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QUAN QUANTI TIT TATI TIVE VE DETE DETERM RMIN INA ATI TION ON OF TOTAL OTAL HARD HARDNE NESS SS IN DRINKING WATER BY B Y COMPLEXOMETRIC COMPLEXOME TRIC EDTA EDTA TITRATION J. FERNANDEZ1 an J. LIM! 1
INSTITUTE OF BIOLOGY, BIOLOGY, COLLEGE OF SCIENCE INSTITUTE OF BIOLOGY, BIOLOGY, COLLEGE OF SCIENCE UNIVERSITY OF THE PHILIPPINES, DILIMAN, QUEZON CITY 1101, 1101, PHILIPPINES DATE PERFORMED: 24 JANUARY 2014
INTRODUCTION Water ater hard hardne ness ss is defi define nedd in term termss f the the !" #n#entratin f #a$#i%m #ar&nate that is e'%i(a$ent t the tta$ #n#entratin f a$$ the m%$ti(a$ent #atins in a sam)$e f *ater+, -1. The determinatin f *ater hardness is im)rtant &e#a%se it )r(ides a meas%re f the '%a$it/ f *ater fr h%seh$d and ind%stria$ %ses+ The ins in hard *ater )re#i)itate *ith sa)s *hi#h $essen the #$eansin a#tin f sa)+ F%rt F%rthe herm rmr re e hard hard *ate *aterr %)n %)n &ein &ein heat heated ed )re#i)itates #a$#i%m #ar&nate *hi#h #$s )i)es -1.+ Ta"#$ 1. The Water ardness 3#a$e Wa%$& Ha&n$'' (() CaCO* 3ft 020 Mderate$/ sft 2050 Mderate$/ hard 51120 ard 121160 7er/ hard 8 1 60 9m)$emetri# titratins *ith EDTA ha(e &een %sed t determine e(er/ meta$ #atin *ith the e#e)tin f
a$;a$i meta$ ins r the $a#; >$a#; T &th &th manesi%min indi#atrs #an &e %sed as indi#atrs in *aterhardness titratins -1.+ The *inered #$r f the Manesi%m=ndi#atr #m)$e ?M=n@ &rea;s %) int at the e'%i(a$en#e )int ?&$%e #m)$e =n 2@ as sh*n in the rea#tin as sh*n: Y4 M=n BC MY2 =n2 =n the initia$ staes f the titratin manesi%m ins are dis)$a#ed frm the EDTA EDTA #m)$e &/ #a$#i%m ins and are free t #m&ine *ith the Eri#hrme >$a#; T therefre im)artin a red #$r t the s$%tin+
RESULTS AND DISCUSSION Water !hardness, is the tta$ #n#entratin f a$;a$ine earth ins *hi#h are main$/ 9a 2 and M2 in *ater+ ardness is #mmn$/ e)ressed as the e'%i(a$ent n%m&er f mi$$irams f 9a9O )er $iter+ Th%s if -9a 2. -M2. 1mM *e *%$d sa/ that the hardness is 100 m )er $iter &e#a%se 100 m 9a9O 1 mm$ f 9a9O+ Water *hse hardness is $ess than 50 m )er $iter is #nsidered t &e !sft+, =f the hardness is a&(e 20 mGH the *ater is #nsidered t &e !hard+, -2. =n a #m)$emetri# titratin ana$/te and titrant frm a #m)$e in and the e'%i$i&ri%m #nstant is #a$$ed the frmatin #nstant I f+ 9he$atin ?m%$tidentate@ $iands frm mre sta&$e #m)$ees than d mndentate $iands &e#a%se the entr)/ f #m)$e frmatin fa(rs the &indin f ne $are $iand rather than man/ sma$$ $iands+ -. Eth/$enediaminetetraa#eti# a#id r EDTA is *ide$/ %sed in titratins f meta$ #atins &e#a%se it frms 1:1 #m)$ees *ith the #atins+ =t is an amin#ar&/$i# a#id *hi#h has 5 &indin sites ?the f%r #ar&/$ate r%)s and the t* amin r%)s@ )r(idin si )airs f e$e#trns+ =n the e)eriment EDTA *as %sed t meas%re *ater hardness+ >asi#a$$/ EDTA #a)t%res the meta$ #atins in the *ater &/ tiht$/ &ndin t them th%s ma;in the *ater sft+ -4. The str%#t%re f EDTA is sh*n in fi%re 1 &e$*+
Figure 1+ 3tr%#t%re f eth/$enediaminetetraa#eti# a#id #mmn$/ ;n*n as EDTA
T start 16+5 f Na 22EDTA22O *ere diss$(ed in 200 mH f disti$$ed *ater+ NaO )e$$ets and 1+0 f M9$ 252O *ere then added+ Additin fmeta$ $i;e manesi%m in the frm f sa$t #a%ses the meta$EDTA #m)$e t frm faster+ =t a$s ens%res that M2 *i$$ &e initia$$/ )resent in the titrant and that there *i$$ &e a shar)er end)int+ NaO #a%ses an in#rease in the diss#iatin f ins and a$s ser(es as a ne%tra$iKer f the frm the EDTA+
The standard 9a9O s$%tin *as then )re)ared &/ diss$(in 1+2L1L f )%re 9a9O *ith 40 mH f disti$$ed *ater+ 9$ *as added in the s$%tin t ens%re fast diss$%tin f the s$ids+ The &%ffer s$%tin *ith ) 10 *as )re)ared &/ miin 2+0 f N 49$ and 14+ mH f N + The indi#atr %sed *as eri#hrme &$a#;T *hi#h &inds *ith the e#ess ins t frm the *inered #m)$ees+ On#e the EDTA has dis)$a#ed a$$ the E>T &%nded t meta$ #atins the s$%tin rea#hes its end)int a #$ear &$%e s$%tin+ 3in#e EDTA is a *ea; a#id the ) %sed *as &asi# at ) 10+ 9a$#%$atin the EDTA and meta$ #atin #n#entratins is ) de)endent s it is im)rtant t ;ee) the ) #nstant+ Fr this )%r)se a &%ffer s$%tin *as %sed+ =n the e)eriment a ) f 6 r hiher is needed in rder fr the &$%e #$r t &e (isi&$e s the NN49$ *as %sed+ Fift/ mi$$i$iters f 0+00L0 M *r;in standard 9a 2 s$%tin and 2L0 mH 0+0100 M *r;in EDTA s$%tin *ere )re)ared frm 0+0L00 M 9a 2 and 0+1000 M EDTA res)e#ti(e$/ thr%h di$%tin+ =n the standardiKatin f 0+0100 M EDTA 10 mH f 0+00L0 M *r;in standard 9a9O s$%tin *as )i)etted int ea#h f the 2L0mH Er$enme/er f$as; *hi#h *as then di$%ted *ith L mH f disti$$ed *ater+ Three mH f &%ffer s$%tin and 2 dr)s f E>T indi#atr *ere a$s added t ea#h f$as;+ The s$%tins *ere titrated *ith the 0+0100 M standard EDTA s$%tin+ Ta&$e 2 &e$* sh*s a s%mmar/ f the net ($%me f EDTA %sed fr ea#h tria$+ Table 2. Net ($%me f EDTA %sed fr standardiKatin Tria$
1
2
Net ($%me f EDTA mH
14+L
14+
14+1
Nte that the (a$%es &tained are '%ite #$se t ea#h ther and #an &e $a&e$$ed )re#ise+ The errrs in titratin *ere ;e)t at $* &/ titratin (er/ s$*$/+ =n the titratin )r#ess the s$%tins *ere first &ser(ed t &e *ine red &e#a%se f the rea#tin f E>T *ith the ins+ As E>T is added t the s$%tin -M=n. *i$$ frm &ased n the rea#tin &e$*+ M2 =n2 ?&$%e@ 2O M=n ?*ine red@ O
+1,
After the s$%tin *as titrated *ith EDTA the #$r rad%a$$/ #haned %nti$ it t%rned int #$ear &$%e s$%tin *hi#h mar;ed the end)int+ At this )int the
rea#tin &et*een the indi#atrmeta$ #m)$e and EDTA is as f$$*s: M=n ?*ine red@ Y4 O C MY2 =n2 ?&$%e@ 2O
+!,
E'%atins 1 and 2 sh* the rea#tins that ta;e )$a#e and te$$ *h/ there is a *ine red s$%tin in the start f the e)eriment and a #$ear &$%e s$%tin after the *h$e titratin )r#ess+ -L. =n the ana$/sis f *ater sam)$e L0+0 mH f the #mmer#ia$ minera$ *ater ?A&s$%te@ *as transferred t a 2L0mH Er$enme/er f$as;+ Three mH f &%ffer and 2 dr)s f E>T *ere added t the f$as; and the s$%tin *as titrated *ith EDTA+ This *as re)eated fr t* mre tria$s+ Ta&$e 2 sh*s a s%mmar/ f the data &tained+ Table 3+ Net ($%me f EDTA fr *ater sam)$e ana$/sis Tria$
1
2
Net ($%me f EDTA mH
0+0L
0+0L
0+0L
Hi;e the data frm the standardiKatin the &tained (a$%es *ere (er/ )re#ise+ =n fa#t the/ are a$$ the same+ With %st a dr) f EDTA the s$iht$/ )%r)$e s$%tins &e#ame #$ear &$%e+ M$arit/ f EDTA and tta$ *ater hardness *ere then #a$#%$ated frm the data+ The &tained *ater hardness *as reater than the &rands #$aimed hardness *hi#h is 0 ))m+ Ne(erthe$ess the *ater is sti$$ #nsidered sft &e#a%se its tta$ *ater hardness des nt e#eed 20 ))m+ Pssi&$e s%r#es f errrs in#$%de titratin errrs *eihin errrs and ther h%man errrs *hi#h #%$d ha(e affe#ted the ) and ($%me f titrant+ SUMMARY AND CONCLUSIONS 9m)$emetri# titratin *as )erfrmed fr the determinatin f the tta$ hardness in drin;in *ater+ 9m)$emetri# titratin in#$%des and interates the #m)$eatin rea#tins f meta$ #atins *ith )arti#%$ar $iands+ Eth/$enediaminetetraa#ti# a#id ?EDTA@ is an rani# headentate $iand that *as %sed as the titrant and the drin;in *ater sam)$e as the ana$/te+ EDTA *as %sed &e#a%se f its 1:1
#m&inatin rati *ith meta$ #atins reard$ess f the #hare+ The indi#atr %sed is Eri#hrme >$a#; T ?E>T@+ E>T &eha(es as a *ea; a#id and is a d a#id&ase indi#atr and at the same time a meta$ in indi#atr+ The red #$r *%$d )redminate in the )resen#e f a meta$ #atin and *%$d t%rn t its &$%e #%nter)art *ith the a&sen#e f the said #atin at ) e'%a$ t r hiher+ The additin f M9$ 2·22O )rir t the )re)aratin f EDTA s$%tin *%$d frm M EDTA #m)$ees *hi#h *%$d hasten the frmatin f 9aE>T #m)$e thr%h the dis)$a#ement f manesi%m ins t and frm #m)$ees f EDTA and E>T+ The dis)$a#ed *%$d &e ne%tra$iKed &/ the added NaO )e$$ets and *%$d ens%re the #m)$ete diss$%tin f Na22EDTA ·22O #r/sta$s+ The additin f 9$ t 9a9O )rir t the )re)aratin f the 9a2 s$%tin *%$d se)arate the in mre effe#ti(e$/ than *ith *ater sin#e the rea#tin f the t* *%$d )rd%#e #ar&n diide *ater and #h$rine and #a$#i%m ins+ 3e(era$ #m)$eatin rea#tins are ha))enin a$$ thr%h%t the titratin )r#ess+ These rea#tins in#$%de the frmatin f meta$EDTA ?9aEDTA and MEDTA@ and meta$E>T ?9aE>T and ME>T@ #m)$ees as *e$$ as the dis)$a#ement rea#tins f the meta$E>T #m)$ees *ith the e#ess EDTA and the rad%a$ dis)$a#ement f #a$#i%m ins *ith the MEDTA #m)$e+ O&tainin a shar)er end)int after the titratin )r#ess *%$d re'%ire a #nstant ) *hi#h fr this e)eriment is at ) e'%a$ t 10+ A &%ffer is re'%ired t maintain the s$%tin at this #nstant ) t ens%re a shar)er end)int+ The &%ffer *i$$ a$s hasten the #m)$eatin )r#ess &/ frmin a sta&$e #m)$e f N $iands and meta$ #atins+ The N $iands *%$d then &e re)$a#ed &/ strner EDTA $iands *hi#h frm m%#h mre sta&$e #m)$ees+ 3e(era$ )ssi&$e s%r#es f errr #an &e f%nd thr%h%t the e)eriment+ These ma/ in#$%de &%t are nt $imited t nt *ashin f the &%rette *ith the titrant EDTA s$%tin ra)id additin f EDTA t the s$%tin fai$%re t maintain &%ffer ) at 10 additin f t m%#h &%ffer and the )resen#e f ther interferin ins in the sam)$e+ The tta$ *ater hardness f the drin;in *ater sam)$e &ased frm the #n#entratins f #a$#i%m and manesi%m indi#ated is 0 ))m 9a9O + The a(erae ))m 9a9O &ased n the titratin data is #a$#%$ated t &e at 0+241 ))m 9a9O *ith Q 0+1221 ))m 9a9O #nfiden#e inter(a$+ =t #an &e #n#$%ded that the sam)$e is a&%t as sft in terms f *ater hardness as the #m)an/ #$aims it t &e+ This ma/
&e d%e t the riina$ ass%m)tin that the hardness *as at 0 ))m a !)erfe#t$/, )%re sam)$e+ Mre
infrmatin n the minera$ #ntent f the )rd%#t *i$$ &e needed t red%#e errr in the e)eriment+