Processing Engineering School For training purposes only

Cleaning Technology
in Advanced Hygienic Design

Cecilia Svensson
BU DBF

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Why Cleaning?

► Food safety
− No product contamination
− Microbiological safety
− Safe product changes

► Processing equipment
− Remove food residues
− Remove
e o eb biofilm
o on su
o surfaces
aces
− Prolong life time through good maintenance

► Meet legislation and

standards

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Why focus on cleaning?

► Ensure consumer satisfaction

− Food safety, homogeneous product quality,
meet legislation
► Optimize Cleaning
− Maximize up time and minimize down time
− Minimize use of utilities
– Energy
– Water
– Cleaning chemicals
− Decrease the environmental load
− Efficient removal of soil and prevention
of bacterial build up

CIP – an integrated part

of the whole production cycle

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Cleaning in Place
Wh t to
What t remove?
?

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What to remove?

► Different soil from different applications

ex milk, orange juice, tomato ketchup, ice cream

► Different soil from different temperature regions

ex milk storage tanks vs milk pasteuriser

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What to clean?

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Dairy soil

► Cold surfaces - tanks,

t k pumps and
d pipes
i

► Heated surfaces – all surfaces at temperatures >60°C

>60 C

Hot surface

Protein Phosphates Fat

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What to clean?
Type of fouling – Indirect heating systems

► 75°C - 115°C ► 115°C - up

► 50-60% protein ► 15-20% protein
► 30
30-35%
35% minerals ► 70
70-80%
80% minerals
► 4-8% fat ► 4-8% fat

Internal
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Fouling in direct systems

Steam injection mode

► Mixture of fouling type

A and B?

Internal
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What to clean?
A wide range of interest areas
PLEXITY
SOIL COMP

CIP COST
CIP TIME

Internal
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Cleaning in Place
H
How tto clean?
l ?

Internal
Cecilia Svensson/1009

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What is Cleaning in place?

► Manual cleaning or cleaning out of
place – COP
The equipment is dismantled and
manually cleaned after production

► Cleaning in place – CIP

No dismantling of equipment after
production. Cleaned
C by circulation off
cleaning liquids through machines and
other equipment in a cleaning circuit.

Internal
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How can soil be removed?

Thermal force
Mechanical force Chemical force

Soil

Adhesive forces holding soil on surface

Internal
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Sinner’s circle

Internal
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Mechanical cleaning effect

► Mechanical force in CIP is given by shear forces
► High shear forces are achieved at turbulent flow
► Minimum 1.5 m/s flow velocity for adequate mechanical
cleaning effect
1.0
y when fouling

0 75
0.75
o clean at velocity

0.5
Time tto clean / Time to

0.25

0
Timperley D.A, Smeulders C,N.M. 0 0.5 1.0 1.5
Cleaning of dairy HTST plate heat ecchanger: Mean velocity of flow (m/s) Internal
optimization of the single –stage procesedure
Journal Soc. Dairy technology Vol 41 (1) 1988 CSV/2013-09-16 / 15

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Mechanical cleaning effect

► Flow rate needed to achieve 1,5 m/s in
straight smooth pipes

Pipe Diameter Flow Volume

(litres/hour) (litres/100 m pipe)
25.0 mm (1") ~ 2 070 ~ 40

38.0 mm (1_") ~ 5 100 ~ 99

51.0 mm (2") ~ 9 600 ~ 184

63.5 mm (2_") ~ 15 400 ~ 287

76 0 mm
76.0 (3"))
(3 ~ 22 500 ~ 408

101.6 mm (4") ~ 40 200 ~ 748

Internal
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Fluid flow coupled to wall

shear stresses

Internal
Internal
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AG/0409

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Chemical cleaning force

► Alkaline detergent
− Usually sodium hydroxide
hydroxide, NaOH
− Removes protein, fat and sugars i.e. mainly
organic soils

► Acid detergents
− Usually nitric acid, HNO3 , phosphoric acid H3PO4
or citric
it i acid
id (HCl andd H2SO4 corrode
d stainless
t i l
steel)
− Removes mineral soils i.e. mainly in-organic soils

− Some removal of fat, sugar and protein

− Nitric acid at high temperature attacks gaskets
and seals. Never use over 90-95°C.

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Formulated alkaline detergents

Detergent component Example Function
NaOH, KOH
Alkalis Soften/ dissolve organic
Sodium silicates
soil
Sodium carbonate
Enhance soil removal
Builders Phosphates and suspension
properties
EDTA Complexes with calcium
Sequestrants NTA and magnesium

Sodium polyphosphate Prevent scale formation

Wetting - Provide
Surfactants Non ionic - anionic
cleaning efficiency
Hydrogen peroxide Intensifying the cleaning
Oxidizers
Sodium hypochlorite effect
Prevent foaming,
Defoamers, corrosion
Minor components corrosion, prolong
inhibitors, stabilisers
storage

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Soil characteristics
Ease of removal
Soil Solubility
Low temp High temp
Caramelisation, more
Sugar Water soluble Easy
difficult to clean

Water insoluble Easy to Polymerization, more

Fat
Alkali soluble difficult difficult to clean

Water insoluble Denaturation

Protein Alkali soluble Difficult
Slightly in acid Very difficult

Water
W t solubility
l bilit varies
i
Mineral salts Varies Varies
Most are acid soluble

Soluble in water and Easy to Glue-like formation,

Starch
alkali moderate difficult to remove

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Optimum detergent concentration

Milk protein deposit

Source: Cleaning agent concentration and temperature optima in the removal of food Internal
based deposition, M.R. Bird, Proceedings of Fouling and Cleaning in Food Processing
1996 CSV/2013-09-16 / 21

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Optimum detergent concentration

NaOH vs KOH vs formulated detergent

DEMONSTRATION OF CLEANING KINETICS USING A PILOT-SCALE PLATE HEAT EXCHANGER AND IMPLICATIONS FOR DAIRY MANUFACTURERS
M.W. Danne, S.C. Warren, G.C. Knight, J.G. Issa, D.V. Irwin, M.G. Weeks
Fouling, Cleaning and Disinfection in Food Processing 2006, Cambridge, UK,
Eds. D.I. Wilson, J.Y.M. Chew, P.J. Fryer, A.P.M. Hasting
p 245-252

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Thermal cleaning force

► Increased effectiveness of a detergent with

increased temperature
► As a rule of thumb, cleaning with alkaline
detergent should be done at the same
temperature as the product has been exposed
to, but at least 60 °C.
► A formulated detergent always has an optimum
temperature which should be used.
► Acid detergents are recommended to be used
at temperatures of 60 – 85 °C

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Common CIP temperatures

Type of Temperature
Cleaning objects
detergent range (C)
60 80 C
60-80 Milk collection tankers,
tankers tanks and pipes

NaOH 70-90 C Milk pasteurisers

90-140 C UHT plants

60-65 C Tanks, pipes, milk pasteurisers

HNO3
80-85 C UHT plants

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Sinner’s circle

Internal
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Deposit removal as a function of time

1.0
NaOH (g/L)
0.6
0.8
Relatiive residuall soil

1.3
2,5
0.6
5.0
10
0.4

Temp: 65°C
0.2
Velocity:1 m/s

0
5 10 15 20 25 30

Time (min)

From Grasshoff, A. Cleaning of heat treatment equipment, Fouling and Cleaning of Heat treatment Equipment ( ed H. Visser) IDF bulletin
328, pp 32-44, 1997

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Detergents

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Cleaning solutions

Prepared by dilution of concentrates with water

► Pure chemicals
− NaOH (sodium hydroxide)
− HNO3 (nitric acid) or H3PO4 (phosphoric acid)

► or
► Formulated detergents
− Based on NaOH, HNO3, H3PO4 + other cleaning aiding
agents such as tensides, sequestrants
− Ecolab,
Ecolab Diversey
► or
► Pure chemicals + additive
− Formulated detergent prepared on site

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Units for concentration

► mol/L,
mol/L g/L
g/L, weight% (wt%)
(wt%), volume% (vol%)
► Pure chemical concentrates are given in
weight%
g if nothing
g else is declared
► Recommendations for cleaning solution
concentrations are predominantly in weight%
► Formulated detergents: Recommendations for
cleaning concentration in weight%
if nothing else is declared

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Detergent concentrates

► Pure chemicals,
chemicals common concentrations
− NaOH: 25 - 45 wt%
− HNO3 : 52 - 68 wt%
− H3PO4 : 75 - 85 wt%

► Formulated detergents (from e.g. Ecolab or

Diversey)
− always 100%

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Example from Ecolab

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Internal
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Internal
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Internal
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Disinfectants

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Disinfection
► Definition

“Disinfection is a process by which

microorganisms are reduced to a
level that does not compromise
food safety or suitability and is
done by means of chemical
and/or physical methods”

i.e. not the same as

sterilisation
Internal
CSV/2013-09-16 / 36

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Disinfection

Thermal disinfection
► Hot water 90-95°C or steam < 1 bar

Chemical disinfection
► Peracetic acid based
− low corrosion risk if water used for preparation
has max 50ppm Cl-
► Chlorine based
− High corrosion risk
− Sodium hypochlorite: max 150 ppm free chlorine
@ max 40°C for max 20 minutes
− Careful rinse if acid before , chlorine gas
otherwise
Internal
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Comparison between thermal and

chemical disinfection

Properties Thermal Chemical

disinfection disinfection
Effect on bacteria Good Good
Effect on spore None Certain effect
Effect on fungi Good Variable
Leaving chemical residues No Yes
Rinsing with water No Yes
after disinfection
Cooling of equipment after Yes No
Penetration ability Good Poor/None
Corrosive No Yes
Energy consumption High Low

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Novel disinfection
technologies

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Disinfection
► Alternative disinfection methods

► Saving energy
► Saving water
► Saving environmental load

Internal
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Ozonated water (O3)

► Created from o
oxygen
gen and electricit
electricity on
on-site
site
► Ozone dissolved in water
► Strong oxidizer, also effective on spores
► Limited active time (~20 min half time)
► Temperature must be < 25°C
► Work environment can be a problem
► Not commercially available for CIP systems

O
O

O
Internal
CSV/2013-09-16 / 41

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Electrochemically activated
water

► Created from water and salt (usually

sodium chloride) which is passed through
an electrolytical cell
► Hypochlorous acid (HOCl)
(HOCl), hypochlorite
(ClO-) and other substances are formed
► Efficient as disinfectant, generally the
same as other chlorine
chlorine-based
based
disinfectants
► Claimed advantages:
− Produced on site
− No handling of chemicals – only water and
salt

Internal
CSV/2013-09-16 / 42

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Electrochemically activated water

► Very good disinfectant with a

broad spectrum of activity
► Electrolysed water is a chlorine-
based disinfectant
► Presence of chlorine compounds
is always a potential
threat to stainless steel due to the
potential corrosiveness to metal
surfaces

► How do these chemicals affect life

time of the equipment and overall
operating efficiency
efficienc of the line?

Internal
CSV/2013-09-16 / 43

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Water quality
- impact
i t on CIP

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Water

► Dairies use huge amounts of water

► Reduced water consumption is an important
aim in Tetra Pak new developments
p
► Important to have good quality water to
produce high quality products
► Meet drinking water quality
► Water used for e.g.
− Preparation of products
− Cleaning
− Starting up processing equipment
− Flushing out and rinsing
− Etc……

Internal
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Water quality
- Hardness
► Water hardness – the amount of Ca2+ and Mg2+
− Temporarily hardness – carbonate hardness
− Permanent hardness – non-carbonate hardness
− Total hardness = temporary + permanent

► Several units for water hardness

− 1°dH German degree = 17,9 mg CaCO3/l

► Classification
− Soft water : 0 – 6 °dH
− Medium hard: 6 – 12 °dH
− Hard water: 12 – 18 °dH
− Very hard: > 18 °dH

Internal
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Water hardness and scaling

- Influence on cleaning
► Ca(HCO3)2 precipitate when heated (scaling)
− Ca(HCO3)2 CaCO3 (s) CO2(g) + H2O
► Process plants rinsed with hot hard water or thermally
di i f t d will
disinfected ill b
be covered
d with
ith precipitated
i it t d C
CaCO
CO3
► React with detergents and forms insoluble salts which
reduces cleaning efficiency
► However easily dissolved with acids under formation of
carbon dioxide and soluble calcium salts
► Hard
H d water
t needs
d tto b
be softened
ft d

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Water hardness and scaling

- Example of scaling issue
► Bactofuge disks after
cleaning sequence
ended with rinse with
h d water
hard t

► Bactofuge disk after

cleaning sequence has
been aborted during
last acid step

Internal
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Water quality
- other issues
► Corrosion risks
− High chloride content may cause corrosion of stainless steel
Chloride content Max. value [Cl-] Max. value [Cl-]
(
(ppm)) AISI 304 (
(ppm)) AISI 316
Temperature <60 ºC 30 30
Temperature 60-100 ºC 20 30
Temperature 100-120 ºC 10 30
Temperature 120-140 ºC 5 10
Temperature 140
140-160
160 ºC
C 1 5

− Chlorine max 0,2 ppm residual in water supply. Over 2ppm

could initiate corrosion
− Low pH in water may also be a cause of corrosion

► Discoloration of stainless steel Internal

CSV/2013-09-16 / 49

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Tetra Pak Design criteria on water

Parameter Unit Tetra Pak general design criteria
Max. value

Total hardness º dH 4-7

Alkalinity (HCO3) mg/l 30-120
Chloride (Cl-) mg/l 30.00 ( depending on temperature)
Chlorine (Cl2) mg/l 0.20
Sulphate (SO4) mg/l 100 00
100.00
Aluminium (Al) mg/l 0.10
Iron (Fe) mg/l 0.10
Manganese (Mn) mg/l 0.05
pH 7-8.5

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Preparation of
cleaning solutions
Calculations
C l l ti off concentrate
t t
volumes

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Preparation of cleaning solutions

► Cleaningstations e.g.
e g Tetra Alcip
► Header batch system e.g. TA Flex & TA VTIS

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Calculations for preparation of cleaning solutions

Cl
Cleaning
i station
t ti

► Addition of concentrate into a fix water volume 

detergent volume = water + detergent concentrate
m det  c det  m conc  c conc
m water  m conc   cdet  m conc  c conc
Vwater  ρ water  Vconc  ρ conc   cdet  Vconc  ρ conc  cconc
Vwater
Vconc  ater
ρ conc c conc
(  1)
ρ water c det

mdet=mass of prepared detergent (kg)

mconc=mass of concentrate (kg)
mwater=mass of water (kg)
Vconc=volume of concentrate (L)
Vwater=volume of water (L)
conc=density of concentrate (kg/dm3, kg/L)
water=density of water (kg/dm3, kg/L)
cconc=concentration of concentrate (wt%)
cdet=concentration of desired detergent solution (wt%)

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Possible errors – Cleaning station

► Ex.2wt% NaOH, NaOH det= 1,019kg/dm3 to be prepared from
2000L water and 32wt% NaOH concentrate, NaOH conc=
1 37kg/dm3
1,37kg/dm

► Concentration of concentrate is assumed to be in vol% or the

higher density of concentrates are neglected
2000 133.3 1.37  0.32
Vconc   133.3L  c det   2.7 wt%
1.0  0.32 
  1
2000  0.998  133.3 1.37 
1 0  0.02 
1.0
► Correct calculation

2000
Vconc   97.3L
1.37  0.32 
  1
1.0  0.02  Vwater
Vconc 
ρ conc c conc
(  1)
ρ water c det

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Calculations for preparation of cleaning solutions

H d b
Header batch
t h

► Addition of concentrate into a fix plant volume 

plant volume = detergent volume

m plant
l  c det
d  m conc  c conc

Vplant  ρ det  c det  Vconc  ρ conc  c conc

Vplant  ρ det  c det
Vconc 
ρ conc  c conc

mplant =mass of plant filled with detergent (kg)

mconc =mass of concentrate (kg)
Vconc =volume of concentrate (L)
Vplant =volume of plant (L)
conc =density of concentrate (kg/dm3, kg/L)
det =density of detergent (kg/dm3, kg/L)
cconc =concentration of concentrate (wt%)
cdet =set point of detergent concentration (wt%)

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Possible errors – Header batch

► Ex. 2000L 2wt% NaOH, NaOH det= 1,019kg/dm3 to be prepared
from 32wt% NaOH concentrate, NaOH conc= 1,37kg/dm3

► Concentration of concentrate is assumed to be in vol% i.e. no

densities are used in calculations
2000  0.02 125  0.32 1.37
Vconc   125L  c det   2.7 wt%
0.32 2000 1.027
► Density of final detergent is assumed to be equal to water

2000  0,998  0.02 91.1 0.32 1.37

Vconc   91.1L  c det   1.96 wt%
1.37 
► Correct calculation0.32 2000  1.019

2000 1.019  0.02

Vconc   93.0L
1 37  0.32
1.37 0 32 Vplant  ρ det  c det
Vconc 
ρ conc  c conc

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Calculation tools

Internal
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Density of NaOH solutions 0.5-4 wt% (5-40g/L)

NaOH conc T=25°C NaOH conc T=25°C
3 3
wt% Density g/dm g/L Density g/dm
0,5 1002,7 5 1003,8
0,6 1003,8 6 1004,8
0,7 1004,9 7 1005,8
0,8 1006,0 8 1006,8
0,9 1007,0 9 1007,8
1 1008,1 10 1008,8
1,1 1009,2 11 1009,7
1,2 1010,3 12 1010,7
1,3 1011,4 13 1011,7
1,4 1012,5 14 1012,7
1,5 1013,6 15 1013 7
1013,7
1,6 1014,7 16 1014,7
1,7 1015,8 17 1015,7
1,8 1016,9 18 1016,7
1,9 1018,0 19 1017,6
2 1019,1 20 1018,6
2,1 1020,2 21 1019,6
22
2,2 1021 3
1021,3 22 1020 6
1020,6
2,3 1022,4 23 1021,6
2,4 1023,5 24 1022,6
2,5 1024,6 25 1023,6
2,6 1025,7 26 1024,6
2,7 1026,7 27 1025,5
2,8 1027,8 28 1026,5
29
2,9 1028 9
1028,9 29 1027 5
1027,5
3 1030,0 30 1028,5
3,1 1031,1 31 1029,5
3,2 1032,2 32 1030,5
3,3 1033,3 33 1031,5
3,4 1034,4 34 1032,5
3,5 1035,5 35 1033,5
3,6 1036,6 36 1034,4
3,7 1037,7 37 1035,4
3,8 1038,8 38 1036,4
3,9 1039,9 39 1037,4 Reference : International Critical
4 1041,0 40 1038,4 Tables (1928), vol.III, p.79

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Density of HNO3 solutions 0.5-4 wt%(5-40 g/L)

HNO3 T=25°C
T 25 C HNO3 T=25°C
3 3
wt% Density g/dm g/L Density g/dm
0,5 999,5 5 999,8
0,6 1000,1 6 1000,3
0,7 1000,6 7 1000,8
0,8 1001,2 8 1001,3
0,9 1001,7 9 1001,9
1 1002,3 10 1002,4
1,1 1002,8 11 1002,9
1,2 1003,4 12 1003,4
1,3 1003,9 13 1004,0
1,4 1004,5 14 1004,5
1,5 1005,0 15 1005,0
16
1,6 1005 6
1005,6 16 1005,5
1,7 1006,1 17 1006,1
1,8 1006,7 18 1006,6
1,9 1007,2 19 1007,1
2 1007,8 20 1007,6
2,1 1008,3 21 1008,2
2,2 1008,9 22 1008,7
2,3 1009,4 23 1009 2
1009,2
2,4 1010,0 24 1009,7
2,5 1010,5 25 1010,3
2,6 1011,1 26 1010,8
2,7 1011,6 27 1011,3
2,8 1012,2 28 1011,8
29
2,9 1012 7
1012,7 299 1012,4
0 ,
3 1013,3 30 1012,9
3,1 1013,8 31 1013,4
3,2 1014,4 32 1013,9
3,3 1014,9 33 1014,5
3,4 1015,5 34 1015,0
3,5 1016,0 35 1015,5
3,6 1016,6 36 1016 0
1016,0
3,7 1017,1 37 1016,6
3,8 1017,7 38 1017,1
39 1017,6 Reference : International Critical
3,9 1018,2 Tables (1928), vol.III, p.58
4 1018,8 40 1018,1

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Density of H3PO4 solutions 0.5-4 wt%(5-40 g/L)

H3PO4 T=25°C
T=25 C H3PO4 T=25°C
T=25 C
3
wt% Density g/dm3 g/L Density g/dm
0,5 999,8 5 1000,1
0,6 1000,3 6 1000,6
0,7 1000,8 7 1001,1
0,8 1001,4 8 1001,6
,
0,9 1001,9, 9 1002,1
00 ,
1 1002,5 10 1002,6
1,1 1003,0 11 1003,2
1,2 1003,6 12 1003,7
1,3 1004,1 13 1004,2
1,4 1004,6 14 1004,7
1,5 1005,2 15 1005,2
16
1,6 1005 7
1005,7 16 1005 7
1005,7
1,7 1006,3 17 1006,2
1,8 1006,8 18 1006,8
1,9 1007,3 19 1007,3
2 1007,9 20 1007,8
2,1 1008,4 21 1008,3
2,2 1009,0 22 008,8
1008,8
2,3 1009,5 23 1009,3
2,4 1010,0 24 1009,8
2,5 1010,6 25 1010,4
2,6 1011,1 26 1010,9
2,7 1011,7 27 1011,4
2,8 1012,2 28 1011,9
2,9 1012,7 29 1012 4
1012,4
3 1013,3 30 1012,9
3,1 1013,8 31 1013,4
3,2 1014,4 32 1013,9
3,3 1014,9 33 1014,5
3,4 1015,5 34 1015,0
35
3,5 1016 0
1016,0 35 1015,5
3,6 1016,5 36 1016,0
3,7 1017,1 37 1016,5
3,8 1017,6 38 1017,0 Reference : International Critical
3,9 1018,2 39 1017,5 Tables (1928), vol.III, p.¨61
4 1018,7 40 1018,1

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Measurement of
concentration

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Measurement of concentration

► Electrical conductivity – inline indirect

method
► Titration – laboratory
y method

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Electrical conductivity

► Ability of a solution
solution, metal or gas to pass an electric current
► Dependent among others on concentration of components
in the solution
► Indirect
I di t way to t measure concentration
t ti
Conductivity vs concentration @ 25°C

300,0

250,0
Conductivitty (mS/cm)

200,0

150,0

100,0

50,0
,

0,0
0,00 1,00 2,00 3,00 4,00 5,00
Concentration (wt%)

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Electrical conductivity
T
Temperature
t dependency
d d

► Conductivity is very
temperature-dependent 250
► Impossible to compare
conductivity values at 200

m)
nductivity (mS/cm
differing temperature 150
► Solution: Recalculate
conductivity to what it 100
should have been at 25°C

Con
2wt% NaOH
50
(reference) by using
detergent-specific -values 0
► -values describes the 0 20 40 60 80 100 120
temperature dependence Temperature °C

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Electrical Conductivity
A
Accurate
t measurementt

► Foraccurate detergent
g preparation,
p p , temperature
p
compensation needs to be correct.

Temperature °C 
Conductivity  at C   
25  Conductivity @ 25°C
-value 1  (  25 )
100

► Temperature dependence is different from

detergent
d t t to
t detergent
d t t thus
th different
diff t -values
l

(    25 ) 100
 25C  =conductivity at °C
25=conductivity at 25°C
 25  (  25)
Internal
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Temperature compensation coefficients

Temperature
Detergent
comp. coefficient
NaOH = 1.7 % /°C

HNO3 = 1.3 % /°C

 = -0,01*T + 1,17
H3PO4 i @ 50°C =
i.e.  0,7
0 7 % /°C

Ecolab P3 MIP SP = 1.8 % /°C

Ecolab P3 MIP CIP = 1.5

1 5 % /°C
/ C

Internal
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Conductivity
Concentration determination

Conductivity vs concentration @ 25°C

300,0

250,0
Conductivitty (mS/cm)

200,0

150,0

100,0

50,0

0,0
0 00
0,00 1 00
1,00 2 00
2,00 3 00
3,00 4 00
4,00 5 00
5,00 6 00
6,00

Concentration (wt% )

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Converting
g conductivity
y to concentration

Available on Orbis

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Conductivity
Concentration determination
► Only possible to convert conductivity into
concentration if the solutes are known
► Calibration curves have to be prepared

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Titration

► Determination of concentrations in strong acids and bases

► Neutralisation reaction: NaOH + HNO3  H2O + NaNO3
or OH- + H+  H2O

► Colour indicators are used to

d t
determine
i when
h solution
l ti hhas a neutral
t l
pH i.e. when equivalent amounts of
acid and base has reacted
► Possible
P ibl tto calculate
l l t concentration
t ti off
sample from volume of titrant, volume
of sample and concentration of titrant

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Titration
► OH- + H+  H2O
►p
pH g
gets neutral i.e. p
pH7 when equal
q amount of OH-
has reacted with equal amount of H+
►n =V*c
► nOH-= nH+
VOH- * cOH- = VH+ * cH+

n – amountt [mol]
[ l]
V – volume [L]
c – concentration [mol/L]

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Titration of Nitric acid, HNO3

14

12

10

8
pH
H

0
0 5 10 15 20 25 30
added ml of 0.5M NaOH

30 ml HNO3 sample titrated with 17.8 ml 0.5 M NaOH.

0 030 L  c HNO 3  0.0178
0.030 0 5 mol  L1
0 0178 L  0.5
c HNO 3  0.297 mol  L1

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Phosphoric acid H3PO4

14
HNO3
12 H3PO4

10 EP2: H2PO4- + OH-  HPO4-2 + H2O

8
pH

EP1:H3PO4 + OH-  H2PO4- + H2O

4

0
0 5 10 15 20 25 30 35
added ml of 0.5M NaOH

EP - Equivalence point
EP1 = 4.7 ( Only H2PO4- present)
EP2 = 9.9 ( Only HPO4-2 present)

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Phosphoric acid
► Moderately strong acid
► Trivalent acid H3PO4
► Titrate until pH is 4.7 (EP1) or until pH is 9.9 (EP2)
► No really good indicator.

► EP1: nH3PO4= nOH-

VH3PO4 * cH3PO4 = VOH- * cOH-

► EP2: nH3PO4= ½ * nOH-

VH3PO4 * cH3PO4 = ½ * VOH- * cOH-

Internal
Cecilia Svensson/1009

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Titration of formulated detergents

► When determining concentration of formulated detergents, titration

instructions are given by supplier
► Example from Diversey Single VC8

Test method
Reagents: 0.1 N Hydrochloric or sulphuric acid
Phenolphthalein Indicator
Procedure: Add 22-3
3 drops of the Indicator solution to 10 mls of the test
solution.Titrate with the acid to a colourless end point.
Calculation: %w/w Single = titre (mls) x 0.17
%v/v Single = titre (mls) x 0.13

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Internal
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Internal
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Cleaning of branded
processing units

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Cleaning of Branded Processing

units (BPUs)

► Guiding CIP programmes which need to be

followed by a cleaning validation and optimisation
► Degree
g of soiling
g is dependent
p on type
yp of food
product and production time.
► All dairy BPU CIP guidelines are based on pure
sodium hydroxide (NaOH) and pure nitric acid
(HNO3).
► If customer pprefer formulated detergents,
g ,
detergent supplier needs to give cleaning
parameters. Tetra Pak should then deliver the
parameters set by detergent supplier.
supplier

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CIP of Tetra Therm Lacta

Default cleaning program

Internal
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CIP of Tetra Therm Aseptic Flex

Default cleaning program

Internal
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CIP of Tetra Therm Aseptic VTIS

Default cleaning program

Internal
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CIP of Tetra Alsafe

Default cleaning program

Internal
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Cleaning
g validation
- How to secure cleaning
efficiency

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Cleaning validation

► Verify the effectiveness of the cleaning procedure for

removal of product residues
► Establish documented evidence that the cleaning
process removes residues to predetermined acceptable
level

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Structured validation of cleaning

► Tetra Pak has developed a structured

method to validate cleaning
► Includes all the necessary steps
− Design qualification
− Installation qualification
− Operational qualification
− Performance
e o a ce qua qualification
cat o

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Cleaning validation

Design Installation Operational Performance

qualification qualification qualification qualification

► Hygienic
yg e c ► Checklist of ►C
Checklist
ec s o
of ► Monitoring/
g
design critical areas critical areas recording
► Hygienic risk critical CIP
assessments parameters
► Validate
surface
cleanliness

Internal
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Design qualification
Fulfilment of basic prerequisites
► Fulfilment of Hygienic Design criteria
► Hygienic Risk Assessment performed
► In compliance with
− National
N ti l standards/legislation
t d d /l i l ti
− Corporate standard/guidelines

Internal
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Installation qualification

Verify installation of equipment is according

to drawings and specification
► Check flow charts and line diagram
► Map
M allll CIP circuits
i it
► Check line physically
► Identify all critical design features
► Identify all valves

Internal
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Operational qualification
Ensure CIP system works as expected
► Check for leakages and possible malfunction
► Verify that all valves and pumps are operating
as planned
► Verify
V if ththatt the
th automation
t ti iis working
ki properlyl
► Verify that spray devices are working properly
to ensure total coverage of cleaning solution
in the tanks
► Monitor and record all relevant cleaning
parameters

Internal
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Performance qualification/validation
► Demonstrate effectiveness and reproducibility of the
cleaning process and verify that the equipment is cleaned
according to predetermined acceptable level
► Worst-case approach
► Special attention to surfaces that are difficult to clean
► Monitor process parameters
− Temperature, flow velocity, time, detergent concentration
► Assessment of surface cleanliness
− Microbiological and/or non microbiological methods

Internal
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CIP parameters to control and

monitor

► Flow
− Flow transmitter
► Temperature
− Temperature transmitter
► Time
► Detergent concentration
− Electrical conductivity

Internal
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Cleaning validation
- Surface
S f cleanliness
l li

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How clean is clean

► Definition of cleanliness according to

International Dairy Federation (IDF):

”A clean surface is one which is free of residual

film or soil and will not contaminate food product
in contact with it.”

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How clean is clean?

Guidelines or standards for clean surfaces vary widely

► Herbert et al (1990) 80 cfu/cm2

► USDA (1994) 5 cfu/cm2
► Swedish Food (1998) 1-3 cfu/cm2
► Mossel et al (1999) 2,5 cfu/cm2
► Griffith et al (2000) 2 5 cfu/cm2
2,5

Internal
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Cleaning validation
Surface cleanliness
► Visual check
− No product residues
► Bacteriological test
− Swab test
► ATP luminescence test
− (adenosine tri-phosphate bioluminescence)

Internal
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Surface cleanliness

Different method to assess cleanliness by using surface

and/or rinse sampling technique

Microbiological Non - Microbiological

Swab Contact
method plates Visual ATP Protein Sugar Other
Visual /AMP
+UV
General or General or
selective selective
media media

Internal
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ATP bio-luminescence
bio luminescence measurements
► ATP (Adenosine tri-phosphate) is the chemical compound in
which energy is stored in all living cells
► If ATP is found there are living cells present
► The test make use of enzyme from firefly. The enzyme convert
the energy in ATP into light
light.
► The quantity of light produced is directly related to the amount
of ATP (microbial and non-microbial) present

http://biochemifa.kikkoman.co.jp

Internal
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UHT CIP optimisation

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CIP monitoring

► Today no method to follow how soil is removed

continuously during cleaning
► If available,, each cleaning
gpprocedure could be
optimized for each product and running time
► Cleaning as per degree of soiling

Internal
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Optimising CIP programmes

► Cleaning procedures based on experience and

probably on the safe side
► No ggood wayy to measure in-line what is
happening
► COD or turbidity can be used for protein soil and
calcium for mineral soil but no good in
in-line
line
methods available yet

Internal
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Where do we have fouling?

Indirect heating system

Protein fouling Mineral fouling

Stabilising UHT
Holding tube Holding tube

Hot water

Hot water

Internal
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CIP sensor
For optimization and tailoring

Caustic CIP step Acid CIP step Caustic CIP step Acid CIP step
URFACE
SOIL ON SU

CLEAN LEVEL
CIP not ready
CIP TIME

Internal
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Default maximum CIP program

For Tetra Therm Aseptic Flex

► 10 hours of production
ACE
OIL ON SURFA

► White milk 1.5% fat

► Alkalinestep (NaOH):
1.4wt% / 137°C / 50 min
SO

► Acidicstep (HNO3 ):
1.2wt% / 85°C / 30min

CLEAN LEVEL

50 min 30 min

CIP TIME
0,00 20,00 40,00 60,00 80,00 100,00 120,00 140,00
Internal
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Optimizing the acidic step

► 10 hours of production
RFACE

► White milk 1
1.5%
5% fat
SOIL ON SUR

► Alkaline step (NaOH):

1.4wt% / 137°C / 50 min
► Acidic step (HNO3 ):
1.2wt% / 85°C / 5 min

CLEAN LEVEL

50 min 5
min

CIP TIME
0 10 20 30 40 50 60 70 80 90 100 110 120
Internal
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Optimizing the alkaline step

► 10 hours of production
SOIL ON SURFACE

► White milk 1.5% fat

► Alkaline
Alk li step
t (N(NaOH):
OH)
1.4wt% / 137°C / 15 min
► Acidic step (HNO3):
1 2wt% / 85°C
1.2wt% 85 C / 5 min

CLEAN LEVEL

15 5
min min

CIP TIME
0 10 20 30 40 50 60 70 Internal
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UHT CIP optimization with CIP sensor

► Unoptimized default
Acidic step
Alkaline step
CIP p
program
g
CE
SOIIL ON SURFAC

= CLEAN
CLEAN LEVEL

CIP TIME

Alkaline step ► Optimized and tailored

Acidic step
SURFACE

CIP program
SOIL ON S

= CLEAN
CLEAN LEVEL

CIP TIME
0 30 90 120 minutes
60

Internal
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Optimizing detergent
concentration
Alk li and
Alkali d acid
id

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Laboratory trials
Set up

STEP 1 STEP 2

Fouling
g 70 ml
70 ml
2% NaOH
1,5% HNO3

Filtration
Centrifug 10 min,
10 min, Wash Drying
85 °C
ation
H2O 85 °C
C

Chemical
analysis

Internal
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Detergent concentration
Eff t off NaOH
Effects N OH on type
t A soilil
12000

10000

8000
TOC mg/l

6000
T

4000

2000

0
0 25 wt% NaOH
0.25 0 5 wt% NaOH
0.5 1 wt% NaOH 2 wt% NaOH

Internal
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Detergent concentration
Effects of NaOH on mineral soil

Internal
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Detergent
g concentration
Effects of NaOH on mineral type fouling

800
700
600
500
mg/l
TOC m

400
300
200
100
0
0.25 wt% NaOH 0.5 wt% NaOH 1 wt% NaOH 2 wt% NaOH

Internal
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Detergent concentration
Effects of NaOH on mineral type fouling
Alkaline step
‐ Fouling: Indirect UHT 0.5% fat milk
onents dissolved (%) 100%
90%
80%
70%
60%
ouling compo

50%
40%
30%
Degree of fo

20%
10%
0%
NaOH 1wt% NaOH 2wt% NaOH 2.5wt% NaOH 3wt%

Ca Mg P S TOC TN
Internal
/
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Alkali concentration optimum

► Protein fouling: 0
0.5-1
5 1 wt% NaOH
► No need for acid to dissolve the protein soil but
needed for other purposes
p p
► Mineral fouling: highest effect at highest NaOH
concentration

Internal
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CIP after long productions

ount soil on surface
Rel. amo

Protein fouling

Mineral fouling

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“Dirty”
Dirty” detergents

Theoretical Conc. from Conc from

pH
conc. conductivity titration

wt% wt% wt%

NaOH 1 1,9 1,5 1,5 13,1
CIP 1
HNO3 1 1,9 0,4 1,6 2,2
NaOH 2 19
1,9 16
1,6 16
1,6 12 9
12,9
CIP 2
HNO3 2 2 1,2 1,7 1,0
NaOH 3 1,9 1,4
CIP 3
HNO3 3 1,9 1,4

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Dirty acid vs clean

Titration
14

Clean Nitric acid

12 Dirty Nitric acid

10 Equivalence point 2 for phosphoric acid

8
pH
p

Equivalence point 1 for phosphoric acid

0
0 0 002
0,002 0 004
0,004 0 006
0,006 0 008
0,008 0 01
0,01 0 012
0,012 0 014
0,014 0 016
0,016 0 018
0,018 0 02
0,02
Added OH- (mol)

 Titration of “dirty” acid will not give correct values Internal

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Acid concentration
Effects of HNO3 concentration on mineral fouling

Step 2: HNO3 85°C, 0.5 ‐ 1.5wt%

100%
%)
ouling componeents dissolved (%
90%

80%

70%

60%

50%

40%

30%
Degree of fo

20%

10%

0%
HNO3 1,5wt% HNO3 1wt% HNO3 0.5wt%
Ca Mg P S TOC
Internal
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Detergent concentration
Eff t off HNO3 on type
Effects t B soilil

10000

Ca
8000
P

6000
mg/ll

4000

2000

0
0,5 wt% HNO3 1 wt% HNO3 2 wt% HNO3 3 wt% HNO3

Internal
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Acid concentration
Nitric acid
► pH increase when mineral fouling is dissolved
► Conductivity decrease
► Acid is consumed:

► Optimal concentration depends on amount of

mineral fouling and thus production time.
► Titration
Tit ti off dirty
di t acid
id gives
i uncorrectt
concentrations.

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Optimizing detergent
temperature
A id and
Acid d alkali
lk li

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Acid temperature
UHT CIP
Step 2 HNO3 65, 75 and 85°C
100%

90%
d (%)
onents dissolved

80%

70%

60%
of fouling compo

50%

40%

30%
Degree o

20%

10%

0%
HNO3 85°C HNO3 75°C HNO3 65°C
Ca Mg P S TOC

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Adjusting cleaning temperature

NaOH 137°C/ HNO3 85°C
3 160
NaOH HNO3
surface

1,4 wt% / 50 min 1,2wt% / 30 min 140

Rinse

Program step
2,5
120

se
Rins
ount soil on s

2 100

80

osing
1,5
osing

60
137 C 85 C

HNO3 do
Rel. amo

NaOH do

CLEAN 40
1
50 min 30 min 20
Run time: 10 h
0,5 0
0,00 20,00 40,00 60,00 80,00 100,00 120,00 140,00 Milk: 1,55% fat
Time (min)

NaOH 120°C / HNO3 85°C

3,0 160
NaOH HNO3
mount soil on surface

DP70: S2+SHC
1,4wt% / 50 min 1,2wt% / 30 min 140
2,5

Program step
Rinse
120
2,0
100
DP71: S3+S4+S5
1,5 80
osing
osing

CLEAN 60
1,0
HNO3 do
NaOH do
Rel. am

40 Program step
Rinse

0,5
20

0 0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 Tetra Pak Restricted
Time (min) AG/1009

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CIP following long production >30 hours

► What happens if new fresh NaOH is introduced after

the first NaOH step?
10 160

9
140
:
8 :

120
7
100
6
P/P0

5 80
95-137°C
4
60
3
70-95°C 40
2
20
1

0 0
0 20 40 60 80 100 120 140 160 180 200
Time (min)

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CIP following long production >30 hours

- Influence of renewed alkali solution
Test 19 100206 CIP 1 - 120°C NaOH/NaOH/HNO3
Milk 1,55% fat, run time 30h
6,0 160

H dosing

Rinse
HNO3 dosing
Rinse
NaOH dosing
NaOH

Rinse

Rinse
NaOH HNO3

Rinse
5,5 1.5wt%
1.4wt% 1.2wt%
140

NaOH
5,0

4,5 120

40
4,0
100

gram step
3,5
95-137°C
P/P0

3,0 80

Prog


2,5
No improvements 60
2,0

1,5 40
70-95°C
1,0
20
0,5

0,0 0
0 20 40 60 80 100 120 140

Fresh NaOH added Time (min) Tetra Pak Internal

AG/0110

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Summary
Temperature and renewal of alkali
► No difference in lab scale on acid temperature
from 65 to 85°C
► No difference when alkali temperature
p was 137
and 120°C
► Refreshing the alkali did not remove more soil

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Material available

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Orbis: Cleaning Solutions web site

http://neworbis.tetrapak.com/irj/portal/?NavigationTarget=navurl://0eb5159cb45d4963e2b4e8
dd2661c96b
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Orbis: Tetra Alcip site

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Cleaning Handbook

► CIP Technology
− Validation
− Hygienic design
− Detergents
− CIP programs
− Etc.

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Cleaning validation document

► Validation structure
− Design
− Installation
− Operational
− Performance

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