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Spectrophotometric determination of germaniun with phenylflurorone after benzyl alcohol extraction
VOL. 18 (rqj8)
The results arc rcprescntccf in Fig. :, curve I. Curve 2 rcprcscnts tlw trrmsniitt;tnq curve of 0.003~;~ phcn~lfl uoronc wrs7fs benq-1 alcol~ol as 8 blnnk. As will bc shown later, the procedure used rcprcsents the optimum working conditions. It *appears that the phcnylfluoronc -gcrmaniuni complcs in benqd alcohol has iL tllf: quite narrow absorption band with a masimuin at .j'55 mkt. At this wavclcngtli value of the absorbancy is o.jgS, giving a molar extinction cocfficicnt of 144,700. * TW>rlcotlr investigatlan wx5 111lxogrcss.
phcnplfluoronc as acolorlmctric germanium complex 15 soluble Refeve2lces
p. 574
S
A.
5743
Conscr~ucntly, the sensitivity iqucous mctlium.
l~IS’rItlf3U’rIoN
fiII.f.ISf3f
, J.
of the reactlon
C:oISI;l~I(:IISS’T
VOL.
fI0Slli
is practically
01’
TIIIS
tw4cc
IS
(xc)g8)
ah high
as in
COMI’I.I+x
To rlctcrmiw the clistril~ution cocfficicnt of tltc complcs, ttw proocclurc described al,osc \VilS IISLXL, wstricting, Ilow:wr, ttw cstraction to one lo ml portion of hcn-/lyl alcofwl. Wrhcn ;L ClCilr-Cl1 t srparation of tllc txvo pliascs is obtainccl, tIlc ben;syl illC01101 fraction is collccte
The nbsorbancy of a solution of tlw complcs, prepared mcaswwl
as dcscribcd above, could be found.
was
Cr,utr3~ stated that the complex formation dcpcnds on both tcagent and acid concentration. In xN l-ICY.1 a waiting period of 30 min was ncccssary, for the reagent concentration considcrcd. As sl~own in ‘I‘ablc I, it is ncccssary to wait 5 min before extracting the complcs to attain a m&mum absorbancy. Referea%3
pa 574
18 (x9$3)
VOL.
SPI~CTI~OPIiOTO~lI3TI~~C
ISI’LUT:XCI: -_ _-..
-.
___
_._-___._. __
_-___ __._
-.
___~
_..
Tsnte 19, ___--_--_--
,,
DETI~RMISATIOS
or THE WAI-TISG _ _ ._----...__-‘-
w**,,
- -
.---
OF
. -----
-...
. 1 hsorhu~lr\ - -.-. 0
556
5
0
59Y
IO
0
w7
0
.igS
30
ISI;I,UESCE
OF TiIE
ACID
571
Tl>lL
0
_ .---
Ge
.._.-.-.-
..-
-_
_-_
-
__- .-___
. _.-. - ._..
-_-____
.-.
_.____.
COSCESTRATIOS
.4s germanium is citlicr extracted or distillccl as tetracl~loriclc from a MC.1solution, the only acid inwsti~attd \vas hydrochloric acid. Our reslllts ;Lrc summarizccl in
In all cxscs the cstraction of tlw complcs \vas carrif2tl out aftor n _so-tnin ivaiting periocl. It appears that a totiLl 0.5.V l-1(:1 concentration is optimal. I.VI~LUIISCE
01: TtII;
I’IIEN\‘I,FI,UOI~OSE
COSCEXTI~ATION
?‘o invcstigatc the influence of the rcagcnt concentration, solutions containing U.015, O.O.), 0.0_15, 0.06 ZlIItl 0.12’;;, 1~licnylfluoronc wcw prcparcd by chssolving appropriate quantities in 9-j parts of ethanol ant1 5 parts of I-I,SO, (x+0). 25 ml of a solution wcrc usccl, containing 0._5 /kg (k/ml in o..jN liC1; 5 ml reagent arc added. After 30 xnin, extraction with bcnzyl alcoliol kvas carried out as alrcatly describccl. Absorbantics wcrc mensurccl at 505 nip wit11 a Ikckman I>lJ slxxtrold~otomcter using matclicd cores cells. licsults arc summarized in Table 11I. ‘1’A RLE ISFLlliSSLI. _
------
.__- -__
___
. -----._-_----_--__-
.
-.--‘:b
01’ I’llI: .___ -. __ I’hnrr’lrlltoroPle -.___
I’~flS.V~I.PL1’01~0SE ..__ ._-.. .____
. __
COXCLSTHhTIOS _.- __.. __
A hsorhuwy _ ___.
0 03
0.9GI 0 982
0
045
0.80.5
o
06
0
015
_- -_--
__ ____
.___-
-.
-
----
_ ____^____..
0 091
0.12
-~
I I I
0
-_--
273
-..____-_-.--_--.
.--_---
--
Table III shows that the reagent concentration is rather critical, 5 ml 0.03~/~ phenylfluorone giving the highest absorbancy. Higher concentrations of phenylRejevences
p. 574
fluoronc~ c;~iiw not only a lowaring of tJw ahsorbanc~*, tlw ilhsorption spectrum xc, can ho swn from Fig. 2.
hllt also change
the whole of
60--.
iCrwn the previous cspern~~cnts it :tJ)Jwws that the sI’cctrophotomctrIc rlctermination of ~(~r~ll~liitlt~~ with J~Jlc~lytfl~~~r~l~~~after bcnayl nJcold cstraction is most sensitive in 0.5X I-ICI anal i\ rmgcmt concentration of -5 ml o.o;~‘:(, for ;L 2=j-nil sample solution. ‘I’hc formation of the complcs is cluantitativc after 5 min. ‘1’1~ distribution coefficicnt is sufficiently high to achicw cJwntltali\‘c cstraction \vith one x0-ml portion &?@%v1C6S
p.
574
573
50
--
60
--
I
i I
/
70
I
- -
/A 1 YI \
80
90
100
--
\
\
\ . .
C.
4’
500
550
475
.
345
415(
400
390
2
1 370
360
350
340
Y
330
(I) ~Iytlroclllor~~ ac~ci. analytical ~raclc 0.72cq g put-c lgnitccl <;cO, arc fiisccl in a plntiiic~in (L) Stnntlartl stock solutwn of px-rnnnItltn Tlw melt is tl~swlvctl in hot wntcr .~ntl clilutctl to 500 nil. crucilh2 with 2.5 g of sotllum cxrlmnatc. This solution contii~nb I ing Gc/nrl 0 030 g ~~hcnylfl~ic~roiic arc tlissolvcrl in a mlxturc of Hg ml ctli;~nol (3) l~hcnylfluoronc solutlcm -t_ 5 ml I-l&O, (I -t 6) OII a stcwn bath. xntl lll~lrlc up to 100 IllI w1tl1 ctl1a11ul
(I) (2)
I -cm matclwrl Ucckman I>li
‘I’hc Referewes
results p. 574
curcx cc1l.s or I)R ~l’cctropllotonlctcr
of typical
mcasuremcntb
arc shown
in Table
IV.
571
The results arc rcprescntccf in Fig. :, curve I. Curve 2 rcprcscnts tlw trrmsniitt;tnq curve of 0.003~;~ phcn~lfl uoronc wrs7fs benq-1 alcol~ol as 8 blnnk. As will bc shown later, the procedure used rcprcsents the optimum working conditions. It *appears that the phcnylfluoronc -gcrmaniuni complcs in benqd alcohol has iL tllf: quite narrow absorption band with a masimuin at .j'55 mkt. At this wavclcngtli value of the absorbancy is o.jgS, giving a molar extinction cocfficicnt of 144,700. * TW>rlcotlr investigatlan wx5 111lxogrcss.
phcnplfluoronc as acolorlmctric germanium complex 15 soluble Refeve2lces
p. 574
S
A.
5743
Conscr~ucntly, the sensitivity iqucous mctlium.
l~IS’rItlf3U’rIoN
fiII.f.ISf3f
, J.
of the reactlon
C:oISI;l~I(:IISS’T
VOL.
fI0Slli
is practically
01’
TIIIS
tw4cc
IS
(xc)g8)
ah high
as in
COMI’I.I+x
To rlctcrmiw the clistril~ution cocfficicnt of tltc complcs, ttw proocclurc described al,osc \VilS IISLXL, wstricting, Ilow:wr, ttw cstraction to one lo ml portion of hcn-/lyl alcofwl. Wrhcn ;L ClCilr-Cl1 t srparation of tllc txvo pliascs is obtainccl, tIlc ben;syl illC01101 fraction is collccte
The nbsorbancy of a solution of tlw complcs, prepared mcaswwl
as dcscribcd above, could be found.
was
Cr,utr3~ stated that the complex formation dcpcnds on both tcagent and acid concentration. In xN l-ICY.1 a waiting period of 30 min was ncccssary, for the reagent concentration considcrcd. As sl~own in ‘I‘ablc I, it is ncccssary to wait 5 min before extracting the complcs to attain a m&mum absorbancy. Referea%3
pa 574
18 (x9$3)
VOL.
SPI~CTI~OPIiOTO~lI3TI~~C
ISI’LUT:XCI: -_ _-..
-.
___
_._-___._. __
_-___ __._
-.
___~
_..
Tsnte 19, ___--_--_--
,,
DETI~RMISATIOS
or THE WAI-TISG _ _ ._----...__-‘-
w**,,
- -
.---
OF
. -----
-...
. 1 hsorhu~lr\ - -.-. 0
556
5
0
59Y
IO
0
w7
0
.igS
30
ISI;I,UESCE
OF TiIE
ACID
571
Tl>lL
0
_ .---
Ge
.._.-.-.-
..-
-_
_-_
-
__- .-___
. _.-. - ._..
-_-____
.-.
_.____.
COSCESTRATIOS
.4s germanium is citlicr extracted or distillccl as tetracl~loriclc from a MC.1solution, the only acid inwsti~attd \vas hydrochloric acid. Our reslllts ;Lrc summarizccl in
In all cxscs the cstraction of tlw complcs \vas carrif2tl out aftor n _so-tnin ivaiting periocl. It appears that a totiLl 0.5.V l-1(:1 concentration is optimal. I.VI~LUIISCE
01: TtII;
I’IIEN\‘I,FI,UOI~OSE
COSCEXTI~ATION
?‘o invcstigatc the influence of the rcagcnt concentration, solutions containing U.015, O.O.), 0.0_15, 0.06 ZlIItl 0.12’;;, 1~licnylfluoronc wcw prcparcd by chssolving appropriate quantities in 9-j parts of ethanol ant1 5 parts of I-I,SO, (x+0). 25 ml of a solution wcrc usccl, containing 0._5 /kg (k/ml in o..jN liC1; 5 ml reagent arc added. After 30 xnin, extraction with bcnzyl alcoliol kvas carried out as alrcatly describccl. Absorbantics wcrc mensurccl at 505 nip wit11 a Ikckman I>lJ slxxtrold~otomcter using matclicd cores cells. licsults arc summarized in Table 11I. ‘1’A RLE ISFLlliSSLI. _
------
.__- -__
___
. -----._-_----_--__-
.
-.--‘:b
01’ I’llI: .___ -. __ I’hnrr’lrlltoroPle -.___
I’~flS.V~I.PL1’01~0SE ..__ ._-.. .____
. __
COXCLSTHhTIOS _.- __.. __
A hsorhuwy _ ___.
0 03
0.9GI 0 982
0
045
0.80.5
o
06
0
015
_- -_--
__ ____
.___-
-.
-
----
_ ____^____..
0 091
0.12
-~
I I I
0
-_--
273
-..____-_-.--_--.
.--_---
--
Table III shows that the reagent concentration is rather critical, 5 ml 0.03~/~ phenylfluorone giving the highest absorbancy. Higher concentrations of phenylRejevences
p. 574
fluoronc~ c;~iiw not only a lowaring of tJw ahsorbanc~*, tlw ilhsorption spectrum xc, can ho swn from Fig. 2.
hllt also change
the whole of
60--.
iCrwn the previous cspern~~cnts it :tJ)Jwws that the sI’cctrophotomctrIc rlctermination of ~(~r~ll~liitlt~~ with J~Jlc~lytfl~~~r~l~~~after bcnayl nJcold cstraction is most sensitive in 0.5X I-ICI anal i\ rmgcmt concentration of -5 ml o.o;~‘:(, for ;L 2=j-nil sample solution. ‘I’hc formation of the complcs is cluantitativc after 5 min. ‘1’1~ distribution coefficicnt is sufficiently high to achicw cJwntltali\‘c cstraction \vith one x0-ml portion &?@%v1C6S
p.
574
573
50
--
60
--
I
i I
/
70
I
- -
/A 1 YI \
80
90
100
--
\
\
\ . .
C.
4’
500
550
475
.
345
415(
400
390
2
1 370
360
350
340
Y
330
(I) ~Iytlroclllor~~ ac~ci. analytical ~raclc 0.72cq g put-c lgnitccl <;cO, arc fiisccl in a plntiiic~in (L) Stnntlartl stock solutwn of px-rnnnItltn Tlw melt is tl~swlvctl in hot wntcr .~ntl clilutctl to 500 nil. crucilh2 with 2.5 g of sotllum cxrlmnatc. This solution contii~nb I ing Gc/nrl 0 030 g ~~hcnylfl~ic~roiic arc tlissolvcrl in a mlxturc of Hg ml ctli;~nol (3) l~hcnylfluoronc solutlcm -t_ 5 ml I-l&O, (I -t 6) OII a stcwn bath. xntl lll~lrlc up to 100 IllI w1tl1 ctl1a11ul
(I) (2)
I -cm matclwrl Ucckman I>li
‘I’hc Referewes
results p. 574
curcx cc1l.s or I)R ~l’cctropllotonlctcr
of typical
mcasuremcntb
arc shown
in Table
IV.
571