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Article history: Although Cleaning-in-Place (CIP) is abundantly used throughout the food industry, it is recognized that
Received 21 April 2017 CIP operations use significant amounts of water and energy. The overall objective of this investigation
Received in revised form was to evaluate parameters needed to improve the effectiveness of water use during CIP pre-rinse. A
20 November 2017
pilot-scale CIP system was operated over a range of Reynolds number (Re) from 16,000 to 260,000, while
Accepted 21 November 2017
evaluating the effectiveness of rinse water to remove a reconstituted skim milk residue film from
Available online 22 November 2017
stainless steel pipe surfaces. Rinse water effectiveness was quantified by comparing the protein con-
centration on the pipe surface after pre-rinse to the initial level. As the Re increased, the effectiveness of
Keywords:
Clean-in-place
rinse step increased, but not in linear proportionality. The efficiency of the rinse water decreased
Rinsing significantly as the volume of rinse water increased. The results of this investigation provide the basis for
Optimization reducing water and energy requirements during CIP operations.
Water conservation © 2017 Elsevier Ltd. All rights reserved.
Milk deposit
https://doi.org/10.1016/j.jfoodeng.2017.11.029
0260-8774/© 2017 Elsevier Ltd. All rights reserved.
M. Fan et al. / Journal of Food Engineering 222 (2018) 276e283 277
For example, Timperley and Smeulders (1987) concluded that flow programmed to be a single-pass step in this experiment, which
velocity had a larger impact on the cleaning rate than Re. The means the rinse water was pumped to rinse the fouled pipe sec-
correlation between wall shear stress (tu ) and the removal of the tions then drained directly without reusing. The contact time be-
foulant from the surface has been demonstrated by many re- tween the rinse water and the pipe sections with deposit films was
searchers (Sharma et al., 1992; Visser, 1970). Lelievre et al. (2002) controlled to 20 s or 60 s during this study. Due to the flow sepa-
demonstrated that both the mean wall shear stress and the asso- ration and gravity, nine velocities levels were achieved in three
ciated time-dependent fluctuation rate would impact the detach- diameter pipes (0.025, 0.035 and 0.050 m) at three system set flow
ment of the foulant under turbulent flow conditions. rates. At the same system set flow rate, the velocity of the flow in
It is important to note that the papers mentioned above were the 0.035 m (1.5 inch) pipe section is highest due to the gravity,
based on the alkaline cleaning step which follows the pre-rinse step while the velocity of the 0.025 m (1 inch) pipe section is the lowest.
in CIP operation. Therefore, results from these studies would serve The pre-rinse experiment was performed three times from which
as good benchmark for investigating the mechanism of pre-rinse three subsamples were obtained under each condition.
step, which has not been studied much by comparison. Further-
more, to our knowledge, there are no prediction models in litera- 2.3. Data treatment
ture to describe the impact of Re and its interactions with other CIP
control parameters on the effectiveness of pre-rinse. Once built, After each CIP pre-rinse, the test sections were disassembled
these models can be used to optimize the CIP pre-rinse step, and the residual deposit film was removed from each pipe section
ensuring rinse effectiveness while reducing water/energy outlay by using a sodium hydroxide solution and the protein was quantified
locating the optimum CIP parameter sets. by Quantipro assay. The effectiveness of the CIP pre-rinse was
The objectives of this investigation were: (1) to establish the determined from the percent residual film, which was calculated by
relationship between rinse water effectiveness and Reynolds comparing the protein content after pre-rinse to the protein con-
Number at various temperatures and contact times, (2) to develop a tent of the deposit film prior to rinsing (Equation (1) and Equation
relationship between the efficiency of water use and rinse water (2))
requirements, and (3) to develop recommendations on CIP pa-
rameters for maximum water effectiveness while reducing water Percent residual film (RF%) ¼ 100 [C/C0] (1)
and energy demands.
Rinse effectiveness ¼ 100 e RF% (2)
2. Materials and methods
Where C (mg cm2) is the protein concentration after pre-rinse and
2.1. Creating the deposit film C0 (mg cm2) is the initial protein concentration.
The efficiency of water consumed during the pre-rinse step was
Rinsing experiments were conducted using pipe sections with evaluated from the rinse effectiveness data. Water efficiency (WE)
known quantities of a deposit film. The deposit film was created was defined as the amount of deposit protein (kg) removed per unit
using an established protocol (Fan et al., 2015). The deposit film was volume (m3) of water, as expressed in Equation (3)
applied to pipe sections with three different diameters: 0.025 m (1
inch), 0.038 m (1.5 inch) and 0.050 m (2 inch). Seven pipe sections WE ¼ PR / WV (3)
of the same diameter were combined to create a test line. The
middle and two end sections of each test line were tested after each Where PR is the mass of protein removed per surface area (kg m2),
experiment. The deposit film contained nonfat-dry-milk (NFDM) which equals to C0 minus C. WV is the volume of rinse water spent
(U.S. Foods, Inc., Rosemont, Ill., U.S.A.) reconstituted to 20% w/w in per surface area (m3 m2).
deionized water at ambient temperature. The pipe sections were As suggested in Equation (4), the volume of water consumed
filled with the reconstituted milk and held for 5 min at room (WV) was computed from the volumetric flow rate (V) of the rinse
temperature. The reconstituted milk was then removed and the water and the contact time (t) between the rinse water and the pipe
pipe sections were allowed to drain at room temperature for section, which was either 20 or 60 s in this study.
30 min. Next, each pipe section was placed in a 75 C oven for
30 min to dry the deposit film. Three pipe sections were selected to WV ¼ (V)(t) (4)
be used in the CIP pre-rinse experiment. The remaining pipe sec-
tions were used to measure the protein content in the initial de- In order to minimize the impact of the system size on the
posit film. The protein content of the deposit film was measured by models, both WE and WV were normalized to per fouled surface
washing the pipe interior using a sodium hydroxide solution. The area. The fouled surface areas were calculated based on the inner
protein assay was completed with QuantiPro™ Bicinchoninic Acid diameter and length of the pipe sections.
(BCA) (Sigma-Aldrich Co.).
2.4. Statistical analysis
2.2. Cleaning-in-place (CIP) pre-rinse
SPSS.21 (IBM, Inc,. USA) statistics software was used for analysis
The cleaning-in-place (CIP) pre-rinse experiments were per- of all data. The data have been reported as the means ± standard
formed by mounting the fouled pipe sections on a test manifold, error. Analysis of covariance (ANCOVA) with 95% confidence in-
which is a part of a pilot-scale CIP system. The CIP system and test terval was used to evaluate the statistical difference of the intercept
manifold were described in Fan et al. (2015). Tap water e pH from and slope between the linear regressions. A one-way ANOVA with a
7.2 to 7.7 (Model HI, 2020; Hanna Instruments, Inc., Woonsocket, 95% confidence interval was used to evaluate the statistical differ-
RI., U.S.A.) e was used in this study. Tap water was recirculated ence between the means.
through the CIP system, except for pipe sections with deposit films,
until the flow rates (0.0016, 0.0028 or 0.0039 m3 s1) and tem- 3. Results and discussion
peratures (22, 45 or 67 C) stabilized. Next, the flow of rinse water
was directed to pipe sections with deposit films. Pre-rinse was The influence of three CIP parameters (temperature, velocity,
278 M. Fan et al. / Journal of Food Engineering 222 (2018) 276e283
4
3.5
ln (Residual Film%)
3
2.5
2
1.5
Ln[RF%]= 3.23 - 1.03 x 10-5 [Re]
1
R² = 0.77
0.5
0
0 20000 40000 60000 80000 100000 120000
Reynolds Number (Re)
Fig. 1. Influence of Reynolds Number (Re) on residual film deposit (RF%) with rinse water temperature of 22 C, and rinse water residence time of 20 s.
M. Fan et al. / Journal of Food Engineering 222 (2018) 276e283 279
Table 1 slopes of different contact times at the same rinse water temper-
ANCOVA results on Regressions of ln (residual film%) over Reynolds Number. ature were not significant. Since the slopes were not significantly
Temperature ( C) Contact time (s) Slope Intercept different, the intercepts of the regression expressions were iden-
22 20 1.03E-05a 3.23 ± 0.14a
tified as an indicator of the rinse effectiveness. Lower values of the
22 60 1.01E-05a 2.99 ± 0.21b intercept suggests the presence of less residual film on the pipe
45 20 6.53E-06b 3.10 ± 0.18b interior surface after rinsing, which meant achievement of better
45 60 6.04E-06b 2.83 ± 0.30c rinse effectiveness.
67 20 4.23E-06b 2.68 ± 0.25c
The impact of contact time on the rinsing effectiveness was
67 60 4.58E-06b 2.73 ± 0.21c
observed in Table 1. The intercept coefficient after 60 s rinsing at
Note- Values with the same superscript letter are not significantly different
22 C was significantly lower than that after 20 s of rinsing at the
(a ¼ 0.05).
same temperature. This indicates that a 60-s rinse at 22 C is
significantly more effective than the 20-s rinse at the same tem-
experiments conducted at higher Reynolds numbers. It needs to be perature. A similar trend was observed on comparison of the in-
noted that extending the contact time from 20 s to 60 s under a high tercepts after 20 and 60 s of rinsing at 45 C. However, when the
level of turbulence (high Re range) did not significantly influence rinse water temperature was increased to 67 C, the difference of
the rinse effectiveness. In another words, the effect of the Re level intercepts between the 20 and 60 s contact times was not signifi-
on rinse effectiveness seems to be the most dominant factor in the cant. These results suggest that rinse effectiveness can be improved
system. If that is the case, it would suggest that longer rinse contact by rinsing for longer periods at 22 and 45 C, but no significant
time is not needed at higher Re level. improvement is achieved when the water temperature is 67 C. It is
A one-way ANOVA with a 95% confidence interval was used to possible that 20 s of contact was sufficient to remove all the water-
analyze the difference in the means of percent residual film after 20 soluble deposit due to the higher diffusivity at elevated tempera-
and 60 s rinsing over the range of Reynolds numbers. Similar to the tures (67 C). Therefore, when the contact time was increased from
results presented in Fig. 1, higher percentages of residual film were 20 to 60 s at 67 C, the rinse effectiveness was not improved. The
removed in experiments conducted at higher Reynolds numbers. It portion of the deposit that was easily soluble in water was removed
was observed that when the Reynolds Number was equal to or after 20 s of contact with rinse water and the portion of the deposit
below 87,380, the effectiveness of rinsing was always significantly attached more tightly to the wall could not be removed even after
improved at longer contact times. Extending the contact time (from 60 s of rinsing. As previously suggested, the deposited film cannot
20 s to 60 s) at higher Re did not significantly influence the rinse be removed by rinse water only, and must be removed by the
effectiveness. This suggests Reynolds number, rather than contact cleaning cycle of the CIP operation (Goode et al., 2013).
time, was the dominant factor impacting rinse effectiveness. The impact of rinse water temperature on the rinsing effec-
Therefore it follows that longer rinse contact times are not needed tiveness is also revealed in Table 1. The slopes of regressions from
at higher Re levels. experiments when rinse water was at 22 C as compared to rinse
This result is consistent with literature. It has been previously water at 45 C were significantly different for both 20 s pre-rinse
suggested that higher turbulence plays a key role in affecting the and 60 s pre-rinse. These observations suggest that the rinse
mass transfer during the initial seconds of contact (Weidemann effectiveness was improved by increasing the rinse water temper-
et al., 2013). According to Goode et al. (2013), there is a point ature from 22 to 45 C. Otto et al. (2014) reported a similar result
during rinse where no further deposit can be removed by water with an approximately 37% increase in cleaning rate of whey pro-
alone and the remaining deposit can only be removed after tein deposit when the temperature of the cleaning fluid was
chemical agents are introduced. It was further stated that all water- increased from 5 to 40 C. These observations indicate that tem-
removable deposit is removed within a short contact time in a high perature of the rinse water impacts the diffusivity of water within
Re system due to the strong physical force introduced by the tur- the deposited film and consequently, influences the rinse water
bulence. The remaining deposit is not removable by rinse water, effectiveness. This is consistent with common observations about
which explains the observation from this study that extended water diffusion into porous media (Rastogi et al., 2002). Higher
contact times do not improve rinse effectiveness. Thus under a high temperatures are expected to enhance the diffusivity of water into a
level of rinse water turbulence, usually measured by a high level of porous media which in this case is the dairy deposit film. Other
Reynolds Number, extending the rinse water contact time is un- researchers have also reported the increase in mass transfer at the
necessary and cannot improve the rinse effectiveness significantly. interface between rinse water and deposit film at higher temper-
atures (Mercade -Prieto and Chen, 2006; Xin et al., 2002). These
studies concluded that high temperature water enhances rinsing
3.2. Combined effect of temperature and contact time on rinse through better mixing and more rapid exchange between film
effectiveness surface and water flowing over the surface (Gillham et al., 1999).
Interestingly, compared to the significant benefits of increasing
Under experimental conditions stated in materials and methods the rinse water temperature from room temperature to an inter-
section, the coefficients of natural log of residual film percentage as mediate temperature of 45 C on deposit removal, increasing the
a function of Reynolds Number were determined at various contact water temperature to the recommended CIP temperature of 67 C
times and temperatures, similar to the regression presented in did not significantly improve the slope of the regression (Table 1).
Fig. 1. These slope and intercept coefficients are reported in Table 1. In other words, the difference between regression slopes for rinse
Higher slope and/or lower intercept of these regressions generally water at 45 C and 67 C was not statistically significant. However,
implies a better rinse effectiveness. The influence of contact time the intercept for a 20-s rinse at 45 C was found to be significantly
and rinse water temperature on rinse effectiveness was evaluated higher than the following-rinsing longer at the same temperature,
by conducting “analysis of the correlation coefficients” (ANCOVA). 20 s at 67 C, and 60 s at 67 C. As mentioned previously, lower
The analysis of covariance (ANCOVA) was used to compare the values of the intercept indicate lower RF% or better rinse effec-
slopes and intercepts of each regression (a ¼ 0.05) and the results tiveness. This suggests that rinse effectiveness was improved by
were presented in Table 1. longer contact times at 45 C. Furthermore, rinse effectiveness was
The results in Table 1 indicated that the differences among not influenced by an increase in temperature from 45 to 67 C when
280 M. Fan et al. / Journal of Food Engineering 222 (2018) 276e283
3.5
3
Ln (Residual Film%)
2.5
1.5
Ln[RF%] = 3.28-0.99 [WV]
1 R² = 0.77
0.5
0
0 0.5 1 1.5
3 -2
Volume of Consumed Water/Fouled Surface Area, WV (m m )
Fig. 3. Improvements in removal of residual film deposits (RF%) with increased water use at rinse water temperature of 22 C and after 20-s rinse water residence time.
the contact time was 60 s. A possible explanation could be that 60 s effectiveness rinsing due to higher mechanical forces, along with
of rinsing is long enough to remove all the water-removable de- better mixing and transfer at the interface between the residue film
posits regardless of the mass transfer rate which is impacted by the and the rinse water.
rinse water temperature. Similar to the linear correlation obtained for 22 C and a 20-s
rinse in Fig. 3, a linear correlation was found between the natural
3.3. Effect of the used water volume on rinse effectiveness logarithm of RF% and volume of water (WV) per fouled surface at
67 C after a 60-s rinse (Eq. (7))
In this section, the correlation between percent residual film
and the volume of water used per fouled surface area was evaluated Ln [RF%] ¼ 2.66e0.3 [WV] (7)
at three different temperatures (22 C, 45 C and 67 C) and two
different contact times. The range of water volumes used per fouled Based on this regression, only 0.38 m3 of water per m2 fouled
surface area was from 0.18 to 3.54 m3 water per m2 fouled surface. surface was needed to remove 87.3% of the residue film. An addi-
The percent residual film (RF%) after the 20 s of pre-rinse at tional 3.7 m3 of water per m2 fouled surface was required to remove
22 C as a function of the volume of water used per fouled area is and additional 8.5% of residue film. This indicates that the water
presented in Fig. 3. A linear correlation was found between the cost increases by nearly 10 times for an improvement in residual
natural logarithm of the residual film (RF%) and the water volume removal from 87.3% to 95.8%. When compared to the film deposit
(WV) per fouled surface area as given by Eq. (6). removed after 20 s of rinse with water at 22 C, improved rinse
effectiveness was achieved with higher water temperatures and
Ln [RF%] ¼ 3.28e0.99 [WV] (6) longer contact times.
Similar regressions were developed for all combinations of
Based on this regression, removal of 79.6% of the film residue contact times and rinse water temperatures. Additional analysis
required only 0.27 m3 of water per m2 fouled surface. However, was accomplished by dividing the regression coefficients into two
removal of an additional 12.7% of the film residue would require groups based on contact times. An analysis of covariance (ANCOVA)
1.24 m3 of water per m2 fouled surface. These results indicate that was used to compare the slopes and intercepts from each regres-
the effectiveness of rinse water decreased as the level of RF% sion (a ¼ 0.05) and the results are presented in Table 2. The results
became smaller. It must be emphasized that relatively small vol- of the analysis indicated that the slopes of the linear regressions
umes of rinse water (0.18 m3 of water per m2 fouled surface) were
required to remove significant amounts (79.6%) of the residue film.
The decrease in effectiveness of the rinse water as larger volumes Table 2
are used suggests that reducing the duration of the rinse cycle ANCOVA results for coefficient for regressions of ln (residual film%) over volume of
would provide an opportunity for significant reduction in water consumed water per unit fouled surface after 20 and 60 s of pre-rinse.
0.7
0.4
rinse water)
[WE] = 0.0495 [WV] -1.41
0.3 R² = 0.83
0.2
0.1
0
0 1 2 3 4
Volume of Consumed Water/Fouled Surface Area, WV (m3 m-2)
Fig. 4. The influence of rinse water volume on the efficiency of residual film removal.
were not significantly different for both contact times and tem- during the initial phases of rinsing, the amount of residue removed
peratures. For the 20-s contact time, the intercept of the linear per unit of water used is largest. Obviously, the initial contact be-
regression decreased significantly when the rinse water tempera- tween water and deposit film is when the efficiency of the rinse
ture was increased from 22 to 45 C and from 45 to 67 C. These water is highest. When the quantities of water used are greater
results suggest that an increase in rinse water temperature from 22 than 1 m3 m2, the water efficiency decreased until it reached a
to 67 C provided an improvement in the effectiveness of rinse relatively low and constant level. Even though the magnitudes of
water at the shorter contact time of 20 s. The same improvement WE continued to be positive, the small WE values may not justify
was not found for the 60 s pre-rinse. It was observed that there was the large quantities of water required (WV) as we move to the re-
no significant difference between intercepts of the linear re- gion in the right of this curve (Fig. 4). In this region, each increment
gressions when the temperature was increased from 45 to 67 C. of deposit removed required a significantly greater amount of
These results suggest that higher temperatures (67 C) do not water.
improve rinse effectiveness when the contact times are relatively These results indicate that the rinse water will continue to
long (60 s). remove film deposits from the pipe surfaces after the water effi-
Based on the results and discussions in this section, it was ciency reach a constant level. The relationship describing the water
concluded that a pre-rinse of 60 s at 67 C is excessive. At these efficiency as a function of water volume used, as given in Eq. (8),
conditions, no significant improvement occurred in deposit must be considered when attempting to optimize the entire
removal. Moreover, these conditions required high energy and time cleaning operation.
inputs. Pre-rinse for 20 s at 45 C would be an appropriate balance
1.41
between rinse effectiveness and energy and time input. A more [WE] ¼ 0.0495 [WV] (8)
specific consideration about water cost and rinse effectiveness is
discussed in next section. In order to evaluate the impact of temperature on water effi-
ciency, the relationships between water efficiency and water vol-
3.4. Changes of rinse water efficiency during the pre-rinse step ume at various temperatures were investigated. In order to change
Eq. (8) into a linear relationship, the natural logarithm was applied
In this study, water efficiency (WE) has been defined as the mass to both water efficiency and volume of water. As reported in Table 3,
of protein film removed per fouled surface area over volume of after the conversion, the natural logarithm of water efficiency
rinsing water per fouled surface area (Eq. (3)). Previous research decreased in a linear fashion (R2 ¼ 0.83) as the nature logarithm of
has indicated that the residue removal rate during the rinse step is water volume increased. The results indicate that the water effi-
not constant (Xin et al., 2002; Weidemann et al., 2013), and the ciency decreased rapidly with an increase in water volume at all
water efficiency (WE) is not expected to be constant. Based on re- temperatures investigated.
sults from this study, as well as observations from other researchers By comparing the slopes and intercepts of each linear regression
(Arnold and Maxcy, 1970; Harper, 1972), longer contact times may
not improve rinse effectiveness when the water temperatures are
high. Optimization of the water rinse step may be achieved by Table 3
knowing the relationship between water efficiency and volume of ANCOVA results on regressions between ln (water efficiency) and ln (water volume/
fouled surface area).
used water.
The results in Fig. 4 illustrate the relationship between water Temperature ( C) Slope Intercept R2
efficiency (WE) and water volume (WV) at 22 C, both WE and WV 22 1.41a 3.01 ± 0.012a 0.83
mentioned here are normalized to per unit of fouled surface area. 45 1.45b 2.94 ± 0.013b 0.83
When the volume of water used was lower, the water efficiency 67 1.45b 2.97 ± 0.014b 0.84
was very high. As the water consumption increased, the efficiency Note- Values with the same superscript letter are not significantly different
decreased rapidly. One interpretation of this relationship is that (a ¼ 0.05).
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