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Dry-hopping Beer and Achieving Consistent Flavor Shellhammer Laboratory Department of Food Science and Technology

Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

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Page 1: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Dry-hopping Beer and Achieving Consistent Flavor

Shellhammer Laboratory Department of Food Science and Technology

Page 2: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

WHIRLPOOL VS. DRY- HOPPING: SENSORY ANALYSIS

Daniel Sharp, Ph.D.Director of Brewing OperationsNinkasi Brewing Company

Page 3: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Hop Aroma:Late vs. Dry Hopping• Background• Basics of Experimental

Design and Setup• Results

OREGON STATE UNIVERSITY

Page 4: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Background and literature review

Page 5: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Background and literature review

Page 6: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Background and literature review

Page 7: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Background and literature review

Page 8: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Background and literature review

Page 9: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Background and literature review

Page 10: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Contributions of select hopping regimes to the terpenoid and aroma profile of ale and lager beers.

Overall

Pine ResinousGrassy Hay

Herbal

FloralCitrus

Stone Fruit

Tropical Fruit

Cooked Veg

Control iso

DH HHA WP HHA

KH HHA

KH Simcoe

DH Simcoe

WP Simcoe

F2 (2

0.37

%)

F1 (75.72%)

PCA Sensory Biplot (96.09%)

Descriptor Group 1 Group 2 Group 3

HHA – Hallertau MFControl – Isohop onlyKH – Kettle Boil (60 min)WP – Whirlpool (10 min)DH – Dry-hop (48 hours)

Daniel C. Sharp, Yanping Qian, Gina Shellhammer & Thomas H. Shellhammer (2018) Contributions of Select Hopping Regimes to the Terpenoid Content and Hop Aroma Profile of Ale and Lager Beers, Journal of the American Society of Brewing Chemists, 75:2, 93-100, DOI: 10.1094/ASBCJ-2017-2144-01

Page 11: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

EXPERIMENTAL DESIGN

Page 12: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Experimental DesignObjectives:• Minimize confounding variation• Factors: Cultivar (12) and Addition (2)

• Subfactors: KO order, Kettle boil, Fermentation variation

Challenges:• Only 2 factors but total treatments = 24• Complete design = 50 units *3 Kettle boils

(* 6 sensory reps = 300 samples.• Brew length

Page 13: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Experimental DesignExperimental Controls• Common wort stream• Psuedo Replication• Split Kettle Boils

• Blocked treatments• Small Treatment vessels

Page 14: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Experimental Setup12 CultivarsAmarilloCascadeChinookCitraHalletauer MittlefrühHuell MelonGalaxyMosaicNelson SauvinNuggetSimcoeSaazUnhopped

Base• 12°P wort• 100% pale ale malt• California ale (18°C)• 25 ppm IAAHopping – 4 g/L (~1 lb BBL)• Whirlpool: 25 min @ 87-95°C• Dry-hopping: 72 hours @ 18°C on yeast at cap. Analysis• Triangle tests on Reps• Descriptive sensory analysis on all treatments

Page 15: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

SENSORY RESULTS

Page 16: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

PCA biplot of Descriptive Data

OHAIherbal/spicey

pine/resinoustropical fruit

green/vegetalcitrus

floralfruity

catty/sweatyAmarillo DH

Chinook DH

Citra DH

Citra WP

Galaxy DH

Mosaic DH

Mosaic WP

Nelson Sauvin DH

Simcoe DH

Amarillo WP

Cascade DH

Cascade WP

Chinook WP

Galaxy WP

Hallertau MF DH

Hallertau MF WP

Huell Melon DH

Huell Melon WP

Nelson Sauvin WP

Nugget DHNugget WP

Saaz DH

Saaz WP

Simcoe WP

Control

F2 (8

.5%

)

F1 (79.5%)

Descriptor Group 1 Group 2 Group 3

Sharp, 2016

Page 17: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

PCA biplot of Descriptive Data

OHAIherbal/spicey

pine/resinoustropical fruit

green/vegetalcitrus

floralfruity

catty/sweatyAmarillo DH

Chinook DH

Citra DH

Citra WP

Galaxy DH

Mosaic DH

Mosaic WP

Nelson Sauvin DH

Simcoe DH

Amarillo WP

Cascade DH

Cascade WP

Chinook WP

Galaxy WP

Hallertau MF DH

Hallertau MF WP

Huell Melon DH

Huell Melon WP

Nelson Sauvin WP

Nugget DHNugget WP

Saaz DH

Saaz WP

Simcoe WP

F2 (8

.5%

)

F1 (79.5%)

Descriptor Group 1 Group 2 Group 3

Sharp, 2016

Page 18: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

PCA biplot of Descriptive Data

OHAIherbal/spicey

pine/resinoustropical fruit

green/vegetalcitrus

floralfruity

catty/sweatyAmarillo DH

Chinook DH

Citra DH

Citra WP

Galaxy DH

Mosaic DH

Mosaic WP

Nelson Sauvin DH

Simcoe DH

Amarillo WP

Cascade DH

Cascade WP

Chinook WP

Galaxy WP

Hallertau MF DH

Hallertau MF WP

Huell Melon DH

Huell Melon WP

Nelson Sauvin WP

Nugget DHNugget WP

Saaz DH

Saaz WP

Simcoe WP

F2 (8

.5%

)

F1 (79.5%)

Descriptor Group 1 Group 2 Group 3

Sharp, 2016

Page 19: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

PCA biplot of Descriptive Data

OHAIherbal/spicey

pine/resinoustropical fruit

green/vegetalcitrus

floralfruity

catty/sweaty

F2 (8

.5%

)

F1 (79.5%)

Descriptor Group 3

Sharp, 2016

Page 20: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

PCA biplot of Descriptive Data

OHAIherbal/spicey

pine/resinoustropical fruit

green/vegetalcitrus

floralfruity

catty/sweaty

F2 (8

.5%

)

F1 (79.5%)

Descriptor Group 3

Sharp, 2016

Page 21: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Take-aways

• Normal process variation = minimal effect• Extraction efficiencies may be very low• Dry-hopping increases aromatic intensity relative to late hopping

• Aroma character may be significantly difference between the two

OREGON STATE UNIVERSITY 20

Page 22: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

DOSING RATES AND EXTRACTION EFFICIENCIES

Scott LafontaineDoctoral CandidateOregon State University

Page 23: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Background

Region Farm (coded)

OSU Hop Oil (ml/100g)

CAS_12_16 WA 2 0.5CAS_27_16 WA 1 0.6CAS_21_16 ID 10 0.6CAS_22_16 ID 10 0.6CAS_24_16 WA 9 0.6CAS_07_16 ID 7 0.7CAS_09_16 ID 14 0.8CAS_19_16 WA 20 0.8CAS_04_16 WA 5 0.8CAS_25_16 OR 13 0.8CAS_26_16 WA 12 0.9CAS_06_16 ID 7 0.9CAS_05_16 WA 5 1.0CAS_11_16 WA 2 1.0CAS_16_16 WA 15 1.1CAS_17_16 OR 17 1.1CAS_15_16 WA 16 1.2CAS_03_16 OR 4 1.2CAS_23_16 WA 21 1.2CAS_20_16 WA 19 1.3CAS_28_16 WA 1 1.4CAS_29_16 WA 11 1.4CAS_02_16 OR 4 1.4CAS_08_16 OR 8 1.5CAS_13_16 WA 2 1.5CAS_10_16 WA 2 1.5CAS_01_16 OR 4 1.7CAS_18_16 WA 18 1.7CAS_14_16 WA 2 2.6

29 Sample lots19 Farms13 Unique oil

valuesDry hopped at

3.8g/L

Cascade from 2015 Harvest

Page 24: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Background

Region Farm (coded)

OSU Hop Oil (ml/100g)

CAS_12_16 WA 2 0.5CAS_27_16 WA 1 0.6CAS_21_16 ID 10 0.6CAS_22_16 ID 10 0.6CAS_24_16 WA 9 0.6CAS_07_16 ID 7 0.7CAS_09_16 ID 14 0.8CAS_19_16 WA 20 0.8CAS_04_16 WA 5 0.8CAS_25_16 OR 13 0.8CAS_26_16 WA 12 0.9CAS_06_16 ID 7 0.9CAS_05_16 WA 5 1.0CAS_11_16 WA 2 1.0CAS_16_16 WA 15 1.1CAS_17_16 OR 17 1.1CAS_15_16 WA 16 1.2CAS_03_16 OR 4 1.2CAS_23_16 WA 21 1.2CAS_20_16 WA 19 1.3CAS_28_16 WA 1 1.4CAS_29_16 WA 11 1.4CAS_02_16 OR 4 1.4CAS_08_16 OR 8 1.5CAS_13_16 WA 2 1.5CAS_10_16 WA 2 1.5CAS_01_16 OR 4 1.7CAS_18_16 WA 18 1.7CAS_14_16 WA 2 2.6

29 Sample lots19 Farms13 Unique oil

valuesDry hopped at

3.8g/L

Cascade from 2015 Harvest

Selected one Cascade lot and dry-hopped at 4 distinct levels

0 g/hL 2 g/L0.5 lb/Bbl

3.8 g/L1 lb/Bbl

8 g/L2 lb/Bbl

16 g/L4 lb/Bbl

Page 25: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

The main goal of this project was to determine a dose response curve for Cascade hop aroma.

Main objective

Page 26: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

The main goal of this project was to determine a dose response curve for Cascade hop aroma.

Does more hop material = more aroma?

Main objective

Page 27: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Things to consider when dry-hopping on small scale..

• Sample inhomogeneity• Dissolved oxygen uptake• Package scalping

Page 28: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Hop Preparation and Dry-Hopping Parameters

• Blend brewer’s cuts of whole cone hops by grinding

Page 29: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Brewing “unhopped” beer

Beer Specifications:• Grist:

• 85% Pale 2-row• 13.5% Carmel 10L• 0.5% Carmel 120L

• Original Gravity: 10.6 P• Real Extract: 3.16 P• BU = 20 mg/L (iso-extract)• ABV = 4.8 % ABV

Page 30: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

OSU’s current small-scale dry-hopping process• All dry-hop events occur in duplicate (40 L beer each)

• During filtration 2 kegs are blended during filtration into 1 keg• Oxygen monitoring

DH Event 1 DH Event 2

Dry-hop for 24 hrs

Filtration

Carbonated

DO

DO

Spec. 110 ppb

3.8 g/L 3.8 g/L

3.8 g/Ltreatment

Vollmer, D. et. al. J. Am. Soc. Brew. Chem. 74(4):242-249, 2016

Page 31: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Evaluations using draft beer Minimized total package oxygen Great for sensory testing implementation

Page 32: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Sensory evaluation - descriptive analysis

Page 33: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Sensory evaluation – descriptive analysis external controls

AttributesBase

(No dry hop)

3.8 g/L 16 g/LBallast Point Grapefruit

Sculpin

Hop ValleyCitrus

Mistress

Asse

ss D

escr

ipto

rs B

ased

on

Aro

ma

Onl

y Overall Hop Aroma Intensity 0 8-9 14-15 14-15 7-8

Citrus 0 7-8 5-6 13-14 6-7

Herbal/Tea 0 5-6 12-13 1-2 6-7

• Panelists came to consensus for attributes on commercial and internally made samples

• References were served to panelists at each DA session

Page 34: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

SENSORY RESULTS

Page 35: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Hop dosage rate – Overall Hop Aroma Intensity

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

0 2 4 6 8 10 12 14 16 18

Sens

ory

Scor

e (1

5pt s

cale

)

Dry Hop rate (g/L)

Overall Hop Aroma Intensity

Page 36: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

*Letters represent Tukey’s HSD groupings

• Panelists could discriminate the different dry hop rate samples (ie 0, 2, 3.8, 8, & 16)

Hop dosage rate – Overall Hop Aroma Intensity

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

0 2 4 6 8 10 12 14 16 18

Sens

ory

Scor

e (1

5pt s

cale

)

Dry Hop rate (g/L)

a

a

b

cc Overall Hop Aroma Intensity

Page 37: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

0 2 4 6 8 10 12 14 16 18

Sens

ory

Scor

e (1

5pt s

cale

)

Dry Hop rate (g/L)

c

a

a

b

c

• Panelists scaled the samples randomly against 28 other samples in the DA panel• Range of DA OHAI ratings (i.e. ~6- 9.5) for 2015 DA Panels –Same DH rate 3.8/g/L

*Letters represent Tukey’s HSD groupings

Hop dosage rate – Overall Hop Aroma Intensity

Overall Hop Aroma Intensity

Page 38: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

0 2 4 6 8 10 12 14 16 18

Sens

ory

Scor

e (1

5pt s

cale

)

Dry Hop rate (g/L)

Herbal/ Tea

Citrus

Overall Hop Aroma Intensity

Hop dose response – hoppy quality (citrus and herbal/tea)

Page 39: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

• Herbal/ Tea response is similar to OHAI

*Letters represent Tukey’s HSD groupings

Hop dose response – hoppy quality (citrus and herbal/tea)

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

0 2 4 6 8 10 12 14 16 18

Sens

ory

Scor

e (1

5pt s

cale

)

Dry Hop rate (g/L)

a

a

b

c

c

c

c

ba

aa

a

bb b

Herbal/ Tea

Citrus

Overall Hop Aroma Intensity

Page 40: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

0 2 4 6 8 10 12 14 16 18

Sens

ory

Scor

e (1

5pt s

cale

)

Dry Hop rate (g/L)

b

a

• Citrus response seemed to be suppressed compared to OHAI and Herbal/Tea

Hop dose response – hoppy quality (citrus and herbal/tea)

*Letters represent Tukey’s HSD groupings

Hop dose response – hoppy quality (citrus and herbal/tea)

a

a

b

c

c

c

c

ba

aa

a

bb b

Herbal/ Tea

Citrus

Overall Hop Aroma Intensity

Page 41: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

CHEMISTRY RESULTS

Page 42: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Solid phase micro extraction GC/MS – Hop volatiles (In Beer)

Dry hopped beer

Internal Standard4-octanol

Target Hop AnalytesLinaloolTerpinen-4-olα-terpineolNerolPhenyl AcetateGeraniolGeranial-citralMethyl GeranateGeraniol Acetateβ-Caryophellyeneα-Humuleneβ-FarneseneGernyal Isobutyrate

Page 43: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Solid phase micro extraction GC/MS – Hop volatiles (In Beer)

Dry hopped beer

Internal Standard4-octanol

Target Hop AnalytesLinaloolTerpinen-4-olα-terpineolNerolPhenyl AcetateGeraniolGeranial-citralMethyl GeranateGeraniol Acetateβ-Caryophellyeneα-Humuleneβ-FarneseneGernyal Isobutyrate

Page 44: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

0

0.5

1

1.5

2

0 2 4 6 8 10 12 14 16 18N

erol

(ppb

)Dry hop rate (g/L)

Hop Compound Concentrations – Terpene Alcohols

#Estimated values lower than LOQ*Average of 4 SPME-GC/MS instrumental runs

020406080

100120

0 2 4 6 8 10 12 14 16 18

Lina

lool

(ppb

)Dry hop rate (g/L)

0

10

20

30

40

0 2 4 6 8 10 12 14 16 18

Ger

anio

l (pp

b)

Dry hop rate (g/L)

##

Page 45: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

020406080

100120

0 2 4 6 8 10 12 14 16 18

Lina

lool

(ppb

)Dry hop rate (g/L)

0

0.5

1

1.5

2

0 2 4 6 8 10 12 14 16 18N

erol

(ppb

)Dry hop rate (g/L)

0

10

20

30

40

0 2 4 6 8 10 12 14 16 18

Ger

anio

l (pp

b)

Dry hop rate (g/L)

##

#Estimated values lower than LOQ*Average of 4 SPME-GC/MS instrumental runs

Detection threshold 1 ppba

Detection threshold 4 ppba

aKishimoto J. Agric. Food Chem Vol 54, no 23. 2006

Hop Compound Concentrations – Terpene Alcohols

Page 46: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Hop total oil + compositional analysis

Internal Standard2-octanol

Target Hop AnalytesLinaloolTerpinen-4-olα-terpineolNerolPhenyl AcetateGeraniolGeranial-citralMethyl GeranateGeraniol Acetateβ-Caryophellyeneα-Humuleneβ-FarneseneGernyal Isobutyrate

Page 47: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Hop Compound % Extraction – Terpene Alcohols

05

10152025

0 2 4 6 8 10 12 14 16 18% L

inal

ool e

xtra

cted

fr

om h

op m

ater

ial

Dry hop rate (g/L)

01234567

0 2 4 6 8 10 12 14 16 18% G

eran

iol e

xtra

cted

fr

om h

op m

ater

ial

Dry hop rate (g/L)

01234567

0 2 4 6 8 10 12 14 16 18%

Ner

ol e

xtra

cted

fr

om h

op m

ater

ial

Dry hop rate (g/L)*Assuming 100% extraction based on hop oil hydrodistillation

Dry hop rate

Terpene alcohol extraction (%)

Page 48: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Dry hopping having other impacts on beer……

4.04.14.24.34.44.54.6

0 2 4 6 8 10 12 14 16 18

pH

Dry Hop Rate (g/L)Bitterness?

pH-Flavor Stability?RE-Bottle Carbonation?

*pH and RE measured using Anton Paar Alcolyzer

*BU measured using ASBC MOA Beer-23

3.10

3.20

3.30

3.40

3.50

3.60

0 2 4 6 8 10 12 14 16 18

Real

Ext

ract

w/w

%

Dry Hop Rate (g/L)

0.05.0

10.015.020.025.030.0

0 5 10 15 20

BU

Dry hopping rate (g/L)

BUHumulinonesISO Alpha Acid

Page 49: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Conclusions

• More hops is not an efficient way of adding aroma to beer• Soon to be published.. Impact of static dry-hopping rate on the sensory

and analytical profiles of beer

• Can spent dry-hops be reused? •Look for Dean Hauser’s work at Brewing Summit- “The Extraction Efficiency of Hop Bitter Acids and Volatiles During Dry-Hopping”

Page 50: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

BITTERNESSOF DRY-HOPPED BEER

Thomas H. Shellhammer, PhDNor’Wester Professor of Fermentation ScienceOregon State University

Page 51: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

How does the nonvolatile fraction influence dry-hopped beer quality?

OREGON STATE UNIVERSITY

Page 52: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

How does the nonvolatile fraction influence dry-hopped beer quality?

OREGON STATE UNIVERSITY

Cellulose/Lignin 35%

Protein 15%

Hop acids 20%

Essential oils 3%

Polyphenols/Tannins 5%

Carbohydrates 4%

Minerals 8%

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How does the nonvolatile fraction influence dry-hopped beer quality?

OREGON STATE UNIVERSITY

Cellulose/Lignin 35%

Protein 15%

Hop acids 20%

Essential oils 3%

Polyphenols/Tannins 5%

Carbohydrates 4%

Minerals 8%

Page 54: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Hop acids (up to ~20% of hops)

OREGON STATE UNIVERSITY

Alpha Acids

Beta Acids

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Hop acids (up to ~20% of hops)

OREGON STATE UNIVERSITY

Alpha Acids

Iso-Alpha Acids

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Hop acids (up to ~20% of hops)

OREGON STATE UNIVERSITY

Alpha Acids

Iso-Alpha Acids

Humulinones(oxidized alpha acids)

Page 57: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Hop acids (up to ~20% of hops)

OREGON STATE UNIVERSITY

Beta AcidsHulupones

(oxidized beta acids)

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Hop acids – what you may find in beer

OREGON STATE UNIVERSITY

Alpha Acids

Humulinones(oxidized alpha acids)

Hulupones(oxidized beta acids)

Iso-Alpha Acids

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Hop acids – what you may find in beer

OREGON STATE UNIVERSITY

Alpha Acids

Humulinones(oxidized alpha acids)

Hulupones(oxidized beta acids)

Iso-Alpha Acids

X

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Regarding dry-hopped beers…Does BU work? What drives bitterness?

Beer: 121 unique brands from 42 breweries • 30 brands multi rep study + 91 brands single rep study

Chemical analysis: 7 factors• Iso-alpha acids, oxidized hop acids, alpha acids, TPP, • ABV, RE, pH• BU

Sensory analysis: • Bitterness intensity • Multiple Replication study: data for model building• Partial Replication study: data for model testing

OREGON STATE UNIVERSITY

Page 61: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Chemistry of beers in commercial survey

OREGON STATE UNIVERSITY

3.8

4.0

4.2

4.4

4.6

4.8

5.0

5.2

5.4

5.6

5.8

pH

5 15 25 35 45 55 65 75

Iso (mg/L)

Multi rep Single rep

2.5

3.0

3.5

4.0

4.5

5.0

5.5

6.0

6.5

7.0

7.5

8.0

8.5

9.0

RE (%)

4.0

4.5

5.0

5.5

6.0

6.5

7.0

7.5

8.0

8.5

9.0

9.5

10.0

ABV (%)

120

200

280

360

440

520

600

680

TPP (mg/L)

0 5 10 15 20 25

Alpha (mg/L)

0 10 20 30 40 50 60 70

Humulinones (mg/L)

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Bitterness comes from Isos & HumulinonesBU predicts bitterness

OREGON STATE UNIVERSITY

0

2

4

6

8

10

12

14

16

18

20

0 20 40 60 80 100 120M

easu

red

Sesn

ory

Bitt

erne

ss

Bitterness Unit

0

2

4

6

8

10

12

14

16

18

20

0 20 40 60 80

Mea

sure

d Se

snor

y Bi

tter

ness

Humulinones (mg/L)

0

2

4

6

8

10

12

14

16

18

20

0 20 40 60 80

Mea

sure

d Se

snor

y Bi

tter

ness

Isohumulone (mg/L)

0

2

4

6

8

10

12

14

16

18

20

0 20 40 60 80 100 120

Mea

sure

d Se

snor

y Bi

tter

ness

(Isohumulone + Humulone) (mg/L)

Page 63: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

OREGON STATE UNIVERSITY

0

2

4

6

8

10

12

14

16

18

20

0 20 40 60 80

Mea

sure

d Se

snor

y Bi

tter

ness

Humulinones (mg/L)

0

2

4

6

8

10

12

14

16

18

20

0 20 40 60 80 100 120

Mea

sure

d Se

snor

y Bi

tter

ness

Bitterness Unit

0

2

4

6

8

10

12

14

16

18

20

0 20 40 60 80 100 120

Mea

sure

d Se

snor

y Bi

tter

ness

(Isohumulone + Humulone) (mg/L)

0

2

4

6

8

10

12

14

16

18

20

0 20 40 60 80

Mea

sure

d Se

snor

y Bi

tter

ness

Isohumulone (mg/L)

Bitterness comes from Isos & HumulinonesBU predicts bitterness

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OREGON STATE UNIVERSITY

Bitterness comes from Isos & HumulinonesBU predicts bitterness

Hahn, C, Lafontaine, S.R., Pereira, C.B. and Shellhammer, T.H. 2018. Evaluation of the Nonvolatile Chemistry Affecting the Sensory Bitterness Intensity of Highly Hopped Beer, Journal of Agricultural and Food Chemistry

Page 65: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

HOP CREEP

Page 66: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

1.005

1.010

1.015

1.020

1.025

1.030

1.035

1.040

1.045

1.050

0 2 4 6 8 10 12

Dens

ity (g

/m3)

Days after start of fermentation

Typical fermentation, no dry-hopping

OREGON STATE UNIVERSITY

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1.005

1.010

1.015

1.020

1.025

1.030

1.035

1.040

1.045

1.050

0 2 4 6 8 10 12

Dens

ity (g

/m3)

Days after start of fermentation

Dry-hopping can create “Hop Creep”

OREGON STATE UNIVERSITY

Dry hop addition

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Cascade hops have broad (low) enzyme activities

Enzyme Hops Malt (130 dp)

α-amylase 0.35 198

β-amylase 0.41 13

Amyloglucosidase 0.02 NA

Limit dextrinase <0.01 NA

OREGON STATE UNIVERSITY

Page 69: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

Hop enzymes stimulate “after-fermentation”AKA – Hop Creep

1.5

2

2.5

3

3.5

4

0 10 20 30 40

Real

Ext

ract

(°P)

Days

Beer + Yeast

Beer + Yeast + Hops

Beer

Beer + Hops

OREGON STATE UNIVERSITY

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0

100

200

300

400

500

600

700

1.005

1.010

1.015

1.020

1.025

1.030

1.035

1.040

1.045

1.050

1.055

0 5 10 15 20 25

Diac

etyl

(ppb

)

Dens

ity (g

/m3)

Days after start of fermentation

Hop Creep & Diacetyl issues

OREGON STATE UNIVERSITY

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0

100

200

300

400

500

600

700

1.005

1.010

1.015

1.020

1.025

1.030

1.035

1.040

1.045

1.050

1.055

0 5 10 15 20 25

Diac

etyl

(ppb

)

Dens

ity (g

/m3)

Days after start of fermentation

Hop Creep & Diacetyl issues

OREGON STATE UNIVERSITY

Dry hop addition

Page 72: Dry-hopping Beer and Achieving Consistent Flavor...Overall Pine Resinous Grassy Hay Herbal Floral Citrus Stone Fruit Tropical Fruit Cooked Veg Control iso DH HHA WP HHA KH HHA KH Simcoe

HOP ENZYMES PERSIST IN PACKAGED BEER

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Dry hopping schedule:• 2 days after yeast harvest• Dry hop warm• 2-4 lb/bbl hops• 2 dry hop additions• 7 days on hops

Finishing:• Crash cool• Centrifuge• Up to 24 hours hold

prior to packaging

Enzyme action during production and post-packaging

OREGON STATE UNIVERSITY

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Sampling plan

• Pre-dry hop addition• Pre-second dry hop addition• 24 hours• 48 hours• 72 hours

In-process samples

Samples measured on Anton Paar Alcolyzer/Densitometer & HPLC

• Fresh• Force aged (3 days @ 37°C)• 3 months 25C (packaged 3 months earlier)

Finished beer samples

RE (°P)Maltose (g/100 mL)ABV (% v/v)

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Results: before dry-hopping

0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

4.5

5

5.5

6

6.5

7

7.5

8

8.5

Pre- dry hopaddition

Pre- second dryhop addition

24 Hours after2nd dry hop

48 hours after2nd dry hop

72 hours after2nd dry hop

Fresh Force Aged 3 Months

RE (°P)Maltose (g/100 mL)ABV (% v/v)

Mal

tose

(g/1

00 m

L)

ABV

(% v

/v) &

°P

7.63%

5.11 °P

0.00 g/100 mL

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Results: during dry-hopping

0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

4.5

5

5.5

6

6.5

7

7.5

8

8.5

Pre- dry hopaddition

Pre- second dryhop addition

24 Hours after2nd dry hop

48 hours after2nd dry hop

72 hours after2nd dry hop

Fresh Force Aged 3 Months

RE (°P)Maltose (g/100 mL)ABV (% v/v)

Mal

tose

(g/1

00 m

L)

ABV

(% v

/v) &

°P

Maltose increases after first dry hop addition

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Results: fresh

0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

4.5

5

5.5

6

6.5

7

7.5

8

8.5

Pre- dry hopaddition

Pre- second dryhop addition

24 Hours after2nd dry hop

48 hours after2nd dry hop

72 hours after2nd dry hop

Fresh Force Aged 3 Months

RE (°P)Maltose (g/100 mL)ABV (% v/v)

Mal

tose

(g/1

00 m

L)

ABV

(% v

/v) &

°P

Maltose increases from post dry hopping to fresh package

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Results: force aged 37°C

0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

4.5

5

5.5

6

6.5

7

7.5

8

8.5

Pre- dry hopaddition

Pre- second dryhop addition

24 Hours after2nd dry hop

48 hours after2nd dry hop

72 hours after2nd dry hop

Fresh Force Aged 3 Months

RE (°P)Maltose (g/100 mL)ABV (% v/v)

Mal

tose

(g/1

00 m

L)

ABV

(% v

/v) &

°P

Increased maltose and ABV in forced aged (37C) for 3 days

Separate batch, stored at brewery

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• Same packages tested 2 months later• Force aging repeated (at 37°C) for 3 and 7 days

Do enzymes transferred into beer after dry-hopping and continue to reduce beer limit dextrins?

Continued aging study – 2 months later

2 months 4°C

2 months 4°C + force aged x 3 days37°C

2 months 4°C + force aged x 7 days37°C

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0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

0.45

0.50

4.5

5

5.5

6

6.5

7

7.5

8

8.5

Fresh 2 Month (cold) 3 Day Force Aged 7 Day Force Aged

Repeat force aging study – 2 months later

RE (°P)Maltose (g/100 mL)ABV (% v/v)

Mal

tose

(g/1

00 m

L)

ABV

(% v

/v) &

°P

*Compared to Fresh package (3/29/17)

*

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Conclusion

• Humulinones coming from hops (during processing and storage) can significantly impact dry-hopped beer bitterness

• Hop-derived enzymes can alter carbohydrate make up of Real Extract• Refermentation in the presence of yeast (for example – bottle conditioning)• Lead to diacetyl spikes• SOLUTION: dry hop timing, temperature, hop variety, pasteurization

• Hop enzymes persist in finished beer• Dry-hopped beers likely become sweeter with age

OREGON STATE UNIVERSITY

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AcknowledgementsOregon State UniversityJeff ClawsonKaylyn KirkpatrickAndrew SuttonCameron McDanielDan Vollmer

HopsJohn I HaasYakima Chief HopUnionCrosby Hop Farm

Funding agenciesFonds Baillet Latour FundHop Research Council

BreweriesAllagash Brewing CompanyCraft Brew AllianceBridgeport BreweryNinkasi Brewing CompanyRussian River Brewing CompanypFriem Brewing CompanyMelvin Brewing Company

OREGON STATE UNIVERSITY

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OREGON STATE UNIVERSITY

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Thank you