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THE EFFECT UT ACIUITY UR KEEPING QUALITY
RE BUTTER WITH SPECIAL REFERENCE
TU SWEET CREAM BUTTER
THESIS FOR DEGREE OF M. 8.

ROBERT EDWARD VINCENT

1928

 

 

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UBRARY
Michigan State
Universii‘y

 

 

 

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5/08 K'lPrqlAcc8PreleIRC/Date0ue Indd

 

 

THE EFFECT OF ACIDITY on KEEPING QUALITY
' or BUTTER WITH SPECIAL REFERENCE To
SWEET exam BUTTER

The Effect OfrAcidity 0n Keeping Quality
Of Butter With Special Reference To

Sweet Green Butter

Thesis

Reapectfully submitted to the Faculty of
Michigan State Gollege in partial fulfill-

nent of the requirements for the degree of

Hester of Science .

BY
Robert Edward Vincent
“a

1928

ACKNO'IILEMLHBNTS

rho author wishes to express his appreciation
to 0. 3. Reed, Professor of Dairy Husbandry and P3 S.
Incas, Associate Professor of Dairy Manufacture, for
their guidance, valuable suggestions, and criticisms
in planning this work and the preparation of this thesis.
The author also wishes to eXpress his apprecia-
tion to c. D. Ball, dssistant Professor of Chemistry, for
information, generous cooperation, and criticisms on the

chemical analysis of this thesis.

10%023

TABDB OF CONTENTS

Page
Introduction
Review of Literature
.A. Sweet cream butter 1
B. Starters
6. Summary of Review of Literature 7
Experimental Work
A. Procedure
1. Object of Experiment 9
2. Part I
(a). Preparation of Starter 10
(b). Preparation of Bream for
churning 11
etc). The Churning Process 12
(d). Preparation and care of
- samples 13
' (0). Judging the butter 15
3. Part II
(a). Analysis of cream. 15
(1:). Analysis of buttermilk 15
(0). .Analysis of butter
Eil). Preparation of sample 16
(2). Determination of moisture,

(3).

butterfat, salt and curd. 15
Determination of amino-

nitrogen 15

P389

(4). Determination of total
nitrogen
(d). IAnalysis of butterfat
(1). Preparation of sample.
(2). 9etermination of Reichert
Meissl Number
(3). Determinatinn of Iodine
Number
(4). Determination of Acid
’ Number
(5). Test for oxidized Fat

(Kries Test)

Results and Discussion

A.

30'

O.
D.
B.
I.
G.
H.

Curd Content

.Amino Nitrogen

Total Nitrogen

Rsichert Meissl Number

Iodine Number

Acid Number

Test for Oxidized Pat (Kries Test)
Scores 1
‘ 1. Summary of results on Flavor

2. Summary of results on Keeping Quality

Conclusions
Bibliography
Appendix

16

16

17

17

17

18

19

21
23

$8

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46
47
4B
51
55

INTRODUCTION

The art of buttermaking originated in Asia and
Burcpe and from there was communicated to other parts
of the world. Records from the Bible show that butter
was used before 2000 B. C. (1) Butter was held in high
esteem and was used for the holiest sacrifices. (2)

Buttermaking was confined in this country to the
farm dairy until the middle of the nineteenth century,
but about this time the factory system of buttermaking
was introduced. inbout the time of the establishment of
the early creameries many revolutionary inventions and
investigations were given to the dairy world. Among these
were pasteurization and the use of pure cultures for the
ripening of cream and developing of desirable flavors and
odors in the butter.

It is quite interesting to note the existing
differences that have developed between what we term
quality today and that of centuries ago. In mediaeval
times peOple thought that butter should be stored for long
periods to develop all sorts of odors and tastes before it
was usable. Today the market demands a butter of dis-
tinguished quality.

Danish butter which is given first consideration
by the critical English butter buyers is made primarily

g4

 

from sweet cream slightly ripened by the addition of a
starter. With the use of starter Danish buttermakers
are enabled to control and maintain a uniform flavor in
their butter. ‘

rho manufacture of sweet cream butter was begun
in the united States about forty years ago. In recent
years there has been an increased interest in the manu-
facture of sweet cream butter. A.group of creameries in
the State oerinnesota are making sweet cream.butter, to
which.no starter is added. The cream must be sweet to
the taste and the acidity not over 0.2 per cent by test.
(3) rho specifications used by this group are simply
modifications of those drawn up by the Bureau of Dairying,
Uhited States Department of Agriculture to'be followed in
the manufacture of butter for the navy.

With the increased interest in sweet cream'butter,
the question arises as to its flavor and keeping quality
as compared with that of sweet cream.butter to which starter
has been added. .Ln attempt to answer this question is
made in this thesis.

L.

REVIEW OF LITBnATURE
Sweet cream butter

In 1890 G. W. Curtis (4) of Texas made comparisons
between sweet and sour cream butter. The sweet cream was
divided equally, one-half churned immediately, while the
other was allowed to become slightly acid before churning.
The results showed that nearly like amounts of butter were
obtained from each and that there was scarcely a notice-
abli difference between the two kinds of butter, the
difference, if any, being in .favor of the sweet cream
butter and this due chiefly to the flavor.

During the same year 0. E. Patrick (5) of Iowa State
College repeated the experiment of Curtis. He concluded
that there was no very marked difference in the keeping
quality of the two butters, what difference there was being
in favor of the sweet cream product. As to flavor, for the
first two or three months most of the scorers preferred the
ripened cream butter declaring that made from sweet cream
to be comparatively "flat", "insipid" or flavorless", but
the longer the butters were kept, even while both were still
sweet, the less marked became the difference between them in
this respect.

In 1892 Patrick (6) made nine comparative trials, by
dividing by weight a quantity of sweet cream into two equal
parts. one of these parts was churned immediately while the

L4

 

2
other part was ripened at 60° 1. for 24 to 48 hours. The
sweet cream butter suffered less deterioration by keeping
five months (50° F.) than did the sour cream product. The
former acquired in a measure the flavor and aroma of
ripened cream butter. In 1895 Patrick (7) repeated the
same experiment and the results agree perfectly with the
results obtained in 1892.

In 1904 (9) Dean compared butter made from sweet
cream with butter made from sweet cream to which 20 to so
per cent starter was added. The butter made by the latter
method was superior in quality to that of the sweet cream
butter. He also reported that when sweet cream to which
27.5 per cent starter was added at the time of churning,
better results were obtained than from ripened cream.

Gray (10) of‘the United States Department of'Agricul-
ture in 1906 found that when butter was-made from sweet
cream, the product kept well while stdred at ~100 to 100 F.
and, when removed from storage, this butter kept well, while
butter made from sour cream kept well in storage at ~10° I
to 10° F. but deteriorated rapidly after removal from
storage, giving on the whole, results which were very un-
satisfactory.

Charron and Shult (11) in 1907 found that when they
compared sweet cream.butter with ripened cream butter, the
keeping quality of the sweet cream butter was superior to

the keeping quality of the ripened cream butter and that by

the sweet cream process there is no greater loss of
butterfat than when churning ripened cream.

Rogers, Thompson and Keithley (12) of the United
States Department of Agriculture in 1912 found that the
scores of various samples of butter stored for 40 days
at 0° P., 150 days at 0° P., and 150 days at 20° P.
respectively, ranged with two exceptions, above 90 for the
butter made from cream with an acidity below 0.3 per cent,
while those fromicream testing higher in acidity were
variable but usually scored below 90. The deterioration
of the sweet cream butter at 200 P. was slight. The de-
terioration in the pasteurized, ripened cream butter stored
at 0° 1., was four times as great as that in the pasteurized,
sweet cream butter at the same temperature.

In 1916 R. 0. Potts (13) stated that the experience
of those who have stored southern creamery butter indicated
that it had about the same keeping quality as other creamery
butter of the same grade or quality; and that low acidity,
good quality of cream used, and good quality of butter were
factors causing it to hold up better. in storage. He
recommends that butter for storage be produced from
pasteurized, sweet cream.

Nortensen (14) did considerable work with sweet cream
butter. He divided a quantity of cream into three lots, one
lot of which was cooled immediately to a temperature of 40° P..

held for three hours or longer, and then churned sweet. .1

_second lot was cooled to 400 F., but from 10 to 20 per cent
starter was added and then was held for three hours. The
- third lot was cooled to ripening temperature. Starter was-
added and the cream allowed to ripen until the desired
acidity was reached. The butter made from ripened cream
deteriorated faster than butter made either from sweet cream,
or from sweet cream and starter. Where low ripening was
employed, the ripened butter at the end of a two months cold
storage period was of about the same quality as the sweet
cream.butter, and the sweet cream and starter butter. He
stated also, that unless a creamery has a special demand for
sweet cream.butter, it would seem to be most advantageous to
produce butter from cream ripened to a low degree of acidity.
The work of White (15) is the most recent on sweet
cream.butter. .A quantity of sweet cream was divided into
three equal parts. The acidity of “A" was 0.15 per cent;
"B" was standardized to 0.25 per cent; and "C" standardized
to 0.51 per cent acidity, using a good lactic culture for
standardizing. In this series the acidity was standardized
before pasteurization. In a second series the cream was
pasteurized sweet, acidity averaging 0.15 per cent, divided
in three lots, and each lot standardized to the same degree
of acidity, as in the previous series, using a good lactic
culture for standardizing. A.third series was run in which
cream was pasteurized sweet and two of the portions ripened

to 0.35 and 0.45 per cent acidity, respectively, then churned.

\—

 

Samples of'all churningawere scored when fresh, then were
stored at 0° P. for eight months and rescored. The con-
clusions drawn from these experiments were: there appeared
to be no material difference in the keeping quality of the
butter due to standardizing the acidity of the cream before
pasteurization as compared with standardizing after pasteuri-
zation. Butter made from.cream.of 0.25 per cent acidity kept
practically as well as that made from cream of 0.15 per cent
acidity, while that from cream of 0.31 per cent acidity kept
nearly as well. That from cream of 0.36 per cent acidity
showed a materially lower score after storage, and that from

cream of 0.45 per cent acidity a still lower score.
STAETERS

.Starters were first used in 1776 when the Mcngclian
Ialmucks (16’ added a natural starter to sour milk intended
for churning: In 1887 a description of the method of using
"lands wei" as a starter for Edam cheese was published in a
pamphlet by Boekel (17). This starter was th ought to exert
a favorable effect on cheese defects and especially to pre-
vent swelling or bloating. Before the development of arti-
fical cultures buttermilk from.a churning of good butter was
apparently extensively used for starting the acid fermentation
in cream intended for buttermaking.

The definition of a starter as given by Hunziker
follows (18): "As used in the manufacture of butter by a

starter is meant a mixed culture in milk or skim milk of lactic

acid bacteria and associated species capable of develOping
in milk, cream, and butter the flavor and aroma character-
istic of good butter."

The use of pure cultures for the purpose of ripening
cream was the result of work done by Storch (17). He
studied organisms from sources such as buttermilg butter,
and ripened cream, and found that different acid pnducing
forms induced very different flavors and aromas. Butter
made from pasteurized cream with pure culture had a very
normal, clean, mild acid flavors.

The first commercial starter cultures were made about
1890 (17). Conn, (19) answering an inquiry, stated that the
question as to whether lactic acid bacteria themselves produce
the aroma of butter or whether in addition other bacteria are
important was not settled, but he pointed out that the so-
called pure cultures are not all alike and that while most are
pure cultures, some are mixtures of different organisms and
that one culture contained no less than ten or twelve different
species mixed together.

Hammer (20) found in a number of starters, of very sat--
isfactory quality and from different sources, that more than
one organism was present. Two organisms were isolated from
starter which in combination gave a volatile acidity, approxi-
mately, the volatile acidity secured from the starter, although
each of these organisms alone gave a volatile acidity con-

siderably below the volatile acidity produced by the starters.

Hammer's work (17) showed that organisms in addition

to Streptococcus lacticus are necessary in a good starter.

The importance of these forms is evident from their ability

to produce a satisfactory starter when either one or a mixture
of the two are grown in combination with Streptococcus lacticus.
The names of these organisms, as prOposed by Hammer, are
Streptococcus citrovorus and Streptococcus paracitrovorus.

The productian of a desirable starter seems to require the
action of Streptococcus lacticus and one of the associated
organisms.-

The variation between starters and pure cultures of
Streptococcus lacticus, in the per cent total acidity that is
volatile at various times during the ripening period, offers
another method of proving that starters are not pure cultures
of Streptococcus lacticus (17). It is thought that the failure
to maintain such a balance in practice is undoubtedly one of

the reasons why unsatisfactory results are so frequently secured.
SUMMKIY'OF REVIEW OF LITERATURE

Cream ripened to a high degree of acidity is no longer
tolerated by manufacturers of quality butter. Results from
investigations show that butter made from unripened, pasteurized,
sweet cream will maintain its quality during storage to a high
degree, while butter from ripened, pasteurized cream usually

deteriorates materially.

As to flavor, investigators find that for the first
two or three months ripened cream butter is preferred to
sweet cream butter, but the longer the butter was kept, the

less marked becomes the difference.

OBJECT OF THE EXPERIMENT

The object of this experiment was primarily to
determine:
1. The effect on the keeping quality of butter when
starter has been added to sweet cream butter at the time
of working.
2. The effect on the keeping quality of butter when
starter has been added to sweet cream Just before churning.
3. The effect on the keeping quality of butter when
sweet cream has been ripened to 0.3 per cent acidity.
4. The effect on the keeping quality of butter when

sweet cream has been ripened to 0.5 per cent acidity.

5. The effect of acidity on the composition of the
butterfat.
6. The effect of acidity on the nitrogen-cue substance

in the resulting butter.

10

PLAN OF EXPERIMENTAL WORK

Preparation of'Starter

Mother Culture._ To find which organism was best suited

 

for use in this work a number of different cultures were ob-
tained. These were propagated for about two months. At the
end of this period it was decided that the culture furnished
by Professor Hammer of the Iowa State College was best suited
for the experiment.

Clean quart bottles were filled two-thirds full of
skim milk, heated to 190° F. and held for one hour at that
temperature. The bottles were then cooled to 70° F. At
about 4:30 P. M. the cultures were examined and the best was
transferred to the bottles of skim milk by means of spoons
which had previously been boiled in water for an hour. Enough
of the culture was used so that the milk would be curdled the
next morning. The cultures were allowed to ripen over night
at a temperature of 720 F. .As soon as the cultures were curdled
they were placed in a refrigerator, the temperature of which was
40° F., and were held at that temperature until time for trans-
ferring the cultures in the afternoon.

The skim milk to be used for starter for the problem
was heated in a glass lined starter can to a temperature of
190° 1. and held for an hour at that temperature. It was then
cooled to 72° F. and inoculated with one per cent of the mother
culture. As soon as the skim.milk was curdled and the curd

sufficiently formed it was stirred and then cooled with water.

11
Preparation of Cream for Churning

As soon as the cream was received it was weighed and
mixed in a 200 gallon Wizard vat. A,test was made to deter-
mine the degree acidity of the cream. A vat test was also
made on the cream to determine the butterfat content. It was
then pasteurized by heating to a temperature of 145° F. and
held for 30 minutes. degular observations of the thermometer
were made so as to keep the temperature as constant as possible.
The cream was cooled by water until it reached a temperature
of 60° r. and ice was used to cool the cream to 40° F. at
which temperature it was held over night.

The following morning the vat of cream was agitated
so that the cream was thoroughly mixed, after which it was
divided into five lots, each containing 256 pounds of 40 per
cent cream. The method of treating each was as follows:

Dot 1. This creamtnas churned sweet, and a sample of
butter saved from it to be used as a check.

Dot 2. This cream was churned sweet and starter was
added to the butter before working at the rate of three per
cent of the weight of the butterfat. The starter was mixed
with the salt. The salt was then added to the butter and the
working process continued.

Dot 3. Starter at the rate of three per cent of the
weight of the cream was added to the sweet cream just before
churning.

Dot 4. The sweet cream was warmed to 70° F. in the vat

12

and starter added at the rate of twenty per cent of the
weight of the cream. The cream was ripened to an acidity
ranging from 0.3 to 0.35 per cent and then cooled to churning
temperature and held for at least two hours.

Dot 5. The sweet cream was warmed to 700 Fa.in the
vat and starter was added at the rate of twenty per cent of
the weight of the cream. The cream was ripened to an acidity
ranging from 0.45 to 0.52 per cent. It was then cooled to

churning temperature and held for at least two hours.
The Churning Process

A.8implex churn of 125 pounds capacity was used. The
churning temperature was reguhsted so that it would require
from 50 to 60 minutes for churning. The temperature ranged
from 46° F. to 56° F. The butterfat content of Lots land 2
was 40 per cent; Lot 3, 38 per cent and Lots 4 and 5, 33 per
cent. The churn was stopped when the butter granules varied
from the size of wheat to corn kernels. The buttermilk was
then drawn off and the butter allowed to drain thoroughly.
The wash water was sprayed over the butter using as much
water as there was buttermilk. The temperature of the water
varied from two to three degrees below that of the buttermilk.
The butter was washed twice in all churnings.

The amount of salt added to the butter was four per
cent of the weight of the butterfat. The wet salting method

was used, the salt being sprinkled over the butter. The

13

butter was worked until it had a compact body and a tough,
waxy texture. Axmoisture test was then made and the butter
worked so as to have, as near as possible, a 15.95 per cent
moisture content, care being taken not to injure the body of

the butter.
Preparation and Care of Samples

When the working process was completed, five one pound
samples of each churning were taken and placed in pint Seal-
right containers. In taking the samples care was exercised
to obtain as uniform a sample of the butter as possible. The
samples were marked for identification and were dated. The
samples were placed in cold storage at a temperature averaging

0° F. during a twenty-four hour period.
Judging the Butter

The butter was scored by Professor P. 3. Lucas and the
writer. The hatter was scored after a storage period of one
day, one month, three months, and will be scored again at the
end of a six months storage period.

The score was made of flavor only, 45 points being
allowed as a perfect score. The other points in the score
card were allowed as perfect, hence in the tables, scores are

given completely.
Chemical Analysis

In addition to scoring the butter a number of chemical

14

tests were made to determine if there is a relationship
between these tests and the keeping quality of the butter.
The following analyses were made: amino-nitrogen content,
total nitrogen, acid number, iodine number, Reichert Meissl
number, and the Kries test.

The amino nitrogen content of butter was run to
determine the change, if any, in the nitrogenvous substance
of the butter after a storage period of three months. The
amino nitrogen content of butter is eXpressed as the per cent
of the total nitrogen.

In order to express the amino nitrogen in per cent of
the total nitrogen, the total nitrogen content of the butter
was also determined.

The acid number, iodine number,.Reichert Meissl number,
and the Kries test were run on the butterfat after a storage
period of three months. This was done to determine whether
or not the numbers had changed any from those determine when
the butterfat was fresh.

The acid number is the number of cc. of .l N. Na.OI
required to neutralize the acids in 100 grams of butterfat.
The iodine number is the per cent iodine absorbed by the
butterfat. The Reichert Meissl number is the number of co.
of’lfl. NaOH required to neutralize the soluble volatile acids
in 5 grams of butterfat.

The Kries test is a measure of the oxidative rancidity
in fats. Because this test is only qualitative, the results
of this test are determined by the intensity of the color
which is obtained.

15
Allof the following tests were run in duplicate.

Analysis on Cream

As soon as the cream was received the Babcock test
for determining the butterfat content of the cream was made.
it the same time a Mann's acidity test was made of the cream.

“I

Analysis on.Buttermilk

n.3abcock test was made of the buttermilk to determine
the butterfat content. Skimmilk bottles were used, and when

the butterfat content was too high, milk bottles were used.
Analysis of Butter

Preparation of sample. The same of butter was com-
pletely melted by placing the closed jar in water at 100° to
1100 F. It was then removed from the warm water and stirred

until the butter solidified.
Determination of Moisture, Butterfat, Salt and Curd

The butter was analyzed for moisture, butterfat, salt
and curd by the gasoline extraction method (21), which is a
slight modification of the Kohman method (22).

Determination of Amino Nitrogen

For the determination of the amino nitrogen in the
butter the procedure suggested by Ferris (23) for the prepara-

tion of the sample was followed. ‘A 50 gram sample was weighed

16

in a 250 cc. glass stoppered bottle while the sample was of
such consistency that it could be poured and yet not have

any separation of the fat and curd. The bottle was next
filled to the shoulder with petroleum ether. The fat was
dissolved by shaking vigorously and the curd allowed to

settle in a compact mass at the bottom by allowing it to stand
for twenty-four hours. The other layer containing the fat

was siphoned off. To the residue was added 2.5 cc. of ten

per cent acetic acid, 15 cc. of a saturated solution of picric
acid, and enough distilled water to make a volume of 50 cc.
The mixture was then filtered and the amino nitrogen determined

by the use of the Van Slyke micro apparatus.
Determination of Total Nitrogen

The method followed in determination of total nitrogen
was the Gunning method as given in Methods of Analysis (24)
with the modification suggested by Scales and Harrison (25)
for the absorption of the ammonia evolved. This involved the
use of four per cent boric acid solution for the absorption
of the ammonia and the use of brom-phenol as an indicator
when titrating with standard sulphuric acid. The sample used
was a portion that one prepared for the amino nitrogen

determination.

.Analysis of Butterfat

Preparation of sample. About one-half pound of butter

was placed in a beaker and kept in water at a temperature

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17

not higher than 1100 F. When the butter was melted, the
layer of melted fat was filtered through a dry filter paper
held in a hot water funnel at a temperature not higher than

100° F.
Determination of Reichert heissl Number

The Leffman and Beam method was used, as given in

Methods of Analysis (24).
Determination of Iodine Number

The Hanus method was used as given in Methods of
Analysis (24). The sodium thiosulfatc solution was standard-
ized against potassium bromate, potassium dichromate, and

electrolytic c0pper.
Determination of Acid.Number

About a ten gram sample of the melted fat was
accurately weighed. Fifty cubic centimeters of a mixture of
equal parts of neutral alcohol and benzene was then added. The
mixture was next titrated with standard sodium hydroxide using
phenolphthalein indicator. The number was calculated so as to
be expressed as a number of cc. of .l N. NaOH in 100 grams of
butterfat. Benzene was used with the alcohol because Steele
and Sward (26) found that this combination was preferable to
alcohol alone in that the end point of the titration was much

sharper.

18

Test for Oxidized Fat (Kriee Test) (27 a 28)

Ten centimeters was measured into a test tube and
ten centimeters of concentrated hydrochloric acid was
added and the mixture shaken for thirty seconds. Ten cubic
centimeters of a freshly prepared one per cent ether solu-
tion of phloroglucinol was added and the mixture shaken as
before. The mixture was allowed to stand. .A recognizable
red or pink shade in the acid lever was regarded as a
positive test and a faint orange or yellow color was re-

garded as a negative test.

19

REJULTS AKD DIJCUJJION
Curd Content

Casein, albumin, ash and lactose are commonly,
though incorrectly called "curd" by the buttermaker (21).

The curd content of butter is determined and ex-
pressed in one or the other of two entirely different ways,
which yield results in per cent curd, that differ from one
another. One method is to determine the nitrogen content
of butter, and by multiplying the analysis by the factor 6.38,
the result is taken as per cent protein. This represents the
true curd content. The other method is to determine the per
cent curd by difference, that is by deducting the sum of the
per cent of fat, moisture, and salt from 100. In this case
the per cent curd so obtained embraces, aside from the pro-
tein, also the traces of ash, acid, and lactose contained in
butter. This is termed physiological curd (38).

The results in Table I are expressed as physiological
curd. The average results show a range from 0.96 to 1.09 per
cent curd in the different lots of butter. The sweet cream
butter had the lowest average curd content while the butter
made from sweet cream to which a starter was added to the
butter at the time of working had the highest curd content.
The average curd content of the different lots showed only a
slight difference. The range is so small that no fear need be
held that any method discussed herein will affect the curd con-

tent of the resulting butter.

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21
Amino Nitrogen Determination

The Van Slyke method for the determination of amino
nitrogen depends on the fact that nitrous acid reacts with
free amino groups liberating nitrogen gas which is measured
in a special burette. This method determines the amino ni-
trogen and also some of the free ammonia. It is found that
the amount of nitrogen displaced from a protein by nitrous
acid is a very small fraction of the total nitrogen but that
as hydrolysis proceeds and the amino groups become free, the
amount steadily increases.

The most common linkage by which amino acids are held
together in the protein molecule is that involving their
amino and carboxyl group and is called the peptid linkage.
During the hydrolysis of a protein decomposition product,
this linkage splits, giving rise to a carboxyl group and an
amino group.

Ferris (23) found that the amino nitrogen content of
sweet cream butter was 1.4 per cent of the total nitrogen
while buttermade from neutralized sour cream had a content
of 3.3 per cent of the total nitrogen.

The average results of the amino nitrogen determination
showed a slight increase with the exception of lot 4, but the
increase in any case is too small to show any significance.
The average results in terms of ascending values of the amino

nitrogen and ammonia determination are lots 1, 2, 3, 5 and 4.

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23
Nitrogen Determination

Nitrogen in butter is found in the non-fatty
portion and also in the portion of the butter that contains
the lecithin. The lecithin content is very small and,
therefore, contains only a very small amount of nitrogen.
The larger portion of the nitrogen is found in the non-fatty
portion of the butter. .

Richmond (31) found that the average nitrogen content
of sweet cream butter was 0.1000 per cent while that of
ripened cream butter was 0.1320 per cent. The results of
nitrogen determination are given in Table III. The average
of each lot for the nitrogen content are shown in Figure I.
The average results of each lot showed that sweet cream
butter has a lower nitrogen content than that of ripened
cream butter. The results also show that the nitrogen con-
tent of the butter is slightly higher after a storage

period of three months.

24.

 

 

 

 

 

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DEPARTMENT OF MATHEMATICS

Reichert Meissl Number

Since the method used in securing the Reichert
Mbissl Number is only an arbitrary one, it is essential
to adhere strictly to the conditions of Operation as laid
down, it comparative results are to be obtained, and, by
so doing, over 80 per cent of the soluble volatile acids
in butter can be secured in the distillate. I

Jensen (32) states that the Reichert Meissl process
yields with butterfat 85 to 88 per cent of the total butyric,
24 to 25 per cent of the caprylic, and 85 to 100 per cent
of the capric acids. The amoint of soluble volatile acid
is likely to increase with the age of the sample (32).

Butyric, valeric, caproic, and capric acids are the
only acids present in fats that can be distilled without
decomposition under ordinary pressure. These acids have
comparatively high boiling points, but owing to their vapor
pressure they can be readily distilled from aqueous solutions
with steam and are termed "Volatile" acids (32).

The quantity of soluble volatile acids is influenced
to a notable extent by the seasons of the year, the nature
of the feed, the period of lactation and the idiosyncrasy
of the cow (33).

The results of the Reichert Meissl determination are
égiven in Table IV. All of the results fall within the
(ordinary values obtained by other workers. The minimum and

Inaximum range of the Reichert Meissl Number given in

27

Fundamentals of Dairy science (34) are 23 and 36 respectively.
All of the samples showed a slight decrease in soluble volatile
acids at the end of a three months storage period.

Figure II shows the average number for each lot at the
end of a one day storage period and also at the end of a three
months storage period. The.average of each lot gave a lower
number at the end of a three months storage period than for a
one day storage period. This is the reverse of what was ex-
pected since it has been found generally that the soluble
volatile acids increased with the age of the samples.

However the differences are so slight that they may
be due to esperimental error. It is nevertheless interesting
to note the slightly lower values in each case after a

storage period of three months.

28

 

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8.8 8.8 88.8 8.8 8.8 88.8 88.8 88.8 88.8 88.8 .8
8.8 88.8 88.8 8.8 8.8 8.8 8.8 8.8 8.8 8.8 .8
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88.88 88.88 88.88 88.88 88.88 88.88 88.88 88.88 . 88.88 88.88 .88
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DEPARTM ENT OF MATHEMATICS

30

Iodine Number (Hanus)

The amount of unsaturated fatty acids in a butterfat
is greatly influenced by the kind of oil or fat given to the
cow with the food (53). Heineman (35) found that the iodine
number was irregular in the beginning, then increased gradually
to within two or three months of the end of lactation, with
a rather sharp rise during the last few weeks. The coincident
increase of the melting point is probably due, as Eckles and
Shaw (35) suggest, to a decrease in volatile acid such as
butyrio which has a melting point below that of oleic acid.

The unsaturated acids and their glycerids assimilate
halogens with the formation of saturated compounds, and tLis'
property serves as a basis:br their quantitative determination.
The structure of unsaturated acids, particularly the position
of the double bond in relation to the carboxyl group, influences
the iodine absorption. If the double bond is located at a
considerable distance from the carboxyl the results are
generally normal but when relatively close together, the iodine
number is likely to be below theory, although lengthening the
absorption period increases the results (32).

The minimum and maximum iodine number, as given in the
“Fundamentals of Dairy écience" (34), are 26 and 38 respectively.
The results of the iodine number are given in Table V.

The iodine numbers for the first five series are very
abnormal. Precautions, such as using acetic acids which

showed no reduction with dichromate, were used. The sodium

31

thiosulfate solution was standardized by three different
methods. The samples of butterfat were weighed into clean,
dry, iodine flasks. The reason for the abnormal numbers for
the first five series is unknown. The possibility of its
being due to feed could not be determined because the

source of the cream was unknown.

All of the samples showed a slight increase at the
end of a three months storage period. Figure III shows the
average iodine number for each lot at the end of a storage
period of one day and also after a storage of three months.
The average of each lot gave a higher number at the end of

a three months storage period.

52

 

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DEFARTM ENT OF MATHEMATICS

Acid Number

The acid number of oils and fats varies with the
purity, age, amount of hydrolysis, and oxidation they have
undergone, Contact with fermenting or decaying matter,
such as animal tissue, casein of butter and the mare of
fruits, tends to rapidly increase the amounts of free acids
due to fat splitting enzymes. Acidity in fats is not always
a measure of rancidity, as hydrolysis may result from the
action of enzymes in the presence of moisture without
accompanying oxidation, which appears necessary fro the
production of strong smelling, acrid tasting bodies that
usually characterize rancid products (32). However, in the
case of butterfat the development of free acids has fre-
quently been termed rancidity; hydrolytic rancidity accord-
ing to the terminology used by Palmer (36).

The limit of error in the determination of the acid
number as given by Holland (32) of the Massachusetts Ex-
periment dtation is 0.10 milligram. The acid number of
butterfatqgiven by Palmer (36) is 0.56 milligrams of
potassium hydroxide per gram of fat, or eXpreSSed in cubic
centimeters of 0.1H sodium hydroxide per 100 gram of butter-
fat, it is about 10.

The results of the acid number determination are
given in Table VI. The acid number for lots 1, 2 and 3
showed very little difference during a storage period of

three months. Figure IV shows the average acid numbers for

35

each lot at the end of a one day and also a three months
cold storage period. The average of lots 1, 2 and 3 showed
a slight decrease after a cold storage period of three
.months. The acid numbers for lots 4 and 6 are very much
higher than for the first three lots. Lot 6 is higher also
than let 4.

The lines on the graph of the acid numbers would lead
to the belief that a relationship exists between the acidity
of the cream and the acid number of the butterfat. The
correlation between the acidity of the cream and the acid
number was 0.428't 0.067. In this case the correlation has
a value of 6.4 times the probable error. The relationship
between the two factors is slightly significant so that the
conclusion may be drawn that there is some relationship be-
tween the acidity of the cream and the acid number of the
butterfat. It may be concluded from the results of these
numbers that an increase in the acidity of the cream causes
a slight tendency towards a higher acid number for the butter-
fat.

36

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DEPARTMENT OF MATHEMATICS

38

Text for Oxidized Fat (Kries Test)

The intensity of the Kries test of samples of an
oxidized fat is proportional to the amount of oxygen it
has abosorbed, or, the amounts ofht necessary for equiva-
lent color intensities are inversely preportional to the
volume of oxygen absorbed (27).

The intensity of the Kries test is not preportional
to the oxidative rancidity or tallowiness of a fat. A ran-
cid fat will give a Kries test but many fats that have ab-
sorbed large quantities of oxygen show only faint traces of
rancidity,or none, yet give intense Kries tests.‘ Some
evidence is;found to indicate that oleic acid when autoxidized,
may be the only unsaturated acid in fats that gives the Kries
test (28).

Powick (8) found that the constituent of rancid fats
responsible for the Kries test,is probably a derivative of 61p-
hydrin aldehyde. It is certain that this constituent gives
rise to epihydrin alehyde when the rancid fat containing it‘
is brought into contact with the concentrated hydrochloric
acid used in the Kries test.

A.positive reaction in the Kries test, when the test
is performed in the usual manner, is not always a reliable
indication of rancidity in fats. ‘A large number of compounds
react with phloroglucin hydrochloric acid to give a red color,
that with the unaided eye cannot be distinguished from the
toolor obtained with rancid fats. When the test is modified

:in such manner that the color obtained is examined spectro-

39

loopioally, however, the modified test becomes a reliable
index or the rancid condition (37).

The results of the Kries test are given in Table
VII. {As this test is a qualitative test only, a comparison
between the five lots of eachsieries could be made. .All
of the tests were very slight. It is interesting to note,
however, that from the results of the qualitative test, the
lot scoring the highest showed no increase in the average I
value or the Kries test, while the lot that scored the lowest

showed the greatest increase in the average value.

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43
DISCUSSION of SCORES
Sweet Cream Butter

The average score for the sweet cream.butter was
the lowest of any of the lots of butter after a storage
period of one day. The butter when scored was criticised
as having no distinct flavor.

Liter a storage period of one month the sweet cream
butter was placed in fourth place. The sweet cream butter
scored a little lower than that of butter made from ripened
cream which had been ripened is an acidity of about 0.3
per cent but scored higher than.butter made from cream which
had been ripened to an acidity of about 0.5 per cent.

After a storage period of three msnths the sweet
cream butter scored higher than either of the two different
lots of ripened cream butter. The average score of the sweet
cream butter at the end of a one day storage period was 92.13;
at the end of one month 91.29; and after a period of three
months 90.66. The sweet cream butter had better keeping
quality than that of the ripened cream butter.

Butter Made rrom.Sweet Cream.To Which A
Starter Was Added-are The Butter At The
Time or Working
.Atter a storage period of one day the average score
of the butter to which starter was added at the time of
working was third highest. tartar a storage period of one

month and three months the starter butter scored second

44

highest of the different lots. The average sco re after
a storage period of one day was 93.04; at the end of one
month 92.42; and after a period of three months 92.04.
The flavor of this butter (lot 2) was not as well
develOped as that of butter to which a starter was added
Just before churning. The keeping quality of the above

two lots of butter were the same.

Butter made From Sweet Cream To Which
A Starter Was Added Just Before Churning

Butter made from sweet cream to which a starter was
added Just before churning scored as high after a storage
period of one day as butter made from sweet cream which had
been ripened to 0.3 per cent acidity.

When.the starter butter was scored after a storage
period of one month, it was given the highest score. The
flavor of the starter butter was well developed.

.After a storage period of three months the butter was
scored again. This time it received the highest score of
any of the other lots. When the starter butter was fresh
the average score was 93.58; after a storage period of one
month 92.96; and at the end of three months 92.54.

ffls butter besides having the best flavor also showed
very good keeping quality. The starter butter after a
storage period of three months lost only 1.04 in points
while the butter made from ripened cream lost 4.58 points.

.. flail}. . inu|i

45

Eur a creamsry using sweet cream in making butter,
these results would indicate that it is best to add starter
to the cream Just before churning. Using this method, the
flavor of the butter would score the highest when fresh or

after a storage period of three months.

Butter'nade Prom Sweet Cream Which.Was
Ripened To.An Acidity Of 0.3 éer Gent

fhe butter made from cream ripened to 0.3 per cent
acidity received the highest average score of any of the
other lots of butter when fresh. The difference between the
ripened cream butter and the butter to which a starter was
added Just before churning was very slight.

'.After a storage period of one month the ripened cream
butter again scored higher than the sweet cream nutter but
lower than the starter butter. After a storage period of
three months the ripened cream butter scored lower than that
of sweet cream butter. The average score Eafter a storage
period of one day was 95.66; at the end of one month 91.46;
and after a period of three months 89.08.

If the butter is to be consumed soon after it is made,
the cream can be ripened to an acidity of 0.3 per cent but
from these results the butter should not be held any length

of time.

Butter Hide Prom.3weet Cream which Was
Ripened so in Acidity or 0.5 Per Cent

‘-

The butter made from cream ripened to 0.5 per cent

46

acidity higher than that of sweet cream butter when the
butter was fresh. “fter a storage period of one month the
ripened cream butter scored the lowest of any of the lots.
When the butter was scored the flavor was criticised as
being slightly off and in some cases slightly unclean.

When the butter was scored after a storage period of
three months it again was scored the lowest. This time the
butter was criticised at the time of scoring as being
slightly fishy.

Summary of desults on Flavor

When fresh the untreated sweet cream butter (lot 1)
scored the lowest. Butter made from.sweet cream to which a
starter was added to the butter at the time of working (lot
2) scored higher than butter made from sweet cream which had
been ripened to an acidity of 0.5 per cent (lot 5). Lot 2
scored lower than butter made from sweet cream to which a
starter was added Just before churning (lot 3) or butter made
from sweet cream which had been ripened to an acidity of 0.5
per cent (lot 4). Lots 3 and 4 scored the highest. The
flavor of lots 3 and 4 as shown by the average score. showed
very little difference. This slight difference could be
accounted for as being due to eXperimental error. Lot 5
scored higher than lot 1 but lower than lot 2.

.After a storage period of one month lot 1 scored

slightly lower than lot 4 but higher than lot 5. The average

illi'i.l rail.

 

, u

 

 

 

47

score of lot 2 was lower than lot 3 buthigher than lot 4.

Lot 3 scored the highest. Lot 4 scored slightly higher than
lot 1 but this slight difference could be due to eXperimental
error. Let 5 scored the lowest.

.After a storage period of three months lot 1 scored
lower than let 2 but higher than lot 4. Lot 2 scored lower
than lot 3 but higher than lot 1. Lot 3 again scored the
highest. The average score of lot 4 was lower than lot 1
but higher than lot 5. Lot 5 scored the lowest.

Summary of fiesults on Keeping Quality

At the end of a storage period of one month, the
difference between the average score of one day and one month
for the untreated sweet_cream butter (lot 1) was 0.84.

Butter made from.sweet cream to which a starter was added to

the butter at the time of working (lot 2) and butter made from
sweet cream to which a starter was added Just before churning
(lot 5) showed the best keeping quality. In both lots the
difference was 0.61. The difference for butter made from

sweet cream which had been ripened to an acidity of 0.3 per cent
(lot 4) was 2.20, and for butter made from sweet cream which
had been ripened to an acidity of 0.5 per cent (lot 5) was 1.71.

After a storage period of three months lot 2 and lot 3
again showed the best keeping quality. The difference between
the average score of one day and three months for lot 1 was

1.47; lot~2, 1.00; lot 3, 1.04; lot 4, 4.53 and lot 5, 4.09.

4e

CONCLUSIONS

1. The flavor of butter made from sweet cream to
which a starter was added Just before churning is superior
to that of sweet crram butter after a storage period of one
day, one month, and three months.

2. The flavor of butter made from sweet cream to
which a starter was added to the butter at the time of work-
ing is superior to that of sweet cream butter after a storage
period of one day, one month and three months.

3. The flavor of butter made from.sweet cream ripened
to an acidity ranging from 0.3 to 0.35 per cent is superior
to that of sweet cream butter after a storage period of one
day. “fter a storage period of one month there is no difference
in flavor of the two butters. The flavor of sweet cream butter
is superior to the ripened cream butter after a storage period
of three months.

4. There is no difference in flavor between sweet
cream butter and butter made from sweet cream which has been
ripened to an acidity ranging from 0.45 to 0.52 per cent after
a storage period of one day. The sweet cream butter is
superior in flavor to that of ripened cream.butter after a
storage of one and three months.

5. The flavor of butter made from sweet cream to which
a starter was added Just before churning is superior to sweet

cream butter to which a starter was added to the butter at the

49

time of working, after a storage period of one day, one
month, and three months.

6. The keeping quality of sweet cream butter to
which a starter was added to the butter at the time of
working is superior to that of sweet cream butter after a
storage period of one and three months.

7. The keeping quality of butter made from sweet
cream to which a starter was added Just before churning is
superior to that of sweet cream butter after a storage
period of one and three months.

8. The keeping quality of sweet cream butter is
superior to butter made from sweet cream ripened to an
acidity ranging from 0.3 to 0.35 per cent after a storage
period of one and three months.

9., The keeping quality of sweet cream butter is
superior to butter made from.sweet cream ripened to an
acidity from 0.45 to 0.52 per cent after a storage period
of one and three months.

10. The keeping quality of sweet cream.butter to
which a starter was added to the butter at the time of working
is the same as butter made from.sweet cream to which a starter
was added Just before churning after a storage period of one
and three months.

11. The acidity of cream does not effect the Reichert
Hkissl number. iodine number, amino-nitrogen content, or the

Kries test.

12. A.re1ationship exists between the acidity of the

If,

5O

cream and the acid number of the fat. The higher the
acidity is developed in cream, the higher the acid
number of the fat will be.

1e
2e
3e

4.

5.

6.

7.

8.

9.

51'
BIBLIOGRAPHY

Genesis 18:8 and Proverbs 30:33.
Judges 5:25

What is sweet cream butter?

New York Produce Review, Vol. 57, No. 4, (1923) page, 131.
Curtis, 9. w. ‘

Quality of sweet cream butter as compared with butter
made from acid cream.

Texas Agricultural Experiment Station, Bul. ll, Aug.,1890.
Patrick, G. E.

Keeping quality of sweet cream butter.

Iowa Experiment Station, Bul. 11, Nov., 1890.
Patrick, G. 3.

Sweet versus sour cream butter.

Iowa Experiment station, Bul. 18, 1892.
Patrick, G. E.

Sweet verSus sour cream butter.

Iowa Experiment 3tation, Bul. 21, 1895.

Powick, W. C. ”

Compounds developed in rancid fats, with observations
on the mechanism of their formation.

Jour. of Agr. Research, V01. 26, (1923), page 323.
Dean, R. H.

Sweet cream with cultures versus ripened cream.

Ontario College and Experiment Farm.

Thirtieth Annual Report 1904.

 

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10.

11.

12.

13.

14.

15.

16.

17.

52

Gray, 0. E.

The keeping qualities of butter made under different
conditions and stored at different temperatures.

U. S. D. A.; B. A, I. Bul. 84, 1916.

Charron,.A. T., and Shult, r. 1.

Sweet cream butter.

Sept. of Ag. Ottawa, Canada. Bill. 15, 1907.
Rogers, L..A., Thompson, S. 0., and Keithley, J. B.
The manufacture of butter for storage.

U. S. D. A.; B..A. T. Bul. 148, 1912.

Potts, Roy 0.

Suggestions for the manufacture and marketing of
creamery butter in the South.

U. S. D. A. Cir. 66, 1916.

Hortensen, 11.

Influence of acidity on flavor and keeping quality
of butter.

Iowa Exp. dta.‘Bul. 207, 1922.

White, M.‘

Effect of acidity content on keeping quality of butter.
The Creamery Journal. Vol. 38, No. 23 (1928), page 5.
Heineman, P. 6.

Milk. (1921) page 21

Hammer, 3. W.

Volatile acid production of Streptococcus lacticus
and the organisms associated with it in starter.

Iowa sxp. Sta. deeearoh Bul. 63, 1920.

 

\_\

 

18.

19.

20c

21c

22.

23.

34c

25.

53

Hunsiker, 0. F.

The Butter Industry.

Second Edition (1927), page 248.

Conn. H. W.

Bacteriology in buttermaking.

Storrs Agr. Exp. Sta. An. Rep., Vol. 11 (1898) page 85.
Hammer, B. W. and Bailey, De E.

The volatile acid production of starters and of organisms
isolated from them.

Iowa.Exp. Sta. desearch Bul. 55, 1919.

Gregory, E. w; tucas, 2.8.; and Spitzer, Geo.

.A comparison of methods of estimating fat in butter.
Purdue Agr. Exp. Sta. Bulletin 244, 1920.

Kohman, 5. F.

A rapid and accurate method for butter analysis suitable
for factory control work.

J. of Ind. and Eng. Chem. Vol. 11 (1919) page 36.
Terrie, I.W.

Some determinations on the soluble nitrogen compounds
of cream and butter.

J. of Dairy Sci. Vol. 5 (1923). page 323.

.lethod.of Analysis of the Association of Official
Agricultural Chemists.

Second Edition (1925), pages 260 to 293.

Scales, P. n; and Harrison, A. P.

Boric acid modification of the KJeldahl method for
crop and soil analysis.

J. of_Ind. and Eng. Chem. Vol. 12 (1920), page 350.

26.

27c

28.

29.

50 e

31.

32.

33.

34.

54

Steele, L. L. and Sward, 8.0.

The determination 5f the acid number.

J. of Ind. and Eng. Chem. Vol. 14, (l922),page 67.
Helm, G. B. and Greenbank, G. R.

Test for oxidized fat.

J. of Ind. and Eng. Chem. Vol. 15, (1924), page 1051.
Holm. 0. E. and Greenbank. G. R.

Test for oxidised fat.

J. of Ind. and Eng. Chem. Vol. 16, (1924). page 518.
Hathews, A. P.

Physiological Chemistry.

Second Edition(1920), pages 123 to 137.

ierris, I. w. '

A method for the determinatiwi of amino nitrogen
and ammonia in cream and butter.

J. of Dairy 301., Vol. 5, (1922), page 403.
Richmond, H. D. '

Dairy Chemistry.

Third Editinn (1920), page 336.

Holland, E. 3.; Road, 3.0. and Buckely, J. B.
Improved methods for fat analysis.

Hess. Agr. Exp. Sta. Bul. 166, page 1915.
Dewkowitsch, Dr. J.

Chemical Technology and Analysis of Oils. Fats

and "axes. ‘

rourth.Edition,(1909t pages 667 to 694.

Fundamentals of Dairy Science.

American Chemical society Monograph (1928). page 80.

55

35. Heineman, P. Q.

Milk (1921). page 121.
35. Palmer, L. S.

Laboratory EXperiments in Dairy Chemistry. (1926), page 25.
38. Hunziker, 0. F.

The Butter Industry.

First Edition (1920) page 546.

APPENDIX

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£33m no 232.8 28 as. .38 $55.33 .3“ gm

.HH Handy

64

 

 

 

 

 

8... 38 8.3 8.8 ... 8.3 8.3 88 8.3 8.8 m 83
8... 88 8.3 8.8 e 83 3.3 88 8.3 8.8 e 83
8. 88 8.3 .8.8 n as 8. 88 8.3 8.8 n «3
8. 88 8.3 8.8 8 9.3 8.3 88 8.3 8.8 8 83
. 8. 88 8.3 8.8 3 83 8.3 88 8.3 8.8 3 «3
3x .388 u 838
3.3 88 8.3 8.8 a «.3 8. 88 8.3 8.8 n «3
8. 88 8.3 3.8 a. 93 8.3 88 8.3 8.8 e 83
8.3 88 8.3 8.8 n ...3 8.3 88 8.3 8.8 n ..3
8. 88 8.3 8.8 8 £3 3.3 88 8.3 8.8 8 £3
8. 38 8.3 8.8 3 «3 8. 88 8.3 8.8 3 a8
- HM ammuom , MM oomuom

W50 Mom moo HR uufloo ”WNW £00 himdfll ”GOO HON .900 MON 80
832 g

......“me wadm 0.3938» mum} 9338 E wdom Egan «WW 5%

 

3.283 .833 8 8388 88 an» .38 .2333. 83 8338 .3 38.3.

 

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