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Fermentation Science at Oregon State University Thomas H. Shellhammer Professor of Food Science Nor’Wester Professor of Fermentation Science Where is Oregon? Oregon State University

Where is Oregon? Fermentation Science at Oregon State ...€¦ · Fermentation Science at Oregon State University ... subtle chemistry of taste and the innovations of ... Beer brewed

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Fermentation Science at Oregon State University

Thomas H. Shellhammer

Professor of Food Science Nor’Wester Professor of Fermentation Science

Where is Oregon?

Oregon State University

Oregon State University

•! Formerly Oregon Agricultural College •! 27,000 students •! Forestry, Oceanography, Agriculture

Engineering, Linus Pauling Institute

Food Science & Technology

OSU Seafood Laboratory - Astoria

Wiegand Hall - Corvallis

Food Innovation Center - Portland

B.S. Degree in Food Science and Technology !! Food Science 26% !! Fermentation Science 62% !! Enology & Viticulture 12%

OSU Food Science Undergraduate Degree Program

Undergraduate enrollment

!"

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Changing the future. Right here. Right now.

Tapping talent:

With one of the nation’s only teaching breweries and an endowed chair in fermentation science, OSU o�ers students the opportunity to develop new brews while they learn the subtle chemistry of taste and the innovations of business. Jobs on tap.

Agriculture is where food begins. Learn more at agsci.oregonstate.edu/foodies

Oregon bubbles to the top of the craft beer industry

Training students to be brewers

Photo’s courtesy of Lynn Ketchum

Training students to be brewers

Photo’s courtesy of Lynn Ketchum

OSU Pilot Brewery 2 BBL brewhouse, 6 CCV

Photo’s courtesy of Steve Werblow

OSU Pilot Brewery Packaging Single head filler + tunnel pasteurizer

Photo’s courtesy of Chris Meuller

OSU Minimalter

Photo’s courtesy of Lynn Ketchum

OSU Fermentation Science

Employers of OSU Ferm. Sci. Grads

Anheuser-Busch MillerCoors Boston Beer Company BridgePort Brewing Boulevard Brewing Deschutes Brewery Full Sail Brewing McMenamins Stone Brewing Widmer Brothers Brewing

Gallo Winery (Sonoma Valley, CA)

St. Michele Winery Hogue Cellars King Estate Winery Corsair Distillery Rogue Spirits Tillamook County Creamery Rogue Creamery

Fermentation Science at OSU

•! Brewing – Tom Shellhammer •! Barley breeding & malting – Pat Hayes •! Hops breeding – Shaun Townsend & John Henning •! Hops pathology – Dave Gent •! Hops & health – Fred Stevens •! Wine – James Osborne, Elizabeth Tomasino •! Viticulture – Patti Skinkis. Laurent Deluc, Walt Mahaffe •! Specialty cheeses – Lisbeth Goddik •! Cereals chemistry & bread – Andrew Ross

Fermentation Science at OSU

New Positions

•! Distillation professor •! Brewing microbiologist professor •! Instructor/Advisor – Fermentation Science

Beer Analytics May 1, June 16 – 20 Beer Proficiency July 15 – 18

Craft Brewery Startup April, May, September Cidery Startup April, May 12 – 16

pace.oregonstate.edu/beer

PACE - Beer Analytics

Beer Analytics Online + Hands-on learning in the lab and pilot brewery

Beer Analytics Engage with industry experts – Fred Strachan, Sierra Nevada

Beer Analytics Learn about hops and OSU’s hop breeding facilities

Beer Analytics Learn about barley/malt and OSU’s barley breeding facilities

Beer Analytics May 1, June 16 – 20 Beer Proficiency July 15 – 18

Craft Brewery Startup April, May, September Cidery Startup April, May 12 – 16

pace.oregonstate.edu/beer

Close connection to the brewing industry

•! MBAA District NW meetings – 200-300 attendees •! 1st International Brewing Symposium, 2007

Hop Flavor and Aroma in Beer •! Hop Research Council

OSU Pilot Brewery – Beer Development

Hops humulus lupulus

OSU has a long connection to hops •! 1932

–! Oregon largest hop producing region in the world with 34,594 acres (14,000 ha)

–! Downy Mildew discovered in Oregon hop yards –! U.S. Department of Agriculture establishes hop breeding

program

•! 1979 –! Hop Research Council created

•! 1996 –! Fermentation Science track created

within Dept of Food Science

Hop breeding at OSU Hop breeding at OSU

Public hop varieties released by USDA/OSU

Bianca Cascade Columbia Comet Crystal Horizon Liberty Mt. Rainier Mt. Hood

Newport Nugget Santiam Sterling Sunbeam Teamaker Ultra Willamette

Cascade Hop & Craft Brewing

Shellhammer Lab Hops research, recent activity

•! Isomerization kinetics •! Bitterness research

–! Native and reduced iso-alpha acids –! Hop-derived polyphenols –! Impact, time-intensity, quality

•! Foam studies –! Reduced iso’s

•! Flavor stability –! Hop-derived polyphenols –! Hop acids

Bitt

erne

ss In

tens

ity!

Time!tmax!

Imax!Area!

Duration!

Sensory testing Consumer as well as trained panel

Widmer Brewing Company

•! Preference Mapping of Widmer Products: Identification of Product Attributes, Consumer Preferences and Psychographics McDaniels, Orth, Shellhammer – 2002

•! Trained panel (12) + Consumers (~300)

•! Part of development efforts leading to Drop Top Amber Ale

Survey results using professional brewers Hop contributions to beer flavor

Cascade Citra

,-./0112""

Simcoe®

34--05""

Chinook

671829"3.4:09""

;<=>?"<214-@48A=2-.B.CDA>748""

,B5.94-""

E7/D4178""

E.117/5.4"=.4/48""

F0117904-""

35G/0.9"H21I09J""

,K2112""

64JJ75""

H.179.""

L.108.I7M""N011.-7O7"

L7/17";P3"2/0J09?""

62/5B7/9"Q/7C7/""

3K.15"3717R5""E.117/5.4"=/.I0S29""

=7O9.9J7/""

Q/7C7/T8"H21I""

Hallertau MittleFreuh

Saaz

L7/17";H7/-.9"2/0J09?""

East Kent Golding

F.J94-""

<14857/""

3K.157/""

U4JJ17""

U12/.1"

U/405G"=/2K0R.1"V/405"<05/48"E7/@.1"

3K0RG"

H/.88G"N22IG"

W9029AH./10R"

F485G"

X7.5B7/"[email protected]"

-2

-1

0

1

2

3

4

5

Y'" Y#" Y+" Y*" Y%" Y$" !" $" %" *" +" #" '"

D2

(20.

86 %

)

D1 (32.90 %)

5.6%$()0,7'8)9:),"-)9;<)=>?@A)B4),C'#)D,#.&,7)#$(,E$")

Shellhammer Lab Hops research, current projects

•! Investigating the sources of citrus aroma/flavor from hops

•! Hop harvest maturity influences on oil quality

•! Basic studies on dry hopping •! How hops affect beer flavor

stability •! New methods for assessing

beer bitterness

Questions?

Shellhammer Lab Hops research, current projects

•! Investigating the sources of citrus aroma/flavor from hops

•! Hop harvest maturity influences on oil quality

•! Basic studies on dry hopping •! How hops affect beer flavor

stability •! New methods for assessing

beer bitterness

Hop maturity and its impact on hop oil composition

Daniel Sharp Thomas H. Shellhammer

Shaun Townsend Michael Qian

Photo by: Jim Solberg, Indie Hops

Hop Oil Composition

Schönberger, C.; Kostelecky, T. 125th Anniversary Review: The Role of Hops in Brewing. J. Inst. Brew 2011, 117, 259–267.

Hop Oil Composition

Schönberger, C.; Kostelecky, T. 125th Anniversary Review: The Role of Hops in Brewing. J. Inst. Brew 2011, 117, 259–267.

Study Design Methods –!Hop Acids

•! ASBC-HPLC –!Hop Oil

•! Steam Distillation •! GC-FID – 17 compounds

–!Moisture •! % Solids at harvest •! Moisture content after kilning

–!Sensory •! Difference •! Acceptance •! Descriptive

Two Hop Varieties •! Cascade and

Willamette Two Farms

•! Willamette Valley Three Harvest Dates

•! Early, Typical, Late

Two Harvest Years •! 2010, 2011

Triplicate samples Total = 72 samples

Experimental Farms participating in hop maturity study

Coleman Farms

Goschie Farms

Harvest Timeline

F1 2010

F1 2011

F2 2010

F2 2011

F2 2010

F1 2010

F2 2011

F1 2011

F1 2011

F1 2010

F2 2011

F2 2011

F2 2010

F2 2010

F1 2010

F1 2011

F1 2011

F2 2011

F2 2011

F1 2010

F1 2010

F2 2010

F2 2010

F1 2011

8/17 8/19 8/21 8/23 8/25 8/27 8/29 8/31 9/2 9/4 9/6 9/8 9/10 9/12 9/14 9/16

Harvest Dates by Farm and Year

Will

amet

te

Cas

cade

Early Typical Late

Harvest Timeline

F1 2010

F1 2011

F2 2010

F2 2011

F2 2010

F1 2010

F2 2011

F1 2011

F1 2011

F1 2010

F2 2011

F2 2011

F2 2010

F2 2010

F1 2010

F1 2011

F1 2011

F2 2011

F2 2011

F1 2010

F1 2010

F2 2010

F2 2010

F1 2011

8/17 8/19 8/21 8/23 8/25 8/27 8/29 8/31 9/2 9/4 9/6 9/8 9/10 9/12 9/14 9/16

Harvest Dates by Farm and Year

Will

amet

te

Cas

cade

8 days

7

days

Early Typical Late

6 days

8 days

4 days

E2K"W01"<2-K249I8"2V"Z957/785"F$&6$G"-)H,&') F%,88.I+,E$") 9'8+#.6E$")[YK09797" Hydrocarbon, Monoterpene Pine

\YK09797" Hydrocarbon, Monoterpne Confierous Pine, woody

\YFG/R797" Hydrocarbon, Monoterpene Green, baslamic, slightly metallic

X0-29797" Hydrocarbon, Monoterpene Citric, Orange

]YRG-797" Hydrocarbon, Monoterpene like Orange wood spice

<./G2KBG11797" Hydrocarbon, Sesquiterpene Woody, Carrot

^_"\"YU./978797" Hydrocarbon, Sesquiterpene H/779_"C22IG_"C77IG_"B7/@.1_"K097".9I"J09"

E4-41797" Hydrocarbon, Sesquiterpene Woody

F75BG1"B7K5292.57" Oxygenated, Ester 3C775_"V/405G_"K7.RB_".K/0R25_"J/779_"@7//G"

H7/.9021" Oxygenated, Monoterpene Alcohol Sweet floral, perfumey

X09.1221" Oxygenated, Monoterpene Alcohol Floral, Orange

<05/2971121" Oxygenated, Monoterpene Floral, Rose Citrus

U./97821" Oxygenated, Sesquiterpene Alcohol Spicy

<05/.1" Oxygenated, other Sweet Citrus

H7/.9G1",R75.57" Oxygenated, Monoterpene or ester Floral, Sweet Citrus

^K2`0I7"Z" Oxygenated, Epoxide Spicy

^K2`0I7"%" Oxygenated, Epoxide Spicy

Traditional Brewing Quality Parameters

H.S.I. Alpha Acids

0.00

0.05

0.10

0.15

0.20

0.25

0.30

H.S

.I.

Cascade Willamette

Early Typical Late Harvest Point

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

% !

-aci

ds

Cascade Willamette

Early Typical Late Harvest Point

Cascade

0

0.5

1

1.5

2

2.5

3

8/17 8/19 8/21 8/23 8/25 8/27 8/29 8/31 9/2 9/4 9/6 9/8 9/10 9/12 9/14 9/16

Con

cent

ratio

n (m

l/100

g ho

ps)

Date

^8879S.1"W01"@G"E./:785"a.57"

U%"%!$!"

U$"%!$!"U$"%!$$"

U%"%!$$"

Cascade F7.98"

^./1G" =GK0R.1" X.57"W01";-1A$!!J?" $b%$" %b$*" %b!*"[YK09797";-JAJ?" !b!$" !b!%" !b!%"\YK09797" !b!(" !b$)" !b$)"\YFG/R797" +b(*" $$b+'" $$b!%"X0-29797" !b!%" !b!#" !b!#"]YRG-797" !b!$" !b!$" !b!$"<05/2971121" !b!*" !b!)" !b!&"F75BG1"B7K5292.57" !b!*" !b!&" !b!)"X09.1221" !b+'" !b)&" !b)$"<./G2KBG11797" !b'#" $b!'" !b&#"^_"\"YU./978797" $b+%" %b$(" $b&#"E4-41797" !b!*" !b!'" !b!#"<05/.1" !b!&" !b$(" !b$*"H7/.9G1",R75.57" !b!%" !b$%" !b$+"H7/.9021" !b!$" !b!%" !b!%"^K2`0I7"Z" !b!&" !b!#" !b!*"^K2`0I7"ZZ" !b%)" !b$%" !b$$"U./97821" !b!%" !b!%" !b!*"

Cascade F7.98"

^./1G" =GK0R.1" X.57" Tukey’s W01";-1A$!!J?" $b%$" %b$*" %b!*" ^c=dX"[YK09797";-JAJ?" !b!$" !b!%" !b!%" ^c=dX"\YK09797" !b!(" !b$)" !b$)" ^c=dX"\YFG/R797" +b(*" $$b+'" $$b!%" ^c=dX"X0-29797" !b!%" !b!#" !b!#" ^c=dX"]YRG-797" !b!$" !b!$" !b!$" ^c=dX"<05/2971121" !b!*" !b!)" !b!&" ^c=dX"F75BG1"B7K5292.57" !b!*" !b!&" !b!)" ^c=cX"X09.1221" !b+'" !b)&" !b)$" ^c=eX"<./G2KBG11797" !b'#" $b!'" !b&#"^_"\"YU./978797" $b+%" %b$(" $b&#"E4-41797" !b!*" !b!'" !b!#"<05/.1" !b!&" !b$(" !b$*"H7/.9G1",R75.57" !b!%" !b$%" !b$+" ^c=eX"H7/.9021" !b!$" !b!%" !b!%"^K2`0I7"Z" !b!&" !b!#" !b!*"^K2`0I7"ZZ" !b%)" !b$%" !b$$"U./97821" !b!%" !b!%" !b!*"

Cascade F7.98"

^./1G" =GK0R.1" X.57" Tukey’s W01";-1A$!!J?" $b%$" %b$*" %b!*" ^c=dX"[YK09797";-JAJ?" !b!$" !b!%" !b!%" ^c=dX"\YK09797" !b!(" !b$)" !b$)" ^c=dX"\YFG/R797" +b(*" $$b+'" $$b!%" ^c=dX"X0-29797" !b!%" !b!#" !b!#" ^c=dX"]YRG-797" !b!$" !b!$" !b!$" ^c=dX"<05/2971121" !b!*" !b!)" !b!&" ^c=dX"F75BG1"B7K5292.57" !b!*" !b!&" !b!)" ^c=cX"X09.1221" !b+'" !b)&" !b)$" ^c=eX"<./G2KBG11797" !b'#" $b!'" !b&#"^_"\"YU./978797" $b+%" %b$(" $b&#"E4-41797" !b!*" !b!'" !b!#"<05/.1" !b!&" !b$(" !b$*"H7/.9G1",R75.57" !b!%" !b$%" !b$+" ^c=eX"H7/.9021" !b!$" !b!%" !b!%"^K2`0I7"Z" !b!&" !b!#" !b!*"^K2`0I7"ZZ" !b%)" !b$%" !b$$"U./97821" !b!%" !b!%" !b!*"

Sensory - Cascade

Difference Testing: n = 18 •! Triangle Test

–! 14 correctly identified different sample (p< 0.001)

Consumer Testing: n = 62 •! Consumer Acceptance

–! Typical preferred over Late (0-9 scale)

Attribute Typical Late

Overall *** 7.11 ( 0.83)

6.26

(1.61)

Aroma *** 6.92 (1.31)

5.82 (1.96)

Flavor ** 6.98 (1.03)

6.23 (1.68)

***, ** significant at p< 0.01 and < 0.05 respectively, (SD),

Preliminary brewing: Cascade

•! Typical harvest hops = apple, apricot/peach, and sweaty/onion/garlic notes.

•! Late harvest hops = higher melon and floral notes.

A Study of Factors Affecting the Extraction of Flavor When Dry Hopping Beer

Dry hopping – experimental design

Instrumental Analysis

–! Beer brewed specifically for this project (5.1% EtOH v/v, 21 ppm Iso-!-acids)

–! Dry hopped for 12 days –! SPME/GC, HPLC, and UV Spec analysis –! Cold extraction, 4 C –! Samples taken at 2 hours, 4 hours, 6

hours, 24 hours, 4 days, 7 days, 12 days.

Sensory Analysis

–! Same beer (samples taken side by side) –! Sampled at 6 hours, 24 hours, 4 days,

12 days –! Trained sensory panel (11 individuals, 3

females 8 males) –! 3 training sessions, 4 testing sessions –! Categories scaled on a 0-15 point scale –! Examined aroma and bitterness

Form - whole cones vs. pellets (Cascade from same farm and harvest time) Extraction - passive contact vs. stirring

Dry Hop Method

•! The dry hop treatments were conducted in 3.5 hL (3 bbl) stainless steel CCVs

•! 90 Gallons (340 Liters) of beer in each treatment

•! 1 lb/barrel (386g/hL) hops used for each treatment

•! One CCV utilized a centrifugal pump for stirring

Overall hop aroma intensity

3.-K17

W:7/.11"Z9579805G

;K.971085"-7.9":.147?

H/24K8

3S//7I_"+"I.G8 &b+*% , " "

3S//7I_"$%"I.G8 &b%%( ,

3S//7I_"%+"B24/8 )b#&$ , Q

3S//7I_"'"B24/8 (b'$+ Q

L.880:7_"+"I.G8 #b(#! <

L.880:7_"'"B24/8 #b#+# <

L.880:7_"$%"I.G8 #b%!# <

L.880:7_"%+"B24/8 #b!%* " " <

Bitterness intensity

3.-K17

Q0O7/9788"Z9579805G ;K.971085"

-7.9":.147? H/24K8

3S//7I_"$%"I.G8 &b&*% , " " "

3S//7I_"+"I.G8 &b((* ,

3S//7I_"%+"B24/8 )b#') , Q

3S//7I_"'"B24/8 (b'$+ Q <

L.880:7_"%+"B24/8 'b%#! < a

L.880:7_"+"I.G8 'b$*' a

L.880:7_"$%"I.G8 #b&*% a

L.880:7_"'"B24/8 #b'#& " " " a

Results

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!b%#"

!b*"

!b*#"

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.S29

";-JA

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=0-7";B24/8?"

NB217"E2K8_"3S//7I" NB217"E2K8_"L.880:7" L71175"E2K8_"3S//7I" L71175"E2K8_"L.880:7"

Linalool

Results

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NB217"E2K8_"3S//7I" NB217"E2K8_"L.880:7" L71175"E2K8_"3S//7I" L71175"E2K8_"L.880:7"

Myrcene

Results

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$b#"

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NB217"E2K8_"3S//7I" NB217"E2K8_"L.880:7" L71175"E2K8_"3S//7I" L71175"E2K8_"L.880:7"

Myrcene – First 6 hours

Results

Compound 6 Hours,

Passive 6 Hours,

Stirred Peak,

Passive Peak,

Stirred Final,

Passive Final,

Stirred

Myrcene 0.5% 2.6% 2.4% 5.6% 1.0% 4.0% Limonene 40.7% 41.8% 42.7% 52.2% 17% 30.8% Linalool 6.8% 9.0% 28.7% 48.5% 21% 48.5% Humulene 0.5% 1.1% 0.94% 0.9% 0.15% 0.64% Geraniol 70.3% 57.3% 70.3% 119% 50.3% 91.0%

Compound 6 Hours,

Passive 6 Hours,

Stirred Peak,

Passive Peak,

Stirred Final,

Passive Final,

Stirred Myrcene 8.4% 19.9% 9.7% 37.2% 5.9% 25.8% Limonene 43.1% 69.1% 43.1% 82.4% 39.5% 75.2% Linalool 55.6% 89.2% 57.2% 100.7% 56.1% 90.6% Humulene 1.3% 8.3% 1.3% 17.1% 1.2% 14.2% Geraniol 90.8% 105.2% 97.1% 117.9% 97.1% 102.9%

Results

!"

%!"

+!"

'!"

)!"

$!!"

$%!"

$+!"

$'!"

$)!"

!" #!" $!!" $#!" %!!" %#!" *!!"

L21G

KB79

21"<

29R7

95/.

S29"

;-JA

X?"

=0-7";B24/8?"

NB217"E2K8_"L.880:7" NB217"E2K8_"3S//7I" L71175"E2K8_"L.880:7" L71175"E2K8_"3S//7I"

Hop Derived Polyphenols

Results

!"

%"

+"

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)"

$!"

$%"

$+"

!" #!" $!!" $#!" %!!" %#!" *!!"

[Y.R

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=0-7";B24/8?"

NB217"E2K8_"L.880:7" NB217"E2K8_"3S//7I" L711758_"L.880:7" L711758_"3S//7I"

!-acids

Conclusions

•! The stirred treatment yielded more overall aroma intensity, bitterness, and astringency relative to the unstirred treatment

•! As expected, !-acid concentration did not correlate to increased bitterness even though significant extraction occurred –! Polyphenol extraction did correlate to increased bitterness

Shellhammer Lab non-hop-related current projects

•! Fermentation performance studies •! Sour beer characterization

Methylsulfonylmethane & Fermentation

0

2

4

6

8

10

12

0.0E+00

2.0E+07

4.0E+07

6.0E+07

8.0E+07

1.0E+08

1.2E+08

1.4E+08

1.6E+08

1.8E+08

2.0E+08

!" %!" +!" '!" )!" $!!" $%!"

Gra

vity

(°B

rix)

Cel

l Cou

nt (C

ells

/ml)

Time (Hours)

J#,K.(/),"-)F'%%)F$G"():LAM)LB)NON)

Cell Count

Gravity

Standard (Normal) pitching rate

0

2

4

6

8

10

12

!" %!" +!" '!" )!" $!!" $%!"

Gra

vity

(°B

rix)

Time (Hours)

10^6, 0% MSM

10^6, 0.25% MSM

10^6, 0.5% MSM

10^6, 0.75% MSM 0.25% MSM

Underpitched

0

2

4

6

8

10

12

!" %!" +!" '!" )!" $!!" $%!"

Gra

vity

(°B

rix)

Time (Hours)

10^5, 0% MSM

10^5, 0.25% MSM

10^5, 0.5% MSM

10^5, 0.75% MSM 0.25% MSM

Underpitched

0.00E+00

2.00E+07

4.00E+07

6.00E+07

8.00E+07

1.00E+08

1.20E+08

1.40E+08

1.60E+08

1.80E+08

2.00E+08

!" %!" +!" '!" )!" $!!" $%!"

Cel

l Cou

nt (C

ells

/ml)

Time (Hours)

Yeast Cell Count

10^5, 0% MSM

10^5, 0.25% MSM

10^5, 0.5% MSM

10^5, 0.75% MSM

0.25% MSM

Sensory Evaluation of Belgian and US Red/Brown Sour Beers

•! 13 Commercial Red/Brown Sour Beers

–! 6 Belgian (Flemish) procured via importer –! 7 US Craft (West, Midwest, East Coast) donated from

US breweries •! Instrumental Analysis •! Sensory Descriptive Analysis

Methods Instrumental Analysis

•! Organic Acids •! Acetate and Lactate •! Esters •! Higher Alcohols •! Volatile Phenols •! Fatty Acids •! Iso alpha acids

•! Apparent Extract •! Real Extract •! Alcohol by Volume •! Real Degree of

Fermentation •! pH •! Color •! Bitterness Units

Volatile Phenols

0

500

1000

1500

2000

2500

3000

0 1 2

PPB

4-Ethyl Guaiacol

American Belgian 0

50

100

150

200

250

300

0 1 2

PPB

4-Vinyl Guaiacol

American Belgian 0

200 400 600 800

1000 1200 1400 1600

0 1 2

PPB

4-Ethyl Phenol

American Belgian

meaty, smoky, clove, apple wood smoked bacon

-! medicinal, rubber, Band-Aid

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