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R
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.2,C
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a
ude D
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oa
nn
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ich
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l Paqu
o
t
-
,
C
h
ris
ti
a
n
Fo
u
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n
iesê,
J
ea
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-C
hri
s
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o
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Lambr
e
cht
s", C
h
r
i
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Bl
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!
1Gembloux Agricultural University. DepanmenrofFood Technology (Head: Prof C.Deroanne),URL:httpJ/www.fsagx.ac.belta2 Gembloux Agricultural University.Department or lndustrial Biological Chemistry (Head: Prof. M.PaqUOC).
Passage des Déportés. 2.B-S030 Oernbloux.Belgium. 3 Cosucra Groupe Warcoing SA.Ruedela sucrerie. 1.8-7740 Warcoing. Belgium
4CERTECH. Analytical Sciences-Microscopy. RueJulesBordet. 1.8-7180, Seneffe. Belgium.
m
cosucra
Groupe Warcoing
Characterization of the physical state of spray-dried inulin
Introduction
l
nu
l
i
n
is a
m
ix
tu
r
e
of
p
o
l
ys
ac
c
har
i
d
es co
m
posed o
f
a
c
h
a
i
n
o
f
fr
ucto
s
e un
i
t
s
w
i
th
ge
n
e
ra
ll
y a
terminalg
lu
cos
e un
i
t
.
Fo
r n
ow,
c
o
mm
e
r
c
i
a
l in
uli
n
i
s ex
t
r
a
c
t
ed
fr
o
m c
h
ic
o
ry r
oo
t and
is ava
i
l
a
b
l
e
as a s
pr
ay
-
dried p
ow
de
r
p
r
odu
c
t
, w
h
i
c
h h
as
th
e a
d
va
nt
ag
e
o
f
l
ow
pr
od
u
c
ti
o
n
co
s
t
s
c
o
mpared
t
o o
t
he
r
d
r
y
i
n
g
t
e
c
hn
i
q
u
e
s
(e
.
g
.
,
f
r
ee
z
e d
r
yi
n
g
)
.
Sp
r
ay-
dryi
n
g
p
r
oduce
s
p
o
wde
r
b
y a
t
o
m
i
zin
g
a
so
lu
t
i
o
n
o
r
s
l
u
rr
y
(
n
a
m
e
d f
ee
d
)
a
n
d e
v
ap
o
r
a
ti
ng
m
o
i
s
t
u
r
e
fr
o
m th
e
r
esu
lti
n
g
dr
o
p
l
e
t
s
b
y s
u
s
p
e
n
din
g
them
in h
o
t
g
a
s.
W
hi
l
e
m
ov
i
n
g
i
n
t
hi
s
h
o
t
m
e
di
um
,
t
he drople
t
s
ar
e
d
r
i
ed i
n
t
o
i
n
d
i
v
i
du
a
l
o
r
agg
l
o
m
erate pow
d
er pa
rti
c
l
e
s.
Sp
r
a
y
-dr
y
i
n
g
t
ri
a
l
s
r
e
rn
ain ve
r
y
co
mp
l
i
ca
t
ed a
nd
e
x
pen
s
i
v
e un
d
e
r
i
ndu
s
tr
i
a
l
c
o
n
d
i
t
i
o
n
s
.
F
o
r th
i
s
r
e
a
so
n
,
pi
l
o
t
sca
l
e
s
pr
ay
-dri
er
s a
re i
n
te
r
e
s
tin
g
t
o
o
l
s
f
o
r
i
n
v
e
s
t
iga
t
i
n
g
the
i
nf
l
u
e
n
ce o
f
fee
d
c
h
arac
t
e
ri
s
ti
c
s o
r d
r
y
i
n
g
p
ara
m
eter
s
o
n
t
h
e
ph
ys
ic
a
l pr
ope
rt
ie
s o
f
t
h
e powder
s,
w
h
ic
h h
a
v
e
a direct i
mp
a
c
t
o
n t
h
e
te
c
h
n
o
fu
n
c
t
i
o
n
a
l
proper
t
ie
s
(
s
ol
u
bi
l
it
y o
r
d
i
s
pe
r
s
i
bi
li
t
y
in
wa
t
er
, s
t
a
b
il
i
t
y
duri
n
g s
tor
ag
e
.
.
.
)
l
n
thi
s s
t
u
d
y,
w
e
i
n
v
e
s
t
iga
t
e
d th
e imp
o
rt
a
n
c
e
o
f
th
e
f
e
e
d te
mp
e
ra
tur
e
(4
0
-
95
°
C
)
a
nd the in
l
e
t
a
ir t
e
mp
e
r
at
ure
of
the
s
pr
a
y
-dri
e
r (
1
2
0
-
2
3
0
°
C) o
n th
e p
h
ys
ica
l
and morp
h
o
lo
g
i
ca
l
p
r
o
p
e
r
t
i
e
s o
f
s
p
r
a
y
-
d
ried p
o
w
d
e
r
.
The ph
y
s
i
c
a
l p
r
o
per
tie
s
e
s
tim
a
t
ed were
th
e g
l
ass
tr
a
n
s
iti
o
n temp
e
r
a
t
u
r
e (
T
g
) a
nd th
e c
r
y
s
t
a
ll
init
y
ind
e
x,
in
v
es
ti
ga
t
e
d b
y
m
o
du
l
ate
d di
ffe
rential
s
ca
nn
i
n
g ca
l
ori
m
e
t
r
y
(
M
DS
C
) a
n
d
w
id
e a
n
g
l
e
x
-
r
a
y
sca
tt
er
in
g
(
W A
XS)
,
r
e
s
p
ec
t
i
v
e
l
y
.
ln
a
dditi
o
n
,
en
v
ir
o
nment
a
l
s
c
a
nnin
g
e
l
ec
tr
o
n mi
c
r
os
c
o
p
y
(
ESE
M)
wa
s
u
s
e
d f
o
r
t
h
e
s
u
r
f
ac
e
a
n
d
p
a
rt
ie
l
e s
h
a
p
e c
h
a
r
a
ct
e
ri
z
a
ti
o
n
o
f t
h
e
p
ow
de
r
.
W
id
e A
n
g
le
X
-R
ay Sca
tt
e
rin
g (W AXS)
...
.
.
1
.,-
./
\
.
,
---
-.
. \
lit
~
)(
.
.
-~
-
\
:
::;
.
/
.
-The:WAXS eparerus was aPW3710 Philips Analytical X-ray B.V.
with
an
anodedevieeoperating alt
OkV
and30mAO
.
'
"'
1.54178 Â)in conjunction withapeœonionnal detecterinthe4<29<300 range.I
n
l
et air
t
e
m
perat
u
re:
1
20
0e
14 24
Diffraction angle (29)
Oiffmctograms in the4°<29<300rangepresent eitherabread halo pattern. ordiffraction pcaks, characteristic of anarnorphousor ascrm -crystaulne sample,rcspectivety.
AnIrcreascin thefeedtemperature induced a highcr sctubilizauon of inulinandthusincreased the amorphous index.
120 140 160 180 200
Temperature(De)
MDSC total beatflow curves presented one or Iwo cndothc:nnic peaks labeled Tml (lcwer melting peak) and Tm2 (highcr mclting peak).
Tml shifted to a highe:rtemperature asthe fecdtemperature increased. butTm2 did notshift.
The maindifferences bcrwcenparticJe morphologies were observed
for the various fccd temperatures, and wereprobably due toa difference in the metting of crystals present in Ihedispersion. Increasmg thetemperature of thefeed 100toasmoother powder surface, probably due10thespray drying ofasolution rathertitana dispersion. Thedrying ofadispersion containing undissolved solid particJcs (Tfccd<800
e
)
.
led10powders withroughsurfaces.120 140 160 180 200
Temperature("q
MDSC total heatIlow curvespresented one or IwO endolhennic pcaks
60 80 100 labelcd Tml (lower melting peak) andTm2 (higher melting peak).
1
-
T_e_m_pe_'_atu_"'_(O_Cl-
f
=~'::=n~~~~:::~~i~a~~t~=~ture IncreesedasalsoConclusions
T
h
e
f
ee
d temper
a
tu
r
e and
t
h
e
i
nl
et temp
e
r
atu
r
e w
e
r
e
fo
un
d t
o
h
a
ve
significanteff
ec
t
s
00th
e
p
h
ysica
l
a
n
d
m
o
r
ph
o
l
ogi
ca
l
pr
o
pert
i
es o
f
s
p
r
a
y-
d
r
i
ed
i
nu
l
i
n
.
A
n
in
cr
eas
e
in
t
he
f
ee
d te
m
pe
r
a
tu
r
e o
r
t
o
a
l
e
sse
r
e
x
t
e
nt
,
t
h
e
in
l
e
t ai
r
t
e
mp
e
r
a
ture
r
es
ult
e
d i
n
a
n in
c
r
e
as
e o
f th
e
a
m
o
r
p
h
o
u
s co
n
t
e
n
t
i
n th
e
s
pr
a
y
-
dr
ied
pr
o
du
ct
s.
B
y s
e
l
e
c
tin
g
a
pp
ro
p
r
i
a
t
e
f
e
ed
o
r
in
l
e
t
a
i
r
t
e
m
pe
r
at
ur
e
s,
we were a
b
l
e
t
o
pr
o
d
u
ce
spray-driedinulin
wi
th th
e
d
e
s
i
r
ed
ph
ys
i
ca
l
properties.Su
c
h
properties
a
r
e of c
ruci
a
l imp
o
rt
a
n
ce
t
o
th
e
h
yg
r
o
sc
op
i
c
p
r
o
p
e
r
tie
s a
nd thu
s
ca
n
affec
t th
e
s
ta
bil
i
t
y o
f th
e
pr
od
u
c
t
in m
a
n
y
domainsl
i
k
e
f
oo
d t
ec
h
no
l
og
y
o
r
ph
a
rm
ace
uti
c
a
l
s
.
A
s
il
i
s
e
s
t
a
b
l
i
s
h
ed
th
a
t
a
m
o
rph
o
u
s
p
ro
duct
s
a
re m
o
r
e
h
y
g
r
o
s
co
pi
c
t
h
a
n
t
h
e
ir
c
r
y
s
tallin
e c
o
unt
e
r
p
a
rt
s,
t
hi
s
co
u
l
d ine
v
i
tabl
y
h
a
ve a
n
i
mp
act o
n
theirb
e
h
a
v
i
o
r durin
g s
t
o
r
age
.
F
o
r t
h
i
s
r
ea
s
o
n
,
the imp
a
ct
o
f
storageco
nd
i
ti
o
n
s
o
n b
o
th
s
t
a
b
i
li
t
y a
nd
p
r
o
du
c
t
q
u
a
l
it
y
o
f
a
m
or
ph
o
u
s a
nd
s
e
mi
-c
r
ys
t
a
llin
e
i
nu
l
in
w
i
l
l b
e eva
l
u
a
t
e
d
a
nd
d
i
sc
u
ss
e
d in fu
r
th
e
r
s
tud
ie
s.
Experimentation
and resuIts
S
pra
y
dr
y
in
g
lnulin (Fibrulinc XL coraincd fromCosucra Groupe Warcoing SA) dispersions were spray dricd into amistby atwo-fluid nozzlebymeansofcompressed air.Thenozzle was situated in the middle of the drying chamber spraying upwards. whereas the hot air was simultaneously introduced through anannular opening in thedryingchamber ceiling. The Iiquid feed ûow and thenoule pressure air Ilcw wcre 21 b-' and 2 bars. respectively. Two inlct airtemperatures of 120 and 230°C were rested, which corresponded to an outlct air
temperature of65-67 and 120 -125°e. respectivety.
Mo
dulat
e
d Diff
e
renti
a
i
Sc
annin
g
C
alorimetr
y
(M
D
SC)
....
0
,
.;-_-The MDSC measurements were reatizedby using a OSC 2920CE TAInstrument in nonhermetic aluminium pans. Heating rate was of 1.5°C.mÎn·1 and the OSC œil was purged with70cmê.min-'dr)' nitrogen.
Inlel air temperature:
BO
o
e
.
o+
-
----__ ---- __ ----~
"
80 00 F•• dl.fT1)ef.luf.("C) '00 14 24 Diffrllction angle (28)Theamorphous content incrcased Oltaninletairtemperature of 230°e. Dcspüe theresidence timeofdried inulin being rclauvely
short inthe spray-dricr. wccanner toraüyexclude thatasmall proportion could havehcatcd alatemperature abovethemetting
pointand thushave ahigher amorphous content.
! .,.1 t,11'1"1..: 11It(,.. -+<, l
1
I •..~Jtcntp •..r,lm, -,"'l
/
Tbe feed temperature affectcd the
sclubility. but also the chemical composition ofthe soluble fraction.
The average degree ofpolymenzauon of this fraction. reüecüng the molecular weight of the amorphous pan of the spray-dried product.
increascd with the feedtemperature.
This augmentation of the molecular
weighrledtc ahigher Tg.High inlet
air temperature alsc induced an increasc: of the Tg. probably from sorne meltcdcrystafs.
Ouring theatcrmzarion ofthefced inthespraydrying chamber. the undissolved solid particles can fuse togetber. probably by the presence ofsclnbilized mutinon their surface. The incrcascof the inlet air temperature induccd a blow ouiof theparticles.
Acknowledgments
Financial support wasprcvidedbytheWalloon Region ofBclgium (DGTRE) andCosucra Groupe Warcoing SA.Theauthors aregratcfultcMrs LynnDoranfor technical assistance.
