international journal of refrigeration 31 (2008) 1134–1144

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Optimization of the freezing process of red shrimp

(Pleoticus muelleri) previously treated with phosphates

Alex Augusto Gonçalves*, José Luis Duarte Ribeiro

Food Technology Department, Food Science and Technology Institute (ICTA), Federal University of Rio Grande do Sul (UFRGS),
Avenida Bento Gonçalves, 9500 Campus do Vale, Prédio 43212, 91501-970 Porto Alegre, RS, Brazil

article info abstract

Article history: The objective of this paper is the optimization of shrimp freezing process and evaluation of
Received 1 October 2007 the influence of phosphate addition on product yield and quality. A systematic experiment
Received in revised form was conducted to obtain data on yield and quality after the following process steps: immer-
10 March 2008 sion in phosphate solutions, freezing, defrosting, and cooking. The best results were
Accepted 12 March 2008 obtained using phosphate and freezing the shrimps (Pleoticus muelleri) with liquid N2. The
Published online 19 March 2008 use of phosphate was efficient in retaining water during thawing and after cooking. These
results were confirmed with the diminishing of drip loss during thawing and after cooking,
Keywords: and with the increasing of moisture content after immersion.
Shrimp ª 2008 Elsevier Ltd and IIR. All rights reserved.
Phosphate
Quality
Optimization
Freezing
Liquid nitrogen

Optimisation du processus de congélation des crevettes

rouges (Pleoticus muelleri) traité auparavant à l’aide de
phosphates
Mots clés : Crevettes ; Phosphate ; Qualité ; Optimisation ; Congélation ; Azote liquide

1. Introduction accepted are those based on the action of low temperatures,

One essential preoccupation, particularly in the seafood
industry, is to improve conservation technologies of perish-
able foods to reach final products with best possible quality.
Among the various methods currently used, the most
which preserve taste and nutritional value (Chevalier et al.,
2000a,b; Delgado and Sun, 2001; Campañone et al., 2002).
Different equipments have become available for freezing
foodstuffs. Freezer systems can be classified considering
how they extract heat from the product being frozen, i.e., air

* Corresponding author. Tel./fax: þ55 51 30290608.

E-mail address: alaugo@gmail.com (A.A. Gonçalves).
0140-7007/$ – see front matter ª 2008 Elsevier Ltd and IIR. All rights reserved.
doi:10.1016/j.ijrefrig.2008.03.005
 international journal of refrigeration 31 (2008) 1134–1144 1135

blast freezing, contact freezing, immersion freezing, cryogenic freez-

ing and cryomechanical freezing (where the food first undergoes 2. Materials and methods
a cryogenic treatment, then is completely frozen by a mechan-
ical process) (Tanikawa et al., 1985; Sikorski and Kotakowska, 2.1. Experimental design
1990; Garthwaite, 1992; Ogawa and Maia, 1999; Agnelli and
Mascheroni, 2001, 2002; Bevilacqua et al., 2004). In industrial research and development, usually it is necessary
Usually, two types of freezing systems are applied to assist to cope with several factors or variables that affect final prod-
the needs of cold chain in seafood industry: mechanical freezing uct quality. Without the use of an appropriate method, optimi-
(air blast freezing) and cryogenic freezing that uses the direct zation can be time consuming and costly. In this work, the
contact of gases (nitrogen or carbonic gas) and, sometimes, methodology of experimental design was used, which is con-
a cryomechanical freezing. These systems are accomplished sidered an effective alternative for product and process devel-
through freezing tunnels and are not necessarily in the same opment, mainly when a large number of variables is involved
production line, although sometime they exist side by side. (Montgomery, 2001; Rodrigues and Iemma, 2005).
In food processing technology, the freezing process affects This methodology demands time investment in under-
not only frozen food quality but also energy saving perfor- standing the process, defining important variables to be
mance of the freezing equipment (Huan et al., 2003). The studied (solution type, solution concentration, immersion
quality of frozen food is closely related to freezing and thaw- time, freezing type, freezing time), and desirable responses
ing processes. The rate of freezing and formation of small (weight loss, residual phosphate, sensorial attributes).
ice crystals are critical to minimize tissue damage and drip As supported by literature, a correct freezing system choice
loss in thawing (Li and Sun, 2002). It was found that slow freez- and phosphate application before freezing can avoid losses
ing produces intercellular ice crystals with large diameters. An during production and, consequently, contribute for final
increase in freezing rate is followed by a change on ice crystal product yield and quality.
location. The number of crystals increased while their size The first step of the experimental work was the identifica-
decreased. The most intensive fiber damage was found in tion of all experimental parameters of the shrimp freezing
samples frozen at slow rate and the least in samples frozen process. Next, the dominant parameters, which could produce
at fast rate with freezing temperature of 50  C (Sikorski and larger effects on freezing process and the application of phos-
Kotakowska, 1990; Bevilacqua et al., 2004; Li and Sun, 2002; phate, were assigned. Considering those parameters, an
Grujic et al., 1993; Anon., 1998; Molina-Garcia et al., 2004). experimental design was elaborated and real data for yield
Factors that influence the quality of drip losses are numer- calculations in each studied stage (immersion in phosphate
ous and opinions of investigators are partly contradictory. solutions, freezing, thawing, and cooking) was obtained.
However, most of the investigators agree that the quantity
of drip losses during meat thawing is lower if the meat was
frozen at a faster rate (Agnelli and Mascheroni, 2002; Petrovic Table 1 – Process parameters and response variables
et al., 1993; Ngapo et al., 1999a,b).
Process parameters Response variables
In animal products, the signs of damage are seen when the
product is defrosted, with an exudate drained from the tissues X1: shrimp specie Y1: weight after immersion
or collected in pockets inside the product. This is composed of (before shelling)
water where various quantities of crystalline or colloidal X2: % STP (before shelled) Y2: weight after shelling
X3: immersion time Y3: shelling yield
substances are dissolved. The formation of exudate is influ-
(before shelled)
enced by various factors: (a) storage time and temperature X4: type of phosphate Y4: % moisture, % P2O5
prior to freezing; (b) freezing rate (slower freezing rates (STP and Blend) (before shelling)
increase exudation); (c) storage time and temperature after X5: % STP (before freezing) Y5: yields
freezing; (d) defrosting rate (slower defrosting rates increase X6: % blend (before freezing) Y6: weight after immersion
exudation); (d) the conservation method after defrosting (before freezing)
X7: Immersion time Y7: % moisture, % P2O5
(Bevilacqua et al., 2004).
(before freezing) (after immersion,
Phosphates help to restore water binding properties of
before freezing)
seafood. Due to phosphate treatment, natural juices are X8: freezing temperature Y8: weight after freezing
bound and almost no drip losses occur during thawing and (N2 liquid)
further processing. Treated seafood can be juicier, tender X9: freezing temperature Y9: weight after glazing
and maintain the expected nutritional value (Teicher, 1999; (spiral freezer)
Schnee, 2004). However, few studies have been conducted to X10: freezing time Y10: % of ice after glazing
X11: product temperature Y11: % moisture, % P2O5
find optimum phosphate type and concentration, as well as
(before glazing) (after freezing/glazing)
optimum exposure time considering yield and quality of the
X12: immersion time (glazing) Y12: weight after thawing
final product (Applewhite et al., 1993; Aitken, 2001; Neto and X13: thawing temperature Y13: % moisture, % P2O5
Nakamura, 2003). (after thawing)
Based on these considerations, the aim of this paper is to X14: thawing time Y14: weight after cooking
compare two freezing systems used in seafood industry (indi- X15: cooking temperature Y15: % moisture, % P2O5
vidually quick frozen in spiral freezer and cryogenic freezer), (after cooking)
X16: cooking time Y16: sensorial analysis
considering weight loss after freezing, thawing and cooking,
after cooking
and verifying the yield obtained with the use of phosphate.
1136 international journal of refrigeration 31 (2008) 1134–1144
Huan et al. (2003) showed that food shape and size, freezing
air temperature and freezing air velocity are important factors
affecting the freezing process. Among the parameters identi-
fied in the frozen shrimp process (Table 1), initially the specie
of shrimp (X1) was fixed to reduce experimental work. The use
of phosphate (X2) and time of immersion before shelling (X3)
are two parameters usually used in seafood industry due to
their influence in water retention and yield (Y1, Y2, Y3).
Even so, phosphate addition before shelling was not used
in this experiment, because the objective of the work was to
verify phosphate’s effect after shelling and before freezing
process (X5, X6 and X7). In that interval, the action of the
additive is more intense and allows a larger control during
the following process steps. As response variables, % moisture
and % P2O5 before shelling (Y4) were used and compared with
weight after immersion before freezing (Y6) and % moisture
and % P2O5 after immersion before freezing (Y7).
Depending on the type of phosphate (STP and/or Blend) used
(X4), the Yield (Y5) can be different. Few studies about the
behavior of different types of phosphate in different times of im-
mersion have been conducted. These studies shown that the
effectiveness of phosphates concerning water retention depends
on type and amount of phosphate, as well as on seafood type.
In this work phosphate (sodium tripolyphosphate and
blend) of a single company was used. The phosphates used
in the experiments are classified as a food grade additive
and GRAS (Generally Recognized as Safe). So, they do not bring
risk to health.
Delgado and Sun (2001) comment that, since the tempera-
ture distribution within a product varies considerably during
freezing process, freezing time must be defined with respect
to a position.
Type and freezing rate (X8, X9 and X10) are parameters that
deserve attention, because they are largely used in seafood
industry and changes on these parameters will affect yield
(Y5) and quality (Y8).
The glazing system was standardized according to the
industrial process. So, parameters X11 and X12 were kept
constant, as well as the responses Y9, Y10 and Y11. It is known
that glazing process does not affect the study significantly, it is
just used to assure moisture loss by sublimation during frozen
storage, which is an important quality and economic factor in
seafood industry.
Following X4–X10, parameters X13–X16 are the most
important in this investigation. They influence the responses
Y12–Y16, which are the ones that reveal the benefits of this
study to the plant manager and the final consumer.
2.2. Experimental design
According to Dal Molin et al. (2005), the use of design of exper-
iments allows maximum information concerning the effect of
process parameters at a minimum cost (Nanni and Ribeiro,
1987). To achieve the objectives of this work, a design com-
prising factors at more than two levels and adapted to the
reality of the freezing process was used. Initially, a survey in
seafood companies was conducted to identify the usual levels
of each parameter, characterizing the range that would be
interesting to investigate. After this survey, parameter levels
were defined, as listed below:
- Type of solutions: water, sodium tripolyphosphate and blend.
- Concentration of solutions: 0%, 1%, 3% and 5%.
- Immersion time (before freezing): 0, 60, 90 and 120 min.
- Type of freezing: Liquid N2 and spiral freezer.
- Freezing time with N2 (86  C): 1, 2.5 and 4 min.
- Freezing time with spiral freezer (35  C): 10, 12.5 and 15 min.
Next, to quantify the effect of process parameter on
response variables, a fractional factorial project composed of
52 treatments was used (see Table 2). To achieve statistical
significance, each treatment was accomplished in triplicate.
To facilitate regression analysis and model building
process parameters were codified. Phosphate percent, immer-
sion time and freezing time are continuous parameters, so the
codification is proportional to the values that the respective
parameters assume. Freezing type is a two level discrete
parameter, thus 1 was chosen to represent N2 (Nitrogen
freezing) and þ1 was used to represent SF (spiral freezer).
Phosphate type is a three level discrete parameter and the
codification was performed analyzing the effect of the
different levels (water, STP and blend) over the observed
yields (the specified codified values are those which minimize
regression error).
2.3. Randomization
To assure statistical independence of the collected data, the
order of the tests was randomized. After the execution of
the 52 treatments, results were analyzed in function of
process yield (after immersion in phosphate; after freezing;
after glazing; after frozen for 15 days; after thawing; and after
cooking). A multiple regression analysis was used to model
the relationship among process parameters and the yields
mentioned previously.
2.4. Phosphate application method
The red shrimp (Pleoticus muelleri) were obtained from Natu-
brás Pescados Ltda., Piçarras, SC, Brazil, selected, de-headed,
shelled but not deveined or standardized1 in 133 pieces per
kg and then used in this study. This standardization was
made because airflow organization (freezing air temperature
and freezing air velocity) as well as shape and thickness of
frozen food are important factors affecting the freezing
process (Huan et al., 2003). No additives were used during
pre-shipping.
The shrimps (300 g) were immerged in a 1%, 3% and 5%
food grade sodium tripolyphosphate solution (STP, Astaris),
in a 1%, 3% and 5% blend solution (sodium tripolyphospha-
te þ sodium tetra pyrophosphate þ NaCl, Globalfood), and in
control solution (drinking water), both at 2  C for 60, 90 and
120 min according to the procedures proposed by Gonçalves
(2005). Then, the samples were drained for 30 s and submitted
to freezing process. Three replications for each solution were
accomplished.
1
Shrimp are graded in quantity per pound or per kilo and there
is substantial standardization in the grades used throughout the
world. Counts expressed per pound or in kilogram are the usual
standardization measure for trade purposes.
 international journal of refrigeration 31 (2008) 1134–1144 1137

Table 2 – Experimental design

Experimental design (actual levels) Experimental design (codified levels)
a
No. Type Phosphate Immersion Freezing Freezing PT PPER IMERT FTP FT
percentage time type time

1 Water 0 0 N2 1 1.5 1.5 1.5 1 1

2 Water 0 0 N2 1 1.5 1.5 1.5 1 1
3 Water 0 0 N2 4 1.5 1.5 1.5 1 1
4 Water 0 0 N2 4 1.5 1.5 1.5 1 1
5 Water 0 60 N2 1 1.5 1.5 0 1 1
6 Water 0 60 N2 4 1.5 1.5 0 1 1
7 Water 0 120 N2 1 1.5 1.5 1.5 1 1
8 Water 0 120 N2 4 1.5 1.5 1.5 1 1
9 STP 1 60 N2 1 1.15 0.9 0 1 1
10 STP 1 60 N2 4 1.15 0.9 0 1 1
11 STP 1 120 N2 1 1.15 0.9 1.5 1 1
12 STP 1 120 N2 4 1.15 0.9 1.5 1 1
13 STP 3 90 N2 2.5 1.15 0.3 0.75 1 0
14 STP 5 60 N2 1 1.15 1.5 0 1 1
15 STP 5 60 N2 4 1.15 1.5 0 1 1
16 STP 5 120 N2 1 1.15 1.5 1.5 1 1
17 STP 5 120 N2 4 1.15 1.5 1.5 1 1
18 Blend 1 60 N2 1 1.5 0.9 0 1 1
19 Blend 1 60 N2 4 1.5 0.9 0 1 1
20 Blend 1 120 N2 1 1.5 0.9 1.5 1 1
21 Blend 1 120 N2 4 1.5 0.9 1.5 1 1
22 Blend 3 90 N2 2.5 1.5 0.3 0.75 1 0
23 Blend 5 60 N2 1 1.5 1.5 0 1 1
24 Blend 5 60 N2 4 1.5 1.5 0 1 1
25 Blend 5 120 N2 1 1.5 1.5 1.5 1 1
26 Blend 5 120 N2 4 1.5 1.5 1.5 1 1
27 Water 0 0 SF 10 1.5 1.5 1.5 1 1
28 Water 0 0 SF 10 1.5 1.5 1.5 1 1
29 Water 0 0 SF 15 1.5 1.5 1.5 1 1
30 Water 0 0 SF 15 1.5 1.5 1.5 1 1
31 Water 0 60 SF 10 1.5 1.5 0 1 1
32 Water 0 60 SF 15 1.5 1.5 0 1 1
33 Water 0 120 SF 10 1.5 1.5 1.5 1 1
34 Water 0 120 SF 15 1.5 1.5 1.5 1 1
35 STP 1 60 SF 10 1.15 0.9 0 1 1
36 STP 1 60 SF 15 1.15 0.9 0 1 1
37 STP 1 120 SF 10 1.15 0.9 1.5 1 1
38 STP 1 120 SF 15 1.15 0.9 1.5 1 1
39 STP 3 90 SF 12.5 1.15 0.3 0.75 1 0
40 STP 5 60 SF 10 1.15 1.5 0 1 1
41 STP 5 60 SF 15 1.15 1.5 0 1 1
42 STP 5 120 SF 10 1.15 1.5 1.5 1 1
43 STP 5 120 SF 15 1.15 1.5 1.5 1 1
44 Blend 1 60 SF 10 1.5 0.9 0 1 1
45 Blend 1 60 SF 15 1.5 0.9 0 1 1
46 Blend 1 120 SF 10 1.5 0.9 1.5 1 1
47 Blend 1 120 SF 15 1.5 0.9 1.5 1 1
48 Blend 3 90 SF 12.5 1.5 0.3 0.75 1 0
49 Blend 5 60 SF 10 1.5 1.5 0 1 1
50 Blend 5 60 SF 15 1.5 1.5 0 1 1
51 Blend 5 120 SF 10 1.5 1.5 1.5 1 1
52 Blend 5 120 SF 15 1.5 1.5 1.5 1 1

PT, type of solution; PPER, phosphate percentual; IMERT,immersion tim; FTP, freezing type; FT, freezing time; STP, sodium tripolyphosphate; N2,
nitrogen freezing); SF, spiral freezer.
a Done in triplicate.

2.5. Freezing method
Two freezing methods were used: (i) cryogenic freezing, where
samples are frozen in a liquid N2 machine (86  C; air products;
1000 kg h1); and (ii) mechanical freezing, where samples are
frozen in a spiral freezing machine (35  C; Brusinox; 650–4500
kg h1).
According to Regenstein and Regenstein (1991) and Johnston
et al. (1994) the ideal frozen storage temperature is 30  C or
lower. Thus, after freezing process samples were immediately
1138 international journal of refrigeration 31 (2008) 1134–1144

transferred to the static tunnel (30  C) for 1 h to standardize the
freezing step (which is a common procedure in seafood industry).
After core temperature reaches 20  C, samples were weighted.
For best protection of shrimps, samples were submitted to
glazing system, according to Ogawa and Maia (1999), i.e.,
immersion in water at 1  C for 10 s, and then weighted and
stored for 15 days (30  C) until the thawing process.
2.6. Yield during freezing, thawing and cooking
For ease of discussion, in this study the term ‘‘drip’’ is used to
describe exudation both from frozen thawed shrimp (drip)
and from chilled or fresh shrimp (weep).
The yield (weight gain or loss) during freezing, thawing and
cooking was determined according to Ngapo et al. (1999a,b)
and Petrovic et al. (1993) by weighing samples before and after
freezing, before and after thawing, and before and after
cooking. The yields were expressed as percentages of initial
weights and measured as:
Yield ¼ ½ðW0  WF Þ=W0   100 ð%Þ
where W0 is the initial sample weight (in grams) and WF is the
final sample weight (in grams).
According to Johnston et al. (1994) weight may be lost by
dehydration or due to physical damage of seafood during
freezing process. Thus, after storage for 15 days (30  C)
samples were weighed to verify possible weight variations
during storage and then they were placed into a cold room
(4  C) for 24 h for complete thawing, as recommended by
Regenstein et al. (1993), after which they were weighted to
evaluated thawing drip loss.
The cooking drip loss was evaluated as previously
described for the thawing drip. The shrimp were boiled using
the standard cook procedure suggested by Applewhite et al.
(1993). The water was brought to a boil, the shrimp added,
the water returned to boiling and the shrimp boiled for
1 min (total approximately 2 min). After cooking, shrimp
were left at room temperature (24  C) for more than 2 min
before weighting.
Preliminary experiments (Gonçalves, 2005) showed that
the yield did not change after 2 min during cooling at room
temperature. Each experimental value represents the mean
of three determinations.
The weight obtained in each step was used to calculate
the yields: yield after immersion (YAI), yield after freezing
(YAF), yield after glazing (YAG), yield after 15 days storage
(YA15), yield after thawing (YAT), yield after cooking (YAC)
and global yield (YG), i.e., global percentage of weight loss
during the processing, according to Campañone et al. (2002).
To identify the treatments, a five element alpha-numeric
code was used, defining: solution type (water; STP; blend);
concentration of the solution (0; 1; 3; 5%); time of immersion
(0; 60; 90; 120 min); freezing type (N2; spiral freezer); and freez-
ing time (1; 2.5; 4 min to N2 and 10; 12.5; 15 min to SF). For
example, the treatment STP-1-60-SF-10 indicates immersion
in 1% sodium tripolyphosphate solution, time of immersion
60 min, freezing type spiral freezer applied for 10 min.
2.7. Statistical analysis
The yield results in each step were submitted to a Multiple
Regression Analysis using the software SPSS for Windows
and adopting a 0.05 significance level. Treatment averages
were compared through an Analysis of variance (ANOVA)
and effects were considered significant when p-value <0.05.
3. Results and discussion
3.1. Yield before optimization
The average yield results after immersion in water (control),
STP and blend solution (YAI), after freezing (YAF), after glazing
(YAG), after 15 days storage (YA15), after thawing (YAT),

Table 3 – Yields (%) for water treatment

Treatment Observed Predicted by regression models

YAI YAF YAG YA15 YAT YAC YG YAI YAF YAG YA15 YAT YAC YG

W-0-0-N2-1 0.00 2.68 10.03 0.00 3.76 19.7 32.9 0.16 2.36 9.90 0.01 6.57 20.5 33.2
W-0-0-N2-4 0.00 1.20 9.78 0.20 6.41 13.3 24.8 0.16 1.47 9.90 0.28 6.66 14.9 25.6

W-0-60-N2-1 1.33 1.30 10.20 0.00 3.99 26.3 41.4 1.65 1.42 10.07 0.01 8.26 23.8 38.9
W-0-60-N2-4 1.77 0.67 9.87 0.20 6.58 19.0 30.7 1.65 0.53 10.07 0.28 9.04 18.2 31.2

W-0-120-N2-1 3.33 1.30 9.80 0.00 3.27 25.7 36.4 3.46 1.53 10.24 0.01 7.08 23.9 35.9
W-0-120-N2-4 3.77 0.83 10.13 0.78 7.11 18.1 27.8 3.46 0.63 10.24 0.28 8.56 18.3 28.3

W-0-0-SF-10 0.00 2.68 10.03 0.10 10.26 22.8 48.2 0.16 2.36 9.90 0.09 8.90 21.7 45.9
W-0-0-SF-15 0.00 1.10 9.78 0.10 10.73 19.9 41.5 0.16 1.47 9.90 0.18 8.99 17.4 39.8

W-0-60-SF-10 1.56 1.30 10.20 0.00 15.30 18.6 44.7 1.65 1.42 10.07 0.09 12.71 21.6 48.9
W-0-60-SF-15 1.56 0.70 9.91 0.20 17.40 18.4 47.1 1.65 0.53 10.07 0.18 13.49 17.3 42.7

W-0-120-SF-10 3.33 1.30 9.80 0.00 16.12 17.1 41.1 3.46 1.53 10.24 0.09 13.65 18.3 43.2
W-0-120-SF-15 3.56 0.83 10.18 0.20 17.72 10.5 32.4 3.46 0.63 10.24 0.18 15.12 14.0 37.1

Positive and negative values representing, respectively, gain and loss of yield.
 international journal of refrigeration 31 (2008) 1134–1144 1139

Table 4 – Yields (%) for STP treatment

Treatment Observed Predicted by regression models

YAI YAF YAG YA15 YAT YAC YG YAI YAF YAG YA15 YAT YAC YG

STP-1-60-N2-1 2.67 1.30 9.87 0.00 3.95 17.1 24.0 2.75 1.66 10.07 0.01 6.42 16.6 22.2
STP-1-60-N2-4 2.65 0.83 10.22 0.39 4.57 18.5 26.3 2.75 0.77 10.07 0.28 5.82 16.7 22.8

STP-1-120-N2-1 5.10 2.30 10.17 0.39 2.60 14.5 16.9 4.56 2.19 10.17 0.01 4.47 16.7 19.3
STP-1-120-N2-4 4.67 1.93 10.15 0.39 3.24 16.5 20.6 4.56 1.30 10.17 0.28 4.56 16.8 19.8

STP-3-90-N2-2.5 6.23 1.70 9.77 0.00 2.55 13.7 13.9 5.71 2.01 10.05 0.14 4.01 14.3 15.2
STP-5-60-N2-1 6.87 2.30 10.41 0.00 0.64 10.9 8.2 5.88 2.24 10.07 0.01 4.11 11.0 8.4

STP-5-60-N2-4 6.83 1.43 9.65 0.38 1.26 11.5 8.6 5.88 1.35 10.07 0.28 3.51 11.1 9.0
STP-5-120-N2-1 7.73 2.30 10.29 0.00 0.63 9.5 5.6 7.69 2.15 9.90 0.01 2.79 11.1 5.5

STP-5-120-N2-4 7.53 1.00 9.60 0.38 1.46 10.4 6.4 7.69 1.25 9.90 0.28 2.89 11.2 6.0
STP-1-60-SF-10 2.67 1.30 9.87 0.00 5.04 16.6 24.7 2.75 1.66 10.07 0.09 3.80 19.0 28.8

STP-1-60-SF-15 2.88 0.83 10.22 0.20 7.39 17.4 28.1 2.75 0.77 10.07 0.18 3.20 20.4 30.8
STP-1-120-SF-10 4.00 2.37 10.29 0.20 4.60 15.6 22.3 4.56 2.19 10.17 0.09 3.97 15.7 23.1

STP-1-120-SF-15 4.00 1.30 9.91 0.20 6.68 16.6 25.2 4.56 1.30 10.17 0.18 4.06 17.1 25.2
STP-3-90-SF-12.5 5.31 1.90 10.07 0.00 3.64 18.2 22.8 5.71 2.01 10.05 0.14 1.99 17.1 22.2

STP-5-60-SF-10 6.00 2.30 9.87 0.00 2.58 14.8 16.3 5.88 2.24 10.07 0.09 0.56 16.3 17.1
STP-5-60-SF-15 6.00 1.50 9.98 0.19 3.40 16.3 18.4 5.88 1.35 10.07 0.18 0.04 17.6 19.1

STP-5-120-SF-10 7.10 2.30 10.19 0.00 2.55 13.5 13.4 7.69 2.15 9.90 0.09 1.37 13.0 11.4
STP-5-120-SF-15 6.87 1.03 9.85 0.19 3.56 16.3 17.2 7.69 1.25 9.90 0.18 1.46 14.3 13.4

Positive and negative values representing, respectively, gain and loss of yield.

after cooking (YAC) and global yield (YG) are presented in
Tables 3–5, and Figs. 1–3, respectively.
According to Campañone et al. (2002), usual weight loss
during freezing is around 1% and could be larger depending
on equipment type and freezing method. Confirming this
indication, Tables 3–5, present data of YAF and YA15 showing
values around 1% or larger.
Although freezing changes a food product less than other
preservation methods, there may be some dehydration or
water loss leading to quality losses and therefore economic

Table 5 – Yields (%) for blend treatment

Treatment Observed Predicted by regression models

YAI YAF YAG YA15 YAT YAC YG YAI YAF YAG YA15 YAT YAC YG

Blend-1-60-N2-1 3.53 1.50 10.24 0.20 2.61 16.6 20.7 3.19 1.42 10.07 0.01 6.50 15.9 20.5
Blend-1-60-N2-4 3.07 0.83 10.20 0.20 3.04 18.1 23.2 3.19 0.53 10.07 0.28 5.72 16.7 22.1

Blend-1-120-N2-1 5.54 1.90 10.52 0.00 1.72 15.1 15.7 4.99 2.02 10.17 0.01 4.43 16.0 17.6
Blend-1-120-N2-4 5.10 0.83 10.85 0.38 2.55 16.4 17.8 4.99 1.13 10.17 0.28 4.34 16.8 19.2

Blend-3-90-N2-2.5 7.10 1.67 10.34 0.00 1.90 14.2 12.8 7.10 1.47 10.05 0.14 4.22 14.1 14.0
Blend-5-60-N2-1 7.73 1.00 9.98 0.00 1.25 12.8 8.9 8.21 1.33 10.07 0.01 4.74 10.5 6.7

Blend-5-60-N2-4 7.50 0.60 9.94 0.19 1.86 13.3 10.0 8.21 0.44 10.07 0.28 3.96 11.4 8.3
Blend-5-120-N2-1 10.64 1.40 9.35 0.00 1.22 9.9 3.0 10.02 1.31 9.90 0.01 3.31 10.6 3.7

Blend-5-120-N2-4 10.42 0.40 10.08 0.37 1.82 10.5 3.4 10.02 0.42 9.90 0.28 3.22 11.5 5.3
Blend-1-60-G-10 2.90 1.50 10.31 0.00 4.61 19.5 28.6 3.19 1.42 10.07 0.09 2.98 18.8 26.5

Blend-1-60-G-15 2.87 0.60 9.98 0.00 5.64 20.5 30.4 3.19 0.53 10.07 0.18 2.20 21.0 29.7
Blend-1-120-G-10 5.11 1.90 10.54 0.00 4.52 18.7 25.6 4.99 2.02 10.17 0.09 3.03 15.5 20.8

Blend-1-120-G-15 5.30 0.83 10.41 0.19 5.73 19.6 25.6 4.99 1.13 10.17 0.18 2.94 17.7 24.0
Blend-3-90-G-12.5 7.07 1.67 10.53 0.19 3.15 17.6 19.0 7.10 1.47 10.05 0.14 1.30 17.4 20.5

Blend-5-60-G-10 8.00 1.00 9.98 0.00 2.49 15.6 13.6 8.21 1.33 10.07 0.09 0.30 16.3 14.8
Blend-5-60-G-15 7.53 0.60 10.19 0.00 3.12 16.5 15.7 8.21 0.44 10.07 0.18 0.48 18.4 17.9

Blend-5-120-G-10 10.89 1.40 9.35 0.18 2.44 14.8 10.0 10.02 1.31 9.90 0.09 0.98 13.0 9.1
Blend-5-120-G-15 10.67 0.40 10.08 0.00 3.23 15.6 11.1 10.02 0.42 9.90 0.18 0.89 15.1 12.3

Positive and negative values representing, respectively, gain and loss of yield.
1140 international journal of refrigeration 31 (2008) 1134–1144

360

340
A B
320

300
Weight (g)

280

260
W-0-0-N2-1
W-0-0-N2-4 W-0-0-SF-10
240
W-0-60-N2-1 W-0-0-SF-15
W-0-60-SF-10
220 W-0-60-N2-4
W-0-60-SF-15
W-0-120-N2-1 W-0-120-SF-10
200 W-0-120-N2-4 W-0120-SF-15
180
ei l

ei l
on

on
er r

ez er

az r

da e r

aw r

ok r

er r

ez er

az r

da er

aw r

ok r
w nitia

w nitia
m fte

gl Afte

th Afte

co Afte

m fte

gl Afte

th Afte

co Afte
g

g
ys

ys
g

g
g

g
t

t
fre Aft

15 Aft

fre ft

15 Aft
in

in
si

si
gh

in

in

gh

in

in
in

in
im A

im A

A
I

I
Fig. 1 – Shrimp weight variation during water treatment (control), freezing with N2 (A) and freezing with spiral freezer (B).

losses. A non-packed food product, which is warmer than the
surrounding heat transfer medium (air, plate, cryogenic liquid
or gas) begins to dehydrate. This process starts at the surface
and immediately beneath it, followed by water transport from
the inner parts of the product to the surface. The longer the
exposure to conditions causing moisture loss, the higher is
the dehydration loss (Delgado and Sun, 2001).
Petrovic et al. (1993) affirm that quality of frozen meat
products is affected by moisture loss during freezing process.
The succulence decrease and other alterations may occur due
to proteic denaturation. However, the same authors comment
that the amount of drip loss during thawing is minimum if
freezing speed is fast, but losses during cooking can be larger,
which corroborates the results found in Table 3 for the sam-
ples treated with water (control).
The greatest weight losses during thawing and cooking
were registered at slow freezing procedures, i.e., spiral freezer
at 35  C, when compared with cryogenic process at 86  C.
This tendency can be better visualized in Fig. 1, where the
largest losses after thawing and after cooking were observed
in samples frozen with spiral freezer (Fig. 1B). According to
Ngapo et al. (1999a,b) this effect would be explained by the
fact that increasing freezing rate decreases the drip loss.
Chen and Pan (1997) comment that any alteration in storage
temperature causes re-crystallization of ice, which increase in
size due to the diffusion of water around myofibrils. Large ice
crystals cause distortion in the arrangement of seafood muscle
components during slow freezing. With decreasing freezing
temperature and storage, small extra-cellular spaces appear
in the shrimp muscle, but they also conduct to a smaller loss
of water (drip loss) during thawing. Thus, a relationship exists
between freezing and extra-cellular space, where the lower the
freezing temperature, the smaller and more uniform the extra-
cellular spaces, resulting in lower loss of water.
Product frozen at 35  C in the spiral freezer showed
a larger water loss in thawing than that frozen at 86  C

360
A B
340

320
Weight (g)

300
STP-1-60-N2-1
STP-1-60-N2-4 STP-1-60-SF-1
280 STP-1-60-SF-4
STP-1-120-N2-1
STP-1-120-SF-1
STP-1-120-N2-4 STP-1-120-SF-4
260 STP-3-90-N2-2.5 STP-3-90-SF-2.5
STP-5-60-N2-1 STP-5-60-SF-1
STP-5-60-N2-4 STP-5-60-SF-4
240 STP-5-120-SF-1
STP-5-120-N2-1
STP-5-120-N2-4 STP-5-120-SF-4
220
ei l

ei l
on

on
er r

ez er

az r

da er

aw r

ok r

er r

ez er

az r

da er

aw r

ok r
w nitia

w nitia
m fte

gl fte

th Afte

co Afte

m fte

gl Afte

th Afte

co Afte
g

g
ys

ys
g

g
g

g
t

t
fre ft

15 Aft

fre Aft

15 Aft
in

in
si

si
gh

gh
in

in

in

in
in

in
im A

im A
I

Fig. 2 – Shrimp weight variation during STP treatment, freezing with N2 (A) and freezing with spiral freezer (B).
 international journal of refrigeration 31 (2008) 1134–1144 1141

380
A B
360

340

320
Weight (g)

300
BLEND-1-60-SF-10
280 BLEND-1-60-SF-15
BLEND-1-120-SF-10
260 BLEND-1-120-SF-15
BLEND-1-60-N2-1 BLEND-5-60-N2-1
BLEND-3-90-SF-12.5
240 BLEND-1-60-N2-4 BLEND-5-60-N2-4 BLEND-5-60-SF-10
BLEND-1-120-N2-1 BLEND-5-120-N2-1 BLEND-5-60-SF-15
220 BLEND-1-120-N2-4 BLEND-5-120-N2-4 BLEND-5-120-SF-10
BLEND-3-90-N2-2.5 BLEND-5-120-SF-15
200
si r

si r
in r

da fter

in r

da fter
in r

in r

in r

in r
gh l

gh l
in r

in r
ei a

ei a
er Afte

er Afte
ez fte

ez fte
aw fte

ok fte

aw fte

ok fte
az te

a z te
w Initi

w Initi
on

on
gl Af

gl Af
g

ys

ys
g

g
t

t
g

g
fre A

fre A

A
th A

co A

th A

co A
15

15
m

m
im

im
Fig. 3 – Shrimp weight variation during blend treatment, freezing with N2 (A) and freezing with spiral freezer (B).

with the cryogenic system (Fig. 1). This result confirms data The equations obtained were showed below and the predicted
presented by Chen and Pan (1997), which reveal that faster values are presented in Tables 3–5:
freezing produces lower losses during thawing. At the same
YAI ¼ 0:615 þ 3:278  ðPTÞ þ 2:260  ðPT  PPERÞ  1:090
time, little difference was verified in the weight after cooking,
 ðPPERÞ  0:314  ðPPER  PPERÞ þ 1:205  ðIMERTÞ
in spite of the results be better when frozen with N2.
According to Table 4, the samples treated with STP (1)
presented lower losses during the experiment, showing effec- YAF ¼ 3:548 þ 1:411  ðPTÞ þ 0:800  ðPT  PPERÞ  0:145
tiveness concerning water retention. The samples treated  ðPT  IMERTÞ  1:380  ðPPERÞ þ 0:364
with larger concentrations and immersion time show better
 ðPPER  PPERÞ þ 0:173  ðPPER  IMERTÞ þ 0:320
results (lower weight loss).
When comparing freezing systems (N2 vs SF), better results  ðIMERTÞ  0:232ðIMERT  IMERTÞ þ 0:446  ðFTÞ (2)
were obtained using samples treated with larger phosphate YAG ¼ 10:071  0:076  ðPPER  IMERTÞ (3)
concentrations and immersion time and with the N2 freezing
YA15 ¼ 0:135 þ 0:052  ðFTP  FTÞ  0:093  ðFTÞ (4)
system (Fig. 2).
It can be observed in Fig. 2A and B that all sample weights YAT ¼ 3:978 þ 0:723ðPTÞ  0:661ðPT  PPERÞ
were close to the initial value after thawing. Even so, sam- þ 0:234ðPT  IMERTÞ þ 1:289ðPT  FTPÞ
ples frozen with N2 (Fig. 2A) reveal better yield after cooking,
þ 0:261ðPT  FTÞ þ 2:192ðPPERÞ  0:461ðPPER  PPERÞ
probably due to the phosphate percentile and the freezing
 0:176ðPPER  IMERTÞ þ 0:193ðPPER  FTPÞ
type when compared with samples frozen in spiral freezer
(Fig. 2B).  1:021ðIMERTÞ þ 0:637ðIMERT  IMERTÞ
According to Table 5, independent of freezing type (N2 or  0:706ðIMERT  FTPÞ  0:145ðIMERT  FTÞ
spiral freezer), the use of blend was effective concerning water  2:238ðFTPÞ  0:711ðFTÞ
retention after thawing. The variation due to blend percentile (5)
was small. Another aspect observed was that, after cooking,
samples frozen with N2 presented superior yields. YAC ¼ 16:622  0:255ðPT  PPERÞ  0:732ðPT  FTPÞ
In general, the best yields were obtained on samples  1:071ðPT  FTPÞ þ 2:034ðPPERÞ  0:587ðPPER  FTPÞ
treated with phosphate and frozen by liquid nitrogen (Fig. 3). þ 0:709ðIMERT  IMERTÞ þ 1:129ðIMERT  FTPÞ
These finds corroborate studies from Petrovic et al. (1993),  1:211ðFTPÞ  0:328ðFTP  FTÞ þ 0:867ðFTÞ
which affirm that the larger weight losses during freezing,
(6)
thawing and cooking have been registered in processes of
slower freezing.

YG ¼ 26:177 þ 4:181ðPTÞ þ 0:748ðPT  FTPÞ  1:543ðPT  FTÞ

3.2. Multiple regression analysis þ 5:322ðPPERÞ  0:435ðPPER  FTPÞ
þ 1:916ðIMERT  IMERTÞ þ 0:909ðIMERT  FTPÞ
A multiple regression analysis was performed to model the
 4:905ðFTPÞ  0:381ðFTP  FTÞ þ 1:128ðFTÞ
effect of the process parameters on the different measured
yields. The models were built using a 0.05 significance level. (7)
1142 international journal of refrigeration 31 (2008) 1134–1144

where PT is phosphate type, PPER is phosphate percent, IMERT

Table 6 – Optimum settings from regression equations
is immersion time, FTP is freezing type, FT is freezing time. To
use Eqs. (1)–(7) these parameters must be informed in codified Treatment YAI YAF YAG YA15 YAT YAC
levels [1.5; þ1.5] as presented in the left columns of Table 2. Water
The yield after immersion (YAI) is affected by three process 0% Phosphate, 120 min 1.5 1.5 1.50 1 1 28.27
parameter (according to Eq. (1)). It can be observed that YAI immersion time, N2, 4 min
present positive relationship with type of phosphate and freezing time

immersion time. This can be explained since the main function STP
of the phosphate is to increase water holding capacity in 5% Phosphate, 120 min 1.15 1.5 1.50 1 1 5.46
shrimp muscle. On the other hand, YAI has a negative relation- immersion time, N2, 1 min
freezing time
ship with the square of the phosphate percent used, what
reveals that there is an ideal intermediary value for its use. Blend
The yield after freezing (YAF) is affected by four process 5% Phosphate, 120 min 1.5 1.5 1.50 1 1 3.72
parameters (Eq. (2)). YAF adds the effects obtained in YAI, immersion time, N2, 1 min
Freezing time
i.e., whole variables related to YAI are added at the variable
‘‘freezing time’’ that has positive relationship with YAF.
The yield after glazing (YAG) shows a significant relation-
ship with two process parameters (Eq. (3)). The glazing process 3.4. Yields after optimization
is constant for all treatments. It helps to protect the shrimp
frozen with a film of ice, impeding moisture loss for sublima- According to Garrido and Otwell (2004) shrimp processors
tion during posterior storage. It was verified that the interac- should verify the influence of several phosphate types on
tion ‘‘phosphate  immersion time’’ affects YAG, but it can the specific shrimp species that is being processed. Therefore,
be considered a small influence in glazing process. the effect of this additive can vary for different types of prod-
The yield after 15 storage days (YA15) shows a significant ucts, including shrimp species.
relationship with two process parameters (Eq. (4)). The YA15 The results of yields after optimization are presented in
was calculated to verify if the glazing process was well Table 8 and show values closer to theoretical yields foreseen
performed, and if the weight loss did not occurred during the by the regression equations (Tables 3–5).
storage period (15 days at 30  C). The YA15 is negatively In agreement with Tenhet et al. (1981a,b) the main advan-
related with the freezing time, as would be expected. At lower tages of polyphosphates use are decrease of weight loss
freezing times, intramuscular water was not totally frozen and during storage, decrease of drip loss and decrease of weight
may present small variations in weight after the complete loss during cooking. As verified in Table 8, treatments with
freezing. phosphate (STP and blend) were effective in decreasing losses
The yield after thawing (YAT) shows a significant relation- during thawing and cooking when compared with control
ship with five process parameters (Eq. (5)), as well as the yield treatments (immerged in water).
after cooking (YAC) (Eq. (6)). The yield after cooking and the According to Murakami (1994), commercial shrimp (frozen
global yield are related with the capacity of water retention and without phosphate treatment) continues to lose weight
by shrimp muscle (i.e., phosphate application) and the forma- (average loss of 15.6%) during cooking process (4 min),
tion of intramuscular ice crystals during freezing (freezing however, it retains its muscular integrity. The loss found in
type). These phenomena are in agreement with the equations the present work (Table 8) is close to the one reported by
of YAC and YG. Murakami.
Global yield (YG) is the sum of all yields, i.e., accumulated The results showed in Fig. 4 corroborate the considerations
effects of all process parameters. YG showed a significant of Garrido and Otwell (2004): the effect of the phosphate type
relationship with five process parameters (Eq. (7)) after immersion has the same trend observed with control
(water). However, after thawing and cooking, the retention
3.3. Optimization of water stayed constant, and tripolyphosphate (STP) had
lower yield compared with the phosphate blend.
Using multiple regression analysis, as described in Section 3.2, That can be explained by blend composition. The blend
it was possible to find the optimum settings concerning global incorporates other components (sodium tripolyphosphate,
yield (YG). The optimization results appear in Table 6. NaCl and sodium tetra pyrophosphate) that can improve the
The optimum setting considering all immersion alterna-
tives (water, STP and blend) corresponds to shrimp immerged
in a 5% blend solution for 120 min and frozen in N2 (86  C) for
Table 7 – Confirmation tests chosen after optimization
1 min, followed by the shrimp immerged in 5% STP solution
study
for 120 min and frozen in N2 (86  C) for 1 min.
No. Type Phosphate Immersion Freezing Freezing
The optimum setting for immersion in water (control) was
percentage time type time
the shrimp immerged by 120 min and frozen with N2 (86  C)
for 4 min. To verify these findings, additional tests were 1 Water 0 120 N2 1
4 Water 0 120 N2 4
performed. Table 7 presents a summary of the confirmation
7 STP 5 120 N2 1
tests executed, contemplating immersion in water (control)
10 Blend 5 120 N2 1
and the optimum settings for STP and blend.
 international journal of refrigeration 31 (2008) 1134–1144 1143

Table 8 – Yields obtained in confirmation tests

Treatment Observed

YAI YAF YAG YA15 YAT YAC YG

W-0-120-N2-1 3.22 1.4 15.5 0.19 15.5 25.3 45.7

W-0-120-N2-4 3.44 0.97 15.0 0.09 14.2 15.3 34.3
STP-5-120-N2-1 7.22 2.18 15.0 0.09 2.86 9.05 7.92
Blend-5-120-N2-1 8.89 1.63 15.3 0.09 1.87 7.61 2.98

Positive and negative values representing, respectively, gain and loss of yield.

response compared to STP. This result is in agreement with
Garrido and Otwell (2004) findings, which suggested that
phosphates could be involved in a protein cryoprotection
during freezing process.
Studies carried out by Lampila (1993) demonstrated the
synergic effect of the NaCl and phosphate combination in sea-
food processing, indicating an improvement in water reten-
tion and, consequently, in the sensorial quality of the product.
It is interesting to note that, while shrimp tends to lose
water from capture to processing, when it is immersed in
water or in phosphate solutions the muscular tissue re-
hydrates. However, after thawing and especially after
cooking, water is lost from shrimp immersed in water only,
showing that the use of phosphate is important to water
retention and sensory quality of the final product.
4. Conclusions
Based on these results it was possible to conclude that the
use of fast freezing (using N2 liquid) improved process yield
when compared to the use of spiral freezer. We presume
that the best yield obtained with the N2 is due to fast freezing
and low temperature used in this process.
It was observed that the use of phosphate (STP or blend)
before freezing process promoted larger water retention
during thawing and after cooking, increasing process yield
when compared with control samples (immersed in water).
The largest retention of water was obtained with the use of
blend. We presume this is due to the presence of other compo-
nents in the mixture (sodium tripolyphosphate, NaCl and
sodium tetra pyrophosphate) that can improve the response
compared to the isolated tripolyphosphate use.
Besides affecting yield and quality, the freezing process
also influences energy consumption. Therefore the choice of
the freezing process and respective parameters should be
done considering financial and quality aspects.

This paper presented a study of the shrimp freezing process,

including the evaluation of the influence of phosphate addi-
tion on product yield and quality. The results of a designed
experiment were analyzed and multiple regression was used
to model the relationship among process parameters and
yield measured at different process phases. The optimum
settings for process parameters were identified and tested
for validation.
400
Acknowledgements
The authors gratefully acknowledge Mr. José Félix Duarte and
Mr. Eduardo José da Borba Duarte, for opening the company
Natubrás Pescados Ltda. for the execution of this work and
to Mr. Estevam Martins for support provided during the
practical execution of this work. The present study was
carried out with the support of CAPES and CNPq (Brazilian
Research Agencies), which are also acknowledged.

350
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