UNIVERSIDAD PRIVADA NORBERT WIENER
FACULTAD DE FARMACIA Y BIOQUÍMICA E.A.P. de Farmacia y Bioquímica QUÍMICA AALÍTICA E I!TRUMETAL I!T RUMETAL PR"CTICA # $% TEMA& DETERMINACIÓN GRA GR AVIMÉTRICA DE CALCIO EN LECHE
FB4M1 !ecci'(& MAÑANA Tur(o& “B” )ru*o& CUARTO Cic+o& La,ora-orio& 505 Máximo Gervacio Gervac io Vergara C!áve" Doce(-e& I(-era(-e/& 1# Ar"a$a%o Cam$o&' ()%i&&a# *# Barre+o Garc,a' Marie%%a Brigi++e# -# Cam$o& .)/ea' Carme 2/i+!# 4# Ca&+i%%o (im3e"' Mar,a# 5# Caao Rega%a/o' Marie%# # Marav, Coo$)ma' G)ia#
Fec0a de rea+i1aci'( de +a *r2c-ica& .)e&' *6 /e &e+iemre#
*015 ITRODUCCI3
2% aá%i& aá%i&i& i& gravim gravim3+r 3+rico ico e&+á e&+á a&a/ a&a/oo e %a %e /e %a& $ro$or $ro$orcio cioe& e& /e7i /e7ii/a i/a&' &' 8)e e&+a%ece 8)e' e c)a%8)ier com$)e&+o $)ro' %a& $ro$orcioe& e $e&o /e %o& e%eme+o& co& co&+i +i+) +)e+e e+e&& &iem &iem$r $ree &o &o %a& %a& mi&m mi&ma& a&'' e %a .e .e /e %a co& co&i& i&+e +ec cia ia /e %a com$o&ici9' 8)e e&+a%ece 8)e %a& ma&a& /e %o& e%eme+o& 8)e +oma $ar+e e ) camio 8),mico m)e&+ra )a re%aci9 /e7ii/a e ivaria%e e+re &,# 2% aá%i aá%i&i& &i& gravim gravim3+r 3+rico ico co co&i& &i&+e +e e /e+erm /e+ermia iarr %a ca+i/ ca+i/a/ a/ $ro$or $ro$orcio cioa/ a/aa /e ) e%eme+o' ra/ica% o com$)e&+o $re&e+e e )a m)e&+ra' e%imia/o +o/a& %a& &)&+acia&
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8)e i+er7iere covir+ie/o e% co&+i+)e+e o com$oe+e /e&ea/o e ) com$)e&+o /e com$o&ici9 /e7ii/a' 8)e &ea &)&ce$+i%e /e $e&ar&e# .o& .o& cá%c cá%c)% )%o& o& &e rea% rea%i" i"a a co co a&e a&e e %o& %o& $e&o $e&o&& a+9m a+9mic ico& o& mo%e mo%ec) c)%a %are re&' &' &e 7)/ 7)/am ame e+a +a e )a )a co& co&+a +ac cia ia e %a com$ com$o& o&ic ici9 i9 /e &)&+ &)&+a aci cia& a& $)ra $)ra&& e %a& %a& re%acioe& $o/era%e& :e&+e8)iome+ria; /e %a& reaccioe& 8),mica
OB4ETI5O!&
MARCO TE3RICO 2 8),mica aa%,+ica' aa%,+ica' e% aá%i&i& gravim3+rico o gravime+r,a co&i&+e e /e+ermiar %a ca+i/a/ $ro$orcioa/a /e ) e%eme+o' ra/ica% ra/ica% o o com$)e&+o com$)e&+o $re $re&e+e &e+e e )a m)e&+ra' m)e&+ra' e%imi e%imia/ a/oo +o/a& +o/a& %a& &)&+a &)&+acia cia&& 8)e i+er7iere covi covir+ie r+ie/o /o e% co co&+i &+i+) +)e+ e+ee o com$oe+e /e&ea/o e ) com$)e&+o /e com$o&ici9 /e7ii/a' 8)e &ea &)&ce$+i%e /e $e&ar&e# .a gravime+r,a e& ) m3+o/o aa%,+ico c)a+i+a+ivo' aa%,+ico c)a+i+a+ivo' e& /ecir' 8)e /e+ermia %a ca+i/a/ /e &)&+acia' mi/ie/o e% $e&o /e %a mi&ma co )a a%a"a )a a%a"a aa%,+ica aa%,+ica $or >%+imo &i %%evar a cao e% aá%i&i& $or vo%a+i%i"aci9#
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.o& .o& cá%c)% %c)%oo& &e rea rea%i" %i"a co a&e a&e e %o& %o& $e&o& a+9mico& a+9mico& mo%ec)%are& mo%ec)%are&'' & e 7)/ 7)/am ame e+a +a e )a )a co& co&+a +ac cia ia e %a com$ com$o& o&ic ici9 i9 /e &)&+ &)&+a aci cia& a& $)ra $)ra&& e %a& %a& re%acioe& $o/era%e& :e&+e8)iome+ria; /e %a& reaccioe& 8),mica 8),mica& #
M6TODO! UTILI7ADO! E EL A"LI!I! )RA5IM6TRICO M6TODO POR PRECIPITACI3& T3cica aa%,+ica c%á&ica 8)e &e a&a e %a $reci$i+aci9 %a $reci$i+aci9 /e /e ) com$)e&+o /e com$o&ici9 8),mica cooci/a +a% 8)e &) $e&o $ermi+a ca%c)%ar me/ia+e re%acioe&' geera%me+e e&+e8)iome+ria& e&+e8)iome+ria&'' %a ca+i/a/ origia% /e aa%i+o e )a m)e&+ra# 2 e&+e +i$o /e aá%i&i& &)e%e $re$arar&e )a &o%)ci9 8)e co+iee a% aa%i+o a 8)e 3&+e 3&+e e&+á e&+á e &o%) &o%)ci ci9 9 ma/r ma/re' e' a %a 8)e 8)e $o&+ $o&+er erio iorm rme e+e +e &e agre agrega ga ) age age+e +e $reci$i+a+e' 8)e e& ) com$)e&+o 8)e reaccioa co e% aa%i+o e %a &o%)ci9 $ara 7ormar 7ormar ) com$)e com$)e&+o &+o /e m) a=a a=a &o%) &o%)i%i i%i/a/ /a/## ?o&+er ?o&+eriorm iorme+ e+ee &e rea%i" rea%i"aa %a &e$araci9 /e% $reci$i+a/o /e %a &o%)ci9 ma/re em$%ea/o +3cica& 2 e&+e m3+o/o e% aa%i+o aa%i+o e& e& cover+i/o e ) $reci$i+a/o $oco &o%)%e &o%)%e'' %)ego &e 7i%+ra 7i%+ra'' &e $)ri $)ri7ic 7ica' a' e& cov cover er+i +i/o /o e ) $ro/ $ro/)c )c+o +o /e com$ com$o& o&ic ici9 i9 8),m 8),mic icaa cooci/a &e $e&a# ?ara 8)e e&+e m3+o/o $)e/a a$%icar&e &e re8)iere 8)e e% aa%i+o c)m$%a cier+a& $ro$ie/a/e&@ Ba=a &o%)i%i/a/ A%+a $)re"a a% $reci$i+ar A%+a 7i%+rai%i/a/ Com$o&ici9 8),mica /e7ii/a a% $reci$i+ar
• • • •
M6TODO POR 5OLATILI7ACI3 POR 5OLATILI7ACI3@ 2 e&+e m3+o/o &e mi/e %o& com$oe+e& /e %a m)e&+ra 8)e &o o $)e/e &er vo%á+i%e& vo%á+i%e# 2% m3+o/o &erá /irec+o &i eva$oramo& e% aa%i+o %o !acemo& $a&ar a +rav3& /e )a &)&+acia a&ore+e 8)e !a &i/o $reviame+e $e&a/a a&, %a gaacia /e $e&o corre&$o/erá a% aa%i+o )&ca/o e% m3+o/o &erá i/irec+o &i vo%a+i%i"amo& e% aa%i+o $e&amo& e% re&i/)o $o&+erior a %a vo%a+i%i"aci9 a&, $)e& %a $3r/i/a /e $e&o &)7ri/a corre&$o/e a% aa%i+o 8)e !a &i/o vo%a+i%i"a/o# 2% m3+o/o $or vo%a+i%i"aci9 &o%ame+e $)e/e )+i%i"ar&e &i e% aa%i+o e& %a >ica &)&+acia vo%á+i% o &i e% a&ore+e e& &e%ec+ivo $ara e% aa%i+o# M6T M6TOD ODO O POR ELE ELECTR CTRODE ODEPO! PO!ICI ICI3& 3& 2&+e m3+o/o &e a&a e %a
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r3/ox e r3/ox e %a &o%)ci9 $ro%ema' 8)e &e mo%/ea oca&ioa/o %a $reci$i+aci9 /e% aa%i+o o /e ) com$)e&+o 7orma/o $or e% mi&mo#
PROCEDIMIETO
8.
-
?e&ar e% cri&o% vac,o ?e&o **#*04
?e&ar co %a m)e&+ra e&o **#-0
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9.:
Ca%e+ar a e)%%ici9 a/icioar go+a a go+a go+a oxa%a+o /e amo amoio io'' &e o&e o&erv rvaa ) co%or ro&a á%i/o
Seguimos adicionando oxalato de amonio y se obse!a un colo
Ee %%eva De$a e"osa "o a% c!orro /e $ara e7riar má& el tiem tiem"o "o ag)a de %&
Ee agi+9 co+i)ame+e !a&+a 8)e vir9 a ) co%or
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<.:
Co%ocar e% $a$e% /e 7i%+ro 8)e co+iee e% $reci$i+a/o e ) cri&o%
?o/emo& o&ervar 8)e e% $a$e% /e 7i%+ro :ce%)%o&a; :ce%)%o&a; &e !a /e&a$areci/o $or 8)e &e !a cover+i/o e CO *
J)emar e% $a$e%
.)ego %%evar a %a m)7%a a %a +em$era+)ra
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DETERMIAR EL FACTOR FACTOR )A5IMETRICO )A5IMETRICO
F'rmu+a PMCa FG = PMCaO
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COCLU!I3 2% ca%cio i9ico /e %a m)e&+ra /e %a %ec!e ac!or &e comia co e% reac+ivo oxa%a+o /e amoio co e% 7i /e $reci$i+ar%o e %a 7orma 7or ma /e oxa%a+o /e ca%cio# 2% com$)e&+o &e !ace reaccioar co áci/o &)%7>rico $ara o+eer aci/o oxá%ico' e% c)a% e& oxi/a/o !a&+a CO * D* c)a/o &e aa/e e% reac+ivo /e oxa%a+o /e amoio# Ee $)e/ $)e/ee /e+e /e+erm rmi iar ar e% io io Ca $or $or $rec $reci$ i$i+ i+ac aci9 i9 co co oxa% oxa%a+ a+oo e me/i me/ioo á&i á&ico co'' $reci$i+á/o%o e 7orma /e CaC *O4#D*O# 2% $reci$i+a/o e& &o%)%e e /i&o%)ci9 aci/a $or8)e e% ai9 oxa%a+o e& )a a&e /3i%# Ee o+iee cri&+a%e& gra/e&' 7áci%me+e 7i%+ra%e& re%a+ivame+e $)ro&' &i &e !ace %a $reci$i+aci9 %e+ame+e# 2&+o &e co&ig)e /i&o%vie/o Ca *L C*O4 e /i&o%)ci9 aci/a' e%eva/o e% $D %e+ame+e $or /e&com$o&ici9 +3rmica /e )rea#
CUE!TIOARIO 8. Medi Mediaa(-e (-e u( dia diara rama i(di i(diq que +a/ +a/ *ri( ri(ci* ci*a+e/ a+e/ o*erac eracio io( (e/ e( +a de-ermi(aci'( ra=im>-rica de+ ca+cio /e?a+a(do +o/ *u(-o/ crí-ico/.
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9. !iuie(do e+ diarama a(-erior@ de/arro++e +a/ ecuacio(e/ química/ de +a/ reaccio(e/ química/ que /e ++e=a( a ca,o dura(-e e+ *roce/o. •
*D L *C% L Mg L :OD;
•
Ca* L CaO4*
•
Ca L O*
•
CO:ND*; L D*O
•
ca%ciaci9@ CaCO - L CA.OR 100 **C
CaC*O4# D*O
*C% L Mg L *D *O CaC*O4 # D*O
CO CO*L *ND*
4*0C
CaC*O4
CaO L CO* 0640C
CaCOCaO #Oxi/o /e ca%cio &e o+iee a% 7ia% /e %a reacci9#
;. Qu> cuidado/ /e de,e -e(er e( e+ *roce/o de com,u/-i'( Ee /ee rea%i"ar e ) reci$ie+e cerra/o' a&orie/o %o& $ro/)c+o& CO *' D *O' EO* o N* e +ram$a& a/ec)a/a ?ara 8)e %a com)&+i9 &ea com$%e+a &e 8)ema %a m)e&+ra e exce&o /e O * em$%ea/o ) ca+a%i"a/or 8)e $)e/e &er ?+' C)O' ?O *#
<. E( qu> co(/i/-e +a *reci*i-aci'( y cu2+ e/ e+ meca(i/mo *or e+ cu2+ ocurre u(a
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N)c%eaci9' $ara +o/o $reci$i+a/o exi&+e ) >mero /e ioe& o /e mo%3c)%a& ece&ario& como m,imo $ara 8)e &e $ro/)"ca )a &eg)/a 7a&e e&+a%e e co+ac+o co %a &o%)ci9# 2&+o e&' mie+ra& o &e re>a e&+e >mero m,imo /e ioe& o /e mo%3c)%a& e )a cier+a /i&$o&ici9 or/ea/a' o $)e/e 7ormar&e e %a &o%)ci9 )a 7a&e &9%i/a co ) +iem$o /e exi&+ecia 7ii+o# c%eo e% $rimer $a&o $ara %a 7ormaci9 /e ) $reci$i+a/o /ee co&i&+ir evi/e+eme+e' e %a geeraci9 /e m)c!o& /e +a%e& >c%eo .a ve%oci/a/ a %a c)a% c)a% &e 7orm 7orma a %o& %o& >c% >c%eo eo&& e e% &eo &eo /e )a )a &o%) &o%)ci ci9 9 /e$e /e$e/ /ee /e% /e% gra/ gra/oo /e &ore&a+)raci9# Ei e&+e e& a=o %a ve%oci/a/ &erá $e8)ea e rea%i/a/ $)e/e ic%)&o %%egar a +e/er a cero# ?or o+ra $ar+e' e )a &o%)ci9 a%+ame+e &ore&a+)ra/a %a ve%oci/a/ /e )c%eaci9 %%ega a &er m) e%eva/a# Crecimie+o /e %a& $ar+,c)%a&' e% &eg)/o $roce&o 8)e +iee %)gar e %a $reci$i+aci9 e& e% /e% crecimie+o /e %a& $ar+,c)%a& a 7orma/a& e %a &o%)ci9# 2&+e crecimie+o &9%o $)e/e em$e"ar c)a/o e&+á $re&e+e& >c%eo& ) o+ro& g3rmee& cri&+a%io Co ) &9%i/o i9ico e% $roce&o co&i&+e e %a /e$o&ici9 /e ca+ioe& e ioe& e %o& $)+o& a/ec)a/o&@
2 e% crecimie+o /e %a& $ar+,c)%a& &e $)e/e &eg)ir ex$erime+a%me+e co 7aci%i/a/' $or %o c)a% e&+e $roce&o e& cooci/o co m)c!o má& /e+a%%e 8)e e% /e )c%eaci9# Ee !a !a%% !a%%a/ a/oo 8)e 8)e %a ve%o ve%oci ci/a /a// /e crec crecim imie ie+ +oo e& /ire /irec+ c+am ame e+e +e $ro$ $ro$or orci cio oa% a% a %a &ore&a+)raci9#
. Qu> e/ e+ ac-or ra=im>-rico E+a,ore E+a,ore u(a -a,+a co( e+ ac-or ra=im>-rico *or
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FACTOR GRAVMPTRCO !e *e/a como CuO y /e de/ea de-ermi(ar Cu& fg =
PA ( Cu ) 63,55 g = =0,7989 PM ( CuO ) 79,55 g
!e *e/a como CaO y /e de/ea de-ermi(ar Ca& fg =
PA ( Ca ) 40,08 g = =0,7147 PM ( CaO ) 56,08 g
!e *e/a como Fe ;O< y /e de/ea de-ermi(ar Fe 9O;& fg =
PA ( Fe2 O3 ) 215,55 g = =0,9309 PM ( Fe3 O 4) 231,55 g
!e *e/a como M 9P9O y /e de/ea de-ermi(ar MO& fg =
PA ( MgO ) 40,31 g = =0,1811 PM ( Mg2 P2 O 7 ) 222,56 g
!e *e/a como M 9P9O y /e de/ea de-ermi(ar P 9O& fg =
PA ( P2 O5) = 141,94 g = 0,6378 PM ( Mg2 P2 O 7 ) 222,56 g
%. I(dique do/ eem*+o/ de a*+icaci'( de ra=ime-ría a*+icada e( +a i(du/-ria armac>u-ica • • •
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