C R C Critical Reviews in Food Science and Nutrition

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Freeze concentration of fruit juices

a b c d e
S. S. Deshpande , Munir Cheryan , Shridhar K. Sathe , D. K. Salunkhe & B. S. Luh
a
Research Assistant, Department of Food Science , University of Illinois , Urbana, Illinois
b
Associate Professor of Food Engineering, Department of Food Science , University of
Illinois , Urbana, Illinois
c
Research Associate, Department of Nutrition and Food Science, Muscle Biology Group ,
University of Arizona , Tucson, Arizona
d
Vice Chancellor, Mahatma Phule Agricultural University , Maharashtra State, India
e
Food Technologist, Department of Food Science and Technolog , University of California ,
Davis, California
Published online: 29 Sep 2009.
To cite this article: S. S. Deshpande , Munir Cheryan , Shridhar K. Sathe , D. K. Salunkhe & B. S. Luh (1984)
Freeze concentration of fruit juices, C R C Critical Reviews in Food Science and Nutrition, 20:3, 173-248, DOI:
10.1080/10408398409527389
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Volume 20, Issue 3 173
FREEZE CONCENTRATION OF FRUIT JUICES
Authors: S. S. Deshpande
Munir Cheryan
Department of Food Science
University of Illinois
Urbana, Illinois
Shridhar K. Sathe
Department of Nutrition and Food Science
University of Arizona
Tucson, Arizona
D. K. Salunkhe
Mahatma Phule Agricultural University
Downloaded by [McGill University Library] at 15:34 29 March 2015
Maharashtra State, India
Referee: B. S. Luh
Department of Food Science and Technology
University of California
Davis, California
I. INTRODUCTION
A. Importance of Fruits in Human Diet

As "accessory foods", fruits have an important role in the human diet. They add a variety
of color, taste, and texture to meals and snacks. Nutritionally, fruits provide significant
amounts of several vitamins and they are major contributors of essential minerals. With the
exception of avocados and olives, which are relatively high in fat, fruits can be considered
low calorie foods. Fresh fruits have a natural laxative effect because of the cellulose and
organic acids present and thus aid digestion. They provide an alkaline residue or ash that
neutralizes the acidic residues formed by the consumption of meat, eggs, and other protein-
rich foods." 2
Several fruits especially the high-acid citrus fruits, are valuable sources of ascorbic acid.
They also supply carotene, which is a precursor of vitamin A in the body. Although tree
fruits are generally low in B-complex vitamins, several of the dried fruits and citrus products
contribute some vitamin B, to the diet. Several fruits are excellent sources of potassium,
calcium, and iron. Data on selected nutrients and their fruit sources are presented in Table
1.
Most fresh fruits contain 75 to 95% water. They are low in protein, but generally contain
substantial quantities of carbohydrates, including varying proportions of dextrose, fructose,
sucrose, and starch depending on the type of fruit and its maturity. The principal acids found
in fruits are citric, malic, and tartaric acids. The pH of fruits ranges from 2.5 to 4.5. Other
important constituents of fruits include cellulose and woody fibers, mineral salts, pectin,
gums, tannins, pigments, and volatile compounds. Nutritional and compositional aspects of
several fruits and fruit products have recently been reviewed by Young." 2 Nutritional con-
tributions of selected fruit juices to the human diet are summarized in Tables 2 and 3.
B. Early History of Fruit Processing

Dehydration is probably the oldest method of preservation of fruits. Sun-dried fruits
174 CRC Critical Reviews in Food Science and Nutrition
Table 1
SELECTED NUTRIENTS AND THEIR FRUIT SOURCES112
Nutrient Examples of fruit sources
Protein (includes enzymes and Low, dried apricots and dried figs are highest
amino acids)
Carbohydrates (starches, sugars, Most all fruits, especially bananas, currants, dates,
and celluloses) and raisins
Fats (oils) Very low, except avocados and olives
Water Fresh fruits are usually high, and dried fruits are low
Calcium Blackberries, currants, dried figs, and rhubarb
Iron Dried apricots, dried figs, dried peaches, and prunes
Iodine Variable depending upon iodine content of soil
Phosphorus Dried peaches, dried raisins, and dried figs
Potassium Apricots, bananas, cherries, dates, currants, figs,
dried peaches, dried prunes, and raisins
Dried apricots, currants, dates, figs, dried peaches,
Sulfur
and olives
Vitamin A (carotene) Dried apricots, cantaloupes, peaches, orange juice,
and watermelons
Vitamin C (ascorbic acid) Citrus juices, cantaloupes, and strawberries
Vitamin B, (thiamin) Avocados, orange juice
Vitamin B2 (riboflavin) Avocados and dried peaches
Niacin Dried apricots, and dried peaches
Vitamin B6 (pyridoxine) Bananas and raisins
Vitamin B, 2 (cyanocobalamine) Low
Vitamin D (includes D2 = calci- Low
ferol, and D 3 = irradiated
dehydrocholesterol)
Vitamin E (tocopherols) Olives
Pantothenic acid Oranges
Biotin Bananas and strawberries
antedate the use of fire for cooking and the roots of the modern dehydrated, dehydrofrozen,
and granulated fruit industry can be traced back to this oldest method of fruit processing. 1 "
Fermentation was another popular mode of fruit juice processing and preservation. Fer-
mented beverages such as beer, wine, cider, brandy, cordials, and nectars have since given
way to fruit juices, punches, nectars, ades, and concentrates. These products could be canned,
frozen, dried, powdered, or concentrated.
Chemical preservation of whole, sliced, or sectioned fruit by soaking them in honey or
sugar syrup or by use of vinegar or wine represents one of the oldest methods of fruit
processing and preservation. Today, these products have been replaced by a variety of fruit
preserves, jams, marmalades, glazes, jellies, fruit butters, sauces, and pickles.23
A major breakthrough in food preservation occurred when Appert laid the foundations of
canning in France in the early part of the 19th century. Thermal processing of fruits, however,
remained an art rather than a science throughout the 19th century, the major hurdles being
the processing equipment, the containers, method of preparation, and procedures. 40 - 4 ' 1 "
With the advent of the National Canners Association (NCA) in 1907, thermal processing of
foods made rapid strides. The classic works of Bitting18 and Bigelow and Catheart,17 pub-
lished in a series of bulletins by the NCA, firmly established the principles underlying
canning and thermal processing of foods. Detailed descriptions and history of the science
and technology of thermal processing of foods are contained in two excellent articles by
Goldblith.40-41 Woodroof" cites the newer knowledge in applied bacteriology, developments
in processing technology, and in the improvements in processing equipment as the three
major factors behind the growth and success of the canning industry during the 20th century.
Table 2
NUTRITIONAL CONTRIBUTIONS OF SELECTED FRUIT JUICES 13 " 2
Food
Weight Water energy Protein Fat Carbohydrates
Fruit juice Measure (g) (%) (cal) (g) (g) (g)
Apple juice
Canned/bottled 1 cup 248 88 120 Tr Tr 30
Apricot nectar
Canned 1 cup 251 85 140 1 Tr 37
Cranberry juice
Cocktail, canned 1 cup 250 83 165 Tr Tr 42
Grapefruit juice
Fresh 1 cup 246 90 95 1 Tr 23
Canned, white
Unsweetened 1 cup 247 89 100 1 Tr 24
Sweetened 1 cup 250 86 130 1 Tr 32

Frozen concentrate, unsweetened
Undiluted; 6-fl oz can 1 can 207 62 300 4 1 72
Diluted with 3 parts water by 1 cup 247 89 100 1 Tr 24
volume
Dehydrated crystals prepared with 4 oz 118 1 410 6 1 102
water (1 lb yields about 1 gal) 1 cup 247 90 100 1 Tr 24
Grape juice
Canned/bottled 1 cup 253 83 165 1 Tr 42
Frozen concentrate, sweetened
Undiluted, 6-fl oz can 1 can 216 53 395 1 Tr 100
Diluted wth 3 parts water by 1 cup 250 86 135 1 Tr 33
volume
Grape juice drink
Canned 1 cup 250 86 135 Tr Tr 35
Lemon juice
Raw 1 cup 244 91 60 1 Tr 20
Lemonade, concentrate
Frozen, 6-fl oz can 1 can 219 48 430 Tr Tr 112
Diluted with 4'/ 3 parts water by 1 cup 248 88 110 Tr Tr 28
volume
Lime juice
Fresh 1 cup 246 90 65 1 Tr 22
Canned, unsweetened 1 cup 246 90 65 1 Tr 22
Limeade, concentrate
Frozen, 6-fl oz can 1 can 218 50 410 Tr Tr 108
Diluted with 4V3 parts water by 1 cup 247 90 100 Tr Tr 27
volume
Orange juice, fresh
All varieties 1 cup 248 88 110 2 1 26
Canned, unsweetened 1 cup 249 87 120 2 Tr 28
Frozen concentrate
Undiluted, 6-fl oz can 1 can 213 55 360 5 Tr 87
volume
Dehydrated crystals prepared with 4 oz 113 1 430 6 2 .100
water (1 lb yields about 1 gal) 1 cup 248 88 115 2 1 27
Orange-apricot juice drink 1 cup 249 87 125 1 Tr 32
Orange and grapefruit juice
Frozen concentrate
Undiluted, 6-fl oz can 1 can 210 59 330 4 1 78
volume
Table 2 (continued)
NUTRITIONAL CONTRIBUTIONS OF SELECTED FRUIT JUICES 13112
Food
Weight Water energy Protein Fat Carbohydrates
Fruit juice Measure (g) (%) (cal) (g) (g) (g)
Pineapple juice
Canned 1 cup 249 86 135 1 Tr 34
Prune juice
Canned/bottled 1 cup 256 80 200 1 Tr 49
Tangerine juice
Canned, sweetened 1 cup 249 87 125 1 1 30
1
Amount from the fruit. Additional Vitamin C may be added by the manufacturers.
b
For white-fleshed varieties, value is about 20 IU per cup; for red-freshed varieties, 1080 IU per cuo.
c
Present only if added by the manufacturer.
Thus, the leading methods of processing fruits have shifted continuously through the
centuries from sun-drying and sugar and chemical preservation towards modern day, tech-
nology-oriented processing methods such as canning, artificial dehydration, concentration,
radiation, and freezing, and combinations of one or more of these methods. With it, the
consumption pattern of fruits also changed. The percentage of fruits processed as compared
to those eaten fresh steadily increased. According to Woodroof,1" this general trend appears
to have been due to improvements in varieties of fruits for processing, horticultural practices
and production of the fruits especially suitable for processing, mechanical harvesting of
fruits, techniques for processing large volumes of fruits, containers more suitable for proc-
essed fruit, extending the shelf-life of processed fruits, raising the standards and nutritional
value of processed fruits, and more attention to marketing of processed fruits, especially for
export purposes.
C. Consumption Trends and Prospects

In the past two decades, there has been a striking shift in the way both citrus and deciduous
fruits are consumed, from the fresh fruit to the processed. Consumption trends for different
forms of processed fruit have also undergone significant changes. These changes have been
brought about by many influences, which have a direct or indirect bearing on the fruit
processing industry.
According to a study conducted by the U.S. Department of Agriculture, (USDA),101
consumer expenditures for domestic-produced food in the U.S. averaged about $531 per
person in the year 1971 (Table 4). This amounted to 16.5% of total per capita personal
consumption expenditures. The expenditures on animal food products (poultry, eggs, meat,
and dairy products) accounted for nearly half (about 51%) of the total expenditure on food
products. In contrast, only about $38, i.e., approximately 7% of the total food expenditures
or nearly 1.2% of the total personal consumption expenditures was fruit. This same general
pattern of overall expenditures on different food groups probably exists today. However,
the total per capita fruit consumption indicates great fluctuations over the past three decades
and appears to have been influenced by seasonal variations in fruit production. The share
of citrus fruits of the total U.S. fruit market increased steadily from 39% in 1950 to about
53% in 1980 and the State of Florida alone produced the bulk of it (Table 5).
Since the advent of fruit juice concentration technology in the mid-1940s, consumption
of fruits in various processed forms increased steadily, while fresh fruit consumption actually
declined. The processed share increased from 43% in 1950 to nearly 65% in 1978. l03 In
1980, approximately 73.6% of the total citrus production in the U.S. was consumed in the
processed form, whereas the processed share for the rest was 66.8% of their production.104
Table 3
Vitamin A
Weight Ca Fe value Vitamin
Vitamin B, Vitamin B2 Niacin Vitamin C
Fruit juice Measure (g) (nig) (nig) (IU) (nig) (nig) (nig) (nig)
Apple juice
Canned/bottled I cup 248 15 1.5 — 0.02 0.05 0.2 2
Apricot nectar
Canned 1 cup 251 23 0.5 2380 0.03 0.03 0.5 8'

Cranberry juice
Cocktail, canned 1 cup 250 13 0.8 Tr 0.03 0.03 0.1 40
Grapefruit juice
Fresh 1 cup 246 22 0.5 0.0" 0.09 0.04 0.4 92
Canned, white
Unsweetened 1 cup 247 20 1.0 20 0.07 0.04 0.4 84
Sweetened 1 cup 250 20 1.0 20 0.07 0.04 0.4 78
Frozen concentrate, unsweetened
Undiluted, 6-fl oz. can 1 can 207 70 0.8 60 0.29 0.12 1.4 286
Diluted with 3 parts water by 1 cup 247 25 0.2 20 0.10 0.04 0.5 96
volume
Dehydrated crystals prepared with 4 oz. 118 100 1.2 80 0.40 0.20 2.0 396
water (1 lb yields about 1 gal) 1 cup 247 22 0.2 20 0.10 0.05 0.5 91
Grape juice
Canned/bottled 1 cup 253 28 0.8 — 0.10 0.05 0.5 Tr
Frozen concentrate, sweetened
Undiluted, 6-fl oz. can 1 can 216 22 0.9 40 0.13 0.22 1.5 c
3n>
Diluted with 3 parts water by 1 cup 250 8 0.3 10 0.05 0.08 0.5 c O
volume
Grape juice drink
Canned 1 cup 250 8 0.3 — 0.03 0.03 0.3 d ft
Lemon juice
Raw 1 cup 244 17 0.5 50 0.07 0.02 0.2 112
Lemonade, concentrate
Frozen, 6-fl oz can 1 can 219 9 0.4 40 0.04 0.07 0.7 66
Diluted with 4'/, parts water by 1 cup 248 2 Tr Tr Tr 0.02 0.2 17
volume
Table 3 (continued)
O5
Vitamin A
Weight Ca Fe value Vitamin B, Vitamin B2 Niacin Vitamin C
Fruit juice Measure (g) (mg) (mg) (IU) (mg) (mg) (mg) (mg)
Lime juice
Fresh 1 cup 246 22 0.5 20 0.05 0.02 0.2 79
Canned, unsweetened 1 cup 246 22 0.5 20 0.05 0.02 0.2 52
Limeade, concentrate
Frozen, 6-fl oz can 1 can 218 11 0.2 Tr 0.02 0.02 0.2 26
Diluted with 4 1 /, parts water by 1 cup 247 2 Tr Tr Tr Tr Tr 5
volume
Orange juice, fresh
All varieties 1 cup 248 27 0.5 500 0.22 0.07 1.0 124 a.
Canned, unsweetened 1 cup 249 25 1.0 500 0.17 0.05 0.7 100 2
Frozen concentrate
Undiluted, 6-fl oz can 1 can 213 75 0.9 1620 0.68 0.11 2.8 360
Diluted with 3 parts water by 1 cup' 249 25 0.2 550 0.22 0.02 l.Q 120
volume
Dehydrated crystals prepared with 4 oz 113 95 1.9 1900 0.76 0.24 3.3 408
water (1 lb yields about 1 gal) 1 cup 248 25 0.5 500 0.20 0.07 1.0 109
Orange-apricot juice drink 1 cup 249 12 0.2 1440 0.05 0.02 0.5 40
Orange and grapefruit juice
§
Frozen concentrate
Undiluted, 6-fl oz can 1 can 210 61 0.8 800 0.48 0.06 2.3 302
Diluted with 3 parts water by 1 cup 248 20 0.2 270 0.16 0.02 0.8 102
volume
Pineapple juice
Canned 1 cup 249 37 0.7 120 0.12 0.04 0.5 22"
Prune juice
Canned/bottled 1 cup 256 36 10.5 — 0.03 0.03 1.0 5"
Tangerine juice
Canned, sweetened 1 cup 249 45 0.5 1050 0.15 0.05 0.2 55
Amount from the fruit. Additional Vitamin C may be added by the manufacturers.
For white-fleshed varieties, value is about 20 IU per cup; for red-fleshed varieties, 1080 IU per cup.
Present only if added by the manufacturer.
Table 4
PER CAPITA EXPENDITURES FOR
DOMESTIC FARM FOOD
PRODUCTS, 1971ICI
Expenditures per
capita
Commodity group $ %
Meat products 154.49 29.1

Dairy products 80.17 15.1
Poultry and eggs 38.18 7.2
Fruits 37.70 7.1
Vegetables 74.17 14.0
Grain mill products 15.42 2.9
Bakery products 55.81 10.5

Miscellaneous 74.91 14.1
All farm food expenditures 530.85 100.0
Total personal consumption 3211.00
expenditures
Table 5
ORANGE PRODUCTION IN FLORIDA AND
THE ENTIRE U.S. 49
Production (1000
boxes) Florida production
as % of total
Crop year Florida Total U.S. U.S. production
1975—1976 181,200 242,780 75

1976—1977 186,800 242,950 77
1977—1978 167,800 220,120 76
1978—1979 164,000 210,500 78
This shift from fresh to processed forms has been more striking with citrus than with
other types of fruits. The consumption of citrus fruits in processed forms increased from
about 43% of total citrus fruit production in 1950 to nearly 74% in 1980.104 Frozen citrus
juices alone contribute the major share of total fruits processed. Since its commercial intro-
duction in 1945/1946, frozen orange concentrate has become, in terms of fresh weight
equivalent consumed, the leading processed fruit product. More than 80% of the Florida
orange crop is reportedly converted to frozen concentrate.103
The upward trend in per capita consumption of processed citrus products, as compared
to the declining consumption of fresh citrus in the U.S., is shown in Figure 1. In recent
years, per capita consumption of both total and frozen citrus products indicates upward
trends. On the other hand, consumption of fresh citrus fruits has declined approximately by
80% in the past three decades. In recent years, canned and chilled fruit juices have captured
a significant share of the citrus fruit market. The increase in consumption of processed citrus
products thus more than offsets the decline in fresh citrus consumption. The consumption
of all citrus products, therefore, has steadily increased through the years. Per capita con-
sumption of processed and fresh citrus products amounts to 76.7 and 23.3%, respectively,
1 I I
1950 1955 1960 1965 1970 1975 1980
Yeaf
FIGURE I. U.S. citrus consumption per person (in kg), A = total; B = frozen juice; C = fresh fruit; D =
canned fruit and juice; and E = chilled fruit and juice. (From USDA, Econ. Res. Serv., Washington, D.C., 1978).
of the total, in terms of fresh weight equivalent consumed (Figure 2). In the U.S., among
the three most popular modes of utilization, frozen citrus concentrates alone share 66.7%
of total processed and 51.2% of overall per capita consumption of citrus products.
Several factors influence the fruit consumption patterns. Year-to-year variations in fruit
production, resulting from changes in growing conditions in the various fruit producing
areas, may be a major factor. The per capita consumption of fruit products, as shown in
Figures 1 and 2, very well illustrates this factor. Population, income, price, technology,
impact of synthetics and substitutes on fruit product markets (especially fruit juices), rapid
growth of the food service industry, and increasing urbanization are some of the other factors
that have influenced changes in the pattern of fruit consumption over the past three decades.97
A major threat to the well-established fruit juice concentrate industry, however, may come
from the rapid development of the fruit juice substitute industry. Rapid strides made in
perfecting freeze-drying technology have given way to a surge of fruit juice powders, both
natural and synthetic, on the market. Breakfast drinks in particular seem to have caught the
attention of the consumer over the past few years. Taste-panel studies of a frozen synthetic
concentrate also indicated a greater consumer preference for the synthetic product as com-
pared to the natural.97 One study, conducted in 1966, predicted a 30% share of the more
than billion-dollar fruit beverage market for fruit juice synthetics and substitutes.'9
Several projections indicate excellent prospects for the fruit beverage industry for the next
two decades.3•2830-48-84 Because of population growth, the total demand for fruit products
is expected to increase in the years ahead. The per capita fruit consumption, however, is
expected to increase only marginally. Citrus fruit products are expected to contribute most
of the increased consumption. The shift from fresh to processed fruit consumption is also
expected to continue in the next two decades. Over the years, the prices of processed products
have increased at a substantially lower rate than those of fresh fruits. Further developments
in technology and use of energy saving processes may also help to increase the consumption
120-
100-
1950 1955 1975 1980
FIGURE 2. U.S. citrus fruit consumption per person (in kg), fresh equivalent basis. A = total; B = total
processed; C = frozen juice; D = fresh juice; E = canned fruit and juice; and F = chilled fruit and juice. (From
USDA, Econ. Res. Serv., Washington, D.C., 1978).
of processed fruit products by stabilizing and/or lowering the market prices. The increased
convenience of processed forms, their year-round availability, and improved uniform quality,
so far, have been major factors influencing this shift. The rising standard of living, increasing
urbanization, increased employment of women, and the desire for more leisure time are
some of the factors expected to increase demand for processed fruit.97 Frozen fruit juices,
particularly citrus, are expected to account for the major share of increased consumption.
Because of their convenience and high quality, increased demands for chilled fruit juices
are foreseen in the near future. Improvements in handling and storage methods of fresh
fruits are expected to increase their consumption.
II. FRUIT JUICE CONCENTRATION
A. Need for Concentration

The common liquid foods encountered in everyday life are mostly aqueous solutions and/
or suspensions. Those prominent in our daily life include fruit juices, soups, tea, coffee,
milk, beer, and wines. The solids content of most liquid foods is low, usually in the range
of 8 to 16% (Table 6). Oftentimes it is expensive to package, store, and ship "single-
strength" liquids, and in many cases it is desirable to remove a part or all of the water from
such liquids.
It is obvious that much of what the consumer eats and pays for in food is water. Huxsoll49
conducted a survey of supermarkets to determine the retail value of water in selected foods.
As shown in Table 7, the water alone would make up 70 to 95% of the total cost of the
products. Another aspect of water in frozen foods can also be judged by the energy required
for transportation. Table 8 summarizes data on the transport-to-fuel ratio for different modes
of transportation. Truck (at 60 ton/mi/gal) and rail (at 190 ton/mi/gal) are the most likely
Table 6
APPROXIMATE SOLUBLE
SOLIDS CONTENT OF SOME
COMMON FOOD
LIQUIDS 1366112
Total
solids
Commodity (%)
Apple juice 12.0

Apricot or nectar juice 15.0
Cranberry juice 10.6
Cranberry juice cocktail 17.0
Grapefruit juice 10.0
Grape juice (Concord) 14.3
Lemon juice 9.0

Lime juice 10.0
Orange juice 12.7
Orange-apricot juice drink 13.0
Pineapple juice 14.3
Pomegranate juice 15.0
Strawberry juice 8.0
Tangerine juice 13.0
American beer 4.5
Coffee 1.5
Tea 0.35
Wine (dry) 2.0
Wine (sweet) 9.0
Table 7
RETAIL VALUE OF WATER IN FOODS49
Retail price Water content Value of water

Food ($/Ib) (%) ($/lb of food)
Apples 0.39 84 0.32

Beef (sirloin) 3.00 70 2.10
Carrots 0.28 88 0.25
Lettuce 0.28 95 0.27
Onions 0.50 89 0.45
Potatoes 0.37 80 0.30
Rice 0.75 12 0.09
transportation modes for almost all frozen food products. However, even between these
modes there is a threefold difference in energy requirements. A greater emphasis on rail
transportation would substantially reduce energy requirements for distribution.
The cost of truck transportation for fruit and vegetable products is shown in Table 9.
Over a period of 5 years, from 1976 to 1981, the total cost of truck transportation increased
by 82%, while the rise in the fuel costs was 156%. The fuel costs rose from 20% of the
total cost in 1976 to 27% in 1980 and 28% in 1981. The cost of energy, therefore, has a
tremendous impact on the cost of food distribution. It is evident that refrigeration, storage,
transportation, and distribution costs of single-strength food liquids could be greatly reduced
by removing a substantial amount of their water content.
Concentration of liquid foods generally offers the following advantages:
1. Reduced requirements for storage space by virtue of smaller volumes

Table 8
ENERGY REQUIRED FOR
TRANSPORTATION49
Transport-to-fuel ratio
Mode of transportation (ton/mi/gal)
Air • 4
Truck 60
Railroad and ship 190
Pipeline 300
Table 9
COST OF TRANSPORTATION BY TRUCK49
Total cost Fuel cost Fuel

cost
as 'x of
Amount % of 1976 % of 1976 total
fear* (cVmi) total cost Amount fuel cost cost
1976 58.6 100 11.6 100 20

1979 76.3 130 15.3 131 20
1980 95.7 163 25.4 219 27
1981 107.4 182 29.7 256 28
Month of March.
2. Reduced refrigeration loads

3. Reduced transportation costs
4. Cheaper packaging
5. More profitable export marketing via efficient handling
6. Operation of local satellite bottling plants served by one large centrally located unit,
particularly for the production of single-strength liquids such as cola beverages, beer,
and wines
7. Improvement in product quality, stability, and shelf life
Fruit juices are watery mixtures of mostly unstable volatile organic compounds. They are
heat sensitive and their color and flavor deteriorate rapidly as processing temperatures are
increased. Even at moderate temperatures, many of their components are unstable. At
temperatures between 40 and 70°C, enzyme-catalyzed reactions can alter juice properties
within a few minutes. In order to inactivate the enzymes, juices must be heat treated. At
the same time, to obtain a quality product, it is essential to have sanitary conditions of high
standards. Since it is the aroma volatiles that give a food product its wide variety of flavor
sensations, even minor changes in aroma during concentration can greatly alter the sensory
qualities of the final product. Thijssen8890 specified the following conditions that must exist
in order to obtain high quality concentrates:
1. Low process temperatures

2. Short residence times in the process apparatus, especially if high temperatures are used
3. Nearly sterile operation
4. Selective dewatering, i.e., the major proportion of all components except water should
be retained in the concentrate
Apart from physical, chemical, and biological analyses, a key quality factor of the con-
Table 10
PROCESSES FOR REMOVAL OF WATER FROM FOODS22
Category Liquid food Structured food
Concentration processes Evaporation

(up to 50—60% solids) freeze concentration
Dialysis
Reverse osmosis
Ultrafiltration
Pervaporation
Clathration
Extraction
Dehydration processes Spray drying Tunnel drying
(>60% solids) Drum drying Packed-bed drying
Freeze drying Fluidized-bed drying
Foam-mat drying Vacuum-contact drying
Fluid-bed drying Freeze drying

Extraction Leaching
centrate is its organoleptic quality. Aroma quality often determines the acceptability of a
food. The loss or retention of the food aroma during water removal is, therefore, one of the
major considerations in the design of any food concentration/dehydration process.
Selective water removal processes commonly used in the food industry can be divided
broadly into two classes: concentration and dehydration processes. The former includes
processes that increase solids content to about 50 to 60% (still in a liquid form) and the
latter those that reduce water content to less than 10% and the final product is in solids
form. These processes are listed in Table 10. The selection of any one of these processes
for removing water from a food product is primarily governed by the physical properties of
the form (liquid or solid), economics, and the desired quality of the final products.
B. Historical Developments in the Fruit Juice Concentration Industry

The historical aspects of the development and organization of the U.S. fruit juice industry
were recently reviewed by Sullivan and Tressler,83 and much of the following discussion is
based on this excellent article. Provost and Cutting were the first commercial canneries
established in the U.S. in 1859/1860. Both of these canneries packed fruits in glass and tin
and shipped them by vessels to eastern ports. In 1869, Welch began commercial bottling
of unfermented concord grape juice at Vineland, N.J. Although fruit juices were made long
before this date, it was Welch which first introduced the principles of heat sterilization for
long-term preservation of juices.
Nationwide expansion of commercial juice production in the U.S., however, did not occur
until the late 1920s. Home canning of fruits and vegetables became increasingly popular.
The commercial juice processing technology during this period centered upon the use of
overripe products that were not acceptable for whole-pack canning. Cloud stabilization of
the juices was a continuing problem and high quality products as well as desired long-term
preservation were still not achieved.
Substantial economic reorganization and technological developments in the 1930s led to
a large-scale expansion of the domestic fruit juice industry. Flash pasteurization of juices
was found to produce a more desirable, high quality product with better aroma, flavor, and
consistency than previous sterilization or pasteurization methods. The per capita consumption
of fruit juices in the U.S. increased from less than 0.45 kg in the early 1930s to over 9.0
kg by 1941. Increasing consumer dependence upon fruit juices as a source of vitamin C and
the introduction of enamel-lined cans, which permitted long-term storage of juices, also
contributed substantially to the industry growth.
Major breakthroughs in fruit juice processing occurred during World War II. Dried fruit
juice powders of lemon, orange, and grapefruit were first prepared for the armed forces
during this period by evaporating the water under vacuum. The introduction of frozen
concentrates during the 1945/1946 season had a tremendous impact on the juice industry.
By the late 1940s, over 60 to 70% of the U.S. orange crop was processed, with the largest
amount going for frozen concentrate production. Florida became the dominant force in the
marketplace, with over 80 to 90% of its crop now being processed into frozen concentrate.
On the other hand, the California orange industry has steadily declined in its market position
since the mid-1940s. Commercialization of freeze drying technology in the 1960s and that
of aseptic processing in the early 1970s also had a great impact. Substitute juice drinks were
first introduced in the mid 1960s, and since then they have been a major influence in
stabilizing levels of grapefruit and orange juice production.
As compared to concentration of liquid foods by evaporation, freeze concentration dates
back many years, although applied in a very elementary form. In Italy, when wines were
exposed to the environment in the cold winter months, freezing temperatures caused part of
the water in the wine to freeze, resulting in a concentrated product.73 "Vernette Lamotte"
was the first technique of industrial importance in which artificially produced cooling was
employed for concentration of wines. Early attempts at concentrating wines by freezing,
however, were neither practical nor economical from the industrial point of view, mainly
due to losses in alcohol, colorant, and cream of tartar. The Monti process, developed in
Italy in 1902, was probably the first one in which quality factor losses were reduced and
significant concentration achieved. Subsequently this technique was used for preparing fruit
juice concentrates, where the advantages of low processing temperatures were evident in
the quality of the final product.
The technique, however, still was not commercially viable. The major limitations of
earlier processes included relatively high investment costs, difficulties in effective separation
of ice crystals without loss of food solids, and a relatively low upper degree of concentration
that could be achieved by this method. Technological beakthrough such as the development
of multistage evaporators and aroma recovery by vacuum distillation made thermal evapo-
ration the best developed and economically the most favorable technique for the concentration
of liquid foods. Heat damage of the product and fouling of the heated surface in the
evaporator, however, are still major limitations of concentration by evaporation.
Recent renewed interest in freeze concentration is mainly because of potential savings in
energy. The past decade has seen considerable developments in technology that have min-
imized the major drawbacks associated with the earlier freeze concentration processes. These
developments were largely pioneered by Struthers Scientific and International Corporation
in the U.S. and by Grenco Special Applications, a Dutch company engaged in industrial
and marine refrigeration. The formation of large spherical ice crystals during concentration
at very slight super temperatures now makes it easier to separate them from the concentrate.
Accordingly, this new technique for separating ice crystals and concentrate avoids the loss
of concentrate and aroma volatiles with the ice. The solid losses have been reduced to less
than 100 ppm. New designs, in which the concentration and separation of ice crystals are
combined in one step, and multistage freeze concentration processes, have substantially
reduced investment and maintenance costs. Energy costs per ton of water removed by freeze
concentration are, therefore, considerably lower than those for the evaporation process. In
the following sections, these developments are discussed in detail.
III. CONCENTRATION PROCESSES
Concentration processes for fruit juices may be broadly classified based on whether
removal of water involves a phase change. Processes which require a phase change include
evaporation and distillation, pervaporation, and crystallization or freezing. In direct and

reverse osmosis processes, phase change of solvent is not required. Maximum separation
of water in evaporation and freezing processes is obtained at phase equilibrium. The rest
are typical nonequilibrium processes, and are based upon differences in velocity of equilib-
rium approach. Detailed descriptions of these processes including theoretical concepts, proc-
ess considerations, commercial designs, and suitability to different food products, are contained
in several excellent articles.l2-15-22-45-51-52-62-64-66-88-92-'06-107 In this section, some of these as-
pects of the various concentration processes are briefly reviewed.
A. Evaporation and Distillation

Evaporation is defined as the removal by vaporization of a part of the solvent (usually
water in case of food liquids) from a solution or dispersion of essentially nonvolatile solutes.51
The term "evaporation" is usually used when the resultant product is still in a liquid or
semisolid state.
Evaporation is probably the oldest method of concentration known to mankind. Some of

the most primitive methods of evaporation are still in use today. For example, the use of
solar ponds is still an economical means of salt production. At present, evaporation is
considered as the best developed, economically the most favorable, and the most widely
used method for the concentration of food liquids.51-90
For food liquids whose quality is not determined by their aroma composition, evaporation
may be conducted at the boiling point of the liquid. The quality of most food liquids,
however, is primarily influenced by their aroma characteristics. Almost all aroma and flavor
constituents of foods are low-boiling volatile compounds. Thus, they maybe removed prior
to effecting water removal or may be destroyed depending on their thermal stability. In
evaporation processes where the liquid is to be concentrated fourfold or more, the loss of
these compounds is almost directly proportional to the loss of vapor.90 Lower processing
temperatures are, therefore, required for such food liquids. The boiling point of these liquids
can be lowered by reducing the pressure. Such water removal at reduced pressure, and hence
at reduced temperature, is known as vacuum evaporation. Concentration of fruit juices by
vacuum evaporation is, however, still a severe process. Milleville and Eskew61 reported that
when apple juice was concentrated by heating under vacuum, the first 10% of the juice
vaporized contained all the volatile flavoring constituents. Commercially, fruit juice con-
centrates are, therefore, produced by first stripping their aroma volatiles in a distillation
column, followed by concentration in vacuum evaporator. The aroma concentrate is then
added back to the concentrate of nonvolatiles to yield a flavorful product. A much simpler
method to restore partly the quality of the final product is to add fresh juice to the concentrate.
The resulting dilution with "cutback" of fresh juice to the concentrate makes it impractical
to obtain products above fourfold the original strength.
Fruit juices contain both soluble (such as sugars and acids) and insoluble (such as fiber)
components and, therefore, cannot be defined as "true solutions". In such a system, the
thermodynamic properties of water deviate from those of pure water; therefore, the phase
diagrams for pure water cannot be applied directly for the purpose of calculating energy
requirements for the removal of water. To effect water removal, the total amount of energy
input necessary is governed by the following factors:
1. The initial temperature of the feed

2. Operating pressure in a particular system
3. The amount of water to be removed
4. The effect of the solubles and insolubles present in the feed on the thermodynamic
properties of water
5. Efficiency of a particular process design
Computing such energy requirements needs knowledge of process design and the equip-
ment used to achieve the desired degree of concentration. In simplistic terms, the minimum
energy required to transform unit mass of saturated liquid water to saturated vapor (at a
constant temperature and pressure) is equal to the enthalpy or the latent heat of vaporization.
Evaporation may be conducted in a batch or continuous mode depending on the need. In
food industry, the latter type is more commonly used. Most vacuum evaporators consist of
multistage units. The heating medium for each stage may be steam, water vapor from the
previous stage, or both. When water vapor from previous stage (boiling juice) is used as
heating medium to evaporate water from juice at a lower temperature, the process is known
as an "effect". As many as seven stages and four effects have been used to concentrate
orange juice. Several aspects of the types of evaporators used in the food industry have been
reviewed.15-51
1. Aroma Recovery in Evaporation Processes

The highly volatile constituents of fruits that are responsible for the characteristic aroma
of the fruit juices are present in only trace amounts. Since these aroma compounds are, in
general, more volatile than water, they may be lost either partly or completely if the vapor
is discarded during concentration of fruit juices by evaporation. The "cutback" process
used to restore partly the quality of concentrated juice was not suited for the production of
concentrates other than citrus juices. l5 With newer, improved technology, the volatile aromas
can be recovered by removing them from either the feed before evaporation or from the
vapor produced in the evaporator. These dilute aqueous aromas can then be concentrated
by distillation or freeze concentration and are returned to the concentrate of nonvolatiles
from the evaporator. Several reviews have described the aroma recovery systems available
for the production of flavorful fruit juice concentrates.15-22-89 The schematics of general
aroma recovery process are shown in Figure 3. A summary of the possible combinations
for aroma removal is given in Table 11.
B. Pervaporation
Fruit juices can be concentrated by using polymer membranes that show a selective
permeability to water.92 On a laboratory scale, such an approach has been shown to produce
juice concentrates without any appreciable loss in aroma quality.
Unlike other membrane separation processes, concentration by pervaporation involves a
phase change of solvent. The water on the vapor side of the membrane may be removed by
a current of relatively dry gas or by applying a vacuum well below the equilibrium vapor
pressure of the water in the membrane. The major advantage for such a process patented
by Thijssen and Paardekooper93 is the retention of aroma constituents of fruit juices that
otherwise would have been lost to the water vapor. However, high flavor retention is observed
only if the water concentration in the vapor side of the membrane is below 8%. Thijssen
and Middelberg92 have summarized the drawbacks associated with the pervaporation proc-
esses as follows:
1. High energy consumption, since the multieffect evaporation principle cannot be applied
to pervaporation (at least 1 kg of steam is required per kilogram of water removed)
2. Low dewatering capacity (approximately 2 kg of water per square meter membrane
area per hour)
3. Longer retention times in the process apparatus
4. High capital investments
C. Direct Osmosis, Reverse Osmosis, and Ultrafiltration

These membrane separation processes do not require a phase change, and can selectively
>• AROMA-RICH PRODUCT
DILUTE AROMA
AROMA CONC FNTRATIDN UNIT
t
1 »- MOSTLY WATER
1
1
1
FOOD _ STRIPPING AGENT
AROMA RFMflVAl CTCD —
(e.g., heat, inert gas,
or solvent)
CONCENTRATED SOLIDS
(for luther concentrating,
drying, or packaging)
FIGURE 3. Schematics of general aroma recovery process. (From Bomben, J. L., Bruin, S., Thijssen, H. A.
C , and Merson, R. L., Adv. FoodRes.. 20, 1, 1973. With permission.)
Table 11
AROMA RECOVERY PROCESSES22
Process Phase I Phase II Phase II formed by:
Fractional distillation (at- Liquid Vapor Evaporation

mosphere or vacuum)
Fractional condensation Vapor Liquid Condensation
Extraction with ether, liquid Liquid Liquid Second insoluble liquid
CO 2 , or other solvent
Liquid chromatography Liquid Solid Gel or solid column packing
Vapor chromatography Vapor Liquid Liquid coating on column
packing
Adsorption Vapor Solid Charcoal, molecular sieves
Gas stripping Liquid Gas Continuous addition of inert
gas
dewater several aqueous solutions at ambient temperatures. In direct osmosis, when water
solutions of unequal concentrations are separated, at equal pressures, by a semipermeable
membrane (ideally, permeable to water but impermeable to low molecular weight com-
pounds), water will pass from where it is concentrated to where it is more dilute, i.e., from
low-Brix solutions to high-Brix solutions. In general, because of the presence of solute
molecules, the chemical potential or activity of the solvent is lower in concentrated than in
dilute solutions. The high activity solvent, in turn, will tend to change into low activity
solvent so as to reduce the total free energy of the system. Such spontaneous transfer of
water occurs from the low to the high concentrated solution till the osmotic pressure of the
system equals the atmospheric pressure.
If pressure is applied to the concentrated solution in excess of its osmotic pressure, fresh
water flows through the membrane in the direction opposite to the normal osmotic flow.
Such a process is known as "reverse osmosis". This process has long been recognized as
Table 12
SOME POTENTIAL USES FOR REVERSE OSMOSIS IN FOOD
PROCESSING62
Concentration without flavor loss, e.g., apple, citrus juices, coffee, jams, jellies, essences
Economic water recovery, e.g., from brackish irrigation run offs, processors' effluents
Concentration without temperature rise, e.g., egg white, beer, fruit juices
Concentration that removes salt, e.g., molasses, whey
Concentration that removes acid, e.g., citrus juices, syrups
one that potentially could be operated at a high thermodynamic efficiency.75 Ultrafiltration

is similar to reverse osmosis, but uses a more porous membrane. Thus, in ultrafiltration
only large molecules are retained by the membrane, whereas most small solute molecules,
including salt, sugars, acids, and most flavor compounds, are lost to the permeate. The
process, therefore, has been limited to concentration and purification of biological com-
pounds, such as proteins. Several aspects of membrane separation processes were recently
reviewed.52
Concentration of fruit juices by direct osmosis has been limited to laboratory scale only.
A filter-press dialyzer has been developed by USDA to concentrate fruit juices, wines, and
coffee.l2 The water is removed from fruit juice or wine by dialysis into a hypertonic solution
of sodium chloride. Cellulose acetate membranes are used to produce concentrates free from
salt. An obvious advantage of direct osmosis process is that the dewatering can be performed
at low temperatures. In addition, it provides an easy method of preparing flavorful fruit
juice concentrates economically.
In addition to advantages such as low operating temperatures and selective dewatering,
the reverse osmosis process, from an energy point of view, is superior to all the other
concentration processes.6292 The only energy expended is the pumping of the juice to a
pressure adequate for reverse osmosis. The process has many potential uses in the food
processing industry (Table 12). So far, cellulose acetate membranes have been the preferred
choice for reverse osmosis processes. However, they have limited temperature and pH
capability. Therefore, the process has been restricted to low pressure/low temperature ap-
plications. Recently, the Reverse Omosis Division of Paterson Candy International, in Great
Britain, has developed noncellulosic membranes that are capable of operating at up to 80
bar pressure.14 According to the company, such high working tolerances overcome the high
osmotic pressure barrier of most fruit juices. In addition, the noncellulosic membranes have
a wide pH (3 to 11) and temperature (up to 80°C) range. The membrane also has good
separation and permeation capacity, and can be cleaned with caustic and acid cleaners at
high temperatures. A combination of ultrafiltration and reverse osmosis, using noncellulosic
membrane, has been used to preconcentrate apple juice prior to its concentration up to 72°
Brix in an evaporator. The schematics are shown in Figure 4.
The selection of any given concentration process is governed by several factors. However,
for fruit juices and liquids containing aroma volatiles, the concentration process has to be
highly selective. The relative energy consumption and economics of different processes also
influence the choice of method to be used. Freeze concentration is superior to many of the
processes described above and has great process flexibility as far as the applications to
different food products are concerned. In the following sections, several aspects of concen-
tration by freezing are described.
IV. THEORY BEHIND FREEZING CONCENTRATION
Freeze concentration involves partial freezing of the product and removal of the pure ice
crystals, thus leaving behind all of the nonaqueous constituents in the concentrated phase.
CONCENTRATING JUICE WITH REVERSE OSMOSIS
Sludge Press Dry Pomace

Enzyme
Press
Juice Condensate
Diffuser 1-2 Brix I
Permeate
UF
t
RO
Diffuser
n Plant Plant Evaporator
Juice
9-10° Brix
Centrifuge Aroma
Stripping
Concentrated
Apple Juice 4
Aroma
Sludger- 72 Brix
Stored
FIGURE 4. Combinations of ultrafiltration and reverse osmosis processes using noncellulosic membranes for
preconcentration of apple juice from 9 up to 16° Brix. (From Anon., Food Eng., p. 106, February 1983. With
permission.)
Although water constitutes more than 85% by weight of most fruit juices and other food
liquids, its properties differ greatly than those of pure water under identical conditions,
Some of the phase transition properties of pure water, under standard conditions, are sum-
marized in Table 13. These properties are greatly influenced by the type and the amount of
dissolved solids in water.
A simple phase diagram indicating the several physical states of water at equilibrium is
shown in Figure 5. Fennema and Powrie37 have defined a "phase" as a homogenous and
physically differing part of a system separated from the other parts of fixed borders. The
equilibrium conditions between the solid, liquid, and gaseous states of water are temperature
and pressure dependent. A state of equilibrium of ice, liquid water, and water vapor exists
only at the triple point with a pressure of 4.579 mmHg and a temperature of 0.0099°C
(Figure 5; Table 13). Below the triple point, the ice is directly sublimed into a gaseous state.
This forms the basis of the freeze-drying technology. As shown in Figure 5, water can exist,
under proper conditions of temperature and pressure, in 11 different physical states. These
include one each for liquid and vapor phases, and nine different crystalline solid phases.
The latter are the different high-pressure polymorphs of ice. Fennema36 has reviewed the
literature on the solid-liquid equilibria of water.
Separation by freezing is based on the difference in component concentrations between
solid and liquid phases that are in equilibrium. The phase transitions that occur in true
solutions can be analyzed fairly accurately based on the regularities of ice formation in
nonstructural systems. However, for multicomponent or pseudosystems, many generaliza-
tions have to be made. Guegov43 has summarized the most important phase transitions in
food products of plant origin that take place at low temperatures as follows:
WE Eufecfic concentration
o TE Eutectic temperature
TA Initial temperature of solution
WA Initial concentration of solution
Tf Freezing point of pure solvent
TA- Freezing point of solvent
wB Final concentration of solution
TB Final temperature of solution
o: Solution
u
a. and
Solute
Crystals
T^E-V
Solijd
wA wB wE
CONCENTRATION OF SOLUTE
FIGURE 6. Phase diagram for a simple binary system. (From Karel, M., in Principles of Food Science. Part II:
Physical Principles of Food Preservation, Karel, M., Fennema, O. R., and Lund, D. B., Eds., Marcel Dekker,
New York, 1975a, 265. With permission.)
1. Crystallization and melting (including the eutectic phenomena)

2. Vitrification
3. Glass (vitreous) transformation
4. Devitrification (crystallization) following glass transformation
5. Recrystallization preceding melting
6. Antemelting
The formation of ice in a simple, diluted binary (two-phase) system is accompanied by:
(1) the separation of water as pure ice crystals, (2) a progressive increase in the concentrations
of the dissolved substance, and (3) a gradual decrease in the melting point of the concentrated
solution. At eutectic temperature, both the unfrozen water phase and the substance dissolved
in it crystallize simultaneously in a fixed relationship, forming a mixed conglomerate (hy-
drate).4376-82 In multicomponent solutions, the dissolved solids crystallize out successively
according to their.eutectic temperatures. Unfrozen water is retained in the systems till the
lowest eutectic temperature becomes saturated.
Fruit juices are not "true" solutions, since in addition to water, they contain a large
number of soluble components. However, for reasons of simplicity, fruit juices are considered
as pseudobinary systems where all substances dissolved in water are considered as one
component.51
A simple phase diagram of a binary mixture is shown in Figure 6. If a binary mixture is
cooled from its initial temperature TA under conditions allowing equilibrium to be attained,
then a solid crystalline phase (pure ice crystals) begins to appear in the liquid phase. This
corresponds to composition WA and the freezing point T A ' in the phase diagram. Usually
only one component in the binary mixture crystallizes out in a pure form. Theoretically,
this allows a single-stage operation of the process, as compared to the incremental separation
and multistage processes required in vapor-liquid separations.
At the initial freezing temperature (TA') where the crystallization process begins, only
Table 13
PHASE TRANSITION PROPERTIES OF WATER46
Melting point at 1 atm 0.000°C

Boiling point at 1 atm 100.000°C
Critical temperature 374.15°C
Critical pressure 218.6 atm
Triple point 0.0099°C and 4.579 mmHg
Heat of fusion at 0°C 79.71 cal/g; 1.436 kcal/mol
Heat of vaporization at 100°C 538.7 cal/g; 9.705 kcal/mol
Heat of sublimation at 0°C 12.16 kcal/mol
°C °K
360 m
80
L ^ ^ ^
320
40 VII
280
0 IV -M
CD
240
\
•
JA I
-40 I
•
^ 1
CO
VI /
CD I
• I
a -80
200
'h'
1 :^
\ I
/
E I
CD
-120 160
*• '.
•
\
\
\ *
i
! VIII
-160 120 - I : ' \ '

i: IX \ : \ /
/: : \ /
i •
-200 80 \ . \ . . /
0 4 8 12 16 20 24
Pressure (kbar)
FIGURE 5. Phase diagram of water. (From de Quervain, M. R., in Freeze Drying and Advanced Food Tech-
nology. Goldblith, S. A., Rey, L., and Rothmayr, W. W., Eds., Academic Press, London, 1975, 3. With
permission.)
77.8
10 15 20 25 30 35 40 45
Concentrate to achieve
(% D.S.)
FIGURE 7. The percentage of feed to be removed from the feed in the form of pure water to achieve a certain
concentration level. (From Van Pelt, W. H. J., Bull. Grenco Special Applications, b.v., Netherlands, 1981. With
permission.)
small amounts of crystals are generated. As crystallization proceeds, the concentration of

liquid water in the solution will decrease. The dissolved substances will be concentrated
progressively in the liquid phase. This decreases the crystallization temperature of the re-
maining liquid; therefore, a lower operating temperature is required to effect further crys-
tallization. At this stage, the remaining liquid; therefore, a lower operating temperature is
required to effect further crystallization. At this stage, the liquid composition follows the
line [(CWA, T A ') (WB, TB)] in the phase diagram (Figure 6). It is apparent that for higher
conversions to the crystal phase, i.e., for effective ice separation, successively lower tem-
peratures are required. At eutectic concentration (WE) and temperature OV), the crystallizing
solid has the same composition as the supernatant liquid. Thus, at the eutectic, both com-
ponents crystallize out simultaneously. At this stage, removal of heat from the system
converts more of the liquid phase to solid, but at a constant temperature.
Theoretically, the concentration process can only be applied to a concentration just below
that of eutectic. However, in most cases, because of the problems connected with separating
ice from a very viscous liquid (both because of concentration and low temperature), it must
stop well below the eutectic. Generally, concentration can be carried to the point where the
slurry at the prevailing low temperature becomes too thick to be pumped. With the com-
mercially available equipment, it is possible to concentrate most fruit juices to about 50%
total solids content.66
The amount of water which must be removed from a solution to achieve a certain con-
centration level is shown in Figure 7. The data are for a feed solution containing 10%
dissolved solids. Muller66 has cited the following equation to arrive at the final concentration
value:
sucrose
coffee extract
apple juice
strawberry juice
blackcurrant juice
20 30 40
.solids concentration, wt %
FIGURE 8. Freezing point curves of sucrose, coffee extract, and some fruit juices. (From Thijssen, H. A. C ,
FoodManuf., 44(7), 49, 1969. With permission.)
«, _ c P - c f
where W; = pounds of water removed as ice per pound of feed; Cp = concentration of

solids in final product, pounds of solids per pound of product; Cf = concentration of solids
in feed liquid, pounds of solids per pound of feed; and Q = concentration of solids in water
removed, pounds of solids per pound of ice.
Since in most modem-day freeze concentration equipment the dissolved solids losses to
ice have been reduced to less than 100 ppm, for all practical purposes such losses can be
neglected. The above equation then becomes:
For the design and economic operation of freeze separation/concentration processes, it is

essential to obtain data on solid-liquid equilibria of the system. These data may be obtained
by techniques such as differential thermal analysis, differential scanning calorimetry, or
from electric resistance measurements.43 Experimental freezing curves have been determined
for several food liquids. One such example is shown in Figure 8. The freezing point for
black currant juice of 10% solids content is around — 2°C. On freezing to - 14°C, the solid
content of the liquid phase at equilibrium becomes 50 wt %, and consequently 90% of the
water originally present in the juice segregates as ice crystals. The freezing point curves,
therefore, can provide useful information on both the initial freezing points and heat capacity/
latent heat data. In many cases, high-recovery operations and eutectic formation can be
predicted from such data.
Nucleation is an integral phenomenon occurring during the freezing process that determines
the temperature at which crystallization is initiated. The process is initiated when a group
of molecules aggregates into particles of a certain order, called "nuclei" of crystallization
under suitable conditions.43 These conditions are determined by the correlation between
temperature, cooling water, solute concentrations, magnitude of forces orienting the mol-
ecules in the liquid, the movement or agitation of the cooled liquid, and the characteristics
of the border phase. The nucleation process is categorized as homogeneous or heterogeneous,
depending on how the nuclei of crystallization are formed. Homogeneous nucleation in-
volving the so-called "ice nuclei"69 occurs due to random aggregation of pure water mol-
ecules into ice structures. In the absence of any preformed ice or other foreign substances,
pure water has to be supercooled to a temperature less than - 39 to — 41°C before freezing
can set in.37-69 Heterogeneous nucleation occurs when solid substances that are usually
insoluble in water act as "ice-forming nuclei" or "freezing nuclei". Heterogeneous crys-
tallization thus always occurs at temperatures higher than those required for homogeneous
crystallization, and occurs without exception during the freezing of all foods. The maximum
limit of supercooling in such a system usually does not exceed 6.6°C in model systems, and
the supercooling temperature of plant tissues cannot be lower than —5 to — 10°C.37
The type of crystal structure and its size primarily determine the solids losses that may
occur during concentration. Improper crystallization during freezing can cause solids losses
up to 20%." The success and efficiency of the modern-day freeze concentration processes
may largely be attributed to realizing this important phenomenon. Ice crystal size during
freezing may be controlled by properly monitoring several process variables, the foremost
being the degree of supercooling.
As mentioned earlier, the aqueous liquids have to be supercooled below their true freezing
points to initiate crystallization. This is the primary driving force responsible for the growth
of existing crystals and for the formation of new crystal nuclei. The supercooling phenomenon
for model food systems has been extensively investigated by Thijssen and co-workers. Their
investigations suggested that the mean residence time required to obtain a certain mean
crystal diameter is inversely related to the bulk supercooling. In addition to the residence
time and the bulk supercooling of the liquid in the suspension, agitation rates and the dissolved
solids concentration also influence the mean crystal size.90-91
From a separation point of view, the formation of a few but large ice crystals is desirable.
Very high supercooling can create a large number of smaller new crystals. Lower rates of
supercooling are, therefore, desirable to prevent excessive nucleation. A decrease in the
bulk supercooling of the liquid with increasing residence times and at a constant crystal
concentration linearly influences the ice crystal size.91 At any given rate of heat withdrawal
per unit mass of suspension, the high supercooling required for high ice crystal growth rates
can only be maintained if the total surface area of the crystals per unit mass of suspension
is small. Thus, lower nucleation rates are required to produce reasonably large ice crystals
at an acceptable residence time. Thijssen90-91 suggested increasing the agitation rates, within
certain limits, to lower the nucleation rates. However, it must be noted that very high mixing
rates may promote nucleation due to mechanical damage. Based on their studies on ice
crystallization and nucleation, Thijssen and co-workers developed "ripening" types of crys-
tallizers in which the larger ice crystals grow at the expense of the smaller ones. These type
of crystallizers are described in the following section.
Thus, over the past decade, the understanding of the basic phenomena behind ice nucleation
and crystallization has resulted in newer, improved freeze concentration processes. The
losses of dissolved solids due to occlusion in the ice crystals have been considerably min-
imized. The now possible formation of large, fairly spherical ice crystals by properly con-
trolling the process parameters also facilitates adequate and efficient ice crystal washing and
separation operations. These operations and the equipment required are discussed in the
following section.
Crystallizers
I
Directly cooled Indirectly cooled
(Vacuum crystallizer)
I I
Internally cooled Externally cooled
I
I
Suspension Layer
crystallizer crystallizer
Ripening Supercooled feed

crystallizers
I I
Liquid recirculation Suspension recirculation
FIGURE 9. Classification of crystallizers used in freeze concentration processes. (From Van Pelt, W. H. J.,
Bull. Grenco Special Applications, b.v., Netherlands, 1981. With permission.)
V. EQUIPMENT
A typical freeze concentration system consists of three fundamental components: a crys-

tallizer, a separation device, and a refrigeration unit. The heart of the system is the crys-
tallization section (also referred to as "freezer", "freezing cabinet", or "chiller"). In the
crystallizer section, ice crystals are produced by removing the necessary heat from the process
fluid. Sometimes an additional crystal growing tank may also be employed.66-91 In the
separation section or the "crystal purifier", the ice crystals are separated from the unfrozen
concentrate and washed with a part of the melted product to wash off any adhering solids
from the crystal surfaces. A refrigeration unit is required to remove the heat of crystallization
from the freezer. It also takes out heat during prechilling of the feed and frictional heat
resulting from hydraulic flow, wall scrapings, and agitation of the slurry. The heat may
either be transferred to cooling water or melt the ice crystals separated in the purification
system. Based on the design, a heat exchanger may often be employed to precool the feed
by using the cold product and the concentrate, thereby reducing the load on the freezer.
Several aspects of this topic have been recently reviewed by Thijssen.91 Commercially
available designs of these equipment are discussed below.
A. Crystallization Section
Almost all the freeze concentration processes developed for concentrating the food liquids
employ indirect-contact crystallizer designs. In these designs the evaporating refrigerant or
coolant is separated from the process fluid by a rigid metal wall, thus eliminating any
problems associated with refrigerant toxicity. The direct-contact crystallizers, which allow
intimate mixing of the refrigerant with the process fluid, are widely used for nonfood
Wet
compressor
Atmospheric
pressure
Water vapour
+
oromo ..
2 mmHg
Feed
Ice
Vacuum separator
crystallization Concentrated
liquid
TIce
FIGURE 10. Flowsheet of a vacuum crystallizer with aroma recovery. (From Thijssen, H. A. C , in Freeze
Drying and Advanced Food Technology, Goldblith, S. A., Rey, L, and Rothmayr, W. W., Eds., Academic Press,
London, 1975, 481. With permission.)
applications, such as sea water desalination and for concentrating and separating chemical
solutions. A general classification of the various types of crystallizers is shown in Figure
9.
1. Direct-Contact Crystallizers
In the direct-contact crystallizers, water vapor itself can be used as the primary refrigerant.
This, however, requires operation of the crystallizer under high vacuum, and compressing
large volumes of vapor at lower pressures. Based on the method by which the vapors are
removed, these may be further classified as: (1) vacuum-freeze, vapor-compression systems,
(2) absorption-freeze, vapor-compression systems, and (3) vacuum-freeze, ejector-absorption
systems. To eliminate problems associated with high vacuum systems, secondary refrigerant
cycles using refrigerants such as freon or butane may be used to facilitate operation of the
crystallizer under normal (near atmospheric) conditions.
Direct cooling of the incoming feed by contact with the refrigerant has some distinct
advantages over indirect cooling.91 It eliminates the cooling wall, which reduces the rate of
heat transfer, and consequently the use of expensive scraped-surface heat exchangers. Con-
siderable energy savings can be achieved by properly controlling the process parameters.
For example, Aackter and Barak1 have reported power requirements as low as 8 kWh/1000
kg ice removed for large evaporation plants with vapor compression. Vacuum-freezing,
vapor-compression systems have been used extensively for seawater desalination.45-66-91
The advantages of low capital costs and low energy costs, particularly in case of vapor-
compression systems, are somewhat offset by the lower quality product obtained as compared
to the quality of concentrate obtained from indirect-contact crystallizers.91 Ordinary vacuum
crystallizers are not suited for products whose quality is primarily determined by their aroma
composition. The aromas can be lost with the vapors leaving the vacuum crystallizer.
Thijssen91 has described a design for a vacuum crystallizer with aroma recovery (Figure
10). In this design, the gas-vapor mixture leaving the condenser is stripped countercurrently
in an aroma absorber with the concentrated liquid leaving the ice-concentrate separator. If
the temperature of the condensers is maintained properly and by recirculating a part of the
noncondensables leaving the first section of the aroma absorber through the condenser, the
condensation of the aromas in the condenser can be prevented. Thus, aromas will be removed
only from the gas-vapor mixture by the liquid in the aroma absorber. Using such a design,
with most fruit juices aroma losses could be reduced to an organoleptically barely detectable
level.
2. Indirect-Contact Crystallizers
The indirect-contact crystallizers have been in wide use in food applications. 6691107 Based
on the method of heat removal, these types of crystallizers can be categorized into two
groups (Figure 9). In the internally cooled crystallizers, the heat of crystallization is removed
through the wall of the crystallizer. The externally cooled crystallizers operate on the adiabatic
principle, in which the heat is removed outside the crystal growth section.
a. Internally Cooled Crystallizers

Based on how the crystallization process is allowed to proceed, these types of crystallizers
are further classified into two categories: the layer crystallizer and the suspension crystallizer
(Figure 9). In layer crystallizers, the unagitated feed is allowed to come in contact with a
refrigerated wall which produces a solidified layer. It can either be washed in situ or
mechanically removed as solid slab or "snow", and separated elsehwere.91-107 The Linde-
Krause crystallizers, consisting of a large stainless-steel drum, internally refrigerated, and
rotating in a trough of the feed liquid, operate on this principle. The solid layer formed
during freezing is continuously scraped off. In some designs, the liquid is sprayed onto a
slowly revolving drum or internally refrigerated discs, and is then removed as flaked ice. 5 - 9 1 "
Although these types of crystallizers are capable of concentrating even dilute solutions to
40% by weight or more, the formation of very small ice crystals presents difficulties.
The second group of internally cooled crystallizers produces pumpable slurries. Both
horizontal and vertical tubular heat exchangers with or without scrapers may be used and
depending on the process, the residence times for crystal suspensions may vary anywhere
from a few minutes to several hours.3I-38-6466 One of the modifications of this design,
developed by Struthers Scientific, utilizes an agitated but nonscraped indirectly cooled
crystallizer. The aim is to avoid the formation of an excessive number of small ice crystals.66
Large crystals are produced in this design by properly controlling the temperature difference
across the wall, turbulence, and crystal concentration. In most of these designs, the nucleation
process begins at the wall surface, whereas the crystal growth takes place in the bulk of the
suspension.
b. Externally Cooled Crystallizers

Externally cooled crystallizers are further subdivided into three types:
1. Crystallizers in which the incoming feed is supercooled

2. Crystallizers recirculating the whole suspension to the heat exchanger
3. Crystallizers using an external heat exchanger to produce subcritical crystals
In the first type of crystallizers, the liquid is supercooled which, to a large extent, takes
out the heat of crystallization. The primary aim is to avoid heterogeneous crystallization
within the crystallizer. The inside wall of the heat exchanger has to be highly polished or
coated with a hydrophobic plastic to minimize changes of primary nucleation and crystal-
lization within the heat exchanger.91-94 With this type of crystallizer, local supercooling of
the feed is virtually eliminated.
REFRIGERANT RECRYSTALLIZER
SLURRY WITH SUBCRITICAL
llN OUT| AND SUPERCRITICAL
CRYSTALS SUSPENSION
FEED WITH
PRODUCT
CRYSTALS
SCRAPED HEAT
EXCHANGER
FILTER
CRYSTAL
FREE RECYCLE
FIGURE 11. Schematics of the Grenco "ripening" type crystallizer. (Fom Grenco Catalogue, Grenco Special
Applications, b.v., Netherlands. With permission.)
In the second type of crystallizer, the entire feed is recirculated from the crystallizer to
the heat exchanger. The residence time of the crystals in the heat exchanger is generally
short compared to that in the crystallizer.91 The longer residence time in the crystallizer
allows proper crystal growth.
The last type of externally cooled crystallizers can be considered as "second-generation"
crystallizers, since the nucleation and crystal growth sections are separated.107 A feed heat
exchanger is used to produce very small ice crystals. The very high heat flux through the
walls of the scraped heat exchanger induces a very strong nucleation. This in turn limits the
residence times to only a few seconds. The slurry containing the small ice crystals is then
fed continuously to a "ripening" crystallizer. Ripening is based on the fact that smaller ice
crystals melt at a lower temperature in a solution than the larger ones.107 Thus, when small
and large ice crystals are mixed in suspension, the mean bulk temperature of the liquid
settles down to a value between the extreme values of the various melting temperatures of
the crystals and nuclei. Since the mean average temperature is higher than the melting
temperature of the small crystals, they melt. This results in a driving force for the growth
of the larger crystals and for the melting of the smaller crystals. The size of the melting
crystals in an adiabatic crystal suspension is called subcritical and the growing ones are
known as supercritical.42 The development of the ripening crystallizer is credited to Thijssen
and co-workers, and it is commercialized by the Grenco Special Applications b.v. The
schematics of such a crystallizer used by Grenco in their process are outlined in Figure 11.
In a continuous operation, the subcritical crystals or "nuclei" are produced in a heat ex-
changer external to the recrystallizer. The extremely small crystals with a residence time of
a few seconds are continuously fed and mixed with the suspension in the recrystallizer. At
steady-state operation, the ice crystal size ranges from 0.2 to 0.3 mm. The small subcritical
crystals melt almost instantaneously, thereby providing the heat of crystallization of the
growing large crystals. The two technical concepts based on this process involve a crystal-
free recirculation design, in which a crystal-free solution is fed to the heat exchanger, whereas
in the suspension recirculation design, a part of the concentrate containing the ice crystals
is recirculated.42-107 Ice crystals of diameters varying from 0.5 to 1.0 mm can be produced
in such a crystallizer, based on the type of feed and by varying the residence times.
B. Separation Devices
Ice crystal separation from the mother liquor is probably the key factor that influences
the dissolved solids losses most. The failure, on a commercial scale, of the freeze concen-
tration processes may largely be attributed to this one process parameter, particularly in
concentrating aroma-rich liquids. Several separation devices have been tried, both on pilot
plant and commercial scales.
Several factors affect the ice crystal separation efficiency, the foremost being the viscosity
of the slurry and the ice crystal diameter. The capacity of all separation devices is inversely
related to the viscosity of the slurry and is directly related to the square of the mean diameter
of the crystals. Van Pelt107 cites the following equation for the superficial velocity of a liquid
through a packed-bed column:
E3 • d2 • 0 2 1 dP
~ 180 ( 1 - E ) 2 ' u / d Z
where V = superficial liquid velocity; E = volume fraction of liquid; dp = particle diameter

of the crystals; 8 = shape factor of the crystals; \L = dynamic viscosity; and dP/dZ =
pressure drop along the packed bed.
Thus, for all the separation devices, the separation becomes easier with larger crystals,
and at lower viscosities. In addition, for filtering centrifuges, the gravity factor, and for the
presses, the pressure differential (dP/dZ) exerted along the bed by compression, must be
taken into account.107
1. Wash Columns
Wash columns have been successfully used for both separating the crystals produced in
the crystallization section as well as purifying them. They are classified as the flooded
column and the drained column.107 The drained columns have been used in desalination
processes and are three-phase systems. The presence of a gas phase, in addition to the crystal
and liquid phases, is undesirable in case of food liquids, largely due to oxidative changes
and losses of aroma compounds.
The flooded wash column was first developed by the Phillips Petroleum Company to
separate xylene isomers, and later tried for liquid foods.56-58-60107 Later on, Thijssen devel-
oped a flooded wash column, especially suited for food applications at the Eindhoven
University of Technology, Netherlands which is commercially used in the Grenco freeze
concentration processes. The schematics of such a wash column are shown in Figure 12.
The ice crystal slurry is fed to one end of the column, and the mother liquor withdrawn
from the same side. The compacted ice bed is forced towards the other end of the column,
where it is melted by means of a grid of internally heated pipes. The melt water is used to
wash the crystals moving countercurrently in the column. Approximately 90 to 95% of the
melted ice is removed from the column, and the rest is recirculated as wash water. The
solids losses to melt water are usually less than 100 ppm. The Grenco wash columns have
a capacity of 3,000 to 10,00 kg/hr ice removal per square meter cross-sectional area of the
column, depending on the ice crystal size and the viscosity of the slurry.42
A major advantage of the wash columns is that since they are operated without a gas
phase, aroma losses are virtually eliminated. Similarly, based on design, a perfect ice crystal
and liquid separation can be obtained without any dilution effects. The formation of relatively
uniform and large (>0.2 mm) crystals is essential for the efficient operation of wash col-
umns.45 Similarly, in many cases, the upper limit on crystal content cannot be over 15 to
A B
FIGURE 12. Schematic representation of a flooded

wash column. A = slurry coming from crystallizer; B
= mother liquid (concentrate); C = ice crystals in mother
liquid; D = wash front; E = ice crystals in pure crystal
melt; F = melter; and G = pure water. (From Thijssen,
H. A. C , in Freeze Drying and Advanced Food Tech-
nology, Goldblith, S. A., Rey, L., and Rothmayr, W.
W., Eds., Academic Press, London, 1975, 481. With
permission.)
20% for the slurry to remain pumpable. In such cases, the column has to remove a great
deal of liquid. Wash columns have been the most successful method for separating ice
crystals from low viscosity liquids and have found many applications in seawater desalination
and in the concentration of beer and wines. The theoretical concepts behind wash column
designs were recently reviewed. 8991107
2. Centrifuges
The filter centrifuges are preferred wherever high viscosity liquids are encountered. They
also have been used for crystal separation in xylene fractionation systems.45 Both batch types
Pure ice
876 kg h"1
Wash
coiumn
Crystallizer
1914 Kg h"1
(24°/' ^
(50-0%)
876 kg h ice ice
1914 kg h' liquid — susDension
(24%)
; 1
/ 333 kg h"
1 1
•^ Concenrraie
1 1 (50-0%)
I 1
Press
_L 1
8 7 6 kg rT ice — Ice cone

ice
coke 584 kg h"1 liquid
mixer
(50 0%)
FIGURE 13. Schematic representation of a typical combination of a press and

a wash column. (From Thijssen, H. A. C , in Freeze Drying and Advanced Food
Technology. Goldblith, S. A., Rey, L., and Rothmayr, W. W., Eds., Academic
Press, London, 1975, 481. With permission.)
and continuous types are in use.66-8991 The filtration capacity of filter centrifuges is strongly
dependent upon the shape factor of the crystals, the mean crystal size, the liquid viscosity,
and the gravity factor.22-91107 Centrifuges can provide forces up to 1000 X G, which forces
even viscous liquid off crystal surfaces. Some mother liquor, however, may still remain
adhered to crystals due to surface forces. Since the centrifugal ice bed is less densely packed
than in the case of presses, the solids losses can be minimized by washing of the filter cake
with water or crystal melt prior to their discharge to melter condenser. The spent wash water
is then returned to the crystallizer if solids are to be recovered. The possibility of washing
of filter cakes renders centrifuges more efficient than presses. The recirculation of spent
wash water, however, dilutes the concentrate or it may have to be treated separately. A
serious disadvantage of centrifuges is the aroma loss, since they must be operated with a
gas head space into which the volatiles can escape.22-89"91-107
3. Presses
Filter presses have proved less effective for crystal separation. Both hydraulic piston and
screw presses are in use. The loss of dissolved solids is primarily determined by the amount
of liquid that remains occluded in the compressed ice cake.22-8991 Depending on the con-
centration of the liquid and the size of the ice crystals, the amounts of occluded liquid can
vary between 0.03 and 0.1 kg/kg of compressed ice.53 Dissolved solids cannot easily be
removed by a wash process even after grinding the cake. The presses are, therefore, employed
for systems with a low concentration ratio, such as increasing the alcohol content of wines
and beers and to certain fruit juices. 74100
4. Combination of Separation Devices

Combinations such as centrifuge and wash column or a press coupled with a wash column
may also be employed for separating the ice crystals from the mother liquor.45-91 For sep-
arating eutectic crystals, it may be necessary to use the centrifuge, followed by reslurrying
of the crystals in a wash column. Ice crystals of different densities can be separated hy-
draulically. Scroll centrifuges have been used for fractional separations based on relatively
small differences in specific gravities, particularly in the chemical industry.45
In many cases, the most economical process can be obtained by a combination of a press
and a wash column." A typical arrangement is shown in Figure 13. The concentrated slurry
leaving the crystallizer is partly separated in a press. The ice cake still containing a substantial
amount of the occluded concentrate is then redispersed in the feed to the system. The diluted
ice suspension is then completely separated in a wash column, and the liquid separated from
the ice is fed back to the crystallizer. With the arrangement shown in Figure 13, the capacity
of the wash column can be increased by a factor of 8.3, since a less concentrated liquor is
being fed to a wash column. This in turn lowers the viscosity of the liquid, thereby increasing
the separation efficiency of the wash column. Thijssen91 cites another important reason for
using such a combination system. Slurries containing ice crystals of too small a mean diameter
or a high viscosity or both do not satisfy the stability criteria of a wash column, and thus
cannot be separated efficiently using a wash column. In such cases, a combination of press
and wash column can perform efficient separation of the ice crystals from the mother liquor.
C. Refrigeration Unit
As mentioned earlier, a refrigeration unit is required to remove the heat of crystallization
during freezing and frictional heat resulting from hydraulic flow, wall scrapings, and agitation
of the slurry. Much of the refrigerant vapor, in turn, can be condensed at low temperatures
by melting the ice crystals. Either direct-contact or shell-and-tube devices can be used.45
The direct-contact condensers are used only with direct-contact crystallizers. In the indirect-
contact systems, the refrigerant remains isolated from the process fluid. Even in some direct-
contact applications, the use of an indirect melter condenser may be mandatory, particularly
where high product purity is desirable or when, due to solubility, excessive refrigerant losses
occur.
The mathematics of the performance of refrigerating unit in freeze concentration systems
have been recently reviewed by Van Pelt.l07 From an energy consumption viewpoint, smaller
differences between the evaporating and the condensing temperatures of the refrigerating
equipment are desirable. This can be achieved by two means. The condensation temperature
of the refrigerating unit can be lowered by using the heat of melting of the ice crystals. On
the other hand, utilizing the heat at the highest evaporation temperature of the refrigerating
unit can effectively lower the driving force for heat exchange. This is strongly dependent
on the type of product and concentration ratio.
VI. COMMERCIAL FREEZE CONCENTRATION PROCESSES
Based on the type of crystallizer used or the freeze-refrigeration cycles employed, freeze
concentration processes are broadly divided into two categories: direct- and indirect-contact
processes.
A. Direct-Contact Processes
In direct-contact processes, the feed is allowed to come into contact with the refrigerant.
Heist45 has classified these processes as follows:
1. Direct-Contact, Triple-Point Processes

The triple point of a substance can be defined as that temperature and pressure at which
its vapor, liquid, and solid phases are in equilibrium. The triple point of water is 4.58 Ton-
pressure and a temperature of approximately 32°F. For an equilibrium to exist, the partial
pressure of water in a solution containing ice crystals must be equal to the vapor pressure
of ice crystals. The removal of vapor from such a solution does not lower the temperature.
It, however, further concentrates the solution by crystallizing out a part of the water. As
the process continues, the solute eventually reaches or exceeds its saturation concentration
and simultaneous crystallization of ice and solute becomes possible. The temperature at
which a crystallized solute can exist in equilibrium with ice and the unfrozen phase has been
variously described as the "eutectic point" or "eutectic temperature" of the solute. The
term "cryohydric" is sometimes used in place of "eutectic", when water is the solvent.
Direct-contact, triple-point processes are further subdivided according to the method by
which the vapors are removed.
Vacuum-freeze, vapor-compression — In this method, a mechanical compressor is used
to remove the vapor phase. The vapor is compressed so as to permit it to condense either
directly as pure crystals or on a heat-transfer surface.
Absorption-freeze, vapor-compression — The vapors are absorbed in a material that
has a vapor pressure below the triple point. In this method, the absorbent has to be regen-
erated, i.e., the absorbed vapors have to be taken out of the system to keep the vapor pressure
sufficiently low. A conventional refrigeration cycle can be used to provide the heat necessary
to drive off the absorbed vapor.

Vacuum-freeze, ejector-absorption — This method uses two mechanisms to remove the
vapor: an absorption cycle and a low-pressure steam ejector. The steam that drives the ejector
is also used to regenerate the absorbent. The ejector acts as a thermal compressor to raise
the quality of the removed vapor so that the vapor can be condensed. The primary advantage
of direct-contact, triple point processes is that the water vapor itself can be used as the
primary refrigerant. This, however, necessitates operation of the unit (crystallizer) under
high vacuum and compressing very large volumes at low pressures. Consequently, energy
costs can be substantially higher. Commercially available direct-contact processes, therefore,
employ secondary-refrigeration cycles.
2. Direct-Contact, Secondary-Refrigerant Cycles

In these processes, a secondary refrigerant such as a synthetic organic halocarbon (freon)
or a volatile hydrocarbon (e.g., butane), is directly injected in liquid form into the process
liquid in the crystallizer. This provides a near-atmospheric pressure in the crystallizer under
normal operating conditions. Since the pressure of the system is less than the vapor pressure
of the refrigerant, the refrigerant boils up, removing heat from the process liquid and causing
crystallization. A mechanical compressor is used to raise the pressure of the refrigerant to
a point at which the refrigerant can be condensed by either cooling water or melting crystals.
These processes can be subdivided further based on the type of refrigerant used, and the
way in which it is mixed with the process liquid.
The secondary-refrigerant processes overcome some of the problems encountered in the
refrigeration cycles of triple-point processes. In the latter, with a vapor-compression cycle,
the volumes to be handled at the triple point are relatively large, and the adiabatic head
requirements often need a multistage compressor. In the absorption cycle of a triple-point
process, any nonabsorbable volatile material present in the process fluid will build up in the
vapor space and inhibit the mass transfer between the process fluid and the absorbent. Thus
the system works only when all volatile materials are absorbed. In the secondary-refrigerant
processes, refrigerants can be selected to yield desired pressure at the freezing conditions.
Both direct-contact, triple-point and secondary-refrigerant processes have been tried suc-
cessfully on a pilot-plant scale, in the desalination of seawater (Tables 14 and 15). The
lower energy requirements as compared to that for distillation, and high production rate at
low capital and operating costs, make these processes especially suited for seawater desal-
ination. The direct-content processes, however, cannot be applied for the concentration of
liquid foods because of the possibility of damage to the product by contact with the refri-
gerant.22-66 Most refrigerants are soluble to some degree in the process liquids and this may
Table 14
VARIOUS FREEZE CRYSTALLIZATION SYSTEMS, APPLICATIONS AND
UNIT SIZES45
Refrigeration Crystal Size

Freezer type cycle separation Washing Application (Ib/d)
Direct-contact, triple- Triple-point Wash column Yes Seawater 750,000

point vapor compression compression
Direct-contact triple-point Triple-point absorp- Wash column Yes Seawater 50,000
tion cycle
Direct-contact, secondary Vapor compression, Wash column Yes Seawater 600,000
refrigerant fluorocarbon
Vapor compression, Wash column Yes Seawater 20,000
butane
cause toxicological and food safety problems. Some of the direct-contact freeze concentration
processes, commercially made available in the 1960s, are described below.
a. Carrier Process
Designed and built in 1960 by Carrier Corporation of Syracuse, N.Y., this was the first
freeze concentration desalination plant of appreciable size built in the U.S. 3435 - 64 The first
pilot plant built at Harbour Island, Wrightsville Beach had a capacity of processing 15,000
gal of seawater per day and used flashing water itself as refrigerant in the crystallizer.
A flow sheet of the Carrier process is shown in Figure 14. The incoming sea water is
first deaerated, cooled, and then fed to a direct-contact crystallizer. A constant pressure of
3 mm of mercury is maintained in the crystallizer by means of steam ejectors. The lowering
of temperature to about 25°F due to evaporation of water vapor causes ice crystallization.
The resulting ice-brine slurry is then pumped into the bottom of a separation column. There
the ice crystals are compacted into a bed which is carried upward by the brine. As it moves
upward, the ice bed is washed by 5% or less of fresh water. When the bed reaches the top
of the column, the crystals are scraped off into a tank and melted to form fresh water. A
concentrated lithium bromide solution is used to absorb the water vapor drawn off the
crystallizer. The resulting dilute absorbent is reconstituted in a generator by distillation. This
process yields a fresh water product containing less than 350 ppm dissolved solids and uses
wash water amounting to less than 5% of the production.
The original plant was dismantled in 1963, apparently because of difficulties encountered
in the refrigeration cycles of the triple-point process. Economics also played a role. Later,
the Carrier Corporation concentrated its efforts on freeze desalination processes using a
fluorocarbon R-C 313 as a secondary refrigerant.70-71
b. Blaw-Knox Process
This process was designed and developed by the Blaw Knox Company of Pittsburgh, Pa.
in 1960. The original pilot plant had a desalinating capacity of 35,000 gal/day. The process
uses a secondary refrigerant cycle with butane as refrigerant.64-71 A direct-contact heat
exchanger is employed both in the crystallizer and the melter condenser. Conventional shell
and tube designs are used for the auxiliary condenser and the heat exchanger. In this process,
all streams are recirculated, with no deaerator, debutanizers, or product water fillers provided.
The ice crystal-brine slurry is separated in wash columns. The ice crystals are compacted
at the bottom of the column and the ice bed thus formed is moved upward by the hydraulic
piston effect of reject seawater flowing up through the bed and exiting through screens near
the top. At the top of the column, the ice crystals are scraped off into a melter condenser
and are then melted by condensation of the compressed butane vapors to form drinking
water.
Table 15 to
o
a
CHECKLIST OF FREEZE CRYSTALLIZATION PROCESSES THAT HAVE BEEN TRIED ON PILOT PLANT OR
COMMERCIAL SCALE4S
Freezers/refrigerators
8
Triple point Crystal separation
Vapor Steam Secondary refrigerant Wash

Melting
I
compression ejector Absorption Butane R-114 R-C3i8 Centrifuge column Direct Indirect Process name Status
X X Brodie purifier Six installations worldwide,

all on organic separations
Phillips crystallizer Several xylene separation
installations
Kureha crystal purifier Two installations on organic
X X Vacuum freeze, vapor 100,000 gal/d plant for Office
compression of Saline Water (OSW) in late
1960s by Colt Industries
Vacuum freeze, ejector 6,000 gal/d bench-scale plant
absorption built for OSW in late 1960s a.
by Colt Industries
X X Absorption freeze, vapor 25,000 gal/d sewer pilot plant
compression now being built for Office of
Water Research and Tech-
nology (OWRT) by Concen-
tration Specialists
X Immiscible refrigerant freez- 10,000 gal/d seawater bench-
ing process scale unit built for process
development by U.K.
Atomic Energy Authority
X X Secondary refrigerant freez- 15,000 gal/d seawater plant
ing process built for OSW in late 1960s
by Carrier Corporation
X X Crystallex 75,000 gal/d seawater plant
built for OSW in early 1970s
X X Direct-freeze separation Bench-scale tests for OSW in
process mid-1960s by Avco
WASH WATER
FIGURE 14. Carrier freeze desalination process using fluorocarbon refrigerant Re-318. A = product stripper;
B = brine stripper; C = auxiliary compressor; D = flash precooler; E = main compressor, F = freezer; G =
receiver-decanter; H = melter; I = auxiliary refrigeration; and J = separation column. (Redrawn from Muller,
J. G., Bull. Inst. Int. Du Froid 46, Annexe 3, 1966a, 15. With permission.)
c. Fairbanks Morse Process

This freeze desalination process was developed by the Fairbanks Morse Division of Colt
Industries, Inc., Beloit, Wis. in cooperation with the Government of Israel.33 The process
is based on a direct-contact, triple-point vacuum freeze-vacuum compression principle. The
sensible heat and the heat of crystallization are removed from the crystallizer by evaporating
the water vapor from the brine under high vacuum conditions. The resulting ice crystal-
brine slurry is separated in a wash column. A large compressor is used to raise the pressure
of the water vapor to permit condensation by direct contact with the washed ice crystals in
a separate melter condenser vessel. The plant constructed in Israel had a desalination capacity
of approximately 250,000 gal/day.
d. North American Aviation Process

This process was developed by Rocketdyne, a division of the North American Aviation
Corporation and tried on a pilot plant scale at Oxnard, Calif, in 1962.64 The 20,000 gal/day
capacity plant employed butane as a secondary refrigerant and wash columns were used to
separate the ice crystals from the brine. Later on, the process was acquired and further
developed by the Struthers Scientific and International Corporation, Washington, D.C.
e. Struthers-Umano Process
This process was developed by the Struthers Scientific and International Corporation,
Washington, D.C. and its basic design was used for the two pilot plants constructed by the
Office of the Saline Water, U.S. Department of the Interior at its test facility in North
Carolina.64-68-70-79-98 The two pilot plants had capacities of 15,000, and 20,000 gal/day. The
schematics are shown in Figure 15.
Briefly, the process is as follows. The incoming seawater is first deaerated and filtered.
!>EA WATER
D
4 1 4
A t | j |- J i t
C - F 1
PRODUCT
WATER
1
TE BRINE
-Ij 1 1 - - 11L - 1
t
\ 1
1
r 4 1
i <
IC
i LU
I
Ii CHILLED SEA WATER £ BUTANE LIQUID
J
t
sii
s m
"*~ 1
B T
1,
EXCHANC
1
HEAT
* E H
1
1 BRINE
PRODUCT WATER
J
T
FIGURE 15. Struthers-Umano freeze desalination process (single-stage plant). A = debutanizer; B = heat
exchanger; C = filter; D = deaerator; E = ice crystallizer; F = main compressor; G = auxiliary condenser; H
= centrifuge; I = auxiliary compressor, and J = melter condenser. (Redrawn from Muller, J. G., Bull. Inst. Int.
Du Froid 46, Annexe 3, 1966a, 15. With permission.)
It then passes through a heat exchanger cooled by the outgoing brine and the product, fresh
water. The chilled seawater (about 35°F) then flows into the crystallizer. Further sensible
cooling down to about 26°F and ice crystal formation occur in the crystallizer. The basic
design of the crystallizer consists of a horizontal cylindrical vessel containing seawater brine
and butane as refrigerant. The ice crystals formed in the crystallizer are then pumped along
with the brine to a wash column. The crystals are scraped off from the top of the column
and melted in a melter condenser by direct contact with condensing butane gas. The resulting
fresh water is then passed through a feedwater heat exchanger to cool the incoming seawater.
It then flows through a debutanizer and activated carbon filter to remove all traces of
refrigerant from the product. Since the amount of refrigerant gas released in the crystallizer
is far greater than can be condensed by melting ice, an auxilary condenser is used to condense
the excess by direct contact with seawater.
This process can be designed and operated to suit both single- and double-stage plants,
and has been suggested for large-scale freeze concentration of chemical solutions.64
B. Indirect-Contact Processes
Indirect-contact processes make use of a closed-cycle refrigeration system, and the heat
transfer from the freezing solution occurs through a heat-transfer surface. The crystallizer
design is, therefore, based on indirect-contact heat removal. In indirect-contact ice crystal-
lizers, the evaporating refrigerant or coolant is separated from the process liquid by a rigid
metal wall. The typical indirect-contact crystallizer is a tubular heat exchanger. The tubes
(usually 6 to 10 in. in diameter) are submerged below the level of the evaporating refrigerant
or chilled heat-transfer liquid in the shell. Based on design, they are classified as follows.
1. Scraped Surface Heat Exchangers

The scraped surface indirect-contact crystallizer is a vertical or horizontal cylindrical vessel
equipped with a rotating scraper to remove the ice crystals which tend to freeze on the heat
exchange surface. The crystal build-up on the transfer surface reduces the rate of heat transfer.
Most conventional designs in freeze and/or thermal processing, therefore, use scraped surface
heat exchangers. A serious drawback associated with these types is their relatively high
power consumption (for rotation), complex design, and high capital costs.
2. Nonscraped Surface Heat Exchangers

Efforts to develop nonscraped surface crystallizers are still underway. It is possible to
reduce or completely eliminate the ice crystal build-up on heat transfer surfaces by proper
control of process parameters. These types of crystallizers may eliminate the complexities
associated with scraped surface crystallizers.
Indirect-contact crystallizers are employed where the desired product, either the concen-
trated liquor or the melted ice, would suffer from contact with the refrigerant, thus eliminating
problems of refrigerant toxicity. Almost all known commercial installations for the freeze
concentration of liquid foods employ crystallizers of the indirect-contact type.66 For certain
food liquids, however, it may be possible to develop direct-contact processes using a com-
patible refrigerant such as carbon dioxide, nitrous oxide, and fluorocarbons such as per-
fluorocyclobutane (duPont Freon C318) or other food-grade freons. The commonly used
refrigerants for indirect-contact crystallizers include ammonia or fluorocarbons such as di-
chlorodifluoromethane (Freon 12) and monochlorodifluoromethane (Freon 22). Occasion-
ally, liquids such as ethylene glycol can also be used.
Some of the indirect-contact freeze concentration processes are described below.
a. Daubron Process
This process was developed by Etablissements Daubron de Paris, France. Made of a line
of portable units, each line of the process uses a vertical ammonia-jacketed scraped surface
crystallizer.31 The ice crystals are separated from the concentrate in a filter press employing
hydraulically operated pistons. The largest of their standard designs has an ice removal
capacity of 505 kg/hr (1131 lb/hr). This process was primarily designed and developed to
meet the requirements of the French wine industry. According to the French law, the wines
must have a certain minimum alcohol content. Some wines having high water content,
therefore, need to be subjected to a modest degree of concentration to bring up the alcohol
content to the legal minimum. Daubron process is a simple batch process.
Using a Daubron apparatus, Jaulmes and Hamelle50 concentrated a wine of 12.7CGL to
20.8°GL. However, these authors reported losses of 36.5 m£ of wine, 0.22 g of tartaric
acid, and 0.33 g of potassium per liter of concentrate. Similarly, losses of wine equivalent
to 2 to 4% and of alcohol (0.755°GL), dry extract (1.5 g/€), and total acidity (0.34 g/€,
expressed as sulfuric acid) were observed in the melting water. These authors also reported
precipitation of nitrogenous substances, calcium, tannins, iron, and the coloring substances.
It therefore appears that the process may not be suited for concentrating liquid foods to a
very high degree without the loss of soluble solids, and thus the resulting product may be
of a lower quality.
b. Gasquet Process
This process is similar to the one described above and was developed by La Societe du
Filtre Gasquet, Bordeau, France, for the freeze concentration of wines.66 The largest of their
installations had a capacity of 1 ton of ice per hour. Horizontal scraped surface tubes, either
enameled or made up of stainless steel, are used to crystallize out water from food liquids.'
The ice crystals are separated from the mother liquor in a perforated basket-type centrifuge
or filter press employing hydraulically operated pistons.
Chiller
\
Feed
i[
Filter
Mother
Liquor
Bed
Purification
Melter
FRCU
Pulse C^L
unitrjT
FIGURE 16. Phillips pulse purification column. (From Muller, J. G., Food TechnoL, 21(1), 49, 1967. With
permission.)
c. Phillips Process
This process was developed by the Phillips Petroleum Co., Bartlesville, Okla. for use in
the brewing industry. It uses a novel pulse purification column to separate the ice crystals
from the concentrated slurry (Figure 16). The incoming beer undergoes sensible cooling and
ice crystallization in a vessel called "chiller". The resulting ice crystal slurry is then pumped
into the top of a crystal purification column. A portion of the liquid concentrate not occluded
by the ice crystals leaves the column at once through a filter zone. The ice crystals move
down the column past the filter zone and approach a heating element. Since the occluded
concentrate has already been removed by a displacement process, only purified ice crystals
actually reach the hot element. A part of the melted ice, due to pressure differentials within
the column, comes back up through the column countercurrent to the descending ice bed.
The refreezing of this water causes separation of the occluded concentrate from those ice
crystals which are farther removed from the heat transfer element. Because of pressure
differentials, the occluded concentrate so removed then rises up to the filter zone and is
FEED IN
COOLING WATER
OUT
CONCENTRATE
• REFRIGERANT GAS
TO COMPRESSOR
3 2 ° F ICE CRYSTAL WASH WATER
FIGURE 17. Flow diagram for the Struthers FreCon method for the freeze concentration of fruit juices. A =
precooler; B = crystallizer; C = melter-condenser; and D = centrifuge. (From Anon., Quick Frozen Foods, p.
90, March 1964. With permission.)
then removed from the column as liquid concentrate. The energy for filtration, bed movement,
and reflux driving force is supplied by a pulse unit in the concentrate product line.
If necessary, a two- or three-stage process could also be used for fractional crystallization
of chemicals.
The countercurrent contacting of the crystal bed with a portion of the crystal melt in the
Phillips process is similar to refluxing in a distillation column. This results in the removal
of the occluded concentrate from the surface of the ice crystals with negligible diluton of
the concentration. The loss of soluble solids with the discarded ice is, therefore, greatly
reduced.
d. Struthers FreCon Method

In the mid-1960s, Struthers Scientific and International Corporation of New York offered
several designs for freeze concentration of liquid foods. Based on about 30 years of experience
in the field of crystallization, first in the chemical and petrochemical industries and then in
the desalination of seawater, the Struthers Company successfully demonstrated the feasibility
of freeze concentrating food and beverage products.
The key to the Struthers FreCon process is controlled crystallization, which permits
efficient separation of water and product. Accurate temperature control, which governs the
rate of ice crystal formation, produces the desired crystal size, and controls the rate at which
ice nuclei form spontaneously. The ice crystals can then be separated from the supernatant
liquid without the loss of product which is normally trapped in crystal interstices of irregular
sizes and shapes. It also allows separation of ice crystals by centrifuging rather than by
complicated wash and tower arrangements.
The Struthers FreCon process is uncomplicated and the process flow is relatively simple
(Figure 17). The single-strength feed is first sent through a precooler, where it is cooled by
32°F water from the melter condenser (downstream in the process). The precooled feed,
along with some slurry from the crystallizer, then passes through a crystallizer and is
supercooled. It is in this stage of the process that accurate temperature control determines
the size of ice crystal, the rate of ice crystal growth, and the rate at which spontaneous
nuclei form. The ice crystals from the mother liquor are separated by centrifugation and
G
FIGURE 18. Struthers Scientific freeze concentration process. A = crystallizer I; B = crystallizer II; C =
compressor; D = centrifuge I; E = mother liquor tank; F = centrifuge II; G = refrigerant vapor; H = refrigerant
liquid; I = feed tank; J = melter; K = precoolers; L = condenser; M = receiver; N = cooling water; O =
process water out; P = feed in; and Q = product out. (Redrawn from Muller, J. G., Bull. Inst. Int. Du Froid
46, Annexe 3, 1966a, 15. With permission.)
then melted in the melter condenser by heated refrigerant gas from the compressors. A part
of this ice water is used to wash ice crystals in the centrifuge free of any adhering concentrate
and is recycled; the remainder is used as cooling medium in the melter condenser. Some of
the advantages claimed for this process include a minimum loss of product (less than 1%),
low energy requirements (about 80 lb of water removed per kilowatt hour of energy con-
sumed), low capital costs, and lower corrosion rates.66
e. Struthers Scientific Process

The Struthers Scientific indirect-contact freeze concentration process was originally de-
veloped for concentration of viscous food liquids, but it can also be utilized for liquids of
low viscosity.6-8"-39-63-64-66-78-85 The process flow for a typical two-stage plant is illustrated
in Figure 18.
The single-strength feed is precooled in plate heat exchangers and then sent to the first-
stage crystallizer. The crystallizer consists of a number of chilled horizontal tubes in which
ice crystals are nucleated and grown. Here, the temperature, turbulence, and other operating
parameters are closely monitored to obtain large uniform sized-and-shaped ice crystals.
Unlike most other processes, the crystallizer walls are not scraped. The mother liquor from
the resulting ice crystal slurry is spun off into a high-gravity continuous screening centrifuge.
The partly concentrated liquor is then pumped into the second-stage crystallizer, which also
consists of a number of horizontal chilled tubes. There, further crystallization and concen-
tration takes place. The ice crystal slurry then passes to a second-stage centrifuge, where
the concentrated liquor after separation is obtained as the desired end product. The dewatered
crystals are washed on the centrifuges with cold water and are melted in an agitated vessel
by contact with plate coils heated by warm water. The ice melt can be employed as a
centrifuge wash liquid and as a coolant for the incoming feed (Figure 18). The entire process,
including the crystallization and centrifugation steps, is a continuous one.
The Struthers crystallizers do not employ any scrapers. According to Muller,66 scraping
causes formation of an excessive number of nuclei or tiny new crystals. It is desirable that
the ice mass created in unit time be distributed among a limited number of crystals. This
allows the formation of large ice crystals. Consequently, solid losses to the ice crystals are
minimized. Similarly, in the Struthers process, the wash columns are replaced with centri-
fuges. Wash column has been the most successful method when liquid viscosity is low,
such as in the case of seawater desalination. Wash columns are not suited for high viscosity
liquids, whereas centrifuges perform well under these conditions.
/ . Struthers Scientific Mobile Freeze Concentration Unit

Struthers Scientific and Industrial Corporation, New York has developed a mobile freeze
concentration unit. The entire plant is mounted on a railroad flatcar or truck and consists of
all the necessary equipment, including two crystallizers, two centrifuges, a refrigeration
unit, pumps, tanks, and other accessories. Once delivered to a food or chemical plant, the
necessary piping and electrical connections can be made quickly, and within a few hours
of arrival, the whole unit could be made to function in a continuous operation. The mobile
unit can be operated at feed rates of aqueous liquids up to 600 lb/hr. The mobile unit has
been successfully used to concentrate a variety of liquid foods including apple juice, beer,
coffee extract, skimmed milk, and orange juice.66
g. Union Carbide Process

Originally developed by the Commonwealth Engineering Co., Dayton, Ohio, this indirect-
contact freeze concentration process was later acquired and improved by the Union Carbide
Corporation.66-677879 It is a two-stage freeze concentration process (Figure 19). Scraped
surface tank crystallizers are used to form the ice crystals, which are scraped and continuously
removed from the crystallizer walls. The ice crystals are allowed to develop in the body of
the slurry to a size suitable for separation. The crystals are separated from the concentrated
liquid by a centrifugal screening action. Both the crystallization and centrifugation operations
are repeated in the second stage of the plant. The ice crystals with entrapped concentrate
from both the first- and second-stage centrifuges then pass through a third centrifuge. The
recovered dilute concentrate is recycled to the feed or the first-stage crystallizer (Figure 19).
Based on this design, Union Carbide has developed an overall process for freeze con-
centration of orange juice. The process includes the following steps:
1. Pulp separation
2. Deaeration to remove oxygen
3. Oil control treatment
4. Enzyme stabilization
5. Chilling
6. Freeze concentration
7. Addition of stabilized essence from evaporator feed
This process was commercially employed in the 1960s by the Minute Maid Division of
the Coca Cola Co. at Plymouth, Fla. One of the two plants installed had a rated capacity
of processing 5000 lb of fresh orange juice. The freeze concentrate produced was blended
with a more concentrated evaporator effluent to produce a 42° Brix product. This process,
however, was apparently abandoned a few years later in favor of evaporation, apparently
1'
1
F
G
F==l
FIGURE 19. Union Carbide freeze concentration process. A = single-strength feed; B = twofold concentrate;
C = ice generator (first stage); D = ice generator (second stage); E = centrifuge (first stage); F = centrifuge
(second stage); G = fourfold concentrated product; H = ice with entrained concentrate; I = recovered dilute
concentrate; J = final centrifuge; and K = pure ice. (From Muller, J. G., FoodTechnol., 21(1), 49, 1967.
With permission.)
due to economic reasons and difficulties in operation. The process was also promoted for
the freeze concentration of beer. However, because of legal restrictions in labeling of the
product, no commercial installations have been reported.
h. Grenco Process
Grenco Special Applications b.v., a Dutch company, has been actively pursuing research
in industrial and marine refrigeration for the past three decades. Their research in the field
of freeze concentration has resulted in eliminating several of the drawbacks associated with
the earlier processes. The success of this process is credited to the formation of large,
spherical ice crystals at very slight super temperatures under controlled conditions.42 The
large size of the spherical ice crystals also makes them easier to separate from the concentrate.
This new technique for separating the ice crystals from the concentrate avoids the loss of
concentrate with the ice. The high capacity of the Grenco Process has considerably lowered
the investment costs per ton of water removed, as compared to those using the existing
methods.
Briefly, the Grenco freeze concentration system consists of a crystallization section and
••Output Final Product Water

Circulating Pump Separated Water
without Ice Crystals Steam
[=M=S»am Supply
Receiver Cooling System

Suction Refrig. Gas Condensate Output
Refrigerant
Supply Refrig.
Storage
Concentrated Tank
Product with
Ice Crystals
Concentrated Product to be Feed
Product without Concentrated Pump

Ice Crystals
Unconcentnted liquid is pumped to * h o t exchanger, where small crystals form in seconds. These small crystals melt
in the recrysiallizer, "feeding" the growth of large crystals. Concentrate with crystals is pumped to a wash column,
where separation takes place. Some crystals are melted to create pure wash water. Concentrate will circulate until a
set ralue is reached.
FIGURE 20. Grenco freeze concentration process. (From Wagner, J. N., Food Eng., p. 98, February 1983.
With permission.)
a wash column. In the crystallization section, the water is separated out in the form of ice,
and the wash column ensures a complete separation of the concentrate from the ice crystals.
The schematics of the process are shown in Figure 20.
Once the equipment has been filled with the food liquid which is to be concentrated, the
stirring device of the recrystallizer, the circulation pump, and the scraped heat exchanger
are started up. The liquid is cooled to its freezing point prior to ice crystal formation in the
scraped heat exchanger. The mixture of large and small ice crystals together with the mother
liquor is pumped into the recrystallizer. The larger crystals grow to large spherical crystals,
whereas the very small crystals melt. After a desired degree of ice concentration has been
reached in the recrystallizer, the wash column is started up, where the ice crystals are
separated from the concentrated liquor. The concentrated liquor, together with the feed, is
fed back into the crystallization section by the feed pump via the feed tank. When the desired
level of product concentration has been reached, the concentrate is forced, via the expansion
vessel, into a product storage tank. Detailed description of the process is given in the company
literature.42
In the Grenco process, the concentration of the end product, as well as the capacity, are
automatically regulated at required values which are set beforehand. The dewatering capacity
can be set at any value between 40 to 100% of the design capacity.
In addition to lower investment cost, Grenco Special Applications cites the following
advantages for their process:
1. Concentration of aroma-rich products without first stripping aromas

2. Concentration of alcoholic products without loss of alcohol and deterioration in quality
parameters
3. Concentration without loss of valuable active components
4. Reduced loss of soluble solids, usually less than 100 ppm
5. No thermal deterioration of the product
CONCENTRATION
(°BRIX)
TEMPERATURE,
FIGURE 21. Four time intervals during single-stage operation of freeze concentration process. (From Van Pelt,
W. H. J., Bull. Grenco Special Applications, b.v., Netherlands, 1981. With permission.)
The Grenco freeze concentration process can be used for almost all food liquids with a
low to medium-high viscosity. The company has successfully tested a number of products,
including coffee extracts (up to 45 wt % concentration), vinegar (48% concentration), sugar
solutions (52% concentration), beer and wine (up to 32 vol % concentration), fruit juices
(55% concentration), milk (36% concentration), several thousandfold concentration of ex-
tracts of various aromas, tea extracts (35% concentration), aqueous protein solutions, and
as a separation process for isolating mixtures of chemical fluids.
i. Grenco Multistage Freeze Concentration Process

Most processes described earlier are single-step processes, i.e., those which consist of
one crystallization and one separation step. According to Van Pelt,107 such single-step freeze
concentration processes could be divided into four time intervals, from the starting up of
the equipment to reach a continuous operation (Figure 21). These time intervals are as
follows:
1. A period of precooling of the feed

2. A period of crystallization to form the first ice slurry
3. A period of crystallization and separation in which the bulk dry solid concentration
increases to the final desired level
4. The continuous stationary operation
Thus, in single-stage continuous freeze concentration processes, the heat of crystallization

has to be removed at one temperature level. Van Pelt107 has summarized the characteristics
of single-stage freeze concentration processes, in which entire crystallization takes place at
the end concentration level as follows:
ICE
CONCENTRATE
C = CRYSTALLIZER S = SEPARATOR
FIGURE 22. Cocurrent multistage freeze concentration process. (From Van Pelt, W. H. J., Bull. Grenco Special
Applications, b.v., Netherlands, 1981. With permission.)
1. All heat has to be removed at the lowest level.

2. All crystals have to grow under the most unfavorable conditions of high concentration
and high viscosity. The continuous rise in viscosity during concentration, caused by
dry solid content and the low process temperatures, results in longer residence times
for the crystals, which in turn requires larger crystallizers.
3. Due to high viscosity, the resulting smaller ice crystals have to be separated under
unfavorable conditions.
4. The increased viscosity of the concentrate puts extra loads on pumping and mixing.
The single-stage freeze concentration processes, therefore, require high energy input.
Most of these drawbacks of the single-stage freeze concentration processes can be elim-
inated by adopting a multistage design. The multistage freeze concentration process can
either be a cocurrent (Figure 22) or a countercurrent operation (Figure 23). In the multistage
freeze concentration process, the ice crystals are separated out at the end of each cycle and
the remaining concentrate is fed to the succeeding crystallizing compartment.107 Thus, in
continuous operation, the heat has to be removed at each level of crystallization. The ice
ICE
CONCENTRATE
ICE
CONCENTRATE
ICE
CONCENTRATE
C = CRYSTALLIZER S = SEPARATOR
FIGURE 23. Countercurrent multistage freeze concentration process. (From Van Pelt, W. H. J., Bull. Grenco
Special Applications, b.v., Netherlands, 1981. With permission.)
crystals, therefore, have to be grown and separated at different levels of concentration and
viscosity. The countercurrent system allows back-mixing of the concentrate within the thick-
ened ice. This results in a somewhat lower processing temperature and a slightly higher
degree of concentration at each level. Since heat has to be removed in both cases at nearly
the same level, both the co- and countercurrent multistage processes have similar energy
economics. Van Pelt,107 however, cites the following reasons, from a process point of view,
for selecting a countercurrent system:
1. Since ice has to be removed at the lowest dry solid concentration, lower viscosities,
and thus, higher separating velocities could be achieved.
2. Because of the lower dry solid content, larger ice crystals can result, influencing to a
great extent the separating velocity.
3. The ice crystals are formed under favorable conditions of viscosity and dry solid
content, resulting in shorter residence times (Table 16) and smaller-sized crystallizers.
4. Since ice is transported from the last stage to the first, it is not necessary to perform
the intermediate separation steps as perfect as for the last definitive separation in the
Table 16
NECESSARY RESIDENCE
TIMES TO OBTAIN
SEPARABLE ICE
CRYSTALS: MODEL
SOLUTION 10% d.s., 50%
d.s. (SACCHAROSE)107
Residence time
System (hr)
One stage 4.0

Three stage
Cocurrent 1.3
Countercurrent 0.8
Table 17
COMMERCIALLY EMPLOYED INDIRECT-CONTACT
FREEZE CONCENTRATION PROCESSES107
Type Crystallization Separation aystem
Combination of Scraped surface Press Daubron

nucleation and SSHE Press Gasquet
growth zone in Rotating drum Press Krause-Linde
the crystallizer Rotating drum Centrifuge Heiss-Neuerburg
Scraped surface Centrifuge Struthers
SSHE Wash column Phillips
Separate nuclea- SSHE/Ripening vessel Centrifuge Doge/Rosenmund
tion and growth SSHE/Ripening vessel Wash column Grenco
zone
wash column. Slurry thickeners, therefore, can be used for the intermediate separation
and transportation action.
The major advantages of multistage over single-stage freeze concentration plants include
lower energy consumption (approximately 37% lower for cocurrent and 47% lower for
countercurrent systems), and approximately 50 to 70% lower operating costs.107
Some of the indirect-contact freeze concentration processs which are currently employed
on commercial scale are summarized in Table 17.
VII. APPLICATION TO OTHER FOOD PRODUCTS
Before discussing the applications of freeze concentration to other areas of food industry,
it would be appropriate to review, briefly, the advantages and drawbacks associated with
this method of concentration. Concentration by freezing has several advantages over other
concentration processes such as evaporation and reverse osmosis. Some of the advantages
claimed are discussed below.
One of the obvious advantages of freeze concentration over evaporative methods is that
the energy needed to freeze a unit of water is much less than that required to evaporate it
(Table 13). At any given process temperature, approximately one seventh as much heat must
be withdrawn from a pound of water to freeze it as must be added to vaporize it as in
evaporative processes. Struthers estimated that with their process, 1 kWh of energy input
could produce approximately 70 to 80 lb of ice.66 Similarly, since the object is to freeze the
final product, considerably less cooling is required after processing and concentration. Sub-
stantial energy savings are, therefore, possible in many applications of freeze concentration
as compared to the more conventional evaporation processes. According to Davis,32 freezing
processes can be designed to either utilize electricity as the sole energy source or to operate
the process in an absorption cycle using waste heat at as low as 130 to 140°F. In many
industrial applications, waste heat at these temperature levels has no value and it represents
a disposal cost. Aceto2 estimated that, based on food industry averages, concentration by
freezing requires only between 1/10 to 1/15 the energy required for water removal by
conventional thermal evaporation. Actual cost analyses of concentration by several methods
will be discussed in a later section.
A distinct advantage of freeze concentration is the low temperature difference required
between the liquid and the cooling medium. Few, if any, food liquids appear to be adversely
affected by exposure to temperature below 0°C for a short time. Some food liquids actually
appear to be benefited by such treatment.66 The low process temperatures also prevent
degradation of heat-sensitive compounds. The food liquids can thus be concentrated without
appreciable loss in taste, aroma, color, or nutritive value. Since the entire process is operated
at or below the freezing temperature of water, and since vacuum treatment is not required,
the loss of low boiling flavor and aromatic esters is almost completely avoided. Aromas are
better retained in the juice and thus polymerization and condensation reactions of the aroma
components, which may occur during aroma stripping in distillation, are fairly well inhibited.
Volatile carryover is thus completely prevented in freeze concentration.
From a process point of view, corrosion rates of equipment are much lower in freeze
concentration as compared to evaporation processes. Corrosion is a major problem in the
concentration of corrosive chemical solutions and seawater desalination. For every 10°C
temperature rise, corrosion rates are doubled. Since most of the process is operated at or
below 0°C, freezing has much lower corrosion rates than evaporative processes. Therefore,
less expensive materials of construction can be used. Davis32 suggested the use of steel
vessels, aluminum heat transfer surfaces, and PVC piping in seawater desalination and 316
stainless steel for concentration of corrosive chemicals.
An inherent advantage associated with lower corrosion rates during freezing is that the
pretreatment of the feed for scale control can be omitted. Scaling is not a problem in direct-
contact processes, where no heat transfer surface is required. Scaling is minimal in indirect-
contact processes where scraped surface heat exchangers are used. Depending on the sol-
ubility, the scaling materials may either leave the process with the concentrate (e.g., the
less soluble calcium sulfate) or must be separated from the ice prior to their washing (e.g.,
high soluble materials such as sodium sulfate).
The loss of soluble solids to the ice crystals could be avoided by proper monitoring of
process parameters. Controlled crystallization allows formation of large, nearly pure ice
crystals, and with adequate washing and recrystallization, dewatering could be made almost
selective. Recycling a part of the ice melt and thus of any entrained solids to the crystallizer
may also reduce solids losses. With modern processes, the solids losses have been reduced
to less than 100 ppm. Unlike membrane separation processes, there is no danger of short
circuiting the process by leaks.
In desalination, freezing concentration offers several other advantages as compared to
distillation and membrane separation processes:64-70-98 freeze desalination plants can employ
direct-contact heat transfer designs. Therefore smaller temperature differences, high cycle
efficiencies, and low energy consumption can be achieved. As much as 90% of fresh water
can be recovered, particularly from high saline-containing feeds. Because of scaling, such
high recoveries are not possible with membrane demineralizers and distillation units. Unlike
freeze desalination, membrane processes cannot handle feeds containing high-dissolved
solids.
Although freeze concentration has been shown to be a superior process as compared to

evaporation, at least as far as product quality is concerned, the process has been seldom
used on a commercial scale. Major drawbacks of some of the earlier freeze concentration
processes are discussed below.
High capital investments and considerable loss of solids and thus loss of quality factors
were the two major limitations associated with the old freeze concentration processes. The
old processes were mostly batch operations, labor intensive, inefficient as compared to their
potential, and limited to low throughput operations.45 Considerable research in the past two
decades, however, has led to development of continuous and/or multistage freeze concen-
tration processes, thus eliminating most of these drawbacks. Studies on crystallization of
water during freezing have led to newer processes, where desired ice crystal formation can
be monitored. This has considerably minimized the solids losses to ice.
In spite of the developments in water crystallography, there always is some loss of solids
by entrainment in the crystals. As the solids are concentrated during freezing, the ice crystal
size progressively decreases. The washing of the ice crystals therefore, becomes more
difficult, and may require larger-diameter wash columns. The minimum desirable size of
the ice crystals is reported to be 100 to 300 (im.32 Larger ice crystals can be grown by
increasing the retention times of the feed in the crystallizer. This may, however, partially
offset the overall economics by lowering the output as well as increased energy requirements.
Since freeze concentration is capable of preserving almost all of the original chemical
constituents, flavor, and aroma of fruit juices, the raw material should be of the highest
quality.66 Thus, rigorous quality control of the feed material is required ensuring that they
are free of below-standard elements.
A major problem, which still remains to be solved, is that the final degree of concentration
that could be achieved by freezing is much lower than that by evaporation process. Because
of low process temperatures, and thus high viscosities, most food liquids cannot be con-
centrated beyond 50 to 55% w/w. The high viscosity retards the rate of crystallization and
makes pumping of the concentrate and washing of crystals increasingly difficult.32-51-64-66-89-90
This also presents difficulties in separation of ice crystals from the mother liquor. Davis32
suggests that some of the problems of high viscosity could be overcome by redesigning
process flows and components. Research conducted at Grenco Special Applications b.v.
also indicates that under such conditions a multistage countercurrent freeze concentration
system is better.107 In such a design, all ice has to be separated at the lowest dry solids
concentration. The resulting lower viscosities, therefore, allow higher separation velocities.
Another problem encountered in the freeze concentration process is that most solids are
only sparsely soluble at freezing temperatures.51 Beyond a certain degree of concentration,
the solubility limit of such solids is exceeded. As a consequence, pure crystals of these
compounds precipitate in addition to ice and are lost. In chemical industries, this may actually
turn out to be beneficial, since in addition to pure water, pure byproducts could be extracted
during the concentration process.32 In food industries, however, the precipitation of solids
can interfere with efficient operation of crystallizers and separators. This problem can be
overcome by modifying the process design. Struthers Scientific and International Corpo-
ration, New York has developed one such process for freeze concentrating tea infusions.81
In this design, the tea extract is cooled and then passed through a settling tank, where some
of the solutes precipitate. The extract is then fed to the crystallizer and separator, where a
part of the water is removed as ice. The precipitate obtained is redissolved in a small quantity
of water and is then returned to the concentrate prior to freeze drying. The schematics of
the process are shown in Figure 24. The process can also be applied to preconcentration of
coffee infusions before freeze drying.
The freezing point of the concentrate has a significant effect on the power consumption
of the process.32 The power consumption varies from 50 kW/kgal water removed at a freezing
FEED
DILUTION WATER CONCENTRATE

MIXING TANK MIXING TANK 2
FIGURE 24. System for precipitation of a portion of suspended solids prior to freeze concentration. (From Karel,
M., in Principles ofFood Science, Part II: Physical Principles of Food Preservation. Karel, M., Fennema, O. R.,
and Lund, D. B., Eds., Marcel Dekker, New York, 1975a, 265. With permission.)
point of 25°F to 120 kW/kgal water removed at — 10°F. Large freezing point depressions
may be observed with increasing concentrations in a single-stage freeze concentration proc-
ess. In addition to higher energy consumption, this also restricts the upper level of concen-
tration by freezing.
In spite of these limitations, freeze concentration is a very versatile process and has found
many uses in seawater desalination, chemical industries, and in waste-disposal. Some of
these applications are summarized in Table 18 and are discussed below.
A. Beer and Wine Industry

Some of the earliest efforts to commercialize this technique for the concentration of food
liquids were attempted in the beer and wine industry. In fact, in many European countries,
freeze concentration was applied in crude forms to increase the alcohol content of wines.
The process makes use of the different freezing temperatures of alcohol and water. Since
alcohol has a lower freezing point than water, proper monitoring of temperatures during
concentration can remove most of the water as ice, whereas the concentrate retains the
alcohol. The two major drawbacks of the earlier processes included loss of alcohol to the
ice and the precipitation of quality factors such as tannins. To a large extent, these problems
are eliminated by modifying the process designs and by using better separation methods.
Most processes described earlier can be used, with suitable modifications, in the brewing
industry. The Phillips fractional crystallization process was specifically developed for con-
centration of beer. In this process, single-strength beer (approximately 3 to 4% w/w alcohol)
is first blended with a recycle stream of concentrate and prechilled. A conventional crystal
forming and growing unit is used to produce a thick crystal slurry. The nonfrozen concentrate
is separated through the wall filters of a crystal pulse purification column, leaving behind
an ice crystal bed. The ice crystals are melted in a heater at just above 32°F and the water
can be reused. A part of the water is forced back through the crystal bed, and as it undergoes
refreezing and subsequent remelting, it exerts rectifying action similar to reflux in a fractional
distillation column. Approximately 99% of the water entering the column as ice is eventually
removed. The process can be used to concentrate beers ranging from conventional types to
malt liquors. Concentrates containing as much as 12.5% by weight alcohol can be obtained
by this process.
Grenco Special Applications b.v. offers freeze concentration processes capable of con-
centrating beers and wines up to 25 to 32% of the original volume.42 Further concentration
was not economically feasible due to large freezing point depression. The schematics of the
Grenco processes were described earlier. Research conducted at this company has provided
Table 18
APPLICATIONS OF THE FREEZE CONCENTRATION PROCESS66
Purpose of concentration Typical application
Reduce the volume of liquid to be stored and handled Concentration of ruh beer
within the plant
Reduce cost of shipping, and storage after leaving pro- Orange juice concentrate
ducer's plant and to reduce the cost of containers
Raise the concentration of material present in quantities Laboratory concentration equipment for oceanographers
too small for proper analysis and/or reaction
Bring about the crystallization and recovery of dissolved Production of magnesium ammonia phosphate from
organic and inorganic salts seawater
Recover pure water from seawater for drinking or other Desalinization
purposes
Raise the sugar content of comestible liquids to such Fruit syrups
level that spoilage will be retarded
Make a more concentrated liquid which can then be Instant or soluble coffee
economically subjected to complete dehydration
Restore to full strength the concentration of preserving Concentration of pickle liquors
liquids diluted during the preserving process
Form a new liquid product Malt made from concentrated beer
Raise concentration of certain components in a liquid to Concentration of wine to raise alcohol content
prescribed levels
Accelerate processing rate by bringing about earlier pre- Freeze concentration to reduce lagering time of beer
cipitation of dissolved or suspended substance
Raise concentration of solids to level sufficient for eco- Concentration of sewage
nomic disposal
Treat products to prevent deterioration during Freeze concentration of wines to be exported
transportation
new insights in freeze concentration of alcoholic beverages. Some of these findings are
summarized below:
1. A three- to fourfold concentration can be achieved by freezing of alcoholic beverages.

2. Use of medium-to-fine filters for clarification is unsuccessful due to very low flow
rates. Bright and clear filtrates could be achieved only by filtering through large filters.
3. Centnfuging the warm concentrate at normal speeds gives a hazy supernatant, with
haze reduced to about one tenth of its original value. The haze that is formed during
concentration can be removed by centrifuging the cold concentrate and its appropriate
dilution and postdilution filtration after a 48-hr stand.
4. Proper washing of the ice crystals in suitable wash columns can reduce the loss of
solids and alcohol to a minimum. The product thus retains most of the bitterness and
volatile components.
5. Due to their high alcohol content, the concentrated products have better stability
towards microbial spoilage.
6. Precipitation of tartarate salts by partial insolubilization is a major problem in freeze
concentration of wines. Although the product gives a good physicochemical stability,
it creates acid-base imbalance. Higher levels of concentration merely give greater
imbalances. Adjusting the acidity of the reconstituted wines by adding tartartic acid
(1 g/€) alters sensory properties, particularly in the case of red wines.
7. High quality raw materials are required, since the characteristics of bitterness, harsh-
ness, and astringency are also concentrated in the final product.
Grenco Special Applications b.v. is cooperating with the National Institute of Viticulture,
Argentina to develop their viticulture industry, and is also actively participating in seeking
DILUTE
CONCENTRATE
STORAGE
FEED
A
INTERCHANGE
FIGURE 25. Votator freeze concentration process for vinegar. (From Muller, J. G., Food Technol., 21(1), 49,
1967. With permission.)
legal authorization of the freeze concentration process as a general practice in Argentina.

Many countries prescribe certain minimum alcohol levels in such beverages. The addition
of pure alcohol to products containing less than the legal minimum level is prohibited by
law. A major hurdle in preparing beer concentrates in the U.S. is concerned with the labeling
requirements. The Alcohol and Tobacco Division of the Internal Revenue Service has issued
a regulation that containers of reconstituted freeze concentrated beer must be labeled "beer
made from beer concentrate". 7 The manufacturers are not willing to market such a product
since the label may imply an "imitation" product. Changing the labeling requirements may
benefit the California wine industry. Considerable savings in shipping costs may be obtained
by freeze concentrating the wines prior to their shipping to East coast markets.
B. Vinegar and Pickling Industry

Vinegar is commonly used in the pickling of vegetables, in preparing meat and fish
specialities, and in the manufacture of various condiments and salad dressings. The use of
single-strength vinegar (4 to 5% acidity) to prepare brine for steeping cucumbers necessitates
periodic addition of vinegar to compensate for dilution by the cucumber water and to maintain
proper acid strength. Oftentimes, the diluted brine has to be discarded causing loss of solids
such as sugars and salt as well as flavoring material. The use of concentrated vinegar (such
as 20-g vinegar) allows pickle packers to introduce smaller volumes of vinegar into the
brines. Such brines can be used for longer periods than usual. It also saves on freight and
storage.
The first commercially feasible continuous process for freeze concentration of vinegar
was developed by the Votator Division of Chemetron Corporation, Louisville, Ky. 6 - 910 The
process flow sheet is shown in Figure 25. The basic principle of the process is slush-freezing
vinegar of intermediate strength and then centrifuging the ice from the slush to produce the
concentrate. The process makes use of a number of conventional horizontal scraped surface
heat exchangers and a batch-type centrifuge. Initially, a blend of 170-g vinegar is prepared
by mixing 120- and 200-g vinegars. It is then continuously metered through an ammonia-
jacketed, votator heat exchanger and slush frozen to about 17°F. The flow through the votator
unit is two to three times that of infeed. The vinegar slurry discharged from the heat exchanger
contains 20 to 25% ice. The slurry is then charged into an agitated stainless-steel
surge tank, intermittently feeding a 200-gal basket-type centrifuge. The centrifuge cycle is
automatically controlled. The loading of about 100 gal of slush into the centrifuge requires
2 to 5 min, and centrifuging about 14 min. About 2 min is required to remove the dewatered
ice crystals using a pneumatically operated plow. After that the centrifuge is made ready
for another batch. The concentrated liquor (200-g vinegar) is pumped to a storage tank and
withdrawn as needed by tank trucks serving the ultimate users. The ice from the bottom of
the centrifuge bowl is taken to a wooden tank. Since it contains vinegar (10 to 20 g), it is
reused in the production of other vinegar.
By recycling some of the stream, considerable energy savings could be achieved in this
process. The ice can be used to precool fresh vinegar (120 g), thereby reducing the sensible
heat load in the votator heat exchanger. Since the ice is not yet completely melted, condenser
water from the refrigeration system can be used to complete the melting process. Where
cooling towers are used, water cooling tower requirements can be greatly reduced.
High strength (200 to 400 g) vinegar can be produced similarly, blending up from 120 g
to starting intermediates of higher strength. The votator process produces a 200-g concentrate
from 120-g vinegar at a rate of 750 to 1000 Ib/hr. Higher concentrates can be produced at
lower rates, such as 300 g at 600 lb/hr and 400 g at 400 lb/hr.
Grenco Special Applications b.v. also offers a freeze concentration process that concen-
trates vinegar up to 48 wt %.42
C. Dairy Industry
The potential of freeze concentration processes in the dairy industry has been realized
only recently.72 Although freeze concentration tehniques can be used to produce conventional
products, such as concentrated milk,42 its application in the area of whey processing seems
to be a very attractive proposition. According to Dairy Research, Inc. (DRTNC), a subsidiary
of the Research and Development unit of the United Dairy Industry Association, if freeze
concentration were to be used by all whey processors, savings of at least S15 million/year
could be realized. Saal72 estimated that freeze concentration could cut the energy costs of
whey processing by a minimum of 15% as compared to that by evaporation. Based on
energy requirements alone, he cites savings of about $300,000/year based on 1979 prices
for oil and electricity and for a plant processing 1 million 1b of whey per year. In cooperation
with Dairy Venture I of DRINC, Concentration Specialists, Inc. (CSI), Andover, Mass, has
developed an indirect-contact process and equipment for whey processing. The process can
also be used to concentrate a variety of other products.32 Schematics of the CSI process are
shown in Figure 26.
The feed may be screened to remove large suspended solids, prior to entering the process,
if required. It is precooled in a plate heat exchanger by the outflowing concentrate and melt.
The precooled feed then flows down through a crystal growth column, countercurrent to the
ice moving upward. From the top of the column, the slurry is pumped to a wash column
where the adhering fluid is washed off by water produced by melting previously harvested
ice crystals. The ice is separated at the top of the wash column, repulped, and pumped to
a shell and tube heat exchanger. There it is melted by condensing the refrigerant that was
evaporated in the freezer. A recirculation flow is maintained between the bottom of the
growth column and the freezer. In the latter, a small fraction of the flow is converted to
ice. The concentrate is then extracted from the recirculation system.
The special features of the CSI process include a HYDRO-SCRUB tubular heat exchanger
and a continuous concentrate separation column. The special tubular heat exchanger is
reportedly much less expensive (1/15 to 1/20/ft2) as compared to the conventional scraped
WASH
WATER
COOLING
WATER
CONCENTRATE REFRIGERANT
SEPARATION COMPRESSOR
COLUMN
WATER
FEED
CRYSTALLIZER
CONCENTRATE
FIGURE 26. Concentration Specialists, Inc. (CS1) freeze concentration process. (From Davis, H. E., Bull.
Concentration Specialists, Inc., Andover, Mass., 1983. With permission.)
surface types.32 The large surface areas in the freezer permit the use of low temperature
differences across it, and thus, lower energy consumption. The energy consumption and
costs are further lowered, since large motors and expensive gear drives to power mechanical
scrapers are not required.
The CSI concentrate separation column apparently overcomes many of the problems
associated with the production of high density concentrates by conventional freeze concen-
tration. Normally, with increasing degree of concentration, extremely small ice crystals are
formed in the crystallizer section. In addition, due to low process temperatures, the slurry
is quite viscous. The separation of ice from concentrate, therefore, requires the use of large-
volume equipment, and the solids losses to the ice may be quite high. CSI claims that their
system promotes rapid crystal growth prior to separation, thus permitting efficient separation
of ice from the product in reasonably sized equipment.32 Some of the other advantages
claimed for this process include simple, reliable operation, very low energy consumption
(10 to 20 kWh/1000 lb of water removed), longer periods between cleaning in food appli-
cations, and shorter start-up times.
D. Chemicals and Pharmaceuticals Industry

Freeze concentration technology can be used for many industrial separation processes. In
many applications, it has been shown to be the only process that is suited for chemical
separations.45 In addition to energy savings, freeze concentration is free of drawbacks such
as equipment corrosion and scaling associated with evaporation and distillation processes.
It is especially suited to separate chemicals from multicomponent solutions. Each component
of such solutions has a specific precipitation or crystallization point at which it can be
selectively removed from the system. The desired separation can be achieved by carefully
monitoring the process temperature. For example, freezing gas-liquor waste streams from
coal-conversion processes crystallizes out water and ammonium bicarbonate at progressively
lower process temperatures. The pure crystals can be separated out from the system. Further
lowering of the temperature then causes precipitation of phenol. Using a similar technique,
impurities and contaminants can be removed from multicomponent solutions. In such cases,
the concentration and type of contaminant in the liquid phase determines the freezing point
of the eutectic composition of the multicomponent system. A multistage crystallization-
melting operation, called zone melting, is used to purify the resulting crystals.27 The mul-
tistage processes are complex, capital intensive, and have high energy consumption. Con-
siderable savings, however, are still achieved by eliminating the need for scraped surface
heat exchangers. The zone-melting multistage freeze concentration processes have been used
commercially for xylene, as well as other organic isomer separations.45
Freeze concentration has potential in the treatment of wastes from many chemical indus-
tries. These waste streams typically contain 1 to 5% organic chemicals. In some cases, the
organic fraction is predominantly acetic acid. Weak, aqueous acetic acid streams are produced
in operations such as fiber spinning and partial-oxidation processes. Separation by freezing
can recover the organic components in these wastes, by crystallizing and separating ice.
According to Heist,45 in the case of acetic acid, no other process is capable of economic
recovery. In addition to recovering economic byproducts, waste treatment prior to its disposal
considerably reduces its BOD requirements, and thus disposal costs are lowered. It also
eliminates problems concerning environmental pollution and human health hazards.

In Pharmaceuticals industry, freeze concentration may find wide uses for concentrating
chemicals that are heat labile. The low process temperatures allow concentration of biological
materials, such as many enzyme preparations that are extremely heat sensitive.
The process has also been tried for concentrating solutions that form gels when cooled.
Since the 17th century, a freezing process has been used in China to obtain agar-agar from
its seaweed source.l05 The process is still used on a home and industrial scale. In this process,
agar-agar is hot extracted from the seaweed. The solution containing approximately 1%
agar-agar is cooled to form a gel. The resulting gel is slowly frozen, thereby allowing the
formation of pure, large ice crystals. The gel is then heated above the melting temperature
of ice. The melt water is drained from the gel under the influence of gravity. Impurities
such as undesirable salts are also removed from the gel during this process. The purified
gel is then dried. Approximately 90% of the water present in the original extract can be
removed during this process of freezing and thawing.
Vahl105 tried a similar process for concentrated gelatin solutions by freezing. Commer-
cially, gelatin is hot extracted from animal bones or skins. The hot extract (approximately
5% gelatin) is concentrated by vacuum evaporation to about 20 to 25% dry matter. The
concentrated solution is cooled and jellified and the gel is then dried at a low temperature.
A major disadvantage of concentration by evaporation is the possible disintegration of the
protein by too-high temperatures, or by too long a retention time combined with high
temperatures. An improvement in quality of the final product, therefore, may be expected
by using the freezing process. However, a process similar to one used for the concentration
of fruit juices, beer, and wine cannot be used for gelatin solution, since they form gels when
cooled to temperatures less than 30°C. The ice crystals formed during the freezing process,
therefore, cannot be separated from the concentrated gel by ordinary centrifuging or wash
column operations. Another problem associated with the concentration of gelatin solutions
by freezing is that the gels swell in cold water. Thus, during the melting of ice crystals, the
gels reabsorb a part of the melt water, thereby showing a dilution effect. Vahl105 observed
that the swelling of gelatin gels depends upon the time that elapses from the melting of the
ice crystals. A concentrated gel, therefore, can be formed if the water is removed quickly
after the melting of ice crystals. The experimental process used by Vahl105 for concentrating
gelatin solutions by freezing is briefly described below.
Gelatin solutions (2 to 5% solids content) were jellied in a plate freezer, especially designed
for these experiments. The gel was then frozen by lowering the temperature of the circulating
cooling liquid. The frozen gel was removed from the freezer and broken down into small
pieces. The ice crystals were melted and the melt water removed from the gel pieces in a
centrifuge. Either cold water sprays or air ventilation during centrifugation could be used
to melt the ice crystals. The amount of run-off water and its gelatin content, as well as that
in the gel after melting, were determined. The results of these experiments are summarized
below.
1. Starting from gelatin solutions of 2 and 4.5% dry solids, concentrated solutions of 14
and 16%, respectively, were obtained.
2. The run-off water from the centrifuge still contained 3 to 5% gelatin.
3. The final concentration of the gelatin solution obtained by the freezing process was
independent of the freezing temperature (and thus, the freezing rate) and the initial
concentration of the solution.
Although concentration of gelatin by freezing seems possible, Vahl105 cites several reasons
against the feasibility of such a process on commercial scale. The capital costs of the
equipment (plate freezer, crusher, centrifuge) are considerably higher than those of a vacuum
evaporator plant. Since the process described above is a discontinuous operation, both
operational and labor costs could be higher. The losses of gelatin in the run-off water are
considerably higher. The final degree of concentration obtained by freezing process is also
lower than that normally obtained in the industrial vacuum evaporators.
E. Soluble Coffee, Tea, and Fruit Juice Powders

The introduction of commercial freeze-drying technology in the mid-1960s had a tre-
mendous impact on fruit product markets. In recent years, both natural and synthetic fruit
juice powders and breakfast drinks are gaining a sizeable proportion of the fruit juice
concentrate market. Although a variety of dehydrated foods such as citrus juices, banana
puree, tomato paste, milk, and eggs are currently manufactured, instant coffee and tea still
remain the principal products in this category. In the U.S., coffee use has tripled since 1920
while population has doubled.77 The gross retail value of coffee sold in the U.S. is about
$10 billion/year and the dollar value of soluble coffee sales alone accounts for more than
25% of the total coffee sales.
Dehydrated powders can be manufactured by using a spray-drying, drum-drying, or freeze-
drying technology. Spray and drum drying are widely used, but have several limitations
when applied to heat-sensitive products and to those susceptible to oxidative deterioration
during the drying process at higher temperatures. Prior to the commercialization of the freeze
drying, the process was also used in the manufacture of soluble coffee. The schematics of
such a process are outlined in Figure 27. The coffee prepared by using the spray-dried
product, however was distinctly inferior in flavor and in aroma to freshly brewed coffee.65
The bulk of the flavor loss in producing soluble coffee by this process, as much as 90% of
the original aroma, occurs during the spray-drying step.77 Apparently most of the aroma
oils and volatiles in the extract are removed along with the water vapor during evaporation.
Partial oxidation and caramelization reactions may also occur, since hot air is used as the
drying medium. The coffee industry, therefore, turned to freeze drying in its efforts to
improve the drying techniques for producing better quality products. In this process, the
water is first frozen as ice in the material and is then removed as vapor (under vacuum) by
sublimation. Except for the substitution of freeze drying for the spray-drying step, the overall
process for the manufacture of soluble coffee has not changed much from that shown in
Figure 27. The equipment and operating costs per pound of water removed, however, are
much greater for freeze drying than for other drying processes, in addition to its other
limitations.
Vacuum drying under frozen conditions proceeds from the outside. The outer layers of
the frozen material, therefore, dry at a faster rate than the inner core. Under vacuum
Green Coffee Beans
i
Blending
Cleaning
Roasting
Grinding
1
Extraction of
• Residue
Soluble Material
I
Spray Drying
1
Aromatization
1
Packaging
FIGURE 27. A schematic representation of preparing soluble coffee by spray drying.

conditions, the thermal conductivity of the deepening shell of dry material is low. Thus, as
drying continues, it becomes increasingly difficult to maintain a proper heat flow into the
frozen core. The rate of freeze drying, therefore, decreases correspondingly.
Mackenzie55 has reviewed various factors that affect the mechanism of conversion of ice
into water vapor during the freeze-drying process. The overall drying times appear to be
very strongly dependent on particle size and on the depth of the bed of particles. The water
molecules evolved from the crystals and the glass-like material pass from the interior of the
particles to the surfaces through voids left behind by ice already vaporized, and even through
the walls of the totally enclosed cavities which previously had been filled with ice. The
longer retention times also cause noticeable flavor changes, although they are much less
than those observed in evaporative drying. Lowering of the water content, i.e., a higher
solids content in the feed, results in decreased heat requirements for water removal during
freeze drying. The overall retention time for the product in the freeze dryer thus could be
lowered, or alternatively, for a similar length of drying cycle, lower temperatures may be
used. A higher total solids content in the frozen mass also provides a greater cross-sectional
area of solid matter for better thermal conductivity. This facilitates an adequate heat flow
into the frozen core without overheating the already dried outer core.
Theoretically, the amount of ice crystals formed when freezing concentrated extract is
much less than when freezing diluted extracts. The number and total surface area of the
voids remaining after sublimation are, therefore, less, and consequently the distance between
the voids is greater. This in turn influences the diffusion of water vapor and organic volatiles
through the solid matter. Since all organic volatiles have molecular weights greater than
water, the greater the distance of travel through the solid matter necessary to reach a void,
the more the larger molecule will be retarded relative to the water molecules. Therefore,
the higher the concentration attained by methods that retain flavor and aroma constituents,
the greater will be the flavor retention through the dehydration stage. Freeze drying of
concentrated extracts thus results in a superior quality product.
Many methods have been tried to preconcentrate the feed prior to freeze drying. Evap-
orative concentration, even with thin-film vacuum evaporators, was found to be undesirable
for aroma-rich, heat-sensitive products like coffee.54 Reverse osmosis, at moderate pressures,
was also tried. Almost all flavor constituents, however, were lost to the permeate leaving
behind a bland extract.
The lower process temperatures and thus better aroma retention during concentration by
freezing made it the preferred method for concentrating coffee extracts prior to drying. It
is also capable of concentrating the extracts to a fairly high degree of solids content. Freeze
concentration followed by freeze drying is, therefore, an economically attractive method of
producing a quality dry-powdered product from an aqueous liquid. The basic differences
between freeze concentration and freeze drying are summarized in Table 19.
Castleton-Hi-Vac Division of Castleton Industries, Inc., Lansdale, Pa. was one of the
first companies to use freeze concentration prior to freeze drying of coffee extracts.54 Their
process consists of partially concentrating the original extract by passing it through a bed
of fresh grounds to about 18 to 20% solids. The extract is then cleared of fine grounds by
centrifugation and clarification. The clarified extract is prechilled in a Votator scraped surface
heat exchanger and then slush frozen in a Contherm (DeLaval) scraped surface vertical heat
exchanger. The ice is separated from the extract slurry in a DeLaval continuous centrifuge,
thereby increasing the solids content of the extract to about 30%. The extract is then passed
through a second Contherm heat exchanger, and the ice slurry produced is separated in a
basket-type centrifuge. The centrifuge wash water is recirculated to recover lost solids. The
ice separated from the product is melted, reheated, and used as make-up water for extracting.
The final extract containing about 40% solids is freeze dried to obtain top quality soluble
coffee. Thus, combining the freeze concentration and freeze-drying steps also minimizes
the operating costs.
Table 19
DIFFERENCES BETWEEN FREEZE CONCENTRATION AND FREEZE DRYING**
Freeze concentration Freeze drying
Materials to which applicable Aqueous liquids Aqueous liquids, purees and

solids
Form of product when process- Concentrated liquid Dry solid
ing is completed
Basic process involved Ice crystallization, followed by Ice crystallization followed by
centrifugation sublimation
Pressure at which process is Above atmospheric Under high vacuum
performed
Temperature at which process is Slightly below freezing point of Below eutectic point or soften-
performed solution but above eutectic ing point of frozen solution
point or softening point
Fraction of initial water content Up to 75% Up to 99%
removable
Water separated from foodstuff Ice crystals Water vapor
in form of
Time to accomplish About I hr overall From 4 to 24 hr
Amount of volatiles lost Essentially none Small amount (in general)
Type of plant operation Usually continuous Usually "batch"
Fruit juice powders can also be prepared in a similar manner to obtain products superior
in flavor and in aroma to those obtained by freeze-drying alone. Taste panel studies have
also proved the superiority of freeze concentrated-freeze dried products over those prepared
by other methods.54-66 Freeze concentration may also be used to preconcentrate the feed
prior to evaporative drying processes, such as spray drying, thereby markedly improving
the flavor profile of final product.77
VIII. QUALITY CONTROL
Fruit juices are primarily valued for their taste, aroma (flavor), texture, and color. Nu-
tritionally, fruit juice provides significant amounts of certain vitamins, and therefore vitamin
retention is also of concern during processing. In addition, microbial spoilage and retaining
the acceptable body (texture) of the product also need to be considered in the quality control
of fruit juices and fruit juice concentrates. Since several fruit juices are quite acidic in nature,
they are capable of dissolving (extracting) metal ions from processing equipment. Such metal
ion extraction is undesirable, since it can impart a metallic taste to the final products and
may catalyze several undesirable changes in color and aroma of the product. This necessitates
use of stainless-steel equipment for processing of fruit juices.
In general, fruit juices that are freeze concentrated exhibit better processing properties
than fruit juices that are concentrated by evaporation and reverse osmosis processes. The
major advantages of the freeze concentration process over the evaporation and reverse
osmosis processes are that it concentrates the fruit juices without appreciable loss in taste,
aroma, color, or nutritive value.4-2022-44-51-52-6466-86-89-91-l07 In this section, some of the factors
that affect the quality of fruit juices are briefly reviewed.
A. Juice Cloudiness
Clear or cloudy juices may be prepared from most fruits. In clear juices, all the insoluble
material is removed by crushing, pressing, and filtering. Cloudy juices are made from citrus
fruits, tomatoes, and pineapples by removal of all the insoluble materials except those small
insoluble particles which will remain suspended in the juice.
Cloudiness of citrus juices is desirable from a consumer viewpoint. The loss of cloudiness
renders the final product unacceptable. The natural fruit enzymes, in particular pectic en-
zymes, affect the consistency of juice products as well as the efficiency of juicing and
clarification operations. A major drawback of the freeze concentration process is that juices
with high concentrations of fibrous and other insoluble matter and pectins cannot be con-
centrated by this process. During the concentration of nectars, obtained by mincing whole
fruit, the insoluble coarse cellular material is lost with the ice. However, if the nondissolved
material is separated from the melted ice in, for instance, a helical cone centrifuge, and is
then fed back to the concentrate, this restriction of the applicability of the freeze concentration
process could be eliminated. The experiments conducted at the Central Food Research
Institute, Hungary4 show that the best way to do this is to concentrate the filtered juice and
then add the fibrous material back to the concentrate.
The loss of cloudiness of citrus juices on storage is attributed to the breakdown of pectins
by pectinesterases. These enzymes have to be inactivated during processing. In a recent
study, Versteeg et al.109 reported three forms of pectinesterases (I, II, and a high molecular
weight form) that accounted for 95% of the total pectinesterase activity in Naval oranges.
These forms were inactivated rapidly at 70, 60, and 90°C, respectively. These investigators
suggested that of these three forms, the one with a high molecular weight, although ac-
counting for only 5% of the total enzyme activity, is responsible for the cloud destabilization
of citrus juices. Therefore, the inactivation of pectic enzymes needs to be controlled, es-
pecially in the manufacture of orange concentrates to avoid gelling during cold storage and
to prevent the juice from losing its uniform cloud on standing.
An alternate approach to cloud stabilization in citrus juices involves the use of pectin
depolymerizing enzymes.16 Limited hydrolysis of pectin to shorter subunits capable of in-
hibiting pectinesterase activity was suggested to be responsible for cloud stabilization in
such treatments.87 Hydrolysates containing polygalacturonic acid residues with an average
degree of polymerization of 8 to 15 were shown to prevent cloud loss. Alternatively,
pectinesterases are also used in the treatment of fibrous apple and peach juice for clarification
purposes.
B. Debittering Citrus Juices

In citrus fruit juices, the bitterness sometimes encountered is primarily due to naringin
and limonin. The removal of these compounds may be accomplished by enzymatic treat-
ments. Biochemical aspects of such processes and the problems associated with them have
been addressed.2595-96108 The use of enzymes in citrus processing has been recently reviewed.24
C. Microbial Spoilage
Most foods of plant and animal origin are subjected to microbial attack as well as physical,
chemical, and biochemical changes. At room temperatures, the microbial attack and the
associated changes play a dominant role in influencing the food quality. During their growth,
microorganisms are capable of releasing enzymes which may alter the color, flavor, texture,
and the appearance of the products, therefore, in most cases, causing deterioration and
spoilage.
Although freezing and subsequent cold storage may inactivate some microorganisms, it
is a relatively slow and variable process. Thus, freezing cannot be relied upon substantially
to reduce bacterial contamination present in the product. Also, several psychrotrophic or-
ganisms can multiply at freezing temperatures. In practice, bacterial growth does not occur
at temperatures below — 10°C. This is probably due to the increasing concentration of soluble
salts and organic compounds in the unfrozen water that lowers its water activity. In this
respect, the lower process temperatures employed during freezing concentration are definite
advantages as compared to processes carried out at ambient temperatures (such as reverse
osmosis).
Table 20
MICROORGANISMS ASSOCIATED WITH SPOILAGE OF
SOME FRUITS AND FRUIT PRODUCTS47-57
Product Microorganism(s)
Oranges (skin surface) Candida krusei, Candida guilliermondii, Candida par-

asipsilosis, Hanseniaspora melligeri, Pichia fermen-
tans, Oospora lactis, Trichosporon cutaneum,
Hansenula anomala, Pullularia pullulans, Alternaria
cilri
Orange juice concentrate Candida tropiealis, Zygosaccliaromyces major, Zygo-
saccharomyees juponicus, Saccharomyces elongaspo-
rus, Torulopsis glabrat, Coliforms, Acetobactor spp.,
Laetobacillus plantarum, Lactobacillus brevis. Leu-
conostoc mesenteroides, Leuconostoc dextranicum.
Streptococcus fecalis var. liquefaciens, Lactobacillus

citrovorum, Lactobacillus buchneri
Raw orange juice Coliforms, Neurospora spp., Penicillium spp., Asper-
gillus spp., and those which occur in orange juice
concentrates
Concentrated lemon juice Candida melibiosi, Candida melinii, Candida pellicu-
losa. Zygosaccharomyces 341Us aceti, Saccharomyces
cerevisiae, Klockera jensenii, Rhodotorula mucilagi-
nosa, Torulopsis citrus
Tomato juice Bacillus thermoacidurans
Grape juice Saccharomyces ellipsoideus, Lactobacillus spp.
Apple juice Lactobacillus. Leuconostoc, Streptococcus, and Pedio-
coccus spp.
Pear juice Lactobacillus, Leuconostoc, Streptococcus and Pedio-
coccus spp.
The primary sources of microbial contamination of fruit juices includes use of poor quality
raw materials and improper sanitary conditions. Inadequate processing and subsequent han-
dling may also contribute to microbial spoilage of the final product. Oftentimes, unpas-
teurized cutback juices are added to concentrates prepared by vacuum evaporation processes
to enhance their aroma profile. This may also become a potential source of microbial
contamination of the final product.
As would be expected, microbial count varies with the type of fruit juice. The different
types of microorganisms associated with selected fruits and their products are summarized
in Table 20. This table is not intended as a complete listing of microorganisms that are
involved in the spoilage of fruit and fruit products; nonetheless, it indicates the tremendous
heterogeneity involved in the microflora associated with these products.
Since fruits and fruit products contain appreciable amounts of sugars as well as high
acidity, microorganisms which tolerate these conditions may survive in such products. The
majority of lactic acid bacteria isolated from fruit juices are heterofermentative, producing
lactic acid, propionic acid, acetic acid, ethyl alcohol, and carbon dioxide.47 In addition to
lactic bacteria, Acetobacter (acetic acid producing) and Clostridia species (butyric acid
producing) may also be involved in the microbial spoilage of fruit juices.
D. Role of Oxygen
Fruits usually maintain low redox potentials. Aeration during extraction of juices, however,
may increase their redox potential. This increase in redox potential favors the growth of
aerobic microorganisms, especially yeasts. The presence of oxygen may also cause oxidation
of vitamin C and off-color and off-flavor developments due to oxidative changes in certain
Table 21
COMPARISON OF THE EFFECTS OF FREEZE CONCENTRATION AND
VACUUM CONCENTRATION ON THE REFRACTIVE INDEX, SUGAR CONTENT,
ACID CONTENT, ASCORBIC ACID CONTENT, AROMA COMPOUNDS
CONTENT, AND pH OF BLACK CURRANT JUICE4
Refractive index Acid content

Total Ascorbic
Liquid Solid sugar Liquid Solid acid Aroma
Test material phase phase (%) phase phase (mg/100 g) (mg/100 g) pH
Initial juice 14.0 9.24 3.72 169.8 13.2 3.10

Frozen
First stage 36.2 1.5 — 9.24 0.09 — — 3.92
Second stage 61.2 1.5 31.23 13.00 0.26 596.2 21.36 2.82
Vacuum concentrated 76.0 38.7 10.64 493.8 2.08 3.06
pigments and flavoring compounds.86 Proper control of aeration is, therefore, necessary
during processing of fruit juices.
E. Nutritional and Organoleptic Quality

In general, nutritional and organoleptic qualities of foods processed and preserved by
freezing are well retained. Available experimental data tend to show that this method of
processing food is less destructive than other processing methods.4-21-22-44-6466-86-89"
Some nutrient losses during processing are inevitable. The process of freezing, as such,
does not alter the nutritive value of the product. However, during some preparative steps
prior to freezing and during subsequent frozen storage, losses may occur in the more labile
vitamins.86 Other nutritional elements, on the whole, remain unchanged. Some selected
examples are discussed here.
Almasi and Perjes4 compared the effects of the freeze concentration and vacuum evap-
oration processes on ascorbic acid and aroma compounds of selected fruit juices. The results
of one such study on concentration of black currant juice are presented in Table 21. Both
the ascorbic acid and aroma compounds were more effectively preserved during freeze
concentration than during vacuum concentration. The reconstituted juices were evaluated
organoleptically for taste, aroma, and color. All concentrates obtained by freeze concentration
were ranked higher than the conventional concentrates. Based on this and similar studies
conducted with juices prepared from strawberries, raspberries, plums, muscat melon, wa-
termelon, sour cherry, apple, and grape, these authors4 recommended a concentration of up
to 40 to 48% followed by cold storage.
That aromas are better retained during concentration of fruit juices by freezing as compared
to other methods is to be expected. The low process temperatures employed during freezing
almost quantitatively retain the low boiling volatile aroma compounds. The only losses that
may occur are soluble solids with the separated ice. Even these losses have been considerably
reduced by controlled crystallization during concentration. Although most studies have em-
ployed organoleptic evaluations as the sole criteria for judging the retention of aroma com-
pounds during concentration, experimental data on flavor profiles of fruit juices as affected
by concentration procedures are sketchy. In general, the method employed to concentrate
fruit juices markedly changes their flavor profiles. For example, Milleville and Eskew61
reported that when apple juice was concentrated by heating under vacuum, the first 10% of
the juice vaporized contained all the volatile flavoring constituents. The physical and chemical
changes that occur during various concentration procedures, therefore, significantly affect
the organoleptic properties of the final product.
One of the authoritative studies in this area was carried out by Bolin and Salunkhe.21
Table 22
AVERAGE VOLATILE RETENTION OF FRUIT
JUICES CONCENTRATED BY VARIOUS
PROCEDURES21
Diffusion Reverse Foam-mat

Freeze membrane Osmosis osmosis dried
Juice (%) (%) (%) (%) (%)
Apple 63 8 12 16 6
Cherry 69 58 44 26 37
Peach 56 35 27 20
Note; Measured changes in all peaks that were large enough to integrate.
Table 23
TASTE PANEL RESULTS OF RECONSTITUTED

CONCENTRATES (CHI-SQUARE VALUES)21
Concentration method
Diffusion- Reverse Foam-mat

Juice Freeze membrane Osmosis osmosis dried
Apple 0.4 0.3 11.4" 1.5 6.0"

Cherry 1.3 1.5 9.4' 0.4 14.2'
Peach 1.3 0 0 10.4-
These authors evaluated various concentration methods (freeze, diffusion-membrane, foam-

mat drying, osmosis, and reverse osmosis) to investigate volatile losses during concentration
of apple, sour cherry, and peach juices. The volatile losses were evaluated by using gas
chromatographic technique. In evaluating the effect of each concentration method on volatile
retention, freezing resulted in the smallest change in chromatographic peaks with a maximum
overall retention (Table 22). The losses of aroma volatiles were only 39 and 31% for freeze-
concentrated apple and cherry juices, respectively, as compared to those for concentrates
prepared by diffusion-membrane, osmosis, reverse osmosis, and foam mat-drying processes.
These authors21 further evaluated the sensory qualities of reconstituted juices using a
triangle taste panel (Table 23). Though juices concentrated by all methods lost some aroma
volatiles, only apple and peach juices concentrated by osmosis and all juices that were
prepared as powders had detectable flavor changes. This indicates that concentrates of fruit
juices prepared by the different methods investigated were essentially as flavorful as the
fresh fruit juices. This is important when one considers the relative economics of different
processes available for fruit juice concentration. Data on the chemical changes during con-
centration of apple, peach, and sour cherry juices by different procedures are summarized
in Tables 24 to 26.
Thus, it has been conclusively proven that concentration of fruit juices by freezing results
in a superior quality product as compared to those prepared by other methods. In addition,
freeze-concentrated juices also have better nutritional quality. This, along with the added
benefit of considerable energy savings, makes freezing a potential method for the concen-
tration of fruit juices and other aroma-rich food liquids.
Table 24
CHEMICAL CHANGES OCCURRING DURING THE CONCENTRATION OF
APPLE JUICE21
Peak areas by concentration methods
Freeze Diffusion- Reverse

Compound Control concentration membrane Osmosis osmosis Powder
Alcohols
Ethyl alcohol 0.16 0.16 0.16 0.06 0.08 0.16
Propyl alcohol 1.50 1.08 0.36 0.30 0.30 0.26
Butyl alcohol 0.32 0.32 0.24 0.20 0.24 0.20
Pentyl alcohol 0.72 0.56 0.36 0.08 0.16 0.16
Aldehyde
n-Hexanal 0.32 0.32 0.20 0.14 0.32 0.26
Esters
Ethyl propionate 0.28 0.06 0.12 — 0.12 0.24

n-Propyl acetate 0.30 0.24 0.56 0.34 0.16 0.30
iso-Butyl acetate 0.24 0.16 0.20 0.20 0.12 0.24
Ethyl butyrate 0.24 0.10 0.24 0.34 0.32 0.22
iso-Butyl propionate 3.00 2.32 0.54 0.98 0.82 0.22
n-Butyl acetate 8.80 5.28 0.64 0.44 1.40 0.08
n-Propylbutyrate 67.84 46.08 2.80 6.56 9.12 0.82
iso-Pentylbutyrate 2.56 1.28 0.16 0.10 0.32 —
n-Pentyl acetate 11.84 10.24 0.80 3.28 3.28 0.12
IX. ECONOMICS
The viability of any process is ultimately determined by the cost of the final product.
Although cost considerations are of prime importance, it is difficult to obtain authoritative
data on this subject. Among the difficulties involved, Karel51 cites the dependence of cost
on a large number of variables: feed concentration, product concentration and maximum
tolerance temperature, and the specific requirements of each process for sanitation, quality,
equipment, and inspection.
Crude estimates for preliminary analyses in designing a freeze concentration system can
be obtained in a number of ways. Probably the simplest system is to use a model binary
system that simulates many of the product characteristics. Solution properties of electrolytes
in water can be predicted by their colligative properties. Using similar data, the temperature-
solubility behavior can be theoretically calculated to near accuracy to predict both temper-
atures and eutectic compositions for most binary systems. Computer programs may be used
to generate the required data. Finally, it is essential to carry out actual laboratory analyses
with real (test) solutions prior to making final decisions. Once the basic data are gathered,
a process can be formulated to achieve the desired goal. Heist45 has summarized the gen-
eralizations for developing a freeze separation system for the chemical industry as follows:
1. Determine the total recovery and at what point during freezing it is economical. Simple
processes can be devised if sufficient recovery could be obtained before the eutectic
point of the system is reached. Multistage systems are more economical for eutectic
separations. The crystal separation should be as nearly ideal as possible, such that the
product-rich stream can be recycled for purification and the unwanted material removed
from the system.
2. If the final crystallization stage is more than 40°F lower than the initial freezing
temperature, then the use of a second-stage crystallization designed to carry half of
Table 25
CHEMICAL CHANGES OCCURRING DURING THE
CONCENTRATION OF PEACH PUREE21
Diffusion- Reverse
Compound Control membrane Osmosis osmosis Powder
Alcohols
Ethyl alcohol 0.32 0.30 0.14 0.04 0.08
Hexyl alcohol 1.12 0.12 0.05 0.05 0.07
Benzyl alcohol 1.31 1.02 0.72 0.33 0.18
Aldehydes
Acetaldehyde 0.46 0.42 0.34 0.10 0.16
Benzaldehyde 1.28 1.26 0.75 0.52 0.49
Esters
Methyl acetate 0.01 0.01 0.01 0.01 0.01

Ethyl acetate 0.72 0.66 0.52 0.54 0.54
Hexyl formate 0.30 0.30 0.30 0.19 0.20
Hexyl acetate 0.50 0.45 0.20 0.15 0.14
trans-2-HexenyI 0.71 0.65 0.45 0.16 0.09
acetate
Ethyl benzoate 0.57 0.38 0.39 0.25 0.11
Benzyl acetate 0.63 0.59 0.34 0.17 0.22
Hexyl benzoate 3.69 3.80 2.19 2.14 1.90
Lactones
ot-Caprolactone 4.00 2.31 1.64 0.96 0.45
a-Heptalactone 0.13 0.06 0.04 0.05 0
a-Octalactone 0.28 0.23 0.10 0.14 0.15
a-Nonalactone 0.48 0.37 0.15 0.19 0.16
a-Decalactone 18.02 6.47 1.20 2.10 0.52
8-Decalactone 5.20 6.28 1.93 1.56 2.02
Caproic acid 0.38 0.22 0.15 0.28 —
a-Pyrone 1.03 0.63 0.15 0.33 —
the freezing heat load is economical due to savings in energy consumption. For small
systems (<500,000 Btu/hr freezer heat load), a single-stage process is most economical.
3. Based on energy requirements, the three-stage systems, unless very large (>25 x 106
Btu/hr freezer heat load), are not economical. These, however, may be used for binary
systems, where a second eutectic point is reached, and it is desirable to separate the
second and third crystals. The addition of a third stage facilitates the production of
the second crystal in stage two independently of the third which are produced only in
stage three.
4. Freezing cycles utilizing the nonscraped surface devices are more economical than
ones using the scraped surface equipment, both from energy and capital investment
points of view.
5. For solid solutions, multistage freeze fractional crystallization processes are better
suited, unless the solid solution concentration of impurities is low enough so as not
to pose major problems during processing.
With slight modifications, a similar approach may be used for formulating a freeze
concentration process for food liquids.
The economics of freeze concentration processes as applied to different food products
have been discussed by several researchers.4-32'4564-66-72-8991'106-'07 In this section, the energy
requirements of freeze concentration process and how the savings are affected will be
discussed.
Table 26
CHEMICAL CHANGES OCCURRING DURING THE CONCENTRATION OF
CHERRY JUICE21
Freeze Diffusion- Reverse

Compound Control concentration membrane Osmosis osmosis Powder
Alcohols
Methyl alcohol 0.52 0.24 0.24 0.16 0.40 0.40
Ethyl alcohol 13.76 3.56 1.68 9.44 2.52 —
1-Propyl alcohol 1.28 1.04 0.82 0.76 0.92 1.06
2-Methyl-l-propyl 1.16 0.94 1.12 0.86 1.16 0.92
alcohol
1-Butyl alcohol 0.50 0.28 0.12 0.64 0.22 0.14
1-Hexyl alcohol 2.80 2.26 0.30 0.76 0.68 —
Aldehydes
Acetaldehyde 0.64 0.52 0.16 0.12 0.20 0.12
Furfuraldehyde 11.12 6.88 5.20 1.44 3.66 4.88
Benzaldehyde 26.88 26.00 22.72 8.00 — 10.64
Esters
Methyl acetate 0.02 0.01 0.01 — 0.02 —
Ethyl acetate 1.08 0.32 0.68 0.60 0.44 0.72
Acetone + isobutyral- 0.04 0.02 0.01 0.01 0.02 0.01
dehyde
A. Energy Requirements
The energy requirements for a freeze concentration process can be broadly divided into
two groups: the process heat loads and those required for other drives such as scraping,
pumping, and mechanical agitation, which add energy, ultimately in the form of heat. The
process heat loads on the freezers consist of the heat of fusion of the crystallized material,
and the sensible heat loads in precooling the process fluid. The ambient heat loads also have
to be removed by the refrigeration systems. The energy requirements of freeze concentration
processes also vary considerably with the process design, i.e., depending upon whether a
single- or multistage design is used. As a general rule, the energy consumption for direct-
contact processes, and for nonscraped heat exchangers, is much lower than that for their
counterpart designs.
Van Pelt107 suggests the concept of "relative energy costs" to calculate energy con-
sumption for different dewatering systems. It may eliminate the differences in fuel prices,
national currencies, and electricity from different sources, existing in different parts of the
world. The concept is based on a ratio as follows:
costs of 1 ton of steam

Ratio R =
costs of 1 kWh electrical energy
The relative energy costs are then defined as follows:
costs of electricity and steam

per ton water removal
Relative energy costs =
costs of 1 ton steam
Based on this concept, Van Pelt107 has calculated the relative energy costs for several
dewatering systems. The data are summarized in Table 27. The energy consumption is
Table 27
RELATIVE ENERGY COSTS FOR DEWATERING PROCESSES107
Relative energy costs for dewatering processes
Rea1 energy
consumption Relative energy costs
kWh/ton kg steam/ton
water water R = 100 R = 200 R = 300 R = 400
Dewatering process removal removal
Evaporation
Effect; 4 1100 1.14 1.12 1.11 1.11
With jet pump 4 550 0.59 0.57 0.56 0.56
With mechanical compression 46 — 0.46 0.25 0.15 0.12
Effect; 6 550 0.61 0.58 0.57 0.57
With jet pump 6 360 0.42 0.39 0.38 0.38

Effect; 8 380 0.46 0.42 0.41 0.40
With jet pump 8 270 0.35 0.31 0.39 0.38
Effect 8 290 0.37 0.33 0.32 0.31
Effect 10 230 0.33 0.28 0.26 0.26
Effect 12 200 0.32 0.26 0.24 0.23
Effect 14 170 0.31 0.24 0.22 0.21
Freeze concentration"
1-stage condensor at +35°C 110 1.10 0.55 0.37 0.28
1-stage condenser at + 10°C 85 — 1.85 0.43 0.28 0.21
4-stage condenser at + 35°C 85 — 0.85 0.43 0.28 0.21
4-stage condenser at + 10°C 60 0.60 0.30 0.20 0.15
Reverse osmosis 10—50 0.1—0.5 0.05—0.25 0.03—0.17 0.02—0.12
- For threefold concentration of wine.

- With use of heat capacity of the ice.
- Total energy requirements: refrigeration + energy requirement for other drives.
greatly influenced by the design for both evaporation and freeze concentration systems. The
relative energy costs are much lower for freeze concentration and reverse osmosis as com-
pared to evaporation processes, since the first two can be operated on a cheaper electrical
energy source.
In a similar study, Van Pelt107 also compared energy requirements for three freeze con-
centration plants designed and developed by Grenco Special Applications, b.v., both on small
and large scale. The characteristics of these plants are summarized in Table 28. In both
cases, the heat of melting the ice crystals was used to partly condense the hot gases of the
refrigerating compressor. The water removal capacity of the three-stage cocurrent plants, as
compared to the single-stage plants, was increased by using an extra wash column in the
first stage and by doubling the amount of scraped surface heat exchangers in the first stage.
Similarly, the amount of scraped surface heat exchangers in the second stage was also
increased by 50%. The energy consumption of these designs per ton of water removed, in
concentrating an aqueous solution from 10 to 50% by weight, is shown in Figure 28. The
multistage processes for both the GFC-W33 and GFC-W60 designs were found to be much
more economical as compared to the single-stage processes. The energy requirements were
lowered by as much as 34 to 40% for multistage cocurrent and by 44 to 50% for multistage
countercurrent processes as compared to the single-stage designs. Almasi and Perjes4 also
reported a 35% savings in power consumption by using a three-stage freezing process to
Table 28
CHARACTERISTICS OF GRENCO FREEZE
CONCENTRATION PLANTS USED FOR
ENERGY CONSUMPTION STUDIES107
Water removal
Grenco capacity
design Type (kg/hr)
GFC-W60
a Single stage • 830
b Three-stage cocurrent 7,000
c Three-stage countercurrent 12,000
GFC-W33
a Single stage 250
b Three-stage cocurrent 2,100
c Three-stage countercurrent 3,600
produce a 60% juice concentrate, as compared to single-stage freezing process. The selection
of an ideal design, therefore, is an important factor which determines the overall energy
requirements and thus the economics of the process.
In addition to basic process design, several process parameters also influence the energy
consumption. Since reduced energy consumption provides economic incentive for the proc-
ess, anything that affects energy requirements becomes an important factor in the evaluation
of the process. Some of the factors that affect power consumption include the initial and
the freezing temperature of the "feed, cooling water temperature, the heat of fusion and the
melting temperature of the crystals, and the heat capacity ratio (Cp/Cv) of the refrigerant.45
Utilizing the latent heat of melting of ice crystals, which is removed during freezing, to
cool some of the process streams considerably reduces energy requirements.
Almasi and Perjes4 studied the power requirements of a freeze concentration process
utilizing the latent heat of melting ice crystals removed during freezing. Since the heat-
absorbing capacity of the ice may be limited, three factors were investigated to study the
energy efficiency of the process. These included precooling of the feed, subcooling the
refrigerant, and cooling the condenser. The energy savings were effected by reducing the
power requirement of the compressor and by reducing the cooling water requirements of
the condenser.
The energy savings were greatly influenced by the method of utilizing the latent heat of
melting of ice. A 7% savings in power requirements of the compressor was achieved when
the entering juice, at 8°C, was cooled to 0°C by the separated ice, compared to when the
feed juice, at 8°C, was fed directly to freezer. The savings were doubled when the entering
juice was at a temperature of 20°C. On the other hand, when the refrigerant was subcooled
with the ice from an initial 8 to 0°C, the savings amounted to only 5 to 8%, as against when
no subcooling was applied. However, when the incoming refrigerant at 20°C was subcooled
to 0°C, as much as 20% energy savings was effected. Based on their results, Almasi and
Perjes4 suggested that the ice may be best utilized during the subcooling of the refrigerant
and that only the residual ice be utilized for precooling of the juice, whenever it is extracted
at room or higher temperatures. Further, about 6% cooling water may be saved, if the melted
ice is recirculated as cooling water for the condenser. Thus, concentration by freezing not
only requires less energy per ton of water removed as compared to the thermal evaporation
processes, but also considerable savings could be achieved by adopting a proper process
design, redesigning the process flows if required, and by utilizing the latent heat of melting
of the separated ice.
300 • = GFC-W 3 3 Units

O= GFC-W 60 Units
•t—' O
c E 200
0 0
E
0 0
O
reqi
D)
o
o
0 ° 100
c
111 1 -
I I I
400 500 600 700 800
Necessary heat removal

(KJ/Kg ice)
FIGURE 28. Total energy requirement per 100 kg water removal as a function of necessary heat removal for
Tcvap = 27°C and T,.,^^^, = + 30°C. A = total energy requirement; B = additional energy requirement; and C
= energy requirement for refrigeration plant. (From Van Pelt, W. H. J., Bull. Grenco Special Applications b.v.,
Netherlands, 1981. With permission.)
B. Overall Process Economics

Typical cost analyses for the concentration of several liquid foods, mostly based on
theoretical calculations, have been reported by several researchers.32-45-64-72-89-91-106-107 Only
selected examples are discussed below.
In a comprehensive study, Thijssen89 compared the cost of concentrating a liquid from
10 to 35% solids for several dewatering systems. The feed rate and the dewatering capacity
were assumed to be, respectively, 1400 kg of liquid food per hour and 100 kg water removed
per hour. The handling costs of the concentrate, costs of floor space, contractor fee, engi-
neering, mounting, and labor costs were not included. The economics were cited for plants
operating continuously for 60 days/year for fruit juices or for 220 days/year for extracts like
coffee and tea. The economical and technical life of the evaporator with aroma recovery,
Table 29
CONCENTRATION COSTS PER 1000 KG OF WATER
REMOVED FOR VARIOUS PROCESSES OPERATED FOR 60
AND 220 DAYS89
$/1000 kg water
60 220
Process Specification days days
Two-stage long tube evapora- Capital costs + maintenance 4.91 1.50

tor with rectification tower Utilities 4.96 4.96
Total 9.87 6.46
Centrifugal film evaporator Capital costs + maintenance 7.03 2.16
with rectification tower Utilities 5.61 5.61
Total 12.64 7.77
Reverse osmosis (4 gal/ft2/ 8.50 2.32
Capital costs + maintenance

day) Utilities 0.11 0.11
Total 8.61 2.43
Reverse osmosis (2 gal/ft-/ Capital costs + maintenance 17.00 4.62
day) Utilities 0.11 0.11
Total 17.11 4.73
Freeze concentration Capital costs + maintenance 8.07 2.49
Utilities 2.73 2.73
Total 10.80 5.22
the reverse osmosis installation, and the freeze concentrator were assumed to be 10 years
and the interest estimated at 10% over the nondepreciated capital. The other assumptions
included the costs of steam, cooling water, and electricity, which were estimated at $2.75/
1000 kg, $0.03/m3, and 0.017/kWh, respectively. The data are summarized in Table 29.
The capital costs for a typical freeze concentration plant were almost double that of a
two-stage, long-tube evaporator with rectification tower. The costs of concentration were
about the same for evaporation and freeze concentration. The higher investment costs for
freeze concentration are partially offset by savings on energy costs. From the data it appears
that reverse osmosis is a competitive process for installations with year-round operation.
The cost of concentration for a reverse osmosis process with a capacity of water removal
of 4 gal/ft2/day is almost half that of evaporation and freeze concentration processes.
Such cost analyses, however, must be considered with respect to the quality of the
concentrate obtained by each of these processes. In freezing concentration, the original
quality of the juice is retained almost quantitatively, thus yielding a superior quality product.
In evaporation processes, thermal decomposition of the product can never be fully avoided.
Even the aroma recovery systems operate at only 50% efficiency.91 Therefore, the original
quality of the juice is never fully restored. On the other hand, commercially available
membranes of acceptable permeabilities are not very selective for the retention of low
molecular weight aroma volatiles. Reverse osmosis, therefore, can be a very promising
dewatering system for liquid foods, such as milk, whose quality is hardly determined by
their volatile constituents.
Even in the dairy industry, freeze concentration can compete with membrane separation
processes, since it can be operated in an absorption cycle using waste heat as low as 130
to 140°F. Moreover, it has the added benefit of being a single-step separation process. For
example, during ultrafiltration of cheese whey, soluble sugars and other low molecular
weight compounds are still lost to the permeate, and require another unit operation if they
are to be recovered. Separation by reverse osmosis of cheese whey, on the other hand, may
not be economical due to high osmolality of cheese whey. The high concentration of proteins
may also cause process problems such as fouling of the membranes.
Table 30
CONCENTRATION OF CHEESE WHEY: FREEZE CONCENTRATION
VS. THERMAL EVAPORATION32
Freeze concentration
Thermal evaporation No waste heat Waste heat available
lb of cheese (whey/day) 1 million I million 1 million

1b of concentrate (45% 133,333 133,333 133,333
total solids/day)
lb of water removed/day 866,667 866,667 866,667
Total Btu required/day 277 million 17.7 million 7.1 million
Steam costs/day 1,102 — —
Electric costs/day 19.00 156.00 64.00
Total energy costs/day 1,121 156.00 64.00
First-year savings
Btu — 78. billion 81. billion

Dollars 289,500 317,100
Membrane separation processes, however, are still economically attractive for the con-
centration of cheese whey. In theory, these processes should be more energy-efficient (since
no change in phase of the solvent is required for dewatering), and the process is quite simple,
requiring only the pumping of liquid over the appropriate membrane surface. In addition,
reverse osmosis will produce very high quality water as the permeate. We have estimated
the operating energy requirements for ultrafiltration of whey to be of the order of 6 x 102
to 5 x 104 kJ/m3 of water removed, or 0.07 to 7 kWh/1000 lb of water removed depending
on the .type of equipment.533 Another estimate for ultrafiltration is about 0.1 to 1.0 hp/hr/
1000 gal of permeate, equivalent to about 0.009 to 0.09 kWh/1000 lb water removed.26
Reverse osmosis, due to the generally lower flux, can be expected to consume about ten
times these amounts, which still makes it less energy consuming than freeze concentration.
Reverse osmosis, however, has several limitations. The maximum solids limit for con-
centrating whey is currently about 18 to 25% total solids. This is due to the high osmotic
pressures developed at the higher concentrations, leading to a dramatic drop in flux or
dewatering rates. Fouling of the membrane by the solids is also a problem and frequent
cleaning is necessary. Also, considerable losses of organic aroma compounds in fruit juices
by permeation through the membrane have been reported.
Davis32 has compared the costs of concentration of cheese whey by thermal evaporation
and freeze crystallization. The comparison included freezing processes using both electric
power and waste heat. The basis was a whey plant concentrating I million lb of raw whey
(containing 6% dissolved solids) per day to a concentration of 45%. The operating conditions
assumed were 20 hr/day and 300 days/year with steam costs as $4.00/106 Btu and electricity
at $0.03/kWh. A typical multieffect evaporator was assumed to use 318 Btu/lb water re-
moved, and an all electric freeze concentration process utilizing 50 kWh/1000 gal of pure
water output. For the waste heat design of the freeze concentration process, the waste heat
was assumed to have no economic value and that an additional 20 kWh/1000 gal of pure
water output was required. The data are summarized in Table 30. The calculations indicated
considerable energy and dollar savings if the freezing process was to be employed. The total
energy costs for a typical freeze separation process were only 14% of those for a thermal
evaporation process. Even these costs could be lowered by more than half by utilizing the
waste heat available within the plant for the freezing process. Thus, savings for over $300,000/
year could be achieved by using the freezing process for the concentration of cheese whey.
With the predicted increase in energy costs in the near future, these savings may become
even greater.
The effects of freeze concentration of coffee extract, prior to its freeze drying, on the
economics of production of freeze-dried coffee were reported by Muller.6466 The capacity
of a given size of freeze dryer can be increased by lowering the water concentration in the
feed to the dryer.22 Freeze concentration is less expensive than freeze drying per pound of
water removed. The total amount of heat which must be added to the freeze dryer may be
reduced by reducing the water removal load through freeze concentration. Therefore, freeze
concentration followed by freeze drying is an economically attractive method of producing
a high-quality dry-powdered product from an aqueous liquid.
X. CONCLUSION
The most popular method of fruit utilization in the U.S. is in the form of frozen fruit
juice concentrates. The major reasons cited for their popularity include reduction in bulk,
cheaper storage and transportation, consumer convenience, and premium economic returns.
Concentration of aqueous foods is a major unit operation in the food industry. Commercially
available processes for the concentration of liquid foods include evaporation, freeze con-
centration, reverse osmosis, and ultrafiltration.
Evaporation is still considered the best developed and economically the most favorable
technique for the concentration of fruit juices. In spite of the thermal instability of the juices,
evaporation well above 30°C, together with distillation as an aroma recovery system, can
be applied without any detectable harmful effects on juice quality, provided other process
parameters are carefully monitored. Even the best of the aroma recovery systems, however,
are not 100% efficient in recovering the delicate flavors. Consequently, there is always
someloss of quality, particularly in case of fruit juices with very delicate flavors, coffee,
tea, and alcoholic beverages. Higher energy requirement is yet another serious drawback of
concentration by evaporation.
Freezing is an energy-efficient process that can concentrate food liquids containing volatile
aromas without any appreciable loss of quality. In the past, the process, however, was
seldom used because of the high investment cost, and the considerable loss of concentrate
in the withdrawn ice. Recent technological developments have minimized these two draw-
backs associated with the earlier freeze concentration processes.
A major advantage of concentration by freezing is that the entire process could be operated
solely on electrical energy. The process also provides great flexibility in terms of products
processed, as well as expansion capabilities without any major alterations in the basic process
design. Also, on a long-term basis, the higher investment costs are overcome by savings in
energy consumption and utilization.
Concentration by phase change of water as in evaporation and freeze concentration proc-
esses, however, requires much energy, and thus it is costly compared to membrane separation
processes such as reverse osmosis and ultrafiltration, where concentration does not involve
a phase change of water. However, commercially available membranes of acceptable perme-
abilities are not very selective for the retention of low molecular weight aroma volatiles.
Similarly, certain nutritive factors such as vitamins and soluble sugars may be lost to permeate
during concentration by membrane processes. A serious drawback of membrane separation
processes is that as the degree of concentration increases, the overriding pressure required
has to be increased proportionately such that the slurry remains pumpable. A higher pressure
in turn can result in the rupturing of membranes. The fouling of membranes by the adsorption
of soluble solids on the inner surface of the membranes also lowers the effectiveness of
these processes. Ultrafiltration has been tried as an intermediate treatment step for juice
concentration, but it cannot be used independently to concentrate fruit juices to an acceptable
degree economically. Nonetheless, reverse osmosis and ultrafiltration are seen as attractive
and very competitive techniques for dewatering of liquid foods, such as milk and whey,
whose quality is hardly determined by their volatile constituents. However, even in these
areas, there is a need to develop porous membranes of sufficiently high selectivity and
capacity and with a reasonable lifetime.
In the coming decade, freeze concentration is seen as a potentially attractive method for
the concentration of aroma-rich liquid floods. In the manufacture of freeze-dried fruit juices,
coffee, and instant tea, partial concentration by freezing prior to freeze drying can consid-
erably lower the process costs. Therefore, freeze concentration followed by freeze drying
is an economic method for producing high-quality dry-powdered products from aqueous
liquids. It could also find wide uses in pharmaceutical industry in concentrating chemicals
that are heat labile, such as enzyme preparations. In the chemical industry, freezing can be
used for the concentration and/or selective crystallization of corrosive inorganic and organic
chemicals. Some uses are also foreseen in the area of waste utilization and disposal.
ACKNOWLEDGMENT
We sincerely thank A. J. Cantrijn and W. H. J. Van Pelt, Grenco Special Applications

b. v., The Netherlands; N. C. Aceto, Manager, Food Products Industry and H. E. Davis,
President, Concentration Specialists, Inc., Andover, Mass.; and H. R. Bolin, Western
Regional Research Center, Berkeley, Calif., for providing useful information. This project
was supported, in part, by Illinois Agriculture Experiment Station, Urbana, Illinois.
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C R C Critical Reviews in Food Science and Nutrition

Freeze concentration of fruit juices

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FREEZE CONCENTRATION OF FRUIT JUICES

Maharashtra State, India

A. Importance of Fruits in Human Diet

B. Early History of Fruit Processing

Nutrient Examples of fruit sources

Sweetened 1 cup 250 86 130 1 Tr 32

C. Consumption Trends and Prospects

Canned 1 cup 251 23 0.5 2380 0.03 0.03 0.5 8'

Meat products 154.49 29.1

Bakery products 55.81 10.5

1975—1976 181,200 242,780 75

1950 1955 1975 1980

II. FRUIT JUICE CONCENTRATION

A. Need for Concentration

Apple juice 12.0

Lemon juice 9.0

Retail price Water content Value of water

Apples 0.39 84 0.32

1. Reduced requirements for storage space by virtue of smaller volumes

Total cost Fuel cost Fuel

1976 58.6 100 11.6 100 20

2. Reduced refrigeration loads

1. Low process temperatures

Category Liquid food Structured food

Concentration processes Evaporation

Fluid-bed drying Freeze drying

B. Historical Developments in the Fruit Juice Concentration Industry

III. CONCENTRATION PROCESSES

evaporation and distillation, pervaporation, and crystallization or freezing. In direct and

A. Evaporation and Distillation

Evaporation is probably the oldest method of concentration known to mankind. Some of

1. The initial temperature of the feed

1. Aroma Recovery in Evaporation Processes

C. Direct Osmosis, Reverse Osmosis, and Ultrafiltration

>• AROMA-RICH PRODUCT

Process Phase I Phase II Phase II formed by:

Fractional distillation (at- Liquid Vapor Evaporation

one that potentially could be operated at a high thermodynamic efficiency.75 Ultrafiltration

IV. THEORY BEHIND FREEZING CONCENTRATION

CONCENTRATING JUICE WITH REVERSE OSMOSIS

Sludge Press Dry Pomace

1. Crystallization and melting (including the eutectic phenomena)

Melting point at 1 atm 0.000°C

-160 120 - I : ' \ '

small amounts of crystals are generated. As crystallization proceeds, the concentration of

where W; = pounds of water removed as ice per pound of feed; Cp = concentration of

For the design and economic operation of freeze separation/concentration processes, it is

Ripening Supercooled feed

A typical freeze concentration system consists of three fundamental components: a crys-

a. Internally Cooled Crystallizers

b. Externally Cooled Crystallizers

1. Crystallizers in which the incoming feed is supercooled

where V = superficial liquid velocity; E = volume fraction of liquid; dp = particle diameter

FIGURE 12. Schematic representation of a flooded

8 7 6 kg rT ice — Ice cone

FIGURE 13. Schematic representation of a typical combination of a press and