Alkali Metal Carbonate Analysis Report

Valentin Uzunov (author) & Luke Weinstein (lab partner)

PSU ID#: 9!"##$%%
&'( ))% Lab )"
ABSTRACT
*n unkno+n alkali ,etal -arbonate +as anal.ze/ 0or usin1 1ravi,etri- an/ evolve/ 1as anal.sis2
+ith -on0ir,ation b. 0la,e test2 to /eter,ine alkali ,etal present3 Usin1 the results 0ro, anal.sis
alon1 stoi-hio,etri- relationships /eter,ine/ 0ro, balan-e e4uations o0 rea-tion2 ,olar ,ass o0 the
unkno+n ,etal -arbonate +as /eter,ine/ an/ -o,pare/ to kno+ alkali ,etal -arbonates o0 si,ilar
,olar ,ass3 5ravi,etri- anal.sis /eter,ine/ the ,olar ,ass o0 the unkno+n -arbonate to be "#6
1 7 ,ol2 +hile evolve/ 1as anal.sis resulte/ in a avera1e ,olar ,ass o0 $63 1 7 ,ol3 8esults o0
0la,e test +ere in/i-ative o0 lithiu, ,etal present2 in/i-ate/ b. -ri,son 0la,e3 9hese results are in
a1ree,ent +ith evolve/ 1as anal.sis2 but in -on0li-t +ith the 1ravi,etri- anal.sis3 :ro, results it is
believe/ that the unkno+n ,etal -arbonate teste/ +as -o,pose/ o0 lithiu, -arbonate2 Li
)
&;
$
3
INTRODUCTION
* sa,ple o0 an unkno+n alkali ,etal -arbonate (*(&) +as re-eive/ 0ro, *stro (inin1 &o2
0or anal.sis3 9he -lient +ante/ to kno+ +hi-h alkali ,etal is present in the sa,ple provi/e/3
9he sa,ple +as teste/ usin1 ) 4uantitative anal.sis ,etho/s: 1ravi,etri- anal.sis an/
evolve/ 1as anal.sis3 * 0la,e test +as also per0or,e/ as a ,eans o0 -on0ir,ation o0 results3
5ravi,etri- anal.sis -onsiste/ o0 /issolvin1 the unkno+n *(& ((
)
&;
$
) into bariu, -hlori/e
(<a&l
)
) resultin1 in the 0or,ation o0 pre-ipitate pro/u-t2 bariu, -arbonate (<a&;
$
)3
(
)
&;
$
(a4) = <a&l
)
(a4) > ) (&l (a4) = <a&;
$
(s) ?r@n "A
9he pre-ipitate +as separate/ 0ro, the re,ainin1 solution thou1h va-uu, 0iltration2 /rie/
over a hot plate to re,ove tra-es o0 ,oisture an/ then +ei1he/3 With the ,ass o0 <a&;
$
-olle-te/2
an/ the stoi-hio,etri- relationships bet+een pro/u-ts an/ rea-tants base/ on the balan-e/ e4uation
?r@n "A2 the ,olar ,ass o0 (
)
&;
$
+as -al-ulate/3 <. ,eans o0 -o,parison bet+een the /eter,ine/
,olar ,ass2 an/ the kno+n ,olar ,asses o0 likel. *(& (Li)&;$2 Ba)&;$2 C)&;$)2 the
-o,position o0 the -o,poun/ +as /eter,ine/3
*n alternative ,etho/ that +as use/ to i/enti0. the unkno+n *(&2 +as b. ,eans o0
evolve/ 1as anal.sis3 (
)
&;
$
+as rea-te/ +ith !#,L o0 "( '&l2 in a a-i/ base rea-tion2 pro/u-in1
&;
)
1as as pro/u-t ?r@n)A3 9he ,ass /i00eren-e bet+een pro/u-ts an/ rea-tants2 b. the La+ o0
&onservation (ass2 +as assu,e/ to be ,ass o0 &;
)
loss to the surroun/in1 environ,ent3 9hrou1h
stoi-hio,etri- ,anipulation o0 the &;
)
,ass2 the ,olar ,ass o0 (
)
&;
$
+as -al-ulate/ an/
-o,pare/ to the kno+n ,olar ,asses o0 likel. *(& (Li
)
&;
$
2 Ba
)
&;
$
2 C
)
&;
$
)3
(
)
&;
$
(a4) = ) '&l (a4) > ) (&l (a4) = &;
)
(1) = '
)
; (l) ?r@n )A
:inall. a ,eans o0 -on0ir,in1 the results o0 the 4ualitative anal.sis2 a 0la,e tests +as also
/one3 *lkali ,etals +hen -o,buste/ e,it li1ht -hara-teristi- to the ,etal ion in the salt3 :or
e@a,ple so/iu, burns +ith a 1ol/en .ello+ 0la,e2 an/ +hen lithiu, is heat it e,its a -ri,son
-olor3 * s,all a,ount o0 the alkali ,etal -o,poun/ +as burne/ over a <unsen burner an/ the
observe/ -olor e,ission in the 0la,e +as use/ as an in/i-ator o0 the alkali ,etal present3
DATA
Sa,ple teste/: nu,ber #) on label
Gravimetric Analysis Data
TABL ! " 5ravi,etri- *nal.sis (easure,ents an/ 8e0eren-e Values 9able
Meas#rements Re$erence %al#es
(ass o0 (
)
&;
$
use/ in rea-tion(1) #3D)D (olar ,ass o0 &;
)
(17,ol) !!3#"
Wei1ht o0 0ilter paper (1) #3)"" (olar ,ass o0 Li
)
&;
$
(17,ol) %$369
Wei1ht o0 +at-h 1lass (1) !3D$# (olar ,ass o0 Ba
)
&;
$
(17,ol) "#D399
Wat-h 1lass = :ilter paper (1) !3%!" (olar ,ass o0 C
)
&;
$
(17,ol) "$63)"
(ass o0 <a&;
$
= +at-h 1lass =
0ilter paper -olle-te/ (1)
!%399 (olar ,ass o0 <a&;
$
(17,ol) "9%3$!
<a&;
$
re-overe/ (/r.) (1) #39D6
volve& 'as analysis
TABL ( E (ass ,easure,ents o0 h./ro-hlori- a-i/ ('&l) solutions
Trials
Meas#rement 1 2 3
!#,L '&l (ass = 1ra/uate/ -.lin/er
F
(1) 9#3#%" 9#3!%# 693$"
(ass o0 1ra/uate/ -.lin/er (1) D#3$# D#3$# D#3$#
(ass o0 !# ,L '&l solution (1) $93!!" $936!# $93##"
F &.lin/er use/ +as a /r.2 e,pt. )#,L 1ra/uate/ -.lin/er
TABL ) E 5as evolution rea-tion e@peri,ental /ata an/ results table
Trials
1 2 3
Avera'e
Relative
&iviation *+,
(ass o0 (
)
&;
$
(1) #3D!# #3D$$ #3D"! #3D)9 !39"
(ass o0 <eaker
F
(1) "#63D6 "#63D6 "#63D99 "#63$6 #3#D!$
!#,L '&l (ass (1) $93!!" $936!# $93##" $93!)% )3"$
9otal (ass (1)
(be0ore)
G
"!63$9 "!93#$" "!63""$ "!63D9! #3"6
9otal (ass (1)
(a0ter)
G
"!%39$9 "!63!$ "!%3D% "!%399# #3$
&;
)
pro/u-e/ (1) #3%## #3D6 #3D! #3#D )D3D
F base/ on the ,ass o0 a )D# ,L beaker
G in re0eren-e to the su, o0 pro/u-ts ,asses be0ore rea-tion2 an/ ,ass o0 rea-tants a0ter rea-tion is /ee,e/ -o,plete
TABL - E ;bservations an/ 0la,e test
Reaction Observation
?r@n "A
+hite pre-ipitate 0or,e/
I3 slo+ to 0or,
II3 heat a--elerate/ rea-tion
possible error
I3 'eatin1 on to lo+ a te,perature
II3 -lou/. 0iltere/ solution
?r@n )A
i,,e/iate violent rea-tion3
I3 0izzin1 an/ bubblin1
II3 hissin1 soun/ ,a/e
III3 e@other,i-
Flame Test &ri,son :la,e
RSULTS
TABL . E *nal.sis results su,,ar.
()&;$
sa,ple
,ass
(1)
9heoreti-al
Hiel/
G
(1)
Hiel/ o0
pro/u-t
(1)
Per-ent
Hiel/
(I)
(olar
,ass o0
()&;$
(17,ol)
Per-ent
/i00eren-e in
,olar ,ass
to Li)&;$
(I)
Per-ent
/i00eren-e in
,olar ,ass
to Ba)&;<
(I)
Per-ent
/i00eren-e in
,olar ,ass
to C)&;$
(I)
Gravimetric
#3D)D #39%% #39D6 963" "#6 $%3D "36% )!3!

v
o
l
v
e
&

'
a
s

a
n
a
l
y
s
i
s
9rial " #3D!# #3$)) #3%## )"% $!3# %! "#! ")#
9rial ) #3D$$ #3$"% #3D6 "%9 !"3$ D3 693! "#6
9rial $ #3D"! #3$# #3D! "%6 !"3! D3! 693" "#6
*vera1e #3D)9 #3$"D #3#D "9) $63 )36 9!3% ""$
G 9heoreti-al .iel/ is -al-ulate/ base/ on evolve/ 1as anal.sis (&;)) an/ 1ravi,etri- anal.sis (<a&;$)results an/ -on-lusion respe-tivel.3
Per-ent Di00eren-e 0or,ula:

molar mass M
)
CO
$
known molar mass of AMC
(molar mass M
)
CO
$
+ known molar mass of AMC) / )

x "##
Per-ent .iel/ 0or,ula:
Actual yield
Theoretical yield
x "##
"3 9heoreti-al Hiel/ o0 <a&;
$
in r@n " base/ on *(& ,at-h2 an/ li,itin1 rea1ent
)3 9heoreti-al Hiel/ o0 &;
)
in r@n ) base/ on *(& ,at-h an/ li,itin1 rea1ent
#3D)D g Na
)
CO
$

" mol Na
)
CO
$
"#D399 g Na
)
CO
$

" mol BaCO
$
" mol Na
)
CO
$

"9%3$! g BaCO
$
" mol BaCO
$
=#39%% g BaCO
$
#3D!# g Li
)
CO
$

" mol Li
)
CO
$
%$369 g Li
)
CO
$

" mol CO
)
" mol Li
)
CO
$

!!3#" g CO
)
" mol CO
)
= #3$)) g CO
)
Gravimetric Analysis Calc#lations
Reaction
(
)
&;
$
(a4) = <a&l
)
(a4) > ) (&l (a4) = <a&;
$
(s)
(oles o0 <a&;
$
in re-overe/:
#39D6 g BaCO
$

" mol BaCO

$
"9%3$! g BaCO
$
= !36D "#
$
mol BaCO
$
(oles o0 (
)
&;
$
in sa,ple:
" mol M
)
CO
$
" mol BaCO
$
= !36D "#
$
mol M
)
CO
$
(olar ,ass o0 (
)
&;
$ :
#3D)D g M
)
CO
$
!36D "#
$
mol M
)
CO
$
="#6
g
mol
M
)
CO
$
volve& 'as analysis *avera1e values use/ 0or all -al-ulations)
Reaction
(
)
&;
$
(a4) = '&l (a4) > ) (&l (a4) = &;
)
(1) = '
)
; (l)
(oles o0 &;
)
pro/u-e/:
#3#D g CO
)

" mol CO
)
!!3#" g CO
)
="3$% "#
)
mol CO
)
(oles o0 (
)
&;
$
in sa,ple:
" mol M
)
CO
$
" mol CO
)
="3$% "#
)
mol M
)
CO
$
(olar ,ass o0 (
)
&;
$ :
#3D)9 g M
)
CO
$
"3$% "#
)
mol M
)
CO
$
=$63
g
mol
M
)
CO
$
TABL / E J@planations o0 observations ,a/e /urin1 e@peri,ent
Observation Reaction 0planation
Met1o& !
2recipitate
$ormation
?r@n "A
In ,i@in1 a4ueous solutions o0 (
)
&;
$
an/ <a&l
)
2 one o0 the
pro/u-ts 0or,e/ is <a&;
$
2 +hi-h is insoluble in +ater-o,in1
out o0 solution as +hite -r.staline soli/3 When /rie/ its a 0ine
po+/er
Met1o& (
Gas ?r@n )A
*4ueous (
)
&;
$
an/ '&l2 rea-t to 0or, an ioni- (&l salt2
'
)
;an/ &;
)
3 9he &;
)
an/ +ater are 0or,e/ in an inter,e/iate
rea-tion3 '= an/ &;$)K rea-t 0or,in1 an/ unstable '
)
&;
$2
+hi-h
4ui-kl. /e-o,poses to 0or, &;
)
(1) an/ '
)
; (l)3
Li'1t mition :la,e test
When lithiu, is heate/2 the ele-trons in the ,etal be-o,e
e@-ite/ an/ Lu,p 0ro, their 1roun/ state to hi1her ener1. state3
*s the ele-trons return to their 1roun/ state the. release a photon3
I0 the the li1ht+aveMs +avelen1th is +ithin the visible spe-tru,2 a
-olor e,ittion o0 that +avelen1th +ill be observe/
DISCUSSION
*stro (inin1 &o2 ha/ re4ueste/ the ele,ental anal.sis o0 an unkno+n alkali ,etal
-arbonate be per0or,e/ to /eter,ine +hi-h alkali ,etal +as is present in a provi/e/ sa,ple3
5ravi,etri- an/ evolve/ 1as anal.sis2 +as per0or,e/ in or/er to /eter,ine the ,olar ,ass o0 the
unkno+n -o,poun/2 0or -o,parison +ith kno+n ,olar ,asses o0 likel. *(& -o,poun/s as
,eans o0 /eter,inin1 -o,position3 * 0la,e test +as also per0or,e/ as ,eans o0 vali/atin1 the
results o0 the 4uantitative anal.ses3
Wei1ht loss b. evolve/ 1as anal.sis .iel/e/ in-on-lusive results3 9he results o0 the anal.sis
+ere in -on0li-t +ith 1ravi,etri- anal.sis2 but +ere in a1ree,ent +ith 0la,e test observations3
<ase/ on the results 0ro, the anal.sis an/ stoi-hio,etri- -al-ulations2 the ,olar ,ass o0 the
unkno+n *(& sa,ple +as /eter,ine/ to be $63 1 7 ,ol (9able D)2 +hi-h is pro@i,all. -losest in
value to the ,olar ,ass o0 Li
)
&;
$
(9able ")2 ho+ever si1ni0i-antl. less (-lose to N the ,ass)3 9he
results in 9able D2 point to a s.ste,ati- error in the a,ount o0 &;
)
-olle-te/2 +ith the a,ount o0
&;
)
-olle-te/ bein1 ,u-h hi1her than e@pe-te/ base/ on theoreti-al .iel/ -al-ulation3 9he error is
not believe/ to be /ue to hu,an error in ,easure,ent or -al-ulation3
* plausible h.pothesis 0or the /isproportionatel. hi1h .iel/ o0 &;
)
,easure/2 -oul/ be /ue
to the in-orre-t assu,ption2 that the /i00eren-e in ,ass2 bet+een total su, o0 ,asses o0 rea-tants
an/ 0inal ,ass o0 pro/u-ts2 is onl. &;
)
3 Sin-e the rea-tion bet+een the unkno+n *(& an/ '&l is
hi1hl. e@other,i-2 it -oul/ be possible that enou1h heat is 1enerate/ /urin1 the rea-tion that so,e
o0 the +ater pro/u-e/2 or +ater present in the '&l solution +as also evaporate/2 lea/in1 to a lar1er
/i00eren-e3 Volatilit. o0 " ( '&l -oul/ also a 0a-tor2 ho+ever a//itional anal.sis +oul/ be nee/e/
to -on0ir, the su11este/ h.pothesis3
In -ontrast2 1ravi,etri- anal.sis o0 the alkali ,etal -arbonate sa,ple i/enti0ies the
-o,position o0 the unkno+n *(& as Ba
)
&;
$
(so/iu, -arbonate)3 <ase/ on stoi-hio,etri-
-al-ulations 0ro, ?r@n "A an/ the ,ass o0 <a&;$ -olle-te/2 it +as /eter,ine/ that the ,olar ,ass
o0 the unkno+n *(& to be "#6 1 7 ,ol2 +hi-h is a ver. -lose to the ,olar ,ass o0 Ba
)
&;
$
2 +ith a
"36%I /i00eren-e bet+een in ,olar ,asses values3 * 96I re-over. o0 theoreti-al .iel/ a//s vali/it.
to stoi-hio,etri- anal.sis3 'o+ever2 these results are -on0li-tin1 +ith the the evolve/ 1as anal.sis 2
an/ observation o0 the 0la,e test +hi-h su11est the -o,poun/ to be -o,pose/ o0 lithiu, -arbonate
rather than so/iu,3
;ne /isa/vanta1e o0 1ravi,etri- anal.sis is that the ,etho/ is sensitive to error in
pro-e/ure3 S,all pro-e/ural ,istakes -an have a ,a1ni0ie/ i,pa-t on the 0inal results3 In or/er 0or
the 1ravi,etri- anal.sis to ,at-h the 0in/in1s 0ro, the 1as evolution anal.sis an/ the 0la,e test2 a
hi1her .iel/ o0 <a&;
$
+oul/ have been re4uire/ (-loser to "3! 1 o0 <a&;$) 1iven the initial sa,ple
,ass use/ in the ?r@n"A (9able D)3 It is believe/ that i0 there +as an error2 it is ,ost likel. to have
resulte/ 0ro, an in-o,plete pre-ipitation rea-tion2 an/ a lo+ .iel/3 Durin1 anal.sis it +as observe/
that the 0iltere/ solution ha/ a -lou/. appearan-e (9able !)2 +hi-h su11ests that a si1ni0i-ant
a,ount o0 <a&;
$
+as not re-overe/3 9he a--ura-. o0 the ,olar ,ass /eter,ine/ 0or, the
unkno+n *(& to the kno+n ,olar ,ass o0 Ba
)
&;
$
2 is attribute/ to -oin-i/en-e2 rather than
a--ura-.3
9he results o0 the 4ualitative anal.sis are overall in-on-lusive3 <ase/ entirel. on the 0la,e
test it is believe/ that the *(& teste/ +as -o,pose/ o0 Li
)
&;
$
3 It is re-o,,en/e/ that i0 a sin1leK
,etho/ /eter,ination is to be use/ to i/enti0. 0uture unkno+n alkali ,etal -arbonate sa,ples2 it
shoul/ be /one usin1 1ravi,etri- anal.sis3 Despite -urrent ina--urate result obtaine/2 the level o0
a--ura-. a-hieve/ an/ the -lear un/erstan/in1 o0 sour-es o0 error in anal.sis2 su11ests that
1ravi,etri- anal.sis -oul/ be use/ to i/enti0. the unkno+n *(& ver. a--uratel.2 1iven a hi1h
stan/ar/ize/ pro-e/ure2 an/ -are0ul e@peri,entation3