LACTOSE CRYSTALLIZATION

FROM SATURATED SOLUTIONS

Aram Galstyan
GNU All-Russia Dairy Research Institute, Moscow, Russia
Department of gerodietical and special products
Тел./Факс: +7 (495) 236-02-36
www:vnimi.org
E-mail: aram@sanavita.ru
 Introduction

Product qualitative index*

Consistence
Not less than 400.000 crystals in 1 mm3 of product
Homogeneous
Crystals average size ≤ 10 µm

Technological operations

Crystallization Germs Fermentation

Isohydric Small dispersion Lactose preparation
lactose (3-4 µm )
Vacuum Immobilizing

Powder Suspension Consumed

* Радаева И.А., Гордезиани В.С., Шулькина С.П. Технология молочных консервов и ЗЦМ: Справочник– М.:Агропромиздат, 1986.
Чекулаева Л.В., Чекулаев Н.М Сгущенные молочные консервы. – М.: Легкая и пищевая пром-ть, 1982.
Чекулаева Л.В., Полянский К.К., Голубева Л.В. Технология продуктов консервирования молока и молочного сырья.– Воронеж: Изд. ВГУ, 1996.
Introduction

Technological requirements
Crystallization Fermentation
Saturation level

Prime material availability To have a ferment

To know the properties, To know the activity,

decide the adding time optimal conditions

To control energy exchange processes

To control mass distribution processes

 Introduction

Crystallization

Homogeneous Heterogeneous

Homogeneous Heterogeneous
crystallization nucleus crystallization nucleus

The composition of exuded crystals The composition of exuded crystals

corresponds to does not correspond to
composition of crystallization centers composition of crystallization centers

1) Shabalin V.N., Shatoxina S.N. Morphology of biological fluids. – M.:Chrizostom, 2001

2) Rosenberger F. Fundamentals of Crystal Growth.— Berlin, 1979
3) Ohtaki H. Crystalization Processes. – Wiley, 2001
4) Hartel R.W. Crystallization In Foods.- Kluwer Academic Publishers, 2001
5) Веригин А. Н., Щупляк И. А., Михалев М. Ф. Кристаллизация в дисперсных системах: Инж. мет. расчета.- Л.: Химия, 1986
6) Портнов В.Н., Чупрунов Е.В. Возникновение и рост кристаллов.-М.:Изд. Физ.-мат.лит., 2006

http://www.wikipedia.org http://www.xumuk.ru http://www.paceka.ru http://www.cheresources.com http://www.geo.web.ru и др.

 Materials and Methods

Principle technological schemes of manufacture

of sugar containing condensed milk products
Condensed milk with sugar Boiled condensed milk with sugar

Raw materials acceptance, storage

and preparation
1
Dry milk products reduction at Lactose fermentative Employed with a purpose
water temperature 40-60 °C hydrolyses (39-41 °C, for 3h)1 of prevention the uncontrolled
Dispergration of the fatty crystallization & speeding-up
component cooking time
Heating (75-77 °C) 2
Duration depends on the
Sugar dissolution temperature & fermentation
process
Heating and pasteurization
Heating
(90-95 °C for 2-3 min)
3
The adding of priming
Cooling (32-37 °C) material in vacuum meant.
Crystallization 3 In manufacture of sugar-
containing condensed milk
Homogenization Heat treatment (cooking) “cooking” is not employed.
(15-16 Pa) at T ≥ 30 °C (95 °C and more for 1-3 hours) 2

Cooling to 80-85 °C and homogenization

Cooling (20 ± 2 °C)
(15-16 MPa)

Packaging Packaging

Marking Marking

Storage and sale

 Materials and Methods

Model product’s normalized indices

Index appellation Standards

Mass proportion of moisture, % ≤ 26,5
Mass proportion of saccharose, % ≥ 43,5
Total mass proportion of milk dry materials, % ≥ 28,5
also fat, % ≥8,5
Acidity,0Т ≤ 45
Viscosity, Pa*с
valid within 2 months ≤ 3-6
valid within 2 to 12 months 15
Allowed size of lactose crystals, µm , ≤ 15
 Materials and Methods

Recipes of sugar-containing condensed milk products

and established conventional coding
Components Recipes Coding
Dry skimmed milk (dry materials proportion 95%, 213,0 Х1
fat proportion 1,5%)
Milk fat (fat proportion 99,8%) 82,0 Х2
Granulated sugar (dry materials proportion 99,8%) 450,0 Х3
Water 255,0 Х4
Total product 1000,0 Х5
Appellation of Coding Appellation of Coding
the operation the operation
Dissolution Y1 Vacuuming Y8
Germs bringing in Y2 Crystallization Y9
Dispergration Y3 Cooking Y10
Х5=Х4 + Х1 + Х2 + Х3
Heating Y4 Packing Y11
Homogenization Y5 Mixing Y12
Pasteurization Y6 Marking Y13
Cooling Y7 Storing Y14
 Materials and Methods

Operative models: condensed milk with sugar (A,B,C) and

condensed milk with sugar “cooked” (С/)
Operations Possible modification of germs adding time
sequence А B C C/
ТО1 Y4X4← Z Y4X4 Y4X4 Y4X4
ТО2 Y1X1 Y1X1 Y1X1 Y1X1
ТО3 Y4X41 Y4X41 Y4X41 Y4X41
ТО4 Y3X2 Y3X2 Y3X2 Y3X2
ТО5 Y5X412 Y5X412 Y5X412 Y5X412
ТО6 Y4X412 Y4X412← Z Y4X412 Y4X412
ТО7 Y1X3 Y1X3 Y1X3 Y1X3
ТО8 Y6X4123 Y6X4123 Y6X4123 Y6X4123
ТО9 Y8X4123 Y8X4123 Y8X4123← Z Y8X4123← Z
ТО10 Y7X4123 Y7X4123 Y7X4123 Y7X4123
ТО11 Y9X4123 Y9X4123 Y9X4123 Y11 X5
ТО12 Y11 X5 Y11 X5 Y11 X5 Y10 X5
ТО13 Y13X5 Y13X5 Y13X5 Y7 X5
ТО14 Y14X5 Y14X5 Y14X5 Y13 X5
ТО15 - - - Y15 X5

ТО – technological operation; Z – time point of bringing in of germs

 Materials and Methods

Time point of sampling for

microscoping

2 15 30 45 60 75 90 105 120
Storage
temperature
6-100C
0 Time (Days)

0 – end of technological process and beginning of analysis

120 – end of analysis
 Materials and Methods

№ Products Molecular Properties, Solubility in water at

formula % рН≤7,0, mg/l
1 Silicon dioxide SiO2 Not present
2 Titanium dioxide TiO2 ≥ 98 not present
3 Calcium carbonate CaCO3 14-15

Crystals average size was calculated by
formula:
D = ∑na / ∑n
D – mean value of crystals size, µm ; n – crystals
frequency; а – crystals linear size, µm
Coefficient of crystals homogeneity was calculated
by the means of N. Figurovskii’s formula
U = ∆а ∑ n /( 2∑ nv 2 )
U – homogeneity coefficient; ∆а – crystal size limit, µm;
n – crystals frequency; v – given and mean sizes
divergence, µm

Crystals average Lactose crystals likely Crystals average Lactose crystals likely
size, µm amount in 1mm3 of size, µm amount in 1mm3 of
product, M product, M
6 770 000 12 98 000
7 500 000 15 50 000
8 270 000 20 21 000
9 220 000 30 7 000
10 175 000 40 2 600
 Results

Distribution of samples with no crystallization effect when germ size

is 3 µm and its corresponding dosage 0,02…0,10% of product mass

Model C
0.10
Y4X4
70
Y1X1 60
Y4X41 50
Y3X2 40

Y5X412 30
0.02 20 14% 0.09
Y4X412 46%
10 16%
Y1X3
0
Y6X4123
Y8X4123← Z
22%
Y7X4123 31%

Y9X4123
Y11 X5
0.05 0.08
Y13X5
Y14X5
 Results

Distribution of samples with no crystallization effect when germ size

is 4 µm and its corresponding dosage 0,02…0,10% of product mass

Model C
Y4X4 0.10
70
Y1X1 60
Y4X41 50
Y3X2 40

Y5X412 68% 30 21%

0.02 20 0.09
Y4X412
10 28%
Y1X3
0
Y6X4123
Y8X4123← Z
Y7X4123
40%
Y9X4123
51%
Y11 X5
0.05 0.08
Y13X5
Y14X5
 Results

Lactose crystals homogeneity coefficient when priming

material size is 3-4 µm
Model C
Y4X4
Y1X1
Silicon dioxide
Y4X41 0.4 Titanium dioxide
Y3X2 Calcium carbonate
Coefficient of homogeneity, U
0.35
Y5X412
0.3
Y4X412
0.25
Y1X3
0.2
Y6X4123
0.15
Y8X4123← Z
0.1
Y7X4123
0.05
Y9X4123
0
Y11 X5 3 4

Y13X5 Germ size, µm

Y14X5
 Results
Rational dosage of priming material for lactose crystallization
by model A
Model А
Y4X4← Z
Y1X1
Y4X41 8
Y3X2
Y5X412
Lactose crystals size, µm

Calcium carbonate
Y4X412

Titanium dioxide
Silicon dioxide
Y1X3
Y6X4123 4

Y8X4123
Y7X4123
2
Y9X4123
Y11 X5
0
Y13X5 0.082 0.089 0.098
Y14X5 Dosage of priming material, %
 Results
Rational dosage of priming material for lactose crystallization
by model B
Model B
Y4X4
Y1X1
Y4X41 8
Y3X2
Y5X412
Lactose crystals size, µm
6
Y4X412← Z

Calcium carbonate
Titanium dioxide
Silicon dioxide
Y1X3
Y6X4123 4

Y8X4123
Y7X4123
2
Y9X4123
Y11 X5
0
Y13X5 0.051 0.061 0.078
Y14X5 Dosage of priming material, %
 Results
Rational dosage of priming material for lactose crystallization
by model C
Model C
Y4X4
Y1X1
Y4X41 8
Y3X2
Y5X412 Lactose crystals size, µm
6
Y4X412
Y1X3
Y6X4123

Titanium dioxide
4

Calcium carbonate
Silicon dioxide
Y8X4123← Z
Y7X4123
2
Y9X4123
Y11 X5
0
Y13X5 0.022 0.029 0.031
Y14X5 Dosage of priming material, %
 Results

Operative model of packaged product lactose crystallization after its

thermal treatment
Model C/
Y4X4
Germs adding
Y1X1 0,03% to products mass
Y4X41
Y3X2
Y5X412 Packing in metal cans №7 (0,4 kg)
Y4X412
Y1X3
Y6X4123
Y8X4123← Z Thermal treatment at 117 0С during
Y7X4123 1 hour
Y11 X5
Y10 X5
Uncontrolled cooling at room
Y7 X5 temperature
Y13 X5
Y15 X5
 Results

Results of packaged product lactose crystallization after its

thermal treatment
Crystals
Crystals Crystals Product Discrepancy,
Model size, v2 nv2
group frequency, n na v
а, µm
C/ 4 26 104 2.98 8.88 230.9
Y4X4 6 14 84 0.98 0.96 13.5
I
Y1X1 8 51 408 1.02 1.04 53.1
Y4X41 10 4 40 3.02 9.12 36.5
Y3X2 12 4 48 5.02 25.20 100.8
II
Y5X412 14 1 14 7.02 49.28 49.3
Y4X412 16 0 - - - -
Y1X3 18 0 - - - -
Y6X4123 III 20 0 - - - -
Y8X4123← Z 22 0 - - - -
Y7X4123 24 0 - - - -
Y11 X5 IV ≥ 25 0 - - - -
Y10 X5
Y7 X5 ∆a = 2 ∑n=100 ∑an=698 - - ∑nv2=484.1
Y13 X5

Y15 X5 М = ∑na / ∑n = 6.98 U = 0.64

 Results

Efficacy gradation SiO2>TiO2>CaCO3

Results of lactose crystallization depending on the

operating model and priming material type
Variant of modification of germs adding time
Priming
material type А B
(1-2µm) К, % D,µm U M, in 1mm3 К, % D, µm U M, in 1mm3

SiO2 0,082 6,41 0,76 770.000 0,051 6,65 0,82 500.000

TiO2 0,089 8,26 0,54 270.000 0,061 6,86 0,63 500.000
CaCO3 0,098 9,13 0,41 220.000 0,078 7,68 0,59 270.000

Priming Variant of modification of germs adding time

material type
C C/
(1-2µm)
К, % D, µm U M, in 1mm3 К, % D, µm U M, in 1mm3

SiO2 0,022 4,48 0,88 ≥770.000 0,022 6.98 0.64 500.000

TiO2 0,029 5,67 0,85 ≥770.000 - - - -
CaCO3 0,031 7,09 0,82 500.000 - - - -
 Farther investigations algorithm
Priming material choice Development of product technology

Security Modeling systems Technological parameters

Physico-chemical
properties Crystallography Technological regulations

Technological Formation Methods of control

peculiarities conformity
PRODUCT
Investigation methods
Growth conformity
Products indices
Availability
Efficacy Security
Economical
expediency Preservation stability

Methods of control
Production approval
 Acknowledgements

Academician Kharitonov V.D All colleagues and staff at the

Professor Radaeva I. A. Department of Gerodietical
Chief of the laboratory Petrov A. N. and special products

Thank you for attention!

Спасибо за внимание!

Aram Galstyan

GNU All-Russia Dairy Research Institute, Moscow, Russia

Department of gerodietical and special products
Tel/Fax: +7 (495) 236-02-36
www.vnimi.org
E-mail: aram@sanavita.ru