Program Book - Master Brewers Association of the Americas
Program Book - Master Brewers Association of the Americas
Program Book - Master Brewers Association of the Americas
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P-74<br />
Optimized analytical methods for <strong>the</strong> determination <strong>of</strong> SO 2 in<br />
beer and malt<br />
THOMAS KUNZ (1), Victoria Schiwek (2), Frank-Juergen Methner<br />
(1)<br />
(1) TU Berlin/VLB Berlin, Berlin, Germany; (2) VLB Berlin, Berlin,<br />
Germany<br />
The determination <strong>of</strong> <strong>the</strong> SO 2 content in beer is becoming more<br />
<strong>of</strong> a focus for brewers. The technological importance <strong>of</strong> SO 2 is<br />
based on its anti-oxidative potential, which protects beer against<br />
oxidation and <strong>the</strong>refore enhances flavor stability. However SO 2<br />
is said to have some allergenic potential, especially for sensitive<br />
individuals it may cause hives, stomach problems and a headache,<br />
even though <strong>the</strong> content in beer is considered to be harmless from<br />
a physiological point <strong>of</strong> view. Never<strong>the</strong>less <strong>the</strong> allergenic potential<br />
has provoked a European directive, which is limiting <strong>the</strong> content<br />
<strong>of</strong> SO 2 and sulfites to a concentration <strong>of</strong> 10 mg/L, o<strong>the</strong>rwise it has<br />
to be labeled. Based on <strong>the</strong>se backgrounds, different analytical<br />
methods for <strong>the</strong> determination <strong>of</strong> SO 2 were compared among each<br />
o<strong>the</strong>r according to <strong>the</strong>ir accuracy, application, linearity, precision<br />
and selectivity and have been optimized. The oldest and most<br />
used analysis in brewing is <strong>the</strong> distillation method according to<br />
Monnier-Williams. Due to <strong>the</strong> high expenditure <strong>of</strong> time, personnel<br />
costs and a recovery rate <strong>of</strong> ≈90% this analysis is less suitable for<br />
determination in beer. Opposite to that for determination in malt<br />
it is more appropriate, because <strong>the</strong>re is no adequate possibility <strong>of</strong><br />
extracting <strong>the</strong> SO 2 from <strong>the</strong> malt without higher losses. Comparative<br />
measurements using whole malt kernels show significantly higher<br />
yields with much lower coefficients <strong>of</strong> variation compared to fine<br />
and coarse grist. The reasons are <strong>the</strong> oxidation <strong>of</strong> <strong>the</strong> SO 2 during <strong>the</strong><br />
milling process and mainly <strong>the</strong> fact that in <strong>the</strong> flask agglutination<br />
occurs by fine and coarse grist in contrast to whole malt kernels.<br />
It is generally possible to determine <strong>the</strong> SO 2 content in whole malt<br />
kernels, because <strong>of</strong> <strong>the</strong> fact that <strong>the</strong> SO 2 is primarily located in<br />
<strong>the</strong> husks. The suitability <strong>of</strong> <strong>the</strong> new method could be confirmed<br />
in several interlaboratory tests. Photometric analysis via CFA<br />
(continuous flow analysis), using pararosaniline, is ano<strong>the</strong>r possible<br />
method. This method showed significantly higher results for SO 2<br />
in beer compared to <strong>the</strong> distillation method. These higher results<br />
can be explained by <strong>the</strong> occurrence <strong>of</strong> background signals caused<br />
by <strong>the</strong> beer matrix. It could be demonstrated that <strong>the</strong> background<br />
signals are mainly caused by Maillard reaction products in <strong>the</strong><br />
beer. By using new developed Teflon membranes it was possible<br />
to eliminate <strong>the</strong> interfering signals almost completely and led to a<br />
significant increase in <strong>the</strong> sensitivity <strong>of</strong> this method. In recent years,<br />
ion chromatography (IC) has been established more and more in<br />
breweries for <strong>the</strong> determination <strong>of</strong> SO 2 . IC is characterized by a low<br />
standard deviation, good reproducibility <strong>of</strong> <strong>the</strong> individual values and<br />
a good recovery <strong>of</strong> up to 100%.<br />
After qualifying as a certified technician in preservation engineering<br />
(1991–1993), Thomas Kunz completed his basic studies in chemistry<br />
at Isny University <strong>of</strong> Applied Sciences (1994–1995) and his basic<br />
studies in food chemistry at Wuppertal University (1995–1998)<br />
before starting to study food technology at Trier University <strong>of</strong> Applied<br />
Sciences (1998–2002). After graduating, he worked as an engineer<br />
(Dipl.-Ing. FH) in <strong>the</strong> area <strong>of</strong> ESR spectroscopy at <strong>the</strong> Institute <strong>of</strong><br />
Biophysics at Saarland University (2002–2004). Since January<br />
2005, he has been employed as a Ph.D. student at <strong>the</strong> Research<br />
Institute for <strong>the</strong> Technology <strong>of</strong> Brewing and Malting at VLB/<br />
Technical University <strong>of</strong> Berlin under <strong>the</strong> supervision <strong>of</strong> Pr<strong>of</strong>essor<br />
Methner. His main research focus is analysis <strong>of</strong> radical reaction<br />
mechanisms in beer and o<strong>the</strong>r beverages using ESR spectroscopy.<br />
P-75<br />
Brewing industry quality control applications using headspace<br />
sampling/gas chromatography<br />
TOM KWOKA (1), Ruth Martin (2), Tim Ruppel (1)<br />
(1) PerkinElmer LAS, Shelton, CT; (2) Sierra Nevada Brewery,<br />
Chico, CA<br />
There are four major HS/GC analyses that are performed at<br />
breweries for <strong>the</strong> purpose <strong>of</strong> quality control and identifying<br />
problems or changes occurring in brewing and fermentation<br />
processes that can adversely affect both <strong>the</strong> taste and quality <strong>of</strong><br />
<strong>the</strong> final product. The first and perhaps most important <strong>of</strong> <strong>the</strong>se<br />
is monitoring for vicinal diketones (VDK’s) in beer. VDK’s are<br />
known to affect <strong>the</strong> taste <strong>of</strong> beer, imparting a butter-like flavor<br />
that is considered undesirable at higher concentrations. Generally<br />
speaking, heavier beers, including stouts etc., tend to have higher<br />
levels <strong>of</strong> VDK’s than do lighter beers. Typically, VDK’s are found in<br />
<strong>the</strong> 1–50 ppb range in lighter beers and can exceed several hundred<br />
ppb in darker beers. Acetaldehyde is a fur<strong>the</strong>r analysis performed<br />
throughout <strong>the</strong> brewing process. Acetaldehyde is reduced to<br />
ethanol by yeast during secondary fermentation, but oxidation <strong>of</strong><br />
<strong>the</strong> finished beer may reverse this process, converting ethanol back<br />
to acetaldehyde. The taste and aroma <strong>of</strong> acetaldehyde has been<br />
described as fresh cut green apples, grass, leaves and even latex<br />
paint. Levels <strong>of</strong> acetaldehyde are generally in <strong>the</strong> 1–20 ppm range.<br />
A third group <strong>of</strong> compounds <strong>of</strong> interest are <strong>the</strong> trihalomethanes.<br />
These are usually introduced into <strong>the</strong> beer through <strong>the</strong> municipal<br />
water supply. Municipal water is <strong>of</strong>ten treated with chlorine,<br />
resulting in a variety <strong>of</strong> chlorinated disinfection by-products.<br />
Chlor<strong>of</strong>orm is usually <strong>the</strong> most prominent trihalomethane identified<br />
during this analysis. The fourth test commonly performed on beer<br />
is <strong>the</strong> isolation and identification <strong>of</strong> sulfur compounds. Dimethyl<br />
sulfide (DMS), sulfur dioxide (SO 2 ) and hydrogen sulfide (H 2 S) are<br />
<strong>of</strong> particular interest to brewers worldwide. DMS has <strong>the</strong> taste and<br />
aroma <strong>of</strong> sweet corn. This comes ei<strong>the</strong>r from <strong>the</strong> malt, as a result<br />
<strong>of</strong> a short boil <strong>of</strong> <strong>the</strong> wort, slow wort chilling or bacterial infection.<br />
SO 2 is <strong>of</strong>ten used as a preservative. Various types <strong>of</strong> yeast will<br />
produce significantly different levels <strong>of</strong> H 2 S. Above very low ppb<br />
levels, <strong>the</strong>se sulfur compounds give <strong>of</strong>f an unpleasant taste and<br />
smell (e.g., rotten eggs). Though traditionally <strong>the</strong>se four QC tests<br />
have been performed individually, <strong>the</strong> use <strong>of</strong> <strong>the</strong> PerkinElmer HS/<br />
GC allows for <strong>the</strong> combining <strong>of</strong> <strong>the</strong>se analyses, thus dramatically<br />
enhancing productivity. In fact, depending on one’s desired level<br />
<strong>of</strong> detection, all four methods can be analyzed simultaneously or, if<br />
need be, broken up into method specific parameters. The improved<br />
application will be described and criteria for performance and<br />
quality control will be outlined.<br />
Tom Kwoka received a B.S. degree in chemistry from California<br />
State University, Sacramento, in 1983. He began employment with<br />
PerkinElmer, Inc. in 2004 as a chromatography product specialist.<br />
Tom’s current functions include pre-sales support, post-sales<br />
customer training, and applications development. Tom has 19 years<br />
<strong>of</strong> environmental laboratory experience, including QA/QC, GC, and<br />
GC/MS analysis.<br />
103