freeze drying report

7/24/2019 Freeze Drying Report

1/23

B. Tech. Seminar (CHE)

A Seminar Report

On

Title: FREEZE DRYI!

ame: San"ana Bhattachar##a

Roll $m%er: &&''

Cop# *or: Department

Date o* +$%mi++ion: '.,-.-,&

Department of Chemical Engineering

Herita/e In+tit$te o* Technolo/#0 1ol2ata


2/23

A Seminar Report

On

Title: FREEZE DRYI!

ame: San"ana Bhattachar##a

Roll $m%er: &&''

Cop# *or: Department

Date o* +$%mi++ion: '.,-.-,&

Department of Chemical Engineering

Herita/e In+tit$te o* Technolo/#0 1ol2ata


3/23

Abstract

Thi+ report pro3i4e+ an o3er3ie5 o* *ree6e 4r#in/ (l#ophili6ation) 5ith partic$lar rele3ance to

pharmace$tical an4 *oo4 an4 in4$+trial application+. The report 4i+c$++e+ the phenomenon

that i+ the *o$n4ation o* *ree6e 4r#in/ metho4 an4 the +peci*ic+ o* the proce++ in3ol3e4. The

compari+on o* %oth pre+er3ation proce++e+0 hot air an4 *ree6e74r#in/0 5a+ 4one ta2in/ into

acco$nt +e3eral important characteri+tic+ +$ch a+ +hrin2a/e0 /la++ tran+ition temperat$re0

proce++89$alit# interaction0 4r#in/ 2inetic+0 co+t+ an4 ne5 impro3ement+. An $p4ate4

%i%lio/raphic re+earch +er3e4 to compare %oth 4r#in/ proce++e+. Eperimental 4ata a+ 5ell a+

theoretical re+$lt+0 *rom +e3eral #ear+ o* re+earch in the +$%"ect0 5ere pre+ente4 an4 compile4

in or4er to +$pport concl$+ion+. F$rthermore0 the po++i%le impro3ement+ ha3e %een +tate4 a+

5ell.

1e#5or4+: *ree6e 4r#in/0 l#ophili6ation0 *ree6in/0 *oo4 in4$+tr#0 pharmace$tical


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Contents

1. Introduction 1

&.& Hi+tor# &

2. Basic principle 2

3. Freeze dring process !

.& ;re7treatment '

.- Free6in/ '

. ;rimar# 4r#in/

. Secon4ar# 4r#in/ o5 relati3e

h$mi4it#0 a+ o*ten *o$n4 on col4 4a#+0 +pee4+ +$%limation0 an4 +o 4oe+ +tron/ +$nli/ht. Sno5

a%+or%+ m$ch o* the near7in*rare4 portion o* +$nli/ht,an4 that ener/# accelerate+ it+ 5ater

molec$le+0 +pee4in/ +$%limation.

Figure 1: Phase diagram of water

The pha+e 4ia/ram o* 5ater repre+ent+ that t5o pha+e+ coei+t alon/ a line $n4er the /i3encon4ition+ o* temperat$re an4 pre++$re0 5hile at the triple point (,.,,' GC at ,.@& 2;a or @&,

m- ,.,& GC at ,.,,@, atm)0 all three pha+e+ coei+t. I* 5ater i+ coole4 %elo5 , GC an4

reheate40 there are t5o po++i%ilitie+. One $n4er normal pre++$re0 or a%o3e0 it 5ill t$rn into

li9$i4. B$t0 at +$%7atmo+pheric pre++$re+0 more preci+el#0 %elo5 ,.,,@ atm0 there i+nt eno$/h

am%ient pre++$re *or 5ater to li9$e*#. So it accept+ the heat o* +$%limation an4 t$rn+ into

3apo$r. Thi+ phenomenon i+ $tili6e4 %# *ree6e 4r#in/. Thi+ proce++ i+ per*orme4 at

temperat$re an4 pre++$re con4ition+ %elo5 the triple point0 to *acilitate +$%limation o* ice.

The entire proce++ i+ per*orme4 at lo5 temperat$re an4 pre++$re0 +o that $+e*$l *or 4r#in/ o*


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thermola%ile compo$n4+. ario$+ important +tep+ in3ol3e4 in l#ophili6ation proce++ 5hich

+tart *rom +ample preparation *ollo5e4 %# *ree6in/0 primar# 4r#in/ an4 +econ4ar# 4r#in/0 to

o%tain the *inal 4rie4 pro4$ct 5ith 4e+ire4 moi+t$re content.

Figure 2: Lyophilization cycle

The concentration /ra4ient o* 5ater 3apo$r %et5een the 4r#in/ *ront an4 con4en+er i+ the

4ri3in/ *orce *or remo3al o* 5ater 4$rin/ l#ophili6ation. The 3apo$r pre++$re o* 5ater

increa+e+ 5ith an increa+e in temperat$re 4$rin/ the primar# 4r#in/. There*ore0 primar#

4r#in/ temperat$re +ho$l4 %e 2ept a+ hi/h a+ po++i%le0 %$t %elo5 the critical proce++

temperat$re0 to a3oi4 a lo++ o* ca2e +tr$ct$re. Thi+ critical proce++ temperat$re i+ the collap+e

temperat$re *or amorpho$+ +$%+tance0 or e$tectic melt *or the cr#+talline +$%+tance. D$rin/*ree6in/0 ice cr#+tal+ +tart +eparatin/ o$t $ntil the +ol$tion %ecome+ maimall# concentrate4.

On *$rther coolin/0 pha+e +eparation o* the +ol$te an4 ice ta2e+ place. I* the +ol$te +eparate+

o$t in cr#+talline *orm0 it i+ 2no5n a+ the e$tectic temperat$re. In contra+t0 i* an amorpho$+

*orm i+ *orme40 the temperat$re i+ re*erre4 to a+ the /la++ tran+ition temperat$re.

Determination o* thi+ critical temperat$re i+ important *or 4e3elopment o* an optimi6e4

l#ophili6ation c#cle. D$rin/ primar# 4r#in/0 4r#in/ temperat$re +ho$l4 not ecee4 the

critical temperat$re0 5hich other5i+e lea4+ to Jmelt%ac2 or Jcollap+e phenomenon in ca+e o*

cr#+talline or amorpho$+ +$%+tance re+pecti3el#.

3. Freeze dring process

A t#pical *ree6e74r#in/ proce++ con+i+t+ o* *o$r important +ta/e+0 that i+0 pre7treatment0

*ree6in/0 primar# 4r#in/0 an4 +econ4ar# 4r#in/. In *ree6in/0 mo+t o* the +ol3ent0 t#picall#

5ater0 i+ +eparate4 *rom the +ol$te+ to *orm ice. The *ree6in/ +ta/e t#picall# ta2e+ +e3eral

ho$r+ to *ini+h. ;rimar# 4r#in/0 or ice +$%limation0 %e/in+ 5hene3er the cham%er pre++$re i+


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re4$ce4 an4 the +hel* temperat$re i+ rai+e4 to +$ppl# the heat remo3e4 %# ice +$%limation.

D$rin/ primar# 4r#in/0 the cham%er pre++$re i+ 5ell %elo5 the 3apo$r pre++$re o* ice0 an4

ice i+ tran+*erre4 *rom the pro4$ct to the con4en+er %# +$%limation an4 cr#+talli6ation onto

the col4 coil+plate+ (KL',MC) in the con4en+er. Secon4ar# 4r#in/ i+ the +ta/e 5here 5ater i+

4e+or%e4 *rom the *ree6e concentrate0 $+$all# at ele3ate4 temperat$re an4 lo5 pre++$re.

3.1 %re*treatment

;re7treatment incl$4e+ an# metho4 o* treatin/ the pro4$ct prior to *ree6in/. Thi+ ma# incl$4e

concentratin/ the pro4$ct0 *orm$lation re3i+ion (i.e.0 a44ition o* component+ to increa+e

+ta%ilit# an4or impro3e proce++in/)0 4ecrea+in/ a hi/h 3apor pre++$re +ol3ent or increa+in/

the +$r*ace area. In man# in+tance+ the 4eci+ion to pre7treat a pro4$ct i+ %a+e4 on theoretical2no5le4/e o* *ree6e74r#in/ an4 it+ re9$irement+0 or i+ 4eman4e4 %# c#cle time or pro4$ct

9$alit# con+i4eration+. =etho4+ o* pre7treatment incl$4e: Free6e concentration0 Sol$tion

pha+e concentration0 Form$lation to ;re+er3e ;ro4$ct Appearance0 Form$lation to Sta%ili6e

Reacti3e ;ro4$ct+0 Form$lation to Increa+e the S$r*ace Area0 an4 Decrea+in/ Hi/h apor

;re++$re Sol3ent+.

Similar tocr#oprotectant+0+ome molec$le+ protect *ree6e74rie4 material.

1no5n a+ l#oprotectant+0 the+e molec$le+ are t#picall# pol#h#4ro# compo$n4+ +$ch

a+ +$/ar+(mono704i70 an4pol#+acchari4e+)0pol#alcohol+0 an4 their

4eri3ati3e+. Trehalo+ean4 +$cro+eare nat$ral l#oprotectant+. Trehalo+e i+ pro4$ce4 %# a

3ariet# o*plant(*or eampleselaginellaandarabidopsis thaliana)0 *$n/i0 an4 in3erte%rate

animal+ that remain in a +tate o* +$+pen4e4 animation4$rin/ perio4+ o* 4ro$/ht (al+o 2no5n

a+ anh#4ro%io+i+).

3.2 Freezing

Free6in/ i+ a critical +tep in *ree6e 4r#in/ proce++ +ince the micro +tr$ct$re *orme4 4$rin/

*ree6in/ 4etermine+ %oth the 9$alit# o* the *inal pro4$ct an4 it+ proce++in/ characteri+tic+0

+$ch a+ the rate o* primar# 4r#in/ an4 +econ4ar# 4r#in/. The pro4$ct m$+t %e *ro6en to lo5

temperat$re to a point 5here it i+ completel# +oli4i*ie4. Free6in/ the pro4$ct 4ecrea+e+

chemical acti3it# %# 4ecrea+in/ molec$lar mo3ement.

In /eneral0 *ree6in/ i+ 4e*ine4 a+ the proce++ o* ice cr#+talli6ation *rom +$per coole4 5ater.

The *ree6in/ proce++ *ir+t in3ol3e+ the coolin/ o* the +ol$tion $ntil ice n$cleation occ$r+. Ice

cr#+tal+ %e/in to /ro5 at a certain rate0 re+$ltin/ in *ree6e concentration o* the +ol$tion0 a
http://en.wikipedia.org/wiki/Cryoprotectantshttp://en.wikipedia.org/wiki/Sugarhttp://en.wikipedia.org/wiki/Monosaccharidehttp://en.wikipedia.org/wiki/Disaccharidehttp://en.wikipedia.org/wiki/Polysaccharidehttp://en.wikipedia.org/wiki/Sugar_alcoholhttp://en.wikipedia.org/wiki/Trehalosehttp://en.wikipedia.org/wiki/Sucrosehttp://en.wikipedia.org/wiki/Planthttp://en.wikipedia.org/wiki/Selaginellahttp://en.wikipedia.org/wiki/Arabidopsis_thalianahttp://en.wikipedia.org/wiki/Fungihttp://en.wikipedia.org/wiki/Tardigradehttp://en.wikipedia.org/wiki/Tardigradehttp://en.wikipedia.org/wiki/Suspended_animationhttp://en.wikipedia.org/wiki/Cryptobiosishttp://en.wikipedia.org/wiki/Cryoprotectantshttp://en.wikipedia.org/wiki/Sugarhttp://en.wikipedia.org/wiki/Monosaccharidehttp://en.wikipedia.org/wiki/Disaccharidehttp://en.wikipedia.org/wiki/Polysaccharidehttp://en.wikipedia.org/wiki/Sugar_alcoholhttp://en.wikipedia.org/wiki/Trehalosehttp://en.wikipedia.org/wiki/Sucrosehttp://en.wikipedia.org/wiki/Planthttp://en.wikipedia.org/wiki/Selaginellahttp://en.wikipedia.org/wiki/Arabidopsis_thalianahttp://en.wikipedia.org/wiki/Fungihttp://en.wikipedia.org/wiki/Tardigradehttp://en.wikipedia.org/wiki/Tardigradehttp://en.wikipedia.org/wiki/Suspended_animationhttp://en.wikipedia.org/wiki/Cryptobiosis


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proce++ that can re+$lt in either cr#+talline or amorpho$+ +oli4+ or in mit$re+. Free6in/ an

a9$eo$+ pharmace$tical *orm$lation can %e con4$cte4 at a temperat$re at %elo5 7' GC.

The phenomena that ta2e place in *ree6in/ +tep are7

3.2.1 +uper*cooling

The retention o* the li9$i4 +tate %elo5 the e9$ili%ri$m *ree6in/ point o* the +ol$tion i+ terme4

a+ +$percoolin/. It al5a#+ occ$r+ 4$rin/ *ree6in/ o*ten in the ran/e o* &,7&'MC or more.

S$per7coolin/ i+ o* t5o t#pe+0

1. ,lobal super*coolingIt i+ the proce++ in 5hich the entire li9$i4 3ol$me ehi%it+ a +imilar le3el o* +$per coolin/.

2. (ocal super*cooling

In thi+ metho40 onl# a +mall 3ol$me o* the li9$i4 i+ +$per coole4. S$per7coolin/ i+ a non

e9$ili%ri$m0 meta7+ta%le +tate0 5hich i+ +imilar to an acti3ation ener/# nece++ar# *or the

n$cleation proce++.

3.2.2. Ice*nucleation

D$e to 4en+it# *l$ct$ation+ *rom Bro5nian motion in the +$per7coole4 li9$i4 5ater0 5ater

molec$le+ *orm cl$+ter+ 5ith relati3el# lon/7li3in/ h#4ro/en %on4+ 5ith +imilar molec$lar

arran/ement+ a+ in ice cr#+tal+. $cleation i+ o* t5o t#pe+:

1.)omogeneous nucleation

The limitin/ n$cleation temperat$re o* 5ater i+ re*erre4 to a+ the homo/eneo$+ n$cleation

temperat$re that appear+ to %e at a%o$t 7,MC. At thi+ temperat$re0 p$re 5ater +ample 5ill

contain at lea+t one +pontaneo$+l# *orme4 acti3e 5ater n$cle$+0 capa%le o* initiatin/ ice

cr#+tal /ro5th.

2. )eterogeneous nucleation


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In hetero/eneo$+ n$cleation ice7li2e cl$+ter+ are *orme4 3ia a4+orption o* la#er+ o* 5ater on

*orei/n imp$ritie+.

3.2.3 Ice crstal gro-th

Once the critical ma++ o* n$clei i+ reache40 ice cr#+talli6ation occ$r+ rapi4l# in the entire

+#+tem 5hich lea4+ to the *ormation o* +ta%le ice cr#+tal+. Once +ta%le ice cr#+tal+ are

*orme40 their /ro5th procee4+ %# the a44ition o* molec$le+ to the inter*ace. A+ cr#+talli6ation

%e/in+0 the pro4$ct temperat$re ri+e+ rapi4l# to near the e9$ili%ri$m *ree6in/ point. A*ter the

initial ice net5or2 ha+ *orme40 a44itional heat i+ remo3e4 *rom the +ol$tion %# *$rther

coolin/ an4 the remainin/ 5ater *ree6e+ 5hen the pre3io$+l# *orme4 ice cr#+tal+ /ro5. Then$m%er o* ice n$clei *orme40 the rate o* ice /ro5th an4 the ice cr#+tal+ +i6e 4epen4 on the

4e/ree o* +$per7coolin/.

3.3 %rimar dring

It i+ characteri6e4 %# rece4in/ %o$n4ar# la#er o* ice in the 3ial. Thi+ +tep tra4itionall# i+

carrie4 o$t at cham%er pre++$re+ o* ,7,, Torr an4 +hel* temperat$re+ ran/in/ *rom 7,MC to

7&,M C. In thi+ pha+e the cham%er pre++$re i+ re4$ce4 $p to ,.,& to ,.&m%ar %# intro4$cin/

3ac$$m in to the pro4$ct cham%er. Heat i+ applie4 to the pro4$ct to ca$+e the *ro6en mo%ile

5ater to +$%lime. The 5ater 3apo$r i+ collecte4 on the +$r*ace o* a con4en+er. The con4en+er

m$+t ha3e +$**icient +$r*ace area an4 coolin/ capacit# to hol4 all the +$%lime4 5ater *rom

%atch at a temperat$re lo5er than the pro4$ct temperat$re. I* the temperat$re o* the ice on the

con4en+er i+ 5armer than the pro4$ct0 5ater 3apo$r 5ill ten4 to mo3e to5ar4+ the pro4$ct0

an4 the 4r#in/ 5ill +top. S$%limation *ront an4 the partial pre++$re o* 5ater 3apo$r in the

*ree6e 4r# cham%er. Since 3apo$r pre++$re i+ relate4 to temperat$re0 it i+ nece++ar# that the

pro4$ct temperat$re i+ 5armer than the con4en+er temperat$re. The molec$le+ o* 5ater mo3e

*rom hi/her 3apo$r pre++$re re/ion in the cham%er to5ar4+ the lo5er 3apo$r pre++$re re/ion

in the con4en+er. It i+ etremel# important that the temperat$re at 5hich a pro4$ct i+ *ree6e

4rie4 i+ %alance4 %et5een the temperat$re that maintain+ the *ro6en inte/rit# o* the pro4$ct

an4 the temperat$re that maimi6e+ the 3apo$r pre++$re o* the pro4$ct. Thi+ %alance i+ the

2e# to optim$m 4r#in/. The con4en+er i+ 2ept at a lo5 temperat$re0 /enerall# aro$n4 7@,GC.

The temperat$re o* the pro4$ct +ho$l4 %e 2ept a+ clo+e to the /la++ tran+ition temperat$re a+

po++i%le *or maim$m e**icienc# in 4r#in/.


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Figure 3: Comparison of minimum chamber pressure as a function of drying

rate

3.3.1 Differential energ balance in the dring laer

here,

NIe =ean 4en+it# o* 4r# pro4$ct &.'-@ 1/m

CIe Sp. heat o* 4r# pro4$ct (C4) P Sp. Heat o* 5ater (C5)0 Q2/.1

, Q2/.1 P &?@ Q2/.1

T& Temperat$re o* 4r# la#er

1Ie Thermal con4$cti3it# o* 4r# ;ro4$ct ,.''- m.1

Ie Thermal Di**$+i3it#0 m-+ec


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5 =a++ *l$ o* 5ater 3apor0 2/m-.+ec =ole *l$ o* 5ater 3apor

(/0molm-.+ec) =olec$lar 5ei/ht o* 5ater 3apor ( =/ &? /mol)

CN/ Sp. Heat o* 5ater 3apor &?', Q2/.1

2* Thermal con4$cti3it# o* the *ro6en material -.' m.1

N* Den+it# o* ice *ace


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4i**er in the metho4 %# 5hich the 4rie4 +$%+tance i+ inter*ace4 5ith a con4en+er. In mani*ol4

*ree6e74r#er+ a +hort $+$all# circ$lar t$%e i+ $+e4 to connect m$ltiple container+ 5ith the

4rie4 pro4$ct to a con4en+er. The rotar# an4 tra# *ree6e74r#er+ ha3e a +in/le lar/e re+er3oir

*or the 4rie4 +$%+tance.

!.1 otar freeze drer

Rotar# *ree6e74r#er+ are $+$all# $+e4 *or 4r#in/ pellet+0 c$%e+ an4 other po$ra%le +$%+tance+.

The rotar# 4r#er+ ha3e a c#lin4rical re+er3oir that i+ rotate4 4$rin/ 4r#in/ to achie3e a more

$ni*orm 4r#in/ thro$/ho$t the +$%+tance. Tra# +t#le *ree6e74r#er+ $+$all# ha3e rectan/$lar

re+er3oir 5ith +hel3e+ on 5hich pro4$ct+0 +$ch a+ pharmace$tical +ol$tion+ an4 ti++$e

etract+0 can %e place4 in tra#+0 3ial+ an4 other container+.

!.2 /anifold freeze drer

=ani*ol4 *ree6e74r#er+ are $+$all# $+e4 in a la%orator# +ettin/ 5hen 4r#in/ li9$i4 +$%+tance+

in +mall container+ an4 5hen the pro4$ct 5ill %e $+e4 in a +hort perio4 o* time. A mani*ol4

4r#er 5ill 4r# the pro4$ct to le++ than ' moi+t$re content. itho$t heat0 onl# primar#

4r#in/ (remo3al o* the $n%o$n4 5ater) can %e achie3e4. A heater m$+t %e a44e4 *or

+econ4ar# 4r#in/0 5hich 5ill remo3e the %o$n4 5ater an4 5ill pro4$ce lo5er moi+t$re

content.

!.3 0ra stle freeze drer

Tra# +t#le *ree6e74r#er+ are t#picall# lar/er than the mani*ol4 4r#er+ an4 are more

+ophi+ticate4. Tra# +t#le *ree6e74r#er+ are $+e4 to 4r# a 3ariet# o* material+. A tra# *ree6e7

4r#er i+ $+e4 to pro4$ce the 4rie+t pro4$ct *or lon/7term +tora/e. A tra# *ree6e74r#er allo5+

the pro4$ct to %e *ro6en in place an4 per*orm+ %oth primar# ($n%o$n4 5ater remo3al) an4

+econ4ar# (%o$n4 5ater remo3al) *ree6e74r#in/0 th$+ pro4$cin/ the 4rie+t po++i%le en47

pro4$ct. Tra# *ree6e74r#er+ can 4r# pro4$ct+ in %$l2 or in 3ial+ or other container+. hen

4r#in/ in 3ial+0 the *ree6e74r#er i+ +$pplie4 5ith a +topperin/ mechani+m that allo5+ a

+topper to %e pre++e4 into place0 +ealin/ the 3ial %e*ore it i+ epo+e4 to the atmo+phere. Thi+

i+ $+e4 *or lon/7term +tora/e0 +$ch a+ 3accine+.


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Impro3e4 *ree6e 4r#in/ techni9$e+ are %ein/ 4e3elope4 to eten4 the ran/e o* pro4$ct+ that

can %e *ree6e 4rie40 to impro3e the 9$alit# o* the pro4$ct0 an4 to pro4$ce the pro4$ct *a+ter

5ith le++ la%o$r.

#. Applications

Free6e74r#in/ (l#ophili6ation)0 5a+ 4e3elope4 to pre+er3e %ioacti3e molec$le+ (DA0

en6#me+0 an4 protein+)0 pharma7ce$tical+ pro4$ct+ (anti%iotic+) an4 other 4elicate0 +ol3ent7

impre/nate4 material+. Free6e74r#in/ i+ %ecomin/ an increa+in/l# pop$lar metho4 *or the

lon/7term pre+er3ation o* 3ario$+ %iolo/ical material+. Altho$/h to4a# a /reat 3ariet# o*

*oo4+0 pharmace$tical+0 etc. are pro4$ce4 %# l#ophili6ation0 a +$cce++*$l application *or lon/

term pre+er3ation o* li3in/ +#+tem+0 li2e cell+0 i+ +till one o* the /reate+t challen/e+ *or

+cienti+t+ in thi+ *iel4. Contin$o$+ inno3ation an4 proce++ optimi6ation ha3e increa+in/l# le4

to more an4 more ne5 application+ o* thi+ proce++ on an in4$+trial +cale. Free6e74r#in/

appear+0 there*ore0 a+ a promi+in/ techni9$e *or 4eh#4ration o* thermal7+en+iti3e material+0

+$ch a+ *r$it+. ;roce++in/ con4ition+ ha3e an in*l$ence on the 9$alit# criteria $+e4 to e3al$ate

*ree6e74rie4 *r$it+0 an4 on *ree6e 4r#in/ time. In *act0 t5o criteria (reh#4ration an4 tet$re)

are clo+el# lin2e4 5ith the $ltimate $+e o* the *ree6e74rie4 pro4$ct an4 cannot %e con+i4ere4

a+ a%+ol$te criteria. Deh#4rate4 *r$it+ are inten4e4 primar# to %e a44e4 to pro4$ct+ +$ch a+

corn *la2e+0 cereal %ar+0 ice cream0 pa+tr# +a$ce+0 etc. Free6e 4r#in/ i+ $+e4 eten+i3el# in

*oo4 an4 pharmace$tical in4$+trie+ eten+i3el#.

#.1 Food industr

The technolo/# 5a+ applie4 to con+$mer *oo4 pro4$ct+ a*ter the en4 o* the 5ar. Co**ee 5a+

one o* the *ir+t *ree6e74rie4 pro4$ct+ to %e mar2ete4 on a lar/e +cale. To4a#0 man# *r$it+03e/eta%le+0 meat+0 e//+0 an4 *oo4 *la3o$rin/+ are *ree6e74rie4.

Free6e74rie4 *oo4 ha+ man# a43anta/e+. Beca$+e a+ m$ch a+


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*oo4 retain+ m$ch o* it+ colo$r0 +hape0 tet$re0 an4 *la3o$r 5hen it i+ prepare4 *or

con+$mption %# reintro4$cin/ 5ater. Thi+ ma2e+ it more attracti3e to con+$mer+ than *oo4

pre+er3e4 %# +ome other metho4+.

#.1.1 a- materials

Some *oo4+ are etremel# 5ell7+$ite4 to the *ree6e74r#in/ proce++0 other+ 4o not *are +o 5ell.

>i9$i4+0 thin portion+ o* meat0 an4 +mall *r$it+ an4 3e/eta%le+ can %e *ree6e4rie4 ea+il#.

Co**ee i+ the mo+t common *ree6e74rie4 li9$i4. Ch$n2+ or +lice+ o* +hrimp0 cra%0 lo%+ter0

%ee*0 an4 chic2en can %e *ree6e74rie4. The# are o*ten mie4 5ith 3e/eta%le+ a+ part o* +o$p+

or main co$r+e entree+.

Figure 4: freeze dried fruit platter retains !a"or and te#ture well

Almo+t all *r$it+ an4 3e/eta%le+ can %e *ree6e74rie40 incl$4in/ %ean+0 corn0 pea+0 tomatoe+0

%errie+0 lemon+0 oran/e+0 an4 pineapple+. E3en item+ li2e oli3e+ an4 5ater che+tn$t+ can %e

proce++e4 thi+ 5a#.

Thic2 portion+ o* meat an4 lar/er0 5hole 3e/eta%le+ an4 *r$it+ cannot %e *ree6e 4rie4 5ith

an# +$cce++. ith man# other *oo4+0 it i+ +impl# not economical to pre+er3e them %# *ree6e

4r#in/.


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#.1.2 /anufacturing process

A *ree6e74r#in/ proce++in/ *acilit# i+ $+$all# a lar/e plant 5ith mo4ern e9$ipment. It *oo4

han4lin/ area+ m$+t %e appro3e4 %# the nite4 State+ Department o* A/ric$lt$re0 an4 thecompan# an4 it+ emplo#ee+ m$+t a4here to /o3ernment re/$lator# proce4$re+. The plant ma#

incl$4e a recei3in/ an4 +tora/e area *or ra5 *oo4+ that arri3e at the plant in %$l2 a *oo4

coo2in/ area *or tho+e *oo4+ that m$+t %e coo2e4 %e*ore proce++in/ a lar/e area 5ith +e3eral

lar/e *ree6in/ an4 4r#in/ cham%er+ an4 a pac2a/in/ area. The *acilit# ma# al+o incl$4e a

re+earch area 5here impro3e4 metho4+ o* *ree6e74r#in/ *oo4+ are 4e3elope40 an4 a te+t

2itchen 5here ne5 preparation techni9$e+ to impro3e the *inal ta+te0 9$alit#0 an4 tet$re o*

the *oo4 are trie4. Some plant+ are 4e4icate4 to *ree6e74r#in/ onl# one pro4$ct li2e *ree6e7

4rie4 co**ee. Other+ proce++ a 5i4e ran/e o* meat+0 3e/eta%le+0 an4 *r$it+. on*oo4 pro4$ct+

+$ch a+ chemical+ an4 pharmace$tical+ are $+$all# proce++e4 in +eparate plant+ *rom *oo4

pro4$ct+. The *ree6e74r#in/ proce++ 3arie+ in the 4etail+ o* temperat$re+0 time+0 pre++$re+0

an4 interme4iate +tep+ *rom one *oo4 to another.

#.1.3 Difference bet-een freeze dring and dehdration

hile %oth t#pe+ o* *oo47 4eh#4rate4 an4 *ree6e 4rie47 are e++entiall# 4rie40 the# 4i**er in a

*e5 important 5a#+. One o* the mo+t important 4i**erence+ i+ the proce++ $+e4 to create the

*inal pro4$ct.

hen *oo4 i+ 4eh#4rate40 the piece+ are place4 into a 5arm en3ironment that remo3e+ m$ch

o* the 5ater content. Thi+ ma# %e 4one nat$rall# %# la#in/ the c$t *r$it in the +$n on a hot

+$r*ace0 or mechanicall# %# r$nnin/ the *oo4 thro$/h machiner# that i+ 4e+i/ne4 to 4eh#4rate

the *oo4. In either ca+e0 there are no a44e4 chemical+ to enco$ra/e the proce++ an4 no +$/ar

a44e4 to the *oo4.

hile *ree6e7*rie4 *oo4 i+ al+o 4eh#4rate40 the proce++ *or preparin/ it i+ 4i**erent an4

+ome5hat more complicate4. Be*ore the 4r#in/ proce++ %e/in+0 the *oo4 i+ *ro6en. It i+ then

place4 into a cham%er that ma2e+ $+e o* a 3ac$$m to /ra4$all# etract the 5ater content.

Heat i+ applie4 in the cham%er an4 +et at a temperat$re that allo5+ the *ro6en *oo4 to 9$ic2l#

tha5 5hile the 3ac$$m etract+ the 5ater. The en4 re+$lt i+ a 4rie4 *oo4 that retain+ the ta+te

o* *re+h an4 al+o 4e3elop+ a cri+p# tet$re. hile %oth t#pe+ o* 4rie4 *oo4 ha3e a lon/ +hel*


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; a / e | 14

li*e0 there i+ a +i/ni*icant 4i**erence in ho5 lon/ the# 5ill 2eep $n4er normal con4ition+. In

/eneral0 4eh#4rate4 *oo4 5ill retain their ta+te an4 *la3o$r *or a perio4 o* one #ear. Free6e7

4rie4 *oo4 can ea+il# %e +tore4 *or +e3eral #ear+0 a++$min/ that the *oo4 i+ +eale4 in a

container that i+ airti/ht an4 moi+t$re *ree. The tet$re o* the *oo4 i+ al+o o*ten 4i**erent.

Foo4 that ha+ %een 4eh#4rate4 ha+ a more plia%le tet$re0 5hile *ree6e74rie4 3arietie+ ten4 to

%e cri+per an4 cr$nchier.

Figure $: Freeze dried and dehydrated fruits di%er "isibly in terms of te#tureand colour

#.2 %harmaceutical industr

;harmace$tical companie+ o*ten $+e *ree6e74r#in/ to increa+e the +hel* li*e o* the pro4$ct+0

+$ch a+ 3accine+ an4 other in"ecta%le+. B# remo3in/ the 5ater *rom the material an4 +ealin/

the material in a 3ial0 the material can %e ea+il# +tore40 +hippe40 an4 later recon+tit$te4 to it+

ori/inal *orm *or in"ection. Another eample *rom the pharmace$tical in4$+tr# i+ the $+e o*

*ree6e 4r#in/ to pro4$ce ta%let+ or 5a*er+0 the a43anta/e o* 5hich i+ le++ ecipient a+ 5ell a+

a rapi4l# a%+or%e4 an4 ea+il# a4mini+tere4 4o+a/e *orm.


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Figure &: 'canning (lectron )icroscopy *'()+ analysis of freeze dried

pharmaceutical product

#.3 0echnological industr

In chemical +#nthe+i+0 pro4$ct+ are o*ten *ree6e74rie4 to ma2e them more +ta%le0 or ea+ier to

4i++ol3ein 5ater*or +$%+e9$ent $+e.

In %io7+eparation+0 *ree6e74r#in/ can %e $+e4 al+o a+ a late7+ta/e p$ri*ication proce4$re0

%eca$+e it can e**ecti3el# remo3e +ol3ent+. F$rthermore0 it i+ capa%le o* concentratin/

+$%+tance+ 5ith lo5 molec$lar 5ei/ht+ that are too +mall to %e remo3e4 %# a *iltration

mem%rane.

Free6e74r#in/ i+ a relati3el# epen+i3e proce++. The e9$ipment i+ a%o$t three time+ a+

epen+i3e a+ the e9$ipment $+e4 *or other +eparation proce++e+0 an4 the hi/h ener/# 4eman4+

lea4 to hi/h ener/# co+t+. F$rthermore0 *ree6e74r#in/ al+o ha+ a lon/ proce++ time0 %eca$+e

the a44ition o* too m$ch heat to the material can ca$+e meltin/ or +tr$ct$ral 4e*ormation+.

There*ore0 *ree6e74r#in/ i+ o*ten re+er3e4 *or material+ that are heat7+en+iti3e0 +$ch

a+protein+0 en6#me+0 microor/ani+m+0 an4%loo4 pla+ma. The lo5operatin/ temperat$re o*

the proce++ lea4+ to minimal 4ama/e o* the+e heat7+en+iti3e pro4$ct+.

#. ! ther applications

Or/ani6ation+ +$ch a+ the Doc$ment Con+er3ation >a%orator# at the nite4 State+ ational

Archi3e+ an4 Recor4+ A4mini+tration (ARA) ha3e 4one +t$4ie+ on *ree6e74r#in/ a+ a

reco3er# metho4 o* 5ater74ama/e4 %oo2+ an4 4oc$ment+. hile reco3er# i+ po++i%le0

re+toration 9$alit# 4epen4+ on the material o* the 4oc$ment+. I* a 4oc$ment i+ ma4e o* a3ariet# o* material+0 5hich ha3e 4i**erent a%+orption propertie+0 epan+ion 5ill occ$r at a
http://en.wikipedia.org/wiki/Chemical_synthesishttp://en.wikipedia.org/wiki/Solutionhttp://en.wikipedia.org/wiki/Waterhttp://en.wikipedia.org/wiki/Filtrationhttp://en.wikipedia.org/wiki/Proteinhttp://en.wikipedia.org/wiki/Enzymehttp://en.wikipedia.org/wiki/Microorganismhttp://en.wikipedia.org/wiki/Blood_plasmahttp://en.wikipedia.org/wiki/Operating_temperaturehttp://en.wikipedia.org/wiki/Chemical_synthesishttp://en.wikipedia.org/wiki/Solutionhttp://en.wikipedia.org/wiki/Waterhttp://en.wikipedia.org/wiki/Filtrationhttp://en.wikipedia.org/wiki/Proteinhttp://en.wikipedia.org/wiki/Enzymehttp://en.wikipedia.org/wiki/Microorganismhttp://en.wikipedia.org/wiki/Blood_plasmahttp://en.wikipedia.org/wiki/Operating_temperature


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; a / e | 16

non7$ni*orm rate0 5hich co$l4 lea4 to 4e*ormation+. ater can al+o ca$+e mol4 to /ro5 or

ma2e in2+ %lee4. In the+e ca+e+0 *ree6e74r#in/ ma# not %e an e**ecti3e re+toration metho4.

In%acteriolo/#*ree6e74r#in/ i+ $+e4 to con+er3e +pecial +train+.

In hi/h7altit$4e en3ironment+0 the lo5 temperat$re+ an4 pre++$re+ can +ometime+ pro4$ce

nat$ral m$mmie+%# a proce++ o* *ree6e74r#in/.

A43ance4 ceramic+proce++e+ +ometime+ $+e *ree6e74r#in/ to create a *orma%le po54er *rom

a +pra#e4 +l$rr#mi+t. Free6e74r#in/ create+ +o*ter particle+ 5ith a more homo/eneo$+

chemical compo+ition than tra4itional hot +pra# 4r#in/0%$t it i+ al+o more epen+i3e.

Free6e 4r#in/ i+ al+o $+e4 *or *loral pre+er3ation. e44in/%o$9$etpre+er3ation ha+ %ecome

3er# pop$lar 5ith %ri4e+ 5ho 5ant to pre+er3e their 5e44in/ 4a# *lo5er+.

A ne5 *orm o* %$rial 5hich pre3io$+l# *ree6e74rie+ the %o4# 5ith li9$i4 nitro/en ha+ %een

4e3elope4 %# the S5e4i+h compan#;rome++a Or/anic AB0 5hich p$t+ it *or5ar4 a+ an

en3ironmentall# *rien4l# alternati3e to tra4itional ca+2et an4 cremation %$rial+.

$. %ossible impro&ements

De+pite +$cce++*$l operation o3er man# 4eca4e+0 tra# *ree6e 4r#er+ ha3e three +i/ni*icant

4i+a43anta/e+. Fir+t0 loa4in/ an4 $nloa4in/ i+ la%or7inten+i3e0 e+peciall# +ince lar/e $nit+

ma# contain +e3eral h$n4re4 tra#+. Secon40 the *ree6e74rie4 ca2e remo3e4 *rom the tra#+

o*ten re9$ire+ /rin4in/ to con3ert it to a *ree7*lo5in/ /ran$lar pro4$ct. Thir40 the *ormation

o* a J+2in o* 4rie4 pro4$ct on the +$r*ace o* the tra# hin4er+ the pa++a/e o* 3apor0 ma2in/

thi+ metho4 o* *ree6e 4r#in/ 3er# +lo5. Re+earch can %e 4e4icate4 to5ar4+ 4e3elopin/ a

9$ic2er an4 le++ la%or7inten+i3e *ree6e 4r#in/ proce++ that can pro4$ce *ree7*lo5in/ po54er+

*rom a +in/le proce++ 3e++el. 1no5n a+ Acti3e Free6e Dr#in/ technolo/#0 the ne5 proce++

$+e+ contin$o$+ motion to impro3e ma++ tran+*er an4 hence c$t proce++in/ time0 5hile al+o

eliminatin/ the nee4 to tran+*er pro4$ct to an4 *rom 4r#in/ tra#+ an4 4o5n+tream +i6e

re4$ction 4e3ice+.

Acti3e Free6e Dr#in/ metho4 can %e 4e3elope4 to %e $+e4 commerciall# at lo5er co+t+. Here0

te pro4$ct i+ *ir+t *ro6en in a +peciall#74e+i/ne4 4r#in/ 3e++el *itte4 5ith an a/itator. hether

the material to %e 4rie4 +tart+ o** a+ a li9$i40 /ran$lar +oli4 or pa+te0 the *orce4 motion in+i4e

the 4r#in/ 3e++el en+$re+ that it *ree6e+ in the *orm o* *ree7*lo5in/ +oli4 /ran$le+. Once the

pro4$ct i+ *$ll# *ro6en0 3ac$$m i+ applie4 an4 +$%limation +tart+. The initiall# coar+e /ran$le+
http://en.wikipedia.org/wiki/Bacteriologyhttp://en.wikipedia.org/wiki/Strain_(biology)http://en.wikipedia.org/wiki/Natural_mummyhttp://en.wikipedia.org/wiki/Ceramichttp://en.wikipedia.org/wiki/Slurryhttp://en.wikipedia.org/wiki/Spray_dryinghttp://en.wikipedia.org/wiki/Flower_bouquethttp://en.wikipedia.org/wiki/Liquid_nitrogenhttp://en.wikipedia.org/wiki/Promessa_Organichttp://en.wikipedia.org/wiki/Bacteriologyhttp://en.wikipedia.org/wiki/Strain_(biology)http://en.wikipedia.org/wiki/Natural_mummyhttp://en.wikipedia.org/wiki/Ceramichttp://en.wikipedia.org/wiki/Slurryhttp://en.wikipedia.org/wiki/Spray_dryinghttp://en.wikipedia.org/wiki/Flower_bouquethttp://en.wikipedia.org/wiki/Liquid_nitrogenhttp://en.wikipedia.org/wiki/Promessa_Organic


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/ra4$all# +hrin2 a+ the ice +tr$ct$re connectin/ the *ro6en material +$%lime+ a5a#0 #iel4in/ a

loo+e po54er con+i+tin/ o* 4r# particle+. Too m$ch 3apo$r creation i+ co$nterpro4$cti3e to

the proce++0 +o +en+or+ can %e 4e3elope4 to a3oi4 thi+ pro%lem.

'. Conclusion

ith h$n4re4+ o* 3ariant+ act$all# $+e4 in 4r#in/ o* partic$late +oli4+0 pa+te+0 contin$o$+

+heet+0 +l$rrie+ or +ol$tion+0 it pro3i4e+ the /reate+t 4i3er+it# amon/ *oo4 en/ineerin/ $nit

operation+. The+e chan/e+ alter the ph#+ical propertie+ +$ch a+ colo$r an4 +tr$ct$re. The# can

al+o 4e3elop $n4e+ira%le %iochemical reaction+0 +$ch a+ 4eterioration o* aroma compo$n4+ or

4e/ra4ation o* n$trient+. All the+e ph#+ical an4 %iochemical chan/e+ certainl# 4imini+h

pro4$ct+ 9$alit# an4 re4$ce proce++ e**icienc#. Free6e74r#in/ i+ a +peci*ic 4r#in/ metho4

5hich allo5+ o%tainin/ 4rie4 material+ 5ith *eat$re+ t#pical o* ra5 material.

Free6e74r#in/ i+ $+e4 *or the relia%le pre+er3ation o* a 5i4e 3ariet# o* heat7+en+iti3e pro4$ct+

an4 4eman4+ the hi/he+t +tan4ar4+ o* relia%ilit# an4 control. In a44ition to *oo4 pro4$ct+0 it

i+ +$ita%le *or other /oo4+0 incl$4in/: *lo5er+0 c$lt$re4 microor/ani+m+0 %$l2

pharmace$tical+0 me4ical 4e3ice+0 an4 co+metic+0 +peciall# chemical+0 pi/ment+ an4en6#me+. The mo+t important in thi+ proce++ are time0 temperat$re an4 pre++$re. I* the# are

5ell 4e*ine4 the# ma# in4ee4 a**ect the 9$alit# o* the *inal pro4$ct. n*ort$natel#0 hi/h

poro+it# o* 4rie4 material+ ha+ a ne/ati3e e**ect on +tora/e +ta%ilit#. Th$+0 *ree6e74rie4

material+ nee4 to %e +tore4 in a hermetic pac2a/e. The *ree6e74r#in/ proce++ i+ +till

epen+i3e0 5hich re+trict+ it+ application on 5i4e ran/e in the *oo4 in4$+tr#. e5 technical

+ol$tion+ are applie4 to mo4i*# the *ree6e74r#in/ proce++ an4 ma2e it time7 an4 co+t7

e**ecti3e0 e.g. i* 5e replace tra4itional heatin/ +o$rce %# micro5a3e+ ra4iation or 5e $+e a

+pra# no66le in 4r#er cham%er. Another +ol$tion to limit proce++ time i+ to $+e pre7treatment

a+ %lanchin/0 4eh#4ration %# in*rare4 ra4iation or o+motic 4eh#4ration.

eferences:

&. Bar%aree0 Q.=. an4 A. Sanche6. &


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-. Bar%aree0 Q.=.0 A. Sanche6 an4 !.. San4en. &

freeze drying report

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