Beer Stabilization Technology - clearly a matter of choice. International Specialty Products 1361 Alps Road Wayne, NJ U.S.A.

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1 Beer Stabilization Technology - clearly a matter of choice Mustafa Rehmanji, Chandra Gopal and Andrew Mola International Specialty Products 1361 Alps Road Wayne, NJ U.S.A.

2 Scope of Presentation Mechanism of Haze Formation Upstream Stabilization : Polyclar Brewbrite PVPP Silica Gel Tannic acid Papain Admixture : Silica +PVPP

3 What is Beer Stability? Beer stability is the extent to which a beer tastes and looks as good after aging as it did when it was first packaged. Stability is assessed by: Changes in colloidal stability (HAZE) Flavor stability (oxidation and staling) Color increase Microbial stability Reference : Jean De Clerck, A Text Book of Brewing

4 Beer Stabilization Guidelines Drinking Life Stabilization Requirements CASK BEER (UK) 4 weeks None - Low KEG BEER 10 weeks Low - Medium EXPORT KEG 36 weeks Medium SMALL PACK Bottle up to 52 weeks High Cans up to 75 weeks High The extent to which a beer requires colloidal stabilization depends on the raw materials, process, required shelf life and storage conditions

Bottle up to 52 weeks High Cans up to 75 weeks High The extent to which a beer requires

5 Non-Biological Haze in Beer Protein-Polyphenol complexes - chill & permanent haze Carbohydrates - starch & ß-glucans Oxalates Other constituents - metal hazes, collapsed fob, PGA, filter aids, iso-α- acids etc.

6 Change in Polyphenols and Flavanoids During Brewing Total Polyphenols mg/l 1,600 1,400 1,200 1, Total Flavanoid mg/l Mash in Last runnings Copper cast Fermenter Mash end Copper up Whirlpool Maturation Brewing Process Step 1 avoid use of very weak wort(<1.5 P) Polyphenols Flavanoids Polyphenols= EBC Flavanoids = EBC 9.9.2

Copper cast Fermenter Mash end Copper up Whirlpool Maturation Brewing Process Step 1 avoid

7 Model for Protein Polyphenol Interaction Polyphenols are depicted as having two ends that can bind to protein. Proteins are depicted as having a fixed number of polyphenol binding sites. polypeptide Proline-rich rich region polyphenol Courtesy : Karl Siebert, Cornell University Formation of Protein-Polyphenol Haze in Beverages, J. Agric. Food Chem. 1996,44,

Proteins are depicted as having a fixed number of polyphenol binding sites.

8 Chill-Haze Development & Shelf- Life Model (Forced Aging at 37 C) for a Stabilized Standard Lager Beer TtlH Total Haze ( EBC) 5 4 Correlation co-efficient i r = Lag Phase Haze Development Rate = 0.47 EBC units/week 1 Shelf life (Time to develop haze = 2 EBC) Permanent or background haze Storage Time (weeks)

9915 3 2 Lag Phase Haze Development Rate = 0.

9 Relative Haze Formation Beer stabilized with 100 g/hl PVPP to remove reactive polyphenols Catechin Haze EBC Catechin Oxidized Catechin Tannic acid Addition rate of reactive polyphenols in g/hl Tannic Haze EBC Step 2 minimize oxygen pick-up! < 0.1 ppm

8 Catechin Oxidized Catechin Tannic acid 0 10 20 30 40 50 Addition rate of

10 Carbohydrate Hazes Prevention - raw material selection - complete starch conversion - process effects identify sources of shear damage Remedies - enzymes - ß-glucanase, amylases dextrinases

11 Oxalate Haze - Green Haze Beer stone - calcium oxalate Octahedral crystal Check oxalic acid levels in malt Treated by addition of calcium salts (CaSO 4 ) to brewing liquor to precipitate oxalate

12 Raw Material & Process Strategies to Optimize Colloidal Stability Process Polyphenol Reduction Protein Reduction Process Optimization Raw material selection Brewhouse Fermentation/ Maturation Low proanthocyanidin malt Hop extract High adjunct ratio Avoid weak worts Rapid onset to fermentation Low protein barley Mashing process ph, temperature Good hot break Early yeast removal Low malt modification Coarse grind of malt Vigorous kettle boil for >60 min. Avoid excess mineral salts Cold wort filtration Minimum 7 days maturation at -1 O C Filtration Low solids count Filter at -1 O C Avoid O2 Pick up Step 3 check & verify cold storage temperatures

Mashing process ph, temperature Good hot break Early yeast removal Low malt modification Coarse grind of malt Vigorous kettle boil for >60 min.

13 Colloidal Stabilization of Beer Adsorption: - Silica gel Adsorption: o - Polyclar Plus (PVPP-Si composites) -Resins Adsorption: - Polyclar (PVPP) Composition of Chill Haze PROTEINS 40-75% Carbohydrates 3-13% Ash 0.7-5% Cu,Fe Traces POLYPHENOLS About 17% Other Polyphenol: P l h l - PVP or PVP-silica Precipitation: -Tannic acid Degradation: - Papain Protein-Tannoid complex: - Chilling

14 What is Polyclar Brewbrite? It is a proprietary composite of a selected Carrageenan and micronized PVPP Kappa Carrageenan PVPP OSO - 3 O CH 2 OH O O O CH 2 O O N O N O N O OH OH ß-D-galactose l 4 sulfate 3,6-anhydro-α-D-galactose n 2-pyrrolidinone,1-ethenyl-, l homopolymer n Marine polysaccharide of galactose & galactose sulfate monomers Cross-linked polyvinylpyrollidone

PVPP OSO - 3 O CH 2 OH O O O CH 2 O O N O N O N O OH OH ß-D-galactose l 4 sulfate

15 Courtesy of Murphy-Savilles Clarification Effect of Cold Wort Clarity on Beer Clarity Bright 3 (<3 EBC) Hazy 2 Clarity (>4 EBC) Rating Cloudy 1 (>8 EBC) Filtered Beer Haze (EBC) Step 4 wort clarity is very important and is related to beer clarity

EBC) Rating Cloudy 1 (>8 EBC) 0 0.7 1.4 2.

16 Increase in Wort Yield - Commercial Trial Polyclar Brewbrite gave 3.2% increase in cold wort collected in FV as compared to untreated wort Volum me of Wort at collectio on, hl Untreated Carrageenan, alone 3.9g/hl Polyclar Brewbrite 15g/hl

Volum me of Wort at collectio on, hl 16.1 16.0 15.9 15.8 15.7 15.6 15.

17 Decrease in Fermentation Time with Polyclar Brewbrite - Commercial Trial Polyclar Brewbrite gave 10 % reduction in fermentation time as compared to untreated Untreated Carrageenan alone, 3.9g/hl Polyclar Brewbrite, 15g/hl

fermentation time as compared to untreated 145 140 135 130

18 Analysis of Packaged Beer - Commercial Trial Accelerated Forcing Test 3.5 Haze, EBC Un nits Total 3.0 Polyclar Brewbrite, g/hl Untreated 0.0 Initial Cycle 1 Cycle 2 Cycle 3 Cycle 4 Cycle 5 Cycle = 24 hours at 60 0 C followed by 24 hours at 0 0 C No. of Cycles (to reach 2.0 EBC Units) = month of predicted shelf life

19 Summary of Trial Results with Polyclar Brewbrite Enhances clarity of wort & beer Increases wort production Decreases fermentation time Improves total productivity of plant Extends shelf life of packaged beer Longer shelf life requires PVPP treatment at filtration PVPP helps reduce astringency in beer* * Measuring Astringency of Beverages using a Quartz-Crystal Microbalance J.Am.Soc. Brew. Chem. 61(3): , 2003

packaged beer Longer shelf life requires PVPP treatment at filtration PVPP helps reduce astringency in

20 Single use PVPP - Methods of Use Added prior to primary filtration and removed at the filtration stage Regeneration Used after primary filtration on a horizontal leaf filter or candle filter and then recovered for re-use

Regeneration Used after primary filtration on a

21 Stabilization with PVPP Slurried in deaerated d water (8-10% wt/wt) t) Hydrated for 1 hour (maximum efficacy) Added to beer during transfer Single use - usually added before DE filter min. contact time Regeneration grade -added d after DE filtration

22 Possible Injection Points for Polyclar Plus and Polyclar PVPP Inlet Buffer Tank DE Stabilizer Dosing Tank DE Filter Buffer Tank To Packaging Bright Beer Tank Trap/Bag Filter Polish Filter

23 Tannoid Reduction with PVPP Tannoids (m mg/l PVP K-90 to peak haze) Detection limit mg/l Untreated 10 g/hl 30 g/hl 50 g/hl Polyclar 10 (g/hl) Step 5 reduce the tannoids with PVPP

24 Increase in Shelf Life of PVPP 8 - Treated Beer Predict ted Shelf Life (mont hs) Untreated 10 g/hl 20 g/hl 30 g/hl 50 g/hl Polyclar 10 (g/hl)

25 Hydrogels vs. Xerogels Hydrogel Contain 30-50% water Easier to disperse Used at up to ~150 g/hl Less effective than xerogels Greater permeability than xerogel Less microbial stability Xerogel Contain 5% water Harder to hydrate & disperse (more dusty) Used at up to ~80 g/hl More effective than hydrogel Greater microbial stability

26 Action of Silica gel Protein adsorption follows three sequential steps: Diffusion of proteins from the beer matrix to the surface of the silica gel (relatively fast step) Attraction: Surface adsorption of proteins to the hydrated silica gel (relatively fast step) Penetration of the surface adsorbed proteins into the silica gel (rate determining step)

27 Protein Stabilizers - Tannic Acid From (Chinese) gallnuts Complexes with haze-active proteins Used at low dosage rates 4-10g/hL Added between FV & MV, or, In-line to DE filter Minimum contact time 10 min. Cannot be used at the same time as PVPP, but can be used sequentially tannic first, then PVPP

28 Protein Stabilizers - Papain Proteolytic enzyme - from papaya Four iso-enzymesy Degrades proteins - non-specific Used at low concentrations 1-6 g/hl Added at maturation or beer filtration Activated during pasteurisation Persists in beer Adverse impact on beer foam

29 What is Polyclar Plus? A proprietary p composite of micronized Polyvinylpolypyrrolidone (PVPP) and selected Silica Xerogel

30 (Warm Da ays) 0 /24 hr. Cycles to 2 EBC 60 C C/24 hr. - Predicted Shelf Results- Plant Trial with Polyclar Plus (Composite 70%Si + 30%PVPP) Si hydrogel Si hydrogel 95 g/hl 95 g/hl + PVPP 20 g/hl Polyclar Plus g/hl Step 6 Balanced stabilization ti is efficient i and cost effective

31 Brewery Trials Filter Pressures, Run Lengths & Beer Stability with Polyclar Plus Stabilizer Dose rate g/hl ΔP/hr* Filter Run Time (hr.) Total Haze** (EBC) Xerogel only PVPP only Polyclar Plus *Pressure increase at steady state Pressure increase at steady state **Total haze measured at 0 o C after 5 days incubation at 60 o C

32 Beer Transport Haze EBC Store 0 C Store 40 C Cycled Shaken 40 C Treatments Step 7 don t forget the beer after it leaves the brewery!

33 Seven Steps to Colloidal Stability 1. Avoid use of very weak wort(<1.5 P) 2. Minimize O 2 pickup throughout the brewing process(<0.1 ppm dissolved O 2 in beer ex-fermenter and into package) 3. Cold store, transfer & filter beer at 0 o C, or below 4. Wort & beer clarity are important optimize finings & filter aid use 5. Ensure that the tannoids are reduced (removed) from fresh beer use PVPP 6. Balanced stabilization is efficient and cost effective silica + PVPP 7. Consider beer transport & storage

34 Thank You!

POLYCLAR PLUS USER GUIDE. Balanced Stabilization Prevents Chill Haze Extends Shelf-Life Enhances Flavor Stability Extends Filtration

POLYCLAR PLUS USER GUIDE. Balanced Stabilization Prevents Chill Haze Extends Shelf-Life Enhances Flavor Stability Extends Filtration POLYCLAR PLUS Prescription Clarification and Stabilization of Beer Balanced Stabilization Prevents Chill Haze Extends Shelf-Life Enhances Flavor Stability Extends Filtration USER GUIDE PERFORMANCE ENHANCING