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Cryogenic Grinding
1
INTRODUCTION
 Cryogenic grinding, also known as freezer milling, freezer grinding
and cryo-milling is an act of cooling or chilling a material and then
reducing it into a small particle size.
 The term “Cryogenics” originates from Greek word “Kryos” and
“Genic” which means creation or production by means of cold.
 Cryogenic grinding technology can efficiently grind most tough
materials and can also facilitate cryogenic recycling of tough
composite materials and multi component scrap.
2
PROBLEMS FACED IN CONVENTIONAL
GRINDING PROCESS
 High heat generation (43°C-92°C)
 Gumming and clogging of mills
 Oxidation and related degradation
 Loss of etheric oil
3
CRYOGENIC GRINDING
 Cryogenics can also be defined as a branch of
engineering specializing in technical operations
at low temperature ( temp. below -150°C).
 Cryogenic grinding process uses cryogenic
liquids (cryogens) to achieve low temperature in
cryogenic grinding system.
4
CRYOGENS
 The extremely low temperature are produced by
using substances called “cryogens” such as
liquid nitrogen.
 All cryogenic liquids are gases at normal
temperatures and pressures. So, these gases must
be cooled below room temperature to liquefy
them.
 They have boiling points below -150°C.
5
FLUID BOILNG POINT
(K)
Helium-3 3.19
Hydrogen 20.27
Neon 27.09
Nitrogen 77.09
Air 78.8
Fluorine 85.24
Argon 87.24
Oxygen 90.18
Methane 111.7
6
 Cryogens are stored in vessels called as Dewar flask
which provides good insulation.
7
HEALTH HAZARDS OF CRYOGENIC
LIQUIDS
 Skin and eye hazard
 Cold embrittlement
 Oxygen enrichment
8
ADVANTAGES OF CRYO GRINDING
WITH LIQUID NITROGEN
 Higher retention of etheric oils
 Prevention of oxidation and rancidity
 Increased throughput and power saving
 Finer particle size
 Reduction in microbial load 9
CRYO GRINDING UNIT
The principal parts of system are :
 Feeder
 Pre cooler
 Liquid nitrogen distribution system
 Grinder
 Temperature controls
 Sensors 10
11
Cryogenic pre-cooler
 The cryogenic pre-cooler is a cooling device made up
of a screw conveyor enclosed in a properly insulated
barrel and a system to introduce liquid nitrogen into
the barrel, thereby providing refrigeration within the
system.
 The function of the cryogenic pre-cooler is to remove
the heat from the material before it enters the grinder.
12
Feeding raw material into the
hopper
Chilling of spices with liquid
nitrogen
Feeding of material in mill
Grinding in mill at lower
temperature and inert atmosphere
Packing 13
INDUSTRIALLY USED CRYOGENIC
GRINDER
14
Traditional grinding system Cryogenic grinding system
 Heat is developed inside the grinding
mill.
 Temperature below 00C inside the
grinding mill.
 Heat developed, leads to evaporation
of essential oil and melting of heat
sensitive fats.
 Negligible loss of volatile compounds.
 Grinding elements becomes greasy
and even harms the machine by
blocking it.
 Not in cryogenic process.
 High energy consumption  Low energy consumption.
 High capacity motors are required to
grind the material.
 Low capacity motors are used to grind
the material.
 No control on particle size.  Particle size is under control.
15
Ambient ground Cryo-ground
16
ADVANTAGES
 Cryogenic grinding improves the aroma by minimizing
the loss of essential oils (approx. 3- 10% loss) which is
approx 15-43% in conventional processing.
 Spices processed using cryo-grinding has better natural
color, as compared to conventional process, this is very
much important for chilly and turmeric.
17
 Finer particle size can be achieved without aroma
loss and natural color change.
 Overall grinding capacity can be increased by 2
to 3 times, as process equipment will not have
thermal fatigue due to heating up.
18
DISADVANTAGES
 The application of cryogen in moist atmosphere
may cause formation of ice around the delivery
nozzle and the piping system carrying the
cryogen. This may cause a possible blockage in
the delivery system of liquid nitrogen
 Expensive
19
APPLICATIONS
 Cryogenic grinding of spices, cocoa and
chocolate, vanilla-sugar, dehydrated meat, etc.
 Thermoplastics
 Thermo sets
 Adhesives & waxes
 Explosives
20
CASE STUDY-1
21
Cryogenic grinding of black
pepper
C.T. Murthy, Suvendu Bhattacharya et al.
Journal of Food Engineering 85,(2010)
22
Objective
 Cryogenic grinding of black pepper at different
temperature and feed rates was conducted, and
was compared with conventional grinding.
 Comparing the particle size of powder, yield of
volatile oil, sensory attributes of powdered
samples are studied
23
Materials and Methods
 Black pepper
The samples were of medium size (4mm dia. ). Broken and
immature seeds and foreign matter was removed from
the samples prior to treatment.
 Grinder and grinding trails
A pin mill was employed for grinding the black pepper
under ambient and cryogenic conditions.
24
 Black pepper was loaded onto the hopper and was fed to
the grinder with the help of a vibratory feeder.
 After adjusting the feed rate to the required level, liquid
nitrogen was introduced into the grinding zone of the pin
mill such that the desired temperature was attained.
 Samples were collected in thick polyethylene bags and
were sealed immediately. All experiments were repeated
twice. 25
26
 Particle size of powder
Particle size distribution of ground black pepper was
determined using a vibratory sieve shaker with a set of
British Standard (BS) sieves. Average particle size was
then calculated for the powder.
 Gas chromatographic analysis
The samples were analyzed in a gas chromatographic
analyser.
27
 Sensory studies
I. The powdered samples were subjected to sensory assessment.
Odour profiles were carried out by a trained panel consisting of
12 members.
II. The overall quality grading indicate that the mean score of up to 2
is not usable, 3 and 4 is poor, 5 is average, 6 is fair, 7 and 8 is
good, 9 and 10 is very good.
28
Results and Discussion
Cryogenically ground samples (C1–C9) are initially
compared with ambient ground samples (A1, A2) in terms
of quantity of volatile oil yield, particle size of the powder,
and quality of volatile oil.
29
Gas ChromatographicAnalysis of
Volatile Oil
30
Sensory Attributes of Powdered
Samples
31
Conclusions
 The pilot scale cryogenic grinding studies of black pepper have been
conducted and the product characteristics are compared with ambient
ground samples.
 The average volatile oil yield in case of cryogenic grinding is 1.7
mL/100 g whereas it is 0.9 mL/100 g for ambient system.
 The gas chromatographic analysis of volatile oil indicates that the
ratio of monoterpenes to sequiterpenes varies from 1.35 to 1.85 in the
case of cryogenic grinding, whereas, the ambient ground samples
have a very low ratio 0.22–0.31.
32
 Sensory assessment of cryogenically ground samples indicated
that these samples are distinctly high in top notes which
represent freshness, and is marginally high in basic notes.
 Hence, the quality of cryogenically ground sample is better
than the conventionally ground samples.
33
CASE STUDY 2
34
Cryogenic grinding technology enhances
volatile oil, oleoresin and antioxidant activity
of cumin (Cuminum cyminum L.)
S. N. Saxena et al
International Journal of Seed Spices 4(2), 2014
35
Objective
 To prove that cryogenic grinding of cumin is better than
non cryo-grinding in terms of higher retention of volatile
oil, total oil, total phenolic content, total flavonoid
content and antioxidant properties of ground powder.
36
Materials and Methods
 Seeds of two varieties of cumin (GC-4 and RZ-209), were
cleaned and used for cryogenic grinding and non cryo
grinding.
 Ground powder was used for extraction of volatile oil and
total oil as well as total phenolic content, total flavonoid
content and antioxidant properties of ground powder.
37
 Grinding of seeds
For cryo-ginding:
Fed in hopper
Liquid nitrogen
sprayed and blend
Brittle material
enters impact mill
Packed quickly
38
 To obtaining seed powder through non-cryo grinding
dried seeds was ground separately by domestic mixer
grinder.
 Essential oil was extracted from seed powder and was
estimated using all glass Clevenger apparatus.
 Crude seed extract was used for determination of the total
phenol and flavonoids concentration, as well as
antioxidant activities.
39
Result
 Cryogenic grinding not only retains the volatiles
in both the genotypes but enhanced the recovery
also.
 Non cryogenic or normal grinding at ambient
temperature causes 18-19 % loss of volatile oil in
both the genotypes.
40
41
42
Conclusion
 From present study it could be concluded that
cryogenic grinding technology is superior to non
cryogenic grinding for retention of flavour and
antioxidant properties of cumin irrespective of
the genotype.
43
SUMMARY
 As the cost of raw materials and energy is increasing day
by day, it is very necessary to use optimum quantity and
at the same time getting the required quality.
 Cryogenic grinding can be used as a solution.
 Value added products are obtained.
 Spice industries of our country will earn considerable
foreign exchange by exporting more value added
processed spices, in place of exporting whole spices.
44
REFERENCE
 Andres, C. (1976). “Grinding spices at cryogenic temperatures retains volatiles and oils”.
Food Processing, 37(9), 52-53.
 D. Landwehr, and M.H. Pahl, “Cold grinding of spices,” International Journal of Food
Technology and Food Process Engineering, vol. 37, 174-185, (1986).
 J.R. Russo, “Advanced techniques in new spice plant-cryogenic grinding material handling,”
Food Engineering International, vol. 1, 33-35, (1976).
 Murthy, C. T., Krishnamurthy, N., Ramesh, T., & Srinivasa Rao, P.N. (1996). Effect of grinding
methods on the retention of black pepper volatiles. Journal of Food Science and
Technology, 33(4), 299-301.
 R.K. Kumar, “Modification and performance evaluation of indigenous cryogenic grinder,”
M.Tech. Thesis, Dept. of Agrl. and Food Engg., IIT Kharagpur, Kharagpur, India, (2001).
 S. Balasubramanian, M.K. Gupta, and K.K. Singh K. K, “Cryogenics and its application with
reference to spice grinding: a review,” Critical reviews in food science and nutrition, vol. 52,
781-794, (2012).
 Singh, K. K., & Goswami, T. K. (1996). “Physical properties of cumin seed”. Journal of
Agricultural Engineering Research, 64(2), 93-98.
 S. Li, S. Ge, Z. Huang, Q. Wang, H. Zhao, and H. Pan, “Cryogenic grinding technology for
traditional Chinese herbal medicine,” Cryogenics, vol. 31, 136-137, (1991).
 Venetucci, J. M. (1980). “Cryogenic grinding of food stuffs” In N. R.Braton, Cryogenic
recycling and processing, 148-181 CRC Press Inc., USA.
 Wolf, T., & Pahl, M. H. (1990). Cold grinding of caraway seeds in impact mill. International
Journal of Technology and Food Process Engineering, 41(10), 596-604.
45
46

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Cryogenic grinding

  • 2. INTRODUCTION  Cryogenic grinding, also known as freezer milling, freezer grinding and cryo-milling is an act of cooling or chilling a material and then reducing it into a small particle size.  The term “Cryogenics” originates from Greek word “Kryos” and “Genic” which means creation or production by means of cold.  Cryogenic grinding technology can efficiently grind most tough materials and can also facilitate cryogenic recycling of tough composite materials and multi component scrap. 2
  • 3. PROBLEMS FACED IN CONVENTIONAL GRINDING PROCESS  High heat generation (43°C-92°C)  Gumming and clogging of mills  Oxidation and related degradation  Loss of etheric oil 3
  • 4. CRYOGENIC GRINDING  Cryogenics can also be defined as a branch of engineering specializing in technical operations at low temperature ( temp. below -150°C).  Cryogenic grinding process uses cryogenic liquids (cryogens) to achieve low temperature in cryogenic grinding system. 4
  • 5. CRYOGENS  The extremely low temperature are produced by using substances called “cryogens” such as liquid nitrogen.  All cryogenic liquids are gases at normal temperatures and pressures. So, these gases must be cooled below room temperature to liquefy them.  They have boiling points below -150°C. 5
  • 6. FLUID BOILNG POINT (K) Helium-3 3.19 Hydrogen 20.27 Neon 27.09 Nitrogen 77.09 Air 78.8 Fluorine 85.24 Argon 87.24 Oxygen 90.18 Methane 111.7 6
  • 7.  Cryogens are stored in vessels called as Dewar flask which provides good insulation. 7
  • 8. HEALTH HAZARDS OF CRYOGENIC LIQUIDS  Skin and eye hazard  Cold embrittlement  Oxygen enrichment 8
  • 9. ADVANTAGES OF CRYO GRINDING WITH LIQUID NITROGEN  Higher retention of etheric oils  Prevention of oxidation and rancidity  Increased throughput and power saving  Finer particle size  Reduction in microbial load 9
  • 10. CRYO GRINDING UNIT The principal parts of system are :  Feeder  Pre cooler  Liquid nitrogen distribution system  Grinder  Temperature controls  Sensors 10
  • 11. 11
  • 12. Cryogenic pre-cooler  The cryogenic pre-cooler is a cooling device made up of a screw conveyor enclosed in a properly insulated barrel and a system to introduce liquid nitrogen into the barrel, thereby providing refrigeration within the system.  The function of the cryogenic pre-cooler is to remove the heat from the material before it enters the grinder. 12
  • 13. Feeding raw material into the hopper Chilling of spices with liquid nitrogen Feeding of material in mill Grinding in mill at lower temperature and inert atmosphere Packing 13
  • 15. Traditional grinding system Cryogenic grinding system  Heat is developed inside the grinding mill.  Temperature below 00C inside the grinding mill.  Heat developed, leads to evaporation of essential oil and melting of heat sensitive fats.  Negligible loss of volatile compounds.  Grinding elements becomes greasy and even harms the machine by blocking it.  Not in cryogenic process.  High energy consumption  Low energy consumption.  High capacity motors are required to grind the material.  Low capacity motors are used to grind the material.  No control on particle size.  Particle size is under control. 15
  • 17. ADVANTAGES  Cryogenic grinding improves the aroma by minimizing the loss of essential oils (approx. 3- 10% loss) which is approx 15-43% in conventional processing.  Spices processed using cryo-grinding has better natural color, as compared to conventional process, this is very much important for chilly and turmeric. 17
  • 18.  Finer particle size can be achieved without aroma loss and natural color change.  Overall grinding capacity can be increased by 2 to 3 times, as process equipment will not have thermal fatigue due to heating up. 18
  • 19. DISADVANTAGES  The application of cryogen in moist atmosphere may cause formation of ice around the delivery nozzle and the piping system carrying the cryogen. This may cause a possible blockage in the delivery system of liquid nitrogen  Expensive 19
  • 20. APPLICATIONS  Cryogenic grinding of spices, cocoa and chocolate, vanilla-sugar, dehydrated meat, etc.  Thermoplastics  Thermo sets  Adhesives & waxes  Explosives 20
  • 22. Cryogenic grinding of black pepper C.T. Murthy, Suvendu Bhattacharya et al. Journal of Food Engineering 85,(2010) 22
  • 23. Objective  Cryogenic grinding of black pepper at different temperature and feed rates was conducted, and was compared with conventional grinding.  Comparing the particle size of powder, yield of volatile oil, sensory attributes of powdered samples are studied 23
  • 24. Materials and Methods  Black pepper The samples were of medium size (4mm dia. ). Broken and immature seeds and foreign matter was removed from the samples prior to treatment.  Grinder and grinding trails A pin mill was employed for grinding the black pepper under ambient and cryogenic conditions. 24
  • 25.  Black pepper was loaded onto the hopper and was fed to the grinder with the help of a vibratory feeder.  After adjusting the feed rate to the required level, liquid nitrogen was introduced into the grinding zone of the pin mill such that the desired temperature was attained.  Samples were collected in thick polyethylene bags and were sealed immediately. All experiments were repeated twice. 25
  • 26. 26
  • 27.  Particle size of powder Particle size distribution of ground black pepper was determined using a vibratory sieve shaker with a set of British Standard (BS) sieves. Average particle size was then calculated for the powder.  Gas chromatographic analysis The samples were analyzed in a gas chromatographic analyser. 27
  • 28.  Sensory studies I. The powdered samples were subjected to sensory assessment. Odour profiles were carried out by a trained panel consisting of 12 members. II. The overall quality grading indicate that the mean score of up to 2 is not usable, 3 and 4 is poor, 5 is average, 6 is fair, 7 and 8 is good, 9 and 10 is very good. 28
  • 29. Results and Discussion Cryogenically ground samples (C1–C9) are initially compared with ambient ground samples (A1, A2) in terms of quantity of volatile oil yield, particle size of the powder, and quality of volatile oil. 29
  • 31. Sensory Attributes of Powdered Samples 31
  • 32. Conclusions  The pilot scale cryogenic grinding studies of black pepper have been conducted and the product characteristics are compared with ambient ground samples.  The average volatile oil yield in case of cryogenic grinding is 1.7 mL/100 g whereas it is 0.9 mL/100 g for ambient system.  The gas chromatographic analysis of volatile oil indicates that the ratio of monoterpenes to sequiterpenes varies from 1.35 to 1.85 in the case of cryogenic grinding, whereas, the ambient ground samples have a very low ratio 0.22–0.31. 32
  • 33.  Sensory assessment of cryogenically ground samples indicated that these samples are distinctly high in top notes which represent freshness, and is marginally high in basic notes.  Hence, the quality of cryogenically ground sample is better than the conventionally ground samples. 33
  • 35. Cryogenic grinding technology enhances volatile oil, oleoresin and antioxidant activity of cumin (Cuminum cyminum L.) S. N. Saxena et al International Journal of Seed Spices 4(2), 2014 35
  • 36. Objective  To prove that cryogenic grinding of cumin is better than non cryo-grinding in terms of higher retention of volatile oil, total oil, total phenolic content, total flavonoid content and antioxidant properties of ground powder. 36
  • 37. Materials and Methods  Seeds of two varieties of cumin (GC-4 and RZ-209), were cleaned and used for cryogenic grinding and non cryo grinding.  Ground powder was used for extraction of volatile oil and total oil as well as total phenolic content, total flavonoid content and antioxidant properties of ground powder. 37
  • 38.  Grinding of seeds For cryo-ginding: Fed in hopper Liquid nitrogen sprayed and blend Brittle material enters impact mill Packed quickly 38
  • 39.  To obtaining seed powder through non-cryo grinding dried seeds was ground separately by domestic mixer grinder.  Essential oil was extracted from seed powder and was estimated using all glass Clevenger apparatus.  Crude seed extract was used for determination of the total phenol and flavonoids concentration, as well as antioxidant activities. 39
  • 40. Result  Cryogenic grinding not only retains the volatiles in both the genotypes but enhanced the recovery also.  Non cryogenic or normal grinding at ambient temperature causes 18-19 % loss of volatile oil in both the genotypes. 40
  • 41. 41
  • 42. 42
  • 43. Conclusion  From present study it could be concluded that cryogenic grinding technology is superior to non cryogenic grinding for retention of flavour and antioxidant properties of cumin irrespective of the genotype. 43
  • 44. SUMMARY  As the cost of raw materials and energy is increasing day by day, it is very necessary to use optimum quantity and at the same time getting the required quality.  Cryogenic grinding can be used as a solution.  Value added products are obtained.  Spice industries of our country will earn considerable foreign exchange by exporting more value added processed spices, in place of exporting whole spices. 44
  • 45. REFERENCE  Andres, C. (1976). “Grinding spices at cryogenic temperatures retains volatiles and oils”. Food Processing, 37(9), 52-53.  D. Landwehr, and M.H. Pahl, “Cold grinding of spices,” International Journal of Food Technology and Food Process Engineering, vol. 37, 174-185, (1986).  J.R. Russo, “Advanced techniques in new spice plant-cryogenic grinding material handling,” Food Engineering International, vol. 1, 33-35, (1976).  Murthy, C. T., Krishnamurthy, N., Ramesh, T., & Srinivasa Rao, P.N. (1996). Effect of grinding methods on the retention of black pepper volatiles. Journal of Food Science and Technology, 33(4), 299-301.  R.K. Kumar, “Modification and performance evaluation of indigenous cryogenic grinder,” M.Tech. Thesis, Dept. of Agrl. and Food Engg., IIT Kharagpur, Kharagpur, India, (2001).  S. Balasubramanian, M.K. Gupta, and K.K. Singh K. K, “Cryogenics and its application with reference to spice grinding: a review,” Critical reviews in food science and nutrition, vol. 52, 781-794, (2012).  Singh, K. K., & Goswami, T. K. (1996). “Physical properties of cumin seed”. Journal of Agricultural Engineering Research, 64(2), 93-98.  S. Li, S. Ge, Z. Huang, Q. Wang, H. Zhao, and H. Pan, “Cryogenic grinding technology for traditional Chinese herbal medicine,” Cryogenics, vol. 31, 136-137, (1991).  Venetucci, J. M. (1980). “Cryogenic grinding of food stuffs” In N. R.Braton, Cryogenic recycling and processing, 148-181 CRC Press Inc., USA.  Wolf, T., & Pahl, M. H. (1990). Cold grinding of caraway seeds in impact mill. International Journal of Technology and Food Process Engineering, 41(10), 596-604. 45
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