CRYOGENIC GRINDING

Cryogenics
Cryogenics is the study of the production of very low temperature (below
−150°C, −238°F or 123K) and the behavior of materials at those temperatures.
Similarly, cryogenic grinding is a term supported by the act of grinding a thing
at very low temperature. This technique is generally used to grind the material,
which contains heat labile constituents viz- volatile oils in seed spices. Due to
high fat content in spices, heat is generated, while energy is used to fracture a
particle into a smaller size in conventional grinding process. During the normal
grinding process, this generated heat causes temperature rise of grinder upto
950C.
The increased temperature is responsible for a loss of volatile content in
the tune of about 30% and also produces dark colour powder. Generally,
continuous operation is not possible in normal grinding process due to melting
of fat and sticking of powder on the grinding surface. The loss of volatile
content can be significantly reduced by cryogenic grinding technique using
liquid nitrogen or liquid carbon dioxide that provides the refrigeration needed to
pre-cool the spices and maintain the desired low temperature by absorbing the
heat generated during the grinding operation. The extremely low temperature
during grinder condenses the volatile matter and retains their presence in spices.
The application of cryogenic technology for grinding of spices has been
scientifically proved to be a suitable technique with negligible loss of volatile
content and improved colour of oil and grinding operation of seeds.
Cryogenic grinding
Cryogenic grinding, also known as freezer milling, freezer grinding,
and cryomilling, is the act of cooling or chilling a material and then reducing it
into a small particle size. For example, thermoplastics are difficult to grind to
small particle sizes at ambient temperatures because they soften, adhere in
lumpy masses and clog screens. When chilled by dry ice, liquid carbon dioxide
or liquid nitrogen, the thermoplastics can be finely ground to powders suitable
for electrostatic spraying and other powder processes. Cryogenic grinding of
plant and animal tissue is a technique used by microbiologists. Samples that
require extraction of nucleic acids must be kept at −80 °C or lower during the
entire extraction process. For samples that are soft or flexible at room
temperature, cryogenic grinding may be the only viable technique for
processing samples. A number of recent studies report on the processing and
behavior of nanostructured materials via cryomilling
Cryogenic grinding was shown to significantly affect active
constituent levels in herbs. Test results showed an average increase of 15.6% in
constituents tested in four medicinal herbs when they were ground
cryogenically. The range was 10.7% to 21.8%, indicating that some herbs are
affected more than others by the temperatures at which they're ground.
Cryogenic grinding provides higher production rate, lower energy consumption,
finer particle size, more uniform particle distribution, lower grinding cost, .no
heat generation which is good while grinding spices and provides an inert
atmosphere thus eliminating the possibility of oxidation.
Freezer milling
Freezer milling is a type of cryogenic milling that uses a solenoid to mill
samples. The solenoid moves the grinding media back and forth inside the vial,
grinding the sample down to analytical fineness. This type of milling is
especially useful in milling temperature sensitive samples, as samples are milled
at liquid nitrogen temperatures.
The idea behind using a solenoid is that the only "moving part" in the
system is the grinding media inside the vial. The reason for this is that at liquid
nitrogen temperatures (–196°C) any moving part will come under huge stress
leading to potentially poor reliability. Cryogenic milling using a solenoid has
been used for over 50 years and has been proved to be a very reliable method of
processing temperature sensitive samples in the laboratory.
Cryomilling is a variation of mechanical milling, in which metallic powders or
other samples (e.g. temperature sensitive samples and samples with volatile
components) are milled in a cryogen (usually liquid nitrogen or liquid
argon) slurry or at a cryogenics temperature under processing parameters, so a
nanostructured microstructure is attained. Cryomilling takes advantage of both
the cryogenic temperatures and conventional mechanical milling.[5] The
extremely low milling temperature suppresses recovery and recrystallization
and leads to finer grain structures and more rapid grain refinement. [6] The
embrittlement of the sample makes even elastic and soft samples grindable.
Tolerances less than 5 µm can be achieved. The ground material can be
analyzed by a laboratory analyzer. Grinding of Seeds
Experimental Procedure
Grinding of Seeds
Two varieties of Coriander namely RCr-436, and Sudha were obtained
from seed store of NRCSS, Ajmer. The seeds were cleaned and used for
grinding. Cryogenic grinding of seeds was done using cryogenic grinder (Hoso-
Kava Alpine, Germany) model Fine Impact Mill 100UPZ at Central Institute for
Post Harvest Engineering and Technology, Ludhiana. Feed rate of material was
set at 1 kg/hr with screw speed 3 rpm. The speed of pin mill was set at 10,000
rpm. Inlet temperature was adjusted to below -50 ºC and outlet temperature was
-5 to 15ºC. Product particle size was set on 50 microns. In the process of
cryogenic grinding the material is feed into a feeder hopper and dropped into a
conveyor where the material to be processed enters the pre-chilled conveyor.
Liquid nitrogen is then sprayed and blended directly onto the material. The
material is conveyed via a stainless steel special design auger. The auger not
only transports the grinding media, but also mixes it with liquid nitrogen for
greater cooling efficiencies. Liquid nitrogen is added until the temperature of
the material is reduced to a predetermined set point. This set point is the glass
transition temperature of the material. The extremely low temperature in the
grinder solidifies oils so that the spices become brittle, Int. J. Mod. Phys. Conf.
Ser. 2013.22:589-592.
Cryogenic Grinding: A Physical Technique to Retain Volatile Content
591 they crumble easily permitting grinding to a finer and more consistent size.
Finally the brittle material enters an impact (pin) mill where it is ground to a
desired particle size. Computer controls the entire process.
The Cryogenic ground powder was quickly packed in aluminum foil
packets using sealing machine and opened at the time of analysis. For obtaining
seed powder through conventional grinding dried seeds (30 gm) was ground
separately by domestic mixer grinder (Sujata, model Dynamix, 810 W) and
packed in sealed polythene bags.
Essential Oil Extraction
The ground powder of coriander genotypes were then examined for
essential oil extraction of each genotype was extracted by hydro-distillation of
50 g ground seeds using a Celevenger apparatus. The oil has a characteristic
odor of linalool and a mild, sweet, warm, aromatic flavor. In the food industry,
coriander oil is used as a flavoring agent and adjuvant.

Practical applications
Cryogenic grinding of spices and herbs not only retain the volatiles with
no loss as well as maintain the originality in flavor quality, thus has prospective
commercial uses. Enhancement of pharmacological properties opens another
important avenue for utilization of this technology for herbal grinding in
Ayurveda and other traditional system of medicine. Particle size up to 50 μm
may be achieved by cryogenic grinding which in turn will be more effective in
medicinal or therapeutic use. Less quantity of herbal drugs will be required if
ground cryogenically.
Applications in biology
Cryogenic grinding (or "cryogrinding") is a method of cell disruption
employed by molecular life scientists to obtain broken cell material with
favorable properties for protein extraction and affinity capture. Once ground,
the fine powder consisting of broken cells (or "grindate") can be stored for long
periods at –80°C without obvious changes to biochemical properties – making it
a very convenient source material in e.g. proteomic studies including affinity
capture / mass spectrometry
References
1. C. T. Murthy and S. Bhattacharya, Journal of Food Engineering. (2008).
2. C. A. Pesek, L. A. Wilson and E. G. Hammond, Journal of Food Science.
(1985).
3. J. Rice, J. Food Processing.