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n\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg1}{\bkmkend Pg1}\par\pard
\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl-230\slmult0 \par\pard\
ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\
f2\fs20 Materiales y mtodos \par\pard\ql \li4352\sb0\sl-322\slmult0 \par\pard\ql\
li4352\sb152\sl-322\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf2\f3
\fs28 3- MATERIALES Y MTODOS \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql
\li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb24\sl-276\slmult0 \up0 \expndtw
-2\charscalex100 \ul0\nosupersub\cf3\f4\fs24 3.1. DISOLVENTES Y REACTIVOS \par\p
ard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb0\sl-276\slmult0 \par\pa
rd\ql\li1418\sb12\sl-276\slmult0 \up0 \expndtw-2\charscalex100 Los disolventes y
reactivos, normalmente de calidad PA-ACS, se utilizaron sin purificacin previa.
\par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb268\sl-276\slmult0
\up0 \expndtw-3\charscalex100 Los disolventes deuterados utilizados para RMN so
n: \par\pard\li1418\sb147\sl-276\slmult0\fi0\tx1778 \up0 \expndtw-3\charscalex10
0 -\tab \up0 \expndtw-3\charscalex100 CDCl\ul0\sub\cf5\f6\fs24 3\ul0\nosupersub\
cf3\f4\fs24 -d, grado de deuteracin mnimo 99,8% (Merck).\par\pard\li1418\sb137\sl276\slmult0\fi0\tx1778 \up0 \expndtw-3\charscalex100 -\tab \up0 \expndtw-3\chars
calex100 TFA-d, grado de deuteracin mnimo 99,8% (Aldrich).\par\pard\li1418\sb138\s
l-276\slmult0\fi0\tx1778 \up0 \expndtw-3\charscalex100 -\tab \up0 \expndtw-3\cha
rscalex100 TFA, grado de pureza 99,8% (Aldrich).\par\pard\li1418\sb136\sl-276\sl
mult0\fi0\tx1778 \up0 \expndtw-3\charscalex100 -\tab \up0 \expndtw-3\charscalex1
00 cido frmico-d, grado de deuteracin mnimo 98% (Aldrich).\par\pard\li1418\sb0\sl-27
6\slmult0\par\pard\li1418\sb274\sl-276\slmult0\fi0 \up0 \expndtw-3\charscalex100
Los enzimas utilizados en los ensayos de biodegradacin son:\par\pard\li1418\sb13
8\sl-276\slmult0\fi0\tx1778 \up0 \expndtw-3\charscalex100 -\tab \up0 \expndtw-3\
charscalex100 Papana (Carica papaya), 30,000 unidades/mg, N 7144 (Merck).\par\pard
\li1418\sb137\sl-276\slmult0\fi0\tx1778 \up0 \expndtw-3\charscalex100 -\tab \up0
\expndtw-3\charscalex100 Proteinasa K (Tritirachium album), 11.3 unidades/mg (S
igma).\par\pard\li1418\sb136\sl-276\slmult0\fi0\tx1778 \up0 \expndtw-3\charscale
x100 -\tab \up0 \expndtw-3\charscalex100 Lipasa (Pseudomonas cepacea), 40 unidad
es/mg (Fluka).\par\pard\li1418\sb137\sl-276\slmult0\fi0\tx1778 \up0 \expndtw-3\c
harscalex100 -\tab \up0 \expndtw-3\charscalex100 Lipasa (Candida cylindracea), 9
43 unidades/mg (Sigma).\par\pard\li1418\sb138\sl-276\slmult0\fi0\tx1778 \up0 \ex
pndtw-3\charscalex100 -\tab \up0 \expndtw-3\charscalex100 Lipasa (Rizophus delem
ar), 0.4 unidades/mg (Fluka)\par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql

\li1418\sb254\sl-276\slmult0 \up0 \expndtw-3\charscalex100 3.2. SNTESIS \par\pard
ql\li1418\sb12\sl-276\slmult0 \up0 \expndtw0\charscalex103 3.2.1. Sntesis de comp
uestos modelo. \par\pard\qj \li1418\sb0\sl-412\slmult0 \par\pard\qj\li1418\ri122
0\sb20\sl-412\slmult0 \up0 \expndtw0\charscalex105 La sntesis de los compuestos m
odelo se llev a cabo segn los procedimientos empleados en la \line \up0 \expndtw0\
charscalex100 preparacin de retro-pptidos.\ul0\super\cf5\f6\fs23 76 \ul0\nosupersu
b\cf3\f4\fs24 Para los dos compuestos con estructura: MeO-OC-R-NH-OC-R-CO-\line \
up0 \expndtw0\charscalex103 NH-R-CO-OMe, donde R es un grupo metileno para el ca
so del aminocido glicina y R\u8217? es el grupo \line \up0 \expndtw0\charscalex10
5 tereftlico (C\ul0\sub\cf5\f6\fs24 6\ul0\nosupersub\cf3\f4\fs24 H\ul0\sub\cf5\f6
\fs24 4\ul0\nosupersub\cf3\f4\fs24 ) u oxlico (CO-CO), el mtodo consisti en hacer r
eaccionar dos moles del ster \line \up0 \expndtw-1\charscalex100 metlico del aminoc
ido con un mol del dicloruro del cido correspondiente en presencia de trietilamin
a \line \up0 \expndtw-3\charscalex100 como base. \par\pard\qj \li1418\sb0\sl-413
\slmult0 \par\pard\qj\li1418\ri1219\sb15\sl-413\slmult0 \up0 \expndtw0\charscale
x100 El modelo: CH\ul0\sub\cf5\f6\fs24 3\ul0\nosupersub\cf3\f4\fs24 C\ul0\sub\cf
5\f6\fs24 6\ul0\nosupersub\cf3\f4\fs24 H\ul0\sub\cf5\f6\fs24 4\ul0\nosupersub\cf
3\f4\fs24 CO-NHCH\ul0\sub\cf5\f6\fs24 2\ul0\nosupersub\cf3\f4\fs24 CO-O(CH\ul0\s
ub\cf5\f6\fs24 2\ul0\nosupersub\cf3\f4\fs24 )\ul0\sub\cf5\f6\fs24 6\ul0\nosupers
ub\cf3\f4\fs24 O-OCCH\ul0\sub\cf5\f6\fs24 2\ul0\nosupersub\cf3\f4\fs24 NH-COC\ul
0\sub\cf5\f6\fs24 6\ul0\nosupersub\cf3\f4\fs24 H\ul0\sub\cf5\f6\fs24 4\ul0\nosup
ersub\cf3\f4\fs24 CH\ul0\sub\cf5\f6\fs24 3\ul0\nosupersub\cf3\f4\fs24 , se prepa
r en dos etapas. La \up0 \expndtw0\charscalex109 primera es una esterificacin con c
ido p-toluenosulfnico de dos moles de glicina con uno de \up0 \expndtw0\charscale
x107 1,6-hexanodiol. A continuacin, un mol del trmero anterior se trat con dos mole
s de cloruro de \up0 \expndtw-3\charscalex100 4-metilbenzoilo en presencia de tr
ietilamina como base. \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10
287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb19\sl-230\slmult0 \up0 \expndtw-4\
charscalex100 \ul0\nosupersub\cf1\f2\fs20 33
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}}\par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart P
g2}{\bkmkend Pg2}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0
\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmult0 \up0 \expndtw-2\charscal
ex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\ql \li1418\sb0\sl
-276\slmult0 \par\pard\ql\li1418\sb216\sl-276\slmult0 \up0 \expndtw0\charscalex1
03 \ul0\nosupersub\cf3\f4\fs24 3.2.2. Sntesis de polmeros. \par\pard\qj \li1418\sb
0\sl-410\slmult0 \par\pard\qj\li1418\ri1220\sb24\sl-410\slmult0 \up0 \expndtw0\c
harscalex100 El mtodo de polimerizacin empleado se eligi en funcin del tipo de polmer
o. Las poliesteramidas y \up0 \expndtw0\charscalex104 poliamidas fueron sintet
izadas por polimerizacin interfacial o trmica, y los polisteres por \up0 \
expndtw-3\charscalex100 polimerizacin trmica. \par\pard\ql \li1418\sb0\sl-276\slmu
lt0 \par\pard\ql\li1418\sb265\sl-276\slmult0 \up0 \expndtw-3\charscalex100 3.2.2
.1. POLIMERIZACIN INTERFACIAL \par\pard\qj \li1418\sb0\sl-412\slmult0 \par\pard\q
j\li1418\ri1221\sb20\sl-412\slmult0 \up0 \expndtw-2\charscalex100 Se trata de un
a reaccin bimolecular que tiene lugar en la interfase entre dos lquidos inmiscible
s. En la \up0 \expndtw-1\charscalex100 fase orgnica se encuentra disuelto el diha
luro de cido, y en la fase acuosa la diamina o el diol segn \up0 \expndtw0\charsca
lex106 se trate de poliamidacin o poliesterificacin, respectivamente. Esta tcnica a
provecha la mayor \up0 \expndtw0\charscalex104 reactividad de los dihaluros de ci

do frente a sus correspondientes disteres o dicidos.\ul0\super\cf5\f6\fs23 77 \ul0
\nosupersub\cf3\f4\fs24 Algunos \up0 \expndtw0\charscalex100 factores como la co
nversin de la reaccin pueden verse afectados por la agitacin del sistema. Dos \up0
\expndtw0\charscalex100 tipos de sistemas pueden ser empleados: sin agitacin y co
n agitacin. \par\pard\qj \li1418\ri1220\sb402\sl-420\slmult0 \up0 \expndtw0\chars
calex102 En los sistemas sin agitacin el polmero no es soluble en la interfase y a
l poner en contacto ambas \up0 \expndtw0\charscalex103 soluciones se observa la
formacin de un film o filamento, l cual puede tener resistencia mecnica \up0 \expnd
tw-2\charscalex100 suficiente para ir estirndose y eliminndose de forma contnua del
medio de reaccin. \par\pard\qj \li1418\ri1220\sb400\sl-420\slmult0 \up0 \expndtw
0\charscalex103 Los sistemas con agitacin se aplican a polmeros que precipitan rpid
amente y no es necesaria la \up0 \expndtw-2\charscalex100 formacin de un film par
a eliminarlo del medio de reaccin, el polmero es aislado por filtracin. \par\pard\q
j \li1418\ri1220\sb405\sl-414\slmult0 \up0 \expndtw0\charscalex103 Algunos facto
res que influyen en el rendimiento y peso molecular de los polmeros obtenidos por
el \up0 \expndtw0\charscalex109 mtodo de polimerizacin interfacial deben ser cons
iderados. En primer lugar, es necesaria la \up0 \expndtw-2\charscalex100 presenc
ia en la fase acuosa de una base inorgnica que neutralice el subproducto cido proc
edente de \up0 \expndtw0\charscalex107 la reaccin de condensacin, en caso contraro s
te reaccionara con la diamina para dar la sal \up0 \expndtw-1\charscalex100 hidro
clrica y se reducira sustancialmente el peso molecular resultante. Aunque las base
s fuertes son \up0 \expndtw0\charscalex100 mejores aceptores de subproductos cido
s y deben emplearse en la sntesis de poliamidas,\ul0\super\cf5\f6\fs23 78 \ul0\no
supersub\cf3\f4\fs24 deber \up0 \expndtw0\charscalex100 considerarse su eleccin en
el caso de monmeros con enlaces fcilmente hidrolizables a pH bsico. \up0 \expndtw2\charscalex100 En stos casos se escogen bases ms dbiles como el carbonato de sdio.
\par\pard\qj \li1418\ri1222\sb402\sl-420\slmult0 \up0 \expndtw-2\charscalex100 E
l dihaluro de cido puede sufrir hidrlisis dando lugar al dicido a concentraciones e
levadas de base y \line \up0 \expndtw-2\charscalex100 a bajas velocidades de pol
imerizacin. La hidrlisis no slo reduce la velocidad de polimerizacin, sino \par\pard
ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql
\li1418\sb37\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2
\fs20 34
}
ex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri1220
\sb390\sl-400\slmult0 \up0 \expndtw0\charscalex102 \ul0\nosupersub\cf3\f4\fs24 t
ambin limita en gran medida el peso molecular del polmero debido a que el dicido re
sultante no \up0 \expndtw-2\charscalex100 resulta reactivo a las temperaturas
en que tiene lugar la polimerizacin interfacial. \par\pard\qj \li1418\sb0\sl-412\
slmult0 \par\pard\qj\li1418\ri1220\sb19\sl-412\slmult0 \up0 \expndtw-1\charscale
x100 La eleccin del disolvente en la fase orgnica tambin juega un papel importante
en el control del peso \line \up0 \expndtw0\charscalex107 molecular, ya que la r
eaccin parece tener lugar en este lado de la interfase. El disolvente debe \line
\up0 \expndtw0\charscalex106 mantener disuelto el polmero en crecimiento hasta qu
e ste alcance un tamao suficientemente \line \up0 \expndtw-2\charscalex100 grande
como para precipitar. Disolventes como xileno y tetracloruro de carbono tienden

a dar polmeros \line \up0 \expndtw0\charscalex103 de peso molecular ms bajo que cl
oroformo o diclorometano porque precipitan todas las fracciones \line \up0 \expn
dtw-3\charscalex100 polimricas. \par\pard\qj \li1418\ri1219\sb408\sl-413\slmult0
\up0 \expndtw-2\charscalex100 A pesar de las ventajas que el mtodo representa, ex
isten ciertos inconvenientes que limitan su utilidad \line \up0 \expndtw0\charsc
alex100 industrial como el elevado coste de los reactivos y la grande cantidad d
e disolvente que es necesario \line \up0 \expndtw0\charscalex100 utilizar y recu
perar posteriormente. La polimerizacin interfacial puede utilizarse para obtener
diversos \line \up0 \expndtw-2\charscalex100 polmeros, aunque los policarbonatos
son los nicos que se obtienen actualmente a escala industrial. \par\pard\ql \li14
18\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb245\sl-276\slmult0 \up0 \expndtw-3\c
harscalex100 3.2.2.2. POLIMERIZACIN TRMICA \par\pard\qj \li1418\sb0\sl-410\slmult0
\par\pard\qj\li1418\ri1220\sb44\sl-410\slmult0 \up0 \expndtw0\charscalex105 El
mtodo de polimerizacin trmica es ventajoso respecto al de polimerizacin interfacial
para la \up0 \expndtw0\charscalex106 produccin industrial debido a que no es nece
saria la recuperacin de reactivos o cualquier otro \up0 \expndtw-3\charscalex100
tratamiento posterior a la polimerizacin. \par\pard\qj \li1418\ri1220\sb402\sl-42
0\slmult0 \up0 \expndtw0\charscalex104 Este proceso tiene un inters particular en
la preparacin industrial de polisteres. Concretamente \up0 \expndtw0\charscalex10
0 podemos ilustrar el proceso caracterstico seguido en la sntesis de los polisteres
relacionados con el \up0 \expndtw-3\charscalex100 presente trabajo. \par\pard\q
j \li1418\ri1221\sb407\sl-412\slmult0 \up0 \expndtw0\charscalex110 Los component
es, dicidos o sus steres y dioles, son aadidos en un recipiente provisto de \line \
up0 \expndtw0\charscalex109 condensador, una entrada de gas, un termmetro y agita
cin. En general se utiliza un exceso \line \up0 \expndtw-2\charscalex100 estequio
mtrico de diol debido a su mayor volatibilidad. Un flujo constante de nitrgeno es
suministrado \line \up0 \expndtw0\charscalex100 para eliminar el aire, mantenien
do la atmsfera inerte. Los componentes son calentados y agitados a \line \up0 \ex
pndtw-1\charscalex100 una temperatura cercana a 140-160\ul0\super\cf5\f6\fs23 \ul
0\nosupersub\cf3\f4\fs24 C para eliminar por destilacin el agua o alcohol, subpro
ductos de \line \up0 \expndtw-1\charscalex100 la reaccin de esterificacin segn si e
l reactivo empleado es un dicido o un dister. La viscosidad de \line \up0 \expndtw
0\charscalex102 la mezcla fundida aumenta conforme lo hace el peso molecular pro
medio del polmero, por lo que la \line \up0 \expndtw-1\charscalex100 agitacin es c
ada vez ms difcil. El polmero puede resultar de bajo peso molecular debido a la men
or \line \up0 \expndtw-1\charscalex100 difusin de los reactivos. El problema se e
vita elevando poco a poco la temperatura del sistema, la cual \par\pard\ql \li10
287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10
287\sb99\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs2
0 35
}
\sb390\sl-400\slmult0 \up0 \expndtw0\charscalex104 \ul0\nosupersub\cf3\f4\fs24 d
epender de la estabilidad trmica del polmero. En una segunda fase se prosigue la re
accin de \up0 \expndtw-2\charscalex100 condensacin sobre alto vaco para eliminar el
exceso de diol empleado en la polimerizacin. \par\pard\li1418\sb0\sl-276\slmult0
\par\pard\li1418\sb0\sl-276\slmult0\par\pard\li1418\sb7\sl-276\slmult0\fi0\tx282
8 \up0 \expndtw0\charscalex104 (1)\tab \up0 \expndtw0\charscalex104 HO\ul0\nosup
ersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R\ul0\nosupersub\cf6\f7\fs
24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 OH + HOOC\ul0\nosupersub\cf6\f7\fs24 \u-1
817?\ul0\nosupersub\cf3\f4\fs24 R\u8217?\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0
\nosupersub\cf3\f4\fs24 COOH \ul0\nosupersub\cf6\f7\fs24 \u8594?\ul0\nosupersub\
cf3\f4\fs24 HO\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R
\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 OCO\ul0\nosupers
ub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R\u8217?\ul0\nosupersub\cf6\f
7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 COOH + H\ul0\sub\cf5\f6\fs24 2\ul0\no
supersub\cf3\f4\fs24 O\par\pard\li1418\sb165\sl-276\slmult0\fi0\tx2834 \up0 \exp
ndtw0\charscalex104 (2)\tab \up0 \expndtw0\charscalex104 HO\ul0\nosupersub\cf6\f
7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R\ul0\nosupersub\cf6\f7\fs24 \u-1817?
\ul0\nosupersub\cf3\f4\fs24 OCO\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupers
ub\cf3\f4\fs24 R\u8217?\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f
4\fs24 COOH + n HO\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs2
4 R\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 OH + n HOOC\u
l0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R\u8217?\ul0\nosup
ersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 COOH \ul0\nosupersub\cf6\f
7\fs24 \u8594?\par\pard\ql \li2834\sb147\sl-276\slmult0 \up0 \expndtw0\charscale
x105 \ul0\nosupersub\cf3\f4\fs24 H\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosup
ersub\cf4\f5\fs24 [\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs
24 O\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R\ul0\nosupe
rsub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 OCO\ul0\nosupersub\cf6\f7\f
s24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R\u8217?\ul0\nosupersub\cf6\f7\fs24 \u-1
817?\ul0\nosupersub\cf3\f4\fs24 CO\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosup
ersub\cf4\f5\fs24 ]\ul0\sub\cf7\f8\fs24 n+1\ul0\nosupersub\cf6\f7\fs24 \u-1817?\
ul0\nosupersub\cf3\f4\fs24 OH + 2n H\ul0\sub\cf5\f6\fs24 2\ul0\nosupersub\cf3\f4
\fs24 O \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1222\sb38\
sl-413\slmult0 \up0 \expndtw0\charscalex100 Cada una de las sucesivas esterifica
ciones que conducen a la formacin del polister constituye un \up0 \expndtw0\charsc
alex107 verdadero equilibrio qumico. As pues, para obtener un polmero de alto peso
molecular debe \up0 \expndtw-4\charscalex100 desplazarse, tanto como sea posible
, el equilibrio de las reacciones hacia la derecha, o sea, eliminando \up0 \expn
dtw-5\charscalex100 el subproducto que se va formando por aplicacin de alto vaco.
\par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1221\sb14\sl-413\s
lmult0 \up0 \expndtw-1\charscalex100 La velocidad de la reaccin puede ser conside
rablemente aumentada por la accin de catalizadores. \up0 \expndtw0\charscalex100
Algunos trabajos de investigacin demuestran que cidos y varios compuestos organome
tlicos son \up0 \expndtw0\charscalex106 capaces de catalizar estas reacciones.\ul
0\super\cf5\f6\fs23 79\ul0\nosupersub\cf3\f4\fs24 Actualmente, los catalizadore
s de titanio son los ms \up0 \expndtw-3\charscalex100 empleados para la sntesis de
polisteres.\ul0\super\cf5\f6\fs23 80 \par\pard\ql \li1418\sb0\sl-276\slmult0 \pa
r\pard\ql\li1418\sb245\sl-276\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosuper
sub\cf3\f4\fs24 3.3. CARACTERIZACIN FISICOQUMICA \par\pard\qj \li1418\sb0\sl-420\s
lmult0 \par\pard\qj\li1418\ri1221\sb6\sl-420\slmult0 \up0 \expndtw-1\charscalex1
00 Los compuestos modelo se han caracterizado por espectroscopa de infrarrojo (IR
), espectroscopa de \up0 \expndtw0\charscalex100 resonancia magntica nuclear de pr
otn (\ul0\super\cf5\f6\fs23 1\ul0\nosupersub\cf3\f4\fs24 H-RMN) y carbono 13 (\ul
0\super\cf5\f6\fs23 13\ul0\nosupersub\cf3\f4\fs24 C-RMN) y determinacin del punto
\up0 \expndtw-3\charscalex100 de fusin (p.f.). \par\pard\qj \li1418\ri1220\sb409
\sl-410\slmult0 \up0 \expndtw0\charscalex109 La caracterizacin de los polmeros se
ha realizado mediante viscosimetra, cromatografa de \line \up0 \expndtw-2\charscal
ex100 permeabilidad en gel (GPC), espectroscopa de infrarrojo (IR), espectroscopa
de resonancia magntica \line \up0 \expndtw-2\charscalex100 nuclear de protn (\ul0\
super\cf5\f6\fs23 1\ul0\nosupersub\cf3\f4\fs24 H-RMN) y carbono 13 (\ul0\super\c
f5\f6\fs23 13\ul0\nosupersub\cf3\f4\fs24 C-RMN), calorimetra diferencial de barri
do \up0 \expndtw-3\charscalex100 (DSC), \par\pard\qj \li1418\ri1220\sb2\sl-420\s
lmult0 \up0 \expndtw0\charscalex100 termogravimetra (TGA), ensayos termodinamomecn
icos (DMTA), ensayos de solubilidad y ensayos \up0 \expndtw-3\charscalex100 de t
ensin-deformacin. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb24

3\sl-276\slmult0 \up0 \expndtw0\charscalex103 3.3.1. Evaluacin del peso molecular
. \par\pard\qj \li1418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri1220\sb24\sl-410
\slmult0 \up0 \expndtw0\charscalex107 Las reacciones de polimerizacin pueden prod
ucir cadenas polimricas con distinto nmero de \up0 \expndtw0\charscalex102 unidade
s repetitivas. La mayor parte de los polmeros sintticos son mezclas de macromolcula
s de \up0 \expndtw-2\charscalex100 distintos tamaos, por lo que el peso molecular
proporciona siempre un valor promedio. \par\pard\ql \li1418\sb0\sl-230\slmult0
\par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb19\sl-230\slmult0 \
up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 36 \par\pard\sect\sectd
\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg5}{\bkmkend Pg5}\par\
pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl-230\slmult0 \par\p
ard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\
cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\sb0\sl-414\slmult0 \par\pard
\qj\li1418\ri1221\sb364\sl-414\slmult0 \up0 \expndtw0\charscalex100 \ul0\nosuper
sub\cf3\f4\fs24 Son muchas las tcnicas existentes para la determinacin del peso mo
lecular medio de un polmero. \up0 \expndtw0\charscalex108 Por tanto, segn el mtodo
experimental utilizado se definen varios valores promedio del peso \up0 \expndtw
0\charscalex103 molecular: en nmero (M\ul0\sub\cf5\f6\fs24 n\ul0\nosupersub\cf3\f
4\fs24 ), en peso (M\ul0\sub\cf5\f6\fs24 w\ul0\nosupersub\cf3\f4\fs24 ) o viscos
imtrico (M\ul0\sub\cf5\f6\fs24 v\ul0\nosupersub\cf3\f4\fs24 ). La relacin entre lo
s valores de los \up0 \expndtw0\charscalex102 distintos promedios (M\ul0\sub\cf5
\f6\fs24 w\ul0\nosupersub\cf3\f4\fs24 /M\ul0\sub\cf5\f6\fs24 n\ul0\nosupersub\cf
3\f4\fs24 ) se conoce como polidispersidad (D) y se utiliza a menudo para dar un
a \up0 \expndtw-2\charscalex100 idea de la heterogeneidad del peso molecular en
las muestras de polmeros, o lo que es lo mismo, para \up0 \expndtw0\charscalex109
evaluar la anchura de la curva de distribucin de los pesos moleculares. Entre la
s tcnicas de \up0 \expndtw0\charscalex107 determinacin del peso molecular podemos
citar: la dispersin de luz, ebulloscopa, crioscopa, \up0 \expndtw-3\charscalex100 u
ltracentrifugacin, anlisis de grupos terminales y viscosimetra. \par\pard\qj \li141
8\ri1221\sb402\sl-420\slmult0 \up0 \expndtw0\charscalex106 Sin duda, una de las
tcnicas ms utilizadas es la viscosimetra. Esta tcnica para medir el peso \line \up0
\expndtw0\charscalex100 molecular de un polmero fue desarrollada por Staudinger e
n 1930.\ul0\super\cf5\f6\fs23 81\ul0\nosupersub\cf3\f4\fs24 Es una tcnica fcil y
rpida que \line \up0 \expndtw-1\charscalex100 permite conocer el peso molecular p
romedio viscosimtrico \up0 \expndtw-1\charscalex100 (M\ul0\sub\cf5\f6\fs24 v\ul0\
nosupersub\cf3\f4\fs24 ). Cuando el polmero es poco \par\pard\ql \li1418\sb99\sl276\slmult0 \up0 \expndtw-3\charscalex100 polidisperso, M\ul0\sub\cf5\f6\fs24 v\
ul0\nosupersub\cf3\f4\fs24 corresponde aproximadamente a M\ul0\sub\cf5\f6\fs24
w\ul0\nosupersub\cf3\f4\fs24 . \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard
\qj\li1418\ri1219\sb18\sl-413\slmult0 \up0 \expndtw-2\charscalex100 Por otro lad
o, la tcnica que proporciona mayor informacin sobre los pesos moleculares es la GP
C. La \line \up0 \expndtw0\charscalex102 determinacin de la polidispersidad a par
tir de la determinacin de M\ul0\sub\cf5\f6\fs24 w\ul0\nosupersub\cf3\f4\fs24 y M
\ul0\sub\cf5\f6\fs24 n\ul0\nosupersub\cf3\f4\fs24 se realiza habitualmente \lin
e \up0 \expndtw0\charscalex106 mediante esta tcnica basada en los principios del
fraccionamiento en funcin del tamao de las \line \up0 \expndtw-3\charscalex100 mac
romolculas. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb265\sl276\slmult0 \up0 \expndtw-3\charscalex100 3.3.1.1. DETERMINACIN DE LA VISCOSIDAD
INTRNSECA [\ul0\nosupersub\cf6\f7\fs24 \u951?\ul0\nosupersub\cf3\f4\fs24 ] \par\p
ard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1219\sb38\sl-413\slmult0
\up0 \expndtw0\charscalex100 La viscosidad de un polmero en solucin depende de la
naturaleza del polmero, del disolvente, de la \line \up0 \expndtw0\charscalex100
distribucin de pesos moleculares, de la concentracin y de la temperatura. Al elim
inar el efecto de la \line \up0 \expndtw-2\charscalex100 concentracin por medidas
a dilucin creciente se obtiene la viscosidad intrnseca que est relacionada \line \
up0 \expndtw0\charscalex104 con el peso molecular promedio de la distribucin deno
minado viscosimtrico, y que para un buen \line \up0 \expndtw0\charscalex103 solve
nte es prximo al promedio en peso. Para cuantificar la relacin viscosidad/peso mol
ecular se \line \up0 \expndtw0\charscalex102 requiere un calibrado con muestras
de peso molecular conocido, normalmente el promedio en peso \line \up0 \expndtw0

\charscalex100 determinado por dispersin de luz. En ausencia de patrones se utili
za la correlacin existente para un \line \up0 \expndtw0\charscalex109 polmero de n
aturaleza similar en el mismo solvente y temperatura. De este modo, se ignoran \
line \up0 \expndtw0\charscalex104 interacciones especficas del polmero en estudio
y el valor que se obtiene es slo orientativo pero \line \up0 \expndtw-3\charscale
x100 adecuado a efectos comparativos. \par\pard\ql \li10287\sb0\sl-230\slmult0 \
par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \
par\pard\ql\li10287\sb209\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosu
persub\cf1\f2\fs20 37
}
\sb374\sl-420\slmult0 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf3\f4\fs24 M
ediante la ecuacin de Hagen-Poiseuille para lquidos con movimiento en flujo lamina
r, se puede \up0 \expndtw0\charscalex102 relacionar el tiempo que tarda en pasar
un fluido por un capilar con la viscosidad del mismo, por lo \up0 \expndtw0\cha
rscalex100 tanto, la viscosidad de una solucin puede definirse como el tiempo que
tarda la disolucin en pasar \up0 \expndtw0\charscalex106 por un capilar fino por
efecto de la gravedad. La viscosidad intrnseca [\ul0\nosupersub\cf6\f7\fs24 \u95
1?\ul0\nosupersub\cf3\f4\fs24 ] es la extrapolacin a \up0 \expndtw-4\charscalex10
0 concentracin cero de la viscosidad reducida (\ul0\nosupersub\cf6\f7\fs24 \u951?
\ul0\sub\cf5\f6\fs24 red\ul0\nosupersub\cf3\f4\fs24 ), segn la expresin:\par\pard\
sect\sectd\sbknone\cols2\colno1\colw5760\colsr60\colno2\colw5940\colsr160\ql \li
4935\sb0\sl-276\slmult0 \par\pard\ql \li4935\sb79\sl-276\slmult0 \up0 \expndtw0\
charscalex100 [\ul0\nosupersub\cf6\f7\fs24 \u951?\ul0\nosupersub\cf3\f4\fs24 ] =
lm\par\pard\column \ql \li20\sb189\sl-276\slmult0\tx680 \up0 \expndtw0\charscale
x80 \ul0\nosupersub\cf6\f7\fs24 \u-1813? \up0 \expndtw-3\charscalex100 t\tab \up
0 \expndtw0\charscalex80 \u-1802?\par\pard\ql \li401\sb0\sl-192\slmult0\tx1200 \
up0 \expndtw0\charscalex104 \u8722?1\tab \up0 \expndtw-3\charscalex100 c\par\par
d\sect\sectd\sbknone\cols3\colno1\colw5780\colsr40\colno2\colw505\colsr160\colno
3\colw5285\colsr160\ql \li5361\sb1\sl-204\slmult0 \up0 \expndtw-3\charscalex100
\ul0\nosupersub\cf9\f10\fs20 c\u8594?0\par\pard\column \ql \li20\sb0\sl-216\slmu
lt0 \up0 \expndtw0\charscalex80 \ul0\nosupersub\cf6\f7\fs24 \u-1812? \up0 \expnd
tw-3\charscalex100 t\par\pard\ql \li20\sb0\sl-152\slmult0\tx237 \up0 \expndtw0\c
harscalex80 \u-1811? \tab \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf8\f9\f
s14 0\par\pard\column \qj \li20\ri5094\sb0\sl-192\slmult0 \up0 \expndtw0\charsca
lex80 \ul0\nosupersub\cf6\f7\fs24 \u-1801? \line \up0 \expndtw0\charscalex80 \u1800? \par\pard\sect\sectd\sbknone \ql \li1418\sb26\sl-255\slmult0 \up0 \expndtw
0\charscalex106 \ul0\nosupersub\cf3\f4\fs24 donde t y t\ul0\sub\cf5\f6\fs24 0\ul
0\nosupersub\cf3\f4\fs24 son los tiempos de cada de la disolucin y el disolvente;
c es la concentracin de la \par\pard\qj \li1418\ri1222\sb46\sl-400\slmult0 \up0
\expndtw0\charscalex102 disolucin en g.dL\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub
\cf3\f4\fs24 . Los tiempos son proporcionales a la viscosidad si son suficientem
ente grandes \up0 \expndtw-3\charscalex100 para lo cual debe elegirse adecuadame
nte el dimetro del capilar. \par\pard\qj \li1418\sb0\sl-400\slmult0 \par\pard\qj\
li1418\ri1220\sb40\sl-400\slmult0 \up0 \expndtw0\charscalex100 Una vez calculada
la viscosidad intrnseca, se puede determinar el peso molecular viscosimtrico (M\u

l0\sub\cf5\f6\fs24 v\ul0\nosupersub\cf3\f4\fs24 ) \up0 \expndtw-3\charscalex100
de un polmero a partir de la ecuacin de Mark-Houwink: \par\pard\ql \li5559\sb202\s
l-253\slmult0 \up0 \expndtw-3\charscalex100 [\ul0\nosupersub\cf6\f7\fs24 \u951?\
ul0\nosupersub\cf3\f4\fs24 ] = K.M\ul0\sub\cf5\f6\fs24 va \par\pard\qj \li1418\r
i1221\sb106\sl-400\slmult0 \up0 \expndtw0\charscalex104 \ul0\nosupersub\cf3\f4\f
s24 donde K (dL.g\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 ) y a so
n constantes tabuladas que dependen de la naturaleza del polmero, del \up0 \expnd
tw-5\charscalex100 disolvente y de la temperatura. \par\pard\ql \li1418\sb0\sl-2
76\slmult0 \par\pard\ql\li1418\sb267\sl-276\slmult0 \up0 \expndtw-2\charscalex10
0 Experimentalmente la determinacin de la viscosidad intrnseca se realiza midiendo
el tiempo de flujo \par\pard\qj \li1418\ri1222\sb6\sl-420\slmult0 \up0 \expndtw
0\charscalex100 (t) requerido para que un volumen determinado de disolucin polimri
ca atraviese el tubo capilar por \line \up0 \expndtw-4\charscalex100 efecto de l
a gravedad y el tiempo que tarda en hacerlo un volumen equivalente de disolvente
puro (t\ul0\sub\cf5\f6\fs24 0\ul0\nosupersub\cf3\f4\fs24 ). \par\pard\qj \li141
8\ri1219\sb400\sl-420\slmult0 \up0 \expndtw-2\charscalex100 Las medidas se efect
uaron en un viscosmetro capilar Cannon-Ubbelhode tipo semi-micro (modelo 150) \up
0 \expndtw-2\charscalex100 termostatizado a 25\ul0\nosupersub\cf6\f7\fs24 \ul0\no
supersub\cf3\f4\fs24 0.1\ul0\super\cf5\f6\fs23 o\ul0\nosupersub\cf3\f4\fs24 C en
un bao de agua. Se utiliz cido dicloroactico como disolvente, en el \up0 \expndtw-3
\charscalex100 rango de concentraciones 0.1 a 0.035 g/dL. \par\pard\ql \li1418\s
b0\sl-276\slmult0 \par\pard\ql\li1418\sb243\sl-276\slmult0 \up0 \expndtw-5\chars
calex100 3.3.1.2. CROMATOGRAFA DE PERMEACIN EN GEL (GPC) \par\pard\qj \li1418\sb0\
sl-412\slmult0 \par\pard\qj\li1418\ri1221\sb20\sl-412\slmult0 \up0 \expndtw0\cha
rscalex104 La cromatografa de permeacin en gel es una potente tcnica de separacin qu
e encontr gran \line \up0 \expndtw-3\charscalex100 aplicacin en el campo de los po
lmeros despus de su desarrollo en 1961.\ul0\super\cf5\f6\fs23 82 \ul0\nosupersub\c
f3\f4\fs24 Actualmente es la tcnica \line \up0 \expndtw0\charscalex100 ms utilizad
a para la separacin de las molculas de una muestra polimrica en funcin del tamao \lin
e \up0 \expndtw-3\charscalex100 molecular. Se produce como consecuencia de la di
ferente penetracin de las macromolculas a travs \line \up0 \expndtw0\charscalex103
de los poros de un gel dispuesto en el interior de una columna cromatogrfica. Los
materiales de \line \up0 \expndtw-4\charscalex100 relleno de la columna son pri
ncipalmente poliestireno poroso (entrecruzado e hinchado) y vidrio poroso. \par\
ard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb29\sl-230\slmult0 \up0 \e
xpndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 38
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\sb390\sl-400\slmult0 \up0 \expndtw0\charscalex102 \ul0\nosupersub\cf3\f4\fs24 L
os cromatgrafos utilizados son similares a los de HPLC, siendo la columna y el de
tector las partes \up0 \expndtw-3\charscalex100 ms importantes del instrumento. \
par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1221\sb17\sl-413\sl
mult0 \up0 \expndtw0\charscalex100 Cuando una disolucin polimrica, con diferentes
tamaos moleculares es introducida en el interior de \line \up0 \expndtw0\charscal
ex102 la columna cromatogrfica tiene lugar un fraccionamento en funcin de su tamao
molecular y de la \line \up0 \expndtw0\charscalex100 distribucin de tamao de poro
del gel polimrico. Las molculas de mayor tamao se arrastran con el \line \up0 \expn
dtw-1\charscalex100 disolvente, tardan menos tiempo en atravesar la columna y so
n las primeras en abandonarla, mientras \line \up0 \expndtw0\charscalex106 que l
as de tamao menor son retenidas durante un tiempo superior. A la salida de la col
umna se \line \up0 \expndtw0\charscalex107 registra la variacin entre el ndice de
refraccin del disolvente puro y la fraccin recogida. Para \line \up0 \expndtw-2\ch
arscalex100 conocer los valores de los pesos moleculares se requiere un calibrad
o con patrones. \par\pard\qj \li1418\ri1221\sb399\sl-423\slmult0 \up0 \expndtw0\
charscalex105 En este trabajo las medidas se realizaron en un cromatgrafo Waters
(modelo 510) equipado con \line \up0 \expndtw0\charscalex100 columnas \ul0\nosup
ersub\cf6\f7\fs24 \ul0\nosupersub\cf3\f4\fs24 -Stiragel (Polymer Lab.) de 10000 y
1000 \ul0\nosupersub\cf4\f5\fs24 \ul0\nosupersub\cf3\f4\fs24 de estireno-divini
lbenceno termostatizadas a \line \up0 \expndtw0\charscalex105 35\ul0\super\cf5\f
6\fs23 o\ul0\nosupersub\cf3\f4\fs24 C, con un detector de ndice de refraccin (RI
410) y un programa para tratamiento de datos \line \up0 \expndtw-1\charscalex10
0 (Mxima 820). El calibrado se realiz con muestras de poliestireno (Polysciences)
de baja dispersidad. \line \up0 \expndtw-1\charscalex100 El eluyente consisti en
una mezcla de cloroformo/ortoclorofenol (90/10, v/v) y su velocidad de flujo fue
\line \up0 \expndtw0\charscalex103 de 0.5 mL/min. El volumen inyectado fue de 1
00 \ul0\nosupersub\cf6\f7\fs24 \ul0\nosupersub\cf3\f4\fs24 L y la concentracin d
e las muestras fue de 2.5 \line \up0 \expndtw-3\charscalex100 mg/mL. \par\pard\q
j \li1418\ri1219\sb408\sl-410\slmult0 \up0 \expndtw0\charscalex100 En este traba
jo solamente se efectu el anlisis cromatogrfico con los polisteres. En los nylons y
en \up0 \expndtw0\charscalex104 las poliesteramidas no fue posible su realizacin
debido a los problemas de insolubilidad de estos \up0 \expndtw-3\charscalex100 m
ateriales en los disolventes orgnicos comunes. \par\pard\ql \li1418\sb0\sl-276\sl
mult0 \par\pard\ql\li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb0\sl-276\slmu
lt0 \par\pard\ql\li1418\sb113\sl-276\slmult0 \up0 \expndtw0\charscalex103 3.3.2.
Espectroscopa infrarroja (IR) \par\pard\qj \li1418\sb0\sl-420\slmult0 \par\pard\
qj\li1418\ri1220\sb6\sl-420\slmult0 \up0 \expndtw-1\charscalex100 Constituye una
tcnica espectroscpica de amplio uso que se basa en la excitacin de los modos de \u
p0 \expndtw0\charscalex107 vibracin de las molculas por la absorcin de la radiacin i
nfrarroja. Aunque esta comprende \up0 \expndtw-4\charscalex100 longitudes de ond
a (\ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosupersub\cf3\f4\fs24 ) entre el visi
ble y el microondas, la regin de infrarrojo medio entre 4000-300cm\ul0\super\cf5\
f6\fs23 -1 \up0 \expndtw-3\charscalex100 \ul0\nosupersub\cf3\f4\fs24 es la ms emp
leada desde un punto de vista prctico. Durante la excitacin es necesaria una varia
cin \up0 \expndtw-3\charscalex100 del momento dipolar de la molcula para que se pr
oduzca una absorcin en el IR que puede asociarse \up0 \expndtw0\charscalex106 a v
ibraciones de tensin (simtrica o asimtrica) o de deformacin. La deteccin de los grupo
s \up0 \expndtw-3\charscalex100 funcionales presentes es la principal aplicacin d
e la tcnica. \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl
-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb187\
sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 39 \par
\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg8}{\b
kmkend Pg8}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-23
\ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri2139\sb390
\sl-400\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf3\f4\fs24 Las ba
ndas de mayor importancia para los materiales estudiados se resumen a continuacin

: \up0 \expndtw-3\charscalex100 Metilenos \par\pard\ql \li2126\sb123\sl-276\slmu
lt0 \up0 \expndtw-3\charscalex100 2940 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersu
b\cf3\f4\fs24 : tensin asimtrica del C-H. \par\pard\ql \li2126\sb144\sl-276\slmult
0 \up0 \expndtw-3\charscalex100 2860 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\
cf3\f4\fs24 : tensin simtrica del C-H. \par\pard\ql \li1418\ri2990\sb6\sl-420\slmu
lt0\fi708\tx2126 \up0 \expndtw-3\charscalex100 1460 cm\ul0\super\cf5\f6\fs23 -1\
ul0\nosupersub\cf3\f4\fs24 : deformacin asimtrica del C-H. \line\tab \up0 \expndtw
-3\charscalex100 725 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : de
formacin simtrica del C-H. \line \up0 \expndtw-3\charscalex100 Amida \par\pard\ql
\li2126\ri5080\sb0\sl-420\slmult0 \up0 \expndtw-3\charscalex100 3300 cm\ul0\sup
er\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : vibracin de tensin del N-H (AMIDA A
). \line \up0 \expndtw-3\charscalex100 3100 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosu
persub\cf3\f4\fs24 : sobretono de la amida II (AMIDA B). \line \up0 \expndtw-3\c
harscalex100 1650 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : vibra
cin de tensin del C=O (AMIDA I). \par\pard\ql \li2126\sb79\sl-276\slmult0 \up0 \ex
pndtw-3\charscalex100 1550 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs2
4 : vibracin de torsin del N-H y tensin del C-N (AMIDA II). \par\pard\qj \li2126\ri
1222\sb34\sl-410\slmult0 \up0 \expndtw-2\charscalex100 1300-1250 cm\ul0\super\cf
5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : interacciones entre las vibraciones de
tensin del C-N y las de torsin del N-H. \up0 \expndtw0\charscalex100 Adems en esta
zona aparecen las vibraciones de tensin del C-C y de torsin de los grupos \up0 \e
xpndtw-3\charscalex100 CH\ul0\sub\cf5\f6\fs24 2\ul0\nosupersub\cf3\f4\fs24 y CH
(AMIDA III). \par\pard\ql \li2126\sb121\sl-276\slmult0 \up0 \expndtw-3\charscal
ex100 627 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : vibracin de to
rsin de N-C=0 (AMIDA IV). \par\pard\ql \li1418\ri3802\sb6\sl-420\slmult0\fi708\tx
2126 \up0 \expndtw-3\charscalex100 700 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersu
b\cf3\f4\fs24 : vibracin de torsin fuera del plano de N-H (AMIDA V). \line\tab \up
0 \expndtw-3\charscalex100 600 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4
\fs24 : vibracin de torsin fuera del plano de C=O (AMIDA VI). \line \up0 \expndtw
-3\charscalex100 ster \par\pard\ql \li2126\sb99\sl-276\slmult0 \up0 \expndtw-3\ch
arscalex100 1740 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : vibrac
in de tensin del C=O. \par\pard\ql \li2126\sb144\sl-276\slmult0 \up0 \expndtw-3\ch
arscalex100 1100 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : vibrac
iones de tensin (simtrica y asimtrica) del C-O. \par\pard\qj \li1418\sb0\sl-420\slm
ult0 \par\pard\qj\li1418\ri1218\sb6\sl-420\slmult0 \up0 \expndtw-1\charscalex100
Los espectros fueron registrados en espectrofotmetros de transformada de Fourier
Perkin-Elmer 1600 \up0 \expndtw0\charscalex106 y Perkin-Elmer 2000 a partir de
muestras slidas dispersas en pastillas de KBr o como pelculas \up0 \expndtw-3\char
scalex100 preparadas por evaporacin lenta del disolvente sobre ventana de NaCl. \
par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb0\sl-276\slmult0 \p
ar\pard\ql\li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb111\sl-276\slmult0 \u
p0 \expndtw0\charscalex103 3.3.3. Espectroscopa de resonancia magntica nuclear (RM
N) \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1222\sb18\sl-41
3\slmult0 \up0 \expndtw0\charscalex109 La tcnica de RMN se utiliza como complemen
taria a la espectroscopa infrarroja y constituye \line \up0 \expndtw0\charscalex1
09 actualmente una de las ms tiles y empleadas para conocer la estructura de los c
ompuestos \line \up0 \expndtw0\charscalex102 orgnicos. Su papel en el campo de lo
s polmeros se destaca especialmente por proporcionar datos \line \up0 \expndtw-2\
charscalex100 sobre su constitucin, organizacin y dinmica, que difcilmente podran obt
enerse por otros medios. \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li
\sb229\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20
40 \par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart
Pg9}{\bkmkend Pg9}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb
0\sl-230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charsca
lex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri122
La tcnica analiza la interaccin entre los niveles de energa de los espines de cier
tos ncleos atmicos \up0 \expndtw0\charscalex104 con la radiacin electromagntica. nica

mente los ncleos con momento magntico nuclear sern \up0 \expndtw0\charscalex105 obs
ervables. Los ncleos de sustancias orgnicas ms usuales en RMN, son los de protn (\ul
0\super\cf5\f6\fs23 1\ul0\nosupersub\cf3\f4\fs24 H) y \up0 \expndtw0\charscalex1
09 carbono 13 (\ul0\super\cf5\f6\fs23 13\ul0\nosupersub\cf3\f4\fs24 C). La posic
in de las seales obtenidas depende en los dos casos del entorno \up0 \expndtw0\cha
rscalex105 electrnico. Los espectros de \ul0\super\cf5\f6\fs23 1\ul0\nosupersub\c
f3\f4\fs24 H-RMN consisten en un registro de las seales de resonancia que \up0 \e
xpndtw0\charscalex104 corresponden a los diferentes tipos de hidrgeno presentes e
n la muestra en forma de picos cuya \up0 \expndtw0\charscalex104 posicin, anchura
, rea y subestructura permiten la potente caracterizacin arriba mencionada. La \up
0 \expndtw0\charscalex104 posicin est asociada a la identidad de los diferentes gr
upos vecinos a los protones y se expresa \up0 \expndtw0\charscalex106 como despl
azamiento qumico en ppm respecto a la seal de un grupo de referencia. El rea es \up
0 \expndtw-3\charscalex100 proporcional al nmero de protones presentes en la mues
tra. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb245\sl-276\sl
mult0 \up0 \expndtw0\charscalex100 Los espectros de RMN se realizaron con un esp
ectrofotmetro Bruker AMX-300 que opera a 300.13 y \par\pard\qj \li1418\ri1221\sb3
7\sl-406\slmult0 \up0 \expndtw-1\charscalex100 75.4 MHz para \ul0\super\cf5\f6\f
s23 1\ul0\nosupersub\cf3\f4\fs24 H y \ul0\super\cf5\f6\fs23 13\ul0\nosupersub\cf
3\f4\fs24 C, respectivamente. Experimentalmente estos espectros se obtienen diso
lviendo \line \up0 \expndtw0\charscalex100 la muestra en disolvente deuterados c
omo son el cloroformo (CDCl\ul0\sub\cf5\f6\fs24 3\ul0\nosupersub\cf3\f4\fs24 ), c
ido trifluoroactico (TFA-d) y \line \up0 \expndtw0\charscalex106 cido frmico. La di
solucin resultante se introduce en un tubo de vdrio especial de 5-10 mm de \line \
up0 \expndtw0\charscalex106 dimetro, se aade una gota de la substancia de referenc
ia \up0 \expndtw0\charscalex106 (TMS) y se introduce en el imn \par\pard\ql \li14
18\sb122\sl-276\slmult0 \up0 \expndtw-3\charscalex100 superconductor del aparato
\slmult0 \up0 \expndtw0\charscalex106 En el caso de los polmeros se pueden determ
inar su estructura qumica, la presencia de grupos \line \up0 \expndtw0\charscalex
100 terminales y posibles ramificaciones. La presencia de grupos terminales en e
l espectro se utiliza para \line \up0 \expndtw0\charscalex100 determinar el peso
molecular (M\ul0\sub\cf5\f6\fs24 n\ul0\nosupersub\cf3\f4\fs24 ) de los polmeros.
Por ltimo, tambin resulta til en el seguimiento \line \up0 \expndtw0\charscalex100
de la degradacin de polmeros. La aparicin de nuevas seales o la disminucin de la int
ensidad de \line \up0 \expndtw-2\charscalex100 otras existentes en el espectro i
nicial del polmero sirve para conocer el avance de la degradacin. \par\pard\ql \li
18\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb112\sl-276\slmult0 \up0 \expndtw0\ch
arscalex104 3.3.4. Anlisis trmico \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\par
d\qj\li1418\ri1221\sb18\sl-413\slmult0 \up0 \expndtw0\charscalex111 El anlisis trm
ico comprende un conjunto de tcnicas cuyo objetivo es la determinacin del \line \u
p0 \expndtw0\charscalex100 comportamiento trmico de un material en funcin de la te
mperatura o del tiempo. En el campo de los \line \up0 \expndtw0\charscalex100 po
lmeros las tcnicas ms usuales son: anlisis trmico diferencial (DTA), calorimetra difer
encial de \line \up0 \expndtw-2\charscalex100 barrido (DSC), anlisis termogravimtr
ico (TGA) y el anlisis trmico dinamomecnico (DMTA). \par\pard\ql \li10287\sb0\sl-23
0\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-23
0 \ul0\nosupersub\cf1\f2\fs20 41 \par\pard\sect\sectd\fs24\paperw11900\paperh168
40\pard\sb0\sl-240{\bkmkstart Pg10}{\bkmkend Pg10}\par\pard\ql \li1418\sb0\sl-23
\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y
mtodos \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb216\sl-276\s
lmult0 \up0 \expndtw-3\charscalex100 \ul0\nosupersub\cf3\f4\fs24 3.3.4.1. CALORI
METRA DIFERENCIAL DE BARRIDO (DSC) \par\pard\qj \li1418\sb0\sl-412\slmult0 \par\p
ard\qj\li1418\ri1220\sb20\sl-412\slmult0 \up0 \expndtw-2\charscalex100 En los ma
teriales polimricos, las transiciones trmicas ms importantes en DSC son la temperat

ura de \line \up0 \expndtw0\charscalex108 transicin vtrea (T\ul0\sub\cf5\f6\fs24 g
\ul0\nosupersub\cf3\f4\fs24 ) y la temperatura de fusin (T\ul0\sub\cf5\f6\fs24 f\
ul0\nosupersub\cf3\f4\fs24 ). En los polmeros amorfos la T\ul0\sub\cf5\f6\fs24 g\
ul0\nosupersub\cf3\f4\fs24 es la nica \line \up0 \expndtw0\charscalex103 transic
in que se registra y aparece como un cambio abrupto de la lnea base. Por otra part
e en los \line \up0 \expndtw0\charscalex100 muy cristalinos la T\ul0\sub\cf5\f6\
fs24 g\ul0\nosupersub\cf3\f4\fs24 es difcil de observar debido a la baja proporc
in de parte amorfa en el polmero. \line \up0 \expndtw-2\charscalex100 Los procesos
de fusin/cristalizacin dan informacin cualitativa sobre la temperatura del pico de
fusin \line \up0 \expndtw0\charscalex104 y cuantitativa sobre la cristalinidad d
el polmero (rea del pico). La fusin se manifiesta en un pico \line \up0 \expndtw0\c
harscalex103 endotrmico con subida ms o menos gradual y regular segn la naturaleza
e histria trmica de la \line \up0 \expndtw-1\charscalex100 muestra, y bajada brusc
a hasta recobrar la lnea base, que si se mantiene tras la fusin, puede decirse \li
ne \up0 \expndtw0\charscalex100 que el material es estable para ser procesado po
r fusin. Lo contrario es indicio de descomposicin y \line \up0 \expndtw-2\charscal
ex100 debe estudiarse con ms detalle por anlisis termogravimtrico. La cristalinidad
se evala usando como \line \up0 \expndtw0\charscalex108 referencia el calor de f
usin de un material 100% cristalino que puede estimarse a partir de las \line \up
0 \expndtw0\charscalex104 contribuciones de grupo.\ul0\super\cf5\f6\fs23 83\ul0\
nosupersub\cf3\f4\fs24 Los valores utilizados fueron -2.5 kJ/mol para el grupo s
ter, 2.0 kJ/mol \line \up0 \expndtw-2\charscalex100 para el grupo amida, 4.7 kJ/
mol para el grupo CH(CH\ul0\sub\cf5\f6\fs24 3\ul0\nosupersub\cf3\f4\fs24 ), 4.0
kJ/mol para el grupo metilnico y 5.0 kJ/mol \line \up0 \expndtw-3\charscalex100 p
ara el grupo p-fenilnico. \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li
1418\ri1220\sb15\sl-413\slmult0 \up0 \expndtw0\charscalex105 Normalmente en una
calorimetra rutinaria se registran 4 barridos. En el primer barrido se obtiene \l
ine \up0 \expndtw0\charscalex113 informacin acerca de la fusin de una muestra cris
talizada directamente en el proceso de \line \up0 \expndtw0\charscalex102 polime
rizacin. Inmediatamente despus de la fusin se procede el enfriamiento lento de la m
uestra \line \up0 \expndtw0\charscalex102 para observar la cristalizacin del fund
ido \up0 \expndtw0\charscalex102 (2 barrido). Posteriormente se realiza un segund
o \par\pard\qj \li1418\ri1220\sb0\sl-413\slmult0 \up0 \expndtw0\charscalex104 ca
lentamiento (3 barrido) para verificar la fusin de la muestra cristalizada a parti
r del fundido y la \up0 \expndtw0\charscalex100 reproducibilidad de las fusiones
observadas. Por ltimo, despus de haber sometido la muestra a un \up0 \expndtw-2\c
harscalex100 enfriamiento rpido, se hace un tercer calentamiento (4 barrido) que p
ermite determinar la temperatura \up0 \expndtw-3\charscalex100 de transicin vtrea
del material. \par\pard\qj \li1418\ri1221\sb409\sl-420\slmult0 \up0 \expndtw-1\c
harscalex100 Los anlisis trmicos se han efectuado en un calormetro diferencial de b
arrido Perkin-Elmer DSC-30 \line \up0 \expndtw-2\charscalex100 equipado con un t
ermoanalizador TA400 y en un calormetro Perkin-Elmer DSC-PYRIS 1. El calibrado \l
ine \up0 \expndtw0\charscalex102 se realiz con ndio (T\ul0\sub\cf5\f6\fs24 f\ul0\n
osupersub\cf3\f4\fs24 = 429.75 K, \ul0\nosupersub\cf6\f7\fs24 \u8710?\ul0\nosup
ersub\cf3\f4\fs24 H\ul0\sub\cf5\f6\fs24 f\ul0\nosupersub\cf3\f4\fs24 = 3.267 kJ
/mol). Las calorimetras se han registrado a una \line \up0 \expndtw0\charscalex10
2 velocidad de calentamiento de \up0 \expndtw0\charscalex102 20\ul0\super\cf5\f6
\fs23 \ul0\nosupersub\cf3\f4\fs24 C/min y de \up0 \expndtw0\charscalex102 10\ul0\
super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C/min para el enfriamiento, determi
nando las \par\pard\qj \li1418\ri1221\sb17\sl-400\slmult0 \up0 \expndtw-2\charsc
alex100 variaciones de entalpia con la temperatura. Se utilizaron muestras en po
lvo (5-10 mg) depositadas en \up0 \expndtw-3\charscalex100 cpsulas de aluminio. \
par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \p
ar\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par
\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb211\sl-230\slmult0 \up0
\expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 42

}
g11}{\bkmkend Pg11}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\s
b0\sl-230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charsc
alex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\ql \li1418\sb0\
sl-276\slmult0 \par\pard\ql\li1418\sb216\sl-276\slmult0 \up0 \expndtw-3\charscal
ex100 \ul0\nosupersub\cf3\f4\fs24 3.3.4.2. ANLISIS TERMOGRAVIMTRICO (TGA) \par\par
d\qj \li1418\sb0\sl-412\slmult0 \par\pard\qj\li1418\ri1217\sb20\sl-412\slmult0 \
up0 \expndtw0\charscalex105 En esta tcnica se detectan los cambios de peso que ti
enen lugar en una muestra sometida a un \up0 \expndtw0\charscalex100 determinado
tratamiento trmico. Los experimentos pueden realizarse midiendo el cambio de pes
o de \up0 \expndtw-2\charscalex100 la muestra al variar la temperatura a una vel
ocidad constante, o bien, variando el tiempo y manteniendo \up0 \expndtw0\charsc
alex100 constante la temperatura. El anlisis resultante se denomina, respectivame
nte, dinmico e isotrmico. \up0 \expndtw0\charscalex108 Tambin es posible medir el g
radiente de la variacin del peso con la temperatura o el tiempo, \up0 \expndtw-3\
charscalex100 constituyendo el anlisis trmico diferencial (DTA). \par\pard\qj \li1
418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri1220\sb20\sl-410\slmult0 \up0 \expn
dtw0\charscalex105 El anlisis de TGA representa una forma fcil y rpida de anlisis de
la estabilidad trmica de los \up0 \expndtw0\charscalex100 polmeros y puede ser ut
ilizada como medida de las posibilidades de transformacin por encima de la \up0 \
expndtw-3\charscalex100 temperatura de fusin del polmero. \par\pard\qj \li1418\ri1
220\sb408\sl-413\slmult0 \up0 \expndtw0\charscalex106 Las termogravimetras se reg
istraron con una termobalanza Perkin-Elmer TGA 6, acoplada a un \up0 \expndtw0\c
harscalex106 sistema de control por microprocesador y una estacin de procesamient
o de datos. Se oper en \up0 \expndtw0\charscalex100 rgimen dinmico a 10\ul0\super\c
f5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C/min, con muestras en polvo (10-20 mg) ba
jo atmsfera de nitrgeno y en el \up0 \expndtw-3\charscalex100 rango de 50-600\ul0\
super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C. \par\pard\ql \li1418\sb0\sl-276\
slmult0 \par\pard\ql\li1418\sb245\sl-276\slmult0 \up0 \expndtw-3\charscalex100 3
.3.4.3. ENSAYOS TERMODINAMOMECNICOS (DMTA) \par\pard\qj \li1418\sb0\sl-420\slmult
0 \par\pard\qj\li1418\ri1220\sb26\sl-420\slmult0 \up0 \expndtw-4\charscalex100 E
l anlisis trmico dinamomecnico suministra informacin cuantitativa de la variacin que
experimenta \line \up0 \expndtw-2\charscalex100 el mdulo durante las transiciones
termodinmicas o relajaciones del material, pudindose detectar la \line \up0 \expn
dtw-2\charscalex100 transicin \ul0\nosupersub\cf6\f7\fs24 \u945?\ul0\nosupersub\c
f3\f4\fs24 , asociada a segmentos de la cadena principal, y otras transiciones \
up0 \expndtw-3\charscalex100 (\ul0\nosupersub\cf6\f7\fs24 \u946?\ul0\nosupersub\
cf3\f4\fs24 , \ul0\nosupersub\cf6\f7\fs24 \u947?\ul0\nosupersub\cf3\f4\fs24 , et
c.), \par\pard\qj \li1418\ri1221\sb9\sl-410\slmult0 \up0 \expndtw0\charscalex100
correspondientes a movimientos moleculares locales. La tcnica es particularmente
adecuada para \up0 \expndtw0\charscalex105 estudiar la transicin vtrea pues suele
ser ms sensible que la calorimetra, especialmente con \up0 \expndtw-3\charscalex1
00 polmeros cristalinos. \par\pard\qj \li1418\sb0\sl-416\slmult0 \par\pard\qj\li1
418\ri1220\sb10\sl-416\slmult0 \up0 \expndtw-1\charscalex100 La aplicacin de una
tensin a un material viscoelstico se traduce en el almacenamiento de energa \up0 \e
xpndtw0\charscalex100 elstica y en una disipacin de energa en forma de calor. El co
mportamiento mecnico-dinmico se \up0 \expndtw0\charscalex108 evala en funcin de la t
emperatura. Para ello se aplica una tensin de forma cclica con una \up0 \expndtw0\
charscalex100 frecuencia angular (\ul0\nosupersub\cf6\f7\fs24 \u969?\ul0\nosuper
sub\cf3\f4\fs24 ), la deformacin causada por dicha tensin tambin vara de forma sinus
oidal \up0 \expndtw0\charscalex103 pero con un cierto retardo en la respuesta. E
l fenmeno se interpreta descomponiendo la tensin \up0 \expndtw-1\charscalex100 apl
icada en dos componentes, uno en fase con la deformacin y otro en desfase con res
pecto a ella. \up0 \expndtw-2\charscalex100 La expresin que corresponde a la defo
rmacin sinusoidal de la muestra es: \par\pard\ql \li10287\sb0\sl-230\slmult0 \par
\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb38\sl-230\slmult0 \up
0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 43
}
}}
}
alex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\ql \li5245\sb0\
sl-276\slmult0 \par\pard\ql\li5245\sb216\sl-276\slmult0 \up0 \expndtw-4\charscal
ex100 \ul0\nosupersub\cf6\f7\fs24 \u949?\ul0\nosupersub\cf3\f4\fs24 (t) = \ul0\n
osupersub\cf6\f7\fs24 \u949?\ul0\sub\cf5\f6\fs24 o\ul0\nosupersub\cf3\f4\fs24 s
en(\ul0\nosupersub\cf6\f7\fs24 \u969?\ul0\nosupersub\cf3\f4\fs24 t) \par\pard\qj
\li1418\ri1221\sb29\sl-440\slmult0 \up0 \expndtw-2\charscalex100 donde \ul0\nos
upersub\cf6\f7\fs24 \u949?\ul0\sub\cf5\f6\fs24 o\ul0\nosupersub\cf3\f4\fs24 es
la deformacin mxima aplicada, \ul0\nosupersub\cf6\f7\fs24 \u969?\ul0\nosupersub\cf
3\f4\fs24 es la frecuencia angular y t es el tiempo. La ecuacin \up0 \expndtw-5\
charscalex100 correspondiente a la tensin (\ul0\nosupersub\cf6\f7\fs24 \u963?\ul0
\nosupersub\cf3\f4\fs24 ) producida por el material es: \par\pard\ql \li5033\sb1
56\sl-276\slmult0 \up0 \expndtw-3\charscalex100 \ul0\nosupersub\cf6\f7\fs24 \u96
3?\ul0\nosupersub\cf3\f4\fs24 (t) = \ul0\nosupersub\cf6\f7\fs24 \u963?\ul0\sub\c
f5\f6\fs24 o\ul0\nosupersub\cf3\f4\fs24 sen(\ul0\nosupersub\cf6\f7\fs24 \u969?\
ul0\nosupersub\cf3\f4\fs24 t + \ul0\nosupersub\cf6\f7\fs24 \u948?\ul0\nosupersub
\cf3\f4\fs24 ) \par\pard\ql \li1418\ri1177\sb29\sl-440\slmult0\tx5112 \up0 \expn
dtw0\charscalex100 donde \ul0\nosupersub\cf6\f7\fs24 \u963?\ul0\sub\cf5\f6\fs24
o\ul0\nosupersub\cf3\f4\fs24 es la tensin mxima y \ul0\nosupersub\cf6\f7\fs24 \u9
48?\ul0\nosupersub\cf3\f4\fs24 es la diferencia de fase entre la deformacin apli
cada y la tensin \up0 \expndtw-3\charscalex100 producida. Las propiedades dinamom
ecnicas se describen mediante el mdulo complejo (E\ul0\super\cf10\f11\fs23 \u8727?
\ul0\nosupersub\cf3\f4\fs24 ): \line \tab \up0 \expndtw-4\charscalex100 E\ul0\no
supersub\cf10\f11\fs16 \u8727?\ul0\nosupersub\cf3\f4\fs24 = \ul0\nosupersub\cf6
\f7\fs24 \u963?\ul0\nosupersub\cf3\f4\fs24 /\ul0\nosupersub\cf6\f7\fs24 \u949?\u
l0\nosupersub\cf3\f4\fs24 = E\u8217? + i E\u8217?\u8217? \par\pard\qj \li1418\r
i1221\sb0\sl-420\slmult0 \up0 \expndtw-1\charscalex100 donde E\u8217? es el deno
minado mdulo de almacenamiento, que es una medida de la energa que puede \up0 \exp
ndtw-3\charscalex100 recuperarse de la deformacin producida en el material y E\u8
217?\u8217? es el mdulo de prdidas que se relaciona \up0 \expndtw-3\charscalex100
con la energa disipada por el material viscoelstico y que no puede recuperarse. La

diferencia de fase \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf6\f7\fs24 \u9
48?\ul0\nosupersub\cf3\f4\fs24 , que es la que determina la evolucin de calor en
un material viscoelstico sometido a una tensin \up0 \expndtw-3\charscalex100 cclica
, queda determinada por la relacin entre estos dos componentes, mediante la llama
da tangente \up0 \expndtw-4\charscalex100 de prdidas o factor de disipacin (tan \u
l0\nosupersub\cf6\f7\fs24 \u948?\ul0\nosupersub\cf3\f4\fs24 ). \par\pard\ql \li5
392\sb136\sl-276\slmult0 \up0 \expndtw-3\charscalex100 tan \ul0\nosupersub\cf6\f
7\fs24 \u948?\ul0\nosupersub\cf3\f4\fs24 = E\u8217?\u8217?/E\u8217? \par\pard\q
j \li1418\ri1222\sb54\sl-410\slmult0 \up0 \expndtw0\charscalex100 El anlisis DMTA
se llev a cabo en un analizador Rheometrics PL-DMT MK3 con una frecuencia de \up
0 \expndtw-1\charscalex100 1 Hz. Las probetas utilizadas fueron de 25 x 10 mm\ul
0\super\cf5\f6\fs23 2\ul0\nosupersub\cf3\f4\fs24 de tamao y 0.4 mm de espesor. E
l calentamiento \up0 \expndtw-1\charscalex100 se efectu en atmsfera de nitrgeno a 2
\ul0\super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C/min en un intervalo de -150
a 150\ul0\super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C. \par\pard\ql \li1418\s
b0\sl-276\slmult0 \par\pard\ql\li1418\sb245\sl-276\slmult0 \up0 \expndtw0\charsc
alex104 3.3.5. Solubilidad \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\
li1418\ri1220\sb38\sl-413\slmult0 \up0 \expndtw0\charscalex108 La disolucin de un
polmero es un proceso lento que ocurre en dos etapas. En la primera, las \line \
up0 \expndtw0\charscalex100 molculas de disolvente se difunden lentamente dentro
del polmero produciendo el hinchamiento del \line \up0 \expndtw0\charscalex108 mi
smo. El proceso de disolucin puede detenerse en esta fase, si las fuerzas intermo
leculares \line \up0 \expndtw-3\charscalex100 polmero-polmero \up0 \expndtw0\chars
calex108 (reticulacin, cristalinidad o enlaces por puentes de hidrgeno) so
n lo \par\pard\qj \li1418\ri1221\sb0\sl-415\slmult0 \up0 \expndtw0\charscalex10
0 suficientemente grandes como para impedirlo. En caso de que estas fuerzas pued
an superarse por la \line \up0 \expndtw0\charscalex110 formacin de interacciones
intensas polmero-disolvente, tendr lugar la segunda etapa de la \line \up0 \expndt
w-1\charscalex100 disolucin. En sta, el polmero hinchado se desintegra gradualmente
convirtindose en una verdadera \line \up0 \expndtw-2\charscalex100 disolucin. El
proceso de disolucin puede ser bastante lento (das o semanas) para materiales de m
uy \line \up0 \expndtw-3\charscalex100 alto peso molecular. \par\pard\qj \li1418
\ri1221\sb387\sl-420\slmult0 \up0 \expndtw0\charscalex112 La temperatura es un f
actor importante que debe ser controlado durante el experimento. La \line \up0 \
expndtw-1\charscalex100 polidispersidad es una caracterstica de los polmeros que d
ificulta sus pruebas de solubilidad debido a \line \up0 \expndtw-1\charscalex100
la coexistencia de molculas de bajo peso molecular; ms fcilmente solubles, y de al
to peso \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\s
lmult0 \par\pard\ql\li1418\sb217\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \u
l0\nosupersub\cf1\f2\fs20 44 \par\pard\sect\sectd\fs24\paperw11900\paperh16840\p
ard\sb0\sl-240{\bkmkstart Pg13}{\bkmkend Pg13}\par\pard\ql \li8764\sb0\sl-230\sl
mult0 \par\pard\ql\li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slm
ult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodo
s \par\pard\qj \li1418\ri1220\sb390\sl-400\slmult0 \up0 \expndtw0\charscalex100
\ul0\nosupersub\cf3\f4\fs24 molecular; que se disuelven con mayor dificultad. Po
r esta razn, en un polmero pueden darse varios \up0 \expndtw-3\charscalex100 casos
de solubilidad: \par\pard\ql \li2126\sb123\sl-276\slmult0 \up0 \expndtw-3\chars
calex100 Insolubilidad total en el disolvente. \par\pard\qj \li2127\ri1220\sb34\
sl-410\slmult0 \up0 \expndtw0\charscalex105 Insolubilidad parcial: cuando tiene
lugar la solubilizacin de las molculas de menor peso \up0 \expndtw0\charscalex102
molecular o cuando se produce un hinchamiento del polmero al penetrar el disolven
te en el \up0 \expndtw-3\charscalex100 material sin llegar a disolverlo. \par\pa
rd\qj \li2127\ri1221\sb10\sl-410\slmult0 \up0 \expndtw-1\charscalex100 Solubilid
ad parcial: en este caso las molculas de menor peso molecular pueden disolverse e
n \up0 \expndtw0\charscalex102 fro y las de mayor peso molecular al calentar la p
reparacin. Estas, sin embargo, vuelven a \up0 \expndtw-3\charscalex100 precipitar
al enfriar. \par\pard\ql \li2126\sb121\sl-276\slmult0 \up0 \expndtw-3\charscale
x100 Solubilidad total en el disolvente. \par\pard\qj \li1418\sb0\sl-413\slmult0
\par\pard\qj\li1418\ri1221\sb18\sl-413\slmult0 \up0 \expndtw0\charscalex102 Los
ensayos de solubilidad consisten en depositar una pequea cantidad del polmero (1

mg) en un \up0 \expndtw-1\charscalex100 tubo de ensayo al que se aade alrededor d
e 0.5 mL de disolvente. Tras la agitacin de la preparacin \up0 \expndtw0\charscale
x100 se observa si se produce algn cambio en el ndice de refraccin del lquido, indic
ativo del proceso de \up0 \expndtw0\charscalex111 disolucin. Por el contrario, si
no se detecta ningn cambio, se dice que no hay disolucin a \up0 \expndtw0\charsca
lex100 temperatura ambiente. Cuando se observa una variacin en el aspecto del polm
ero se considera que \up0 \expndtw-1\charscalex100 se ha disuelto parcialmente.
En aquellos tubos donde no se ha apreciado disolucin se calientan como \up0 \expn
dtw-2\charscalex100 mximo a la temperatura del disolvente y se observan los cambi
os en la solucin. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb0
\sl-276\slmult0 \par\pard\ql\li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb113
\sl-276\slmult0 \up0 \expndtw-2\charscalex100 3.4. CARACTERIZACIN ESTRUCTURAL \pa
r\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb268\sl-276\slmult0 \u
p0 \expndtw-2\charscalex100 3.4.1. MICROSCOPA ELECTRNICA \par\pard\qj \li1418\sb0\
rscalex100 En la ciencia de los polmeros generalmente el trmino morfologa se refier
e a la organizacin y forma \line \up0 \expndtw-1\charscalex100 superior al orden
atomstico y el trmino estructura se refiere a los detalles de la disposicin atomstic
a \line \up0 \expndtw0\charscalex105 y molecular. La microscopa electrnica de tran
smisin (TEM) es capaz de resolver estructuras a \line \up0 \expndtw-1\charscalex1
00 nivel atomstico y molecular y presenta un importante papel con respecto al anli
sis morfolgico de los \line \up0 \expndtw-2\charscalex100 polmeros. Su principal l
imitacin es el efecto destructivo que ejercen los electrones sobre los polmeros \l
ine \up0 \expndtw0\charscalex105 y las muestras orgnicas en general. Aunque morfo
lgicamente la muestra parezca inalterada, el \line \up0 \expndtw-2\charscalex100
deterioro de la estructura cristalina se manifiesta con la extincin progresiva de
l diagrama de difraccin. \line \up0 \expndtw0\charscalex106 No slo se destruyen la
s interacciones moleculares de tipo secundario, sino tambin los propios \line \up
0 \expndtw0\charscalex107 enlaces covalentes. El control riguroso de la dosis de
radiacin y el uso de sistemas de registro \line \up0 \expndtw-2\charscalex100 ex
traordinariamente sensibles hace posible obtener los mejores diagramas de difrac
cin de electrones. \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\
sb0\sl-230\slmult0 \par\pard\ql\li10287\sb99\sl-230\slmult0 \up0 \expndtw-2\char
scalex100 \ul0\nosupersub\cf1\f2\fs20 45 \par\pard\sect\sectd\fs24\paperw11900\p
aperh16840\pard\sb0\sl-240{\bkmkstart Pg14}{\bkmkend Pg14}\par\pard\ql \li1418\s
b0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb1
0\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Mater
iales y mtodos \par\pard\qj \li1418\sb0\sl-420\slmult0 \par\pard\qj\li1418\ri1221
\sb354\sl-420\slmult0 \up0 \expndtw0\charscalex105 \ul0\nosupersub\cf3\f4\fs24 E
l fundamento de la microscopa electrnica es esencialmente el mismo que el de la mi
croscopa \line \up0 \expndtw0\charscalex102 ptica, siendo la naturaleza de la radi
acin empleada en cada caso la principal diferencia entre ellas \line \up0 \expndt
w-3\charscalex100 (Tabla 3). \par\pard\ql \li3075\sb0\sl-276\slmult0 \par\pard\q
l\li3075\sb243\sl-276\slmult0 \up0 \expndtw-2\charscalex100 TABLA 3. Diferencias
entre la microscopa ptica y la electrnica. \par\pard\li2693\sb176\sl-276\slmult0\f
i0\tx5143\tx7034 \up0 \expndtw-1\charscalex100 Caracterstica\tab \up0 \expndtw-1\
charscalex100 Microscopa\tab \up0 \expndtw-1\charscalex100 Microscopa\par\pard\li2
693\sb0\sl-274\slmult0\fi2449\tx7034 \up0 \expndtw-1\charscalex100 ptica\tab \up0
\expndtw-1\charscalex100 electrnica\par\pard\li2693\sb16\sl-276\slmult0\fi0\tx51
43\tx7034 \up0 \expndtw-1\charscalex100 Tipo de radiacin\tab \up0 \expndtw-1\char
scalex100 UV o visible\tab \up0 \expndtw-1\charscalex100 Haz electrnico\par\pard\
li2693\sb137\sl-276\slmult0\fi0\tx5143\tx7034 \up0 \expndtw-1\charscalex100 Reso
lucin\tab \up0 \expndtw-1\charscalex100 300 nm\tab \up0 \expndtw-1\charscalex100
0.2 nm\par\pard\li2693\sb136\sl-276\slmult0\fi0\tx5143\tx7034 \up0 \expndtw-1\ch
arscalex100 Rango de aumentos\tab \up0 \expndtw-1\charscalex100 2 - 2000\tab \up
0 \expndtw-1\charscalex100 200 - 2 x 10\ul0\super\cf5\f6\fs23 6\par\pard\li2693\
sb138\sl-276\slmult0\fi0\tx5143\tx7034 \up0 \expndtw-1\charscalex100 \ul0\nosupe
rsub\cf3\f4\fs24 Entorno\tab \up0 \expndtw-1\charscalex100 Ambiente\tab \up0 \ex
pndtw-1\charscalex100 Alto vaco\par\pard\li2693\sb137\sl-276\slmult0\fi0\tx5143\t
x7034 \up0 \expndtw-1\charscalex100 Destructiva\tab \up0 \expndtw-1\charscalex10

0 No\tab \up0 \expndtw-1\charscalex100 Si\par\pard\li2693\sb137\sl-276\slmult0\f
i0\tx7034 \up0 \expndtw-1\charscalex100 Preparacin de muestras Fcil\tab \up0 \exp
ndtw-1\charscalex100 Difcil\par\pard\li2693\sb137\sl-276\slmult0\fi0\tx5143\tx703
4 \up0 \expndtw-1\charscalex100 Observacin\tab \up0 \expndtw-1\charscalex100 Supe
rfcies\tab \up0 \expndtw-1\charscalex100 Pelculas\par\pard\li2693\sb136\sl-276\slm
ult0\fi0\tx5143\tx7034 \up0 \expndtw-1\charscalex100 Detecta orientacin\tab \up0
\expndtw-1\charscalex100 Si\tab \up0 \expndtw-1\charscalex100 Si\par\pard\qj \li
1418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri1221\sb57\sl-410\slmult0 \up0 \exp
ndtw0\charscalex100 La TEM se ocupa de la informacin suministrada por los electro
nes que traspasan una muestra slida \up0 \expndtw0\charscalex100 sobre la que se
ha hecho incidir un haz electrnico coherente y a gran velocidad. La interaccin de
los \up0 \expndtw-3\charscalex100 electrones con la materia es un fenmeno complej
o. \par\pard\qj \li1418\ri1221\sb407\sl-414\slmult0 \up0 \expndtw0\charscalex100
Cuando hacemos incidir un haz electrnico sobre una muestra los electrones pueden
no desviarse de \line \up0 \expndtw0\charscalex100 la trayectoria inicial, o se
r desviados elstica o inelsticamente dependiendo, respectivamente, de que \line \u
p0 \expndtw0\charscalex103 la interaccin sea con el ncleo o con algn orbital electrn
ico de alguno de los tomos que forman \line \up0 \expndtw0\charscalex107 parte de
l material. Los electrones desviados de forma inelstica experimentan un cambio en
su \line \up0 \expndtw0\charscalex103 velocidad como consecuencia de la energa p
erdida en la colisin con la muestra, mientras que los \line \up0 \expndtw0\charsc
alex105 desviados de forma elstica mantienen su velocidad y son los responsables
de los fenmenos de \line \up0 \expndtw0\charscalex100 difraccin. Los electrones no
desviados y los desviados elsticamente son los nicos que contribuyen \line \up0 \
expndtw0\charscalex100 de forma constructiva a la formacin de la imagen, mientras
que los desviados de forma inelstica son \line \up0 \expndtw-2\charscalex100 los
responsables del ruido de fondo presente en toda imagen de microscopa electrnica.
La proporcin \line \up0 \expndtw0\charscalex100 de electrones dispersados de for
ma elstica es directamente proporcional al grosor de la muestra. Por \line \up0 \
expndtw0\charscalex100 esta razn, los experimentos de difraccin se realizan a un v
oltaje mayor (100 kV) que los de anlisis \line \up0 \expndtw-3\charscalex100 morf
olgico (80 kV). \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\s
l-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb8\sl-23
0\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 46
}
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}
}}
}
alex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri12
20\sb380\sl-412\slmult0 \up0 \expndtw0\charscalex108 \ul0\nosupersub\cf3\f4\fs24
El microscpio electrnico de transmisin consta de un sistema de iluminacin formado p
or un \line \up0 \expndtw0\charscalex108 filamento de tungsteno o wolframio que
emite electrones, que sern acelerados por la elevada \line \up0 \expndtw0\charsca
lex102 diferencia de potencial a que son sometidos (80-100 kV). El haz de electr
ones es enfocado hacia la \line \up0 \expndtw0\charscalex100 muestra mediante do
s lentes condensadoras, la primera recoge la imagen del filamento y la segunda \
line \up0 \expndtw0\charscalex109 controla el rea de iluminacin. El vaco existente
en la columna permite la transmisin de los \line \up0 \expndtw-1\charscalex100 el
ectrones, a travs de ella, hacia la muestra. A continuacin, se encuentra la lente
objetivo que amplia \line \up0 \expndtw0\charscalex103 la imagen y finalmente la
lente proyectora que la dirige hacia la pantalla fluorescente que recoge la \li
ne \up0 \expndtw0\charscalex103 imagen final. Todas las lentes son de naturaleza
electromagntica y su potencia se puede controlar \line \up0 \expndtw-3\charscale
x100 variando el voltaje. \par\pard\qj \li1418\ri1221\sb402\sl-420\slmult0 \up0
\expndtw-1\charscalex100 La resolucin es una ventaja importante de sta tcnica frent
e a la de difraccin de rayos X y depende \up0 \expndtw-3\charscalex100 de la long
itud de onda del haz de electrones segn la ecuacin: \par\pard\ql \li5307\sb0\sl-27
d = \ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosupersub\cf3\f4\fs24 / n sen \ul0
\nosupersub\cf6\f7\fs24 \u952? \par\pard\qj \li1418\sb0\sl-420\slmult0 \par\pard
\qj\li1418\ri1220\sb46\sl-420\slmult0 \up0 \expndtw0\charscalex104 \ul0\nosupers
ub\cf3\f4\fs24 siendo d la resolucin, \ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosu
persub\cf3\f4\fs24 la longitud de onda, n el ndice de refraccin del medio y \ul0\
nosupersub\cf6\f7\fs24 \u952?\ul0\nosupersub\cf3\f4\fs24 el ngulo de \up0 \expnd
tw-3\charscalex100 apertura de las lentes de microscopio. \par\pard\qj \li1418\r
i1222\sb384\sl-440\slmult0 \up0 \expndtw0\charscalex103 Las modificaciones en el
voltaje (V) modifican la longitud de onda del haz de electrones segn la \line \u
p0 \expndtw0\charscalex100 frmula \ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosupers
ub\cf3\f4\fs24 = (1.5/V)\ul0\super\cf5\f6\fs23 1/2\ul0\nosupersub\cf3\f4\fs24 .
As, para voltajes de 80 y 100 kV las longitudes de onda de los electrones son \p
ar\pard\qj \li1418\ri1222\sb4\sl-412\slmult0 \up0 \expndtw-1\charscalex100 0.041
756 y 0.037013 , respectivamente.\ul0\super\cf5\f6\fs23 84\ul0\nosupersub\cf3\f4\
fs24 La mxima resolucin se obtiene con longitudes de onda \up0 \expndtw0\charscal
ex100 ms cortas, es decir, diferencias de potencial ms elevadas y lentes de gran a
pertura. Generalmente, \up0 \expndtw0\charscalex100 para una substancia estable
en un microscopio operando correctamente, la resolucin prctica viene \up0 \expndtw
0\charscalex100 determinada por la aberracin cromtica debida a la presencia de ele
ctrones inelsticos. Dado que su \up0 \expndtw0\charscalex100 proporcin aumenta de
forma exponencial con la cantidad de materia con la que colisiona, el espesor \u
p0 \expndtw-3\charscalex100 de la muestra es decisivo para obtener buenas imgenes
. \par\pard\qj \li1418\ri1222\sb408\sl-413\slmult0 \up0 \expndtw0\charscalex108
La preparacin de las muestras para microscopa electrnica de transmisin se efectu con
un \line \up0 \expndtw-2\charscalex100 evaporador de alto vaco Balzers BAE 080T.
Los cristales se observaron con Microscpios Electrnicos \line \up0 \expndtw0\chars
calex103 Philips EM301 y Philips Tecnai 10/12. El calibrado de los diagramas de

difraccin de electrones se \line \up0 \expndtw-2\charscalex100 realiz con oro (d\u
l0\sub\cf5\f6\fs24 111\ul0\nosupersub\cf3\f4\fs24 = 2.35 \ul0\nosupersub\cf4\f5
\fs24 \ul0\nosupersub\cf3\f4\fs24 ) y la rotacin de la imagen se determin mediante
cristales de MoO\ul0\sub\cf5\f6\fs24 3\ul0\nosupersub\cf3\f4\fs24 . \par\pard\qj
\li1418\sb0\sl-400\slmult0 \par\pard\qj\li1418\ri1222\sb38\sl-400\slmult0 \up0
\expndtw0\charscalex109 La caracterizacin por microscopa electrnica de barrido (SEM
) de los materiales polimricos \line \up0 \expndtw-1\charscalex100 comprende una
serie de aplicaciones que difieren en su estructura y micromorfologa. En cada cas
o la \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\sl
mult0 \par\pard\ql\li10287\sb21\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul
0\nosupersub\cf1\f2\fs20 47 \par\pard\sect\sectd\fs24\paperw11900\paperh16840\pa
rd\sb0\sl-240{\bkmkstart Pg16}{\bkmkend Pg16}\par\pard\ql \li1418\sb0\sl-230\slm
ult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmu
lt0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos
\par\pard\qj \li1418\ri1221\sb390\sl-400\slmult0 \up0 \expndtw0\charscalex108 \
ul0\nosupersub\cf3\f4\fs24 estrategia de la exploracin es distinta dependiendo de
la naturaleza de cada material y de las \up0 \expndtw-3\charscalex100 posibilid
ades que se tienen para la preparacin de las muestras. \par\pard\qj \li1418\sb0\s
l-410\slmult0 \par\pard\qj\li1418\ri1221\sb22\sl-410\slmult0 \up0 \expndtw0\char
scalex100 El microscopio electrnico de barrido forma la imagen con los electrones
secundarios que se generan \up0 \expndtw0\charscalex100 en la interaccin de la r
adiacin electrnica con una capa superficial y fina de la muestra mediante un \up0
\expndtw-3\charscalex100 proceso de rastreo. \par\pard\qj \li1418\ri1221\sb409\s
l-412\slmult0 \up0 \expndtw0\charscalex109 Una analoga simple que describe perfec
tamente el mecanismo de operacin del microscopio \line \up0 \expndtw0\charscalex1
02 electrnico de barrido es una habitacin completamente oscura en donde se sita un
exposmetro y \line \up0 \expndtw-1\charscalex100 una luz flash que va iluminando
las paredes de manera continuada y sistemtica. El exposmetro mide \line \up0 \expn
dtw0\charscalex106 la luz reflejada sealando mximos para las zonas blancas y lisas
, y mnimos para las oscuras y \line \up0 \expndtw0\charscalex103 rugosas. El regi
stro del exposmetro para toda la habitacin proporciona el mapa de la pared. En el
\line \up0 \expndtw0\charscalex108 caso de una muestra observada con SEM las reas
oscuras corresponden a las zonas de baja \line \up0 \expndtw0\charscalex104 ref
lectividad y las rugosas a los relieves superficiales. Podemos tener un contrast
e composicional, \line \up0 \expndtw0\charscalex100 dependiendo de la composicin
qumica de la muestra, o un contraste topogrfico, dependiendo de la \line \up0 \exp
ndtw-3\charscalex100 morfologa superficial de la muestra. \par\pard\qj \li1418\sb
0\sl-413\slmult0 \par\pard\qj\li1418\ri1220\sb15\sl-413\slmult0 \up0 \expndtw-1\
charscalex100 La resolucin espacial de una observacin por SEM viene dada por el rea
de la muestra reflectante, y \line \up0 \expndtw0\charscalex102 depende del gra
do de interaccin de la radiacin con la muestra. Esta interaccin genera electrones \
line \up0 \expndtw-3\charscalex100 reflejados \up0 \expndtw0\charscalex112 (secu
ndarios o elsticos) que son atrados por un detector para dar las imgenes \line \up0
\expndtw-3\charscalex100 topogrficas. \par\pard\qj \li1418\ri1220\sb408\sl-412\s
lmult0 \up0 \expndtw0\charscalex100 La simplicidad en la preparacin de muestras p
ara SEM es quizs la principal ventaja que ofrece esta \line \up0 \expndtw0\charsc
alex100 tcnica. El hecho de que la observacin de la muestra se haga punto a punto,
permite la utilizacin de \line \up0 \expndtw0\charscalex104 muestras de cualquie
r tamao y forma, y da lugar a una gran profundidad de campo. De hecho, la \line \
up0 \expndtw-1\charscalex100 preparacin de muestras finas para microscopa ptica (0.
1-0.3 mm) o hiperfinas para TEM (5-100 nm) \line \up0 \expndtw0\charscalex106 co
nstituye la mayor limitacin prctica en el anlisis microscpico de muestras de polmeros
por \line \up0 \expndtw-3\charscalex100 transmisin. \par\pard\qj \li1418\sb0\sl413\slmult0 \par\pard\qj\li1418\ri1220\sb15\sl-413\slmult0 \up0 \expndtw0\charsc
alex100 En la SEM el metalizado de las muestras polimricas es indispensable y su
funcin, adems de hacer \up0 \expndtw-1\charscalex100 conductiva la superficie, es
eliminar la electricidad esttica, minimizar el dao por radiacin y aumentar \up0 \ex
pndtw0\charscalex106 la reflectividad electrnica. Normalmente, el metal utilizado
suele ser el oro en presencia de una \up0 \expndtw-3\charscalex100 atmsfera ioni
zante de argon. \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\

sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl
-230\slmult0 \par\pard\ql\li1418\sb39\sl-230\slmult0 \up0 \expndtw-2\charscalex1
00 \ul0\nosupersub\cf1\f2\fs20 48 \par\pard\sect\sectd\fs24\paperw11900\paperh16
840{\shp
{\*\shpinst\shpleft0\shptop0\shpright11900\shpbottom16840\shpwr3\shpfblwtxt0\shp
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40051451400514514005145140051451401fffd9}}}}}\pard\sb0\sl-240{\bkmkstart Pg17}{\
bkmkend Pg17}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex10
0 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri1221\sb3
82\sl-410\slmult0 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf3\f4\fs24 La mo
rfologa de la superficie de las pelculas de polmero sometidas a un proceso de degra
dacin se \up0 \expndtw0\charscalex100 observ con un Microscopio Electrnico de Barri
do JEOL JSM-6400. Los films fueron metalizados con \up0 \expndtw-3\charscalex100
oro usando un evaporador Balzers SCD-004 Sputter Coater. \par\pard\ql \li1418\s
alex104 3.4.1.1. Morfologa cristalina \par\pard\qj \li1418\sb0\sl-413\slmult0 \pa
r\pard\qj\li1418\ri1219\sb38\sl-413\slmult0 \up0 \expndtw0\charscalex102 Los niv
eles de organizacin supramolecular de un polmero cristalino se identifican con dos
tipos de \up0 \expndtw0\charscalex111 morfologias: las lamelas y las esferulita
s. As pues, un fenmeno peculiar en la organizacin \up0 \expndtw0\charscalex100 mole
cular de los polmeros cristalinos es el plegamiento molecular con la consiguiente
formacin de la \up0 \expndtw0\charscalex102 estructura lamelar (Figura 24). Las
lamelas son microcristales de espesor muy pequeo (< 25 nm) y \up0 \expndtw-2\char
scalex100 dimensiones basales que pueden llegar a ser de decenas de micrmetros. E
n estos cristales, la cadena \up0 \expndtw-2\charscalex100 molecular se dispone
mas o menos perpendicularmente a las bases y se pliega sobre si misma con una \u
p0 \expndtw-3\charscalex100 cierta periodicidad que determina el grosor de los m
ismos. \par\pard\qj \li3743\sb0\sl-240\slmult0 \par\pard\qj\li3743\sb0\sl-240\sl
mult0 \par\pard\qj\li3743\sb0\sl-240\slmult0 \par\pard\qj\li3743\sb0\sl-240\slmu
lt0 \par\pard\qj\li3743\sb0\sl-240\slmult0 \par\pard\qj\li3743\sb0\sl-240\slmult
0 \par\pard\qj\li3743\sb0\sl-240\slmult0 \par\pard\qj\li3743\sb0\sl-240\slmult0
\par\pard\qj\li3743\sb0\sl-240\slmult0 \par\pard\qj\li3743\sb0\sl-240\slmult0 \p
ar\pard\qj\li3743\sb0\sl-240\slmult0 \par\pard\qj\li3743\ri3524\sb90\sl-240\slmu
lt0 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf9\f10\fs20 Figura 24. Modelo
de la formacin de lamelas cristalinas en \line \up0 \expndtw-3\charscalex100 polme
ros con una nica direccin de puentes de hidrgeno. \par\pard\qj \li1418\sb0\sl-420\s
lmult0 \par\pard\qj\li1418\ri1221\sb112\sl-420\slmult0 \up0 \expndtw-2\charscale
x100 \ul0\nosupersub\cf3\f4\fs24 Mediante cristalizacin en disoluciones diluidas
es posible obtener estos microcristales con hbitos bien \up0 \expndtw-2\charscale
x100 definidos que suelen revelar la geometra de la celdilla cristalina (Figura 2
5). \par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par\p
ard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167
\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-23
0\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\
par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par\pard\l
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\cf9\f10\fs20 C.\par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\s
lmult0\par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par
\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par\pard\li31
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28a00fffd9}}}}}\pard\sb0\sl-240{\bkmkstart Pg18}{\bkmkend Pg18}\par\pard\ql \li1
Materiales y mtodos \par\pard\qj \li1418\ri1219\sb377\sl-416\slmult0 \up0 \expndt
w0\charscalex100 \ul0\nosupersub\cf3\f4\fs24 Los monocristales de polmero suelen
tener un grosor adecuado (< 100 \ul0\nosupersub\cf4\f5\fs24 \ul0\nosupersub\cf3\f
4\fs24 ) para su estudio por sta \line \up0 \expndtw0\charscalex110 tcnica, pero p
resentan una imagen de bajo contraste, porque ste suele ser inversamente \line \u
p0 \expndtw-2\charscalex100 proporcional al peso atmico de la muestra. Este incon
veniente se soluciona sombreando los cristales \line \up0 \expndtw0\charscalex10
8 con una fina capa de un metal pesado (Cr, Pt, Pd, U, etc). El metal es evapora
do a alto vaco \line \up0 \expndtw0\charscalex102 (10\ul0\super\cf5\f6\fs23 -4\ul
0\nosupersub\cf3\f4\fs24 - 10\ul0\super\cf5\f6\fs23 -5\ul0\nosupersub\cf3\f4\fs
24 torr) sobre las rejillas a un cierto ngulo y se deposita sobre los cristales
resaltando las \line \up0 \expndtw-2\charscalex100 caractersticas topogrficas de l
a muestra. Conociendo el ngulo de sombreado y midiendo la longitud \line \up0 \ex
pndtw-2\charscalex100 de las sombras resultantes se puede conocer el grosor apro
ximado de las lamelas del cristal. En este \line \up0 \expndtw-2\charscalex100 t
rabajo, el sombreado se realiz con Pt-C con un ngulo de aproximadamente 15. En la F
igura 26 se \line \up0 \expndtw0\charscalex102 muestra esquemticamente el ngulo de
sombreado (\ul0\nosupersub\cf6\f7\fs24 \u945?\ul0\nosupersub\cf3\f4\fs24 ) y su
relacin con el grosor lamelar (a). La \line \up0 \expndtw-3\charscalex100 morfol
oga de los monocristales es un buen indicador, aunque no infalible, de la simetra
presente en la \line \up0 \expndtw-4\charscalex100 estructura cristalina. \par\p
ard\qj \li1418\ri1221\sb401\sl-420\slmult0 \up0 \expndtw0\charscalex103 En gener
al, las celdillas tetragonales proporcionan cristales de base cuadrada, las hexa
gonales y \line \up0 \expndtw-2\charscalex100 trigonales proporcionan cristales
de forma hexagonal y las rmbicas cristales con forma de rombo. \par\pard\ql \li33
\sb0\sl-230\slmult0 \par\pard\ql\li3312\sb0\sl-230\slmult0 \par\pard\ql\li3312\s
\sl-230\slmult0 \par\pard\ql\li3312\sb0\sl-230\slmult0 \par\pard\ql\li3312\sb0\s
0\slmult0 \par\pard\ql\li3312\sb0\sl-230\slmult0 \par\pard\ql\li3312\sb0\sl-230\
slmult0 \par\pard\ql\li3312\sb7\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul
0\nosupersub\cf9\f10\fs20 Figura 26. Esquema del sombreado para determinar el gr
osor lamelar. \par\pard\qj \li1418\sb0\sl-412\slmult0 \par\pard\qj\li1418\ri1221
\sb28\sl-412\slmult0 \up0 \expndtw0\charscalex102 \ul0\nosupersub\cf3\f4\fs24 La
esferulita consiste en un agregado esfrico con un tamao que puede oscilar entre dc
imas de \up0 \expndtw0\charscalex100 micrmetros y varios milmetros, y pueden ser o
bservadas claramente en el microscopio ptico. Una \up0 \expndtw-1\charscalex100 m
orfologa esferultica se obtiene por la cristalizacin del polmero a partir del estado
fundido o por la \up0 \expndtw0\charscalex108 cristalizacin del polmero a partir
de soluciones muy concentradas por evaporacin lenta del \up0 \expndtw0\charscalex
104 disolvente. En el microscopio ptico de luz polarizada son fcilmente reconocibl
es como crculos \up0 \expndtw-4\charscalex100 fuertemente birrefringentes que exh
iben una cruz de malta caracterstica (Figura 27). \par\pard\ql \li1418\sb0\sl-230
\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\s
lmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slm
ult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmul
t0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0
\par\pard\ql\li1418\sb109\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nos
upersub\cf1\f2\fs20 50 \par\pard\sect\sectd\fs24\paperw11900\paperh16840{\shp
z-10000\shplid18
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alex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li3456\sb0\
sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl
-220\slmult0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-2
20\slmult0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-220
\slmult0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-220\s
lmult0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-220\slm
ult0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-220\slmul
t0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-220\slmult0
\par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\ri3233\sb99\sl-220\s
lmult0 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf9\f10\fs20 Figura 27. Esfe
rulita simple presentando extincin en forma de cruz \line \up0 \expndtw-3\charsca
lex100 de malta observada en el microscopio ptico de luz polarizada. \par\pard\qj
\expndtw-2\charscalex100 \ul0\nosupersub\cf3\f4\fs24 Las esferulitas estn consti
tuidas internamente por lamelas que irradian del centro. En muchos casos la \up0
\expndtw0\charscalex103 lamela se retuerce sobre si misma, de forma que la orie
ntacin del eje molecular gira alrededor del \up0 \expndtw0\charscalex104 radio es
ferultico. Este fenmeno se refleja en la esferulita como una serie de bandas de ex
tincin \up0 \expndtw-1\charscalex100 concntricas que muestran una periodicidad dep
endiente de las condiciones en que ha cristalizado. La \up0 \expndtw0\charscalex
100 medida de la birrefringencia permite diferenciar dos tipos de esferulitas: l
as positivas y las negativas. \up0 \expndtw-2\charscalex100 De esta manera, si e
l ndice de refraccin en la direccin radial es mayor que en la direccin tangencial, \
up0 \expndtw-3\charscalex100 la esferulita es positiva, en caso contrario es neg
ativa. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb265\sl-276\
slmult0 \up0 \expndtw0\charscalex103 3.4.1.2. Difraccin de electrones \par\pard\q
j \li1418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri1220\sb24\sl-410\slmult0 \up0
\expndtw0\charscalex104 Los diagramas de difraccin de monocristales consisten en
retculos puntuales que representan la \up0 \expndtw0\charscalex105 proyeccin de l
a red cristalina sobre el plano perpendicular al haz electrnico. Suponiendo que l
a \up0 \expndtw-2\charscalex100 radiacin electrnica es paralela al eje cristalogrfi
co c las manchas de difraccin se indexan como hk0, \up0 \expndtw0\charscalex103 a
unque en ocasiones pueden observarse reflexiones hkl con l distinto de 0 debido
a una inclinacin \up0 \expndtw-2\charscalex100 parcial de los cristales o a una d
isposicin no ortogonal de la celdilla unitaria. \par\pard\qj \li1418\sb0\sl-410\s
lmult0 \par\pard\qj\li1418\ri1221\sb20\sl-410\slmult0 \up0 \expndtw0\charscalex1
09 El diagrama de difraccin de una muestra refleja su organizacin estructural a ni
vel atmico y \line \up0 \expndtw0\charscalex104 molecular. Para las muestras amor
fas consiste en un halo difuso que rodea a una mancha central \line \up0 \expndt
w0\charscalex100 correspondiente a la radiacin no desviada, mientras que para las

cristalinas se observan diagramas \line \up0 \expndtw0\charscalex103 con mximos
y mnimos, cuya disposicin en el espacio viene determinada por el tipo de estructur
a \line \up0 \expndtw-3\charscalex100 presente. \par\pard\ql \li10287\sb0\sl-230
\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230
\slmult0 \par\pard\ql\li10287\sb109\sl-230\slmult0 \up0 \expndtw-2\charscalex100
\ul0\nosupersub\cf1\f2\fs20 51 \par\pard\sect\sectd\fs24\paperw11900\paperh1684
0{\shp
z-10000\shplid19
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a28a2800a28a2800a28a2800a28a2800a28a2800a28a2803ffd9}}}}}\pard\sb0\sl-240{\bkmks
tart Pg20}{\bkmkend Pg20}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li
1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmult0 \up0 \expndtw-2\
charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li141
8\ri1219\sb369\sl-426\slmult0 \up0 \expndtw-3\charscalex100 \ul0\nosupersub\cf3\
f4\fs24 Las posiciones de las reflexiones definen los espaciados de los planos c
ristalogrficos, realizndose su \up0 \expndtw-1\charscalex100 determinacin segn la le
y de Bragg. Dado que los ngulos \ul0\nosupersub\cf6\f7\fs24 \u952?\ul0\nosupersub
\cf3\f4\fs24 con que son difractados los electrones \up0 \expndtw-2\charscalex1
00 son muy pequeos (1-2\ul0\super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 ) se pue
de admitir la aproximacin tan 2\ul0\nosupersub\cf6\f7\fs24 \u952?\ul0\nosupersub\
cf3\f4\fs24 = 2 sen\ul0\nosupersub\cf6\f7\fs24 \u952?\ul0\nosupersub\cf3\f4\fs2
4 y puede utilizarse la ley de \up0 \expndtw-3\charscalex100 Bragg simplificada
: \par\pard\ql \li5455\sb138\sl-276\slmult0 \up0 \expndtw-3\charscalex100 R d\ul
0\sub\cf5\f6\fs24 hkl\ul0\nosupersub\cf3\f4\fs24 = \ul0\nosupersub\cf6\f7\fs24
\u955?\ul0\nosupersub\cf3\f4\fs24 L \par\pard\qj \li1418\sb0\sl-420\slmult0 \pa
r\pard\qj\li1418\ri1221\sb26\sl-420\slmult0 \up0 \expndtw0\charscalex108 donde R
es la distancia de la mancha de difraccin al centro del diagrama, d\ul0\sub\cf5\
f6\fs24 hkl \ul0\nosupersub\cf3\f4\fs24 el espaciado \line \up0 \expndtw-3\cha
rscalex100 interplanar, L la longitud de cmara entre la muestra y la placa de reg
istro y \ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosupersub\cf3\f4\fs24 L la const
ante de cmara \line \up0 \expndtw-4\charscalex100 (Figura 28). \par\pard\ql \li30
slmult0 \par\pard\ql\li3023\sb147\sl-230\slmult0 \up0 \expndtw-3\charscalex100 \
ul0\nosupersub\cf9\f10\fs20 Figura 28. El microscopio electrnico considerado como
una cmara de difraccin. \par\pard\qj \li1418\ri1220\sb414\sl-420\slmult0 \up0 \ex
pndtw0\charscalex109 \ul0\nosupersub\cf3\f4\fs24 El anlisis de la difraccin de ele
ctrones requiere un calibrado previo del aparato para poder \up0 \expndtw0\chars
calex100 correlacionar las manchas de difraccin obtenidas en el diagrama con las
distancias reales de la red \up0 \expndtw-2\charscalex100 cristalina. Los valore
s de \ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosupersub\cf3\f4\fs24 y L pueden v
ariar de un registro a otro debido a inestabilidades del circuito \up0 \expndtw0
\charscalex104 elctrico, pequeos desajustes del alto voltaje utilizado o de la cor

riente en las lentes objetivas y \up0 \expndtw-1\charscalex100 proyectoras. Por
esta razn, se debe determinar de forma precisa la constante de cmara para cada \up
0 \expndtw-3\charscalex100 conjunto de lentes utilizadas. \par\pard\qj \li1418\r
i1220\sb406\sl-413\slmult0 \up0 \expndtw0\charscalex110 El calibrado de la const
ante de cmara se realiza evaporando una fina capa de un material \line \up0 \expn
dtw0\charscalex107 policristalino sobre las rejillas con la muestra problema. Su
bstancias cristalinas que presenten \line \up0 \expndtw-3\charscalex100 espaciad
os prximos a los del problema como (Au, Al, TlCl, etc.) son adecuadas como patron
es. En el \line \up0 \expndtw-3\charscalex100 campo de los polmeros se utiliza no
rmalmente oro (reflexiones caractersticas a 4.08, 2.35, 2.04, 1.44, \par\pard\qj
\li1418\ri1221\sb0\sl-420\slmult0 \up0 \expndtw0\charscalex100 1.23, 1.18 y 1.02
\ul0\nosupersub\cf4\f5\fs24 \ul0\nosupersub\cf3\f4\fs24 ) como substancia patrn p
ara calibrar la constante de cmara. Su evaporacin \up0 \expndtw-1\charscalex100 so
bre las rejillas se realiza a partir de 1 cm de un filamento de 0.25 mm de dimetr
o cuidadosamente \up0 \expndtw-4\charscalex100 enrollado alrededor de otro filam
ento (en este caso de tungsteno) en forma de V. \par\pard\ql \li1418\sb0\sl-230\
slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\sl
mult0 \par\pard\ql\li1418\sb9\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\
nosupersub\cf1\f2\fs20 52 \par\pard\sect\sectd\fs24\paperw11900\paperh16840{\shp
z-10000\shplid20
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ffd9}}}}}\pard\sb0\sl-240{\bkmkstart Pg21}{\bkmkend Pg21}\par\pard\ql \li8764\sb
0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb10
\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materi
ales y mtodos \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1220\
sb366\sl-413\slmult0 \up0 \expndtw0\charscalex105 \ul0\nosupersub\cf3\f4\fs24 Po
r ltimo, debe tenerse en cuenta que no es posible relacionar directamente una dir
eccin en el \up0 \expndtw0\charscalex103 diagrama de difraccin y la misma en la im
agen morfolgica porque existe una cierta rotacin entre \up0 \expndtw0\charscalex10
9 ambas imgenes (Figura 29). La rotacin del diagrama de difraccin con respecto al c
ristal se \up0 \expndtw0\charscalex109 determina experimentalmente, superponiend
o la imagen morfolgica de un cristal de xido de \up0 \expndtw0\charscalex100 molib
deno y su diagrama de difraccin de electrones en una misma placa de registro, de
forma que la \up0 \expndtw0\charscalex102 direccin de mayor crecimiento coincida
con el eje de la red recproca cuyo parmetro es menor. La \up0 \expndtw-3\charscale
x100 rotacin del diagrama debe calibrarse para cada constante de cmara. \par\pard\
li3871\sb0\sl-276\slmult0\par\pard\li3871\sb0\sl-276\slmult0\par\pard\li3871\sb0
\sl-276\slmult0\par\pard\li3871\sb0\sl-276\slmult0\par\pard\li3871\sb0\sl-276\sl
mult0\par\pard\li3871\sb0\sl-276\slmult0\par\pard\li3871\sb0\sl-276\slmult0\par\
pard\li3871\sb0\sl-276\slmult0\par\pard\li3871\sb0\sl-276\slmult0\par\pard\li387
1\sb0\sl-276\slmult0\par\pard\li3871\sb1\sl-276\slmult0\fi0\tx7630 \up0 \expndtw
0\charscalex100 a)\tab \up0 \expndtw0\charscalex100 b)\par\pard\ql \li2511\sb202
\sl-230\slmult0 \up0 \expndtw-1\charscalex100 \ul0\nosupersub\cf9\f10\fs20 Figur
a 29. Correlacin entre la imagen de difraccin y la morfolgica: a) incorrecta, b) co
rrecta. \par\pard\qj \li1418\ri1220\sb354\sl-420\slmult0 \up0 \expndtw0\charscal
ex106 \ul0\nosupersub\cf3\f4\fs24 Las tcnicas ms habituales para la preparacin de l
as muestras para su observacin mediante \up0 \expndtw-3\charscalex100 microscopa e
lectrnica de transmisin son: \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\
li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb97\sl-230\slmult0 \up0 \expndtw3\charscalex100 a) \ul0\nosupersub\cf9\f10\fs20 CRISTALIZACIN EN DISOLUCIN \par\pa
rd\qj \li1418\sb0\sl-412\slmult0 \par\pard\qj\li1418\ri1219\sb48\sl-412\slmult0
\up0 \expndtw0\charscalex102 \ul0\nosupersub\cf3\f4\fs24 Los monocristales se pr
eparan a partir de soluciones diluidas y estn generalmente constituidos por \line
\up0 \expndtw-2\charscalex100 pequeas lamelas de 50-100 de grosor. Su obtencin es
la fase de mayor dificultad en la preparacin \line \up0 \expndtw-2\charscalex100
de muestras para microscopa. La cristalizacin del polmero siempre se realiza a par
tir de disoluciones \line \up0 \expndtw0\charscalex106 muy diluidas (0.05-0.20 %
) en un disolvente a temperatura ambiente o elevada y bajo un estricto \line \up
0 \expndtw0\charscalex100 control de concentracin y temperatura. Los mtodos utiliz
ados habitualmente para obtener cristales \line \up0 \expndtw-2\charscalex100 co
n el grosor adecuado y estudiarlos por TEM son los que se describen a continuacin
. \par\pard\qj \li1418\ri1221\sb402\sl-420\slmult0 \up0 \expndtw0\charscalex107
Cristalizacin isotrmica: consiste en solubilizar el polmero en un mal disolvente a
temperatura \line \up0 \expndtw-2\charscalex100 elevada y dejarlo cristalizar a
una temperatura menor en un bao de cristalizacin. Los disolventes ms \line \up0 \ex
pndtw-2\charscalex100 utilizados para la cristalizacin de los polmeros de este tra
bajo fueron: \up0 \expndtw-3\charscalex100 2-metil-2,4-pentanodiol, \par\pard\ql
\li1418\sb99\sl-276\slmult0 \up0 \expndtw-3\charscalex100 1,4-butanodiol, hexan
ol y glicerina. \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb
0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb
192\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 53
\par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg2
2}{\bkmkend Pg22}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0

ex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\sb0\sl
-415\slmult0 \par\pard\qj\li1418\ri1220\sb363\sl-415\slmult0 \up0 \expndtw0\char
scalex106 \ul0\nosupersub\cf3\f4\fs24 Cristalizacin por precipitacin: en este caso
se disuelve el polmero en un buen disolvente y se \up0 \expndtw0\charscalex112 c
ristaliza con la ayuda de un agente precipitante. Como disolventes se utilizan ci
dos como \up0 \expndtw0\charscalex103 dicloroactico o frmico y como precipitantes
agua o alcoholes como etanol, metanol o butanol. La \up0 \expndtw0\charscalex110
degradacin de estos cristales en los disolventes empleados se evita al mximo trab
ajando a \up0 \expndtw-3\charscalex100 temperatura ambiente o prxima a ella. \par
\pard\qj \li1418\ri1218\sb405\sl-416\slmult0 \up0 \expndtw0\charscalex103 Los cr
istales obtenidos se separan por centrifugacin, se lavan con un no-solvente sufic
ientemente \up0 \expndtw-3\charscalex100 voltil \up0 \expndtw0\charscalex106 (n-b
utanol) hasta eliminar totalmente el disolvente utilizado para su crist
alizacin, y \up0 \expndtw0\charscalex102 posteriormente se suspenden en el mismo
no-solvente. Una gota de esta suspensin es depositada \up0 \expndtw0\charscalex1
03 sobre una rejilla de cobre de 3 mm de dimetro, cubierta por un film de carbono
delgado (< 200 ), \up0 \expndtw0\charscalex100 obtenido por evaporacin de grafito
a alto vaco (10\ul0\super\cf5\f6\fs23 -4\ul0\nosupersub\cf3\f4\fs24 - 10\ul0\su
per\cf5\f6\fs23 -5\ul0\nosupersub\cf3\f4\fs24 torr) sobre una lmina exfoliada de
mica y \up0 \expndtw-3\charscalex100 flotado posteriormente sobre las rejillas.
\par\pard\qj \li1418\ri1221\sb409\sl-410\slmult0 \up0 \expndtw0\charscalex106 E
l film de carbono es el sustrato ms idneo para trabajar con monocristales porque e
s bastante \up0 \expndtw0\charscalex104 resistente, amorfo y relativamente trans
parente a los electrones. Despus de dejar evaporar el no\up0 \expndtw0\charscalex
100 solvente sobre la rejilla quedan los cristales adheridos sobre el film de ca
rbono y puede obtenerse el \up0 \expndtw0\charscalex107 diagrama de difraccin. La
visualizacin de los detalles de superfcie de los cristales requiere el \up0 \expn
dtw-3\charscalex100 sombreado posterior de la muestra. \par\pard\ql \li1418\sb0\
sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb119\
sl-230\slmult0 \up0 \expndtw-3\charscalex100 b) \ul0\nosupersub\cf9\f10\fs20 CRI
STALIZACIN EPITAXIAL \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\
ri1220\sb26\sl-413\slmult0 \up0 \expndtw0\charscalex106 \ul0\nosupersub\cf3\f4\f
s24 Esta cristalizacin consiste en el crecimiento inducido de un cristal sobre la
superfcie de otro en \up0 \expndtw0\charscalex106 contacto con l. En el campo de
los polmeros se utilizan como substratos sustancias fcilmente \up0 \expndtw0\chars
calex105 solubles y de bajo peso molecular como el cido benzico o la hidroquinona.
\ul0\super\cf5\f6\fs23 85\ul0\nosupersub\cf3\f4\fs24 Estas substancias \up0 \ex
pndtw0\charscalex100 tienen un parmetro cristalogrfico prximo a 5 \ul0\nosupersub\c
f4\f5\fs24 \ul0\nosupersub\cf3\f4\fs24 , valor cercano a la distancia reticular e
ntre cadenas \up0 \expndtw0\charscalex102 de diferentes polmeros como polietileno
, polisteres alifticos y poliamidas (en stas la distancia es \up0 \expndtw0\charsca
lex107 ligeramente menor por la presencia de puentes de hidrgeno). Los planos sep
arados por estas \up0 \expndtw-2\charscalex100 distancias se disponen perpendicu
larmente a la superficie del sustrato. \par\pard\qj \li1418\ri1220\sb407\sl-413\
slmult0 \up0 \expndtw0\charscalex103 Esta tcnica puede resultar complementaria a
la difraccin de electrones de cristales obtenidos por \line \up0 \expndtw0\charsc
alex106 cristalizacin isotrmica o por precipitacin, porque puede proporcionar orien
taciones cristalinas \line \up0 \expndtw0\charscalex105 diferentes. As, en la cri
stalizacin epitaxial puede conseguirse que el eje molecular se encuentre \line \u
p0 \expndtw-2\charscalex100 orientado perpendicularmente al haz de electrones y
no de forma paralela como normalmente ocurre en \par\pard\ql \li1418\sb0\sl-230\
slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb99\sl-230\s
lmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 54

}
4 los cristales obtenidos de disoluciones diluidas. La proyeccin diferente de la
celda unitaria aumenta la \up0 \expndtw0\charscalex104 informacin cristalogrfica,
aunque las reflexiones suelen ser ms arqueadas debido a una mayor \up0 \expndtw-3
\charscalex100 desorientacin de los cristales.\ul0\super\cf5\f6\fs23 86 \par\pard
\qj \li1418\ri1219\sb406\sl-415\slmult0 \up0 \expndtw0\charscalex100 \ul0\nosupe
rsub\cf3\f4\fs24 La cristalizacin epitaxial empieza con la evaporacin de una soluc
in diluida de polmero en un buen \up0 \expndtw-1\charscalex100 disolvente como el c
ido frmico. As, se obtiene un film delgado de polmero sobre el que se aade el \up0 \
expndtw-1\charscalex100 inductor de la cristalizacin. Ambos, se funden conjuntame
nte sobre un portaobjetos hasta obtener una \up0 \expndtw-2\charscalex100 disolu
cin homognea que posteriormente se enfra lentamente bajo un gradiente de temperatur
as. Los \up0 \expndtw0\charscalex108 cristales orientados del inductor favorecern
la cristalizacin del polmero. Mediante un lavado \up0 \expndtw0\charscalex102 exh
austivo con metanol se elimina el inductor del crecimiento. A continuacin, se eva
pora sobre los \up0 \expndtw0\charscalex106 cristales un film de carbono y por m
icroscopa ptica de luz polarizada se seleccionan las zonas \up0 \expndtw0\charscal
ex106 orientadas epitaxialmente. stas se separan del portaobjetos con la ayuda de
una gota de cido \up0 \expndtw-3\charscalex100 poliacrlico que puede eliminarse p
osteriormente en un bao de agua. \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\par
d\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb98\sl-230\slmult0 \up0 \exp
ndtw-3\charscalex100 c) \ul0\nosupersub\cf9\f10\fs20 PELCULAS ORIENTADAS UNIAXIAL
MENTE \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1220\sb26\sl
-413\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf3\f4\fs24 La orient
acin uniaxial de un polmero requiere el estiramiento del material, procedente del
fundido o de \up0 \expndtw0\charscalex105 una disolucin muy concentrada, en
una nica direccin del espacio. El procedimiento es \up0 \expndtw0\charscale
x100 esencialmente idntico a la obtencin de fibras o pelculas orientadas para difra
ccin de rayos X, pero \up0 \expndtw-2\charscalex100 en este caso el grosor de la
muestra es crtico para obtener buenas difracciones. \par\pard\qj \li1418\ri1217\s
b407\sl-413\slmult0 \up0 \expndtw-1\charscalex100 La tensin aplicada sobre el mat
erial se realiza con la ayuda de un material inerte como el tefln capaz \up0 \exp
ndtw0\charscalex109 de producir una fuerte cizalla durante el proceso simultneo d
e orientacin-cristalizacin.\ul0\super\cf5\f6\fs23 87\ul0\nosupersub\cf3\f4\fs24 S
e \up0 \expndtw-1\charscalex100 seleccionan las zonas birrefringentes y despus de
evaporar sobre ellas un film de carbono se separan \up0 \expndtw-2\charscalex10
0 de forma anloga a la cristalizacin epitaxial. \par\pard\ql \li1418\sb0\sl-230\sl
mult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb119\sl-230\sl
mult0 \up0 \expndtw-3\charscalex100 d) \ul0\nosupersub\cf9\f10\fs20 DECORACIN DE
CRISTALES CON POLIETILENO \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\l
i1418\ri1220\sb26\sl-413\slmult0 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf
3\f4\fs24 Esta tcnica fue desarrollada por Wittmann y Lotz en 1985.\ul0\super\cf5
\f6\fs23 88\ul0\nosupersub\cf3\f4\fs24 El fundamento es el mismo que el de la \
up0 \expndtw0\charscalex103 cristalizacin epitaxial, slo que en este caso el polmer
o es el substrato y sobre l se deposita una \up0 \expndtw0\charscalex103 substanc
ia, de estructura cristalina conocida, que cristaliza sobre los monocristales de
l mismo. Nos \up0 \expndtw-3\charscalex100 permite determinar las caractersticas
superficiales de las lamelas. \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard
\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard
\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard
\ql\li10287\sb229\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\c

f1\f2\fs20 55
}
}}
}
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62ddff0009d9bdb4875ad3bec71cf035d4cda76a76fa26af65776d345a8d9dad8b4ff8263fed6b6b
e74e9e08b53a85cebb1db7da65f19fc3fbb58bc377da4584fa8a5ecb7be20b81acdb47e23d3acdae
0ea9a75e5fea7670ccb7565713cdf6f3fd4051401fcc6597fc134bf6b38162b8b5f015ae8d7176cc
b10b4f1af806297c3d6f79632ea52584d15af895ac750b2d2fc56cde4de581b6bfbcd3ce9f750c1a
6dce990dbaadbffc1377f6b786dadee07c33b1b69cddcd737ba6dbf8d3c00f22efd4ad91e6b2d46d
fc65a3c4d7f756ba75aeab24b2dadac2925edde988b1f93f69bdfe9ca8a00fe65a2ff8275fed8b6f
06a8a9f0faceee39acaf560b5bbf1a7c3e491ef2d3c4dadddd91b7ba8bc5b2342352f0e5e68fa78b
cba696e44b6daa49a92f9b35ac8d761ff826efed61653a983c1d6b756f64ae9a74973e25f0025fcb
63aceb709d42c3538ecbc5f63a7bdfe8fa447e759ebda6c5a65ccf22416ba847aebc2b715fd2e514
01fce558fec07fb5bda5887ff841eddef66b6d6aeee6d65f17f805905d6a7ac4da85b696b776de29
b2925b4b65fb28920949b38f64b3b4ba9ba5b5a2cb67ff0004f8fda9bcab8926f072ab5c683ab22d
b5c7897e1eb3b4da8ea5656f2685a9aaf8b751b79dec2d34cd275df0ceb3693adc4371697969a9de
402fee2d2e3fa30a2803f9cc87fe09f9fb575b5fcf247e03b26b232697aba2a78e7c1d13a6bba1eb
17d2e9e6cfccf10ceeb669652c37f1c72cb6e8baa5cdc4b2c6e6dad95b423fd81bf6a4d3e3d2cdbf
80dee63897c3362b141e31f87d15ee9705a5ce9967ae4f7725c78a92d35bd3becf68dace8da6dc34
d75a5491449a7dddacf6f61696dfd11d1401fcf1dbfec07fb50db437a0f82adc4df6fd725b792c7c
4fe06334edad6a7a79b6d5dee24f16e9d24977a35bd8d85ccb6977ba0d6a1d16d61b836f3dedd435
2dcffc13f7f69ab9d4ad675f07dbc5671d9dff0095671f8bfc2762ba3cb0ea2e2d62d2efacfc5124
b04d78a0df5aa9d367b0b5d3ae0699a89b8310b35fe85e8a00fceafd807e037c60f80f6ff13748f8
9ba2dbe93a56a70781a3f0a3c3ac68da89ba9345baf1e5b6ae4db689ab6a16d68874eb9f0c5f3cf3
db5a5e5edf6a37e2796ec5aa2dafe8ad145001451450014514500145145007c65e28fd8afc109e25
f09f8dfe0bf8a7c45f023c45e08f1e6b3f14744f0df8522b0d5fe0bea5e3fd7bc1be25f006abaff8
97e0eeaf1ff61a4ba8785fc63e25b6d467f87fa8fc3ad6752d43536d6aff005ab8d5adedeee3c43e
00fdb02dff00680d1fe2eea167fb3978d749f0e7c30f1a7c31d3ac2cbc65f13fe15dcea16fe34f1b
fc35f1449e20bfd367f00fc64b6b3bcd1acfc09796d0e9d6facdda6a736ad123ea3a6c568f2dc7dd
145007c3f63e08fdabf4cf8f3f18be2a691e11fd9e74ed33e227827e0bf817466d4be2efc49f115f
d85a7c2ed47e36ead7fadea7a05afc0bf0adb9b8d567f899a2595a6916be2d923b7874fd56f66d5d
dfec96335cd2bf648d5bc47aef8dfc41f1b7e2eebbe2fb1f88faf45e23f187c2ef869a3c1f073e14
ebb7a9e04f0ffc3d5b3f138d16ff0058f8abe3ad363f0ff86f4db7934af167c51bdf0c6a2eb31bdf
0bfd8e4834fb4fb528a00c4f0df86bc39e0dd074af0b7843c3fa27857c31a159c5a7689e1cf0de95
61a1e83a369f00c4163a5691a6416ba7e9f670824456b696f0c118384402b6e8a2800a28a2800a28
a2800a28a2800a28a2800a28a28032f5cd0f44f1368daa7877c49a3e97e21f0feb9a7dde93ade85a
e69f69ab68dac6977f03db5f69baa6997f0dc596a1a7dedb4925bddd9ddc135bdcc123c5346f1b32
9f88bc63fb0ec2be1ab0f0a7c10f8d5f107e0ef85f47f1bfc2cf1f685f0e35782c3e2f7c24d0b58f
843e3ef0f7c47f0c58f87fc2fe3897fe12ff0007786e7d7fc31a5dbea5e18f87ff0011bc1da02e8c
6eec747d3b489a68af2dfef1a2803e21f127c3afdaefc53e3ef845aef892f3f664d7741f849e38d4
7c7f6173a6dafc5cf06eb9a9eb77ff000cfe227c35089a63eabe33d374fb5b7d37e22ea3334577a9
ebab7125ac722adacad19b6e76cfe00fed6de24f8d4ff1b3c4ff001b7e0e7c31d465f85f17c24bad
0be18fc2ad7fc71a84da143e31baf1826bba678bbe22f8cac748d1b5b59ee0582dadff00c35f1469
a21f3a7944f23c096dfa0145007cd1e04fd93be11783be211f8cfadd9eaff15be39be9569a19f8d3
f162f2cbc51e3ab3d1f4eb9d7ee74fd33c3515a699a3783fc0561667c53e21852d3e1df853c256f3
c1ac6a11de47726eee1a4fa5e8a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2803fffd9}}}}}\pard\s
b0\sl-240{\bkmkstart Pg24}{\bkmkend Pg24}\par\pard\ql \li1418\sb0\sl-230\slmult0
\par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmult0
\up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \pa
r\pard\qj \li1418\ri1220\sb380\sl-412\slmult0 \up0 \expndtw-1\charscalex100 \ul0
\nosupersub\cf3\f4\fs24 La observacin detallada de los cristales polimricos sugier
e que debe existir un cierto plegamiento de \line \up0 \expndtw0\charscalex100 l
as cadenas debido a que en general, el espesor de las lamelas resulta mucho meno
r que la longitud \line \up0 \expndtw0\charscalex100 promedio de las cadenas. Ad

ems, se acepta generalmente que ste debe ser paralelo a la direccin \line \up0 \exp
ndtw0\charscalex106 de crecimiento del cristal.\ul0\super\cf5\f6\fs23 89\ul0\nos
upersub\cf3\f4\fs24 As, esta tcnica permite conocer la sectorizacin de los cristal
es del \line \up0 \expndtw0\charscalex107 polmero asociada a una direccin privileg
iada de plegamiento molecular durante el crecimiento \line \up0 \expndtw-3\chars
calex100 cristalino (Figura 30a). \par\pard\qj \li1418\ri1219\sb406\sl-415\slmul
t0 \up0 \expndtw0\charscalex100 En la prctica se evapora lentamente bajo vaco (10\
ul0\super\cf5\f6\fs23 -4\ul0\nosupersub\cf3\f4\fs24 - 10\ul0\super\cf5\f6\fs23
-5\ul0\nosupersub\cf3\f4\fs24 torr) una pequea muestra de polietileno \up0 \expn
dtw-1\charscalex100 (~ 2 mg, M\ul0\sub\cf5\f6\fs24 w\ul0\nosupersub\cf3\f4\fs24
= 20.000 y M\ul0\sub\cf5\f6\fs24 w\ul0\nosupersub\cf3\f4\fs24 /M\ul0\sub\cf5\f6
\fs24 n\ul0\nosupersub\cf3\f4\fs24 = 1.1) en un filamento de tungsteno. Durante
este proceso se produce la \up0 \expndtw0\charscalex100 escisin parcial de las c
adenas moleculares de polietileno que cristalizan epitaxialmente en forma de \up
0 \expndtw-2\charscalex100 pequeas barritas alargadas sobre las lamelas del polmer
o a decorar (Figura 30b). Todas las muestras \up0 \expndtw-2\charscalex100 son s
ombreadas con Pt/C despus de la decoracin para su observacin microscpica. \par\pard\
li3761\sb0\sl-276\slmult0\par\pard\li3761\sb0\sl-276\slmult0\par\pard\li3761\sb0
\sl-276\slmult0\par\pard\li3761\sb0\sl-276\slmult0\par\pard\li3761\sb0\sl-276\sl
mult0\par\pard\li3761\sb0\sl-276\slmult0\par\pard\li3761\sb0\sl-276\slmult0\par\
pard\li3761\sb0\sl-276\slmult0\par\pard\li3761\sb0\sl-276\slmult0\par\pard\li376
1\sb0\sl-276\slmult0\par\pard\li3761\sb0\sl-276\slmult0\par\pard\li3761\sb235\sl
-276\slmult0\fi0\tx8174 \up0 \expndtw0\charscalex100 a)\tab \up0 \expndtw0\chars
calex100 b)\par\pard\ql \li1583\sb0\sl-230\slmult0 \par\pard\ql\li1583\sb101\sl230\slmult0 \up0 \expndtw0\charscalex105 \ul0\nosupersub\cf9\f10\fs20 Figura 30.
a) Cristal simple de polietileno cristalizado en p-xileno a 70\ul0\super\cf11\f
12\fs19 \ul0\nosupersub\cf9\f10\fs20 C y decorado con vapores de polietileno. \pa
r\pard\qj \li1583\ri1503\sb10\sl-230\slmult0 \up0 \expndtw0\charscalex106 b) Rep
resentacin esquemtica de la decoracin de cristales con polietileno. Disposicin de la
s lamelas sobre \up0 \expndtw0\charscalex104 parafina exenta de plegamiento que
da lugar a una disposicin del polietileno decorador completamente al azar \up0 \e
xpndtw-2\charscalex100 (izquierda), y polietileno con planos de plegamiento 110
que origina una decoracin sectorizada (derecha). \par\pard\ql \li1418\sb0\sl-276\
mult0 \par\pard\ql\li1418\sb44\sl-276\slmult0 \up0 \expndtw-2\charscalex100 \ul0
\nosupersub\cf3\f4\fs24 3.4.2. DIFRACCIN DE RAYOS X \par\pard\qj \li1418\sb0\sl-4
20\slmult0 \par\pard\qj\li1418\ri1221\sb26\sl-420\slmult0 \up0 \expndtw0\charsca
lex104 Los rayos X son una radiacin electromagntica cuya longitud de onda se encue
ntra comprendida \line \up0 \expndtw0\charscalex108 entre la radiacin UV y los ra
yos \ul0\nosupersub\cf6\f7\fs24 \u947?\ul0\nosupersub\cf3\f4\fs24 . Las propieda
des ms importantes de sta radiacin fueron \line \up0 \expndtw0\charscalex102 descri
tas por Rntgen en 1896, pero no fue hasta principios del siglo pasado que von Lau
e (1912) y \line \up0 \expndtw0\charscalex106 Bragg (1913) demostraron que los c
ristales, debido a su ordenacin regular, podan difractar los \line \up0 \expndtw0\
charscalex105 rayos X dispersados por todos los elementos que los const
ituyen, segn unas direcciones \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\par
d\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\
ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb217\sl-230\slmult0 \up0 \expn
dtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 56 \par\pard\sect\sectd\fs24\pap
erw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg25}{\bkmkend Pg25}\par\pard\ql
\li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl-230\slmult0 \par\pard\ql\
li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\
fs20 Materiales y mtodos \par\pard\qj \li1418\ri1222\sb390\sl-400\slmult0 \up0 \e
xpndtw0\charscalex103 \ul0\nosupersub\cf3\f4\fs24 determinadas. Este descubrimie
nto fue til para la determinacin de la estructura tridimensional de \up0 \expndtw2\charscalex100 numerosas molculas biolgicas,\ul0\super\cf5\f6\fs23 90 \ul0\nosupe
rsub\cf3\f4\fs24 pero tambin en el caso de los polmeros sintticos.\ul0\super\cf5\f6
\fs23 91 \par\pard\qj \li1418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri1220\sb22
\sl-410\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf3\f4\fs24 Esta tc
nica permite obtener el diagrama de difraccin del material y la ordenacin de sus to

mos en el \up0 \expndtw-1\charscalex100 espacio mediante anlisis de Fourier. Aunq
ue es aplicable a muestras slidas, lquidas o gaseosas, en \up0 \expndtw0\charscale
x108 el campo de los polmeros su uso est restringido casi completamente a la deter
minacin de la \up0 \expndtw-1\charscalex100 ordenacin atmica en la parte slida crist
alina, es decir, regularmente ordenada como mnimo en una \up0 \expndtw-3\charscal
ex100 de las tres direcciones del espacio. \par\pard\qj \li1418\ri1221\sb420\sl423\slmult0 \up0 \expndtw0\charscalex102 Cuando los electrones emitidos por un f
ilamento calentado a temperatura elevada se hacen incidir \line \up0 \expndtw0\c
harscalex104 sobre un nodo metlico, de forma que las capas ms internas de los tomos
que lo constituyen \line \up0 \expndtw-1\charscalex100 puedan producir transicio
nes, se generan rayos X cuya longitud de onda se sita entre 10\ul0\super\cf5\f6\f
s23 -7\ul0\nosupersub\cf3\f4\fs24 y 10\ul0\super\cf5\f6\fs23 -11\ul0\nosupersub
\cf3\f4\fs24 m. \line \up0 \expndtw-3\charscalex100 Normalmente se utiliza un no
do de cobre y se obtiene un espectro de rayos X formado por una banda \line \up0
\expndtw-2\charscalex100 ancha responsable de la radiacin blanca y unas lneas car
actersticas (CuK\ul0\sub\cf10\f11\fs24 \u945?\ul0\nosupersub\cf3\f4\fs24 y CuK\u
l0\sub\cf10\f11\fs24 \u946?\ul0\nosupersub\cf3\f4\fs24 ) que se pueden \line \up
0 \expndtw0\charscalex103 separarse mediante filtros adecuados. Para el estudio
de los polmeros se utiliza la lnea CuK\ul0\sub\cf10\f11\fs24 \u945?\ul0\nosupersub
\cf3\f4\fs24 de \line \up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf6\f7\fs24
\u955?\ul0\nosupersub\cf3\f4\fs24 = 0.154 nm y un filtro de nquel para eliminar
al mximo la radiacin CuK\ul0\sub\cf10\f11\fs24 \u946?\ul0\nosupersub\cf3\f4\fs24
y la continua. \par\pard\qj \li1418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri12
21\sb18\sl-410\slmult0 \up0 \expndtw-4\charscalex100 La difraccin de rayos X sigu
e el principio de Huyggens, donde cada rendija presente en el cristal acta \line
\up0 \expndtw-1\charscalex100 como un nuevo foco emisor de ondas que interfieren
constructiva o destructivamente para producir la \line \up0 \expndtw-1\charscal
ex100 difraccin. nicamente se produce interferencia constructiva cuando se cumple
la ley de Bragg: \par\pard\ql \li5195\sb0\sl-276\slmult0 \par\pard\ql\li5195\sb2
65\sl-276\slmult0 \up0 \expndtw-3\charscalex100 n \ul0\nosupersub\cf6\f7\fs24 \u
955?\ul0\nosupersub\cf3\f4\fs24 = 2 d\ul0\sub\cf5\f6\fs24 hkl\ul0\nosupersub\cf
3\f4\fs24 sen \ul0\nosupersub\cf6\f7\fs24 \u952? \par\pard\qj \li1418\sb0\sl-44
0\slmult0 \par\pard\qj\li1418\ri1221\sb9\sl-440\slmult0 \up0 \expndtw-3\charscal
ex100 \ul0\nosupersub\cf3\f4\fs24 donde d\ul0\sub\cf5\f6\fs24 hkl\ul0\nosupersub
\cf3\f4\fs24 es el espaciado de los planos de Miller, \ul0\nosupersub\cf6\f7\fs
24 \u952?\ul0\nosupersub\cf3\f4\fs24 el ngulo de incidencia o reflexin, n el nmero
de \line \up0 \expndtw-4\charscalex100 orden y \ul0\nosupersub\cf6\f7\fs24 \u95
5?\ul0\nosupersub\cf3\f4\fs24 la longitud de onda de la radiacin utilizada \up0
\expndtw-4\charscalex100 (Figura \up0 \expndtw-4\charscalex100 31). El conjunto
de espaciados \par\pard\qj \li1418\ri1220\sb0\sl-430\slmult0 \up0 \expndtw0\char
scalex103 cristalogrficos permite determinar la celdilla unitaria determinada por
los parmetros a, b, c y los \up0 \expndtw-1\charscalex100 ngulos existentes entre
ellos \ul0\nosupersub\cf6\f7\fs24 \u945?\ul0\nosupersub\cf3\f4\fs24 , \ul0\nosu
persub\cf6\f7\fs24 \u946?\ul0\nosupersub\cf3\f4\fs24 , y \ul0\nosupersub\cf6\f7\
fs24 \u947?\ul0\nosupersub\cf3\f4\fs24 . Esta celdilla representa la unidad ms pe
quea que refleja la \up0 \expndtw-5\charscalex100 simetra del cristal. \par\pard\q
l \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\
ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\
ql\li10287\sb65\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1
\f2\fs20 57 \par\pard\sect\sectd\fs24\paperw11900\paperh16840{\shp
z-10000\shplid25
ffd8ffe000104a46494600010101006000600000ffdb004300010101010101010101010101010101
01010101010101010101010101010101010101010101010101010101010101010101010101010101
010101010101010101ffdb0043010101010101010101010101010101010101010101010101010101
0101010101010101010101010101010101010101010101010101010101010101010101010101ffc0
00110803e702c203012200021101031101ffc4001f00000105010101010101000000000000000001
02030405060708090a0bffc400b5100002010303020403050504040000017d010203000411051221
31410613516107227114328191a1082342b1c11552d1f02433627282090a161718191a2526272829
2a3435363738393a434445464748494a535455565758595a636465666768696a737475767778797a
0101010101010101010000000000000102030405060708090a0bffc400b511000201020404030407
05040400010277000102031104052131061241510761711322328108144291a1b1c109233352f015
6272d10a162434e125f11718191a262728292a35363738393a434445464748494a53545556575859
5a636465666768696a737475767778797a82838485868788898a92939495969798999aa2a3a4a5a6
0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a2bf2d3fe0a1df03bf6d
9f8bbe2af853aefeca3f12353f0368ff000c7c21e39f156bda2699e3cf10f8365f889f1021f881f0
56f3c1fe0fff00892f8d3c27a379da9781f4af8ab636faefc43d33c7be01d19afe4b6d57c197d3ea
d6d756a01fa97457f3f361f16ffe0b79e7cbe09bcf86fe00d0fc71e37f19fed01a8f8417c51a5f81
bc4e9e11f853e01f077c3ef13781aeee7c5fe01d4b4ef87575af78b3c75adf89be127856d7c68fe1
4b89617d13c65ab41ab58e9daf5c47f44fecb5ae7fc152efbe297c40b2fdabbc232ddfc15b9fd9ff
005697c08de1aff852be07f1ba7c41b5d645bf86ed75dbcf07f8d7c50e3e2ef8c3c26d35df8ae7d0
756d13e11781bc5319b3f0e8b9d3934fd735000fd7da2bf0dfc2de10ff0082bd781ff64ad1ec5b50
b4f1b7ed7f27ed0d0cdafebbe30f1cf833c55e04b2f8137df0c354d33c2971a1e9fa74bf0e34dbbd
47e1f09bc1fa37c48d2755b7697e22fc68f0f78ebe2369cf77e12f16684f61cff8b7e297fc16c341
d6ecf4ed1fe0b689e34d4341b682deea4b1f0ffc25d3be1b789fc33a3e8be2e82e7e2449e2bff868
0d23c5f07c5bf12ebf16913c3f036dbc193780d2c574757f1d686751d42f2c403f7a28afe773e117
c4ff00f82ef6a171e2df08f897e17784747d16f353bd9fc07f173e25f833c0b378ac783bc45f1e74
c7d33c5be24f871e08f8bada068fe35d27e176a9e2db0d43e1047e2cbdb0f0c689e1bf076ab078b7
c47ab5fea76b73b3aafed1bff05b8d1b53d6ad62fd9bbc17369937c3ff001e78ab4dd7b51f05af88
adec7c57268b0dee97e0fb4d1fc09e3d6d667ff843af934db6f0bc17f1dd5ffc42935cf115bdddf3
dc785ade2ba00fe82a8af1dfd9efc4ff00123c69f037e1378b3e30f846f7c07f14fc43e01f0ceabf
103c1da8dae9f617de1ef165de976f2eb5a75d58695aef89ac2c268af4cacd616faf6a62cb7fd964
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}}}\pard\sb0\sl-240{\bkmkstart Pg26}{\bkmkend Pg26}\par\pard\ql \li1418\sb0\sl-2
0\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y
mtodos \par\pard\li1871\sb0\sl-276\slmult0\par\pard\li1871\sb0\sl-276\slmult0\pa
r\pard\li1871\sb0\sl-276\slmult0\par\pard\li1871\sb187\sl-276\slmult0\fi0\tx7344
\up0 \expndtw0\charscalex100 \ul0\nosupersub\cf3\f4\fs24 a)\tab \up0 \expndtw0\
charscalex100 b)\par\pard\ql \li7954\sb0\sl-276\slmult0 \par\pard\ql\li7954\sb0\
-276\slmult0 \par\pard\ql\li7954\sb0\sl-276\slmult0 \par\pard\ql\li7954\sb0\sl-2
\slmult0 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf6\f7\fs24 tan 2\u952? =
D/2L \par\pard\qj \li1871\sb0\sl-240\slmult0 \par\pard\qj\li1871\ri1713\sb34\sl240\slmult0 \up0 \expndtw-3\charscalex100 \ul0\nosupersub\cf9\f10\fs20 Figura 31
. a) Geometra de la difraccin de rayos X, b) relacin entre el dimetro de la difraccin
(D) y el ngulo \up0 \expndtw-4\charscalex100 de dispersin (2\ul0\nosupersub\cf1\f
2\fs20 \u952?\ul0\nosupersub\cf9\f10\fs20 ). \par\pard\qj \li1418\sb0\sl-430\slm
ult0 \par\pard\qj\li1418\ri1220\sb34\sl-430\slmult0 \up0 \expndtw0\charscalex100
\ul0\nosupersub\cf3\f4\fs24 La difraccin de rayos X se realiz utilizando cmaras Wa
rhus (W.H. Warhus, Wilmington, Delaware, \line \up0 \expndtw0\charscalex104 USA)
tipo Statton con monocromador de grafito incorporado que selecciona la radiacin
K\ul0\sub\cf10\f11\fs24 \u945?\ul0\nosupersub\cf3\f4\fs24 del Cu \line \up0 \ex
pndtw0\charscalex106 (\ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosupersub\cf3\f4\f
s24 = 0.154 \ul0\nosupersub\cf4\f5\fs24 nm\ul0\nosupersub\cf3\f4\fs24 ) y un ge
nerador Phillips modelo P-W 1130/90 provisto de un tubo Phillips sellado \line \
up0 \expndtw0\charscalex111 (PW 2113 de 1200 W) de foco plano y con filtro de ni
quel. El calibrado se realiz con calcita \line \up0 \expndtw-2\charscalex100 d\ul
0\nosupersub\cf5\f6\fs16 B\ul0\nosupersub\cf3\f4\fs24 = 0.3035 \ul0\nosupersub\
cf4\f5\fs24 nm\ul0\nosupersub\cf3\f4\fs24 o sulfuro de molibdeno d\ul0\nosupers
ub\cf5\f6\fs16 002\ul0\nosupersub\cf3\f4\fs24 = 0.6147 \ul0\nosupersub\cf4\f5\f
s24 nm\ul0\nosupersub\cf3\f4\fs24 dependiendo de la longitud de cmara. \par\pard
\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb242\sl-276\slmult0 \up0 \ex
pndtw-3\charscalex100 Las muestras analizadas por difraccin de rayos X correspond
en a: \par\pard\ql \li1418\sb0\sl-241\slmult0 \par\pard\ql\li1418\sb0\sl-241\slm

ult0 \par\pard\ql\li1418\sb91\sl-241\slmult0 \up0 \expndtw-3\charscalex100 a) \u
l0\nosupersub\cf9\f10\fs20 DIAGRAMAS DE POLVO \par\pard\qj \li1418\sb0\sl-413\sl
mult0 \par\pard\qj\li1418\ri1219\sb24\sl-413\slmult0 \up0 \expndtw0\charscalex10
7 \ul0\nosupersub\cf3\f4\fs24 Son los diagramas de difraccin de muestras totalmen
te desorientadas y se caracterizan por la \line \up0 \expndtw0\charscalex100 pre
sencia de una serie de anillos concntricos cuya intensidad y dimetro son caracterst
icos de cada \line \up0 \expndtw0\charscalex105 polmero. Estos anillos estn ligado
s a la reflexin producida por los planos cristalogrficos de los \line \up0 \expndt
w0\charscalex110 cristales del polmero. Se obtienen colocando una muestra del polm
ero finamente triturado y \line \up0 \expndtw0\charscalex102 fuertemente compact
ado en un capilar de vidrio sin plomo con dimetro variable entre 0.5 y 1.5 mm. \l
ine \up0 \expndtw-1\charscalex100 Dado que cada uno de los cristales est dispuest
o al azar con respecto al resto, la difraccin final tiene \line \up0 \expndtw0\ch
arscalex106 forma de anillo que ser tanto ms definido cuanto ms cristalino sea el p
olmero. El nmero de \line \up0 \expndtw-1\charscalex100 reflexiones presentes en e
stos diagramas es muy reducido, por lo que en muchas ocasiones la celdilla \line
\up0 \expndtw0\charscalex103 unitaria no queda inequvocamente designada. As pues,
para tener una buena aproximacin de la \line \up0 \expndtw-2\charscalex100 estru
ctura es de vital importancia disponer de diagramas de difraccin de muestras orie
ntadas. \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\s
lt0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 58 \par\pard\sect\
sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg27}{\bkmkend Pg2
7}\par\pard\li1418\sb0\sl-230\slmult0\par\pard\li1418\sb0\sl-230\slmult0\par\par
d\li1418\sb21\sl-230\slmult0\fi7346 \up0 \expndtw-3\charscalex100 \ul0\nosupersu
b\cf1\f2\fs20 Materiales y mtodos\par\pard\li1418\sb0\sl-276\slmult0\par\pard\li1
418\sb207\sl-276\slmult0\fi0 \up0 \expndtw-3\charscalex100 \ul0\nosupersub\cf3\f
4\fs24 b) \ul0\nosupersub\cf9\f10\fs20 DIAGRAMAS DE FIBRA\par\pard\qj \li1418\sb
0\sl-413\slmult0 \par\pard\qj\li1418\ri1221\sb16\sl-413\slmult0 \up0 \expndtw0\c
harscalex103 \ul0\nosupersub\cf3\f4\fs24 Un diagrama de fibra muy orientado prop
orciona una informacin ms precisa que un diagrama de \line \up0 \expndtw0\charscal
ex102 difraccin de polvo, en cuanto a la asignacin de los ndices de Miller correspo
ndientes a los planos \line \up0 \expndtw-1\charscalex100 difractados y a la det
erminacin de la simetra cristalina. Las propiedades trmicas y el peso molecular \li
ne \up0 \expndtw0\charscalex106 del polmero son condicionantes para la aplicacin d
e este mtodo. Debido a que el polmero es \line \up0 \expndtw0\charscalex100 estira
do segn el propio eje molecular, estos diagramas se caracterizan por la aparicin d
e manchas \line \up0 \expndtw0\charscalex100 relacionadas con la repetitividad d
e cadena con orientacin meridional (M) o fuera del meridiano (oM) \line \up0 \exp
ndtw-1\charscalex100 segn el sistema cristalino, y manchas ecuatoriales \up0 \exp
ndtw-1\charscalex100 (E), relacionadas con el empaquetamiento \par\pard\qj \li14
18\ri1220\sb10\sl-410\slmult0 \up0 \expndtw-1\charscalex100 cristalino. La orien
tacin de la muestra se consigue a partir del estirado de la masa polimrica fundida
. \up0 \expndtw0\charscalex105 sta puede mejorarse al someter la muestra a un pro
ceso posterior de templado que consiste en \up0 \expndtw-1\charscalex100 \u8220?
reestirarla\u8221? bajo tensin constante en estufa o en atmsfera de vapor de agua.
El grado de orientacin \up0 \expndtw0\charscalex106 de la fibra resultante se es
tima cualitativamente mediante la birrefrigencia de la muestra bajo un \up0 \exp
ndtw-3\charscalex100 microscopio de luz polarizada. \par\pard\ql \li1418\sb0\sl230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb99\sl-2
30\slmult0 \up0 \expndtw-3\charscalex100 c) \ul0\nosupersub\cf9\f10\fs20 DIAGRAM
AS DE SEDIMENTO CRISTALINO \par\pard\qj \li1418\sb0\sl-411\slmult0 \par\pard\qj\
li1418\ri1219\sb50\sl-411\slmult0 \up0 \expndtw0\charscalex102 \ul0\nosupersub\c
f3\f4\fs24 Estos diagramas estn orientados parcialmente segn el eje de apilamiento
de las lamelas. Aportan \line \up0 \expndtw0\charscalex108 informacin adicional
sobre la naturaleza lamelar de los cristales, ya que aparecen reflexiones \line
\up0 \expndtw-2\charscalex100 meridionales relacionadas con el espesor de la lam
ela debido a que la muestra se irradia paralelamente \line \up0 \expndtw0\charsc
alex100 a la superficie de deposicin. Tambin proporcionan informacin acerca de la i

nclinacin de la cadena \line \up0 \expndtw-1\charscalex100 respecto a la lamela y
del nmero de unidades repetitivas que pueden existir en el interior de la misma.
\line \up0 \expndtw0\charscalex103 Cuando ste es reducido, se producen unas refl
exiones dbiles adicionales denominadas mximos \line \up0 \expndtw-1\charscalex100
subsidiarios. El nmero de los mismos observado entre las reflexiones correspondie
ntes a dos rdenes \line \up0 \expndtw-1\charscalex100 consecutivos de la repetiti
vidad de residuo es igual al nmero de unidades repetitivas menos dos. \par\pard\q
j \li1418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri1222\sb20\sl-410\slmult0 \up0
\expndtw0\charscalex111 La preparacin de estos sedimentos requiere una optimizac
in previa de las condiciones de \line \up0 \expndtw0\charscalex100 cristalizacin d
el polmero. Entre 20-25 mg de polmero perfectamente cristalizados son centrifugado
s \line \up0 \expndtw0\charscalex104 para obtener el sedimento de cristales que
se separa por decantacin. Despus de lavarlos varias \line \up0 \expndtw0\charscale
x106 veces con n-butanol, son suspendidos en l y filtrados lentamente en un dispo
sitivo como el que \line \up0 \expndtw-3\charscalex100 muestra la Figura 32. \pa
r\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \p
ar\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \p
ar\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \p
ar\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb189\sl-230\slmult0
\up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 59
}
}}
}
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0af847c47f12f56f8abf08ef3e3268171e08d574db7bff001de853fc344f88da3787f5cb8d6b50b9
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f1e3c21e0bfda63c3ff1cfc71e26f8b5f0ff00c51e1ed5fc53e21d63e07e9fe19f107c0c80d8c9a9
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7c79f0afc1e934afda275e1af78edbe267c6ad4fc3cf71a95beb9ac687f08b5af8b7e34d5be07f84
bc55af5a6eb7d7fc5be12f84b79e0ef0f789b578aeb5337babe9d74f2eb7aece25d6affe99a2803f
97bff82987c04ff839d3c5b73e2793f62bfdae3f656ff856b71737d268de10f869e08b1f82df19bf
b2d371b2b09bc4df16a0f897a23eab2c521865d4f4af88de118649e2fb4476da7e6351ce7fc122fe
06ff00c178b44fd98fc41a2fc6ff00da13c21f097e34597c61f1d4ff00102c3f6bef815f10bf681f
891e279afd348b9d07c51a17c63d33f68cd3bc27e29f024fa19b4d2b43d3fc236565a5f86ef34ad5
74eb9b53a99bcbebff00ea9e8a00fca2ff00853dff000596ff00a3ddfd893ff10abe22ff00f44d57
d0765f0a3f693f10fec9bf1cbe177ed45e21f841fb4cfc4af1cf837e28787b4cd27e1ef877c6bfb3
7f80bc5de1ff0011782e6d2743f87dae6a56be3cf1bf8bbc2efacea52dee9dad78eb40d7edf50d33
4ed592f34cb286ef4c592e3edaa2803fcd67c59fb3a6a5fb3efecd5f18ff006a7f897ff06cff0086
fe02fc1ef827e24d1f46f88b07887fe0a39fb5d7c3bf16ea0da86bfa3f8522f10784fc1abf116cef
3c71a30d675dd2f4bb4f10e850eab6ba8c978b2e8afab595a5e4b07f7dff00b0d7ecebfb3ffecc3f
b327c32f875fb34fc159ff0067ef865aa68965f10a2f861a9dceb77fe26d07c43e3eb0b2f116bf17
8d352f126afaf6bba878c61bbba163afcfa96b17f2c57765f628655b4b4b68a3fc94ff0082ebea32
7c7df89fff0004bdff00826569938b88bf6c8fdb2fc31f10be31e916c924f7d71fb3afecac96df15
bc7f14f1a4f6c96b637fa945a1ceb7b2ce8e27d0dd2d1269c6cafe88a803f2f7e00ffc120bf62dfd
9bff006e3f8fdff0502f879e09d43fe17afc7cbbbbd52e23d6af2d351f097c31d77c4d6fb3e28f88
7e15e8ff00d9f0dc786f5df8bf7ab16a3e3dd52e750d4eeee1c5d69da2c9a3689a9ea7a5ddf9e7fc
1777f659d77f6a7ff82697c76b0f87d677b2fc70f80f1e89fb52fc00d4749758f5dd1fe2bfc04bff
00f84db4f9741760776adabf86ad7c4fe19b3841579a6d7116264b810c89fb0b51cd0c57114b04f1
473c13c6f0cd0ca8b2453452a94922963705248e446647460559495604122803e41ff827efed51a6
fedb7fb157ecd3fb55e9b67fd9a7e35fc29f0df8b358d301b62ba578b1219347f1a69517d92e6ee1
10699e2fd335bb0b75f3cccb05bc6b731c17225823fb0abf9d5ff822706fd92bf694ff00829a7fc1
27351dd65e1dfd9bbe3e47fb4b7ecc5653068633fb337ed5501f1958f8774180b32cba4fc36f17f9
fa3dfdd4442b6b5e23b88e48d24197fe8aa800a28a2800a28a2800a28a2800a28a2800a28a2800a2
8a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28af1dfda1be34785ff00671f80df19be
3f78d668a1f0a7c17f85fe39f89faf99678ed84da77827c37a8f8867b38e694845b9bf1602c6d149
cc975710c6819dd54807e10fecb1a8bfed99ff0007097edd5f1fe56bbd47e1affc1377e00f80ff00
628f861e7dc470d8da7c5df8a3a8ddf8ebe316b561a7c72acf25f58b697e20f05df5eddc2d15c5a2
d9796c4416863fe902bf9f7ff8369be16f8af41ff826d59fed1ff1312cae3e2dfede3f1c3e31fed8
7e3fd5e349db54d49fe2578a66d3bc38756bcb986292e0be83e1eb5d5ec23817ec36f69ada8b61e6
4b70f27f41140051451401fce97fc152d5bf62bff82987fc132bfe0a73a446963e08f1d78ce7ff00
82707ed613c16c6186e7e1d7c78babad5fe0cf8b35ebbb6653f60f007c49b4bfd4ee6e6f629c051a
4d8a4b144552bfa2daf807fe0a93fb2059feddbfb01fed39fb32792ade26f1dfc36d5351f867780e
c9b48f8bde0a921f1afc2ad520b8578e5b5fb3f8f340d0a3bb9a096295b4e9ef6012059981e5bfe0
90ff00b5d5dfedb9ff0004f0fd9afe3a7887cc83e24c9e0bff008573f1a74bba5962d4b48f8d1f09
afae7e1e7c4ab7d4ed2748e7b1bad47c49e1ebaf10c36732f99169dad5892f22bac8c01fa4f45145
00145145001451450014514500145145001451450014514500145145001451450014514500145145
00145145001451450014514500145145001451450014514500145145001451450014514500145145
00145145001451450014514500145145001451450014514500145145001451450014514500145145
00145145001451450014514500145145001451450014514500145145001451450014514500145145
0015fcdaff00c1d09f1c35df0dfec0de07fd90be1f5c4e7e2b7fc143ff00688f853fb2ff00866c34
e0d2eaf2786350f1369be21f1a5e59db46c27b8b7b8934ff000d783efe38d245787c66904a364f83
fd2557f26ff1fd6fff006fbff83a0bf65ff83fa2c96d7bf0a7fe093ff01756f8f3f12ee62b88aee2
8be2e7c4ab6d3ef340d25e39229ad23d521bcd7be0ddec16c02ea16b068be21bc8ae219ad5638803
fa82f83df0c7c35f04fe137c32f83be0db4b7b1f09fc2bf00f843e1e786ed6d6ced6c208745f06e8
161e1fd3425959470da5b6eb5d3e2778ade24895d9822815e8d4514005145140057f3c7ff04f0897
f623ff0082b47fc146bfe09e17519d2fe18fed2274bff829a7ecb168d35c269f0dbfc46bdb6f02fe
d29e14d2e1b8568226d2fe2669d61a969da569d398ed34586e2f1eda113123fa1cafe7c7fe0b8563
2fecd1f10ffe09edff000563d12da7587f61efda2ed3c01fb404ba72cb0dd5efeca7fb522da7c27f
88977a8cd02b7db6d7c17ae6a1a0eafa5d85e836305e6af797ccd0c89e6800fe83a8a82dae6def6d
adef2d278ae6d2ee08ae6d6e6075960b8b79e359619e1910949229637592375255d18329208353d0
01451450014514500145145001451450014514500145145001451450014514500145145001451450
01451450014514500145145001451450014514500145145001451450014514500145145001451450
01451450014514500145145001451450014514500145145001451450014514500145145001451450
01451450014514500145145001451450014514500145145001451450014514500145145001451450
060f8abc4da1f82bc31e23f19789f518348f0d784b41d63c4de21d5ae9b65b699a1e83a7dc6abab6
a370ff00c3059585a5c5cccdfc31c4c7b57f2fdff06c6695af7c78d13fe0a25ff053df1c6956bff0
907ede3fb63f8dafbc0fadddc570be20ff008543f0def350b5f0e686c248d2d2db43d1754f116a5e
1ed3e0b2dd23c9e1b912f5dbec96690fd7dff0726fed3f7dfb32ff00c123ff0068c4f0cdf5f5a7c4
3fda107877f661f87b0695b8ea9a86a7f17efdb4ef15d9d8a45225cb4f2fc32b0f1d2c4d6a1e75b8
36e2342eea0fe807fc1353f664d3ff00638fd81ff64cfd9b2cb468b42bef861f047c11a778b6c238
0dbbb7c45d634a8bc4bf12efee636925617baa78ff0059f126a57a4c8d9b9ba976844da8a01f70d1
4514005145140057cf5fb5a7ecf5e17fdacbf662f8fbfb33f8c9611e1df8e5f09bc73f0d2f6ea78d
e51a54fe2af0fdf699a5ebd0a46f1c9f6cf0eead358ebb60f1bac91dee9d6f22306406be85a2803f
1bff00e0841fb43f8a7e38ff00c13b3e19781fe2a49710fed03fb216bbe2afd8bbf683d1f51bdfb6
eb5a5fc48fd9d3511e09827d5de48e1bb7bad7fc176fe13f114971770ac97171a9dc9f3ae9a37b89
3f642bf9e1f854ebfb0e7fc17f3e37fc24b873a1fc16ff0082b2fc08d3bf685f86f6cf771ae8d27e
d65fb3b44de1ff008c3a469b6d70d11b5d6bc5bf0deea0f1d6b22d4dc1d52e63b37215a2d91ff43d
40051451400514514005145140051451400514514005145140051451400514514005145140051451
40051451400514514005145140051451400514514005145140051451400514514005145140051451
40051451400514514005145140051451400514514005145140051451400514514005145140051451
40051451400514514005145140051451400514514005145140051451400514514005145140051451
401fc997fc16374ff157ed3fff0005ccff008228fec43e33b1d3b48fd9d342d6fc51fb5adedff88e
e65d3b45f89ff11be1a5cebdaddc7822d649e3974fd6b55f0ee87f0ef44b3b5d1225fb6cf1fc51be
82ebcab5beb4926feb36bf18ff00e0b8bfb0df8bbf6bdfd9117e22fc059aff0042fdb3bf631f135b
fed41fb2378c3416962f115b7c43f87fe46b3acf81acde0647bbb6f88da1694fa3c5a54adf62bbf1
4d9f84eeaf524b7d3de293e14f86dff0732f87eefe1f782ee3e2affc12effe0aa5a4fc4c97c33a39
f1f69de0cfd942fb5bf085b78b96ca14d78785f56d4bc53a3ea37fe1f97515b89f479f50d2b4fbf3
a7cb6eb79690dcacaa003fa87a2bf9aeff0088973e10ff00d2333fe0aeff00f88767ff009bba3fe2
25cf843ff48ccff82bbffe21d9ff00e6ee803fa51a2bf9aeff0088973e10ff00d2333fe0aeff00f8
8767ff009bba3fe225cf843ff48ccff82bbffe21d9ff00e6ee803fa51a2bf9aeff0088973e10ff00
d2333fe0aeff00f88767ff009bba3fe225cf843ff48ccff82bbffe21d9ff00e6ee803b0ff838c5ad
7e18fc08fd8dbf6bef065c470fed2bfb2c7ededfb3ceb3fb3be8d6c14ebbf14754f893e268bc15e3
ff00827a5030dc7996fe3df064975aaeaf0189d66b2f0714c17288ff00d0e42ef2c3149244d04924
51bbc2e559e17740cd133292acd1b128c549524120e2bf925f0b7c47f1f7fc1777fe0a81fb2078b6
e7f66afda63f677fd857fe09c7a7defed27e29f0ff00ed55f0a2fbe186b3f17ff6a2d6350b9d27e1
4d9e87a4c926bba4eb561e056d234ef12c170757125ada5bf8b6cef6cedffb6f497bafeb7e800a28
a2800a28a2800a28a2800a28a2803fffd9}}}}}\pard\sb0\sl-240{\bkmkstart Pg28}{\bkmken
d Pg28}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\sl
mult0 \par\pard\ql\li1418\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0
\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\ql \li2880\sb0\sl-230\slmul
par\pard\ql\li2880\sb0\sl-230\slmult0 \par\pard\ql\li2880\sb0\sl-230\slmult0 \pa
r\pard\ql\li2880\sb0\sl-230\slmult0 \par\pard\ql\li2880\sb0\sl-230\slmult0 \par\
pard\ql\li2880\sb0\sl-230\slmult0 \par\pard\ql\li2880\sb0\sl-230\slmult0 \par\pa
rd\ql\li2880\sb0\sl-230\slmult0 \par\pard\ql\li2880\sb0\sl-230\slmult0 \par\pard
\ql\li2880\sb0\sl-230\slmult0 \par\pard\ql\li2880\sb0\sl-230\slmult0 \par\pard\q
l\li2880\sb0\sl-230\slmult0 \par\pard\ql\li2880\sb0\sl-230\slmult0 \par\pard\ql\
li2880\sb0\sl-230\slmult0 \par\pard\ql\li2880\sb0\sl-230\slmult0 \par\pard\ql\li
0 Figura 32. Dispositivo para obtener un sedimento de cristales para difraccin de
rayos X. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb256\sl-2
76\slmult0 \up0 \expndtw-3\charscalex100 \ul0\nosupersub\cf3\f4\fs24 3.4.3. COMP
UESTOS MODELO \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb268\
sl-276\slmult0 \up0 \expndtw0\charscalex104 3.4.3.1. Obtencin de monocristales \p
ar\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1219\sb38\sl-413\slm
ult0 \up0 \expndtw0\charscalex105 En general, el crecimiento de un cristal debe
ser lento para que las molculas o iones formen una \up0 \expndtw0\charscalex105 d
isposicin regular interna altamente ordenada llevando a la obtencin de un cristal
bien formado \up0 \expndtw-1\charscalex100 (monocristal), adecuado para el anlisi
s por difraccin de rayos X. El objetivo es alcanzar un estado de \up0 \expndtw0\c
harscalex112 saturacin de la solucin, el cual promueve la formacin de algunos ncleos
cristalinos que \up0 \expndtw0\charscalex102 posteriormente llegarn a formar cri
stales de tamaos mayores. Cuando se inicia la cristalizacin el \up0 \expndtw0\char
scalex109 sistema evoluciona hacia un equilibrio entre las partculas de la fase sl
ida y la fase lquida, lo \up0 \expndtw-1\charscalex100 suficientemente lento como
para que las molculas puedan ordenarse en una red cristalina. El proceso \up0 \e
xpndtw0\charscalex105 depende de factores tales como: la solubilidad, la tempera
tura, la fuerza inica, la nucleacin y el \up0 \expndtw0\charscalex105 crecimiento
del cristal. El crecimiento depende de la naturaleza de las fuerzas en la superf
icie del \up0 \expndtw-2\charscalex100 cristal, de la concentracin de la muestra
y del medio de cristalizacin. \par\pard\qj \li1418\ri1221\sb408\sl-412\slmult0 \u
p0 \expndtw0\charscalex102 Normalmente, las caras del cristal que se desarrollan
con mayor rapidez son aquellas en las que las \line \up0 \expndtw-2\charscalex1
00 partculas se enlazan fuertemente por puentes de hidrgeno o fuerzas de van der
Waals. Dependiendo \line \up0 \expndtw-1\charscalex100 de las caractersticas prop
ias de la molcula se forman cristales aciculares o bidimensionales debido a \line
\up0 \expndtw0\charscalex100 la existencia de direcciones de crecimiento favore
cidas. Variando las propiedades de los disolventes y \line \up0 \expndtw0\charsc
alex102 precipitantes como: densidad, constante dielctrica, viscosidad, solvatacin
y volatilidad, se pueden \line \up0 \expndtw-3\charscalex100 evitar estos probl
emas. \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slm
lt0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 60 \par\pard\sect\
sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg29}{\bkmkend Pg2
9}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl-230\slmult0

\par\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosu
persub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\sb0\sl-416\slmult0 \p
ar\pard\qj\li1418\ri1221\sb361\sl-416\slmult0 \up0 \expndtw0\charscalex111 \ul0\
nosupersub\cf3\f4\fs24 Para la cristalizacin de una substancia se han de determin
ar los disolventes y precipitantes \line \up0 \expndtw0\charscalex100 adecuados.
Un buen disolvente ser aquel que permita una concentracin de 5-200 mg/mL y un bue
n \line \up0 \expndtw-2\charscalex100 precipitante ser aquel en que la solubilida
d sea menor que 1 mg/mL. Si la concentracin del disolvente \line \up0 \expndtw0\c
harscalex100 es menor de 5-200 mg/mL, el flujo de soluto es bajo y se favorece l
a nucleacin sin crecimiento; si es \line \up0 \expndtw0\charscalex104 mayor, la v
iscosidad de la solucin es elevada por lo que la difusin es baja y se obtiene un sl
ido \line \up0 \expndtw-3\charscalex100 vtreo. \par\pard\qj \li1418\ri1220\sb401\
sl-420\slmult0 \up0 \expndtw-1\charscalex100 Entre las diferentes tcnicas utiliza
das para la obtencin de monocristales destacamos dos que fueron \up0 \expndtw-3\c
harscalex100 empleadas en este trabajo: \par\pard\ql \li1418\sb0\sl-230\slmult0
up0 \expndtw-3\charscalex100 a) \ul0\nosupersub\cf9\f10\fs20 EVAPORACIN LENTA DEL
DISOLVENTE \par\pard\qj \li1418\sb0\sl-412\slmult0 \par\pard\qj\li1418\ri1219\s
b28\sl-412\slmult0 \up0 \expndtw0\charscalex107 \ul0\nosupersub\cf3\f4\fs24 Evap
oracin lenta del disolvente es un mtodo disponible para la obtencin de cristales de
alta \up0 \expndtw0\charscalex102 calidad y, primariamente, usado para molculas
pequeas. La velocidad de crecimiento es regulada \up0 \expndtw0\charscalex100 por
el ajuste de condiciones (concentracin inicial, temperatura, velocidad de evapor
acin) tal que los \up0 \expndtw0\charscalex102 cristales son obtenidos en pocos da
s. La velocidad de evaporacin puede ser ajustada cubriendo la \up0 \expndtw0\char
scalex100 solucin con un vidrio de reloj o un Parafilm\ul0\super\cf5\f6\fs23 \ul0\
nosupersub\cf3\f4\fs24 en cuya superficie se habrn inyectado algunas agujas. \up
0 \expndtw-2\charscalex100 La solucin es dejada en reposo evitando cualquier tipo
de pertubacin posible. \par\pard\qj \li1418\sb0\sl-400\slmult0 \par\pard\qj\li14
18\ri1221\sb38\sl-400\slmult0 \up0 \expndtw0\charscalex100 Experimentalmente, se
aade el precipitante sobre la muestra y luego se adiciona el disolvente hasta \u
p0 \expndtw-2\charscalex100 disolucin total. El producto cristaliza al dejar evap
orar lentamente el disolvente. \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard
\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb121\sl-230\slmult0 \up0 \exp
ndtw-3\charscalex100 b) \ul0\nosupersub\cf9\f10\fs20 PRECIPITACIN POR DIFUSIN DE V
APOR \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1219\sb46\sl413\slmult0 \up0 \expndtw0\charscalex104 \ul0\nosupersub\cf3\f4\fs24 En el mtodo
de difusin de vapor, se prepara una disolucin del compuesto (1 mg/200 \ul0\nosuper
sub\cf6\f7\fs24 \ul0\nosupersub\cf3\f4\fs24 L de una \line \up0 \expndtw-1\charsc
alex100 mezcla de precipitante:disolvente) y se coloca en un porta excavado (spo
t plates, Corning\ul0\super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 ). Luego, se
\line \up0 \expndtw0\charscalex100 prepara un recipiente (bao o depsito) que conti
ene una mezcla precipitante-disolvente ms rica en \line \up0 \expndtw0\charscalex
100 precipitante (5-10%) y se coloca todo en una cmara de cristalizacin cerrndola h
ermticamente. Al \line \up0 \expndtw0\charscalex107 aproximarse al equilibrio, si
los porcentajes son correctos, la gota dentro del porta se enriquece \line \up0
\expndtw0\charscalex113 lentamente en precipitante y el producto cristaliza dan
do lugar a monocristales de grandes \line \up0 \expndtw-3\charscalex100 dimensio
nes. \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\sl
mult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\sl
mult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb209\sl-230\
slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 61
}
}}
}
4 Los cristales obtenidos deben ser analizados previamente en una lupa binocular
de luz polarizada. Los \up0 \expndtw-3\charscalex100 criterios para su seleccin
son los siguientes: \par\pard\qj \li1418\ri1217\sb30\sl-413\slmult0 \up0 \expndt
w-3\charscalex100 \ul0\nosupersub\cf6\f7\fs24 \u8226?\ul0\nosupersub\cf3\f4\fs24
que posean una estructura interna uniforme y, por lo tanto, que no corresponda
n a maclas cristalinas \up0 \expndtw-1\charscalex100 o diversos dominios cristal
inos. Los cristales tampoco pueden estar fracturados ni tensionados. En la \up0
\expndtw-1\charscalex100 realidad, sin embargo, los cristales son imperfectos ya
que estn compuestos de pequeas regiones \up0 \expndtw-3\charscalex100 algo desori
entadas que dan lugar al trmino denominado mosaicidad. \par\pard\qj \li1418\ri122
0\sb13\sl-430\slmult0 \up0 \expndtw0\charscalex103 \ul0\nosupersub\cf6\f7\fs24 \
u8226?\ul0\nosupersub\cf3\f4\fs24 que tengan un tamao y una forma apropiados, si
endo la dimensin lateral ptima del orden de \up0 \expndtw-4\charscalex100 0,2-0,4
mm. En todo caso el grosor ptimo debe situarse alrededor de 2/\ul0\nosupersub\cf6
\f7\fs24 \ul0\nosupersub\cf3\f4\fs24 , donde \ul0\nosupersub\cf6\f7\fs24 \ul0\nosu
persub\cf3\f4\fs24 es el coeficiente de \up0 \expndtw-5\charscalex100 absorcin l
ineal. \par\pard\qj \li1418\ri1221\sb403\sl-415\slmult0 \up0 \expndtw-1\charscal
ex100 Una vez obtenido el monocristal y despus de haber comprobado su calidad, se
fija en el extremo de \up0 \expndtw-1\charscalex100 un capilar por medio de un
adhesivo amorfo para no interferir en la difraccin. El soporte consiste de \up0 \
expndtw0\charscalex100 una base de metal (pieza de latn) junto al cual el capilar
(vidrio) est pegado con cera y, en la otra \up0 \expndtw0\charscalex104 extremid
ad, tiene el adhesivo para fijar el monocristal. Una vez montado se coloca en la
cabeza \up0 \expndtw-5\charscalex100 goniomtrica del difractmetro. \par\pard\qj \
li1418\ri1221\sb401\sl-420\slmult0 \up0 \expndtw-4\charscalex100 En este trabajo
se utiliz el mtodo de evaporacin lenta del disolvente y el de difusin de vapor para
la \up0 \expndtw0\charscalex100 obtencin de los monocristales. La recogida de da
tos se realiz con un difractmetro Enraf-Nonius \up0 \expndtw0\charscalex109 CAD4.
El aparato est equipado con un generador Enraf-Nonius modelo FR590D, utiliza un \
up0 \expndtw-4\charscalex100 monocromador de grafito y una radiacin de Cu K\ul0\n
osupersub\cf6\f7\fs24 \u945?\ul0\nosupersub\cf3\f4\fs24 . \par\pard\ql \li1418\s
alex100 3.4.3.2. Recogida de datos \par\pard\qj \li1418\ri1221\sb277\sl-430\slmu
lt0 \up0 \expndtw-2\charscalex100 Los difractmetros utilizan una geometra ecuatori
al en la que el haz difractado se mide siempre en un \up0 \expndtw0\charscalex10
6 plano horizontal definido por el haz incidente y la rotacin del detector alrede
dor de un eje que \up0 \expndtw0\charscalex100 atraviesa el cristal. El detector
slo se mueve en este plano y forma un ngulo de 2\ul0\nosupersub\cf6\f7\fs24 \u952
?\ul0\nosupersub\cf3\f4\fs24 (entre 0-160\ul0\super\cf5\f6\fs23 \ul0\nosupersub\
cf3\f4\fs24 , \up0 \expndtw-1\charscalex100 dentro del rango del instrumento) co

n el haz incidente. El goniostato ms utilizado es el de geometra \up0 \expndtw-2\c
harscalex100 euleriana que da lugar al difractmetro de cuatro crculos con tres rot
aciones para el cristal (\ul0\nosupersub\cf6\f7\fs24 \u969?\ul0\nosupersub\cf3\f
4\fs24 , \ul0\nosupersub\cf6\f7\fs24 \u967?\ul0\nosupersub\cf3\f4\fs24 , \ul0\no
supersub\cf6\f7\fs24 \u981?\ul0\nosupersub\cf3\f4\fs24 ) y \up0 \expndtw0\charsc
alex106 una para el detector (2\ul0\nosupersub\cf6\f7\fs24 \u952?\ul0\nosupersub
\cf3\f4\fs24 ). Segn si \ul0\nosupersub\cf6\f7\fs24 \u967?\ul0\nosupersub\cf3\f4\
fs24 es perpendicular o no a \ul0\nosupersub\cf6\f7\fs24 \u969?\ul0\nosupersub\
cf3\f4\fs24 , el gonimetro se denomina de \up0 \expndtw-3\charscalex100 geometra E
uler o Kappa, respectivamente. \par\pard\qj \li1418\ri1221\sb399\sl-420\slmult0
\up0 \expndtw0\charscalex103 El gonimetro gira y orienta el cristal de forma que
cada familia de planos cumpla la condicin de \line \up0 \expndtw0\charscalex103 d
ifraccin de Bragg. La cabeza goniomtrica, que produce la rotacin \ul0\nosupersub\cf
6\f7\fs24 \u981?\ul0\nosupersub\cf3\f4\fs24 (tipo spin) en el cristal, \par\par
d\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard
\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb207\sl-230\slmult0 \up0 \exp
ndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 62 \par\pard\sect\sectd\fs24\pa
perw11900\paperh16840{\shp
z-10000\shplid30
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5145140051451401ffd9}}}}}\pard\sb0\sl-240{\bkmkstart Pg31}{\bkmkend Pg31}\par\pa
rd\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl-230\slmult0 \par\par
d\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf
1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri1220\sb369\sl-426\slmult0 \u
p0 \expndtw-1\charscalex100 \ul0\nosupersub\cf3\f4\fs24 descansa sobre el bloque
\ul0\nosupersub\cf6\f7\fs24 \u954?\ul0\nosupersub\cf3\f4\fs24 soportado por el
bloque \ul0\nosupersub\cf6\f7\fs24 \u969?\ul0\nosupersub\cf3\f4\fs24 que a su
vez es colineal con 2\ul0\nosupersub\cf6\f7\fs24 \u952?\ul0\nosupersub\cf3\f4\fs
24 . El centro del \up0 \expndtw0\charscalex100 sistema (donde se coloca el cris
tal) y el detector estn en un plano perpendicular al eje \ul0\nosupersub\cf6\f7\f
s24 \u969?\ul0\nosupersub\cf3\f4\fs24 /2\ul0\nosupersub\cf6\f7\fs24 \u952?\ul0\n
osupersub\cf3\f4\fs24 . Para \up0 \expndtw0\charscalex103 evitar la prdida de int
ensidad por la absorcin del aire hay un tnel de helio en el camino del haz \up0 \e
xpndtw-5\charscalex100 difractado (Figura 33). \par\pard\li2448\sb0\sl-230\slmul
t0\par\pard\li2448\sb0\sl-230\slmult0\par\pard\li2448\sb68\sl-230\slmult0\fi0\tx
6680 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf9\f10\fs20 a)\tab \dn2 \expn
dtw0\charscalex100 b)\par\pard\ql \li1871\sb0\sl-230\slmult0 \par\pard\ql\li1871
mult0 \par\pard\ql\li1871\sb118\sl-230\slmult0 \up0 \expndtw-3\charscalex100 Fig
ura 33. a) Esquema del difractmetro CAD4. b) Esquema simplificado de las rotacion
es que mueven el cristal. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\l
i1418\sb256\sl-276\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf3\f4\
fs24 La recogida de un espectro consta de diferentes etapas: \par\pard\ql \li141
8\sb144\sl-276\slmult0 \up0 \expndtw-1\charscalex100 1)\ul0\nosupersub\cf4\f5\fs
24 \ul0\nosupersub\cf3\f4\fs24 Seleccin, montaje y centrado del cristal. \par\p
ard\ql \li1418\ri1219\sb26\sl-420\slmult0\tx1778\tx1778\tx1778\tx1778\tx1778\tx1
778 \up0 \expndtw0\charscalex109 2)\ul0\nosupersub\cf4\f5\fs24 \ul0\nosupersub\
cf3\f4\fs24 Determinacin de la celda unidad. A partir de la rotacin en el ngulo \u
l0\nosupersub\cf6\f7\fs24 \u981?\ul0\nosupersub\cf3\f4\fs24 y registrando las \
line\tab \up0 \expndtw0\charscalex109 difracciones sobre un film Polaroid\ul0\su
per\cf10\f11\fs23 \u-2342?\ul0\nosupersub\cf3\f4\fs24 o buscndolas aleatoriament
e en un rango de \ul0\nosupersub\cf6\f7\fs24 \u952?\ul0\nosupersub\cf3\f4\fs24 ,
se \line \tab \up0 \expndtw-3\charscalex100 encuentran \up0 \expndtw0\charscale
x107 25 reflexiones a partir de las cuales se selecciona automticamente una celda
\line \tab \up0 \expndtw-1\charscalex100 compatible con el espacio recproco estu

diado. Se definen dos matrices: la matriz de orientacin, \line \tab \up0 \expndtw
-3\charscalex100 que relaciona las dimensiones de la celda y su orientacin respec
to al sistema de coordenadas del \line \tab \up0 \expndtw-1\charscalex100 difrac
tmetro, y la matriz mtrica recproca que informa de las dimensiones y simetra de la c
elda \line \tab \up0 \expndtw-2\charscalex100 recproca. \par\pard\ql \li1418\ri12
19\sb20\sl-420\slmult0\tx1778\tx1778 \up0 \expndtw-3\charscalex100 3)\ul0\nosupe
rsub\cf4\f5\fs24 \ul0\nosupersub\cf3\f4\fs24 Estudio de la calidad del cristal
a partir del diagrama \ul0\nosupersub\cf6\f7\fs24 \u969?\ul0\nosupersub\cf3\f4\
fs24 /\ul0\nosupersub\cf6\f7\fs24 \u952?\ul0\nosupersub\cf3\f4\fs24 . Permite ve
r si el cristal est tensionado o \line\tab \up0 \expndtw-3\charscalex100 si es mo
saico. Se determinan los parmetros de recogida del espectro de difraccin que depen
den \line \tab \up0 \expndtw-4\charscalex100 del tamao, dimensiones de la celda y
calidad del cristal. \par\pard\ql \li1418\ri1220\sb0\sl-426\slmult0\tx1778\tx17
78\tx1778 \up0 \expndtw-3\charscalex100 4)\ul0\nosupersub\cf4\f5\fs24 \ul0\nosu
persub\cf3\f4\fs24 Recogida del espectro. La medida de las intensidades difract
adas se realiza hasta un valor mximo \line\tab \up0 \expndtw-2\charscalex100 de 2
\ul0\nosupersub\cf6\f7\fs24 \u952?\ul0\nosupersub\cf3\f4\fs24 , habiendo determi
nado previamente la zona del espacio recproco a investigar a partir de la \line \
tab \up0 \expndtw0\charscalex105 celda hallada. Durante el proceso de recogida s
e mide peridicamente la intensidad de tres \line \tab \up0 \expndtw-2\charscalex1
00 reflexiones para controlar que el cristal no se ha descentrado ni ha sido daad
o por la radiacin. \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\
sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\
sb0\sl-230\slmult0 \par\pard\ql\li10287\sb12\sl-230\slmult0 \up0 \expndtw-4\char
scalex100 \ul0\nosupersub\cf1\f2\fs20 63 \par\pard\sect\sectd\fs24\paperw11900\p
aperh16840\pard\sb0\sl-240{\bkmkstart Pg32}{\bkmkend Pg32}\par\pard\ql \li1418\s
0\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Mater
iales y mtodos \par\pard\ql \li1418\ri1221\sb382\sl-410\slmult0\tx1778\tx1778 \up
0 \expndtw0\charscalex106 \ul0\nosupersub\cf3\f4\fs24 5)\ul0\nosupersub\cf4\f5\f
s24 \ul0\nosupersub\cf3\f4\fs24 Reduccin de datos. Con las intensidades obtenid
as se procede al clculo de los factores de \line\tab \up0 \expndtw0\charscalex102
estructura observados, |F(hkl)|\ul0\sub\cf5\f6\fs24 o\ul0\nosupersub\cf3\f4\fs2
4 . Se aplican las correcciones de Lorentz y polarizacin y, si fuera \line \tab \
up0 \expndtw-3\charscalex100 necesario, las de absorcin o decaimiento. \par\pard\
ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb245\sl-276\slmult0 \up0 \exp
ndtw0\charscalex104 3.4.3.3. Resolucin y refinamiento de la estructura \par\pard\
qj \li1418\sb0\sl-411\slmult0 \par\pard\qj\li1418\ri1219\sb42\sl-411\slmult0 \up
0 \expndtw0\charscalex100 Los mtodos estructurales de resolucin se pueden dividir
en dos tipos segn la estrategia que siguen \line \up0 \expndtw0\charscalex105 par
a resolver el problema de la fase, as tenemos los mtodos directos e indirectos. Lo
s mtodos \line \up0 \expndtw0\charscalex100 indirectos se basan en la localizacin
de un tomo pesado en la estructura sin tener un conocimiento \line \up0 \expndtw2\charscalex100 previo de las fases. Por otro lado, los mtodos directos acceden d
irectamente a las fases a partir de las \line \up0 \expndtw0\charscalex107 inten
sidades de los haces difractados, no siendo necesario tener informacin estructura
l previa. \line \up0 \expndtw-2\charscalex100 Suponen la asignacin de una fase pr
obable a un cierto nmero de factores de estructura. Son ptimos \line \up0 \expndtw
0\charscalex111 en el caso de compuestos con tomos de nmero atmico parecido, como e
s el caso de los \line \up0 \expndtw-3\charscalex100 compuestos orgnicos. \par\pa
rd\qj \li1418\ri1220\sb402\sl-420\slmult0 \up0 \expndtw-2\charscalex100 La base
del desarrollo de los mtodos directos estriba en las caractersticas de la funcin de
densidad \up0 \expndtw0\charscalex102 electrnica: real, positiva y continua en t
oda la celda. Esta se localiza en zonas aproximadamente \up0 \expndtw-2\charscal
ex100 esfricas conocidas como tomos que deben estar situados a determinadas distan
cias y ngulos para \up0 \expndtw0\charscalex102 formar molculas qumicamente razonab
les, lo que restringe mucho las posibilidades. El problema \up0 \expndtw-2\chars
calex100 estructural se plantea desde un punto de vista ms prctico admitiendo el p
rincipio de aditividad de la \up0 \expndtw-3\charscalex100 densidad electrnica. E
l objetivo no es una descripcin exhaustiva de la densidad electrnica \ul0\nosupers

ub\cf6\f7\fs24 \u961?\ul0\nosupersub\cf3\f4\fs24 (x, y, z) \up0 \expndtw-4\char
scalex100 en toda la celda, sino la localizacin de sus mximos. \par\pard\qj \li141
8\ri1221\sb407\sl-412\slmult0 \up0 \expndtw-2\charscalex100 Como hay muchos ms da
tos que parmetros no todos los factores de estructura son independientes \up0 \ex
pndtw-4\charscalex100 por lo que deben existir relaciones de algn tipo en las que
estn implicadas sus amplitudes y fases. En \up0 \expndtw0\charscalex100 primer l
ugar, la resolucin por mtodos directos implica la formulacin de relaciones de fases
en las \up0 \expndtw-1\charscalex100 que participen varios factores de estructu
ra. stas deben ser independientes a la eleccin del origen. \up0 \expndtw-3\charsca
lex100 Las relaciones expresan la probabilidad de que una fase tenga un determin
ado valor, calculado a partir \up0 \expndtw0\charscalex103 de los valores de la
amplitud escogidos. Luego, hay que fijar el origen de la celda para eliminar la
\up0 \expndtw-2\charscalex100 indeterminacin de las fases a l ligadas, y as pasar d
e relaciones de fases a conjuntos probables de \up0 \expndtw0\charscalex102 fase
s. La eleccin del origen no es totalmente arbitraria, intentndose que coincida con
uno o ms \up0 \expndtw-5\charscalex100 elementos de simetra presentes en la celda
. \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0
up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 64 \par\pard\sect\sectd
\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg33}{\bkmkend Pg33}\pa
r\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl-230\slmult0 \par
\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersu
b\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri1221\sb382\sl-410\slmult
0 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf3\f4\fs24 Existen diferentes es
trategias para abordar el problema de la asignacin de las fases a los factores de
\up0 \expndtw0\charscalex106 estructura. Los mtodos de multisolucin son los ms uti
lizados en la aplicacin de los mtodos \up0 \expndtw0\charscalex103 directos, pues
en ellos se basa el programa SHELXS-97\ul0\super\cf5\f6\fs23 92\ul0\nosupersub\c
f3\f4\fs24 con el que se ha trabajado. El programa \up0 \expndtw0\charscalex105
trata de obtener una solucin estructural mltiple, mediante varios conjuntos de fa
ses, uno de los \up0 \expndtw-3\charscalex100 cuales debe corresponder a la solu
cin correcta. \par\pard\qj \li1418\sb0\sl-416\slmult0 \par\pard\qj\li1418\ri1228\
sb10\sl-416\slmult0 \up0 \expndtw0\charscalex100 Una vez resuelto el problema de
fases, se dispone de un conjunto de parmetros que especifican la \line \up0 \exp
ndtw0\charscalex102 situacin de cada tomo dentro de la celda unidad. Como las fase
s obtenidas en la resolucin son \line \up0 \expndtw0\charscalex100 aproximadas, p
ues sta se efecta con un nmero selecto de reflexiones, es necesario efectuar un \li
ne \up0 \expndtw0\charscalex102 proceso de refinamiento de los valores obtenidos
. Los mtodos de refinamiento son dos: series de \line \up0 \expndtw0\charscalex10
4 Fourier sucesivas y mnimos cuadrados. En el primero, se realiza una sntesis de F
ourier con los \line \up0 \expndtw0\charscalex107 |F(hkl)|\ul0\sub\cf5\f6\fs24 o
\ul0\nosupersub\cf3\f4\fs24 a los que se les asigna la fase que se deduce de lo
s F(hkl)\ul0\sub\cf5\f6\fs24 c\ul0\nosupersub\cf3\f4\fs24 calculados a partir d
e las \line \up0 \expndtw-2\charscalex100 coordenadas de que se dispone. En el s
egundo caso, se minimiza por mnimos cuadrados el factor de \line \up0 \expndtw-2\
charscalex100 estructura observado y el calculado a partir de las coordenadas y
los coeficientes de agitacin trmica \line \up0 \expndtw0\charscalex103 que se disp
onen de la estructura. La funcin es del tipo R\ul0\sub\cf5\f6\fs24 w\ul0\nosupers
ub\cf3\f4\fs24 = \ul0\nosupersub\cf6\f7\fs24 \u8721?\ul0\nosupersub\cf3\f4\fs24
w\ul0\sub\cf5\f6\fs24 hkl\ul0\nosupersub\cf3\f4\fs24 [F(hkl)\ul0\sub\cf5\f6\f
s24 o\ul0\nosupersub\cf3\f4\fs24 - F(hkl)\ul0\sub\cf5\f6\fs24 c\ul0\nosupersub\
cf3\f4\fs24 ]\ul0\super\cf5\f6\fs23 2\ul0\nosupersub\cf3\f4\fs24 en la que el \
line \up0 \expndtw-1\charscalex100 coeficiente w\ul0\sub\cf5\f6\fs24 hk\ul0\nosu
persub\cf3\f4\fs24 expresa el peso que se atribuye a F(hkl)\ul0\sub\cf5\f6\fs24
o\ul0\nosupersub\cf3\f4\fs24 y corresponde al inverso del cuadrado de la \line
\up0 \expndtw-2\charscalex100 desviacin estndar de su correspondiente medida \up0
\expndtw-4\charscalex100 (w\ul0\sub\cf5\f6\fs24 hkl \up0 \expndtw-2\charscalex1
00 \ul0\nosupersub\cf3\f4\fs24 = 1/\ul0\nosupersub\cf6\f7\fs24 \u963?\ul0\super\
cf5\f6\fs23 2hkl\ul0\nosupersub\cf3\f4\fs24 ). De esta forma se da ms \par\pard\q

l \li1418\sb140\sl-276\slmult0 \up0 \expndtw-3\charscalex100 importancia a las r
eflexiones de menor desviacin estndar. \par\pard\qj \li1418\sb0\sl-411\slmult0 \pa
r\pard\qj\li1418\ri1221\sb22\sl-411\slmult0 \up0 \expndtw0\charscalex106 Con el
mtodo de mnimos cuadrados el programa SHELXL-97\ul0\super\cf5\f6\fs23 92\u
l0\nosupersub\cf3\f4\fs24 ajusta los parmetros \line \up0 \expndtw-1\charscal
ex100 (coordenadas, factores de escala, factores de ocupacin, factores de tempera
tura) para obtener una \line \up0 \expndtw0\charscalex100 mejor concordancia ent
re los F(hkl) observados y calculados que se cuantifica mediante el ndice de \lin
e \up0 \expndtw-2\charscalex100 acuerdo, R. Este mtodo permite calcular las desvi
aciones estndar de los parmetros atmicos, que \line \up0 \expndtw-2\charscalex100 s
e emplean en determinar las incertidumbres en las longitudes y ngulos de enlace.
Todo proceso de \line \up0 \expndtw-1\charscalex100 afinamiento se acompaa con un
a sntesis de diferencias, cuya finalidad es determinar la posicin de \line \up0 \e
xpndtw-2\charscalex100 los tomos que no se afinan y de aquellos que no se han loc
alizado (tomos de bajo nmero atmico, \line \up0 \expndtw-3\charscalex100 como el hi
drgeno). \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb0\sl-276\s
lmult0 \par\pard\ql\li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb113\sl-276\s
lmult0 \up0 \expndtw-3\charscalex100 3.5. CLCULOS COMPUTACIONALES Y MODELADO MOLE
CULAR \par\pard\qj \li1418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri1221\sb44\sl
-410\slmult0 \up0 \expndtw0\charscalex108 La qumica terica proporciona un amplio r
ango de metodologas para el estudio de sistemas \up0 \expndtw0\charscalex107 poli
mricos. Bsicamente, stas pueden ser clasificadas en dos grandes grupos: los mtodos \
up0 \expndtw0\charscalex103 cunticos y los mtodos clsicos. \par\pard\ql \li10287\sb
0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb
39\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 65 \
par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg34
}{\bkmkend Pg34}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\
sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmult0 \up0 \expndtw-2\charscale
x100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\sb0\sl414\slmult0 \par\pard\qj\li1418\ri1218\sb364\sl-414\slmult0 \up0 \expndtw0\chars
calex100 \ul0\nosupersub\cf3\f4\fs24 Los primeros realizan una descripcin del sis
tema basada en el formalismo de la mecnica cuntica. \line \up0 \expndtw0\charscale
x105 Se caracterizan por su rigurosidad en resolver la ecuacin de Schrdinger por m
edio de mtodos \line \up0 \expndtw-2\charscalex100 ab initio o semiempricos para u
na molcula o sistema molecular. Una vez conocida la funcin de onda, \line \up0 \ex
pndtw0\charscalex105 todas las propiedades fisicoqumicas de la molcula pueden ser
determinadas fcilmente. As, se \line \up0 \expndtw0\charscalex100 puede determinar
no solo la energa molecular sino otras propiedades que pueden estar directamente
\line \up0 \expndtw0\charscalex107 relacionadas con las caractersticas estructur
ales de las molculas. Pero el uso de la mecnica \line \up0 \expndtw0\charscalex107
cuntica en el anlisis conformacional est limitado a sistemas de tamao reducido debi
do a su \line \up0 \expndtw-3\charscalex100 elevado coste computacional. \par\pa
rd\qj \li1418\ri1220\sb408\sl-412\slmult0 \up0 \expndtw0\charscalex102 Los mtodos
clsicos, en cambio, utilizan un formalismo basado en la mecnica clsica que permite
\line \up0 \expndtw0\charscalex100 aplicar los estudios tericos a sistemas de gr
an tamao con un coste computacional reducido. Dentro \line \up0 \expndtw0\charsca
lex107 de la mecnica molecular, la energa de un sistema qumico se evala a travs de ex
presiones \line \up0 \expndtw0\charscalex104 analticas clsicas y de parmetros ajust
ados que incorporan de forma promediada la informacin \line \up0 \expndtw0\charsc
alex100 electrnica. El conjunto de expresiones y parmetros utilizados constituye l
o que se denomina campo \line \up0 \expndtw-3\charscalex100 de fuerza. \par\pard
\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1222\sb15\sl-413\slmult0 \u
p0 \expndtw0\charscalex109 Los parmetros de un determinado campo de fuerza estn op
timizados para poder reproducir \up0 \expndtw0\charscalex102 resultados experime
ntales o clculos mecanicocunticos para un determinado colectivo de sistemas \up0 \
expndtw0\charscalex100 qumicos. As, por ejemplo, hay campos de fuerzas diseados par
a estudiar polipptidos y protenas, \up0 \expndtw-2\charscalex100 otros para estudi
ar cidos nucleicos, otros para estudiar compuestos orgnicos, etc. \par\pard\qj \li
1418\ri1221\sb404\sl-417\slmult0 \up0 \expndtw0\charscalex104 Para describir la
estructura cristalina de un polmero, habra que determinar diversos parmetros \line

\up0 \expndtw-4\charscalex100 intramoleculares (posicin de los tomos en cada caden
a) e intermoleculares (posicin y orientacin de \line \up0 \expndtw0\charscalex102
las cadenas). Normalmente, su estudio se lleva a cabo en dos pasos. En primer lu
gar, se busca la \line \up0 \expndtw-3\charscalex100 conformacin de una cadena ai
slada. Una vez obtenida la conformacin molecular para una cadena se \line \up0 \e
xpndtw0\charscalex110 genera el empaquetamiento cristalino a partir de sta y en f
uncin de la simetra del cristal. \line \up0 \expndtw0\charscalex103 Presuponiendo
que como punto de partida se conocen experimentalmente las dimensiones de la \li
ne \up0 \expndtw-1\charscalex100 celdilla unitaria (a, b, c, \ul0\nosupersub\cf6
\f7\fs24 \u945?\ul0\nosupersub\cf3\f4\fs24 , \ul0\nosupersub\cf6\f7\fs24 \u946?\
ul0\nosupersub\cf3\f4\fs24 , \ul0\nosupersub\cf6\f7\fs24 \u947?\ul0\nosupersub\c
f3\f4\fs24 ) se deben optimizar las posiciones relativas de las diferentes caden
as \line \up0 \expndtw-1\charscalex100 dentro de la celdilla (desplazamiento de
las cadenas respecto a los ejes cristalogrficos y orientacin \line \up0 \expndtw-1
\charscalex100 azimutal). Esta aproximacin se ha demostrado vlida para muchos sist
emas polimricos.\ul0\super\cf5\f6\fs23 93 \par\pard\ql \li1418\sb0\sl-230\slmult0
r\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\
pard\ql\li1418\sb148\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosupersu
b\cf1\f2\fs20 66 \par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-2
40{\bkmkstart Pg35}{\bkmkend Pg35}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\p
ard\ql\li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \e
xpndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\
ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb216\sl-276\slmult0 \up0 \exp
ndtw0\charscalex100 \ul0\nosupersub\cf3\f4\fs24 3.5.1. El programa PCSP. \par\pa
rd\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1220\sb18\sl-413\slmult0
\up0 \expndtw0\charscalex102 Dentro de los mtodos usados para estudiar el empaque
tamiento cristalino en la presente memoria, \line \up0 \expndtw0\charscalex100 d
estaca el programa PCSP (Prediction of the Crystal Structure of Polymers).\ul0\s
uper\cf5\f6\fs23 94 \ul0\nosupersub\cf3\f4\fs24 Este es especialmente \line \up0
\expndtw0\charscalex100 til debido a su simplicidad y, al mismo tiempo, a su gra
n eficiencia. Partiendo de un modelo de varilla \line \up0 \expndtw-1\charscalex
100 rgida, es decir, sin optimizar la geometra molecular de las cadenas del polmero
, permite obtener una \line \up0 \expndtw-1\charscalex100 rpida y precisa estimac
in de la energa asociada a un determinado empaquetamiento cristalino. Esta \line \
up0 \expndtw0\charscalex104 metodologa ha sido de gran utilidad para la determina
cin de la estructura cristalina de diferentes \line \up0 \expndtw-2\charscalex100
familias de poliamidas alifticas estudiadas en el Departamiento de Ingeniera Qumic
a de la UPC.\ul0\super\cf5\f6\fs23 95 \par\pard\ql \li1418\sb0\sl-276\slmult0 \
par\pard\ql\li1418\sb245\sl-276\slmult0 \up0 \expndtw0\charscalex102 \ul0\nosupe
rsub\cf3\f4\fs24 3.5.2. El programa Cerius. \par\pard\qj \li1418\sb0\sl-406\slmu
lt0 \par\pard\qj\li1418\ri1221\sb51\sl-406\slmult0 \up0 \expndtw0\charscalex110
El programa Cerius\ul0\super\cf5\f6\fs23 96\ul0\nosupersub\cf3\f4\fs24 se emple
a en la simulacin de diagramas de difraccin de rayos X y de \up0 \expndtw-1\charsc
alex100 electrones. Se trata de una herramienta computacional que permite llevar
a cabo diversas aplicaciones \up0 \expndtw0\charscalex100 adems de la simulacin d
e la difraccin, siendo muy til para el estudio de compuestos qumicos, en \up0 \expn
dtw-3\charscalex100 particular de polmeros cristalinos. \par\pard\qj \li1418\sb0\
rscalex102 El programa consta de diferentes mdulos que permiten al usuario realiz
ar numerosas operaciones. \up0 \expndtw0\charscalex106 Tales operaciones se llev
an a cabo de forma interactiva, facilitando la labor del usuario, y son de \up0
\expndtw0\charscalex104 naturaleza muy diversa, abarcando desde la visualizacin y
construccin de modelos moleculares \up0 \expndtw-3\charscalex100 hasta la simula
cin de diferentes propiedades. \par\pard\qj \li1418\ri1220\sb406\sl-415\slmult0 \
up0 \expndtw-2\charscalex100 La generacin de las estructuras se realiza a partir
de coordenadas previamente existentes, o mediante \up0 \expndtw-2\charscalex100
las propias herramientas de que dispone el programa. La generacin de un empaqueta
miento cristalino \up0 \expndtw-2\charscalex100 es una de las herramientas ms pot

entes del programa Cerius, permite generar la celdilla a partir de los \up0 \exp
ndtw-1\charscalex100 parmetros de red, incluyendo la posibilidad de especificar e
l grupo espacial. De esta forma, es posible \up0 \expndtw-2\charscalex100 constr
uir la estructura cristalina a partir de su unidad asimtrica. \par\pard\qj \li141
8\ri1219\sb407\sl-413\slmult0 \up0 \expndtw0\charscalex100 El mdulo proporciona d
e forma rpida y muy verstil el patrn de difraccin para un modelo cristalino \up0 \ex
pndtw0\charscalex103 determinado, pudiendo considerarse tres tipos de radiacione
s: rayos X, electrones y neutrones; as \up0 \expndtw-1\charscalex100 como tres ti
pos de diagramas: polvo, fibra y monocristal. Para las reflexiones obtenidas se
calculan los \up0 \expndtw-3\charscalex100 correspondientes espaciados e intensi
dades. \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\
slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\
slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb229\sl-23
0\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 67 \par\pard
\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg36}{\bkmke
nd Pg36}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\s
lmult0 \par\pard\ql\li1418\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul
0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri1220\sb381\sl
-411\slmult0 \up0 \expndtw0\charscalex111 \ul0\nosupersub\cf3\f4\fs24 El mdulo de
difraccin presenta como ventajas la posibilidad de comparar directamente las \up
0 \expndtw0\charscalex100 intensidades calculadas y experimentales, al incluir e
n aqullas diferentes correcciones. Adems, su \up0 \expndtw0\charscalex103 naturale
za interactiva agiliza el estudio del efecto de los cambios estructurales sobre
el patrn. Ello \up0 \expndtw0\charscalex105 permite llevar a cabo el refinamiento
de una estructura de forma iterativa (prueba y ajuste), hasta \up0 \expndtw0\ch
arscalex100 conseguir una concordancia aceptable entre la simulacin y los datos e
xperimentales. Los ajustes se \up0 \expndtw0\charscalex100 basan fundamentalment
e en los cambios de la conformacin molecular, los movimientos de rotacin y \up0 \e
xpndtw0\charscalex100 translacin de las molculas en el interior del cristal y en e
l clculo de la energa de empaquetamiento \up0 \expndtw-3\charscalex100 considerand
o las diferentes contribuciones energticas. \par\pard\ql \li1418\sb0\sl-276\slmul
\par\pard\ql\li1418\sb113\sl-276\slmult0 \up0 \expndtw-2\charscalex100 3.6. PRO
PIEDADES \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb0\sl-276\
slmult0 \par\pard\ql\li1418\sb12\sl-276\slmult0 \up0 \expndtw0\charscalex102 3.6
.1. Propiedades mecnicas \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1
418\ri1219\sb18\sl-413\slmult0 \up0 \expndtw0\charscalex100 Los ensayos de tracc
in-deformacin permiten evaluar la capacidad del material para soportar cargas \up0
\expndtw0\charscalex100 y deformarse cuando se le somete a una tensin. Estos ens
ayos son habituales en la caracterizacin \up0 \expndtw0\charscalex102 del comport
amiento de los materiales frente a un esfuerzo mecnico. La geometra de la muestra,
la \up0 \expndtw0\charscalex103 temperatura y la velocidad de deformacin son fac
tores que han de controlarse rigurosamente para \up0 \expndtw0\charscalex104 obt
ener resultados reproducibles. Normalmente, los ensayos de traccin-deformacin a ve
locidad \up0 \expndtw-1\charscalex100 constante se utilizan en la comparacin de p
roductos similares o en la evaluacin del efecto producido \up0 \expndtw-3\charsca
lex100 por un cambio en las condiciones de produccin del material. \par\pard\qj \
li1418\ri1220\sb402\sl-420\slmult0 \up0 \expndtw0\charscalex103 En el caso de lo
s materiales viscoelsticos, como los polmeros, la resistencia a la deformacin a \li
ne \up0 \expndtw0\charscalex103 velocidad constante posee una componente elstica
que corresponde a una deformacin lineal y \line \up0 \expndtw-1\charscalex100 rec
uperable ante un esfuerzo (ley de Hooke, \ul0\nosupersub\cf6\f7\fs24 \u963?\ul0\
nosupersub\cf3\f4\fs24 = E\ul0\nosupersub\cf6\f7\fs24 \u947?\ul0\nosupersub\cf3
\f4\fs24 ). A medida que aumenta el esfuerzo, el material \line \up0 \expndtw0\c
harscalex109 responde con una componente viscosa que corresponde a una deformacin
que deja de ser \line \up0 \expndtw-3\charscalex100 recuperable. \par\pard\qj \
li1418\ri1221\sb400\sl-420\slmult0 \up0 \expndtw-1\charscalex100 Los ensayos de
traccin-deformacin se realizaron en un minitensimetro Miniature-Materials Tester \l
ine \up0 \expndtw0\charscalex109 (Minimat Instrument) de Polymer Laboratories a
temperatura ambiente y a una velocidad de \line \up0 \expndtw0\charscalex102 est

iramiento constante de 0.8 mm/min. La distancia de sujecin entre mordazas fue de
10 mm. Se \line \up0 \expndtw-3\charscalex100 cortaron probetas de forma rectang
ular (3 x 30 mm\ul0\super\cf5\f6\fs23 2\ul0\nosupersub\cf3\f4\fs24 ) a partir de
films de 200 \ul0\nosupersub\cf6\f7\fs24 \ul0\nosupersub\cf3\f4\fs24 m de espeso
r obtenidos \line \up0 \expndtw-1\charscalex100 por compresin trmica del polmero a
una temperatura 10\ul0\super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C inferior a
su temperatura de fusin. Los \line \up0 \expndtw-1\charscalex100 parmetros que se
determinaran en los ensayos fueron el mdulo de Young (E, en MPa), la tensin \par\
ard\ql\li1418\sb37\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosupersub\
cf1\f2\fs20 68 \par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240
{\bkmkstart Pg37}{\bkmkend Pg37}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\par
d\ql\li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \exp
ndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj
\li1418\ri1221\sb374\sl-420\slmult0 \up0 \expndtw0\charscalex103 \ul0\nosupersu
b\cf3\f4\fs24 mxima alcanzada (\ul0\nosupersub\cf6\f7\fs24 \u949?\ul0\nosupersub\
cf3\f4\fs24 , en MPa) y la deformacin a rotura (\ul0\nosupersub\cf6\f7\fs24 \u964
?\ul0\nosupersub\cf3\f4\fs24 , en %). Se realizaron 10 ensayos por \up0 \expndtw
0\charscalex100 muestra y los resultados se utilizaron con fines comparativos en
tre las poliesteramidas de diferentes \up0 \expndtw-5\charscalex100 composicione
s de grupos ster y amida. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li
1418\sb263\sl-276\slmult0 \up0 \expndtw0\charscalex100 3.6.2. Degradacin \par\par
d\qj \li1418\sb0\sl-415\slmult0 \par\pard\qj\li1418\ri1221\sb15\sl-415\slmult0 \
up0 \expndtw0\charscalex106 Los ensayos de degradacin in vitro de los polmeros pue
den realizarse mediante degradacin \line \up0 \expndtw0\charscalex106 hidroltica
o mediante biodegradacin con sistemas biolgicos. La degradacin hidroltica \l
ine \up0 \expndtw0\charscalex104 generalmente es muy lenta y requiere tiempos de
incubacin largos para observar cambios. Los \line \up0 \expndtw-1\charscalex100
ensayos de degradacin hidroltica se llevaron a cabo con muestras en forma de films
(dimensiones: \line \up0 \expndtw0\charscalex105 15 x 15 mm\ul0\super\cf5\f6\fs
23 2\ul0\nosupersub\cf3\f4\fs24 , espesor: 200 \ul0\nosupersub\cf6\f7\fs24 \ul0\n
osupersub\cf3\f4\fs24 m) que se prepararon por prensado trmico a partir de 200 mg
del \line \up0 \expndtw-2\charscalex100 polmero en forma de polvo. De esta forma
, las placas se incubaron en 30 mL de una solucin tampn \line \up0 \expndtw0\chars
calex103 a pH 7.4 (Na\ul0\sub\cf5\f6\fs24 2\ul0\nosupersub\cf3\f4\fs24 HPO\ul0\s
ub\cf5\f6\fs24 4\ul0\nosupersub\cf3\f4\fs24 /KH\ul0\sub\cf5\f6\fs24 2\ul0\nosupe
rsub\cf3\f4\fs24 PO\ul0\sub\cf5\f6\fs24 4\ul0\nosupersub\cf3\f4\fs24 0.1 M) y t
emperatura de 37\ul0\super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C. La hidrlisis
tambin fue estudiada en \line \up0 \expndtw-3\charscalex100 condiciones acelerad
as, por ejemplo, a 55\ul0\super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C y a 70\
ul0\super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C en agua desionizada. El segui
miento del proceso \line \up0 \expndtw0\charscalex107 degradativo se evalu basndos
e en la prdida de peso del material y en la disminucin de la \line \up0 \expndtw-3
\charscalex100 viscosidad intrnseca. Los cambios en la estructura qumica de los po
lmeros degradados se evaluaron \line \up0 \expndtw-4\charscalex100 mediante espec
troscopa de FT-IR y \ul0\super\cf5\f6\fs23 1\ul0\nosupersub\cf3\f4\fs24 H-RMN par
a identificar los enlaces lbiles. Se analizaron tambin \line \up0 \expndtw0\charsc
alex100 las modificaciones que ocurren en la superficie de la muestra por micros
copa electrnica de barrido \line \up0 \expndtw-5\charscalex100 (SEM). \par\pard\qj
\expndtw0\charscalex107 A diferencia de la degradacin hidroltica, la degradacin enz
imtica ocurre superficialmente y \line \up0 \expndtw0\charscalex102 generalmente
es ms rpida.\ul0\super\cf5\f6\fs23 97\ul0\nosupersub\cf3\f4\fs24 Los ensayos de b
iodegradacin se realizaron con enzimas del tipo \line \up0 \expndtw-3\charscalex1
00 proteasa como son papana y proteinasa K, y estearasa como son las lipasas. Las
dos primeras fueron \line \up0 \expndtw0\charscalex106 selecionadas por su efic
acia demostrada en trabajos anteriores\ul0\super\cf5\f6\fs23 45\ul0\nosupersub\c
f3\f4\fs24 con polmeros que contienen \line \up0 \expndtw0\charscalex100 aminocid
os como glicina y L-alanina. De esta manera, las poliesteramidas que contienen g
licina se \line \up0 \expndtw0\charscalex106 degradan ms rpidamente en papana, mien

tras que las que contienen L-alanina lo hacen en \line \up0 \expndtw0\charscalex
103 proteinasa K. La papana presenta una especificidad bastante amplia sobre el e
nlace peptdico,\ul0\super\cf5\f6\fs23 98 \line \up0 \expndtw-3\charscalex100 \ul0
\nosupersub\cf3\f4\fs24 siendo adems capaz de hidrolizar enlaces steres.\ul0\super
\cf5\f6\fs23 99\ul0\nosupersub\cf3\f4\fs24 Las lipasas se utilizaron especficame
nte para la \line \up0 \expndtw0\charscalex100 degradacin de los polisteres pero t
ambin se han efectuado a efectos comparativos ensayos con \line \up0 \expndtw-3\c
harscalex100 poliesteramidas. \par\pard\qj \li1418\sb0\sl-410\slmult0 \par\pard\
qj\li1418\ri1221\sb20\sl-410\slmult0 \up0 \expndtw0\charscalex103 La incubacin de
las muestras de polmero tiene lugar en una solucin de tampn fosfato 0.05 M \line \
up0 \expndtw-2\charscalex100 (10 mL) que contiene 0.03 % de NaN\ul0\sub\cf5\f6\f
s24 3\ul0\nosupersub\cf3\f4\fs24 a pH 7.4 y 37\ul0\super\cf5\f6\fs23 \ul0\nosupe
rsub\cf3\f4\fs24 C. En el caso de la papana el pH fue de 6.0 y se \line \up0 \exp
ndtw-2\charscalex100 requiri adems la presencia de activadores enzimticos (34 mM de
L-cistena y 30 mM de EDTA). Se \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\par
d\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb39\sl-230\slmult0 \up0 \e
xpndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 69 \par\pard\sect\sectd\fs24\
paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg38}{\bkmkend Pg38}\par\pard
ql\li1418\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\
f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri1221\sb369\sl-426\slmult0 \up0
\expndtw0\charscalex106 \ul0\nosupersub\cf3\f4\fs24 han utilizado muestras en f
orma de films obtenidos por prensado trmico, como en el caso de la \line \up0 \ex
pndtw0\charscalex100 degradacin hidroltica, films preparados por evaporacin lenta (
14 mm de dimetro y 100-150 \ul0\nosupersub\cf6\f7\fs24 \ul0\nosupersub\cf3\f4\fs24
m de \line \up0 \expndtw0\charscalex100 espesor) de una disolucin del polmero en
cloroformo/hexafluoroisopropanol (1/3, v/v); y muestras en \line \up0 \expndtw-2
\charscalex100 polvo (50 mg) pasadas por un tamizador (dimetro inferior a 100 \ul
0\nosupersub\cf6\f7\fs24 \ul0\nosupersub\cf3\f4\fs24 m) para homogeneizar el tamao
\slmult0 \up0 \expndtw0\charscalex108 La solucin enzimtica se renov cada tres das pa
ra mantener durante todo el experimento la \up0 \expndtw-1\charscalex100 activid
ad constante. Al final de la incubacin se inactiv el enzima con 1 mL de HCl 1M y s
e separaron \up0 \expndtw0\charscalex103 las muestras de polmero resultante. La d
egradacin enzimtica del polmero se evalu como en el \up0 \expndtw-1\charscalex100 ca
so de la degradacin hidroltica, sin embargo no se consideraron las medidas de visc
osidad debido a \up0 \expndtw-1\charscalex100 que este tipo de degradacin ocurre n
icamente en la superficie del material. \par\pard\ql \li1418\sb0\sl-230\slmult0
\par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \p
ar\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par
\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\p
ard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\par
d\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\
ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql
\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\l
i1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1
8\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\
sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb
0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\
-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-2
\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\s
ult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmul
r\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb69\sl-230\slmult0 \up0

\expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 70 \par\pard\sect\sectd\fs
24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg39}{\bkmkend Pg39}\par\p
ard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\
pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\
pard\ql\li10287\sb30\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersu
b\cf1\f2\fs20 33 \par\pard\sect\sectd\fs24}

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{\rtf1{\fonttbl

{\f2 Times New Roman;}

ar), 0.4 unidades/mg (Fluka)\par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql

provecha la mayor \up0 \expndtw0\charscalex104 reactividad de los dihaluros de ci

como para precipitar. Disolventes como xileno y tetracloruro de carbono tienden

ensin-deformacin. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb24

de peso molecular conocido, normalmente el promedio en peso \line \up0 \expndtw0

la viscosidad intrnseca, se puede determinar el peso molecular viscosimtrico (M\u

g7}{\bkmkend Pg7}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0

ndas de mayor importancia para los materiales estudiados se resumen a continuacin

tos ncleos atmicos \up0 \expndtw0\charscalex104 con la radiacin electromagntica. nica

teriales polimricos, las transiciones trmicas ms importantes en DSC son la temperat

{\sp{\sn shapeType}{\sv 0}}{\sp{\sn fFlipH}{\sv 0}}{\sp{\sn fFlipV}{\sv 0}}{\sp{

con la energa disipada por el material viscoelstico y que no puede recuperarse. La

ensayos de solubilidad consisten en depositar una pequea cantidad del polmero (1

x7034 \up0 \expndtw-1\charscalex100 Destructiva\tab \up0 \expndtw-1\charscalex10

calex103 Philips EM301 y Philips Tecnai 10/12. El calibrado de los diagramas de

zante de argon. \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\

w0\charscalex100 correspondiente a la radiacin no desviada, mientras que para las

\charscalex104 elctrico, pequeos desajustes del alto voltaje utilizado o de la cor

2}{\bkmkend Pg22}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0

{\sp{\sn pVerticies}{\sv 8;4;(0,20);(2231,20);(2231,0);(0,0)}}

\ql\li10287\sb229\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\c

r que la longitud \line \up0 \expndtw0\charscalex100 promedio de las cadenas. Ad

nica permite obtener el diagrama de difraccin del material y la ordenacin de sus to

en a: \par\pard\ql \li1418\sb0\sl-241\slmult0 \par\pard\ql\li1418\sb0\sl-241\slm

alex100 a la superficie de deposicin. Tambin proporcionan informacin acerca de la i

9}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl-230\slmult0

cf3\f4\fs24 , \up0 \expndtw-1\charscalex100 dentro del rango del instrumento) co

\line \tab \up0 \expndtw-1\charscalex100 compatible con el espacio recproco estu

l objetivo no es una descripcin exhaustiva de la densidad electrnica \ul0\nosupers

cf5\f6\fs23 2hkl\ul0\nosupersub\cf3\f4\fs24 ). De esta forma se da ms \par\pard\q

estructura cristalina de un polmero, habra que determinar diversos parmetros \line

miento cristalino \up0 \expndtw-2\charscalex100 es una de las herramientas ms pot

temperatura ambiente y a una velocidad de \line \up0 \expndtw0\charscalex102 est

licina se \line \up0 \expndtw0\charscalex106 degradan ms rpidamente en papana, mien

r\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb69\sl-230\slmult0 \up0

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