A V A B I: Pplication Apodest

APPLICATION VAPODEST
ALCOHOL IN BEVERAGES AND INTERMEDIATES

PAGE 1 OF 9

C.21 Alcohol in Beverages and Intermediates.doc
26.06.08 mkr-rbr
Principle
The actual content of alcohol is determined with the help of the density of the distillate assuming the same
amount of volume for the sample and distillate.
Using a water steam distillation alcohol (ethanol) is distilled from the matrix, which has to be examined.
The density can be determined using the pycnometer method, the araeometer method (spindle), or the
oscillating U-tube method.

This application is divided into the following chapters acc. to the sample matrices to be examined:
1. Beer
2. Wine
3. Sparkling wines
4. Liqueurs
5. Essences and denaturates
6. Spirit
7. Production cooler sludge, wine cooler sludge, fruit mash, red wine mash

The procedure is the same for all distillations. However, there are different methods for the sample preparation
or the parameters of the distillation.

Area of usage

Type of Sample Alcohol Content
[%vol]
Amount of Sample Amount of Distillate
Beer 3 - 10 50 ml 100 ml
Wine 8 - 15 50 ml 50 ml
Sparkling wine 9 - 14 50 ml 50 ml
Liqueurs 15 - 25 50 ml 100 ml
Spirits Up to 40 50 ml 100 ml
Apple/Fruit mash Up to 10 50 g 50 ml or g
Wine cooler sludge 100 g 100 ml or g
Production cooler sludge 100 g 100 ml or g
Essences Up to 60 50 g 100 ml
Acetators Up to 3 50 g 50 ml
Denaturants Up to 60 50 g 100 ml

1. BEER
1.1. Chemicals
Silicone antifoam
Aquadest

1.2. Instruments
VAPODEST 10s 45s, modified for the alcohol determination
Kjeldahl flask with wide neck opening 500 or 750 ml, cat. no. 6465 or cat. no. 6467
Pycnometer, oscillating U-tube, spindle.
Folded filter and funnel
Erlenmeyer flask 500 ml
Glass beaker 800 ml
Volumetric flask 100 ml
Thermostat


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26.06.08 mkr-rbr
1.3. Procedure
1.3.1. Sample Preparation
In order to decarbonise the sample it is filtered using a folded filter. Putting the sample in an ultrasound bath
afterwards can support this process. The thus defoamed sample is then put into a 100 ml volumetric flask and
brought to 20 C in a water bath.
After the thermo stability has been achieved the sample is put into the distillation flask for the VAPODEST
while thoroughly rinsing the sample with distilled water.
The following program settings are recommended for the various VAPODEST models. Please note however,
that these can only be regarded as guidelines for the use of C. Gerhardt equipment.
Users may have to adapt this method to meet their own analytical requirements.

1.3.2. Distillation and Programming of the VAPODEST

VAP 10s VAP 20s VAP 30s VAP 45s
H
2
O Addition - - 0 ml 0 ml
NaOH Addition 0 ml 0 ml 0 ml 0 ml
Reaction Time 0 s 0 s 0 s 0 s
Distillation Time 160 s 160 s 160 s 160 s
Steam Power 90 % 90 % 90 % 90 %
Suction Sample manual manual 30 s 30 s

Use the VAPODEST following the instruction manual. As a start run a blank distillation in order to heat up and
clean the instrument. Check whether all chemicals are present in the required quantities!

After 3 drops of silicon anti foam have been added the distillation flask with the sample is put into the
VAPODEST. The 100 ml volumetric flask containing 20 ml Aquadest is used as a receiver. The outlet tubing of
the distillate has to be immerged in the Aquadest. Then the program is started and the distillation is run. The
sample is distilled until the calibration mark on the volumetric flask is nearly reached.

The first distillation should be watched closely to optimize the amount of distillate and the distillation time. If
needed, the parameters chosen for the VAPODEST can be corrected. After the distillation is terminated, the
receiver is taken out and the outlet tubing is rinsed with distilled water.

1.4. Evaluation
The measuring flask containing the distillate is tempered and filled with distilled water up to the calibration
mark. After intensive mixing, the relative density 20 C / 20 C is detected using an oscillating U-tube. When
over distilling into a pycnometer, the density is detected using a weighing comparison. The alcohol content is
then determined using the alcohol table.

The following pages 3 and 4 give a sample of a result and the comparison to the traditional method.


PAGE 3 OF 9

26.06.08 mkr-rbr
Sample of a result / Comparison to traditional method: Alcohol standard

Table 1: Expected standard deviation

Traditional distillation VAPODEST Difference
+ Pycnometer + Pycnometer
%vol %vol

0,94 0,93 0,01
1,04 1,04 0,00
3,24 3,24 0,00
3,05 3,04 0,01
3,21 3,21 0,00
3,58 3,59 0,01
3,19 3,21 0,02
3,64 3,67 0,03
3,62 3,63 0,01
4,23 4,21 0,02
4,27 4,28 0,01
4,13 4,14 0,01
4,18 4,14 0,04
4,83 4,87 0,04
4,76 4,80 0,04
4,71 4,80 0,09
5,61 5,70 0,09
5,40 5,40 0,00
9,31 9,31 0,00
9,06 9,15 0,09
10,93 11,00 0,07
4,93 5,02 0,09
3,49 3,43 0,06
5,68 5,72 0,04

Mean value traditional distillation: 4,64
Mean value VAPODEST distillation: 4,63
Bias (methodic deviation of the result): 0,017916
SEP 0,0467
SEP (probability 95 %) 0,0935
Number of samples 24


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26.06.08 mkr-rbr
Sample of a result /Comparison to traditional method:

Table 2: Precision - repeatability

Sample with average alcohol content:
%vol
3,51
3,51
3,53
3,48
3,51
3,51
3,53
3,51
3,51
3,48

Repeatability (probability 95 %): 0,047
Average 3,508
Range: 0,050
No. of samples: 10

Sample with high alcohol content:
%vol
8,61
8,67
8,70
8,64
8,63
8,63
8,66
8,63
8,59
8,67

Repeatability (probability 95 %): 0,0905
Average : 8,64
Range: 0,11
No. of samples: 10


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26.06.08 mkr-rbr
2.WINE
2.1. Chemicals
Silicone antifoam
Aquadest

2.2. Instruments
VAPODEST 10s 45s, modified for alcohol determination
Kjeldahl flask with wide neck opening 500 or 750 ml cat. no. 6465 or cat. no. 6467
Pycnometer, oscillating U-tube, spindle
Volumetric flask 100 ml
Thermostat

2.3. Procedure
After the thermo stability has been achieved the sample is put into the distillation flask for the VAPODEST
while thoroughly rinsing the sample with distilled water.
The following program settings are recommended for the various VAPODEST models. Please note however,
that these can only be regarded as guidelines for the use of C. Gerhardt equipment.
Users may have to adapt this method to suit their own analytical requirements.

Distillation and Programming of the VAPODEST:

H
2
Distillation Time ~120 s ~120 s ~120 s ~120 s
Steam Power ~95 % ~95 % ~95 % ~95 %

Use the VAPODEST following the instruction manual. As a start run a blank distillation in order to heat up and
clean the instrument. Check whether all chemicals are present in the required quantities!

The distillation flask with the sample is put into the VAPODEST after 3 drops of silicon anti foam have been
added.
The 100 ml volumetric flask containing approx. 20 ml Aquadest is used as a receiver. The outlet tubing has to
be immerged in the Aquadest. The program is started, the distillation is run. The sample is distilled until the
calibration mark on the volumetric flask is nearly reached.
The first distillation should be watched closely to optimize the amount of distillate and the distillation time.
If needed, the parameters chosen for the VAPODEST can be corrected. After the distillation is terminated, the

2.4. Evaluation
The measuring flask containing the distillate is tempered and filled with distilled water up to the calibration
mark. After intensive mixing, the relative density 20 C / 20 C is detected using an oscillating U-tube method.
When over distilling into a pycnometer, the density is detected using a weighing comparison. The alcohol
content is then determined using the alcohol table.

A sample of a result and comparison to the traditional method: see page 6

2.5. Comments
Samples known for their heavy foaming can be treated with a little bit of bentonite to avoid foaming.


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26.06.08 mkr-rbr
Add. to 2. Wine: Sample of a result /Comparison to traditional method:

Trad. distillating unit VAPODEST Difference Mean Deviation
+ density measurement + density measurement deviation in percent
%vol %vol %vol %

Acetatores and compounds: 1,01 1,01 0 0,021 1,3
1,35 1,28 0,07
1,76 1,69 0,07
3,17 3,17 0
1,82 1,76 0,06
0,54 0,61 0,07
1,01 1,01 0
2,31 2,24 0,07
1,69 1,69 0
1,01 1,01 0
1,82 1,82 0
1,48 1,48 0
1,35 1,35 0
2,18 2,18 0
1,82 1,82 0
2,24 2,24 0

Cidre / fruit mash: 6,42 6,46 0,04 0,039 0,6
6,27 6,12 0,15
6,27 6,27 0
6,34 6,34 0
6,42 6,34 0,08
6,34 6,34 0
6,34 6,34 0

Red wine / white wine / wine mash: 11,05 11,1 0,05 0,021 0,2
11,05 11,02 0,03
10,61 10,61 0
10,95 10,87 0,08
10,55 10,55 0
11,38 11,38 0
10,61 10,52 0,09
11,05 11,05 0
11,38 11,38 0
10,87 10,87 0
10,61 10,61 0
11,05 11,05 0


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26.06.2008 mkr-rbr
3. SPARKLING WINES
Sparkling wines are treated the same way as regular wine. However, they have to be decarbonized prior to
the analysis.

4. LIQUEURS
The special advantage of the water steam distillation used for those samples compared to the traditional
method is the stirring effect of the incoming water steam. The sample does not burn and as an additional
benefit is stirred well. The settings for the program depend very much on the content that is expected. It is
recommended to use a steam output of 100 %. The distillation time and amount of sample have to be set
on a trial basis. Samples with excessive foaming should be decarbonized or mixed with antifoam prior to the
analysis.

Enclosed you find an example on how to test the linearity of the method.

5. ESSENCES and DENATURANTS
Depending on the structure of the essences 4 different approaches have to be distinguished:

5.1. Method 1: Sample consisting of distillate and alcohol
Up to 50 vol% 100 g weighted in quantity and 20 g water
More than 50 vol% 50 g weighted in quantity and 70 g water

5.1.1. Instruments
VAPODEST 10s 45s, modified for alcohol determination
Kjeldahl flask with wide neck opening 500 or 750 ml cat. no. 6465 or cat. no. 6467
oscillating U-tube, spindle
Volumetric flask
Thermostat

5.1.2. Procedure
Prepare the samples according to standard procedure and put them into the distillation flask.
The following program settings are recommended for the various VAPODEST models.
Please note however, that they can only be regarded as guidelines for the use of C. Gerhardt equipment.
Users may have to adapt this method to suit their own analytical requirements.

Distillation and Programming of the VAPODEST:

H
2
Distillation Time ~240 300 s ~240 300 s ~240 300 s ~240 300 s
Steam Power 100 % 100 % 100 % 100 %

Use the VAPODEST following the instruction manual. As a start run a blank distillation in order to heat up
and clean the instrument. Check whether all chemicals are present in the required quantities!

The distillation flask with the sample is put into the VAPODEST. A 200 ml volumetric flask filled with about
30 ml distilled water is put under the outlet tubing. The outlet tubing has to be immerged in the water.
Then the program is started and the distillation is run. The sample is distilled until the calibration mark on
the volumetric flask is nearly reached.
The first distillation should be watched closely to optimize the amount of distillate and the distillation time. If
needed, the parameters chosen for the VAPODEST can be corrected. After the distillation is terminated, the


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26.06.2008 mkr-rbr
5.1.3. Evaluation
The volumetric flask filled with distillate is moderated and distilled water is added to reach the desired
volume. Now, the measurement of the density can be done by using various methods.

5.2. Method 2: Samples consisting of distillate, alcohol and extract
Follow procedures for method 1

5.3. Method 3: Samples consisting of distillate, alcohol and essential oil
5.3.1. Chemicals
Silicone anti foam
Aquadest
Common salt
Ether

5.3.2. Instruments
VAPODEST 10s 45s, modified for alcohol distillation
Kjeldahl flask with wide neck opening 500 or 750 ml cat. no.6465 or cat. no.6467
oscillating U-tube, spindle
Volumetric flask
Separating funnel 250 ml
Thermostat

5.3.3. Procedure
The samples are weighted in a separating funnel; 50 g ether and 10 g salt are added, shaken out and left to
stand over night in a closed container. The next day, the ether phase is separated from the water phase
and rejected. For the further procedure see Method 1.

Up to 50 vol% 100 g weighted in quantity and 20 g water
More than 50 vol% 50 g weighted in quantity and 20 g water

5.4. Method 4: Samples consisting of distillate, alcohol, extract and essential oil
This kind of structure requires the distillation into a separating funnel, which contains 50 ml ether and 40 g
of a 4 % salt solution. Then continue following method 3.

6. SPIRIT
The distillation of spirits is similar to method 1 used for essences. The amount of distillate used is vital for
the accuracy. It is recommended to work with a bigger amount of sample than in the wine analysis and thus,
a bigger amount of distillate in order to obtain an adequate accuracy. 200 ml sample measured in a
volumetric flask have been proven successful in such a case.

7. PRODUCTION COOLER SLUDGE, WINE COOLER SLUDGE, FRUIT MASH, RED WINE MASH
The special advantage of the water steam distillation used for those samples compared to the traditional
method is the stirring effect of the incoming water steam. The sample does not burn and as an additional
benefit is stirred well. The settings for the program depend very much on the content that is expected. It is
recommended to use a steam output of 100 %. The distillation time and amount of sample have to be set
on a trial basis. Samples with excessive foaming should be decarbonized or mixed with antifoam prior to the
analysis.

APPENDIX

VERIFICATION OF THE LINEARITY
PAGE 1 OF 1

26.06.2008 mkr-rbr
Linearity is the capability of a method to present results within a given concentration range which are directly
proportional to the concentrations of the analytes.
In order to verify the linearity of method 3
*)
, ethanolic solutions of various concentrations have been made and
distilled. A total of 6 concentrations have been selected, all in the range of about 5 %vol to about 50 %vol according to
the samples to be examined. Each of these solutions was used seven times for the 50 ml to 100 ml distillation: 50 ml
solution, measured with the help of a pycnometer, is distilled over into a 100 ml measuring flask; the alcohol content is
then measured using a flexural resonator after tempering to 20 C. Table 5.6. shows the results.

Table 5.6. Verification of the Linearity - Measured Values

The single values which are then obtained for the determination of any alcoholic solution have been analyzed using
the statistic program Ebel (also see enclosures).
Ebel contains statistical tests, like e.g. the analysis of the mean value, the median, the standard deviation, the
variation coefficient, a test of the normal distribution (test acc. to David, test acc. to Kolmogoroff-Smirnov), the test of a
trend (test acc. to Grubbs, test acc. to Dixon), as well as the determination of the regression of the straight line of the
entire measurement. Some values were identified as outliers (are marked with an asterisk in the table). These values
should be eliminated for a correct analysis.

In order to set up the calibration line, the true alcohol contents (prior to the distillation) are plotted against the alcohol
contents measured after the distillation and with taking the dilution factor 2 into consideration as well. The illustration
below shows the calibration line of measuring points and the corresponding regression line.

0
10
20
30
40
50
60
0 10 20 30 40 50 60
Alcohol Content %vol prior to Distillation
A
l
c
o
h
o
l

C
o
n
t
e
n
t

%
v
o
l

a
f
t
e
r

D
i
s
t
i
l
l
a
t
i
o
n

Illustration 5.1. Calibration line of the linearity verification

A line is described by the equation y=ax+b. In the procedure described above, the coefficients should be ideally a=1
and b=0. The deviations from the ideal case coefficient are [0.0015] for a and [0.0146] for b. The values obtained
make it possible to say, that there is linearity in the verified range.

*)
Method 3 Water steam distillation: Distill 50 ml on 100 ml (dilution factor 2) at 85 % steam pressure for 250 s
Point 1 Point 2 Point 3 Point 4 Point 5 Point 6
Alcohol content, %vol 5,08 13,35 19,76 29,66 39,91 49,73
Single values %vol 5,09 13,24 19,69 29,63 39,85 49,63
5,06 13,30 19,76 29,66 39,94 49,52
5,10 13,33 19,75 29,67 39,88 49,62
5,12 13,34 19,76 29,65 39,87 49,56
5,08 13,32 19,74 29,62 39,83 49,84*
5,10 13,39 19,83 29,75* 40,06* 49,54
5,10 13,32 19,77 29,65 39,84
Mean value %vol 5,09 13,32 19,76 29,66 39,90 49,62
Standard deviation %vol 0,02 0,04 0,04 0,04 0,08 0,11
Variation coefficient R, % 0,39 0,30 0,20 0,13 0,20 0,22
Recovery % 100,20 99,78 100,00 100,00 99,98 99,78
* Values identified as outliers
y = 0,9985x + 0,0146

R
2
= 1

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APPLICATION VAPODEST

ALCOHOL IN BEVERAGES AND INTERMEDIATES

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