- Email: [email protected]
The determination of formaldehyde and acetaldehyde liberated in the periodate and ninhydrin reactions
360
ANALYTICA
THE DETERMINATION LIBERATED IN THE
CHIMICA
VOL.
ACTA
OF FORMALDEHYDE PERIODATE AND
19 (1958)
AND ACETALDEHYDE NINHYDRIN REACTIONS
by
s. J3iochcmacul
LuLorutory,
Norfhern
TOM 13 IX’I-
I..
Gcm_wd
kIlosQ~ld.
Bdiuburglr
(Great
Urtfuin)
Smallquantiticsofformaldchydcand acetaldehycle may be determined colorimetritally by means of chromotropic acidI* and fi-hydroxybipl~cny13-6 respcctivcly. In the cast of biological materials these have their grcatcst application to the determination of these aldcllydcs after their liberation by chemical reaction. ‘L’able I is a summary of the more generally used of these reactions.
-
1. action actlon 3. action 4. action
2.
uf of of of
Acetuldclrydc x. nctlon of 2. action of 3. action of
conccntratcrl sulphurlc acid ninhydrirl at pH 5 pcriodatc in acid nv2tl1uti~ pcriodatc in neutral medium Iibevalion conccntrntcd sulpliuric acid ninliydrm at prr 5 pcriddatc in a&dmcf.liiim
4. action of perioclatc in neutral mccllum
--.
.-_-Subsln~tcc or group drtermtncd
_ __-__
gl~collc ac1d~ glyclnc7a8 CI-1,01-I-CO-, ~rlneYal2,l:~
CH20HCHOH-“-‘I
lacttc ac1t1’3lfi( alaninc~7 - I9 CI-l,XX-IOH*COand CH..CHOH~CHOHs0.a’
The individual reactions are specific for the group of substances conccrncd but when applied to biological materials, formaldchydc and acctaldehydc arc usually liberated simultaneously and in particular, formaldehyde tends to interfere with the colorimetric determination of acctaldchydc. SIIINX AND NICOLET 21 have achieved the separation of these aldehydes after reaction of mixtures of glycinc and alanine with ninhydrin but the apparatus employed may not be generally applicable. Cox20 has described a simple aeration technique for the separation of the acctaldehyde liberated from pregnanetriol by reaction with pcriodate. When reactions 2, 3, and 4 are applied to biological materials, it is preferable as an initial step to separate the libcratecl aldehydes from the reaction mixtures by distillation at xoo”. The recovery of formaldehyde and acetaldehyde in microgram quantities by distillation at 100' has already been discussed eoll. The Cos aeration technique has proved very successful in the separation of the formaldehyde and acetaldehyde present in these distillates. Formaldehyde and acetaldehyde show marked differences in properties with respect to aeration at room temperature (zoo). When aqueous’solutions References
Q. 3611363
\‘oL.
19 (x958)
DETERMINATION
OF
FORMALIIEHYDE
AND
341
ACETALDEHYDE
containing both aldehydes in microgram quantities are aerated, acetaldehydc is completely removed and may be trapped in bisulphite solution whereas formaldehyde remains quantitatively in the initial solution. EXPERISIESTAL
The oxrdation reactrons and the preparation af the dtstttintes have been dcscrlbcd .\ total volume of 15 ml are hcntcd and 10 ml of dlstiilatc arc collected. A~rulro~r proccdrrrc ‘I‘tic apparatus 1s s:mrlnr to that dcscrlhcd by C’ox2o. I 0 ml of dlstillntc roturc for 45 min into 2 ml of 1% sodium hyclrogcn sulphlte.
prcviousIye*s.
arc acratctl at room tcmpc-
l’he colorrnrrtrrc ticfcv*nr~iafaor& of Jo~tttaldehydr atad aretaldehydr The rcsrrlue after the acratron proccclure IS diluted to IO ml with water and the formaklchytlc content cictcrmincd its dcscrii~ecl below The sulphitc solutmn 1%diluted to rn ml with water and the acctnkleh~dc content dctcrn~rnctl as dcscrihcd bctct\v .+I_ ~Tor?ttafde/&ydc ncltl reagent. Thus 19 prepnrccl fresh heforc use 0.2 g of purlfrccl Reagents: I. Ch romotroptc III z ml of wntcr ant1 48 ml of 13Af sulphurlc nctd ncltlcd; 2. 9M chrornotroplc acid IS dlssolvetl sttlphuric card. Procedure: Into a test tube ilrc meastlrcd I -3 ml of solution contalnmg up to toldg of formnklchydc. The volume 1s made up to 3 ml by the ndrhtmn of water. 5 ml of chromotroprc ncld rcagcnt arc acldcd nncl after mi.xmg. the tube is placctl 111it Ix~il111g water bath for 30 nun. After coohng. the mtxtrrrc w d~iutctl to IO ml with 9.W sufphuric ac~cl. fic:ulings arc made ngztrnst a blank at 570
nvi
W. Acetafdclryde
Reagents: 1. conccntratcd sulphurlc nc~d ; z.209& copper sulphatc sofutlon ; 3. p-hydroxybiphcnyl rcagcnt. I 5 g of p-hydroxyblphcnyl arc tllssolvcd In IO ml of so/n sodium hydroxide and clllutod to IOO ml with water Procedure: ‘To I ml of sulph~tc solution. contulnlng up to IO pl: of acctalclchytlc, arc nddcd 0.1 ml of 20% copper sulphatc solution followctl by 6 ml of concentri~tetl sulphurlc ac~cl. After mixing and coohng, o. I ml of p-hydroxyblphcnyl reagent is ;~ldcd and the mixture kept at 30~ for lfsh. ‘t’hc mixture is then placed tn R botltng water b;ttlr for exactly c)o set After cooling:, 7 ml of concentrated sttlphuric ac~ti arc added and after mtxmg read against a hlnnk at 560 rnp. Stanffardisatiotr For stanclnrdisation purposes, except that aeration IS cxclutletl. tlistlllatcs.
the tntllvidual qubst;mcc\ arc sttbjcctcd to the siimc procednrc, The colorimetrlc rcnctlr)n.s arc thercforc npphcd directly to the TABLE
THE
RECOVERY
OP
FORhlALl3P,ZIYTBP,
Peraodnte oxidahott --.---ClucoSr
__---_
udded I’K
(reactiotr - actd) - ---._-_l Nlmmt‘osr added I’K
_--_ ~-
If
AN11
_____--__--_--
ACRTALDRMYOSZ
AFTER
-
___..__.___~cxttmse rrcovcrcd I’R
.-- _
fikamwosc rccoucrcd l’lz
---._----v
92 (92%)
n
ARRATfON
0
0
2390 wwd
100
9:
(94%)
250 2-50 .-.a---_
100 “a%.:: 1%
_
References p. 3621363
XC0
250
250
100
.-
9: (9r%f 238 (9s%f (95%) 242 (97%) 96 (96%) ._.._---_-. _ _._*_ .I GIucosc f~~wcosc W0XWTCd I%
93
(93%)
241 W’S,)
rccmlsred I’K
2;;
g;zp; 0
VOL. Y 9 (19~8)
S. L. TOMPSETT
TABLE
11 (cont:nucd)
Pertodale oxidalron (vencCton - *telrlvnl) A.___ ___ --.-~ _~______ Scttnc 7 krronr,tr added 4%
-...
added J+I
---
100
0
2.50
0
0
x00
0
250
100
__~
31 236
c --11_ Nrrthydvra
8: 238
----.
8:
(89%) (95%)
---__-
Gfgcrrre
add&
cfiatirrtr
recnvctcd
PK
recovered Pi? P-
Pg --0
100
250 0 0
100 250 -
---o/0 Rccovcrtcs
arc
(92%) (93%) (92%)
--___-
.ttanrnc
/‘&! __.
(89%)
230 232 92
_a*..
Ycnclcn?& _-
Glyctnc udded
0
(3~%?10) (94%)
0
250 TOO
250
Thrronrnt recoueml m
Scrine
rccfnJrrtd JG
(91%)
0
0 TOO
232 0
(93%)
0
250 250 100
8; 232
P9?c,) (93%)
91
._-
92 234 240 91
-_- .- _ _ _.-_
--_._
(W%) (94%) (96%) (91%)
______
recorded in brnckctrl
The procedure involving the separation of formaldehyde and acetaldehyde from the _ distillates has been applied to: r. mixtures of glucose and rhamnosc or fucosc allowed to ma& with periodic acid in an acid medium, 2. mixtures of scrine and threonine allowed to react with periodate in neutral medium, 3. mixtures of glycinc and alaninc allowed to react with ninhydrin at per 5. From the results shown in the Table II it will be seen that the aeration procedure provides an efficient separation of the two aldchydcs.
The use of an aeration proccdwc for the separation and clctcrmination of formaldehyde and acetnlclchyclc Iibcrated by the followng rcnctwns: (I) sugars/pcriodntu, (2) scrinc and tlireomncfperlodate, (3) glycinc and alanmc/nmhyclrin, has been cxammcd and shown to bc satisfactory. REFERENCES g E. EEGRIVB, Z. nrtat. D. A, >hCl?AD\‘EN,
.a 3
E:.
Chevt.,
t to (1937)
Rejcvmces
3.
COURTOtS
$. 3621363
n.
22.
\Vr\TKINS AND I’. R, t\SDERSOW, EmtuVt3, Z. anal. Chewa., 9.5 (1933) 323. STOTZ, J. BtoC. Chem., I.@ (1943) 585. XV. WESTISRPELD, J. Lob. Clrar. Med., 30 (1945) 1076.
4 E. 5 W. a P. PLtwRY,
f-1.
AND
R.
Ptc~tiSs,
J
a!3101 C/WJM.,
Mlk~ucjiet~l~e tfey. Mikrockim.
I 58
(1945)
107.
AC&Z. 36137 (xggi)
863.
VOL.
19
(1958)
DETERMIXATION
OF FORMALDEHYDE
AXD ACETALDEHYDE
363
B. ALEXASDER. G. LASDWEHR ASD A. M. SELICMAS, J Btol. Chew., 160 (1945) 51. 8 D. C. SNIITH, J Med. Lab. Technol , I 1 (x953) 205. o S L TOMPSETT ASD D.C. S~~~~,Analysf. 78 (1953) 209 10 VV. H. DAUCHADAI-. H. JAFFE AND R. H WILLIAMS. J. Clan. Endocrlnol, 8 (x948) 166. 11 S. L. TOMPSETT ASD D. C. SMITH, .4cla Endocrtnol.. 20 (x955) 311 1% B. H. XICOLET ASD L A SHISS, J. Bzol. Chcm, 139 (1939) 6s:. UJ P. DESSUELLE AND S. ANTOSIO. Baocham. Bzophys. Acta. I (1947) 50. 14 R. H. KOESEMAIW, J. Bzof. Chcm., 135 (1940) 105. l* S. B. BARKER ASD XV. H. SUXMERSOS, J. Bzol Chem., 138 (1941) 535 10 J. A. RUSSELL, J. Biol. Chem., x56 (1944) 463 I7 A. I. VERTASES, T LAINE AKD T JAVESSES. Z. physaol Chrw , 266 (1940) 193. 111 B. ALEXANDER AND A 31. SELIGMAN, J Btol.Chem . 159 (1945)g. le B. F FOELKES, AlzaCysl, $3 (1953) 496. zo R. I Cox, Bsochem. J , 52 (1952) 339 21 L. A. SHINS AND B A. XICOLET, J Utol. Chem , r3S (194x) gr. Pa F. D. SSELL ASD C. T SSELL. Colorlwwtrtc Mrthods o/ Analysis. Vol.4,3rd ed , D. van Nostrand co Inc , X.Y., p. x19 7
Recelocd
DETERMINATION
OF URANIUM, ZIRCONIUi\l, IRON IN BISMUTH ALLOYS
February
Tth, 1958
MAGNESIUM
AND
by K. Research
Laboru:ory,
XV. KIRBY Brrlrsh
R.
ASD
Thomson
-
H.
A. CRAWLEY
Houston
Co.
Lfd
, Rugby
(Crenf Britain)
There has recently been considerable interest in developing chemical methods of analysis for bismuth alloys, because of the possible uses of liquid bismuth in atomic reactors. Uranium, zirconium and magnesium are three metals which are sometimes added to liquid bismuth, and in this paper methods are described for the analysis of bismuth containing these additions. As liquid bismuth is usually contained in steel systems it is also important to know its iron content and the method described here is suitable for the amounts of iron commonly found in liquid bismuth in a steel container. It is \-ery important to have a sound sampling tcchniquc and there arc various ways of ensuring that the sample is representative. Rapid quenching of the liquid bismuth is essential to prevent segregation of the additives and it may bc necessary to filter the liquid if there has been considerable corrosion of the steel container. If there is any suspicion that segregation has occurred during the cooling of the sample it may be advisable to dissolve the whole of the sample taken and then take aliquots of this solution for the individual determinations. (In all the procedures nitric acid is used for dissolving the bismuth). DETERMINATIOX
OF UHANIUN
Inlrodirclion
Procedures MILNER References
for the determination
AND EDWARDSI p. 368
describe
of uranium
a method
where
in bismuth
uranium
have been
is precipitated
described.
as phosphate
ANALYTICA
THE DETERMINATION LIBERATED IN THE
CHIMICA
VOL.
ACTA
OF FORMALDEHYDE PERIODATE AND
19 (1958)
AND ACETALDEHYDE NINHYDRIN REACTIONS
by
s. J3iochcmacul
LuLorutory,
Norfhern
TOM 13 IX’I-
I..
Gcm_wd
kIlosQ~ld.
Bdiuburglr
(Great
Urtfuin)
Smallquantiticsofformaldchydcand acetaldehycle may be determined colorimetritally by means of chromotropic acidI* and fi-hydroxybipl~cny13-6 respcctivcly. In the cast of biological materials these have their grcatcst application to the determination of these aldcllydcs after their liberation by chemical reaction. ‘L’able I is a summary of the more generally used of these reactions.
-
1. action actlon 3. action 4. action
2.
uf of of of
Acetuldclrydc x. nctlon of 2. action of 3. action of
conccntratcrl sulphurlc acid ninhydrirl at pH 5 pcriodatc in acid nv2tl1uti~ pcriodatc in neutral medium Iibevalion conccntrntcd sulpliuric acid ninliydrm at prr 5 pcriddatc in a&dmcf.liiim
4. action of perioclatc in neutral mccllum
--.
.-_-Subsln~tcc or group drtermtncd
_ __-__
gl~collc ac1d~ glyclnc7a8 CI-1,01-I-CO-, ~rlneYal2,l:~
CH20HCHOH-“-‘I
lacttc ac1t1’3lfi( alaninc~7 - I9 CI-l,XX-IOH*COand CH..CHOH~CHOHs0.a’
The individual reactions are specific for the group of substances conccrncd but when applied to biological materials, formaldchydc and acctaldehydc arc usually liberated simultaneously and in particular, formaldehyde tends to interfere with the colorimetric determination of acctaldchydc. SIIINX AND NICOLET 21 have achieved the separation of these aldehydes after reaction of mixtures of glycinc and alanine with ninhydrin but the apparatus employed may not be generally applicable. Cox20 has described a simple aeration technique for the separation of the acctaldehyde liberated from pregnanetriol by reaction with pcriodate. When reactions 2, 3, and 4 are applied to biological materials, it is preferable as an initial step to separate the libcratecl aldehydes from the reaction mixtures by distillation at xoo”. The recovery of formaldehyde and acetaldehyde in microgram quantities by distillation at 100' has already been discussed eoll. The Cos aeration technique has proved very successful in the separation of the formaldehyde and acetaldehyde present in these distillates. Formaldehyde and acetaldehyde show marked differences in properties with respect to aeration at room temperature (zoo). When aqueous’solutions References
Q. 3611363
\‘oL.
19 (x958)
DETERMINATION
OF
FORMALIIEHYDE
AND
341
ACETALDEHYDE
containing both aldehydes in microgram quantities are aerated, acetaldehydc is completely removed and may be trapped in bisulphite solution whereas formaldehyde remains quantitatively in the initial solution. EXPERISIESTAL
The oxrdation reactrons and the preparation af the dtstttintes have been dcscrlbcd .\ total volume of 15 ml are hcntcd and 10 ml of dlstiilatc arc collected. A~rulro~r proccdrrrc ‘I‘tic apparatus 1s s:mrlnr to that dcscrlhcd by C’ox2o. I 0 ml of dlstillntc roturc for 45 min into 2 ml of 1% sodium hyclrogcn sulphlte.
prcviousIye*s.
arc acratctl at room tcmpc-
l’he colorrnrrtrrc ticfcv*nr~iafaor& of Jo~tttaldehydr atad aretaldehydr The rcsrrlue after the acratron proccclure IS diluted to IO ml with water and the formaklchytlc content cictcrmincd its dcscrii~ecl below The sulphitc solutmn 1%diluted to rn ml with water and the acctnkleh~dc content dctcrn~rnctl as dcscrihcd bctct\v .+I_ ~Tor?ttafde/&ydc ncltl reagent. Thus 19 prepnrccl fresh heforc use 0.2 g of purlfrccl Reagents: I. Ch romotroptc III z ml of wntcr ant1 48 ml of 13Af sulphurlc nctd ncltlcd; 2. 9M chrornotroplc acid IS dlssolvetl sttlphuric card. Procedure: Into a test tube ilrc meastlrcd I -3 ml of solution contalnmg up to toldg of formnklchydc. The volume 1s made up to 3 ml by the ndrhtmn of water. 5 ml of chromotroprc ncld rcagcnt arc acldcd nncl after mi.xmg. the tube is placctl 111it Ix~il111g water bath for 30 nun. After coohng. the mtxtrrrc w d~iutctl to IO ml with 9.W sufphuric ac~cl. fic:ulings arc made ngztrnst a blank at 570
nvi
W. Acetafdclryde
Reagents: 1. conccntratcd sulphurlc nc~d ; z.209& copper sulphatc sofutlon ; 3. p-hydroxybiphcnyl rcagcnt. I 5 g of p-hydroxyblphcnyl arc tllssolvcd In IO ml of so/n sodium hydroxide and clllutod to IOO ml with water Procedure: ‘To I ml of sulph~tc solution. contulnlng up to IO pl: of acctalclchytlc, arc nddcd 0.1 ml of 20% copper sulphatc solution followctl by 6 ml of concentri~tetl sulphurlc ac~cl. After mixing and coohng, o. I ml of p-hydroxyblphcnyl reagent is ;~ldcd and the mixture kept at 30~ for lfsh. ‘t’hc mixture is then placed tn R botltng water b;ttlr for exactly c)o set After cooling:, 7 ml of concentrated sttlphuric ac~ti arc added and after mtxmg read against a hlnnk at 560 rnp. Stanffardisatiotr For stanclnrdisation purposes, except that aeration IS cxclutletl. tlistlllatcs.
the tntllvidual qubst;mcc\ arc sttbjcctcd to the siimc procednrc, The colorimetrlc rcnctlr)n.s arc thercforc npphcd directly to the TABLE
THE
RECOVERY
OP
FORhlALl3P,ZIYTBP,
Peraodnte oxidahott --.---ClucoSr
__---_
udded I’K
(reactiotr - actd) - ---._-_l Nlmmt‘osr added I’K
_--_ ~-
If
AN11
_____--__--_--
ACRTALDRMYOSZ
AFTER
-
___..__.___~cxttmse rrcovcrcd I’R
.-- _
fikamwosc rccoucrcd l’lz
---._----v
92 (92%)
n
ARRATfON
0
0
2390 wwd
100
9:
(94%)
250 2-50 .-.a---_
100 “a%.:: 1%
_
References p. 3621363
XC0
250
250
100
.-
9: (9r%f 238 (9s%f (95%) 242 (97%) 96 (96%) ._.._---_-. _ _._*_ .I GIucosc f~~wcosc W0XWTCd I%
93
(93%)
241 W’S,)
rccmlsred I’K
2;;
g;zp; 0
VOL. Y 9 (19~8)
S. L. TOMPSETT
TABLE
11 (cont:nucd)
Pertodale oxidalron (vencCton - *telrlvnl) A.___ ___ --.-~ _~______ Scttnc 7 krronr,tr added 4%
-...
added J+I
---
100
0
2.50
0
0
x00
0
250
100
__~
31 236
c --11_ Nrrthydvra
8: 238
----.
8:
(89%) (95%)
---__-
Gfgcrrre
add&
cfiatirrtr
recnvctcd
PK
recovered Pi? P-
Pg --0
100
250 0 0
100 250 -
---o/0 Rccovcrtcs
arc
(92%) (93%) (92%)
--___-
.ttanrnc
/‘&! __.
(89%)
230 232 92
_a*..
Ycnclcn?& _-
Glyctnc udded
0
(3~%?10) (94%)
0
250 TOO
250
Thrronrnt recoueml m
Scrine
rccfnJrrtd JG
(91%)
0
0 TOO
232 0
(93%)
0
250 250 100
8; 232
P9?c,) (93%)
91
._-
92 234 240 91
-_- .- _ _ _.-_
--_._
(W%) (94%) (96%) (91%)
______
recorded in brnckctrl
The procedure involving the separation of formaldehyde and acetaldehyde from the _ distillates has been applied to: r. mixtures of glucose and rhamnosc or fucosc allowed to ma& with periodic acid in an acid medium, 2. mixtures of scrine and threonine allowed to react with periodate in neutral medium, 3. mixtures of glycinc and alaninc allowed to react with ninhydrin at per 5. From the results shown in the Table II it will be seen that the aeration procedure provides an efficient separation of the two aldchydcs.
The use of an aeration proccdwc for the separation and clctcrmination of formaldehyde and acetnlclchyclc Iibcrated by the followng rcnctwns: (I) sugars/pcriodntu, (2) scrinc and tlireomncfperlodate, (3) glycinc and alanmc/nmhyclrin, has been cxammcd and shown to bc satisfactory. REFERENCES g E. EEGRIVB, Z. nrtat. D. A, >hCl?AD\‘EN,
.a 3
E:.
Chevt.,
t to (1937)
Rejcvmces
3.
COURTOtS
$. 3621363
n.
22.
\Vr\TKINS AND I’. R, t\SDERSOW, EmtuVt3, Z. anal. Chewa., 9.5 (1933) 323. STOTZ, J. BtoC. Chem., I.@ (1943) 585. XV. WESTISRPELD, J. Lob. Clrar. Med., 30 (1945) 1076.
4 E. 5 W. a P. PLtwRY,
f-1.
AND
R.
Ptc~tiSs,
J
a!3101 C/WJM.,
Mlk~ucjiet~l~e tfey. Mikrockim.
I 58
(1945)
107.
AC&Z. 36137 (xggi)
863.
VOL.
19
(1958)
DETERMIXATION
OF FORMALDEHYDE
AXD ACETALDEHYDE
363
B. ALEXASDER. G. LASDWEHR ASD A. M. SELICMAS, J Btol. Chew., 160 (1945) 51. 8 D. C. SNIITH, J Med. Lab. Technol , I 1 (x953) 205. o S L TOMPSETT ASD D.C. S~~~~,Analysf. 78 (1953) 209 10 VV. H. DAUCHADAI-. H. JAFFE AND R. H WILLIAMS. J. Clan. Endocrlnol, 8 (x948) 166. 11 S. L. TOMPSETT ASD D. C. SMITH, .4cla Endocrtnol.. 20 (x955) 311 1% B. H. XICOLET ASD L A SHISS, J. Bzol. Chcm, 139 (1939) 6s:. UJ P. DESSUELLE AND S. ANTOSIO. Baocham. Bzophys. Acta. I (1947) 50. 14 R. H. KOESEMAIW, J. Bzof. Chcm., 135 (1940) 105. l* S. B. BARKER ASD XV. H. SUXMERSOS, J. Bzol Chem., 138 (1941) 535 10 J. A. RUSSELL, J. Biol. Chem., x56 (1944) 463 I7 A. I. VERTASES, T LAINE AKD T JAVESSES. Z. physaol Chrw , 266 (1940) 193. 111 B. ALEXANDER AND A 31. SELIGMAN, J Btol.Chem . 159 (1945)g. le B. F FOELKES, AlzaCysl, $3 (1953) 496. zo R. I Cox, Bsochem. J , 52 (1952) 339 21 L. A. SHINS AND B A. XICOLET, J Utol. Chem , r3S (194x) gr. Pa F. D. SSELL ASD C. T SSELL. Colorlwwtrtc Mrthods o/ Analysis. Vol.4,3rd ed , D. van Nostrand co Inc , X.Y., p. x19 7
Recelocd
DETERMINATION
OF URANIUM, ZIRCONIUi\l, IRON IN BISMUTH ALLOYS
February
Tth, 1958
MAGNESIUM
AND
by K. Research
Laboru:ory,
XV. KIRBY Brrlrsh
R.
ASD
Thomson
-
H.
A. CRAWLEY
Houston
Co.
Lfd
, Rugby
(Crenf Britain)
There has recently been considerable interest in developing chemical methods of analysis for bismuth alloys, because of the possible uses of liquid bismuth in atomic reactors. Uranium, zirconium and magnesium are three metals which are sometimes added to liquid bismuth, and in this paper methods are described for the analysis of bismuth containing these additions. As liquid bismuth is usually contained in steel systems it is also important to know its iron content and the method described here is suitable for the amounts of iron commonly found in liquid bismuth in a steel container. It is \-ery important to have a sound sampling tcchniquc and there arc various ways of ensuring that the sample is representative. Rapid quenching of the liquid bismuth is essential to prevent segregation of the additives and it may bc necessary to filter the liquid if there has been considerable corrosion of the steel container. If there is any suspicion that segregation has occurred during the cooling of the sample it may be advisable to dissolve the whole of the sample taken and then take aliquots of this solution for the individual determinations. (In all the procedures nitric acid is used for dissolving the bismuth). DETERMINATIOX
OF UHANIUN
Inlrodirclion
Procedures MILNER References
for the determination
AND EDWARDSI p. 368
describe
of uranium
a method
where
in bismuth
uranium
have been
is precipitated
described.
as phosphate