required by FDA. (Rinse water testing)
• Yeast Viability
• Absolutely necessary to ensure fermentation performance, unless 100% of beer is made with yeast bought in

pitchable amounts.

• Improper fermentation is very likely to produce off flavors as well as decrease cellar capacity by extending

fermentation times. A microscope is cheaper than additional fermenters!

• Gravity / Density
• Needed to determine strength of wort (Original Gravity)
• Monitor Fermentation (Apparent Extract)
• Carbonation
• This is a simple test that can be performed with a Zahm & Nagel “shake style” tester
• Cleaning Chemicals
• Can usually get simple “drop test” kits to perform a simple titration from your chemical supplier
• Chemical concentrations are very important to ensure proper cleaning and sanitation, which is a pre-requisite for

quality beer

• Measuring chemicals added to a volume of water is insufficient. CO2 can neutralize caustic, poor rinsing of caustic

can neutralize acid, improperly activated ClO2 is ineffective as a sanitizer, etc.

• Remember to always titrate for carbonates when checking Caustic! CO2 will turn Sodium Hydroxide into Sodium

Carbonate, which has comparatively very little cleaning power. CIP skids with conductivity probes will not catch a CO2 neutralization!

• Taste
• At the very least a “Go / No-Go” taste test should be performed on every beer prior to packaging or serving
• Forced Diacetyl Tastes at end of fermentation.
• A taste of the process water should be done regularly (daily). (Hot Liquor, Cold Liquor, etc.)
• If the water is dechlorinated and stored in a cold liquor tank; beware that this water can contain pathogens.

Table Stakes:

Process Measurements for every Brewery

• Every Packaging Brewery should be able to measure:
• Container Seals
• Crown Crimp Gauges are a minimum for bottles
• Secure Seal Tester is nice to have for larger breweries to compare crowns or bottle finishes
• Micrometer and equipment to tear down can seams are a minimum for canning breweries
• Package Airs or TPO
• Measuring Air in package is a relatively simple caustic titration using equipment from Zahm &

Nagel.

• This equipment is much less expensive compared to DO meters
• Can give you a way to measure headspace O2 levels with bottles packaged weeks ago.
• Is fairly time consuming
• Does not help determine whether the beer has high DO levels.
• TPO (Total Packaged Oxygen)
• Gives you an overall score for how much oxygen was picked up during packaging
• Measured by shaking the package to get the O2 in equilibrium in the package
• Must be measured as soon as possible. Will drop rapidly as the beer chemically oxidizes
• Can be used along with the DO level of the beer to troubleshoot the cause of the TPO

level.

• High TPO w/ Low DO = Headspace issue (FOB, low fills, etc.)
• High TPO w/ High DO = Problem prior to or during filling (High BBT DO, Leaking

Pump Seal, Poor Bottle Evacuation, Improper Undercover Gassing, CO2 impurity)

• TPO is not just the “shaken DO”. Rule of thumb: TPO is always > 2.5x the DO.

Table Stakes:

Process Measurements for every Brewery

• ATP Meter
• Cost is around $2000 for a meter, and about $1 per test.
• Give instant results after cleaning, but do not specify what type of organisms are present

(non beer-spoilers)

• O2 Meter
• O2 Meter can be an invaluable tool to troubleshoot processes and determine points of air

ingress

• Can be used to measure DO and TPO (calculated) in packaging when used with a piercer
• Good beer can be quickly ruined by a bad pump seal or a cracked CO2 line letting in air.
• Cost is around $20k, depending on make and model.
• Optical instruments vs. Membrane instruments

These instruments may be too expensive for a smaller brewery, but every brewery would benefit from them, if they can afford it. All distributing breweries should consider these instruments as important as a hydrometer.

Table Stakes:

Process Measurements for every Brewery WISHLIST

Brewery Lab Space and Requirements

• Water and drains. City water is fine. Nice to have multiple sinks for equipment

connections.

• Counter space. You can’t have too much of this. Build for the future. However leave room

for floor equipment; Fume Hood, Sterile Hood, Centrifuge, Autoclave, etc.

• Power. Make sure to have enough amperage for all of your current and future equipment.

Outlets every 3 feet along benchtop are a good idea. You will likely have some 240V and possibly even 3 phase equipment in the lab.

• Connections for compressed air, CO2 and natural gas are nice to have.
• Floor should be hard surfaced, mop-able. Concrete must be sealed.
• Needs to be kept at constant temp for equipment to function. HVAC
• Safety Shower and storage for compressed gas cylinders, flammable cabinet, acid base

storage.

Small Brewery Quality Program Example

• Taste Process Water Daily
• Check Grist Particle Size Distribution Weekly (Mill sieve test)
• Record Brewhouse Measurements and Calculate Brewhouse Extract Efficiency
• Check Yeast Viability and Concentration on every brew
• Daily Apparent Extract measurements on Fermenters
• Forced Diacetyl Tastes at End of Fermentation, prior to chilling tank
• Check BBT Carbonation prior to packaging
• Taste Beer after Maturation prior to processing into BBT
• Taste Beer prior to packaging
• Taste First bottle/can from Packaging
• Package Airs or DO/TPOs and carbonation.
• Check First and Last package for dilution and pH
• Keep retains of packaged beer to taste and in case of complaints
• Send out samples for analysis if problems occur (high/low AE at EOF, off-flavors, etc.)
• If filtering or treating beer for haze, check in a light box for a comparative turbidity.
• GMP Walkthroughs Monthly
• Verification / Calibration of process thermometers and other instruments on a regular

schedule

• Collect measurement data and use it to generate control charts
• Determine what actions should be taken when measurements are “out of spec”

Resources

• MBAA
• Technical Quarterly
• Local Meetings
• Local Presentations available online
• Ask The Brewmasters Forum
• Comunities of Practice: Container Quality
• Networking!!
• ASBC
• Journal of the ASBC
• Proficiency Testing Program (LPP)
• Methods of Analysis
• Guideline to Growing Your Quality

Laboratory (Equipment List)

• ASQ
• Local Meetings
• Control Chart Templates available for free
• asq.org/quality-resources/control-chart
• FDA has GMP guidelines
• http://www.ecfr.gov/
• Title 21 → Chapter I → Subchapter B → Part

110

• TTB lists regulatory requirements
• List of Accepted Methods of Analysis
• ttb.gov/images/pdfs/ssd/list_of_beverage_meth
• ds.pdf

MBAA Presentations online ASBC Methods

Literature

Available at mbaa.com

• Quality Management: Mary Pellettieri
• Beer Packaging, 2nd Edition: Edited by R. Klimovitz, K. Ockert
• Quality Systems: C. Bamforth
• The Yeast in the Brewery: Annemüller, Manger, Lietz

Available at carllibri.com

• Colour Atlas and Handbook of Beverage Biology: Werner

Back

• MEBAK Volumes: Various

The End

Questions?

bbailey@troegs.com