U.S. patent number 3,860,729 [Application Number 05/403,970] was granted by the patent office on 1975-01-14 for preservation of beverages with poly(hexamethylenebiguanide hydrochloride).
This patent grant is currently assigned to The F. & M. Schaefer Brewing Company. Invention is credited to John B. Bocklemann, Frede B. Strandskov.
United States Patent |
3,860,729 |
Strandskov , et al. |
January 14, 1975 |
**Please see images for:
( Certificate of Correction ) ** |
PRESERVATION OF BEVERAGES WITH POLY(HEXAMETHYLENEBIGUANIDE
HYDROCHLORIDE)
Abstract
Beverages are preserved against undesirable microbial growth by
incorporating into the beverage a polymeric biguanide compound of
the formula ##SPC1## Wherein n is such that the average molecular
weight lies between 900 and 1,300.
Inventors: |
Strandskov; Frede B. (North
Caldwell, NJ), Bocklemann; John B. (Tenafly, NJ) |
Assignee: |
The F. & M. Schaefer Brewing
Company (Brooklyn, NY)
|
Family
ID: |
23597601 |
Appl.
No.: |
05/403,970 |
Filed: |
October 5, 1973 |
Current U.S.
Class: |
426/330.3;
426/335; 426/599; 514/635; 426/326; 426/592; 426/330 |
Current CPC
Class: |
A23L
3/3526 (20130101); A23L 2/44 (20130101); C12H
1/14 (20130101) |
Current International
Class: |
A23L
2/42 (20060101); A23L 2/44 (20060101); A23L
3/3526 (20060101); A23L 3/3463 (20060101); C12H
1/00 (20060101); C12H 1/14 (20060101); A23l
003/34 () |
Field of
Search: |
;426/151,227,326,329,330,335 ;424/326 ;252/401,405 |
References Cited
[Referenced By]
U.S. Patent Documents
Other References
P A. Leeming et al., Chemical Abstracts, Vol. 70, 1969, 116162d.
.
W. Keane, Chemical Abstracts, Vol. 74, 1971, 128000v..
|
Primary Examiner: Monacell; A. Louis
Assistant Examiner: Ribando; Curtis P.
Attorney, Agent or Firm: Wenderoth, Lind & Ponack
Claims
We claim:
1. A method of preserving a beverage selected from the group of
fruit and vegetable juices, soft drinks and light alcoholic
beverages against undesirable microbial growth which comprises
incorporating into the beverage prior to packaging the polymeric
biguanide material of the formula ##SPC4##
wherein n is such that the average molecular weight lies between
900 and 1,300
the amount of the polymeric biguanide incorporated being sufficient
to preserve the beverage against undesirable microbial growth.
2. A method according to claim 1 wherein the amount of polymeric
biguanide incorporated into the beverage is from 0.4 to about 50
ppm.
3. A method according to claim 2 wherein the amount of polymeric
biguanide incorporated into the beverage is from 1 to about 10
ppm.
4. A method according to claim 1 wherein the beverage is a light
alcoholic beverage.
5. A method according to claim 4 wherein the beverage is a
beer.
6. A method according to claim 5 wherein the amount of polymeric
biguanide incorporated into the beer is from 0.4 to about 5
ppm.
7. A method according to claim 6 wherein the amount of polymeric
biguanide incorporated into the beer is from about 1.0 to about 2.0
ppm.
8. A composition which comprises a beverage selected from the group
of fruit and vegetable juices, soft drinks and light alcoholic
beverages having incorporated therein the polymeric biguanide
material of the formula ##SPC5##
wherein n is such that the molecular weight lies between 900 and
1,300
the amount of the polymeric biguanide present being sufficient to
preserve the beverage against undesirable microbial growth.
9. A composition according to claim 8 wherein the amount of
polymeric biguanide present is from 0.4 to about 50 ppm.
10. A composition according to claim 9 wherein the amount of
polymeric biguanide present is from about 1 to about 10 ppm.
11. A composition according to claim 8 wherein the beverage is a
light alcoholic beverage.
12. A composition according to claim 11 wherein the beverage is a
beer.
13. A composition according to claim 12 wherein the amount of
polymeric biguanide present in the beer is from 0.4 to about 5
ppm.
14. A composition according to claim 13 wherein the amount of
polymeric biguanide present in the beer is from about 1.0 to about
2.0 ppm.
Description
This invention relates to the preservation of beverages against
undesirable microbial growth to prevent spoilage during
storage.
It is necessary in the beverage industry to take steps to make
certain that the beverage does not become spoiled due to
undesirable microbial growth in the package between the time of
packaging and ultimate consumption. In the past this has involved
such measures as pasteurization of the packaged article or constant
refrigeration of the packaged beverage from the time of packaging
until consumption. Each of these measures is, of course, expensive
and thus adds to the final cost of the beverage to the consumer.
Pasteurization is also attended with the disadvantages that the
strength of the beverage container must be greater in order to
withstand the high temperatures and pressures involved and that
adverse affects on the quality of the beverage often occur.
In recent years other measures have been tried in order to
eliminate the need for pasteurization and/or refrigeration. One of
these is the microfiltration method whereby harmful microorganisms
are filtered out of the beverage immediately prior to its
introduction into the final package. This method is attended with
difficulty also since the filtration procedure is somewhat
expensive and highly sterile conditions must be maintained during
the filling operation if it is to be effective.
Another, and more acceptable measure which has been developed is
that of incorporating one or more preservative agents into the
beverage prior to place it into the final container. The
preservative is used in an amount which will prevent the growth of
the beverage spoiling microorganisms. An example of this method is
disclosed in U.S. Pat. No. 3,175,912 wherein the heptyl or octyl
ester of parahydroxybenzoic acid or an alkali metal or alkaline
earth metal salt thereof is incorporated into the beverage, e.g.,
finished unpasteurized beer. While this method, and particularly
utilizing these materials, has met with very great success, it is
still attended by certain difficulties. The materials to be used
are sometimes expensive and it is frequently necessary to use large
amounts of the materials. Often the materials are only slightly
soluble in the beverage and it is necessary to work at levels which
approach the limit of solubility of the material. Extensive
research has thus been devoted to locating additional materials
which will act as preservative agents in beverages and the use of
which will not be attended with the difficulties encountered in the
past. The present invention is based upon the discovery of such a
material.
The beverages which can be preserved according to this invention
are quite numerous and extend to all of those which do not have a
chemical incompatability with the particular material which is
utilized. These would include fruit and vegetable juices, both
natural and artificial, soft drinks, both carbonated and
non-carbonated, as well as light alcoholic beverages such as cider,
wines and beers, e.g., lager beer, porter and stout; ale and malt
liquor are also intended within the meaning of "beer." In the
present description, the emphasis is primarily directed to the
preservation of beers, however, it is to be understood that the
invention is applicable to a broad range of beverages.
The material which is employed as the preservative agent in the
present invention is a polymeric biguanide compound of the formula
##SPC2##
wherein n is such that the average molecular weight lies between
900 and 1,300.
The material may be prepared in the following manner:
Hexamethylene diamine carbonate is formed by passing CO.sub.2 into
hexamethylene diamine. This is then reacted at 60.degree.C. with
zinc dicyanimide to form a solution of the hexamethylene diamine
salt of dicyanimide. This solution is further reacted with
hexamethylene diamine hydrochloride at 150.degree.-155.degree.C. to
give the product of the above formula. See U.S. Pat. No. 2,643,232
and No. 3,428,576 for more detailed information regarding the
product and the method of making it.
The polymeric biguanide material has been described in terms of the
hydrochloride salt. It is to be understood, however, that other
inorganic acid salts may be employed and for purposes of this
invention are deemed to be the equivalents of the hydrochloride. It
is also to be understood that the average molecular weight of the
product may vary from the specific range given without adversely
affecting the results. This material is known to be a biocide and
solutions containing the material have previously been marketed as
a disinfecting solution for plant equipment used in the brewing,
foodstuffs and soft drink industries. In connecting with the
previously proposed use of the material as a sanitizing agent for
brewing plant equipment, very small amounts of the material have
been added to beer to determine any adverse effects upon foam,
chill stability, and taste due to the possibility of any chance
contamination of the beer which might occur if any of the compound
were to be employed in filler sanitation. The amounts of the
material added were, however, far below the amounts employed in the
present invention and also well below the levels necessary to
achieve preservation of the beer. To the knowledge of the present
inventor, this material has not previously been suggested for
incorporation into a beverage for preservation or at a level which
would be necessary to achieve effective preservation of the
beverage without pasteurization.
In accordance with this invention, the preservation of the beverage
is achieved by the incorporation into the finished beverage, e.g.,
beer, for intimate admixture therewith the polymeric biguanide
material: ##SPC3##
wherein n is such that the average molecular weight lies between
900 and 1,300. The term "finished beverage" is used herein to refer
to beverages which contain all of the necessary additives to make
them commercially acceptable products and which have been subjected
to any final filtration which may be necessary or desirable. In the
case of beer, it refers to beer which has been subjected to polish
filtration. The material can, of course, be added at any time
during the processing of the beverage so long as it does not
interfere with the subsequent processing and so long as the
subsequent processing does not interfere with the effectiveness of
the material in achieving preservation of the beverage.
The material can be added to the beverage in any convenient form.
It is preferred, due to ease of handling, to add it in the form of
a stock solution wherein the material is dissolved in solvent which
itself has no deleterious effect upon the beverage. In view of the
high solubility of the polymeric biguanide material in water, an
aqueous solution, e.g., a 20 percent aqueous solution, is
particularly suitable. This high water solubility of the material
is one of the factors which increases the value of the present
invention since the aqueous solutions offer particularly noteworthy
ease of handling.
The amount of the polymeric biguanide material employed will vary
over a wide range depending upon the type of beverage being
preserved and upon the magnitude of preservation to be obtained. In
general, the amounts will extend from as low as about 0.4 parts by
weight per million parts by volume (ppm) of the beverage employed
up to about 50 ppm. The preferred range in beverages generally will
be in the range of about 1 to about 10 ppm. In beer, it has been
found that the range will generally be from about 0.4 to about 5.0
ppm, with a range of about 1.0 to about 2.0 ppm being preferred.
Greater amounts of the material can be employed but are not
recommended since they are unnecessary to achieve preservation and
since the addition of any foreign material to a consumable beverage
should be held as low as possible. One of the outstanding
advantages of this invention is that the polymeric biguanide
material can be utilized in extremely small amounts to achieve
effective preservation of the beverage.
The minimum level of the material necessary to achieve preservation
will, of course, be affected by the degree of sanitation achieved
in the plant facility wherein the beverage is filled into the final
container. It therefore is advisable to maintain the degree of
sanitation at the highest level which is economically feasable.
The present invention is applicable to various forms of containers
for the beverages. It is contemplated that cartons, bottles, cans,
kegs, tank trucks and the like can be employed.
The beverage to be preserved can also be one which contains
additives of various types which are used to improve the desirable
properties of the beverage. Such additives may for example be color
or taste improvers, or, for example, in the case of beer, additives
which are used to improve the foaming qualities and/or chill
stability properties of the beverage. Another outstanding advantage
of the present invention is that the amounts of the polymeric
biguanide material which achieve effective preservation are so low
as to have a slight, if any, effect upon the properties of the
beverage. This is not always the case with other materials which
have been previously used to achieve preservation of beverages.
Some of these have been found to impart adverse effects upon the
quality of the beverage and have necessitated in certain cases the
addition of other additives to overcome such adverse effects. It
may be found that the polymeric biguanide material can also
effectively be utilized in conjuction with other preservative
materials. Such combinations of preservatives may be found to be
particularly effective for the preservation of certain particular
beverages.
In the instant disclosure, the relationship between parts by weight
and parts by volume is the same as that between grams and
milliliters. Parts per million (ppm) is uniformly parts by weight
of additive per million parts by volume of finished beverage.
The Examples as set forth hereinafter are purely illustrative of
the invention and should not be construed as being exhaustive or
limitative thereof. In the Examples, beer is utilized as the
beverage. It is, however, to be understood that the instant
invention is applicable to other beverages as well.
EXAMPLES 1 AND 2
From the regular production line, each of a group of clean, 12
ounce brown beer bottles is filled with cold, unpasteurized
finished beer into which no microbiological preservative has been
incorporated. The beer in foamed up to expel headspace air and the
bottles are capped. Each of these bottles contains 350 ml. of
unpasteurized lager beer. These bottles are utilized as the control
in the Examples.
Stock Solutions
A series of stock solutions are made up in the following
manner:
A required amount of the 20 percent aqueous solution of the
polymeric biguanide material is diluted to 200 ml. with distilled
water. The amount of the 20 percent water solution is chosen so
that the addition of 0.5 ml. of the thus prepared stock solution to
350 ml. of beer yields a solution containing a desired amount of
the polymeric biguanide material.
The stock solutions thus prepared are as follows:
Amount of Polymeric Biguanide Present When 0.5 ml. of Stock
Solution is Added to 350 ml. Stock Solutions of Beer (PPM)
______________________________________ 1 0.1 2 0.2 3 0.4 4 0.5 5
1.0 6 2.0 7 5.0 ______________________________________
EXAMPLE 1
Into each of a group of three clean, 12 ounce brown beer bottles is
placed 0.5 ml. of stock solution 2. These bottles are filled from
the regular production line with cold, unpasteurized finished beer.
The beer is foamed up to expel headspace air and the bottles are
capped. Each of these bottles contains 350 ml. of beer together
with the stock solution. In the same manner 0.5 ml. of stock
solution 3, 5 and 6 are respectively added to groups of three
clean, 12 oz. brown beer bottles and the bottles are filled with
cold, unpasteurized finished beer. The beer is foamed up to expel
headspace air and the bottles are capped. Each of the bottles
contains 350 ml. of beer together with the stock solution.
All of the thus prepared bottles together with control bottles are
stored at room temperature and periodically (weekly) examined for
microbial spoilage. Spoilage is readily observed by a marked amount
of sediment in the beer and by the unpleasant taste and odor
produced by microbial growth and metabolism.
In the observations, the amount of sediment is visually observed
and estimated on a scale of 1 to 9+. A value of 9+ reflects
spoilage of the beer.
The results are set forth in the following Table A:
Table A
__________________________________________________________________________
Polymeric Biguanide SEDIMENT READINGS AFTER: PPM. 5 Weeks 9 Weeks
14 Weeks 24 Weeks 30 Weeks
__________________________________________________________________________
Control 0 9+-9+-9+ 9+-9+-9+ 9+-9+-9+ 9+-9+-9+ 9+-9+-9+ 0.2 2-3-9
9+-9+-9+ 9+-9+-9+ 9+-9+-9+ 9+-9+-9+ 0.4 1-1-1 1-2-1 1-2-3 3-3-4
3-3-4 1.0 1-1-1 1-3-2 1-3-3 2-2*-2* 3-4-4 2.0 1-1-1 3-1-2 2*-2-2
2-2-3 6-4-5
__________________________________________________________________________
*The slightly lower sediment readings on these bottles compared
with the values in the previous readings were due to minor
experimental error in the visual estimation method employed.
EXAMPLE 2
Into groups of three clean 12 oz. brown beer bottles is placed 0.5
ml. of each of stock solutions 1, 2, 4, 5, 6 and 7 respectively in
the manner of Example 1. These bottles are filled with cold,
unpasteurized finished beer from the production line. The beer is
foamed up to expel headspace air and the bottles are capped. Each
of the bottles contains 350 ml. of beer together with the stock
solution.
The bottles together with control bottles are stored at room
temperature and periodically (weekly) examined for spoilage in the
same manner as Example 1.
The results are set forth in the following Table B:
TABLE B
__________________________________________________________________________
Polymeric Biguanide SEDIMENT READINGS AFTER: PPM. 7 Weeks 12 Weeks
22 Weeks 28 Weeks
__________________________________________________________________________
Control 0 9+-9+-9+ 9+-9+-9+ 9+-9+-9+ 9+-9+-9+ 0.1 9+-9+-9+ 9+-9+-9+
9+-9+-9+ 9+-9+-9+ 0.2 9+-9+-9+ 9+-9+-9+ 9+-9+-9+ 9+-9+-9+ 0.5
9+-6-2 9+-9+-4 9+-9+-5 9+-9+-9+ 1.0 1-2-4 3-3-9+.sup.(1) 4-4 3*-6
2.0 1-1-1 2-3-2 4-3-3 3*-2*-3 5.0 1-3-2 2-3-2 3-3-3 3-4-2*
__________________________________________________________________________
.sup.(1) negative acetic acid bacterial growth; test terminated
with respect to this bottle. *The slightly lower sediment readings
on these bottles compared with the values in the previous reading
were due to minor experimental error in th visual estimation method
employed.
The foregoing Examples demonstrate the extremely good preservative
ability of the polymeric biguanide material at very low levels.
EXAMPLES I TO VI
The following Examples demonstrate the chill stability and foam
properties of beer containing the polymeric biguanide material as
well as other materials for comparative purposes.
Stock Solutions
Various stock solutions are prepared as hereinafter disclosed for
use in the following Examples.
Stock Solution No. I
Dissolve 1,680 mg. of n-heptyl para-hydroxybenzoate (WS-7) in a
sufficient amount of 95 percent ethanol to make 200 ml. of
solution. The addition of 0.5 ml. of this stock solution,
containing 4.2 mg. of WS-7, to 350 ml. of beer yields a solution
containing 12 ppm. of the benzoate.
Stock Solution No. II
Dilute 1.4 ml. of the 20 percent aqueous solution of the polymeric
biguanide to 200 ml. with distilled water. The addition of 0.5 ml.
of this stock solution, containing 0.70 mg. of the polymeric
biguanide, to 350 ml. of beer yields a solution containing 2 ppm.
of the polymeric biguanide.
Stock Solution No. III
Dissolve 10.5 gms. of Kelcoloid-O (Kelco Co.) a propylene glycol
alginate produced in accordance with a process disclosed in U.S.
Pat. No. 2,659,695, (hereinafter referred to as KDO), with vigorous
agitation in sufficient distilled water to make 1,000 ml. of
solution. The addition of 2.0 ml. of this stock solution,
containing 21 mg. of KDO, to 350 ml. of beer yields a solution
containing 60 ppm. of KDO.
In these examples, the following procedures and standards are
employed.
The Determination of Beer Foam Adherence
The procedure is that of Henry L. Ziliotto, John B. Bockelmann and
William Tirado of The F. & M. Schaefer Brewing Company,
Brooklyn, N.Y. Said procedure was presented before the annual
meeting of the American Society of Brewing Chemists in 1962. It
comprises the creation of foam, the development of foam curtains
and the measurement of foam adhering to the glass.
A. Formation of Foam Curtains
Attemperate beer at least over night at 10.degree.C.
Use 6 oz. shell glasses that have been numbered on the side near
the base and marked with five spots uniformly spaced around the
periphery of the bottom, one of the marks being more pronounced
than the others. These marks serve as position guides when reading
the instrument. Pour the beer into a glass by the method for Foam
Life (Ziliotto, H., Bockelmann, John B., "American Society of
Brewing Chemists Proceedings," 1954, page 108) to form a head of
foam between 20 and 35 millimeters (mm.) in height. When the foam
has collapsed (indicated by a change in color of the foam surface
or by the beer's starting to show through), encircle the glass at
the beer-foam interface with an 8 inch length of black adhesive
tape of 3/4 inch to 1 inch width. (The foam height at zero time and
the rate of foam collapse need not be measured unless it is desired
to determine Foam Life at the same time.) Immediately remove every
drop of beer in the glass by means of an aspirator, taking care not
to disturb the adhering foam. Let the glass dry in air a minimum of
ten minutes, and measure the height of the exposed surface between
the tape and the top of the glass. Wipe the exterior of the glass
with a damp cloth and polish dry.
B. Instrument Readings
The Radiometer described by Thorne, R. S. W., and Beckley, R. F.,
"Journal of the Institute of Brewing," 64, 38 (1958) is employed
for making the readings, but the light intensity is reduced by
inserting a variable rheostat in the lamp circuit in a manner that
will not affect the operation of the built-in fan or other
circuitry. Set the rheostat to give 60 volts for measurement of
foam adhesion. Raise again to full current at the termination of
the test for future turbidity readings.
On the leading edge of each vane of the centering mechanism of the
instrument slip on a 45 mm. length of rubber tubing (6 mm. bore and
2 mm. walls) that has been slit its full length. Fasten a piece of
tape over the top end of the tubings so that they will not slip
down. When in position, the bottom ends should just clear the top
of the support described later. This modification properly centers
the glasses despite slight differences in diameter between them and
their support.
Do not use water in the cell compartment.
Place a stack of four discs centrally at the bottom of the
compartment to act as a support for the glasses. The discs have a
diameter just a trifle larger than that of the glasses (59 to 60
mm. diameter for a 55 mm. I.D., 58 mm. O.D., glass) and are painted
a dull black. The bottom one is 25 mm. thick while each of the
other three is 10 mm. thick.
Invert the glass with foam curtains onto the stack of discs and
position the principle mark on the glass toward the light source.
Close the cover of the instrument and after turning the current on,
momentarily depress the lamp switch to activate the incident light.
Note any deflection of the meter needle. Release the lamp switch
and adjust the diaphragm dial by an amount estimated to be
sufficient to bring the needle to zero. Repeat the illumination and
the adjustment a number of times until a dial reading is obtained
that is constant within 0.1 unit for a zero needle deflection.
Record the reading. Rotate the glass one-fifth turn around its
axis, using the marks on the glass for guides, and obtain a new
reading as previously obtained. Continue in this manner for five
readings. If another level of adhered foam must be read, remove the
topmost disc to lower the glass and obtain another five readings
around the glass. Proceed thusly for a third level. Use the
following table to decide on the number of levels to be
measured.
______________________________________ Height of Number of Levels
Foam Curtains to be Measured ______________________________________
0 - 14 mm. 1 15 - 24 2 25 - 36 3
______________________________________
Calculate to the second decimal the average of all readings.
Obtain blank readings on the clean glass without removing the tape,
by the procedure followed for the run. When blank readings have
once been obtained on a glass at the three planes, use the data for
subsequent determinations. Occasionally, recheck the readings to
correct for surface changes.
Subtract the average blank reading from that of the run to obtain
foam adhesion in the one glass. Report to the first decimal the
grand average of six determinations (two pours from each of three
replicate bottles, or single pours from six bottles) as the foam
adhesion of the beer tested.
Tests have shown that no detectable change in readings of dry foam
occur during the three day's standing at room temperature. This
finding makes it convenient to postpone reading the glasses in the
instrument until all beers of a series have been poured. As a
precautionary note, do not cover wet glasses for any reason
inasmuch as the entrapped vapors dissolve the foam or change its
appearance.
C. Visual readings
Subsequent to the cited publication estimations of the adhering
foam have also been obtained visually as follows:
Critically examine the beer glass containing the dry film of foam
and estimate the average per cent of the circumferential surface
between the tape and the top of the glass that was originally
covered by foam bubbles. Express foam adhesion as one-tenth of the
percentage figure obtained.
Chill Haze Measurement
The procedure utilized is that of The F. & M. Schaefer Brewing
Co., Brooklyn, N.Y. and as the procedure for the determination of
foam adherence, does not constitute a part of the instant
invention, it is described only to assist in the full appreciation
of the data presented.
Chill the upright samples of bottled beer for the specified time in
a bath maintained at 0.degree.C.
Using a viewing box, such as Clark turbidimeter (Cargille
Scientific Co., New York, New York), determine the turbidity of the
sample by visually matching the haze of the supernatant fluid with
the suspended haze of standards in bottles of the same shape and
color as that containing the sample. The haze standards may be
either the Formazin standards of the American Society of Brewing
Chemists (A.S.B.C. Proceedings 1957, page 165) or suspensions of
insoluble substances that have been visually standardized against
the Formazin standards. The Schaefer haze standards have nominal
values ranging from 0 to 9, a unit of which is the visual
equivalent of 30 Formazin units; i.e., a Schaefer haze of 2 equals
60 Formazin units.
Description of Foam Life Measurement
The foam life measurement is carried out according to the procedure
described by Ziliotto and Bockelmann in the American Society of
Brewing Chemists Proceedings of 1954, pages 108-210. This method
incorporates the pouring of the beer from a 12 oz. bottle into a
standard 6 oz. glass in such a way that a foam head of about 25
millimeter height (20 to 35 mm. is acceptable) is formed. The
average time, in seconds, required for the collapse of the foam
head of twelve pourings is recorded. By direct proportion calculate
the life of 25 mm. of original foam and express the average results
of twelve calculations as the foam life.
EXAMPLES I TO VI
Example I
Fill each of a group of clean, 12 oz. brown beer bottles with cold,
unpasteurized finished beer to which no preservative has been
added. Foam up the beer, to expel headspace air and cap. Pasteurize
the bottles from this group. Each bottle prepared in this manner
contains about 350 ml. of pasteurized lager beer. These bottles are
utilized as the control in foam and chill stability tests, the
results of which appear in Table I.
Example II
Fill each of a group of clean, 12 oz. brown beer bottles with the
same beer as used in Example I. Add, to each filled bottle, 2.0 ml.
of stock solution No. III (KDO). Foam up the beer to expel
headspace air and cap. Pasteurize the bottles from this group. Each
bottle prepared in this manner contains about 350 ml. of
pasteurized lager beer and 60 ppm. KDO. The results of foam and
chill stability tests on these bottles appear in Table I.
Example III
Place 0.5 ml. of stock solution No. 1 (WS-7) into each of a group
of clean 12 oz. brown beer bottles. Fill each of the bottles with
the same beer as used in Example I. Foam up the beer to expel the
headspace air and cap. Each bottle prepared in this manner contains
about 350 ml. of unpasteurized preservative treated beer. The
concentration of WS-7 present is about 12 ppm. The results of foam
and chill stability tests on these bottles appear in Table I.
Example IV
Place 0.5 ml. of stock solution No. I (WS-7) into each of a group
of clean 12 oz. brown beer bottles. Fill each of the bottles with
the same beer as used in Example I. Add to each bottle 2.0 ml. of
stock solution No. III (KDO). Foam up the beer to expel the
headspace air and cap. Each bottle prepared in this manner contains
about 350 ml. of unpasteurized preservative and KDO treated beer.
The concentrations of WS-7 and KDO are about 12 and 60 ppm.,
respectively. The results of foam and chill stability tests on
these bottles appear in Table I.
Example V
Place 0.5 ml. of stock solution No. II (polymeric biguanide) into
each of a group of clean 12 oz. brown beer bottles. Fill each of
the bottles with the same beer as used in Example I. Foam up the
beer to expel the headspace air and cap. Each bottle prepared in
this manner contains about 350 ml. of unpasteurized preservative
treated beer. The concentration of polymeric biguanide is about 2
ppm. The results of foam and chill stability tests on these bottles
appear in Table I.
Example VI
Place 0.5 ml. of stock solution II (polymeric biguanide) into each
of a group of clean 12 oz. brown beer bottles. Fill each of the
bottles with the same beer as used in Example I. Add to each bottle
2.0 ml. of stock solution No. III (KDO). Foam up the beer to expel
the headspace air and cap. Each bottle prepared in this manner
contains about 350 ml. of unpasteurized preservative and KDO
treated beer. The concentrations of polymeric biguanide and KDO are
about 2 and 60 ppm., respectively. The results of foam and chill
stability tests as these bottles appear in Table I.
TABLE I
__________________________________________________________________________
CHILL HAZE AFTER
__________________________________________________________________________
EXAMPLE 3 DAYS 2 WEEKS 4 WEEKS 6 WEEKS 8 WEEKS 12
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WEEKS I Control 0-0-0-0-0-0 0-0-0-0-0-0 3-3-3-3-3-3 3-3-3-3-3-3
3-3-3-3-4-5 4-4-4-4-4-5 II KDO 60 ppm 0-0-0-0-0-0 0-0-0-0-0-0
1-1-1-1-1-1 1-1-1-1-1-1 1-1-1-1-1-1 1-1-1-1-1-1 III WS-7 12 ppm.
0-0-0-0-0-0 0-0-0-0-0-0 3-3-3-3-3-3 3-3-3-4-4-4 4-4-5-4-6-6
4-4-4-6-7-7 IV KDO 60 ppm. + WS-7 12 ppm. 0-0-0-0-0-0 0-0-0-0-0-0
1-1-1-1-1-0 1-1-1-1-1-1 1-1-1-2-2-* 3-3-3-3-3-* V Polymeric
biguanide 2 ppm. 0-0-0-0-0-0 0-0-0-0-0-0 0-0-0-0-0-0 1-1-1-1-1-1
1-1-1-1-1-1 3-3-3-3-3-3 VI KDO 60 ppm. + Polymeric biguanide 2 ppm.
0-0-0-0-0-0 0-0-0-0-0-0 0-0-1-1-1-1 1-1-1-1-1-1 1-1-1-1-1-1
2-2-2-2-2-2
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FOAM PROPERTIES
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FOAM LIFE (SEC.) FOAM ADHESION FRESH 2 Weeks at 90.degree.F FRESH 2
Weeks at 90.degree.F
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102 94 7.1 6.8 114 102 6.8 7.6 92 86 3.8 3.8 108 111 2.6 0.5 100
100 7.3 6.9 107 108 6.8 6.7
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*Bottle opened for inspection.
From the foregoing Examples I to VI it is seen that the WS-7
preservative material has an adverse effect on the foam life and
foam adherence properties of the beer. These adverse effects on
foam life are overcome by incorporating KDO into beer. In
contradistinction, the polymeric biguanide material has no adverse
effect upon the foam life and foam adherence properties of the
beer. The data demonstrate that a commercially acceptable beer can
be produced using the polymeric biguanide material alone without
the addition of KDO.
The invention has been illustrated above by reference to small
quantities of the beverage. It will be apparent to the art skilled
that the preservative method can be scaled up to producing
commercial quantities of the beverage. In this respect a stock
solution of the polymeric biguanide material is first prepared.
This stock solution is then injected into the beverage pipeline at
the desired stage of production as the beverage flows through the
line. The rate of injection is, of course, correlated to the flow
rate of the beverage. The proper proportioning is achieved through
means which are per se known. The beverage containing the additive
is then filled into the desired container. In a batch operation a
desired amount of a stock solution is added to the beverage batch
and admixed therewith. The filling operation is then completed to
obtain the final packaged beverage article.
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