Food Science and Technology Department

Faculty Publications in Food Science and Technology

Fat Separation in Evaporated Milk I. Homogenization, Separation, and Viscosity Tests

H. H. Sommer
University of Nebraska - Lincoln

This paper is posted at DigitalCommons@University of Nebraska - Lincoln. http://digitalcommons.unl.edu/foodsciefacpub/47

Published in JOURNAL OF DAIRY SCIENCE 37 (1954), pp. 60-71.

I.

F A T S E P A R A T I O N IN E V A P O R A T E D M I L K H O M O G E N I Z A T I O N , S E P A R A T I O N , AND V I S C O S I T Y T E S T S 1
R . B . M A X C Y 2 AND H .

~. SOMMERa

Department of Dairy and Food Industries University of Wisconsin, Madison

The rising of fat in evaporated milk on prolonged storage will inevitably occur since the density of the fat particles is lower than that of the concentrated milk plasma in which they are suspended. I t has been shown that the velocity of rise of individual fat globules in milk plasma is in good agreement with the velocity as predicated by Stokes' law ( 5 ) . T r o y and Sharp ( 7 ) also found the velocity of rise of globule clusters in general agreement with this law. Their observations on clusters were less precise, however, because of inherent complications arising from the irregularities in the shapes of clusters and the occlusion of plasma within the clusters. Accordingly, it must be expected that the factors controlling fat separation in evaporated milk are: the size of the fat particles, the difference in density between the fat particles and their suspending medium, and the viscosity of the suspending medium. The size of the fat globules is obviously of first importance, since the velocity of rise is inversely proportional to the square of the globule radius. The importance of smallness is f u r t h e r accentuated t h r o u g h density considerations. The difference in density between the fat particles and the medium in which they are suspended does not lend itself to direct control in a product of defined composition such as evaporated milk. This factor may, nevertheless, be i m p o r t a n t to an understanding of differences in fat separation. Insofar as heavier components become associated with the surface of fat globules b y adsorption or coagulation, the density of the fat particles is increased. Through this effect the density of the fat particle can approach, equal, or even exceed that of the suspending medium, as smaller globule sizes are obtained, or as the amount of associated material is increased b y processing conditions. Smallness of globules is i m p o r t a n t in this connection because the ratio of area to volume varies in inverse proportion to the radius of the globules. The density of the suspending medium in evaporated milk is not positively fixed, even though the ratio of solids-not-fat to water is closely controlled. I n aqueous solution the density of the three main classes of components of solidsnot-fat ranges from about 1.35 for proteins to 1.63 for lactose and 2 to 3 for the Received for publication August 3, 1953. i Published with the permission of the Director of the Wisconsin Agricultural Experiment Station. Present address : Geo. J. Meyer Manufacturing Co., Milwaukee, Wisconsin. 3Deceased May 8, 1953. 6O

:PAT S E P A I ~ A T I O N I N E V A P O I ~ A T E D M I L K

61

milk salts. In normal milk the content of salts and lactose is relatively constant. On the other hand, the casein content is directly related to the quantity of butterfat. Since evaporated milk is standardized to a definite ratio of solids-not-fat to fat, the quantity of casein would be greater in evaporated milk made from milk with a high butterfat content than from milk with a low butterfat content. Thus, the evaporated milk with a high casein content would show a low density of the suspending medium. Even though this consideration has theoretical significance, it is not obvious how density should be considered for a nonhomogeneous medium comprising particles that are relatively large. In connection with the density factor, it is interesting to note that fat separation in unconcentrated, homogenized, sterilized milk is less troublesome than in evaporated milk, presumably because of the lower density of the suspending medium. This condition exists e ve n though the apparent viscosity is somewhat less than in evaporated milk. The viscosity factor in Stokes' law relates to the viscosity of the suspending medium. For ideal application, the medium should be homogeneous and should exhibit true viscous flow characteristics. Neither of these conditions obtains in the concentrated milk plasma of evaporated milk. In unheated skimmilk, however, fat globules rise in good agreement with S t o k e s ' law; this suspending medium is not perfectly homogeneous, containing casein particles up to 0.780 tL in diameter (4). As the fat globule size is decreased by homogenization, and as the protein particles are increased in size by coagulation to sizes that may exceed the size of the fat globules, the system becomes more difficult to interpret in relation to Stokes' law. The " v i s c o s i t y " of evaporated milk decreases rapidly on vigorous agitation and slowly during quiescent aging. " A g e t h i n n i n g " of evaporated milk is retarded significantly by cool storage temperatures (3). These facts indicate that the suspending medium in evaporated milk does not exhibit true viscous flow characteristics. Industry practices in seeking to minimize fat separation in evaporated milk have been: (a) efficient holnogenization, (b) attainment of maximum viscosity, just short of " gr a i ni ne s s , " (c) cool storage, and (cl) periodic inversion of the cans during storage. In connection with a study of fat separation in evaporated milk, the following tests were selected or developed, and evaluated.
METHODS

A. A Test to Rate the Effectiveness of Homogenization.

62

R. B. 1VfAXCY A N D I-I. I t . S O M M E R

t h r o u g h objective tests applied to the homogenized product, r a t h e r t h a n t h r o u g h specification of homogenizing conditions. Microscopic observation of the globule sizes in the homogenized p r o d u c t is the obvious and quick method of checking on the effectiveness of homogenization. This approach, however, lacks strict objectivity; its main use is in yielding a quick general impression ; it does not lend itself to the recording of an "effectiveness r a t i n g " for later consideration in relation to the various degrees of fat separation that occur in the stored products. A t t e m p t s to make this a p p r o a c h objective are laborious, entailing the observation of a n u m b e r of microscopic fields and complete globule counts by size g r o u p s ; even then the personal f a c t o r enters, and the final rating of the data is arbitrary. I t was for these reasons that the effectiveness of homogenization in the U.S.P.II.S. definition for homogenized milk was specified in terms of relative f~eedom from fat separation on 48-hour quiescent storage. The evaluation of homogenization by means of a centrifugally accelerated f a t separation test has received attention by several m a n u f a c t u r e r s of evaporated milk. I n addition, Snyder and Sommer (6) described a test of this type in which the diluted product was centrifuged in a Babcock milk test bottle and the cream layer was read in terms of the Babcock test scale. A difficulty of this test is that the cream layer frequently lacks distinctness, especially when the fat is lightly pigmented. I n the test described below, the fat separation is measured by f a t tests to determine the fat enrichment that has occurred in a selected u p p e r layer as a result of centrifuging. Procedure. I n this work 50 ml. of the homogenized milk at room t e m p e r a t u r e was measured into a 50-ml. centrifuge tube ( r o u n d bottom, u n g r a d u a t e d ) . F o r evaporated milk, the test was applied to the concentrated milk before sterilization, diluting it with an equal volume of water, and measuring 50 ml. of this diluted product into the centrifuge tube. The samples were centrifuged for 10 minutes at 1,500 r.p.m. ( I n t e r n a t i o n a l Centrifuge, Head No. 240, radius 8 in. to the bottom of the extended pocket). W i t h continuous, gentle suction applied through an assembly as illustrated in F i g u r e I, the surface of the centrifuged milk was scanned with the suction inlet barely (or intermittently) in contact with the surface. This was continued until 10 ml. had been collected, as measured in the g r a d u a t e d receiving tube. A f t e r thorough mixing of the 10-ml. sample its fat content was determined. ~ F r o m the known percentage fat content of the uncentrifuged sample (A) and the f o u n d percentage fat content of the 10-ml. sample (B) the per cent enrichment was computed as follows: P e r cent enrichment ~ (B - - A) X 100 A

4In the present study the fat content was determined by the Babcock test, applied to an 8.8-ml. sample in an 8% Babcock test bottle. No water was added to compensate for the reduced volume of the bottle charge before adding the sulfuric acid. Ten ml. of sulfuric acid was used, added in three separate portions with vigorous agitation for 2 minutes after each addition. The 8.8-ml. sample was considered to be a "half sample," and the Babcock reading was multiplied by 2.

F A T SEPAI%ATION I N E V A P O R A T E D M I L K

63

~'" 5Oral. IOml.

CENTRIFUGE TUBE

FIG. 1. Assembly for removing the upper 10 ml. for determining the effectiveness of

homogenization. The per cent enrichment m i g h t be considered as an effectiveness r a t i n g t h a t parallels the tendency for separation and is inversely related to the size of the f a t particles. The effectiveness r a t i n g m a y r a n g e f r o m 0 for p e r f e c t l y homogenized milk to a p p r o x i m a t e l y 400 for unhonlogenized milk containing 4.0% fat.

B. Gravity Fat Separation Test I f the centrifugal test, as just described, is to measure differences in the effectiveness of homogenization, it must be applied before the other factors t h a t affect f a t separation have been altered b y additional processing. I n e v a p o r a t e d milk the centrifugal test should be applied before sterilization of the product. On the other hand, a n y f a t separation test applied a f t e r sterilization will reflect not only the effectiveness of homogenization but also the consequences of protein coagulation and increases in viscosity. The inclusion of these additional factors, however, is precisely what is desired in a test to determine how effectively f a t separation d u r i n g storage of the p r o d u c t has been precluded. An accelerated test for the latter purpose should recognize t h a t " a g e - t h i n n i n g " of e v a p o r a t e d milk d u r i n g storage is p a r t of the f a t s e p a r a t i o n problem. F o r this reason the test t h a t was adopted to measure f a t separation tendencies included the acceleration of " a g e - t h i n n i n g " t h r o u g h an elevated t e m p e r a t u r e . Procedure. The test was p e r f o r m e d in duplicate b y placing two 141/2 oz. cans of the e v a p o r a t e d milk in an u p r i g h t position in an incubator at 100 F. immediately a f t e r the sterilization of the product. The cans r e m a i n e d u n d i s t u r b e d f o r exactly 7 days. Then, with careful handling to avoid mixing, the top of each can was cut out a n d a 25-ml. sample was removed f r o m the u p p e r surface. This removal and m e a s u r e m e n t was conveniently accomplished b y the use of a 25-ml. pipette with its inlet tip bent u p w a r d . This tip was inserted in the center of the can so t h a t the r i m of the tip was parallel to and just below the surface.

64

R, B. ~ A X C Y

AND It. It. S O M M E R

B y means of v e r y gentle suction the pipette was slowly filled to its m a r k , k e e p i n g the inlet tip just below the surface b u t otherwise stationary. The f a t content of the 25-ml. portion was determined b y means of the Mojonnier f a t test. The known f a t content of the e v a p o r a t e d milk was s u b t r a c t e d f r o m the f o u n d f a t content in the 25-ml. sample and the difference was expressed as " p e r cent e n r i c h m e n t " by calculation as in the preceding test. This also m a y be spoken of as a f a t separation rating.

C. Viscosity Measurement
I n s o f a r as the viscosity m e a s u r e m e n t is to indicate the probable rate of f a t rise in the product, the m e a s u r e m e n t ideally should be confined to the viscosity of the m e d i u m in which the f a t particles, or fat-containing particles, are suspended. I t is' obviously impossible to attain this ideal; the m e a s u r e m e n t is of necessity confined to the rheological p r o p e r t i e s of the p r o d u c t as it exists. The " v i s c o s i t y " of the e v a p o r a t e d milk decreases on vigorous agitation, even a f t e r the weak, continuous gel, which m a y be evident i m m e d i a t e l y a f t e r sterilization, has been disrupted. I n other words, e v a p o r a t e d milk exhibits plastic flow characteristics, which p r e s u m a b l y should be recorded in t e r m s of " y i e l d v a l u e " and "consistency." I t is, however, questionable whether the " y i e l d v a l u e " has a n y reality in terms of the p r o d u c t as a whole. A f t e r the gel has been disrupted, the " y i e l d v a l u e " most p r o b a b l y reflects the s t r u c t u r a l stability of suspended particles of indeterminate size and shape. The m e d i u m in which the particles are suspended undoubtedly exhibits true viscous flow. I n order to measure plastic flow characteristics, the flow rates of each sample m u s t be measured at a n u m b e r of different pressures or applied forces. Such a procedure might be used to provide i n f o r m a t i o n as to the s t r u c t u r a l stability of suspended particles in e v a p o r a t e d milk. I t is, however, not a p p a r e n t how such data should be i n t e r p r e t e d in relation to the f a t separation problem. A t a n y rate, in the s t u d y in which the present methods were applied the flow of evapor a t e d milk samples was measured u n d e r a single set of conditions, a n d the observed flow rates were expressed in t e r m s of viscosity units. The plastic flow characteristics are tacitly acknowledged, and the results are k e p t ' o n a basis t h a t justifies comparisons between samples, in t h a t the same set of conditions was used for all samples.

The modified Gardner Mobilometer. The i n s t r u m e n t t h a t was used for measu r i n g the viscosity of e v a p o r a t e d milk was a modified G a r d n e r Mobilometer (1). W i t h this i n s t r u m e n t the viscosity was measured b y timing the descent of a disc or piston t h r o u g h the liquid in a vertical cylinder of u n i f o r m bore. A stem, attached to the piston, served to control the positioning, release, and t i m i n g of this disc or piston. The applied force could be varied by placing weights on a small p a n at the top of the stem.
I t has been found t h a t this t y p e of instrument, when used for liquids t h a t exhibit true viscous flow, yields flow rates t h a t are directly p r o p o r t i o n a l to the applied forces over a wide range of forces; deviation finally occurs, as in all

FAT SEPARATION

]N EVAPORATED

MILK

65

viscosity methods, when the velocity is sufficiently high to produce turbulence. This t y p e of i n s t r u m e n t was originally adopted in this l a b o r a t o r y for c r e a m viscosity m e a s u r e m e n t s to obviate erratic results t h a t will occur with c a p i l l a r y efflux i n s t r u m e n t s when the size of suspended particles approaches or exceeds the bore of the capillary. The modifications consist of the following f e a t u r e s : a leveling s t a n d f o r holding the removable cylinder, the entire assembly being of suitable design for placement in a w a t e r b a t h for convenient a n d accurate t e m p e r a t u r e control; a stem guide to fit the top of the cylinder; and a piston-like p l u n g e r of suitably chosen clearance in relation to the cylinder diameter, b u t with f o u r small high points on the piston r i m to serve as centering guides with a m i n i m u m of friction against the cylinder wall. The hollow piston-like p l u n g e r is illustrated in F i g u r e 2, and the entire assembly, in F i g u r e 3. B y using a piston, instead of a disc of limited thickness, the length of the flow channel, between two parallel surfaces, is increased, and the clearance can be correspondingly increased. E x c e p t for v e r y limited flow t h r o u g h the air escape vent, all of the flow. occurs between two parallel surfaces, viz., the piston clearance in relation to the cylinder wall. The cylinder was made out of a 10-in. length of 2-in. stainless steel s a n i t a r y tubing. I n use it was filled u n i f o r m l y to a height of 21 cm. Piston travel was timed t h r o u g h a distance of 10 cm. by sighting the passage of suitably placed m a r k s on the stem in relation to the top of the stem guide. The position of the

(b)

(a) (c)

"-~

t .1~)5
.250

Z6G4

. OG2.S

J~,

/. ro63 A BOB

-J

Fro. 2. The phmger of the modified Gardner Mobilometer.

66

R. B. MAXCY AND H. It. SOMMER,

FIG. 3.

Tile m o d i f i e d G a r d n e r

Mobilometer.

marks was established to allow at least 5 cm. travel for acceleration before starting the t i m i n g and to t e r m i n a t e the timing 2.5 cm. f r o m the bottom to avoid a possible "end effect." Procedure, standardizing the instrument. To standardize the i n s t r u m e n t so that t i m i n g observations can be t r a n s l a t e d into viscosity units, it was necessary to determine the flow rate of a liquid of accurately known viscosity, using an accurately known applied force. F o r solutions of known viscosity, sucrose solutions are conveniently used, r e f e r r i n g to detailed tables t h a t have been published for this purpose b y the U. S. B u r e a u of S t a n d a r d s (2). The applied force is the total weight of the traveling p a r t s minus the b u o y a n t force of the displaced liquid. D u r i n g a m e a s u r e m e n t the piston is completely immersed, but the stem immersion varies. Accordingly, the volume of the piston and stem is to be determined to a point m i d w a y between the i m m e r s e d stem length at the s t a r t and at the end of the t i m i n g interval. The displacement volume to this point can be most conveniently determined by weighing the piston and stem (a) suspended in air, and (b) suspended in water to the selected point on the stem. A torsion balance, accurate to 0.01 g., is suitable for this purpose. The difference between a and b in grams, divided b y the density of the w a t e r in grams per cubic centimeter represents the displacement in cubic centimeters.

FAT SEPARATION

IN EVAPORATED

MILK

67

The i n s t r u m e n t used i n this s t u d y was c a l i b r a t e d i n a c c o r d a n c e w i t h t h e above p r i n c i p l e s , a n d the essential d a t a are as follows: W e i g h t of p i s t o n a n d stem i n a i r ............................................. 71.32 g2 W e i g h t of p i s t o n a n d stem 6 i n w a t e r , 35 C .......................... 63.79 g2 W e i g h t of w a t e r d i s p l a c e d ................................................... 7.53 g. D e n s i t y of w a t e r at 35 C .................................................... 0.99403 g./cc. V o l u m e of w a t e r d i s p l a c e d .................................................. 7.58 cc. 5 Net weight, i.e., corrected for the weight of the suspension wire used in connection with the weighings. Immersed to the selected point on the stem as explained. T h e r e f o r e , the effective force ( i n g r a m s ) e m p l o y e d i n t i m i n g the d e s c e n t of the p i s t o n t h r o u g h the l i q u i d i n the c y l i n d e r is : 71.32 - (7.58 }( the d e n s i t y of the l i q u i d i n g . / c c . ) . I f the p a n a n d weights are a p p l i e d at the top of the stem, t h e i r w e i g h t is a d d e d d i r e c t l y to the effective force. The c o n s t a n t (k) for the i n s t r u m e n t was d e t e r m i n e d b y u t i l i z i n g a 6 0 % sucrose s o l u t i o n at t e m p e r a t u r e s s h o w n i n T a b l e 1, p r o c e e d i n g as d i r e c t e d below f o r viscosity m e a s u r e m e n t . The i n s t r u m e n t c o n s t a n t (k) reflects the p i s t o n clearance a n d the d i s t a n c e of t r a v e l . W i t h these f a c t o r s fixed, the t i m e ( t ) i n seconds will be d i r e c t l y p r o p o r t i o n a l to the viscosity of the l i q u i d (n) i n centipoises, a n d i n v e r s e l y p r o p o r t i o n a l to the effective force ( f ) i n grains. T h u s , the r e l a t i o n s h i p can be expressed b y the f o r m u l a kt ~ n / f . The fixed f a c t o r s are t h e r e f o r e t a k e n i n t o c o n s i d e r a t i o n t h r o u g h the i n s t r u m e l l t c o n s t a n t (k). W i t h n and f known, and with t determined by experimental observations, k c a n be e b m p u t e d b y m e a n s of the p r e c e d i n g f o r m u l a . The d a t a p e r t a i n i n g to the d e t e r m i n a t i o n of the i n s t r u m e n t c o n s t a n t are p r e s e n t e d i n T a b l e 1. The five f o u n d v a l u e s for the i n s t r u m e n t c o n s t a n t are i n s a t i s f a c t o r y a g r e e m e n t ; t h e i r a v e r a g e v a l u e is 0.01318.

Procedure, viscosity measurement. The cans of e v a p o r a t e d m i l k were p l a c e d

Determining the instrument constant for the modified Gardner Mobilometer

(cp.)
156.0 109.8 56.5 43.86 26.52

(g./cc.)
1.29334 1.29114 1.28640 1.28396 1.27876

(g.)
61.516 61.533 61.589 61.588 61.627

(sec.)
190.76 134.12 70.26 53.86 32.98

a The values were converted to g./cc, by multiplying by 0.999973. b Weight of piston and stem, 71.32 g.; displacement volume, 7.58 cc. The observed time represents the mean of 5 determinations in each case.

68

R. B. MAXCY AND H. H. SOMMEt

in a w a t e r b a t h at the chosen t e m p e r a t u r e 7 for 1 hour. The viscosity stand and cylinder also were placed in the w a t e r b a t h a n d the leveling screws were adjusted so t h a t the stand was level and the cylinder was p e r p e n d i c u l a r . E a c h can was opened j u s t p r i o r to the viscosity test, a n d the contents were t r a n s f e r r e d to the cylinder with a m i n i m u m of agitation. The piston was inserted to such d e p t h as to eliminate the air pocket f r o m the hollow piston, allowing the air to escape t h r o u g h the vent for t h a t purpose. The stem guide was then placed into position. W i t h the eyes on a level with the u p p e r surface of the stem guide, the piston was released and its time of descent was determined b y sighting the stem nlarks in relation to the guide. The observed time in seconds was converted to centipoises b y s u b s t i t u t i n g the p r o p e r values for f, k, and t in the f o r m u l a : n ~ f k t . I n using this procedure with the sucrose solution, or a n y other fluid t h a t exhibits true viscous flow, replicate determinations can be made with the same cylinder contents. This cannot be done, however, with e v a p o r a t e d milk; r e p e a t determinations lead to successively lower readings, a p p a r e n t l y because s t r u c t u r e s are being disrupted.
EVALUATION OF ]METHODS

H o m o g e n i z a t i o n effectiveness test. The c e n t r i f u g a l procedure was evaluated by a p p l y i n g it to unconcentrated, homogenized milk with k n o w n a d m i x t u r e s of unhomogenized milk and to milk t h a t had been homogenized at different pressures. Typical results are given in Table 2. The procedure also was evaluated in relation to e v a p o r a t e d milk m a n u f a c t u r e , and these findings arc r e p o r t e d in connection with the g r a v i t y f a t separation and viscosity determinations in Table 3. The results demonstrate t h a t the procedure, as outlined above, will detect small a d m i x t u r e s of unhomogenized milk or sma]l differences in the thoroughness of homogenization. These results were obtained with the f a t contents m e a s u r e d by the Babcock test; g r e a t e r precision p r o b a b l y could be achieved b y using g r a v i m e t r i e f a t determinations. Composite evaluation of the tests. To evaluate the homogenization effectiveness test in conjunction with the viscosity test in relation to the g r a v i t y f a t separation test, the three tests were applied to 27 samples of e v a p o r a t e d milk f r o m the commercial operations of five different e v a p o r a t e d milk plants. F o r each sample one can of unsterilized milk and three cans of the same milk a f t e r sterilization were obtained. The homogenization effectiveness test was applied to the unsterilized product, diluted with an equal volume of w a t e r ; one can of the sterilized p r o d u c t was used for the viscosity determination, and the other two cans were stored for the g r a v i t y f a t separation test in duplicate. The results are given in Table 3.
I n t h i s s t u d y t h e v i s c o s i t y of e v a p o r a t e d m i l k s a m p l e s w a s m e a s u r e d a t 37.78 C. ( 1 0 0 F . ) u s i n g a p i s t o n a n d stem w e i g h t of 71.32 g., a n d a s s u m i n g t h e d e n s i t y of t he s a m p l e s to be 1.06. The effective fo rce w a s 71.32 - - (7.58 X 1.06) o1" 63.285 g. B e c a u s e the e ffe c t i ve forc e (f) was c o n s i d e r e d to be c o n s t a n t f r o m s a m p l e to s a m p l e , t h i s f o o t e r w a s c o n s o l i d a t e d w i t l i /~; //~ = 63.285 X 0.01318 or 0.834. Thus, n ~- 0.834 X t.

FAT SEPARATION IN EVAPORATED MILK

69

TABLE

2 Homogenization effectiveness (% enrichment) 47.8 60.7 67.8

T h e s e n s i t i v i t y o f t h e h o m o g e n ~ a t i o n e f f e c t i v e n e s s test
D e s c r i p t i o n of milk sample 100 98 96 94 ml. ml. ml. ml. homo. homo. homo. homo. milk" m i l k + 2 ml. unhomo, m i l k b m i l k + 4 nil. unhomo, m i l k m i l k + 6 ml. unhomo, m i l k F a t c o n t e n t of t o p 10 In]. 5.1 5.5 5.8
6.0

5.1 5.6 5.8

M i l k ' h o m o g e n i z e d a t 1,750 psi. M i l k h o m o g e n i z e d a t 2,000 psi. M i l k h o m o g e n i z e d a t 2,250 psi. M i l k h o m o g e n i z e d a t 2,500 psi. a F a t c o n t e n t 3.45% b :Fat c o n t e n t 3.6qv TABLE 3

5.1 4.8 4.6 4.4

5.2 4.7 4.6 4.4

49.3 37.7 33.3 27.5

Gravity f a t separation in evaporated mil~ in relation to the homogenization effectiveness and viscosity tests
S a m p l e No. and P l a n t No. 1- 3 2- 3 3- 5 4- 4 5- 4 6- 5 7- 2 8- 3 9- 2 10 - 1 11 - 5 12 - 1 13 - 5 14 - 1 15 - 1 16 - 3 17 - 3 18 - 2 19 - 4 20 - 4 21 - 2 22 - 4 23 - 1 24 - 3 25 - 2 26 - 1" 27 - 1" Gravity fat separation 1.7 2.0 2.1 2.3 2.5 2.8 3.2 3.8 3.9 4.3 5.1 6.6 7.2 8.8 10.0 10.2 10.6 11.8 13.7 18.1 19.8 23.5 26.8 30.5 37.5 76.9 124.0 tIomogenization effectiveness (% enrichment) 17.4 19.3 20.6 19.3 26.3 21.8 22.5 12.4 21.2 30.0 18.7 23.1 21.8 32.6 23.4 25.0 22.5 21.7 31.3 28.8 23.7 29.6 46.4 24.4 24.4 70.5 106.0 Viscosity

(cp.)
30.0 27.4 40.7 37.0 39.9 37.4 26.9 22.9 22.3 31.8 40.9 22.1 25.0 23.4 20.5 18.1 15.3 15.3 17.6 11.9 14.7 13.8 14.7 10.8 9.0 9.8 9.2

HE/V h 0.58 0.70 0.51 0.52 0.66 0.58 0.84 0.54 0.95 0.94 0.46 1.04 0.87 1.39 1.14 1.38 1.47 1.42 1.78 2.42 1.61 2.14 3.16 2.26 2.71 7.19 11.50

Specially prepared samples. b H o m o g e n i z a t i o n effectiveness r a t i n g d i v i d e d b y v i s c o s i t y . These data show that Likewise, there there is less gravity is less gravity obtaining separation fat separation in the samples with

a high viscosity. of homogenization rating. Since the rate

fat separation

as the effectiveness effectiveness size of the

is increased, of gravity fat

a lower

homogenization related to the

is directly

70

1%. B. M A X C Y A N D I-I. I-I. S O M M E R

fat globules and inversely related to the viscosity of the suspending medium, these latter terms should somehow be combined. This may be accomplished by dividing the effectiveness of homogenization b y the viscosity of the sample. Thus, a f o u r t h term is obtained and this figure is directly related to the extent of gravity fat separation. This relationship is positive and is linear over the range of samples in this trial. The precision of the relationship between fat separation and the term reflecting homogenization effectiveness and viscosity can best be expressed by the statistical term coefficient of correlation. The data in Table 3 show a positive coefficient of correlation of 0.989.
DISCUSSION

It is logical to expect that the general phenomenon of fat separation can be viewed in light of the f u n d a m e n t a l concepts relating to the rise of fat particles in unconcentrated milk. This permits the division of the problem into a n u m b e r of separate entities, e.g., viscosity, size of the fat particles, and the density difference between the fat particles and the suspending medium. It is then necessary to adopt or devise methods for measuring the individual factors which can be related to the general phenomenon. F o r example, the rate of rise of the individual fat particles (likewise fat separation) would be directly related to the square of the radii of the fat particles. F r o m the theoretical standpoint the size of the individual fat particles is of interest, but from a practical standpoint the interest is p r i m a r i l y in the combined effect of the various sizes. The total effect of the various sizes will determine the extent of fat separation. The total effect of the various sizes is the basis of the methods developed in this work for effectiveness of homogenization and gravity separation. This m a y be explained by the following reasoning : The sample to be tested is in a container of fixed height and the quantity removed from the u p p e r layer is equivalent to a fixed height, or a fixed p r o p o r t i o n of the total sample. The size of the fat particles influences the rate at which they travel. F o r example, a 2 ~ fat particle would travel x distance under the conditions of the experiment, and a 6 ~ fat particle would travel 9x distance, since the rate of travel is directly proportional to the square of the radius. Thus, the larger globules would travel a greater distance, and a greater number would travel from the lower section to the u p p e r section to be removed in the sample for enrichment. I t t h e r e f o r e follows that the tendency for enrichment is directly related to the size of the particles. On the basis of this reasoning, the previously described tests are f u n d a m e n t a l l y sound and measure the tendency for concentration in the u p p e r layer, reflecting practical conditions. The general phenomenon involves another factor, viscosity, which m a y b e . isolated and measured. The importance of viscosity can be determined by its influence on the rate of rise of the individual globules or the over-all problem of fat separation. W i t h our present knowledge, however, the effectiveness of the method for measuring viscosity can be evaluated only in terms of the other tests, as a total relationship.

FAT SEPARATION IN EVAPORATED ~IILK

71

The over-all evaluation of methods using commercial samples showed a good correlation between gravity fat separation and the combined value for effectiveness of homogenization and viscosity. These results substantiate the efficacy of the methods and establish the relative importance of the individual factors of the general problem of fat separation.
SUMMARY

The problem of fat separation in evaporated milk can be divided into at least three factors. The extent of fat separation is inversely related to the viscosity, directly related to the square of the radii of the fat particles and directly related to the density difference between the fat particles and the suspending phase. A suggested procedure is given for determining the effectiveness of homogenization. This method is based on the total effect, or the result of the rate of travel, of the fat particles. E x t e n d i n g the same logic, a method is given for determining the extent of gravity fat separation during storage. In addition, the procedure and description are given for a modified Gardner Mobilometer as a means of measuring viscosity. These methods were applied to samples of commercially prepared evaporated milk, and the correlation between the tests was highly significant.
ACKNOWLEDGMENTS This work was financed in p a r t by a grant from the Carnation Company. REFERENCES (1) BALDESCH~VIELER,E. L., AND WILCOX, L. Z. Determination of High iscosities by Means of the Gardner Mobilometer. Ind. Eng. Chem., Anal. Ed., 11: 525. 1939. (2) Bulletin of the Bureau of Standards. Government P r i n t i n g Office, Washington, D. C., p. 86, Appen. B. 1918-19. (3) DEYSHER, E. F., WEBB, B. H., AND HOLM, G. E. The Viscosity of Evaporated Milks of Different Solids Concentrations. J. Dairy Sci., 27: 345. 1944. (4) HOSTETTLER, H., RYCHENER, ELIZABETH, AND KUNZLE, LILLY. Untersuchungen fiber das in der Kuhmilch in nativem (Genuinum) Zustand Vorliegende Kasein. Landwirtseh. Jahr. Sehwetz, 63: 31. 1949. (5) RAHN, O , AND SHARF, P. F. Physil~ der MiIch~virtschaft. Verlagsbuchhandlung Paul Parey, SW 11, Hedemannstrasse 28 u. 29, Berlin. 1928. (6) SNYBER, W. E., AND S0~MEI~, H. H. Quick Test for Homogenized Milk. Wis. Agr. Expt. Sta., Bull. 456. 1942. (7) TROY, H. C., AND SHARP, P. F. Physical Factors Influencing the Formation and F a t Content of Gravity Cream. J. Dairy Sci., 11" 189. 1928.