Diagrama de solubilidad Contenido I. RESUMEN.... RESUMEN........... ............. ............. .............. .............. ............. ............. .............. .............. ............. ............. ................. ................................ .........................2 ...2 II. INTROD INTRODUCC UCCIÓN IÓN.... ....... ...... ....... ....... ...... ....... ....... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ........ ......... ......... .......... .......... .......... .......2 ..2 IV. IV. DETAL DETALLES LES EXPERIMENT EXPERIMENTAL ALES..... ES........... ............. .............. .............. ............. ............. .............. ................ .....................6 ............6 V. TABLA TABLA DE DA DAT TOS........... OS................. ............. .............. .............. ............. ............. .............. ............. ............. .............. ..................... ..................8 ....8 VI. TABLA TABLA DE RSULT RSULTADO ADOS...... S............. ............. ............. .............. .............. ............. ............. .............. ............. ................... ..................10 .....10 VII. CÁLCULOS CÁLCULOS Y GRAFICOS.... GRAFICOS........... ............. ............. .............. .............. ............. ............. .......................... ..............................12 ...........12 VIII. VIII. DISCUSI DISCUSIÓN ÓN DE RESUL RESULT TAD ADOS. OS.... ...... ....... ....... ...... ....... ....... ....... ....... ...... ....... ....... ...... ........ .......... .......... .......... ..........14 .....14 IX. CONCLU CONCLUSIO SIONES NES Y RECOME RECOMENDA NDACIO CIONES. NES..... ....... ...... ....... ....... ...... ....... ....... ...... ....... ......... .......... .......... .......15 ..15 X. BIBLIO BIBLIOGRA GRAFA. FA.... ...... ....... ....... ...... ....... ....... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ........1 ....166 XI. AP!NDICE.... AP!NDICE........... ............. ............. .............. ............. ............. .............. .............. ............. ............. .............. .............. ...................... ......................16 .......16
1
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Diagrama de solubilidad
I.
RESUMEN
El objetivo de esta práctica es el de determinar la curva de solubilidad en una mezcla de tres componentes utilizando para ello el diagrama de solubil solubilidad idad triang triangula ularr. Se prepar preparó ó 4 mezclas mezclase e de agua, agua, ácido acético al 10, 1, !0 " !# en volumen " a cada una de ellas se le mezcló con una cantidad de n$butanol %asta observar la turbidez en las mezclas. mezclas. De la misma misma manera se realizó para las 4 soluciones soluciones de ácido acético en n$butanol donde a cada una de ellas se mezcló con agua %asta observar la turbidez en la mezcla. &na vez realizado esto se calculó el # en peso de cada componente de las mezclas. 'uego con una solución de (a)*
≅
1( se tituló gastando un volumen
de 15.4 mL " se calculo el t+tulo ue -ue de 0.0/gml. Enseguida se preparó una solución de !0ml con 10, 4 " 4# en volumen para ácido acético, n$butanol se separó en dos tubos de ensa"o tanto la parte orgánica " acuosa se tituló nuevamente con (a)* gastando para para ca caso so un volu volume men n de /,!m /,!mll " ,m ,ml, l, co con n el valo valorr del del t+tu t+tulo lo calculado se calculó el porcentaje en peso del ácido acético para la -ase orgánica de 11,# " para la -ase acuosa de 2,04#. &na vez %allado matemáticamente estos datos se pudo representar la curva de solubilidad en diagrama triangular " la l+nea de reparto3 conc co nclu lu"e "endo ndo ue ue los los punt puntos os pres presen ente tess en la l+ne l+nea a de so solu lubi bili lida dad d indic ndican an la cant antidad idad de # en peso peso ue ue se encue ncuent ntra ra de ca cada da componente -ormando una sola capa " los puntos debajo de la curva es la part parte e inmi inmisc scib ible le de la me mezc zcla la dond donde e es está tán n pres presen ente tess los los componentes.
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Diagrama de solubilidad
II.
INTRODUCCIÓN
L"# $%&'(')*'"# $+,*$ -#$# /&$$+ "**$#/"+$* ("# 3# *'"# ,'/"# $ #'#,$# $,$*"7+$"# $,$*"7+$"# &+ (9%&'" (9%&'" $+ $%&'(')*'" $%&'(')*'" "+ #& /"*: "# #;('"# #;('"# ,",($+,$ ,",($+,$ #"(&)($# $+ $%&'(')*'" "+ #& -#$ -&+': #"(&'"+$# ('%&'#: $,. E( "/"*,'$+," "/"*,'$+," $ $#,"# #'#,$# $+ $%&'(')*'" $%&'(')*'" #$ $#,&' $#,&' /"* $'" $ *3-'"# %&$ #$ "+"$+ "" '*# $ -#$ #$ "),'$+$+ *-'+" $+ -&+';+ $ *')($# "" /*$#';+: "+$+,*'"+$#: $,. E( ")<$,'" $ $#,$ $=/$*'$+," $# ( "),$+';+ $( '* $ -#$# $( #'#,$ (9%&'" ,$*+*'" &>+>)&,+"(>3'" 7,'" ? +('@* #& "/"*,'$+," $ #"(&)'('.
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Diagrama de solubilidad
III III.
PRI PRINCIP CIPIOS TEÓRIC RICOS
Solubilidad 'a so solu lubi bili lida dad d es una una me medi dida da de la ca capac pacid idad ad de diso disolv lver erse se una una determinada sustancia 5soluto6 en un determinado medio 5solvente63 impl+ impl+cit citame amente nte se corre correspo sponde nde con la má7im má7ima a cantid cantidad ad de sol soluto uto disuelto en una dada cantidad de solvente a una temperatura 8ja " en dic%o cas aso o se establ ablece ue la solución está saturada. Su concentración puede e7presarse en moles por litro, en gramos por litro, o también en porcentaje de soluto 5m5g6100 m'6. El método prepre-eri erido do para para %ace %acerr ue ue el so solu luto to se disu disuel elva va en es esta ta clas clase e de solu so luci cion ones es es ca cale lent ntar ar la mues muestr tra a " en-r en-ria iarr %ast %asta a temp temper erat atur ura a ambiente 5normalmente ! 96. En algunas condiciones la solubilidad se puede sobrepasar de ese má7imo " pasan a denominarse como :soluciones sobresaturadas. Factores que afectan la solubilidad 'a so solu lubi bili lida dad d se de8ne de8ne para para -ase -asess es espe pec+ c+8c 8cas. as. ;or ejem ejempl plo, o, la solubilidad de aragonito " calcita en el agua se espera ue di8eran, si bien ambos son polimor-os de carbonato de calcio " tienen la misma -órmula u+mica. 'a solubilidad de una sustancia en otra está determinada por el euilibrio de -uerzas intermoleculares entre el disolvente " el soluto, " la variación de entrop+a ue acompa
u"en en este euilibrio, cambiando as+ la solubilidad. 'a solubilidad también depende en gran medida de la presencia de otra otrass es espe peci cies es disu disuel elta tass en el diso disolv lven ente te co como mo por por ejem ejempl plo o la ist ia de plejos plejos metáli metáli los l+uid l+uid 'a sol solubi ubilid lidad ad
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Diagrama de solubilidad de las las so solu luci cion ones es.. 'os dos dos ?lti ?ltimo moss e-ec e-ecto toss me menc ncio iona nado doss pued pueden en cuanti8carse utilizando la ecuación de euilibrio de solubilidad. ;ara un sólido ue se disuelve en una reacción redo7, la solubilidad se espera ue dependa de las posibilidades 5dentro del alcance de los potenciales en las ue el sólido se mantiene la -ase termodinámicamente termodinámicamente estable6. ;or ejemplo, la solubilidad del oro en el agua a alta temperatura se observa ue es casi de un orden de magnitud más alta cuando el potencial redo7 se controla mediante un tampón altamente o7idante redo7 =e!)$=e)4 ue con un tampón moderadamente o7idante (i$(i).1 'a solubilidad 5metaestable6 también depende del tama
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Diagrama de solubilidad ejemplo, (a9 a9ll en agua6 e7%iben una solubilidad basta stante independiente de la temperatura. &nos pocos, como el sul-ato de cerio 5FFF6, se vuelven menos solubles en agua a medida ue aumenta la temper temperatur atura. a. Esta Esta depend dependenc encia ia de la temper temperatu atura ra se re8er re8ere e a veces veces como como Gretr Gretrógra ógradaG daG o Gso Gsolub lubili ilidad dad invers inversaG. aG. En ocasio ocasiones nes,, se observa un patrón más complejo, como con sul-ato de sodio, donde el cristal deca%idrato menos soluble pierde agua de cristalización a ! 9 para -ormar una -ase an%idra más solubles. 'a solubilidad de los compuestos orgánicos casi siempre aumenta con la temper temperatu atura. ra. 'a técnic técnica a de la recri recrista staliz lizaci ación, ón, utiliz utilizado ado para la puri puri8 8ca caci ción ón de só sóllidos, dos, depe depend nde e de un so solluto uto de di-e di-errente entess solu so lubi bili lida dade dess en un diso disolv lven ente te ca cali lien ente te " -r+o -r+o.. E7is E7iste ten n algu alguna nass e7cepciones, e7cepciones, tales como determinadas ciclode7trinas.
Sistema de tres comonentes &n sis sistem tema a ternari ternario o puede puede -ácil -ácilmen mente te repr represe esenta ntarse rse me media diante nte un diagrama triangular 58gura adjunta6.9ada vértice representa el 100# del componente representado en dic%o vértice. 'os lados del triángulo repr represe esentan ntan me mezcl zclas as binari binarias as de los compon component entes es situad situados os en los vért vértic ices es e7tre 7tremo mos. s. &n punto punto situ situado ado en el inte interi rior or del del triá triáng ngul ulo o repr repres esen enta ta a una una me mezc zcla la tern ternar aria ia.. ;ara es esta tabl blec ecer er el punt punto o ue ue representa una mezcla de !# de @, !# de H " 0# de 9, podemos proceder del siguiente modoI El punto GaG sobre el lado @H representa el !# de @. Jracemos una l+nea de trazos desde el punto GaG al lado opuest opuesto o del triángu triángulo lo parale paralela la al lado lado H9. H9. Jodas odas las me mezcl zclas as ue contengan !# de @ se %allarán sobre esta l+nea de trazos. El punto GbG del lado @9 representa el0# de 9. Jracemos una l+nea de trazos paralela a @H %asta el lado opuesto del triángulo. Del mismo modo se selecciona un punto de H9 ue represente el !# de H " se traza la l+nea adecuada. 'a intersección de estas tres l+neas se
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Diagrama de solubilidad
I!. I!.
ET"# ET"##E #ES S E$%E E$%ERI RIME MENT NT"# "#ES ES
M"TERI"#ES & RE"CTI!OS aterialesI
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Diagrama de solubilidad > >
Solución de (a)* 1(. =enol-tale+na.
%ROCEDIMIENTO E$%ERIMENT"# Determinación de la curva de solubilidadI &na vez lavados " secados los Erlenme"ers, los tubos " las pipetas se prepara 4 soluciones de 10ml ue contienen 10, 1, !0 " !# en volumen de ácido acético e agua. Se mide la temperatura de cada componente puro. Se titula titula las sol soluci ucione oness con n$buta n$butanol nol,, agitan agitando do consta constante ntemen mente, te, después de cada agregado, %asta la aparición de turbidez. De la misma manera se prepara otras 4 soluciones de 10ml ue contengan 10, !0, 0 " 40# en volumen de ácido acético en n$butanol " se titula las mezclas con agua destilada %asta observar en cada una la turbidez.
Kaloración de solución de (a)* 1(I ;ara determinar el t+tulo de la base con ácido acético se pesa 1 erlenme"er de 100ml con tapón " seco, luego se mide 1ml de ácido acético en el erlenme"er se tapa " se vuelve a pesar " por di-erencia se tiene la masa del ácido acético usado usado.. Ensegu Enseguida ida se titula titula con la base usando usando como indica indicador dor la -enol-tale+na. Determinación de la l+nea de repartoI En la pera de decantación se prepara !0ml de una mezcla ue contenga 10# de ácido acético, 4# de n$butanol " 4# en volumen de agua. Se agita bien la mezcla durante ! minutos apro7imadamente, " luego
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Diagrama de solubilidad
!.
T"'#" DE D"TOS
Condiciones experimentales PRESION (mmHg)
TEMPERT!R("C)
H. R. (#)
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Diagrama de solubilidad
!0#
!#
n$Hutanol @cido @cético @gua n$Hutanol @cido @cético @gua n$Hutanol @cido @cético
.0 1.0 .00 4./0 !.00
0#
/.0 /.!0 !.0
40#
V("*';+ V ("*';+ $ S"(&';+ $ NO
≅
1N
W erlenmeyer +tapón
2:6155
W erleneyer +tap tap ón + C H COOH
:22
W C H COOH
1:6
3
3
V titulado
T9,&(" $ ( )#$ T NaOH =0,099
n$Hutanol @cido @cético @gua n$Hutanol @cido @cético @gua n$Hutanol @cido @cético
g mL
1 :8(
.00 !.00 1!.00 /.00 .00 !0.0 .00 4.00
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Diagrama de solubilidad
( ) W W
=
15,374
C H 3 COOH
F#$ &"# W erlenmeyer +tapón
8:0122
W erleneyer + tapón+ 5mL defaseorgá nica nica
102:0
V titulado ( NaOH )
: L
$+ /$#" $( 3'" 7,'" $+ ( -#$ "*3+'
( ) W W
= 20,057
C H 3 COOH
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Diagrama de solubilidad
!0#
!#
Solución 10#
!0#
@cido @cético @gua n$Hutanol @cido @cético @gua n$Hutanol @cido @cético 9omponen te @gua n$Hutanol @cido @cético @gua n$Hutanol @cido
1.0
1./
1!.12
.00 4./0
/.22 ./2
/.2 !/.
!.00
!.02
1.0
/.0 /.!0
/.42 .1
4/.0 .42
!.0
!.!
K 5m'6
N 5g6
.00 2.00
!.22 /.
1.00
1.0
2.12
.!0 .00
.12 .
/. 4/.!/
! 00
! 02
1./
1.21
1.44
N total 5g6 11.2
1.1
#ON !.0 4.!
1 1
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Diagrama de solubilidad $ VV 4#
7.3467 g
39.89
45
8.9838 g
48.78
10
2.0860 g
11.33
100%
/$#"#
Wtotal= 18.4165g
P* ( -#$ "*3+' → Φ =11.568 P* ( -#$ &"# → θ =9.054
R
H 48.8 11. .8 J
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Diagrama de solubilidad
!II. !II. C(#C C(#CU# U#OS OS & )R"F )R"FIC ICOS OS
A. C(&(" C(&(" $( HKKJ HKKJ $ "/"+$+,$ "/"+$+,$ $ ( #"(&';+. #"(&';+.
A( 10 HVVJ $ ( #"(&';+ ,$+$"# '.
C( C(&( &( "# "# $( $( /$#" /$#" $ $ " "/"+ /"+$+ $+,$ ,$ $ $ ( ( #"(& #"(&' ';+ ;+.. P* $((" +$$#',"# (# $+#'$# H O =0.9982 g / mL 2
n−!utanol =0.8163 g / mL ácido "c#tico =1.0463 g / mL
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Diagrama de solubilidad B. G*-'* G*-'* /&+," /&+," /* /* -"** -"** ( &* &* $ #"(&)'('. #"(&)'('. C. II. II.
C(& (&(" (" $( $( ,9,9,&( ,&(" $ $ ( ( )# )#$ $
T NaOH =
W CH COOH 3
V NaOH . gastado
g 15.4 mL
= 1.0317 =0.067
D. T*@" T*@" $ ( (9+$ (9+$ $ $ *$/*, *$/*," "
A7,'" 7,'" .H#"(&';+ 20 LJ 45 +>B&,+"( : 45 A& ? 10 $ A'" A I
C(&(" $( /$#" "/"+$+,$
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Diagrama de solubilidad
( )
=
( )
=
R
W W
W W
OH
" . "
W OH W Total
=
W " . " W Total
7.3467 g 18.4165 g
=
$ 100 =39.89
2.0860 g 18.4165
g
$ 100 =11.33
H 48.8 11. .8 J
E. P* ( -#$ "*3+' W 1= 4.17 y V NaOH . gastado =7.2 mL→Φ=11.568 P* ( -#$ &"# W 2= 4.81 y V NaOH .gastado =6.5 mL→θ= 9.054
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Diagrama de solubilidad
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Diagrama de solubilidad >
Descartar las primeras gotas de la -ase acuosa " orgánica "a ue en estas estas se presentan presentan una mezcl mezcla a de ambos, " lo ue ue se uiere es %acer los cálculos para cada una de las -ases puras.
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Diagrama de solubilidad E#,$ '* $ -#$# /$*',$ &)'* &+ /&+," "+$ ( '+,$*#$';+ $ $#,# (9+$# /$*',$ $#,)($$* $( /&+," $ $@( " ($';+ ? #9 /"$* $,$*'+* ( /*"/'$ $( ,$*'( ? # "/"+$+,$# %&9'"# $+ -#$ ? &+" $#,3+ #$/*"#. )J D$#*') /*"$#"# %&9'"# +'$( '+,*'(: "+$ ,'$+$ /('';+ ("# *',$*'"# $( '* $ #"(&)'('. E( '* #$ &,'('@ /* /"$* $,$*'+* $( /&+," $ ($';+ $ ( $@( $ ,$*'($#. P* $,$*'+* $( /&+," $ +$&,*('@';+ $+ &+ *$';+ &+" #$ /*"&$+ $#,# +'$( '+,*'(