Studies On The Detection and Spectrophotometric Determination of Organic Compounds and The Synthesis of A New Inorganic Ion-Exchanger

studies on the Detection and
Spectrophotometric Determination
of Organic Compounds and the
Synthesis of a New Inorganic
Ion-Exchanger
SUMMARY
A THESIS SUB vIITTED FOR THE DEGREE OF
BottOt of Pt)tlO£iOpl){>
IN
CHEMISTRY
THESIS SECTION
BY
"^L^q^ SHAHANA ANWAR
DEPARTMENT OF CHEMISTRY
ALIGARH MUSLIM UNIVERSITY, ALIGARH
JUNE, 1982
S 0 NNA • T
-I
i
«tMi«i«l Xiitro4MtiMi* glvlag •> •««oait •f tli» i«|^rt«a«« ftf tli«

vork to • ! • « 9t tli« fast dsTslopasat ta <^<Mile»l tsshaology. flw
laportaae* af aaparatiaa liaa l»«aa diaeaaaad alongvitli ike rariaas
faatora affaotlag I t . A l l a i of aTallnbla aaparatton aathoda hat
baea Rlvaa trhloli alnglaa aat tha v a r a a t l l l t y mni a f f i e l a a e j of
eliroaategra|>liy. Slnea tha ioB«axaliaaga ehravatography la ana af
th« aaat inportflnt a a a l y t l e a l t a o l a , i t baa baea daaaribad ia
d a t a i l clvlng ^^* d l f f a r a a t ty^taa af tbe applieatioaa in aaalytiaal
ehaaiatiy. IB tbe end tba ayathaait aad analytlaal appllaetioaa
of iaorgi^nio naterlala bava baen bigblightad irhlob ara tha proaiaiag
ian-axebeng^ra for tana d i f f l e u l t aaparations, p a r t i o a l a r l y a l k a l i
• a t a l a and radioaneleidaa.
CSiaptar I I sonaariaaa tba aa loot I r a rola af oxldanta ia

tha praaanea af aat Ian axahanga raaln f a r tb« dataation and
d i f f a r c a t i a t i o n af aeldlat baale and nentral aninoaalda* tlia
dataatioa and d l f f a r e n t i a t i o n proaedaraa ara BB f a l l a v a t
^* i—«^> taati To ana drop of tha tast aolation takan in an

ignition toibo vara addad a drop of t% potaaaian paraaaganata
aolntioa and 9»iO iatt«>axahanga baada (Na^.foni)* fho aontonta wv
haatad in a boiling vatar bath f o r 2*3 niaatoa and a f t a r aooling
tho anpomatant l i ^ a l d nmt daaantad o f f . Tha baada vara vaahad
by daaantation v i t h 5 ar % portioaa of doninaralisad vatar and
vara tranafarrad t a a v h i t a apot plata* Aftar drying v i t i i a
o
^
f i l t e r iMH>*r tb«y mtn t i « a t « « v i t l i • dmp o f 1l«»«l«r*s r««(4mt*
iM i M W d l a t * pink o o l v r en tb« •arf«o« l i i d l e a t « a t h * prttwno* ^ f
aai»0 aeld*
B* Petacttca of a e t d l c and mantra 1 tnwAno aetdat f » a t A wa»
p a r f o n w d by t a k i n g 1 ^ tBTO^/KjflrjÔ^/KlO^/njÔQ i n plaoa of tha
IMmmmaiiata a o l n t i w i * Baale aaino aelda geva a aegatiTo t a a t .
e« patootlon o f baa to a«ljio aotdai I f a e i d i c and n a u t r a l aaino
aoida ara abaant tha t e a t aay ba perfomad by repleelng pamangaaata
by one drop aaeb of %M hydroehlorlo aoid and t% potaaatna broaato
aolatiott*
D* P l f f a r a n t l a t l o p botwaaw a c t d l c and n a u t r a l awtno aetdat I n tha
ganeral t a a t Aaaertbad aboira tha pamaaganato vaa replaead by a
drop of 0«005N aodiim hydroxlda follawod by a drop of 1 ^ potaaalim
dlohrcmata a o l n t l m i * A poaltiira t a a t I n d i e a t e a tha praaanoa of
• o i d i o aalno aelda o n l y .
r a b l a X givoa tha I t a l t of I d o n t l f l o a t i o n of a e l d i e , baalo
•ad a o n t r a l aaiao aetdsvblla t a b l a o I I - X T anaaartoo t t e o f f a o t of
foroiga oAotaaooa on tho dotootioa of o i l tha throa typoo of aalao
aotdo* A t o a t a t t v o aeohoaioa haa alao boea proposed f o r t h e
roaotioB tavolTod*
Cbapter XXI gtvoo aa aoooiait of a aonottlya «ad opoelf to
raata bead t o o t f o r t i t o t i d i a a aad I t a opoetropliotoaetrio dotomtaotii
no lag t B r O j • • a laagoat* The aothod f o l l o w e d f o r the dotootioa off

'.«
A* m»»qtion »roe»<«f f»r titttldlBai A f«v re* in beadt (Va^^fom)

ver* taktts Is a alerotaaitaba followad by a dro|» of a t% aqaaona
KBfO. aoloiloB attd a drop of IM ROl* Hie eontento vara hoatod in
a waior 1»«tb for 2*3 •lantae which roBnltad a hluo.irlolat eolor
of tho aolntloB. Ifio oolatton was reaovad and the baada vera
washed aeveral tlaea and tranaferred to a white apot p l a t e . After
drying the heeda with f i l t e r paf»er (free fro* aanonlni iono) a
drop of Neaslcr'a reacant waa added to obtain a pink oolor <» the
beads surfnee. The limit of detootiom was 20/ng of h l s t l d l n e . A
large naisber of ecNopounds wore found to giro a negatlTO t e s t with
t h i s reagent. The proposed aethod of deteminatitKi of t h i s aaino
acid i s as followst
B* Psteriination of hietldinot A s a a l l aaotmt ('-Ô.i • ! ) of tho

toot solution ernitainlng 1 to i*5 ng h l s t l d l n e was taken in a
boiling tobo followed by a O.i a l of the t% aqneons IVrO- solntlen
sad a 0*1 a l of IN RCl. The solution booeao yollow after 19 aiantos
whioli was allowed to stand for two hours and then two a l of tbo
buffer solution {k% MHêi in aaaonia) wore added. TM oolor of the
oolttttoB tnraod blao iriolet whleh was dilutod to 25 a l with MfV
oft o r 90 aiautos and tho aboof%aaee was taken at 590 aa.
I f f o o t s of ^ 9 roagstttOf t i a e aad toaporaturo have boon

studied on tho oolor produood with h i s t i d i n e aad the reprodnoibility
and proooslan data are SMsnarioad in table • , The aoohaaiaa of tbo
roootioB has boon propoood at the end of tiM obaptor*
4
f ABIS :I
UNIT or HKMTIF:EOATIOIf <NP ACIDIC. BASIC AKD
RBtDTRAt AJflNO ACXDB
f
1 ^
Aiiao a o l d t Hilar •olOM Of AnOIMIv
oono«ati«tion anino aeiaa detootaA
of Miiao
JL -Alan In* 5s 10-5 0.05 22.8

/^•Alanine 531 io-« 0.05 22.8
L^Proltna i X 10-2 0.02 25.0
OlyotB* 5 « 10-5 0,05 18.8
NitiiioBiBe 1 X i<r® o.ot 29.8
*nir»«MBiiie 5 » 10*' ©•05 8f.5
l«tteln« i X 10"* O.Oi lO^.O
01<»s«riBi« 5 « 10*' 0.05 8«.0
Aspurtio a o K 2 s »•• 0.0« 155.0
ftlntMiio ««i4l 5m tr' O.Oi 58*9
I«rtta« 1 X ir* 0.05 750.0
Ai«taln« i X to-* 0.05 870«0
lliti<llii« 1 X io 0*05 775.0
:i
UMIT OF TOIBHAWCE OP VAaiOPS rOBEI«m SUBSTAHCTS

FOR TUB BBTBCTKW OF OLYCniE ( 7 ^ . 0 ^ )
' • I " '" t '' I

foretgii sttliKtsDew 0(m««Btratt<m VOIOM e«d«d tAmit of
(M) (»I) <«•)
erotfmaidehyd* 2 a 10"^ 0*t B«3
SttoroMi 1 x 10*' 0.2 1.4
At«ton« 1 X toT^ O.t e*9
iU«ti9 aei« 1 m iST^ 0.9 IS.O
rfil41ii« 1 X to** 0*5 2«4
Bmstno 1 X 10** 0*5 2.3

G
u m r <y TOUIKMICE or TAmopg roHEigK BmstmcBB

FOR tm MITBCflOit or A8PABTIC ACIP (358 ^Wg)
' ' I ' I ' 't

For* ifn ««a>0t«Bee OoBOcatmtioa T«lnM «d!fl*dl Ubilt of
tol«ranis«
(tf) (>1) im)
ett» ton A1 dehydd 2 X 10"* 0,2 2.t
8«eros« 1 JE 10*^ 0.3 1«0
M«t<MI« 2 X 10** 0.2 2.3
Fyrldlne 1 X to** 0.2 l.«
Aalsidlne 1 X 10"* 0,3 2.9
A««it« aeid 1 X 10"* 0.3 it.o

WBSMw 1 X 10"* 0.3 2.3
ilC»t«Bi«* i X 10"* 0.3 l.t
BthF^mia* l.« 0.% 19.0

M
i
VABIX Vf
UMn OF TOUMIAIICB OF •AMOPS FOBEIOM SOaSTAMClS

FOB rag mfBCffiQif OF L t s i w inomt)
" '• I f
F«r«lgii ivAistanoft OanmatmttoM • • ! « • • «dil«4 Idmit of
tol«r«iio«
(») (•!) im)
Ao«toii« 2 X 10*^^ 0.4 4.€
A4Mitio a e i a ^
1 K 10*^ 0.5 5.0
JUMtMlidO 1 X 10*^' 0.5 3.0
•MIS«II« t s ur^^ 0.5 3.5

99mmBl4»hy4l^ 1 X 10*^^ 0.5 5.3
fhnmtwu 1 X 10*^^ 0.5 9.0
W^Kfl • • t t l F l IC«tQM« 1 X tO*^^ 0.6 4.3
FFTitfln* 1 X 10"^^ 0.5 3.5

||itil|rlM|ln« l.« 0.4 19.0
8
f ABUB •
IIBFIKMDOeiiXUTT AND nOEOISlON DATil m

T8E WfBSMIllATXOir <^ RZ8TXDXIIB
1 '1
81. im»tmt of A1i»ot1lenoe a t 990 m
MA* Mttidlac T i •'
1
I XI 111 XT T Av«r«g«
1. 1.0 ©•30 0,38 0.33 0.94 0.30 0.98
9* t»t 0.35 0,9% 0.33 0.3% 0.3% 0.3%
5. 1*8 o.«e 0.%1 0.%8 0.99 0.38 0«%0
«• 1.3 0.%9 0.%9 O.M 0.%7 0.%7 0.%8
f. 1.% ••9i 0«93 0.9% 0.93 0.99 0.9%
«• 13 o.i^ 0.0 0.65 O.M 0.69 0.i%

9
eii«ft«r I T •anMiri»«t tiMi stodr i n the a»t*9tUm 9t

friMto«« sad •neroM* t k * fiiiHMidur* adopted i s •« followet
About 4*6 tim«*4»xeli«iig« rmniM lb««d» imprtgiiat*4 v l t l i tii«

elilorofom •olvtion of l«obl<iro»2,%»ai»iti^b«iis«ii« ««i« pl«e»4 la
a iiierot««ttub« follow«d by a ilrop of the toat ioltttioa and a drop
of 9(K a u l f a r l e aeld* Hia eflmtaato vara tiâtod oa a liolling
vator bath f o r 2«»4 nlnataa* Bavalopsiaat of aa oraaga eolor oa ilia
raaSa baada tadioatad tba praaoaea of froetoaa «id aaoroaa. Tha
l l a l t a of data at ton vara 14i,% /ag for f ractooa aad 3-2 nm f9r
aaoroaa. Tba aanaltlirity of t ^ taat ia aahaaeadf i f fraahly
praparad raaia la aaad i ^ i l a a t l l l noiat* Tlia orgâio aoapomida
eoatainiag verioaa fmettoaa], groapa vara foend aot to tatarfera
v i t b tba t a a t .
Ilbaptar •» tba laat Mia, aaaiiarlaaa th« airatbaalo of a

aav iaofiaale laa*axiâagar aaaaljr tiB(XV) araoaoailloato aad I t o
applioattoaa f o r tba ooparatlea» of « a t e l loaa of m a l y t t o a l
laportaaoa. «lia i i a t a r i a l vaa praparod bjr tba f o l l o v l i C aatbodoi
j^ytpawttoa of tlio toaôydiiaago » a t a r t a l » i Tba oolatioa of aodftaa

•llioatoy aodioM arooaato aad otaaaio oblorida vor« aixod ta •
irolMMO r a t i o i t l t l aad tba pB of tba gal prodeead vaa f i j M d - ^ l
vltb tho bolp of m o . * ffho a l o r r r « » • tbaa kapt at V9m toaporateya
for 2k boara aad f i l t a r o d * Aftor vaabiag v l t b Mvlaaraliaod vator
f o r oovaral tiaaa to raaova tba oxooaa of roagaato^ tlio gal vao
driod at 45*6* H M drtod a a t o r i a l vao plaood i a vator to oraok i t
iO
Uit« MMll gr«iiiil«s« After watthtng v i i h d«iiiii«r«liMA ^mfr,

t i l l th« pn mt tti« Mishincs 1>«e««« 6*7t the naterlal WA» pl«««d
la a l.OM HNO. solttticm to oonvort It Into the R^^fom, Fiiialljrt
aftar 2% boar kaapiag at room t«ap«ratara» tlia graaalaa war*
waahad to ra«ova axeaea of aeid and driad at 45 0* Vbia aaaqyla
vaa found to he l>«tt«r than othar oaaplaa pr«parad on TarjrlBg
tlia iroloaa ratioa asd e«iaantratl<»ia in It a apparent atabllltjr
and loii«-axehange oapaeity. It wn*^ tharafora, aalaetad for
farther atadiaa. flam eenpoaitlon of tha ion-axehanga aatarlal vaa
dateminad hy the atandard owthoda and i t VBB found to bo aa
SniAatSl • i t l | l . Ita ion»ax«haaga oapaoity «aa>^ 1 awq/dry g».
flK» alntion, pR t i t r a t i o n , IH and TOA atadiaa ware perforaad in
order to eharacteriaEo tha n a t e r i a l , irhieh aoggeat ita fomula aa,
fti02*RÂaO^|,Si02 •nRÔ
In order to aY«ia«te the potential of an toaMNnhanga

• a t e r i a l i t ia vary aoaantial t o have a haovladge of ! « • diotribntion
hohOTiowr* for t h i s pnrpooo t M K^ Taltioa wero deteiiitBeg of
•arlotto a e t a l to«o on ai(IT) arsonoailieato* Baaed «a thoao
• t o i i e a the following binary oofarationo have boon aehtorod nhioh
aro praoiao and ropro4aeibloi ei(XI)«lli(XI)« fti(XX)*m(XI)»
Ot(XX)«Clr(XXX)» Tb(XXX).T(XXX)« Yl<X).lig(XX), Oa(XX).ro(XXX)»
tr(XXMa(XX), Oo(XX).Ba(XX)«
studies on the Detection and
Spectrophotometric Determination
of Organic Compounds and the
Synthesis of a New Inorganic
Ion-Exchanger
A THESIS SUBVIITTED FOR THE DEGREE OF
'Bottox of ^t|tlo0opl||>
IN
CHEMISTRY
BY
SHAHANA ANWAR
DEPARTMENT OF CHEMISTRY
ALIGARH MUSLIM UNIVERSITY, ALIGARH
JUNE. 1982
'V
T2498
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(0Mi«r8l litroiliwttîi) i
mmf^mt • f t
(••l««ttir« W9U of osttfAttt* l a ^ pf«««tt«* «f ««tlon*

mn^mm^ ! • • ! « • to ini^*f»iii fi»r i l M «tt««tl«a • • €
«lff«ir«iitl«tliiii ttf mildtot ^•Bim MIA «««tfttt « i t e # IMTIAS)
Xilff94wHilMi W$
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l i t s f i ^ v t r M t ^ l i M i t r l * i « t « i i i l M i t l « i witof f«l«iMli«i %r«wit«
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tttMlt* 911
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BifHitimtott 71
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(Sjmtii**!* 0f « tii«nMiUr H i i b i * M d i r ) arMNiMUlett*

••tlott •x«liaiii«r «Mi H t «]iflt««tioB f « r tiM M I « M
«livMMi««iit»^te Mfiumttott of a t t i i l ! « • • )
liitt««««tt«i t5
lB|i«rl«««t»l 7%
tlMIIMlMI f4
fli« mitHor •i|^f««t»» tt«r • l a e t m grtitfttia* %m
Or* K«0«Viirtlnierf ISIiciilttffy i««tl«i» t*li* ^ I t « « 9 #f itegin««riiit
mtt fMAmologrt Alti«fb Wmtim mtwrnttt^ Alliafftet nmStr II^«M
Irfntf 9w$mvwi9tm eatf cttt««ft«« t^l» wofle ««• eoii|pl*t«i* fli« ! •
NMlla l%itv«««li|F^ ifbtt saiMiivti^d tiw «»!% fta ! « • l i i t t t « l t t i ^ * *

Hiaiile* ®f« otuft atw to tNfaf«««<it« MaAitla Q«f««lit end V«il«iiaaHi
for fffovltfttti t»t«aveli f i i e i l l t t * « * A i ^ r l «f tii» voitt « • • |»«rfer»«tf
to «li« Ilii<ll«fiiiel9rtt«tit l«t»of«t<irl«o <if tlm miwrwtty «f ]lMfft««
(tlitfta) for wnteli tiio « « t i i ^ t« tlisiilrfnl «# fvof«o«or t*^*?^!^^!
for tit* kind li«l9 imfl iMofel ooggoottmo*
Wm ootiior oloo vltiioo to tli«»k Iwr frtwido* oolloogaoo

oii« foatly iMaiboro for tiMtr t t a t i r b#tp «HI oooforotlon tforloi
tlM ifHoto toooro of fooooroli, yioolljri otio grotofoltr oefeoowloiioo
ttio f ioooolAl ooitotoooo gtiroii to kor %f tiMi Hoiwotl of toioottfto
OBA foAiotriol Rtooorolif lliv otUit (lii<lio)«
( illlîUIIA AMVAt )
( i )
•rwMitte «Idtliyi««*
t* i»I«0ttV9 V » U t f tUttfilllt* In tll« f y t M B M Ot «»%t«ll««[»»ll8ttg«

iw»l»* I n ll«^*foi« f « r t&« 4tt«iiti«tt mM ifff«fwatifttioii • §
• o l i i e » l>i>«te mi« a t i i f i w l Mitii« • « ! « • •
fr«»«nto» 2:*Aiial«€fe«»*t j ^ 89S Ct9t9)*
%• A t w i c i f t i ^ aiii tiptelf 1« f««tii*%»o4 t « » t f o r fti»tttfiii* antf

i t * tiMetvoiôtnMitrlo tf«t«f»ta«tt«i wiliig p^fmttm %wmmtm
• • « ff9«g«ttt«
9* HfBiiMtid of • tb«nMiily •i«%l« i i i ( t i r ) «f«Mi»9lli«»t« • i i t l M i

•soliMf^r SMI t«0 avi^lttfCtiM f « r ilMi « • ! « • » ^fttsetflgriiplit*
•tpiiffwtittt of S i t * ! ! • « • •
OkrowiiagiNiylil* <eMM«il««t««>»
( it )
UMf or wjmmn
9*hU t A l i s t mt «v«tl«%l« Mpafattttt «ttli«tfs MMI
ta%U II A tufVir 9t t ^ i««t»i «»fli Ml til* tttteljptt**!

•pplt««tt09t •f 99m imkm9m9llimm0 aattrUlt* it
ffibl* III §mm l«poftmt AoiÎ« •»!$• iiiwfSPti imtf tli«tr
«iiereot«rt*tle i»f<ip«ytt«»» 19
?•%!# IT tiiiiftis of latnttf t«9tt<w ^f •0iai«» li«ste «aA
ii«ittffittl 8»l»* •at4* 54
t t « t t « •# t»l«if«ii«« «f iNirton* fomigii titbtw
t«ao«» fftr tb« a«t*otlon of glSFOtno* 99
Ittnlt* of totorvBOO of v«rtoa» fofotgn oObo*
t«iie«« for tiM MtootlOB of oapartio oottf* 3$
f«%t« VII Motto of tolomooo of vorloot forvtgo oiilit*
t«Qo«» for tlio ••tootloo of Irctoo. 57
v«iiu f i n lllotKtoc oootoot of • ooriior of urotetoo* 4$
Mtfroiootitlttr (mi trooteion data in H M
ittoroiaotioo of litotttfiiio* S%
Vlio o n t a r t m M oooorronoo o f ooat oliiplo
ooioro* i%
f«%l« XI Uotto of tol«r«woo of vartooe fortlfo oiiM*
tMooo for tlio iotootioR of frootott aoi tnorooo* T(
( ill )
f«1ll« XII l$oiiposttlaii ftf ttii(I?) «f«Q»ottll«iit«« 7€
ftlbU XIII Ioii««x^ffi^« Mpttottr of f iii<IV) •rtmio«tlte«t«* 78
fli«ni0l •ttibtlttr nf tltiCIf> «t««ii(ittllo«t«» it
tttÛ X? Dt«trlt»atioii ooeffieletife of tono «et«l tono on
tl»Clv| f)ro«iioolite«t«« §7
BlotvtIitittoR eo«ffietettt* of son* iMtol iono oa
f Incur) ari«iiootltofit« at |)ll»0 attag fsdiotraaava* M
( tir )
vwf (MP wtamam
rigsr* i •ffcttt of pR « i tli« ttolttr pfoAiio«tf 1» tlM

lit«ttatnt»XliiO« vi«ation« 99
iptffttfift d Rff«et of tlt0 f«ioint of %tiff«r en tlio imlor
{irodtie«4 in tbe btettiitmi«<»8BrO« ivftotiOR* 96
Ftfttim 9 A eelt^mtloQ esrv* for tiie <l»t«f»tiuitl«i «f
lll0tli!tfi« Mttng X8lO« «• « f«^«llt* 97
FlgttHi 4 eoa«iîitff«tt9ii enrvo for i t i i ( I ¥ ) uronnoitlloftto
toRHROhi^Bg^r* 79
Ftgsvi 9 ElotioB eixrm for t l a ( I 7 ) ^rMitooilteoto too*
oxabmigor* 90
Pigim i 9ir ttiffcttion ottrvw for t t a f l T ) ertoaootlieiito
tiotiiii ifm'M»ci Mixtttw* §9
Wigmm 7 nwopootroR for t i n (17) «ro«iio»tli««to ion**
oat«liiiBior* a%
Ftcttfv • flio fflA «t«rv»« f o r t t o ( X V ) u r o e n o i t l t e v t o Sn
a^ Mid Hii^ f ovao* 89
fiswm 9 Bffoet of neio^ wi n^ imlMo of eo^ OK timitf)
•ro«ooollle«to tott«>oxoliitiiior» 99
f t f a t v to Mfsnitlen of m C t l ) f r o * ea(n) miA milt) «MI
t t a ( t 7 ) oroavoelltoato oolonno* 90
<ir )
f»^9_
WH^w it Septratlm «f GoClI) froB er(lll) end fii(ni)

frmn T<Xff) as tln(tv) <»r«f*iiosllie«!t« eoltwn** 91
Ftgnrft 18 Stpmtittoii df fl(T) froia l%(xi) »iia Ito(XX) twm
IÎXfl) m ttnfiv) »rtffB9«llief^te eolssns* 98
rigt2f« 19 8eisaristi<m nf Ba(ti:) fr^M Co(XX) end Sr(XX) an
tlii(W) ftmimii9Stloftt« e&iwm9» 99
(irt )
0HAF7EB»I
GPIBiAl* WTBQVtOOftQB
i
MKRlytleetl 4^««t«try 1» atae af the f{»fitly r r a v t i i i fields
of e h « » l » t r y sd i t hnv Ofiplleatioiifi in etieititeftl teehnology* To
laaderstKtKf f u l l y th« titviuiet of ® p e r t l c t t l a r »ttb»ti»ncl ^nd e ^ c » t e n l , f t i s iwtf»ort<Bnt t o knot^
how t h * S!!f>«ti»nc«e Ti»«»hfiv«» imtfer th« eanrtttlons *f»!lf*h |cov*»ni the
f»hy8tc?'l «!i<1 etêmlool proc^BJ^fs fjotns cm tn a »y8tf>r?j <»h«»Bifo«»l
etialvsts RlvfR siscti « »mo^vl©<!ê, A ehesBte«'l ttuelysis way h© of
the eliir«<pntf5 or of th«» f»wcttonPl «^ro«rn* pren^^nt in « fOHipoimil,
Pine© ©Ipfsfrotf. ore tê biRsle u n i t e of MJf^tter the olpm«»ntJ*l
rniPlywIe ploye f*n Iwport^nt rolllf^wtnp rcasoiist
(1) I t «»t«t»lt8h©® the l d » n t t t v of «l#ra©ntf*l owii»tttwttan of «
e»»rt»tn coBipoHn*! «si»««t«lly thr orftawle o n # t .
(2) Tt !*lv«8 thi» pressnc!** tm«1 aaioisit of » c e r t a i n w e t a r i n l v i a
the A e t « r a i n a t i o n or d e t e c t i < » of c h e r n c t e r l s t t e elements.
(3) t t in<Si©ete» the firp»enoe of ?* »i>eclfic «lo»eiit iaioS4>
firesenee or fihB««iee pro«f«o<'ei o e r t n l n <ieeire(l or uadesired
resettons or e f f e c t s ,
A t o n o t i o n a l fronf) in a noleeole i s f comhinattoii of
atons w i t h eharf»eteri»ttc profMirties. It i s the profmrty of the
f u n e t t o n a l group t h a t g e i i e r e l l y goyerns the property of ths t o t e l
woleonle* fha t e r a V m e t tone 1 tp^roup" i s ootmRonly eonsiderod a
t e r a f o r o i v * n f c eonftiBatioo of atoms such as hydroacyl^ earbonyl^
ester« aaii'to e t e * gronpa* nowever^ earhcRietey sulphato^ a l t r a t o .

2
n i t r i t « e t e * , thoufh tnovR^nte, al«o f i t the d e f i n i t i o n of
fimotlonfil Rroofifi. Vim t«ehnl<Qtt«« tMMid t o d«t{»et and fmasoro
th© f m o t i o n a l s;roap» »r»» the mmm wh<»fhi»r ori«nl«5 or Inorei^tnlf*
«ioto<ffi1»a or© I n v o l v e d , Since f i m o t l o n a l ji^rooft is e ehBrt^cter*
I s t l p porticRi of « Boloewlf'f I t Biskea ?IOP O? th*r» !>c»»t han<Îes
f o r n [ o » l l t « t l r « *f«»tofti(» of eheasloi^'l tmterlBl» or thf^ ( f t i n n t i t a .
t l v e d<^tereiination of the®,
fh© QOJ^ntIti^tlv© f^nnlyaia may he elttser e e?»«rl©«^l or «
ptwatoftl, dep#n''»1n" on the rsethovis ©wp1oy©d, a t o t c M o w c t r y In a
chamlff'l r « a e t i o n or n aijltjp>f>l© phv6te«l f>rofi«rty of titc 8fi»|>l©»
Taeh elowp life f'drt^^tn i»'1vrnt«'if*»» and •^MmneWfrntSiRê, The-
ehesalorl @4»tho'^8 ore alwaya Sf^colfle, a l t h o t ^ h t h r l r t1f*f;rc<> of
»r»a<*lf I c l t v v»rle«» 'Wi#» eqwlpw^p-nt n«©c! In a oi'i<»«!»lc' 1 BM^tht>*?
t©nd t o he almplog lne«f»©n*ilve »n^ êsiy t o saelntaln. The soopo
and tho raactlon eondlti^ma ar© In »oat casaa v a i l nn<!ar»tood
ttad aocuracy of feattor thiw ©.SI* i « r o o d i l y a t t a i n a b l e * Roway«r»
th© etiemioal laathods ara I n a f f a o t i i r e f o r aniiatanitea t h a t mrm
ehamloally t n a r t . Alao^ they do not d i f f © r a n © l a t a a n a l l y botw^«n
aiâtaneaa witti a t o i l a r ohanlaîl p r o p e r t i © * * f h j r a i e r l tiethoda
ara thoaa l a wlileh th© e n t i r a net of phyaleal p r o p a r t l a a i «
mtaaorad omnvaaiantly v i t h a aini;!© Inatrnen^nt, For a rout In©
wortc i n a t m n a n t a l fa©thoda ara s a n © r « l l y praferr©d aa qniok
r a a n l t a ara raqnlrad l a aneh a enrnt^ l a o ncm»ro»tlne work^
hovavar^ tlw wmm f o n e t i o n n l group i « found in d l f f a r e n t eoBq»oand»
in a wldaly ramrtng altttatiany and I t i a aot aaononierl t o

«alt%ir»t« tiMi l»«trammts tn ttuis* oa»*»« rttrtbîraord tlui
»T9 i«ti«rAl]r tb«» emtmrn ilii»»wei«t tma rtegvnte ftrt •aelljr

Qvallflbl** That, tn w>a«ni preettcw, ehevtAiil m d filiytteel
nH»tliotf» of f|tiitiittti}tlT» analyst* «r* of ooor^tnoto ifit{iort«iieo«
fa » ehrmierl {taalyvls, tfio s«{>sriittoii of mirfono

<»o«p|)(Ni«fits ftreeent In e $;1v«n 0fi9»fl«> t« elso «»i»«»nttfil» lit
•titttftoABOo ibeco«N»o »anyfol<l wtoen th« eosifHMeientii totorfcro with
oaeli oth«r* 8ofMiratt«Mi» nra eaellir oodorstood on ttm liiteto of
tho |Mii:^fitea«>eh«Rleel prlnolploo involvod fm^ ttM» niiRltor of
poO0l1})e v»rifibl«», ffi#re «r® only t h i * * »tet«« of matter tmA
e U n i t e d nuatiar of phyoteiil proi»ortieo of cheniorl e|}«ete« on
Ktiteli aofiaretloas eim 1>« bnaedf auch aa al%e a»4f 8ba|»«y val^nca
of an ion^ polarity^ potarli!c*btllty, ttydroeaa-liondlnf a b i l i t y
of 1^ mol«oole« and f^hantO'al r a a e t l r i t y . tn praetloo* bowavart
tbo altwitioo la qntta d i f f e r e n t * Exeept f o r v a l m e e , Krtiloh
obanRea to a ate?wftinotton» a irtrtttal oontlamaa exienda fro« an
axtrewe to tba othor tn oaob firofterty idietbar I t be molaenlar
welfbt or iondon Intoraettono* Hi •ddltton* tbo noatbar of
ohealoal eoatiMrande tbat oam bo oallod mprnt to iîarpen toipamttoBa
by oniwrlaqkoelni eoaiMittttve oboateal raaottona or pbyatoal
teteraetiona la extroaely largo* rnrtbar«of«t any t»artleolar
•oadilnatioB of aiieelea ean hm I t * lateraetlona fmrtbar iiodlfled
by ebaafo* te te«perettti« or fir»a*oro» rortanatoly, the one or
two aftproaabo*, aost l i k e l y to •neoeod for a iMirtletilar oanplo.
0m wBoellr %• 0«lffet«tf OR tii« a&»aaptiom ibat «M( or tvo faotoro
w i l l doMlnato ib<<> root*
HM ooleotloD of tho opt 1mm |»roooduro would liitfood IM

rolatlTol^ al»pl« if only ]phyaioo->ohoiilot 1 prinolplaa w«f«
liivolT«d« bat there er« otiior oonaldomttont wtiich of tan proro
to ba otrarrlding* Vlrat, tbe natnra of tha aaiipla oan be a
powerful eonstrnlnt. Yf the aanple ta very a a a l l , thertaellr
and/or ohenloQlly unatablo, very Inaoluble or l i k e l y to eontaln
a noirtiar of anknowa subat»nees, e nunbar of otherwise obTloua
eholeee «(^y be ruled oat. A aeeood oonatratnt le the tlaie
awallnble for the analysis* Tine nay be a Heoldlnr faetor when
a large Hinder of annplea are to be analyEed or n rapid reaetion
hae t o be followed* A third constraint In the lore) of aceuraey
and/or praoiaion required* tHasaoeaaerily high requirenenta for
qoantitatioB uaaolly lead to axeassively tiaeoconsusing
prooeduros* flia final l i n i t a i i o n ariaos froei a ocmbiaatioB of
a v a i l a b i l i t y of a<|uipsK»nt and f a n i l i a r i t y of tha ohesiist with e
wido variety of separation •athoda* Hie oMthods ganorally awed
f o r oopsvottotts isolodo d i s t i l l s t i o B » o ^ r a o t i o a , pvaolpltation
erystslllMition^îslysis,^ diffusion ate* as l i s t e d in foblo X*
OhrosMitofrafiiiyi ioB*oxirtianga and aleetrophorasis are

o f f i o i o n t oad vorootilo annlsrtioal teohniqoes* Tlioy are osafnl
for tho ooaparioon of sslbstattoasy for providing s l o e s as to the
strootoroo of organio sdbstaneea^ and for the dotootisa of
s t m o t o r a l ohaagos prodoood by varions ohasiieal raogaato or
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WMl^mr em^ %lolcN|ioal proe«9Si»« oaHiiia*a v i t b ecmvtiittonal
i^Nmloisl emd tttetroMvnte 1 f m a l r t i e i a l nwthotfs* ft%r servv t o
t d « n t l f y tmA wmp&mf tHe cthewlesl • ^ e l « i i « psflrtltii • l « ; i i l f l e ^ n t
r»e««t «4fviin«»es I n ehrooMitoicrenhle t h e o r y , vhieh hav* providadi
fsnefi Inforfiietlon about the mcohAotam of ovparatlona ern^ SCHIO
n i f r a t i o n , the a«l<»ettirlt^ of ohnmitftgrtiphie mytmsn is atill
iaconplately miAeratood ao t h a t th« QCMndltiona ra(}iiiratf t o
a«|>arata P ft Ivan ffilxttirv oaa not o a a a l l y ha t h e o r a t t o a l l f
pradiota4»
Ioii*a:sohfinge forme one of th« »oat lisportant ^ i n l y t i o a l
tools with a wtila ran^« of eppraoietigms* I t i a v e i l asttodi
f o r the aer>aration of Inorgf'iiio iona, hoth eati^tna and (mi<m«,
hoenaaa tho o^pari^tion i a huaod on the axohnoga of i<»ia* S«f»ef«tion
of t r a n a t t i o B al«nonta (fti t o 19B) on Dowax-1 ealmma ( 1 ) way ba
o i t o d a t «na of the iiN)at otrtklnic «x8«r>l«* 9t i t a anal^Htioal
apT>lleBtiono, ffttcHh work haa he^n Aooa on tho M p a r a t t o e of imiona
em« «ora p a r t i f ^ u l a r l y OB tho ooparattoii of ntotal t o n a , o i t h o r ea
oottona or ao anlomto eonnloitoo ( 0 ) « Boi>«r»tton of t r e e o aloawata
f r o n « wtdo v a r i a t y of v a t a r t o l o on anion oxohasfo roaino oaint
nci^llf oa «a o l n a a t i a of p a r t i o a l a r t n t o r o a t ( 5 ) « A aurvty o f
I t t a r a t n r a hao r o v f a l o d t h a t oirhonatiira o t a d i o t have hoan aado
i s t b i t dirootiOB (%»t9).
IB organie analyato a l o o , ioB->oxeh«ngo toelmiâo has
•holm a Kvaat p o t a n t i a l (i%)» IB tho f i o l d of "Functional gr^mp

8
««t««tl(Ni In oivAiito •o«p«aa««* t b l * t«eliiit<itMi li«« %•«« of mwli

tet«r»»t (19*17)• I t i s hm—4i OB th« lat«iui« • o l o m t t M i iirodae«a
OR tlw onrface of 1 i f lit eolorotf toii««xelsi^Bi« rtotn %3r tftlctng tlui
tons hoTlag eliaiwetorlotio oolor fron ttio foaotioa •edlMi* It
irit» devolof»«A hy Fajtmito (19919) In the dvtootloo of aloro
owointo of 8M»t«lt only* Uitor 90 ^^rtsttl ot e l * (SM>»ai) f o r tlm
f l f « t tlMOy OKtinKSod i t s ci»(i In th«* 4eti)etlon eiidt dNttomlnettoo
of orxfîite ooe^>ot»ido. SOMO tooto hur* aloo Itooa dosorllHid f o r
tli« datoetlin of phenols, aliplifltie aaltieo^ primary aroaotlo
nalnoOf ftld«livltoo ffisd oaliotttotod tiydrastiioo (23^23). A l l tliooo
tooto are raaln ofiot nodiflofttloiia of a l r o o ^ imoi^ color
roaotloKia (2%)* TIaey h^vo the foUowinK edriôtngoot
t« fliojr «r« raora aontttlira lioeenaa tha oolora^'i tonlct aiiaotaa

la oiMioaiitratod on ttia rooln aarfaw»«
ft* flUa ooloratloa lo often aN>ra atebla to ttie roaln f4»a»a tOion
In aQmouo iiAiaao and oonatlaia iMieanea proivoaalvoly sort
tntonoo on otandinc*
)« l l M toota am novo oalaotl^po* TlmOf tons hairing a obeno
9^p9&H9 to tha tonlo opooloa adoor%od by tho roolo,
nnnnll|r «o not tntortaro*
%• fbono tooto nood I H t l o oipit|MMnt and raâlro vary l l t t l o
t m l n l n g en tho part of tlia Invoottgator*
11M nno of ootid ion-onoliantora hao o nmrtiar of

9
!• fli« o«»tfly«t «»ii b« f«o«^lly roflioved fra« the rcôiton

pro<lur>5p ^y ''fltrf'tlw or bv <'eo«'nt0tl«i.
2« Tto« purltv of th«» f»r«>f1«t»t 1» »><i»tter ftlnce th#» side r#jf»otlcm©
«ri» !sln*iiil'/««!.
5« Ttie tfW»rsphjnnp<»r t» more self^ctlve, !,«»« tt ••Hiitlrj"«i8»i«»«>
%• Ho new liisB of^ lntro.''uf><»a In the ri»aetlMj •MP'r*!© «»Tc<*tit the

imiii %'Mel3 Rr«» )f»ro'''iioet'' KB & ITPIIH of h'^^'rilrRln,
A« I* rpsnlt, tfi tisp of rrêln h«fi^f efrsfIff 1«»IB to f» srrr«t fxt.-^nt,
the f»ro'^*»'i«rc of detcrftLjn. For pvamp*!**, F«r4'»l»» test (25) for
tbp rairrap-r^ffl rVtsT'tlm 3f b-ilogfUK tn or'» «l€« cor^'-oaM^R WJPB
frently tisproveil onf* a«wrl *'*'1*'<^ ^'*y tfw intr'*'imtloo of the r«»@tn
pnot tt'chntquc (26)*
lon-exehfiig* r(*Bln <*lfio ficts «« *n e f f i c i e n t CBtalyet,

I t onrt brlop hytlrolyftld «n(f«r r»l«ttvi>lv wHil eon^litions, i^ttltout
Uie Introdtiottjii «f amy nev tonii* It iti^ tberpfore, adiTBntageotMi
to a«« tott*M;ehMii« rssfiia In All tho»i» r#eetl>ti« «rhoro hyarolynts
i« j^rformod prior to th« dctoetlon* Boteetion and deteratimttoB
of Allptiatio mtl/lo* o«<f osfffrfli (20« fi7*29) w^y he (slven a» an
ex»ar»le of ouch • OMI of th« reotn hciadt,
A« i t h«e hoon |>oi»t«d oat ahave, ion-«xohange sorroo

woot e f f i e l e n t l y no « oorioration teohniciun, A lorô ntmbor of
ion-oxotiango oMiterials are icnoim today, both orgf>nl(* and
inorânio (50), vhieh oro ostonoiirelv need for tho oeparetion
i^
o f • v « r i « t y of •uhfitaneoti* T»bl« f l tttiMitriistte mtnm of tii«
roof»iitl)r a»vl9p%6 M i i « r i « l » v l t h thwlr onalytlonl »pplloattons,
Atihotigh th« d«Telopoi4»at In thlit ft«l<f hat hmen <»oor!ioo» durtne
tlio Ifiat •'!«oa<So« r»«o«re^«» ar« » t t l l oontlmsod te e b i d t o
«yntli«tlx« ton* wi^terlnlw »rt)toh »»y •«rve h i g h l y a«1«otlT« f o r «
cl?»»« of iyoii»r»o«w»dlii o r mBy not «» » npeeifiti n^sorheni tttr ©
p » r t t « « l » r •ob«t^n«e. The mT l i t l e t whioh uny lcm-exehaiig«r
nQ«t poosoos 111 ord#r t o hove vlrte iippltootliMafl uoy be snBnnariasfid
»m f o l l o w s !
I, The m a t e r i e l »tt«t h«» v i r t u a l l y l « a o l « b l t In »tr<in^ly aflr! or
alt;olln» solwtlamB i»« snob »i^<1i» ar« otteu pncoijntf»r<pa I n
r®pr90©»»lnr work,
2» I t s lon-.exebaniir<» cppeettv wuat be hl|?h eoaiiTJs to en**nre «
prt'c^tto'I wtlltty,
5» It«i aorptl'W ©n*i w l i i t l m 1>#hovls»ur raiist bf r«plr! so that
eoltffima enn be op«»rat«a «t r«flsonf*bl« r n f e a .
%• I t a raslatanoi) to a t t r i t i o n nuat bf> ftood «o tht: t oaliwnie
een ba lo»da<l and e l u t a d siaay tlinoa without Bmvi^re e l o g f l n g
or ebimnallinc*
9« TiM ionâxehaaKor aoat be of « r«>produc!lhl<» behovlotir ao t b a t
a «1nor ebaiiia I n tba aotbod or ffiaterlcle uaad f o r prapifrattoo
nay not eaoio a a j o r obaiifoa la I t a parfomitnee*
6* t t a a a l a o t t v t t y f o r tho aofbatnacaa of l n t « r a a t wast b« h i g h ,
ao t b a i ^ a eoavaalaat • • p a r a t l o a batwaae tflffarant atibataaoao
eea ba a f f a o t a d a a a t l y .
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7* ff the MimrattOB I0 i»B &9p0n6tint th«ii the •obstenoe* t o b«
wif%e4 •?« tt%l# to eowp^te • u e e e s t f o l l y with tht hyilrogan
lonit for th« ftmetlin^l f^ronpB^ trithtn the arc^lleble rnnt^m
of i>ff.
<lfiafilc re»ln« arc quit© satltfiôtoiry fi« frr c« the «ôve

•fvpis <|aelftles am oono m«<l» noi»»v«»r, wtion tb»y i*r© ooBiparetl
for th«tr stnbllfty at ol«vatod t«mp«r«turt» nw^ un<^»r fftrong
rrdletliin* tf»«»y nw* fownd to b«» Inferior to th« Inorgi^nle ion*
«»iretj«nff«r«5 ( 6 t ) , It 1© dii« to thla roiiffon thnt #>o tntemst ve»
rfvlv«»<! In thi» liMi»««ohftiiiR« «t»?/»y of tnorg-f'iilp ««»t#rli»l». They
can holyT«*«'«t wetf^lo,
5« S«5lt» of het<>roi>oly«et(l«,
4* Tnoolohl^ h»K8eyoiiof«rri»t«»(tT)»
9* Synthetto fitiMiino stltenten^ And
6* 9ftseellmi^0110 tnorgf^nto oxofiasiero^ f»«g« »«ro(>rt>lri« oîilts
and potnonton iiolyiitiofifhfitoo*
C*fl«il»|>hl«tt» 1C«A«lCri»«t9 l.*n*n»C!tiil«> t>iiA 0«Alhertt nro

tho orif tiiAtor* •»§ wmin eonirthotoro lo t h i s ft«ldl ptort foul arty
MMorphooo «»tortal»« A«Clo«rft«l<l «t al« h«iro eontrtbutad
otKfitfloAiitly OR tho oindiea of eryatalllno •ireoniiMi pbooT>hcto
whilo 6»ff*llttiieolloi' vork has boon MOtnly on tt» tharwodynaale
itiidloo* mot tvotity y«ar« liovo ooen » trp»«ii<!oa8 8dTt>ne«R«cit
14
to th« f i e l d of inorgcnie ««t©rl«l», wtileh hi*» •arcell«ntly hemn

r«vl«w«4 by Y»»«ly aad pelcarek (62t63)f Albertl fin4 Cocteiitlno (6%)
9fei« a»in drewhaok It) the u«« of tnorgonle lonoovehoogo

laiitfirlel* h«»» be«»ti tb©tr poor ropro<!«etl>tllty ami cbniBloal
Rti^bflity. ntw to thl» rentBtm they find United Oftplleiitloii« In
•ctnal anrt]yii#f> p«oh np tli.>?5#> of roc':9, ®fne»rPll nn6 Alloys. Ffooi
thto point of VIPW further iito<St«» on tJsfs elaoo of <*o»potin<S»
«Pi» « » f f n t t o l , Since the iaf»t«rt«l prodHC<»«1 in tMn atudy helooge
t o th«» firat ei»toff->ry 'ôa T»ar the claaatf lej'tl >n ««<!« ebova) our
me'in mvmhBtim wtll be cm aM<*h i«ifiti*rfal»#
Tha Inaolttbla ©ei«i aalta of polvTnl?»nf tsPtiflB wt-r©

Inlttfllly obtalnati e» gels with no d«»ftnlte compoalttm en<3 not
v«ry atabl© towards hydrolyala of t h e i r eolr^ rro«pa, Saw
r©»a«reh«a In thla tttsl^ have now led to tb« ajTsthoula of aavaral
astch/^ngara bavtnf « fixed eonpoaltiim and e well daflaad oryatalllna
atrtietttra (69»85)« StiMsa double aalta nanelly ahi^ a prowlelnt
loB«»a«eh»iiga bataevtour« they have reeetvad niieli attention raoantly*
Ooneei}ti«ntly aevpral double aalta have been prepi^rad* £ireoDim(XT)
plioeplioeilleate (S6»88) ia probably tbe f i r e t of thta kind^ wliieb
hae eneoeaafnlly bean need tor the plntontaa laolation* Tit««ini(nr)
fOioephoailieate hat elao been oeed for the eeparetlon of radio*
tttieleidee (99) • Siailarlyy t i n (TV) areenopfooaphate (90t9i)t
prepared to tbeee laborttorieet hae iriboim enhanoed ionêsebonge
propertiee for eone oonnon nM«ta1 lt)ne« Table I t l saMnBriaee the
#1% -J
t J*
« S C 8
I
•^1
m
ft*
8
»
tfg
III
il H v
M
a
»4 f
I I if
I i»
m
I
g «• • •
S
i 41
!
I 'taf**' %#li»' (««i N;^
»11 jB
II ¥1
it ¥1
if ^
F !• I* I* I
4 it 1^ i 1^ 4
8<
0^
#Mt #Mk 4«^ ^^

«
Jft O 16
8
I ft ih ^ ^ ^ ^
I
h « ••I IN
!*• m
^^W I^MI
tX^H IM M
^^^ 1 ^ ^ 1^^ ^^^
t m U
i H i mm e ^^* T^ ^ ^ ^ ™ W^
s i 1 si
8 ff iiai
€ 4fO
•r «-«»
(M
KB
^-'^
J^S.
*»-&
I •I w £. C^ «•
i • I
i ffS
'^jf
wO^
B**
ff*»
mm
sjs
ai«\
mm
^**
<<«»
MIÎ
f*m
§*r%
Jl«< Se« Mm Bm
I
{]
I
i si i I
?! #•*
• I-
a * i
m
i
m
i
m
4 J^
m m
i
iv
teporiDBt dioicAU iMsltt pr»p«r«d ao f»r wltii •(MK» of tb«lr
0B«e th« <l«t«ettofi mid trnpamtifm aMtbodt are 0V»tlabl«

fdr iMsy eoiRfiouBd In fi fiftmiii aeoiple, tbo ae«t proiHleu artt«« of
tta <l«t«rmtnAtt<N), Colorfoietrt© »«tho?f8 tiere b»©» extresMtly
popular bfionufte of their Bp«0d« stoollf^lty, end eeeurôy* 1ti«
ffietbade hare been used •xt(»n«ltr«ly tn c l l n i e ^ l ebeatRtrsr (10%»109)
find a i r pollution f i e l d * (106)* fn eoloriaH^trle afialyaia, tbo
» ! • Is to ohfinfe the teat Bubatnnee Into fin tntenaply colored
ohrowo8?cii vhtch w i l l absorb) with grreater Intensity fwrtlter Into
tô v l e ! b ! e , so th^t tb«» mB»v of n l t r e v l o l e t nbaorbtnj^ baf«%groand
wntertrl *»tll not Ititprfert? In tbe analyala. Fortbermore, It fa
preferre*! th«^t the ;nttbod be hlgbly aoleetlyc for e l t b e r <»•
eoiRpormd or B froup of cowpotinde whirh b«ve e reeeting ftmctlonal
gronf tn eoiôn (107)« ^ very l u n e nnnber of eolortraeirlo
metbadt bave been eoeiplled by the Snella (i09)*
Xi vtaw of the above Vam follovtn^ a a e l y t l o e l aapeeta

Of ebeaitatrr liave baen ati^lad la tlio praaeat works
t* B*v«l«pwnit of a now dataotlan and datamtoatlon prooedaro
for aaliio aelda^
8* fpaeifle dataotton of anoroaa and frtieio»e,| and
9* Syntbaal* of a aaw Inorimile ioti«e]t<4iango Material foDvlog a
potoailal f o r awtal t<n aepaifatiai,
flM followtag ebapter glvo* an aoeooat of tba •alaetlva role of
^>
lU
«•!«•• A M t t s H l w Mi4 •p««tft« i » t « « t l M i fPMNMhnw f « r Iit««l4lis«
• • t r t « i * t « m i i H i t i « i ttif t 6 l » Mii»« aoM* f k U vvilt t« •iwrnwyt—<

to ^ A f t ^ r t n « tm etiei^tAr S?» • • p « e t f i « «#t«eitMi ««tlio« f « r
M«ro»« Mtf f v o e t M * has %•«« 4»««rito«i w i t e i rvsto 1i««i«« uliila
to «li«9t«r • tiM • j m t ^ s t s M M ton«»«xtfii«iii« |»r9i>«ril«« hamm %••«
« ! • • • • f • •«» te«iv«iit« t«ihMnK«liaac« mitvrttfl mmmtf t t o ( n r )
•rM«««lli««to« flito • a t a r t a l ! » • %««ii u t i l i M a f o r aoa* toiMHeat
Mltlll •»f»ftl«tlflll(i INI l i s OOlOMKi*
19
piiKHEltCRt
1« K*A.Xt»ii« m« O.B.NMirt* JÂM.OkeM.Soe,. 22» 1%€0 (1959)*

8* G*D«(%triiiit«iiii "Aaiilirtteal Cli«wisti7*» ted £««, p» l%8^
JoHn Vll«y « SoRii, 1l«v Toiic (1977)*
5 • ^•F«P@rl»« «S«]i«retton of Hit* I Ions t>y Aatoa Ei<dickiif« tii
Ntittiir»« of H^rootilorle oeta endt HydroflKorte a«ta*«
Affonti* Hetlaiifil UtDor^tofy, Amcmiie, llltnotft* (A Report
pfprnmei for tlie O*S«])»f»0rtoent of Bn«rfy» iite«19'!ni)»
4* 0*T«At *t«}iii]»r « i i E»A*iKalilM}tto«t lta»t«Jf»tooaii«Qli<iii«9
%, i t (1!«I9)«
% If*Ariel anâ t»Kiro««» Tolanta,, Sj^ 214 (t961)*
Aeto. 12, *3S (l%t).
<{p 206 (i96S)«

8* F»A«INmoQii« ¥,o«ltoll»ii<3 emd n^n^Smith^ Aaal»Qi«M«« ^ ttt3
(t96ff).
9* V«A«1to»Brteicnaiip p»^«j,6iorff«olitirg «i»l O.dotrioo,
if.Cbrwiioin, J S **9 (i971).
10* C.IUQbM OMtf J . n i i t l o y , il««l«cailn,A«t«t ^2^ 103 (1967).
if* J . n f o r i t , AMl«fito«ii*, ^ 5S0 (i9i0)«
18* K,A«Kip««o ond 0*8«N»ont l*At*Ch«ii«Soo.« 22> ^ ^ ' (t959)*
i9« C.A«Kr»«o, G.K.Noofo ana P.ltolooii, ibid, 2Sf "^^ (1994)•
i«» O.nwOlirioiiiqi, •itealytUiei flUoMiotrsr** ted Bd., p. i9i»
ôlMi inior A 8Mft, now viMrtt (1977)«
20
19* y*V*Wi»tt lf»QBrt»lii end S.Z.Qaffvslity ilii«l»Cbtn*Aot«9

}§, 97 (19661•
16* S«Z,Qiim0h|« N«8«fl«thl imd S.Raiiat An*l*Oli«»«t %g^ 1159 (197(e)*
17. S«X«Qiir»«tii and i i , 8 . i M t l i l , li»t«, 42^ l%8% (1975)*
18« N«FiiJliiotOy Biill«CbMi«&<ie«Ja|K»a« ]0^ 99 (1957)*
19. ll,r«Jl«oto, tt>l«, 20^ 5»i3 (1957)*
90« N*Qiir«iitil« 8«JS»Qart«lit mafi S.C.SIiigtiaty Aiiel«ehla*A«t«,
%2^ 1781 (1968).
81. M«Qiir(»«hl» S.ft.Qmrvahl OIHI Tl*?:ebr<i, lbt<l« 4 ^ 169 (1969)*
28* A.ThaJl, Nlppan ^«(nfeti ^âahl, Qtj 1090 ( I 9 6 0 ) *
@5« Vm'B9armh<e>im9rf 8,Crl*on antf S»Yâiii« AtiaI«Oliiflr«Mt«y
89, 988 (1965)•
2%» ff*8:«t»llii»ii«,, T.We^rl imd TB«R«salcey Iflppon Kagelcti Z««8hiy
2 1 , 907 ( 1 9 9 * ) .
29. F . F « l t l , **!%p9t Taat la OfiGnlo Aaal^rsla* Ela^vier ra^llahlBg
emxptmy^ Anfttarden, 6tii £a», |ip* 85, 95 And 96 ( I 9 6 0 ) *
86.S.Qtir»ehl anfl N.B.flatlil» M i e l , O M « . , %2, 118% (1979).
87. r.V.Weat and If.Qttraaiilt ABal*Chlai.A«t«t ^ 906 (1968).
88. lf*Qiiraahl and 8«2*Qttra^l« I b l i l , 2|p 108 (1966).
89. N.Qinrtaiil Mid 8«X*Qiiraalil, Aaal«Oha«*, J|8^ 1996 (1966).
50« r . n a l f f a r l e t i , *X«ii Esdiaiiga*, pp* 18-14, MeOmir t r i l l 99«k
0 » . , I n e * , Hair tl»tt (1968)*
51. H.r.Taasar and A«8ia«k» AnalÔiaa*, "H^^ 968 (1979).
58. V*R*Ba«|ililii and f:*p*ltofwlta, Iftld, ^ 8%5 (1978).
55. l.Blaalfta, K.F.Janaattg lf»l«iaiibaiigart Y.B.NtttKlii, lf«fCl»ts
aiMI J«8toeiNmart J.OhtaMattttr*, 1^7« 507 (1978).
5%» I«Bl««iiHi9 K«p*jMiseii and V«ltoaM«Baf lfleroalitsi*iUit«9
879 (1977)•
95* BtWmmmnWf S»8tilbtiat«« K.ltkrotski aad B.Tslivslitta»
ABfll,Oiito,A«i«« 1 1 ^ 885 ( i 9 7 t ) .
96* P«R«Iity^«fi9 T«A«P»it«r*citi and <l»J*Alh#rt8y Aiuil«Clli«a«y
•2;i 733 (1975).
37* 8*A*A«lfiiBs«f«lll end RftRo««A)«ttl, Aaal«CI)t»*A«tA»
S2fi 35 (1974)t 22^ 883 (19T%)»
3S* M»!t«lJiatst) end G*T«7«A<I, ÂChronatogr*, t6$> 85 (197S)*
39* JthmBtlte^ ABal«Olitii«A«%«p tO»» 307 (1979)*
4MI« R*A*9ad!c;)rai nnr! O.H.MMrrlaan, Aiiiil«Cli«n*t %^ 838 (197%)|
%2^ aaS9 (1975).
%!• W.AMtaii, B.naflirer and Dt.Stovtr, Anai«Cblia*Aet«y ItO^ Si
(1979).
4i* A»!llr«»«« and D«l»hil9 ^•]|^dl4»eoal*eiien.« ^ h7 (1977)|
^ 211 (1978).
%3. N.Kfitm and J.C*V)an UMUt âl«Iitft«y Atl^ 991 (1978).
%%• NÂbe fnnd K.iai«« 8aipa»Sel«Taetiaolft» |%^ 335 (1979).
%5. «l»Ch«l«lovl«« end V.Steant OmamtograpliUy It^ 99 (1978)*
%6« A.S*9» and 8.1.IMiit l^l8t HJI 998 (1978).
«y« ••ii,tt«BliMPfa» • r t . - l M f t * >r—<»8t>t %1» 98 ( 1 9 7 i ) .
%»• CÂklllnnll, l . t i m i Md V.MMMiMt^ Anal«eiMMi,, ^ 165 (1979).
Ii9* 8,Slebiik and B.enaaldTf Ibid, ^ 1%3% (1979).
90* y.Sdittabraolitay E*MiMltt]r nad a»4»Bb3rica«rtaf a.OHroiMtof r . ,
17%^ 351 (1979)1 132, 63 (1979).
5t* A«llBiea«« KmWnruyB^ T.NttBkf* Dod lf.n««ti«k«, Wlppiin i:ag«>kl
l&itBhl, 1655 (1977)1 217, 70S (1978).
9?*« A«W,Wo1koff ©lid R.M^Lftrofte, J.€^rQiRiiitogr«Soi.« U^ 35? (1976)•
59* «f«F«Coluratoô nud R.f.Ed'fyy Aii«l«aiMi,« fl^^ S{l% (1977)*
5*» r,l>«ff«'nfom and R«1%roqae« Colloid poljnn.Scl*, 555* 545
(1977).
55» T»BJ^lt?lewenB, Anel.ChtiB., *^ I H ? (1975)»
56. J.fCorf<tKoti »ii«! U<toedl, Talititr., 21^, 1035 (1974).
57* Jm^nVnisoh nnA 1,Stiffen, Aoal.Chte.Aota, 22^ ^^'^ (1975)»
58. K.Ftr^lcl, O.Toehllg ft.nlr*?y»<wf«, y,Nl6hlte«>*r« end T.^hlpetsstsa,
il»ld, 7«2 (1973).
59» fl*I«l*i«koir and f*»TlB90f«<!>v, Sî.i^ntl.iailia., 22» 1023 (1974).
60, U.N.Cvjr^tleciialn i»nd M.Pf.Vacctle, IMd, 2£» 5<^5 (1975).
61. C.B.Anphlttt, •tnorgniile Ion Pxoh«iij^«r«*, r i t e v l e r l»ii!ili»blnc
C<mp^ny^ Mm»ter6?»n3/\j!in^4m/t^%v YorH (1964)*
68. V.Ve»«»ly and ir.petearelCy Tfll«otR, Ig^ 219 (1972).
65. V.Vesi^ly ond V,r«?c«rtlt, Ibid, Ig^ 1245 (1972).
64. G«Alb«rtt end l7«C!otiteatliia, J*C9}roi9iitogr., 108, 5 (1979).
65* R«r«Viiltan, Aiial»Oh«tii», 4 ^ 398R (197%).
66* ll.P.Wiltoii, Itild, 48y 53ft (1976).
67. R.P.VUlton, Ibid, Jj^ 3611 (1978).
68. R . F . ^ l t o n , l»)ld, 2£t ^'^ (1980).
69. A^VtekUr «i»d F.Tbilo, e.Aaorf •All^«Ob«iii., 346« 98 (19M).
70* A,0lei»rfl«ld and ^vAAStynes, .l.tnors«lla«l«Ch«»,, 2£^ 117
(1964).
2O «!t
71* 0«A11>«rtt« r.CvCkilltt i;»eo«t«tttiiio aB<! R*forr«c««» tlild,

§2, 97« (t967).
72. K«R«K<Milf »»« E.MByn, ibid, 22^ 1193 (1967).
79. i«Torr»eeag fr.cost^nttfio and N«A.NiMt]«<;t« J.C^rowatai;r.«
2 0 , 9«l% (1967).
7%. O.Alb«rti ckod n.Torrf>e4Mi« J.fnorg.Woel.Gliim*, 22f 917 (1969).
79. O.Albprtl^ U,c;o0t8iitlno» F^dlOrwiôrlo, P.Celll i^nd E«Torr8eii««
lbl«t 22> ^ ^ (1968).
76, A.Clfârfleldy a.H.Snlth and B.H«»«<ind, lt>t<!, 2£t 277 (1968).
77. O.Alb»rti ooif l^.Torreeeii« l b l « , Ô, 3073 ( 1 9 ^ ) .
7d. A.Cl««*rfleId, ft.lt.Blefsluf 0»«f J.A.f^tynee, lbt«, ^2;, 2S%9
(<*>6JI).
79. il.AlbertIp 0.Ci>6tri»tliiOy F.dlCregorlo ©nil E,Torr«©c», Ibid,
][!, 3195 (1969).
«0. O.Albertl «ii«f W.A.Messttoci, ibid, ^ 17t9 (1970V.
81. lf.«y.FiiU«r, tbtd, 22b ' ' ^ (1971).
89. O.Aibertl, ir.Roiiteiitliio nnd L.2tliik«i, Ibid, ^ 39*9 (1978).
85* A«C?l«arfl«ldt A.W.I^nate, A«F,|«idlae and J.N.Trotip, Ibid,
Xb 1099 (1973).
8%. O.Albtrtl, S.AUitll, l?.Co«t«iitliio, ll»A«li»«»tte«i and
F^Torrfteea. I«Ni«Bx0iieng« to tli* rftK»«t» l s ^ e t r l « » , Soelcty of
Obvttlorl IndiistiT, p . 918, fjondon, (1970).
89* A«OI«ftrri«ld, O.R.HoBOOllas SBd fl.R.Bl«»»liig, to J.A«Nirtiislcr
m»a T«l8ir«tt»*, •lOB.ilxelimig* and Solvent Rxtrfl«tlcMi*, •!»• 9,
Oh. 1, MBrMl SelElwr, lltit ttorfl, (1979).
86* 0.irauM«i, Kcrnraerf i e , |^ 173 (1963)*
24
87« K«T«Bar«iilc<yva and G«lf»fl«<llanoT«), nBdiokimiyOf J%^ 223

(t97t).
88» II«OOR«| F«!SehQiilc«iiy V«f)ot«»lag«n«UR«B««tsl« and N.B'hofit,
90. K.a^YHrsfniffjr a«d A«A.1Cli«tt, tbia, %t, 241 (1979).

ft. 1t»G.Vlir»tm«y eii<f A»A*lClii»ii|| tulcofc**, £2, 525 (1978)•
l ^ t t . , n. It (I971).
93# «»0,f5«ttn», W.F#n>eoi80¥« an^ I .s,Botet»laov«, ?!h,f»r«kl .Khtw,
(Letiingri!*?), ^ 2*32 (1973).
J«l»«»» S i , 2923 (1979).

95. T.lftaht and I.Fcu^lwara, fCyotr mig'^kn Ktjîtkn fCwotc^ûatm fbo,
J2^ 25 (197«).
96. M.Quraahl and R.C.ICetiahlliy Aoel«C!ft«»,, 42, 169 (1977).
97. F«S.Thiii<f9 6«S*!{«a<tl3u and J«P«ftaifet, C^tn.Anal* (Varaaw),
84^ $5 (1979).
98* NtQnraality R.KnHiar ana R.C.Kaoablk, S«^«Sei« A Tfiohnol^^
12^ *t5 (197S).
99* lf*Q«f«ahi« R.Vonary •.Sbama and T.IRiattt J.Ctironatogr,,
t i t . «79 (1976).
too* ff»Fv4Soroff vnA L*mvirr«| e.R»A«nd«Soi»<(cr.C., 279t 11^^
(1979).
101. K.G.I^rahnajr and A.pramaOaa, 8«|MI.(NS1. A Teehnol.^
I t 795 (19«t).
m
10S« KvO.Tarahaey and A^Frtneda*, J»Ll(|«ild ClinMiatogr*^
%, 915 (1981).
105* K«G«T«r«hfi«3r end A.Frtwudas^ lbl4« kf 1249 (1981).
104* H*f)irl«3ry **Fi«otleal Ollaloal BlcM^mil*tr3r% 3rd Id*,
IMt«r»eleiie« Polbllshers (BlYlsion of 3<Qltm Vll«y «t Sons Xne.)
H«w Yortt (1963)«
105* R«J»n«iiry, •Clinical CSiwwlstiyi Prlnelples «nd T«ehnle»*,
H8rp*r and Row pabllshere Ine. Hov Toi* (196%)•
106» M*B*#oo<)il)», "llie (Shemlenl AaaljrMle of Air Pollutant**',
Je^m Vllejr A Son* Ine«, H«w York (I960).
107. E.Sawleltl, fleetind«Cfeiem.Progr«t 2||^ 249 (1961).
108* p . n . S n e l l , C.T.f^rll an<< C.A.Snell, "Colorlwetrlo Metbods
of Aaaljral**! Vol. fffA, n.Van Hoatrend Co.Inc.Princeton
N.J. (1959) (And othrr Volnrace In the s e r l o a ) .
muFCTtw mu: or OUP^NTS I S tm. rnESFwcE OF CATIQW PXcmmE iiEsiiis
TO Hn^^poBM ron rm BBTI CTKIM A^T^ PirrEirKTiATioii or ACIDTC.
BASIC Alio m^mukh ANHIO mtm
J.
ti
A«to« MitHc are th^ batltflii^ blootea of pr9t«iii«t vtite!}

a«1(« Ofi a Initio {»£^rt df i*i« Awlsiai bodjr* Tlifty ftre eailioxsrlle
•«t<1ff to wttteh M
( M» liydr<H(9n ^ton hea !»••« r0fiiaii«il by an is«itno
groupn '"''^t* ^ ^ <«in9 aotdTe tbat ai« olitatnat! from protein*
art alpha anlno sctda, with the aislno grooi) Attaehod to two
o»fl»0ii atofR fiaxt to tha eorhoxylle groti^* In addttlisMi to tbo
oerbosyltc r.rotip »Bd the omttto groofi cslpha to it^ aoaie aaitno
ael<A» eootatn a aaeoii^ oarôiEylie group (••«• aa|>artie aoiA or
glotoorie acid) or a |»otoiitlftl e&rftoatylle rroup In the form of »
of^ffttoxonl^ (e»g« aapnraglfio)* fHosa are oalledl ael^le nnlno
actda* SoM) oontaln a oeoiMid haelo gronpy trfttoh awiy he mi
anlno groof) (oag* lyatne)^ » pro^nldlno grotip (argInlne)« or the
ii»faasole ring (htstl^lno)} th{>e« are o«lle4 haale amtno aelde*
Son* of the enino aotda oontatn hensseae or heteroeyelio ring
•yoteniOy phenol to or aloohollo hyi^rmcyl grottpo, halogeiia or
•itlftir otoeia* ra<^ of theae ring ojreteiao or foaetloiial groopa
laKlergooa Its own tirpleal oet of voaottofio.
Stitee awliio aotiâ are the Haeie eoBotitaento <rf protetno*

tlietr dotoottae, detonainattoa end oeparattio iMthodo or* volnahle
to the hioohewtet as an aid la the etooldattoo «r protein atroetofo*
tlw protetn ffogaente are degraded to anino aolde, vhleii miet He
dotofnteod* A oorvey of llteratore for the loot ten yoaro hae
roipoelod that a taiio nonpar of awthoda have boon devo loped for
tbooo analytloot aapeoto of aiilao aotdo (l«8t)« ffo aontloB a few
(-4 i
• odllaloM thill imfT •l««tr(iiilir<MifltQCr»|iliie nethod !!•• lieMi

^milofwA \if Stt<!«lc0 miA r*rviiftii«t« t«r tiM Mfmmtton of 25 m i s o
•elUt {!)• ststlarlrt tli« Idtimttf ioatioii of miiftiMil mtoo ftettfs
mid rtlatttd ooK|>(itniA» tiy ««im« of ttotoMtttod oolamB eliroiMitof rafMliy
ban IMNWB diiir»lof>«4l by Omttiw ernd 1%IIM{>«OII (8)» Aldaromi ftndl
FfMiôvii (3) b«ir« tMd» n iltff«f<«»iitl»l dN»t»nniRfttloa of a nlxtorB
«^ anioo aettlOf spcotroiôtOMOtrleally* Al»Oy a oao»tft««Bstonal
ttila-olAyor ohraiietoirit]»hie tMitbodi for the dotoetl^n of oemn
anteo eoidi* and « two>»<lltt«Ba tone I iribrowatograpliie ntatliod for ilio
imalyato of ortnarr awtno aelAii liev« baen ao^^lopod (%) l>y Btekel.
I«n«4meliango ehroiii«to^ra|»tty oan b« iiood to oapareto

eoflfilox etxtaroo of aailjio aetaa oonesonly aiioomitarafl to l>to»
eliMitatry* Oap^ridtni?; on th« f^ enntno aetda oen oxtet tn on« of
tlio following thro* oiatoa of aloetronto 4Brtioi||E*t
m^ im^ Mil
k • e
roiw Bf oallod swtttortdiiy to tlio dontsast fom «t tiio pB

o o r w y o a d l t to tiM tooolootrto point of tHo oaino oeid* flmo,
ot o f ivoB iRt tlio oaitto oetdo oon bo ooparototf teto tbtoo gronpo
by botaf iôoo« OMOOtotvoly tbrongli on onion ontf ootton oxobonfo
•olonn* flMi nnobantod sirtttortona will poot tbroogb botb oolanBO,
9o
wtili* positl'r&ly and ii«fiottvely c^firgttA amlao AGI^S w i l l eaeh

be ititelned liy one 9f ttie colunos* HM graop* esm further b*
oubalvi^cd l>y ohimgtng tbe pR* Iteeetit y^t^rm titîre wltnesMKS tmieb
work in th!« dlreotlon A1»O (28>»%2)«
Ntafaydrin I0 tho m»et eenslttv® reagent (%5) for fittitno

aot<l8 (r/riBsd ^ - ) , I t c.^n bt» uft«d for their deanln^tloii* Ho«r«v©r,
prlBifiry «o<1 »e©<«i<!rry rtllphetlc «eit£ie«» slBtril© flsKlMB product*
of protolnB stieb o© polsti^ptldMiit* fltad e«eo»%lc acM »l8o r:lr« a
po«ltlv« t e s t irtth nltitiv^lrfn, Anotti^r t©»t {kk} for <>^ «>>@»liio<»
oorboxyltc? Bet**f In bfloedl on tr®«stia«»nt wltb hypochlorite or
ehlortimlnomf (%5)t the nldehyiie fafi»«e1 belitM det«etedl wltb
fmjhslo-sul^tuirottfi »el«l but tbe s e n v l t t v t t y te poor anc^ the t««it
fnll® t»lth cfj«potjnd» wblfb ar© oxidised by tlic r®ttp;©«t, aoeb o«
t b l o l a , pâfnlnepbonoly nItroeoooeipotifida «ii<! Inongianle raûetonis*
Falgl (46) d«aerlba<9 e taat for s a l t s of a l l p b a t l e iKttd

•maatli? awlnoa baaod 00 tbalr fualoa with dry poiaaalna
thioeirfmata and da toot 1 cm of tba hydrogan anlT^ldte prfiMAuoad*
Vttla t o s t vaa a«tandad t o a gaiiaral taat for amliio aolda bavlng
earboxyllc^ attlpbor and liatdo gro«pa (%9)« Aeoordln^ t o f a i g l f
Mateo eail»0Kylle aolda, aronatlc aailno aulpbo aolda aod ooarpoanda
oontelntng botb an aeltfle bydrogan etcMi (lltl|^, m(m^ «>e0on, iÔJR«
groupa) and (In another poaltlon) a baale nitrogen atoai, alao
behove lite* ealta of anlnea* The teat ean be applied for iwlno
aelda fa preeenee of free imlnee, bat anlnasrand eoMMmlMi eitlte
toterfere* fftle t e e t la not applteeble In ^ « preaenee of
org^niti eonpouRAfi witleli fom «ot«r dNirtiii; tumim »n6 thmrmhf
evolv* hydrogen sisliftitlki from ifet* iôtnaalan tiil<»«srîi«t«*
lt»m«niitmg9 r»tln 1>«RAi hove be«n uMd «xiMif>iv«ly twr

d«t«Gtton ffoA d«t«mtnfitl m of orgtmio fimetloosl giôp* (^7»96).
Th« followinr pages •oMMearts* lêlr use for the deieetl.)n audi
(8tff«rentt«ti'io 9t eiiino etm^caylie oelde.
3vj
iiatao Attd •ol»iioii« «*r« pr»i»ar«d tti iNit»r tr— trmt

mnBoata* Afuvoiit fiS flolotloos of |M>i««9iwi dtobroRiai«f olirMM»$«,
BroMOt* end lo«ftt« nod a 0*8 volam hydrogMi p*rtnt«« •olutloB
« » f « QM4*
Bair«x 50ir x 8 (iO»90 «Mi»ti) ««• »»«<! after %h% usaiil

i«g«n«riiil<»i ana eanvvrsida into tbi> Ne^»faf«r. fli* r«fttB w««
w«tli«d vltfe deainerellsoa ««i«r until no eolor vr 0 obti^ttiod
with NtsBler*8 roBf«iit«
^* toaoywl toott t^ on* d r ^ of tho foit •olntton t^li«a In am

ignition tab« wnn «dded i» dvop of i f |>ot»»«itai p«n»«ttganiit«
oolotlon tmA 9*10 tott««o»olii»n«« itoiido (lMi'*«for»)« 1fa« oontonto
novo hoo«o« la o boiling wmfr batis for 0*5 nlnotoo and eftar
eooltag «1M onpofMitont lifntd « • • daooatod off* TIM bo«do «ai«
wealiod by «o«an%ntl«n vttb 5 or % portloBO of imlnotnllsod «»%or
and nore tronnforrttf to a nlitto oi>ot plafa« Aftor drying «itb a
f i l t a r î>or thoy noro f roatod witli a divp of ll»oalor*a raagant*
»m ianodioto light pinic oolor on tbo onrfaoo indioatoa tbo
fifooanoo of aaino ooii«
•• f^—otion of aoidio and nootral aaino aoidot foot A woo

9 •<
f « r f « n M d l»y t«ktiig i l l mvOv/kg^gOykêrO^/klQij/Ô^ i n pl»im

• f tli« ii«r»«i^tftiiet« t o l n t t o n * Basle aalao setd* ginrv e «•§•%!«•
e* Patent loo »f hmtio awtoo a«t<»t I f ooldlo mid iii>atr«l aatno

aold» af« Absent tite tost esay ^ performed \>y rtplaotag fNirBancs-
nets hy one drofD eseh of VH hydroehlorie aetd eta of 0»00!»l eodltaa hydroottde followed by e drop of 1<
potessiura dieliroisete solution* A |>e«ttive test Inatontes the
ftresenoe of set«lie Dnteo aeids enly*
r^
f b * toltmiim ttRlao a«tA« gmn a p o s i t t m t * « t t g i r e l t i * ,

lp»fif9llit«» HMt!)loiiiii«t ai-vsrlncy ^ •4il«Btfi«| B«>«liiiili}#9 leooinog
ilil«ontii«» l3r«t»«« airiKtiitii*, ht«tt41ii*» «y«tlii«« e3r«tl«i}ii« VfillttMi,
••fMirtgln^y Iso-lKooln^y l^lyeil^glyotney asiitkrtte aotd end glotiwie
tteUlm 1%Mi l l n l t of td«iitiflos^ttaii of those afalao Rotdo woo
dotomtBOd and tlio rooulto i»r« oanntariood In t^l^lo XT*
A iiOK«tl'<r« t«ot wofi obtained f o r lyrootnoy phony la I i^n too

(Mid tiTfttoplôw*
A aoadior of typtof^l org(<^le oowpomido on givmk belotf woro

tootod i>y tlio meQmmm^6 prooodart mt^ ifore t(nmd not to tetorforot
Wrdroo«i»opo on<g tliotr derttrottypoi Bensone* tolnono« etilorofoTia,

nitrcônsNmt^ broMlNnisoaOy oei%on tetroehlorldo.
Aoiî OxellOt oootlo« fofwio oiid proptQiilo»
Efliorot Oto«a»y oatoolo «nd dtothyl otiior*
2||^gMt|j||^t VltOBOl And OfOOOl*
O»i%oliydroto«t eineooo, frvetooeg ooerooo*
mtrtloit yropionttrtloy oootonltrllo«
ijgjgî npipriiMitto, «Biittto, ^ntFimitBo*
gitOBOOt AsotoBOt otbjrlsotliyl kototto*

Aleoteoltt Mttbanol, ii*pro|»aii<il Mud iM>ttt«iiol«
A«td»»t Ac»«t«i3l(l« and t}0»sninta««
rjibl«« 1^ to tit mmmmrixe tb© ©ff»et of fon&iga

8tiT}stni}oee OB the te«t for a l l th« tbre* typ99 (neutrttlf ael€lto
ond baste) of the ontno aolds* One eminQ acid fron eaoti elas«
tins becm tek«ii Aft e repreoontatiiNi.
34
Tiaig IT
UMiT or in^TiFXCATiQH or Acinic* BASIC AND

MEfnmAL AMINO ACIP6
• ' ' ' • • • •
"1 '" " •' i

Amino acltis Tolttne of Aaouni
ecmcrent nation imlno eeldv doteofod
of Awttto
«ol(f»
J. -Alatilnt 5« tU' 0,09 88.8

[^•Alanifitt 5» to-^ 0.05 88«2
Ij»Frolfii« 1 X lO"^ 0*08 23.0
CSlyolnt 5x 10*' 0.09 18*8
Methionine 1 X to-« 0*08 29.8
l^roonine 5x to-' 0.09 29.5
t^nuelBe 1 X to"* 0*08 iCI.O

1II->»«rin« 5s lor' 0*09 86.0
A«|i«rtte eeM 2 X 10-* o.o« 133.0
ttltttMite aetd 9 X to-' 0.08 98.9
trvla* 1 X 10** ©•09 738.0
Afi;liiliKi i X fo-^ 0.09 870.0
Rt«tltftn« 1 X io-* 0.09 779.0
POR THE rrTFCTiqw or QLITCBIF. (75*o>«y)
' " • I I'' " 1

Forelifii »ttf»«»triic« Coneentrfttlcwi Volume Hfi^ptf Llislt of
tolftrnnee
Crotoaflifefn '<f« 2 X 10** o.s 2.3

Sttcroao 1 X to"' 0.2 1.4
Aod'OR# 1 X 10"® 0*3 2.3
Aocitte i!ettf t X 10** 0.3 IS.O
f3nrl4in« t X to** 0.3 ^-4
tmn»*n9 1 X to** 0.3 2.3

op
dU
htmr tar tounAnfn or ymioi^ roiriGN ÎBFT^NCES
yon THE mwtmm or AS^^/I^TIC ACTP <532ytiK)
•~~~—-—^ 1 — ' " 1 1

Foreign sabstniiee C^sieentrctlon Voltme nM»d Ltmti of
tolerancMi
Crotoorld«hy*i 2 X 10"* 0*8 2,8

Ba«roft« 1 X ±0"^ 0.5 1.0
AoCl%9ll# 2 X 10*"* 0*2 ^•3
pyrtrflfi© t X 10** 0*2 1.6
Aiii«iaiii« 1 X 10** 0.5 2.5
A o « t i o ©nW 1 X 10*"* 0.3 18.0
Btrnvsim^ 1 X t«** ©•3 8.3
A99ttmHf 1 X 10** 0.3 1.8
E t h y l A« i n * U€ 0.4 19*0
uwn or TOLERAwct: or VAMQPS romiCtN SPPSTANCKS
FOR TflF pRTECyTIOK OF LtSlHR (TiOvtMl)
— — — " " • " • • ' "f " ' I"" " I
(M) (wl) («f)
JMMI»OBQ 8 « lO"** 0.4 %«6

Ae«tto «eld 1 X W** 0.5 5.0
AiMitaait^ 1 » tlT* 0.5 9.0
MNRQMMNIW 1 x fir* 0.5 3.9
Bioaiiltftliyll* 1 X 10** 0*5 9.9
rVIM^tHMI 1 X icr* 0*5 9*0
I t l l t r l «»tb3rl I m t w i * t X »•* 0«6 ••9
rjnrKltiHi « S !«•* 0.9 9#9
liith]rl«ite« u$ 0*% 19.0
«)0
ntsemBtm
<Ri« onttto selde in fot»l« IT o i l nlve povlti've rftiiults
In the gen«ri?l t«Kt nnd so do ey»ttn«« eysteifict^ v a l i n e ,
a8p«rogin« ttnd flyeirlglrotne* ll«gf^tlv<s t e s t s are given hy
tjrroelne, phenylf^lnnln© POffl tryptophon* Isaleueioe, v s l t n e ,
r»eporn(rin© nnd ftjyt}yl%lyeine f o i l to ftve the t e s t for neutrr.l
evilno eei^s*
Vhen fin aqueou* solution of smino ieiot<! i s heated with

potassioB pefiiiABgf«ni>te in the presence of Qatiaii->«»xohpnte resin
b««^<le tn the H^-foro, <Seowlnt?tl m t«?re8 fiooe with evoltJtiOR of
iMfimontfi* A positive t e « t Is given by on© drop of Meseler^s
reagent on the resin h#eas, Itiie t e s t otmnot he applied to the
detection of oralno eeias« «s other orgonie fim«iti(xi»l i^roups,
sitioh as eeines, fwtdeo, intldes nntf n i t r i l e s , a l s o give a positive
t e s t beoense of the oxidetton of the enines or aoid hydrolysis of
tiw Qiîdesy inides end n i t r i l e s *
Sarprislnfly^ i f the resin heade ere need in Hs^-forsi*

s f o s i t i v * t e s t Is i^teined only with smino aeids* We snppass
that ia eonvsrsion of the resin into If«^»f9r«>|^ f^ swell freettim
of the R^ Ions w i l l he l e f t fm^n the resnltsnt very low otmeNsititre*
tion of R**^ ions in the hends v i l ) he snffleient t o smlce potssslwi
pomengenete e s e l e e t i v e oxidant for enino»aoide« bat inenffieieat
t o hring ehoot sold hydrolysie or oarid«tlan of other Ofianio
fwiationel sroopt*
39
H I * mmM w i l l e|>ply i « tli« otiMtr <Kit4aat« tfttt*^!^ Itent

« • t l M M hflv» io«r«r (nldntlcns putmittalt ilian p^nMrnc^nnt* th«
t«»t b«eoii«« a t l l l «or» mil<i«ilv«|^ v l t b h&mie ttmino-tiaiaK f « t l l i i i
t o roAot* 1li« r«e<iCNi f o r tli« a«i«tlini t««t f o r Imolo imtiio i>«ldo
1« not ttnown tint w»r ^« farthor rt^tietl^B of tlio B'**ioo ooiio«iitr«*
t l o n by prot9B«tiv>n of the anlno e«ld» ffito viow to o«fi|>ortotf
liy th9 fBot th«t i«h«ii a t>»«ie omtiioâet^ •olotioB to aoltltftod
wltli « <lrop of M hytfroohlorlo aetd I t f l w o « fiooitlvo toot In
tHo proooiiee of potaosttai brontiito (E S*%5V)y but not la tho
prooonoo of potnoolnn diohroitate (1 t«59Y) or ehrcmrate or
potaoalott lotfftte or hjrdroi^B poroottdo (fi 1*23V)«
Tbo followtni; tontattiro Moohantao la propoeod* ttilo

mathoif (9»p«iidlR on the tiao of reatno with e suX]M»oiile aold gronpf
vtfi'kly aeldle roolna do aot flmt tho tost*
BUCiUCOOR • 0 " J"' •?' ' ' > ll»0»€CKIf! • fLO

f Faobljr II *
oottdotlvo II
RHg Rfl
ilatBo aeld iMlno aetd
R#olii(Vo^ • ir^) 4 MiOjJl -—-^ lloolii(lla^) • B^ • MiO^

So loot tiro oxldoiit
luceooB • «»o > IM;*COOIIB^

I ^ toiootm 11 *
I osUlaiit p
Koto»aold aMK»i«B oalt
4J
ll«»ln(1«lff) • ft««»l«»r«« r»iig«iit —;• pink 1i«(i<9«.
?lo liit«rf«»r*ne>« ! • gtiwn by hydroortrbmtt «»lc<Miol«,

etherBy e«rhosvltc oelrt», |>^©no1B, !i«t?»ro«ycltc l»«8e», iHBldCB,
nltrtlevy umlnps f»ru1 •s«t<me«» Al<fe!!y<1«« are toBlly »orti«d on
rfttio 'bmi'^B and give a r«»artlBh plnft colour wMeh f i n a l l y ehnQ|;«8
to blBcic (d«p«ndlnr "pon th^ eonoentret low) whpo the »)r*«<S# crt
«flrpctly tr#«t#d with N«»Bl«r*ii r»»«*'nt, ftowever, i f th« roain
b«(^<1« Pr© thoroughly wn»h#d wtth water hefore n<f<fltl(Mi of th*
r©)Rg«»nt no pink or hlrHc |ir©el|ilt«tf l» o*»tfitn«<i.
41
MfBBBIKtgS
!• P«8ttd«kfi and O.FermnndlSt F t n i l l B i o l , , 10, p, %9 (1969)*

S« 1f*(l»0r8h«sn and 8*V«tli(Mssoii« Colloq.ihiiBO aeld Aoal*,
6th P.d, pp. BJ^tGh (1968)*
3* H«8«Ald«r(rrfi and M«T»I^naaleoTa, Pro^lÂnal.niliB,, | ^ 229
(t9?0).
%• n^Biekaly Theraplawoohe, 81^ 2053 (1971).
5« UR.Harrold, Jêhroâtogr*, 61, 1*9 (1971).
6« H«i:«hlwata antS S.Kato, F>lr«l0h«k«n4 Rokalcti, 116 (1971)•
7* 1C«9«marel, R^loalcwakl and V.C.Plahrlag, O.ông., IS, 299
(1971).
8. 0»J.1Crausa, J.Cbrometogr., 2!b ^'^ (1978) •
9* A.K.Sead and W.lC.MBthar, llleroolimi*,^,, 18, 300 (1973)*
10* A.Cimatantlnacii end CvLltaenn, 1tair«Rolnt*Gfilai,, i^^ 1591
(1974)»
11. K.S^lllKy K»P*Sohnaek«rK and R«ir*Gr««yg Anal«Bloelifta«,
St, 33 (1977).
12* S.*ni<N»n«»t B.Fnreh and R«Tateli«lip JmCkronatogr^^ 193« 996
(1978)•
19. S.T.SIiaytiy C.V,8«lth and J«0»B«eota, flid«Blol.EB«.Coni>at.,
1 ^ 1S6 (1978).
14« J . B i l l * , A»llollettd and A.B^llelland, Aaal«eiila.A««a, 22^ 9%9
(1977).
19. T.lf.Slitto and ll.K.fyMiidi<rra» atÂnal^Khto*. 2& ^^^ (1977).
4^
39 (1977) •
t7» r*IiSltl»o uttd r#6a«ihlsa» B«lii0«trt X«gfii(tif ^ 76% (1978)«
!•• r»V«liio*P«aaf 1f*d«#îii0ont X«B«etitel and 0»L«4li»t
^*CSirwetogr«» tjg^ %76 (1979)*
19* ll«l«ni*«t r»falcf8e&l and A*iiii«tf dl«n»l%«nB«8itll«f
a * 3 ^ (1979)»
fiO» 8«A»Cafitodos« V»r*Selitiilctl» V.UqH^s and ii*2»?liiad««
Bftir«Ceiit»€lano« Sand*, 97 (1979)*
ei. }f«8;«!lad;)al OBd B*T«Rateli» d«CbrQiBBtogr»9 196#^19 (1980).
8S» Aftfielcartoat P»S»Watteryf f«j«B«tla3r and HftBoIton*
^•Clirmatogr«» JdJ, tTO (1979).
09* ^•HcEaalgmmn and MvOetalnpfiolas^ Ibtdf toy« 7 (1979)*
S%« E«W«l«iigtoii^ V»J*6«rsliilcea« A«T*BaialeJlaii and S»B«!l«edle»aBf
imUMioehtm.^ 22^ 5%3 (197%).
89. C.Uttfai; and ^.YtGitgert Bloebew.llid.t I2]i»^1267 (1979).
26. 0.6.»aaiai» #»eiiiimat(»gr»» 10%. 17« (1979).
S7. X.aaeli end V«fiMlt«r« ehroMatogi^plila^ 9^ 990 (1979).
88« B.Haamaalf J.0brwiatOfr.« 10%. 967 (1979).
89. B.liiMtal and ie«Bay«r» lutd, Jg;^ %9 (1979).
90. A^naag and K.taaiarp Obronatograplilnt 2f ^'^ (1979).
91. E«W«iiittli«fray r.0.B*B3rflaid and I.Maelmtsrra, J.dironatafr.,
lia» 5«^ (1979).
39. T.iaiMi1»a, ff.jrakai and R.Xalcamira, ll>ld» 12%^ 999 (1979).
99. #.C.l.ln«an and G.Utai^tadt 11»ld» |22f 1^5 (1979).
3
S%« ^ • H . L l t t U ma « « J * r » I l t ^ » tl»id« 121^ n9 (1979).

5$« #«Y,9*l««r« ilMeI,I«t««« f^ Si5 (1979).
3^ ft»V«Q9iadl^« ^«eiir«iiAt^r*« i03« fHI9 (1979)*
57« A»if*e«M«lMiTie8, D»S*iifAiiii«an aiui n*C9w!lmmt t1»itf,
| 0 | , 107 <197%)#
98* S.S««»» v«ir«f»lt«» #«e«iin»(»2i«ir and s^mommft ihia^
tGU 193 <t97*)*
39* ^•BoTlloek «snd OtSasm^lecRi^ eiircMiatotrephia^ 2» 961 (197%)*
%0« J«B8vllefile ofld 0«8aafi«l«oiit ^«GiirQiset<igr«0 tl%> 393 (1979)*
Hm ir«jr«8lBgli, i^Jeev end 8,ir*teiid<m» Isaieii 4r«caiett., |2^ 981
(1977)»
4a« 8,E«Qitn»sfal end Xss«tallim» 4iiel*C9ils«Aet«t ^ SOI (1977)«
«9« 6«fi«li«tt«iit ^•Cli«««S«o»» 2]^ i4i36» 0089 (1910)i 22^ 798t 1%86
(1911)*
%%• O,n«l!d0ii Qua UOftlAteliMiat, lfleit>etiln.Aota» 8^ 186 (1937) •
%9* F#l>%lgl» *Sp9t T«»t In OfiMile Analysis*, Ttli B8«« pp* 899*
296* BUerUtTt A»st«r«Nat {1966)*
«i* r*F«lgl saa B*l?*Pelgl» llloinielils,Aeta, 89 (1994)*
«7* N*Qnf«0hl9 8*X»Qinr«t^l and 6«0*8tiiglial« ilaal»Oli«ii»y %8^ 1781
(1968)*
%8* lf«%ira«lil aad 8»8*Q«r«^l« AAai«aila,Aaf«g 2ib ^ * (1966)*
%9* r«ir*«»a«9 ]f.Qar»«lil ana 8,x*Qamalil» IHUM 2fr ^ (^966).
98* ff*%nraahl, 8«S,Q«raalil aaa tt.UhvB, I b i d , , j^ 169 (1966)*
91* 8*8«4«raaiil, M*S«8attil aaa 8*Baaa« Aaal.Oiaa*, 4 ^ 1139
(197*).
44
9t* • • I » « u « 8 l i i «iid lf«8*B«tlit« » i i 4 « , «2y t^n (1975)•

$$« lf«QKf»ittl imfl 8«Z.0iff««lii« l»l««t ; g ^ 1996 ( I 9 6 i > .
9%« 8 » S * ^ i « 8 b i fwa Z89i««tilleli» e*iiBal.»€fiQn*» j y g , 865 (1977)*
59* 8*8«Qitf<»id)t «»fl ii«8««iflii» ltierooltlii*il«t«t i ^ 11 ( 1 9 7 7 K
96* S«i*QDf«flil me ttm^tunnh^ folenteg 8|^ 929 <1977)»

45
flie iniao aots Ii«>&tettdinef Is Q noie^l esaetittieiit of

mm% pmtotiie troa «tiieb i t to ltli#rat«d %y ^y^rolytM vtth eeias*
1^ t8<^ bt»tidlii« ireo Hmwmv9A pmettemllf uimaltan^^mly tor
KoM«l (1) ma Bedin <e)* flM foiwer Itnrestigetor i«ol6t«4 tlM
1»@sG froe €31 aold by^drdlsrsote of the proteifttiiOy eturto* the
Istter ^taliiea I t f roe ti3^rol|rsftto« of a iiiiei)«r of omnoQ
protetao* Xn ftanittim to tte oeoarrenee to ptot«tiio» Miell
eeoonto of tlie ealiio cold art fomd in oceb satoral taiitortolo as
îi^r«MM9«, gomlaatteg ieedSf atat ottreot^ ii7iB« obooe®^ nneet^
tsriiie ona Mood (S)* flio dtfiefttao i»oli!iiyl«>iî©ttdtee {er^raootne)
ie 6 nofnal eoattttoefit of fni^msslftai} tsosole* ISie tstttiain®
eo^teat of n noiôr of protofas Is ebo^n (4) In f^DIo fftx«
fbo oormot itrootato of titottdia® ttm pootoletod by

teoly C9)f wlio l>«««d iilo @rgaon®iit notnly on tiio o^torvattoii ttmt
litotiaiii«« itlm ftiAiiy other lnlABsoloOt tmo ttio eoprotty to f o m
ooiorttf •olnttono vitti dtasotiatd milîtatlte iêld* iQioop end
Vlndaoo (6»7) firovldM ohtntofti itvtdeaee In sopport of lPtaly*o
otrnotora*
A good Bombor of aotbodn art airotlnblo for tbe datarmtiia*

tiflB (9*19) of biatidttio« looael and SUtaohar (8) dav^lopad a
^neatttatlva prooadttra for tbt dttamtiiatioa of arsiMiaa hiatidlaa
and Isrataa la protaln bjFdrolsraataa* fbta natbod ksomi aa
•flilvarwbaryta ««tbod* la blatorteolly taportent ateea i t
4G
fMm TO!
m s f x&itiE cowTEwr or A nmmM or vrnmim
mottlB Maomt of litstiato« Usm)

pew too i « of i»fot«ttt
Alioioot %«dl
<^»etii ^ 5*00
ClirHNitrypotiiaigeii t«39
OlottrlAtm HotnltttOK tnmin (type A) tt05
Oolootrtai |>»eiiAaiIOIiciltii C«QO
Edeottn S«90
ril>rlii«êti (fotaieii) @«^
Oolstta 0*79
Oltedta t*m
T«4iltibtiitii (iHMMni) s«90
lls»oglol»tii (fa«r«*) d«7t
niaollit %f9t
^ wlAetaelolyiil tn t «9i
Uroeôttitfi (iiovM) <)*90
%o»i» 8»%t
OvalbOMtii 8*5f
ropala 0*90
Ktb«BIIOl«OM %»8t
Stroll iilliaMtn (Torino) 9*iO
Sorm olHwiUi (liao«ft) 5*90
Stlk f tbroitt 0.x
irtttrtB t9«90
fOboooo «oiiit«o yrtnm 0*00
Trloo* plioof)h«t« MhyArofOfiaoo 9*01
Tfopoi^footw 0*99
I R M I aromtta i»09
Kite t«99
47
pr0wt§»B tut fo«iiatt<Mi for most of tbo gtitvia«triO| wid OOOHI

of tiMi oolorliMtrte lilotldteo dotomliiattoBO* Him iiroioiii to
hfm^ljn%€ wttli talfiKirto soldi ona %im liartlrolfosfo neuraltstfl
w i ^ dorian lijriraitii* flio Hairtiii onlôto I t toiiovod nr
f tltf«(tt«it ani aiitiifat imi fttotiattio aro pf«elpil#t«tf oiimttto*
nofwoljr In IHo fom of tHotr olliror m%i» tur ^Mimg otlYor
itilpbeto em hswiws ttfinmt^ to emmtm to ttie f lltr£)t«« flie
otiiwr mlt iB Bimpmmik la ailoto ootp&orto oelit ttm olliror
lirootptt@toi witk bfirogeti snli^laet ana t&« filtrato nostrollstd
irttib D@rli»i hf&mxi^0 im mtmem of ollvor ttiti^to Is ^€@^^t ^B^
tit@ til»tl3iiio»olivor I t ttitottvtty pvtolpitttta ^ oniofisl
aa^ttlî &S ttarlat fii^rdfrost^* f t Is aeoaoi^ttd irltti ^ ^ n ^ t t i
ti}l|ibli«0 @Bd tli« iilti^@« ooatttit 1^ t l ^ 9tlmtw>»^tr^& f I t t r ^ t t
I t #ttef@l»ei W 1 ^ tijtldtltl attfoaa* the tilttiatoo cxsntttit of
Hit tolntlsm I t eo^nttd fmm I t t nltrogea eoattnt*
ffet fm#«t»tiil tIrttrv&ttoB txy m^lf (9) ^ i t t hltttdlnt

fotmt • meptf mtt&na tolotttn v l ^ ^rlloti*t rti^tot (aittotttta
tali^tnlllQ tolA) pfoviatt tilt %etlt for a ^ i l o r i ^ t r i e t t t l a t t l t o
9t blttltflRt* mm&f9Wf %%9 ditto rttotlan I t tot tptelfit for
iiltttdtats Alt otHtr tvtiltlile oolorlMtrlo ntt&oat {Id»l9) t r t ,
vltHoat txotptlott f^Mllf lo>^t|jiit of ttit orlitntl Kottsltr^tnlet
ftrtetanrt (80>* f M Vno^ t t t t pnrriatt ît Ifttit for ^lotiitr
ootorl«ttrl« Mttlioa tmt atttrtiliittltii of blttldlot* iô^
o^ttrvttf ( i t ) tlitt titttlng of t tolotloQ of tilttldlnt l» ^rtnlat
wittr r t t o l t t In tbt fofwttltfi of t «iitrrfwr«« oolor mk«t fImiUir
4'''0
• hitmen fir»ot|»lt6t«» Utim vMeiioii liac huma (litmitwpttM Into •

fwrntttfittv* pw9Wt0xan W KB|»«lter*A4l«r (88)*
W9lUmfaB iÔits Bmrnmrim @ otttiotf f»r tii» d»t«faitiifttt«i

of ttlsiiatmi bftfti {» tiM ootor ptoaseea vttlt iMitftMioi
49
A l l iqwetraiiiiotQMetrie •tii«t«» ir«m ptrfofatA OR •

Bfiii^ end Ma^ Bp9e%rml9mts(i imlwUmtev or im « H i t i ^ r (India)
file f>eiefMit8 und i^tfitoalt otaa tii tlw»@ stadltfs wsf® of

4ii«l«ll gmio* 0Qf»«at 90^ X 8 ioii«i«sotieiigo tooln of laesli eia»i
(fiXI*90) «@» tisod after t i e mttml fogetierettaii ma eonterotcm to
ttio llo^fofm* Ii08tler*e r e i g ^ t irno pwtpBwtS W mix$aB %00 » I
e^noooB oolitttos eontAtiiliii too <pii of tlR^^ «sA 70 p i of Kt to a
too » l egoeoitOy eolotton emtetotiMS 100 m Wa&R vim emtetent
•ttrrtng* I t woo atliitoll to one l i t r o witli voter eod «ii» elloife^
to etana ovemiis^t* A brown red fifooipltete eettlee aown to tei&ve
« elear mpemeteot i i f o t d «lii«ii voe oe^rotea oet mn ooea*
« t # «<pe9ttt KfifOj •otnttoB aiMI « att^ #f Iff Bei» H i * eontimts
iptrt ti«at«A I B « «at«r t^^ for d»5 nlmitcB vliteli r««ttlt«<l •
l»l«««vtol«t «olor of ttie nolttitflsi* l^m mtlvtimk ven tosoved
«ad tii« hmm WW if8«li«6 •ovoivl il»e» ^ d tresavferred to o
«titt« opof {»t«t«* Aft«r A f y ^ ttio lioedo with f l l t o r paper
(free fffOBi i^Motwi tout) o drop of Motolorê f»egfi»t woo a«dod
to Obtain 0 pink color OB tlio lioed ourfooo* flHi limit of
^tootioa ««» 80 iOi of liiotidlao*
Vim followtiii oonpotBiifo «ero trtod wliteti g&m @ Bogotive

toot (no color to proaoeoA)*
AwlBO ootgot OlyelaOf <«C«>«l0BtB0« BÔIRBIBO, I«»proliBOt mi»o«rta«,

UBolBOt loo<»l«eoto«« tyrooftno* tiyptoptioBt MettiloBtB«« e^ttoOf
OFototBO^ BOpsrtIo oetAy tlntiiqite «eia« IjrofBat «ad ntgiBino*
AI|îrtB>foot A«otol<Mi9rilo» HoBSOltfoliydtt orotOBOltfotiT^^ otBoeiuil*

aolqniOt forBOlAolijrtfd antf wlio]rl«ltf#liy^«
IttOBOOi AOOtOBOt AOOtOpiltBOBO RB<| totOOlO*
O»i»qoylto ootfot Aootto aolAf ItBBBote «ot4« o l t r t e ooti« ottollo

ooidf ooltoylio ooitf» «iOM!%ie ooid OBA odtpto oottf*
aaa2!£l f m t . U . 1 . l.,«r«or,»l-.l, « t t r . , l . « i , l « « ^ M . t b . l .
iiiteft Atetttijri amines ^HHifltm^ airnkte^ iioJitttyl ^ t i i » rad
^Mwntolnteii isgwiicitindfi 8!ilp!ia#t«8t»«, talptittitllo field «itd
Rytgpaettiiwitt 8i»ieai«« toledtttft end iQrleti**
<liiiliol>ytfyittft|it Glfi09t«t fmotos^ ffiaa s»ettit«*
Smimmt Aettimtae mid beiss*8itd««
Only i«tttlli»9 mm aiiiltiie lnt«rf«rrt« «ltb tlui t « t i »

H I tk« f«fiMr OAM i n * mfita I»tft4t« toriMtf hr«/im nbllt la His
l«tt«r tai«7 teiiita bin**
ihowi afuliin ilktM witii iitttidtttt {kU9fm) do mot totorrtv*

1» tfco atthodt
Aowtte sold (tiM m)* AMtdn* («»6% « • ) •
A««tsldfiii9^ (fi.dO «g)» 1lfiiisi«i<!o (%«M « K ) «
J>2
eitrto Qeitf C9*tiO mh fyrJUUnt O a o • « ) •
1* »»t»fiilnettaB of fcUtiatii»t A Miftll eaowt CÔ*i s i ) ^ tte

i«»t •olntlod oontetiitiiK t to t«9 MS iitotiaiiio mo iekmi in •
Ikotltfig ttA»« fotlowoa t>]r 0*t Hi of o tfl atiiiooao nbro^ oolottoit
mA 0 0*t « ! of i n BOl* Hie oolitttoii Hoeeao ylUm of tor
19 wittiiteo ifiit^ WHO allomia to otend for t«9 iioiiiv «ia tiieii two n l
^ tlio tioffor ooletlon C%f m(|Gl in omimlo) woto oadod. 9lio
•oI«r of tlio oolottoii timioa %%m Tiolot imteli vao dtlutoA to
^ n l v i t ^ msir «ftor 50 iiiiiBtoo ona ttio filieosliiisoo iioo tokoai
ot 990 iHi*
i f f o o t of 1 ^
fit 000 tHo of foot 9t pn m ^ o oolor doiroiopneat lioffor

ooliittoao of wrtotto i ^ nort aootf W) in ^ o ^roooanro dooortHoli
o%ovo* A wrtotion of tlie oolor tetonoitr vttti tbe i ^ to Olioifii
to riforo 1*
gffoot of «io rtiMtottto
flM oolor intwaiottsr of tHo oolotltm «*ii«tt<lo opon tlio

OMMOt of tlw rtoiont* I f tlw volwio of Kiva. ootnttott noo
liiori»ffiood tlie ttoloor doirolopo^ in o longor tine* SlwIUrlir tlio
toortooo of ml aoloyofl «M oolor «oirolO|wi«nt» flMi oolor intottoltjr
oloo AôBdo on tiw onoont of tiNi feoffor oolatlon oo oliown in
y i f aro t *
do
I f f »• #g t t o i
flM «olor liit«it»ity 4tii«a4» HIMHI tilt ttrn^ 9S •tunatng

f 9 r i l l * tvAottiiii ttlstiiiw liiifof« ttie adailloa of 1i8tff«r« A wiste»
99it9w tttttitttty ««• i^talnta vttlitii two itoium iâa wit fomd
•tnlite tor enotber 9 to % boffini* fke oolor «£• fonwl atoftpfMiftrtiig
am o ^foolftttAttOB otortod ottor tbto tiim Intonnil*
ttfoot. of to«^f«tato
ftrootpttottoii Qoetanrtfl utten ^k0 toeottOB »t«t<ii« «»•

Hootoi la • wsttr I M ^ *
fli« îlor aoiroloiiod • • donertHotf el>of» oOioyod ttw

BoofwtMil^ft lav «» ôvB la ftsovo % falilo IX ooMartiwo ^ «
«t»«ofl^ô« velveo obtained on ^mwying ^ « mtocnt of htottHliio
eftor tofetag tlio OfôervnttoBO ooforoi tl«Mio» tn ovior to nhetlk
tim rofkroAaetntlttar of tlui toot tm§ prootolisn t» tbo rooalto*
i)4
f ABM: m
SEfllOPTClBl i J i f i«ip rM:cxs:tm wmf* i H

WE »'TCllMllfA1t<m o r HISTiPUtE
it* Jibsufâttcto a t 330 iHi

mm iitstiaiii«
I II Iff f* Avtfsg*
m # 1*0 ©•30 0.3S 0«35 0«3% ••30 0«3S

2» ta ©•35 0*3% 0,33 0.3* 0»3% 0.3%
3* t*t 0«%0 0*%t o.m 0.39 0.30 0«40
%• t»3 0»%9 0«%f 0«%8 ©•*7 0»*7 0*M
3» i«% 0*56 0«35 0«3% 0*55 O.fS 0*5*
<• l.f 0*63 0.63 0«4B 0*^ 0«^ 0«$%
D5
0.7 MM
Ul
U 0.5 >if
z
00
o
</)
en 0.3 M>
< • - ^ • ^ "
OJ mt
f- - T - ? - -•—f-^1 t 1 1 t 1 i
0 2 4 6 8 10 12
pH OF THE SOLUTION
FIG-.1. EFFECT OF PH ON THE COLOR PRODUCED IN
THE HISTIDINE - KBfOs REACTION
0.5 1.5 2 5 3.5 4.5
VOLUME OFTflC BUFFER SOLUTIONC^L^
FIG--2.EFFECT OF THE A M O U N T OF BUFFER

ON THE COLOR PRODUCED IN THE
HIST 1 DINE - K B r 0 3 REACTION
' i I
• ""
0 7
/
UJ
u 0.5
<
, /
y
cr
o
</)
<
0.3
- V
. • /
0!
1 1 1 I i l l
40 48 56 64
C O N C , OF H I S T I D I N E IPP^'^^
F I G - 3 . A CALIBRATION CURVE FOR THE

DETERMINATION OF HISTIDINE
USING KBr03AS A REAGENT
lid
Hi* eeifiljrtle aottoft 9t s estlonMixiêiit* i«eiii for ttm

dNit«ottoB of nlort^raai emouiit* of awino eeldv &«• eftrll«r botii
Inireettiiitta (8%t®9) <^^ bro«iii« li@o %««ii tiM<3 for the qoeiittto*
ttvo <lotoitttii«tto» of ooeie l>aoto OitBO eotd* < S i t ^ ) * f ^ ^ o two
M ^ m t o mnetiotif^ protieliljr^ fonsi tfoe êoto for e opeeifto
afttootton eaa âotltetiiro detoratoatliMi of falMtldtao* Althoagh
iiio oxeot i9»e!iî8» em not lie givoii «t thts otngo t ^ follonrteg
eoneliitl mo ear tÔf tontotifolr mtmm oo tlio bests of tb«
0!D8orv£ittoo® isoao tn tbete •ta^t«o«
ta eot^lto im^tvBf fiototstmi tiroaato fyrodcooo Hitn^too

eoeoratng to tb« oQoattooi
SfOj • <SS(^ • 5o — - ^ i »rg • 5%0 (B* • 1.58)
9rsiitii«» ttmt proîie«d« pro^bljr otieotf the tntdflôlo rtag of

lit«tt«ta« m0 hrmnlnmttm oooart (§6) wfetoli to rtoi>9ii«tblfi for
tlio il«rolo|Mitat of o Moo vtolot eolor to tlie oolnttoo* Btoeooo
• f t h . M r » « «,UUm . . t w . Of . f O y t h . n i , gr,«p , « h U i t d t n .
MsaorKooo OKtmtttdn ood totno acta to fonsotf* I t to liytfrolsrsodl
t . f . r . . k . t . . . U « « « » t « . » U iri>i«h gl<«t of* t h . W^ i o .
to b« oAooilioa OB tlio fottii ii«i*^» A ptok oolor t * tfeeo <i*velO|ioa
i4ii« tlio lioiiAo oro trvatoA wtth ttit iro««ior*» roagcfat* Tli«
b'S)
follanrlag telhmm emy IMI firopo««d for A l l titese step* ta ttm

•mte llB* e« pT9pt»Hi for g«B«rsl îlno aiil«o (Gbeiptor XX)t
m^
X w CH <» 0K)ll • 0 •^ X • e * com • ii|0
10!
fftctidlao itoHio sola
X • l»liMssol« ring
( ^ • l a (W®* • IT*) • Brag »• > l^stn (8©*) • fl* • BrOj
Sel6otftir«
<mldaot
X «» 0 * <KKM • HLO «9^ X • C • 000^1
R!oto»^Qll{ fiimioiitfiit salft
lte»tii (Ka^) • 1^2 "^ lltffl!! (SBJ) • Ho*

^
^ t t a (i^]|) • H«««l«r** r0«g«Bt -^ Pink tm&a*
ThMg tti« dtwiopitmt of 0 l>liMh»vtol«t oolor ta tiio ooltttion

vtth WBtOj sad i> pink color on tlt« lioatftt (after vj^thtng i«a
trotting vltli lf»t«lor«ii roogtnt) «iip« e tfoftaite eloe for ttio
proo<iao«^ of litotitflno ta a ciima oflniplo* fha toat ta soro
63
tin
MBstttv* îni ttiAt/nnoop ( e l ) bceaiiM of tb« resin spot t « t t
ttelmtiivw wtileli ti«l|p8 In ecHie«atrating ih9 imotmt tut %h» «tino
tola on the lie«d*« •nrfaee*
A ctaiSr of ^B^ffeot on ili« eolor Intensity (Fignre t )

•tiowe tti(4ffiSxittOMeolor dovolopient ot a pB /-v i t * Aaonnt of t!io
bnffer eolation t^^md to o flxoa oonoc'ntration of tbe o^n^le
oolotion filto oeeas to offset the ooior intensity es siaomi la
riiors 8« fits eolor tfovelopstf et tite o^ttnoei eonîttons of pS
tiê ena tsniieratars Obeys %%% Bsofwt^niiliert likv (Ptnajrs 3) tuns
lîvlng the liseis of €> oolorlsietrio êteminetion of bistiiiins*
61
Sssincr* Bi!t««l« p« %09* toterseleiicw ftlbStfitiertt, Xne»«

Wiw Tofk ( t 9 5 f ) .
%• 6»t«7i*i»tr»i»« *Aav0tte«ii to py0t«to Clieeistvjrt iTuI* T» |»« 39,
8« AvKaMel ana F*Ktitti^®rt ^•pt)t8iol«Cli(s»«t |S^ t69 (i900)«

9» A#Ko88©irasaA.«i«!>i!tteiit i b i a , 22^ 59 (1905) •
(i928)#
tt. H.B.Vtcfeery, lt)l«, J^l^ 303 (t9S7).
13. ll«J.Bl«ekt ^•Biol.ClNMi., i22» 67 (19%0).

i^« I>«s«Doliertrf y«!r«St«la m0 n^nergmm^ iîA^ t3g# %97 (i9%0}«
19* n.H.Vlelcvty ana ^•lC.1#1iit«niit», tUtat | 2 & ^^^ (t9%%)«
16* 1C«lMiir» ^•pht»tol,eiitm«y »g« 3 (1939)«
17* K.jroriHiff, Btoelicw*^*, fl|^ 1907 (1998).
18« Il.r«l«io fli*r«oo» ihU^ ^ 99 (t9^8>«
19* e«ii*%«fiii» x»A«Kitiic«ii nBd r»iioie| j»Bii»i«eiiMi*f i7i« 233
CI9I7)»
6'*(^
20« K««.Ko«t«l«r and li»r,n«iilie» ibtd^ ^ 497 (1919).
m r pQbltoti^rit li»»eair (1979)*

S%« 8*]S«^rest)t m^ leratollfili, Aiiel«€l}|ii»A<it«^ ^ OOt (t977)«
Q9« 8«?>*Qisf«@t)i ana Bîsmeitf falmtaf | ^ 89$ (t978)«
C6* K«I!dfi!»isst vtfstdeEOle ana Its dtrlv@ttf«t«« part Z» p« ttt«
tQt@reolaie« l>a!t)ltet}«raf utms TofftEt (1995)*
63
flttsfctkgriftmtas mm Urn •lUMtittat «oii«ttte«iit» • ! a l l

tlirtiig witter* Hhmy am pwmt to a l l aaliMil ttmitaa «aali3r<lv«taa« anoti aa etfiteh« iMxtrtoat aiwvoaa £>!id laetoaa «r
atlk angar aia takao to iiia faadf a l l lâa atibaieiiaaa atâ
avtniiiallsr naamivtad ta mm atopla aiiâr« glaeoaaf «&ii^ to th»
pHtmwy oaytootiftffata attltsaa bjr tlM %o^ tiaaiia*
flfOBtta asmtliaataa aagar try tba pmeaaa af ptiatcMiyiitliaato

froii atoea|)li«irle itatar and aaitooo dtoxida* Wmf pUmtm eoatato
langa foaatittoa af etn^tAnf^mt/B* oa a toad raearvo and tbasa
mv aaafol Bmr^» «f «»f4iiAy<lfiitaa to tlie dtot far saa asA
anlMiI* JlNNii 60?S af tlia fatal anarsy re^titraMMita to nan to
l^rarliSaA %y tita eagragattaa af aailiatiyfirato eaiqianida* Oaitia«>
liSfîatoa ara alaa to^rtani aanpaaaota af aana af ilia atroatoral
aatortola af ItTtog affaalMi aa far aitaHi^la aall lialla to plaaf,
Îjraaaaluirliaa to ttia aaâlaa af %aatorfa moi a«MM»i>alyaAaaiiartdaa
af akto aa« aaanaetlipa ttoaita to aatoala* MMaaaatfhartdaa ara
aafwuata af topartaBt %la«AHMiiaal aaapawida aoab aa nitatoto aaid^
aaaaayaa^ f larapratato aad %laa« graap aribatanaaa* ffibto S
aoamriaaa ilia aatwri tmA aaautiaaaa af aaa« atopto aagara« ntaa,
toa atady af aatô^ydtatoa to ana af tba aaat aoialtlag f tolda af
aifaato aiMatotty^
64
tMlUB 1
•«f«r iNKimnPVlitMl m B TCBvllOB
BnWiOSKSffmOmWlXiMUl 40 lapoft«iie «eMittito(Ri* of t ^ mmrt/mtênH

^•iKiyriôiiiioIelo field ( H I A ) ^ » f«i*tttt
«at«rt»l fiHwA i» « l l l l v i i i i i»fi«BlMrti«
tMSMh9t* Ai « » « ^ t t « l part «f ritiffiAiielftte miM dNA)
t%9 iBi«r<MHit{ii»il6 «OB««niea In pr«t«lB t i v ^ t t l t ,
•Ico pftntni la tti« ewm^xymu Afp« rAS»» 1IA»
UMi tt»«t wtmiT il«triiittt«# sf nit tttiiirai

i t w i « M I t tt««tpori«tf i» «Mi %l«KNi MMI « i l « l M i
In t i l * « • ! ! • td |Mnii««t Mittgr*
ftofVMtOM flMi •w»«t«tt of •agertf foina in fimit tMimf

«UI a w i i a i f l a l i * flKMi^tt ••t«i« * f i
iap»rt«it tettnw4i«i#» la fl3nMil]r»lff«
8-i
CliikU X eoBtlawKI)
'iWBlHi'"*^ CNitUIU'f'VBVV mft jPOBHltlUl
IMNilaotot*
In tftt« ily«»ti|it^ of imrvmm ttmm «i«
«lll0tl»9U«t «tl0liWft««» QsUotOtaiitlMI I t
m&mm
of «]!<> poitmtialljf rtdrnetfig RTÎ^B of «li«
noiiooAooliaylAoo* Oooom i n plmtB oad to
0%%«tao« wfttoly froai •«toi'0*AO ovA %••%•

^ H « tomittSf til* i0mkiM%wf %t t'tmm MbntMiitB SMMilljr l«voli«»
« i l r tv» liattii ktiia* • f fmn&%%m»t gtwips * twin or aMitiinit
•af%«iylft Mid •lt«li»ll« liyifîQrl giw^t* flw ••ilMNiirtffVMpt0m
tt«t ttttnitlly •Miir a» •w^ iHit • ! •ttiMKblwNlvttti tli* hyifwqrl
givipt in ili« f»ftt «f li««lai««tiil wr «ott«l Il»lei««»«
Qtii«9t» ! • til* )Mi«r «f iil«(Nl Mitf «tii«r n^dr f lotat*

WlmA ti«f»»llr ttntalii* fv«i 60 to tNI «g t t ftottMHi te Moi too •!»
tbiit t» ttdt dtiiNitto ttoiidtttmtt w&m tutu tOOO Hg wmt %« fftMiitt
iily<Kic«si nfeleii iir iiratieiBitfoutttuvimi^ wmar mM eo^pitx f«««tt«i«
l»fovtlN» ciHiiigir t9 09«f«tii ttw ttcan* sioiitnorir* QI«ieot» i« ostdts^s
9i«f«v»»tlslir liT ttw ttscii* #t t6« imdsr t« fvovt^ Aotngî
^n9tofiril3r» «•!« ttiim tiÎf of tt» ciitiigy of ^ o lio<lr to i^roiriiNN!
Ttff tllOfimt^tttOCIof glOOOSO*
nrnetMW p»oo0tooo iNioollor olier«oterlotto» I t dtffovo

fvon otiior kotoooo tmA oo tlie otnor lio»d t t loowiiUo tl»oo«o la
OMO fooottono* flito to oo oeeoont of tlHi tootftlsr oBttftsa^to
ttoi^pioi «»OiMliyw(lB f roooot to tlio «olo«olo* 11M ton<<*os«lMmgo toot
for kotoooo (t> «oo# for mmmU^ foni4 oogottvo for frootooo oo«
Oolor vMottooo to oit«oio oUtolotiar oto of grtot

loportoooo (•)• l%or M O oaofol for tHo ittoottoo ooi Ootowloottoo
of foootloool grtiqNi* A oolor ffooott«i of oattoHspgrttoo ottft
oottirooo oao iofolopoi %r ItftvOi SIMWO ong tMilto (9> oktoli woo
67
•p««tfie for l»toft«» A • l i p U tmA Msctttvo itot«eti«n of
«bi«ii moMf* mi* fi^folsrvâ to fliiottt* ma fr«ittt»««» StotUrlrt

• eogof^titatttoB mmptmt t9T tlMi 4»t«eilMi of •ag«r» IIF piiitr
^nwiitiitftti^r woo lNiit«l«p«6 %ir iiGlc!3ti ma s«iilv««ic ($)# fortmis
otiior wettMMt* wtr* el«» Hvmolopod <6»t9l «liiel» •!« Moottfvo* A
ttUHlitr «r oiiol #••%« liA«e t w ^ aot0irit}«# ^ f^tgl (9) f «r tte
<l»t«otlaii of ongovo* for îMHiÎOy o lileo oolor IMIB fomoA ^/b»m
kotoii«toM» ova liooto^ vttit «til|^«rto oeia oolottoo of moo
oontottttng otABBOoo ^ l o r t ^ « ASdo&esofioo iimi • rod oolor wltli
ilito f»ie«n!% %«l 0013^ oftor pyotODgoA ttootlog* vim cêmiottBr of
ttiooo oolor voBOl>tooo iOf iiooor)0r§ o t t l l ttot- tenovB*
f6o folloirltig pegem oonsMiriso 0 toloottfe aotôd for tUm

^teîm of oaorooo tme fvoctooo on tbo toolii t»e@<!o ootng tôtilorOf
0»%»dl8ltrf]Ai«oooiio 00 0 foogent*
38
mmmimmmmmimmmmmmmm
ifm^totmi^%km4iMt%w9llmmmmm « « • a pt»exm% off l o d l i ^ M i M
SQW0S WSf^m tWMff wm9ll$} wi» iNMNi • f t t i ' i t t mmftl nnitMi**
t i l l im mtmw ««• «ibtiiiii«d vttli llft«*l«]f** i«it«ttt tma wee p»l In •

m%wm%9i€ •ftlntioe 9f t«i^l9if»»t»tiMllnitf»iabtiit«ii« to îWMnimm •
SSSsSSsmSS»
Jioiit %»$ iiMi««i»^tftngt fttitt M e i i laiprlpi«t^ wttti tit*

#il«ff»f9m tttsttoo of l*i^tovo*@tlMtiiltr9l>«»«iNi« wttit pla««i ^
• tit«v» t«ott«^ f^t%mm§ %3r a dfop t f tlia t « i t •atnttaa m& m
Hffofi off 9(H( •al,|iiiiiPt# aoM* UMI aaatatttP wttwtf iNiataA an a lNilltn§
wataip %at1i far 8«t ttiaittaa* gtytlapnat at i«i ttiwiga aalar an t i a
taaltt %aa«a Inilaatatf «Ni fvaatnaa aff ftwytasa ar MMvaaa* H M
Itetta af aataattan aaia !!»•% / « far frnetaa• mtH %U (m f^
mmwm* flM aaiifttlintf af tHa tatt la afâaaaAf I f fratiilr
fivafMiran raKxa la tiaaî miHa a t i l i iRaiat*
H M faltairtag att«»t« c a i ^ f K a w^f taatatf i r tiM

69
tMmhwtfl olealtol*
Jfit»» *«t^«t 01f«t!i«f ftl«ti»% iH!««tfii*« ti9t^<*l^<'Af 9f<»lta«t
f«%l« XI • i m r i — » HM l l a t t t 9f tolcnmoe of mm
70
MtMCTs or fomnmm or rmmm mmtm Bmsf»m^B roa fm mmanftm
WWntipCk MibSflllKMI '•'••W"l I "'""I" • "••"••Wll ' I |I[IIIIKMIIII •IWWITIIW
III ^se f motote t e s t to ttie • o o t ^ * t t » t
Bmmtm 85*% 19*9
19tfr9l»Qiigtii« 2%*6 Ollill
A«e«oii« S!f8«0 690*0
AmttK^mMm^ 809«0 790*0
Ae«tte ool4 99*6 iC«0
tei»iatii« d*t9 6*10
mtKyt eeet®t« %*%0 t«76
ABitlM 99.6 2%.0
rrrldtnt 89*0 19*0
Olfelnt t«90 1*90

jptiCDiticii
tmetn—, xyioM, fiiMiii9«t «iitf ef«l>liioMi gav* ii«gattv» t«tt««
I t l« el«er frow fwbid X tUt «««t is ^ l t « M a t t t t v i m& mmtnt

b«eetoie of thm litgli tol«v®iieo I t n t t fur vartoot foreign oiOioteBoot,
V2
|MWIWS»08f
imBftfim (t966)»
9* f«1C»yMMif Y«f•Klaitife and S«S*liaclkt»« lekngalnt stt^tii^
•S^ 1090 (i960>*
%• K«X«8«ikI*a<l«r eofl ¥,A«l«vlBt JafiI«lllo«lie»*t 22» ^^^ (1979)*
9* Ii«ll*i«lt«l end B»8i^t«»Qlc» fliDiiiaste*^ |g^ 99 (1979)*
$• A«K*tll«twlt A«lt*Aaar*s end f!«llilQ%>«ftOf lE»v,69e»firgtiitf«« %ioI»9
gk, 1%7 <t9*«)#
7* ir«^«rotf%8lfiif Oheatstiy mid XliAattfyt 06 (1999)*
§• 4«fiB«l» €ôHi»iirt | t y 889 (t99i)#
9» l»S0Me «iiO 0»6«fortert ABel*t9iiett*» JLP ^^^^ (^999)*
10* il*0«60l»«rt» il«Amntli«*fBetaiol«i 2|» 97 (t96S)t
ti* V«0tott«l» nmt*natmmU9 0hMi*» g ^ 170 (1979)*
to* 8»ill«lc«atiOr» «iiO 0»8*llle!»«tî il»«l«eiw»l«*« |ji^ 879 (1909)*
19* ll*Kliisii» OtAliti«i B.BifiMi miO K*S6tiiicOt immUebammf
^ 1%96 (1970).
i%« e«V««i«0»v»IO aao StXittHpt ^•OlimnfttQir.t 22^ 99 (i97t)*
19* 8«i»tV««««r imO A«ll*«ttM» J*efar9naitogr»8«o*, 2» ^'^ (t97t)*
tO« 0«lta, J«S,ni««<Mi «iio ••lf*1iiertadr, e«i«oii|«,lltft«» 12^ 899 (i971)«
17* l*V«0»lllii« n o AJI«lAi«»t V«99tf Sf ^ ' " (t978)«
10* 0«lllilra«te« 8tliilmtliik«« FtlftnririMMlt fi«iMi^l»» ottO 8«fliit«M»
Jiial,I#«t*, 1^ 909 (1979)*
19* OtltMin* C*CHrte»to, IC*K«ktlii •«« X«K«kltif«» Aii0l«Obt«»A«tft9
fl, 91« (1979).
mmmmmmmmmmmmmmmmimmiiimmiimmm
mmmntB m A nm tatCtvi immm BtuoAm eAtxmmmumrM MB its

»mdmm wm mm, mum mmmmmmmm Btpmmtm oy mm\h mm
V3
vnmtmftm
tmkmmttllismg9 funietttv ta laofiante ««tertAi» hnw httnn of
MOli ts«i»r*«t for tli« Ifiot so euHir yoftr*t partloolerlsr tn tuo
oo^mttoii of f«dioiiiiel«td«o« for OBtntiplOf tbo iîotptiooilteato
ooi^lexoe of iltceatnay sireaRifi»t liftfol<titi« or ttiorlon Koy bo ased
for tJ^ ooiiersttOB of troeo eisoiait^ of jplntoiitiiiB frt^ m OQIMOHO
set<i toltittoii of Imdtotoa tiraniiia (t«9)* Vt»(IT) oalto hmm
boon foimd to tm ttebio Dotti oHotiloeltr «ad itieraally. Por tliio
reesoii o otnaibor of tla(fV) salto h&we been otodloa Sa detail onefe
fi» t»tios|i}!at« (4)» arsesAtt {3$6)$ fliitt«oii(ite C?)^ molyfideto (8),
ttmgfiteto (9) OBA vimadett CtO)« Slnee aooblo oalto bavo fitioim
eahmeeQ iimmmteihmm^ proportlos tin (XV) baeoa double selto bavo
elio foee tired otttnttoB (tt<»l6)*
811 Ion beood double oelto opfiear to be ooefol oat ton

oxebanKoro e» tbosr genorolly obow tm extrt ebmstoRl end thermal
•tebtltt^r* Por liioteiM»o« IpboepbottlloDtes of Zr<XV)t ftCnr}^
Ot(Y¥) oad iii(Iir) bove obo«tt (t»9ft7il8) Ojppreoteble toeôxebaioiô
oopeelty eêo oa boetfag ttpto btgb teiiperiitorto* Ao tbe littretart
•baifo oroeao •llieeteo of tetroimlât mete to bairt laeetvod aefltgtble
attoattmi ea taeri«iilo ioa*exeb{ioiera» It ««a» tbereforoy deetdod
to explore tbie field for ae«e aeefol lietel aepar^ttoaa* Aa a
rtealt tfa<fY) araeao atltoate bee be«n |>r«p(»f«d aad atadted for
tta ioa«axabeBfe bebavloar* Ibe folloatag pegea aamnifirlae aoab
a atadp*
V4
Btmmie etiloriao tis«d Is tl)«»e •ti»fl«9 «»• o PolltH

FreSaet Cl>«P«B* 9oltlct« Odoisriniltct Oh«si«aiii« Oltvles)* All
oilier reegents tm& ehemie^l^ «»¥• sttlser froa B*D«Il« (Cnglena)
or of Ana far i$nitf«#
Apparctog
M ttteo aoS«l MÎO pf! ni«tor VB» aced for pQ moBmawrwKmt*

vhtle I*fi« 9tQdl«8 Here nado on a F«rirtii Elner 6St Orsttiig InfrRrta
op«etroE>!iotQi8eter« fb« sMretiaatoel iluiêr oma veo fron the
8ot«ii«roiiie Ibfttrttteiito (Hitfto) ^tf iiie tis«roi0gr8vitietrto eaalyett
««• |)«rfcinsea oo « ll»atm fQA tialfmee of FOI (lodlA)* Ruaiotto^
topto ««ac»r«iii«fita irort iift4« oitlior on a eolnttllotioo Comtor
(for V «.ro41ottQ»o} or on a 6*tl« Counter (for p »raatattooa)«
yraoaratiaB of t i e ioo«*a«otiaM[a watarlala
flia oolottaBa of aoAtoo allieetet aodiim araanate «nA

SBCI^ vert iilxaa la a voloaa ratio l i t i t aafl the i>n of the gel
frodtieed was fIxeA ^ 1 with the help of mo.» fhe •lurry ma*
then kept at roQ« taaperatttre for 8% hoara ana ftlteraa* After
waehtng with aentnemllsoa water for aaveral ttoea» to renoire the
exoeaa of reagenta^ the gel «aa tfrlea at ^5 e* The artea aatertal
vaa plaeea In irattr to oraeic f t Into anell iraniilea. After further
d
wsfthftiii vttH 4t«liitralts«4 v«t«r» t i l l tti« ^n of tbe «ftshtiif{«

%•«»»(» 6»7* til* M«t«rlfil w«ii p^*o*^ ^ A tmtM WKij •olutton to
eosvurt i t Into tli« B^ fom* Ftaalljry aft«r 84 iKiar Iretfitiii at
roam tewpcratotv^ ttie grmiiilet INIV« vesti«a to remove oseoto of
eetd fisa ^rled «t %5 6* "Rii* oaitple ««• foimd to tie better thm
otti«r oanpios profi^red on vcrying ttie "voltaiio r&ttoo end eonoeotrt*
tiooo iY\ i t e af^petât otal^llitsr to ooi6« ead loii-<»xelieni;« oapeotty,
f t naoy ttier9fore« oeleoted for fttrôr otodloo*
vMvposttion
Offfortnt opoiaito of ttte eaeohengor «raf« tmtlea vttti so «1

of ooQQ* net to dlsoolvte the ar«fict«t« and t i n preomt to ttio
oalipotmd* Slltea rtpelniia to tHe oolotton ao pr«oinitato wtitcli
WHO filtered out and doteit»in«d grovtnetrtoelly (t9)« fbe f t t t r o t e
won dtlotod vttfe dt«ttll«d vKt«r end t i n ood aroenlo prcolpltotod
fio Oftlphldft* fiy iioAolnff H ^ gao la tlio oolottoa* f i n v«o oeparRtod
fnm mr»cnte tiy botllni ttio fvvotiiltatt iiltti eooo* R61 mid ««•
dotorwtnad %y tttmitcm wltti CÔrgO. oolutloB oftor nKtoettoB
«itlt load CiO)« Araaoto anlpHtda waa than diaaolv«d In WaOB
aolatton (ill) awf araania vaa dataniiBad hy %im Tolliard«a thioojraiiata
awttiod (Sl)« fka taaolta ara atianarlsad la faUla X I I *
Iaa»a«al>aaga oapaatty
flia iMtarlal waa fonod to l>a a oatioa axeheaKtr aad tiaaoa

ita ton axaliaaga ti»p»9Uy (t«a*a«) naa dataiwtaad oalos dlffaraat
&
s 10
•
•I m
ve
I m
••
8 S
i S s s
9 8
st«s
9 6^ S
9 tnl O* o*
g I Si «i o 5
I
lA
§ M MOO 16
s I
CD
<"( •»< (^ ft S
o e'
g
i« %
9
s|* m i
9 s
I s » s
g i
'^ • fe" R 8 ti«
I «• I*
e
e
il IS
0
f
8III I 5
i
I % %
ss •:
V7
« t t a l M i n t lout %y tli« «otii«i pro««s« «• umml» OB« grav of tlio

•Hfffit* « • • t^k^n tor tfm oolom |>r»p«ff«ti9B Aa^ tlM f I w mto vti«
solatfitiied At 0*9 MlAila atlng i«0 II •olatlont of fbo olnftato*
fable SXfT iboini tti« t»o«e« of thto esohongor for Alffortnt notolo*
Copctotwittoti ima olottoo carr#»
Tbe a»omkt of tbe J^ lose oliited fron tlio oolwm <!ep«tids

iifYOti tile oaQccRtratlaii of tlte oloaat* Zt vae observea tbat t«Clff
oointtmi of fraMO- (185 al> vae stiffioieiit to olotc #.li!i9»t a l l %tm
Qf^ lotto fro0 a eoltMm of 1 g^ Ion eaiângor* ftila eoQeeiitvatlon
usOf thoivfore^ eaad to flran t t ^ elation ourvo* Miont $0 s i of
tho elnent vera oeoSea for the ooiiplete elotlon of l ^ tons froei
a eolfifisi of 1 gn eseti^nfi^^r* The eooeentrntlon and elation eurreo
eratfhoKBIn Plgorea^ênd 9*
Chewloel aart therBial atelitllty
YUe appftrant (Aenleal ataiillltr «^0 e6eofire<! In BStQm and

MaOR of dlffertnt atrengtita* Zt mam âarra^S tbftt t!ii^ exeliâger
mrnw f a i r l y ataxia «li^n ica|>t In 1*0 MflNO«and 0*01 M n»m aolntlona
for oramlffHt, nowavart I t atartad dlaaolvln# in O.OSt 0.1 aa«
1,0 n VaOR aolotlotto.
Da order to f Inff oat tfta tfiatwal atebtllty of tlie exolianger

I t vaa kept at Aiffartnt tanparatana for one tiour eaeh onA ttie
!ra*li9n esoliasge oaikaottsr vaa dattralnad after eoollng the aewfilea
at rooM teaperatnraa* flia loaa la the to^.osiflii^lôa|i8olt3r eaA
ri M
tmm xxit
iiw^îaimgor chvmtrt or taidv) AiesEHQ sii^tcAi^
Mitel aoIiitloiiB Iaii«>«x«hitiijg« eapoetiy

(weQ/diT fs»)
H^l^^ 0*95
V9
20
Z>
o
o
a)
I-
=?
-J
m
•X.
o
*
X
a.
O
z
UJ
<
>
a
UJ
0 0.5 1.0 1.5

MOLAR CONC.OF NaN03
FIG. 4 CONCENTRATION CURVE FOR T I N (iV)ARSENO

SILICATE ION-EXCHANGER
89
o
o
-J
UJ
to
2
O
LU
<
>
a
-J
0 25 50 75 100 125
VOLUME OF EFFLUENT { m l )
FIG - 5 . E L U T I 0 N CURVE FOR TIN C1V)ARSEN0S1L!CATE
I O N - EXCHANGER
3?i
tiM ira^rii of tti« •xetiaagftr on li«ettiig »t different «l«vet«A

t«iii|Hir«t«ir«t er« wporteH tn Table XfT*
itg • t t r a t t o B t
Vbey vero earrtea out br the followtiig »etfeod (88) end

tlie reeolte ere mmmrizea In Ptgnre 6«
^H) ng of the tooêxobaniêr vere tekeo In eaeti of tlie

•evneriil 230 nl conloi&l fIcelte followed by ttie ed^ttton of tbe
equtiioler eolntione (0*09 it) of altrell tM»tel eblortdee e>n6 their
ti:^rostdo In dlffert^nt volore ratioOf the finel volnne hetng 50 tsl.
the e^tilllhrlfii!! ^m ettfdned hy feeeptng tho eolottons overnight
KBd the ^H reeorded*
TO end fOJfc ettidtee
fhe XR efwotrnii of the eenple i s eho^ti tn l^tinre 7 i^tch

wee dre^B t^klni Iffijcil ee the hlenk* The themo^revtni^trio
melyele gnve the eanre ee ehotm tn Fit ore 8*
pt»trthiitt<wi etodtee
(e) BeterMlnetten of X. •elneet Bletrlhiitioo etitdtes for 1% oMtel

•III •III! . I l l I I * I
tone were fierfomed In dtlnte eoltstione of fBR>.t ITGlO^t Mi end

In nmt hjr teklng 890 m nf the exehanger In e oonteel f leeh
eontetntng 89 • ! of the eolntlon «hoee netel ten eoneentretion wee
•djneted to ^ 9 4 of the total tott<»exehenge oepeoity of the Mtterlal*
The e^ttillhrliM wee ettelaed hy keoiîng the oolatione oremighty
82
fmmi'.h Bfi^Bitn*? OF f m d v ) APSIUO SILICATE
"" '" r '""» " "

Orjrtng ttrnfiemftire lta*i<m esetia»i« eepcoitir INre^nt lit« ! « • •
(oc)
«0 0.99 0*0
€0 0*69 9*0
too 0*69 S.0
800 0.60 %$
^00 0.90 t5*i
4500 O.flO 10*%
0*00 t7»0
Q 9
00
0 0.18 0.36 0.54 072 0.90

MILLIEQUIVALENTS 0 F 0 H~ ADDE 0 / 0 5 gm.EXCHANGER
FIG. 6 PH TITRATION CURVE FOR T I N ( l V ) ARSENOSILCATE
USING N a O H - N a C l MIXTURE
84
TRANSMITTANCE (PERCENT)
O
I
:-j
(/>
m
O
o
H
>
m
21
O
cn
r-
o
>
-!
m
O
I
m
X
o
>
o
m
30
85
Vo W E I G H T L O S S
-n
o
1
00
X H
»* X
+ m o
75 H o
^ o
2 >
•^ -^ ro
o
o
<
m
ir> u
o
o
7D H o
H 2 45.
2 o
f^ X)
o
>
<
^*oi«»
CJ^
>
a o
m
33 o
(f> o
m r> •«M«'
z <T>
o o
S£! o
1—
o
> o
m o
z 00
X o
o
>
86
fli« dtttrtbotioii ooefft«teai0 of 8om« sicitr.l ions were olto
tîtb nsio^* for tbte pnrpciee tOO isg of tfite esditîigor %>«re ei3«tlt«
tir7tte^ Witt} io IBI «aeb of the lebellea eototiim® ai«l ttie rraioaottvity
of the 0olQtit»i mm reoorae^ ofter filteratioas*
fte K^ ir3lt»8 were et^lctitetoa hy ttie fornQlo
« « i*y « V
^ e r e r is t!i« fraetiî of rsetol los |»res0i3t Isi tfee solotton ^fter

eqoili!>risxK» ? is t!if^ voli»e© of tbr> coltition In s i cud M is tbe
mnu» of tbo esottrnger in gms* Ti!t>les SV CISKS STt soMNsriaie tlie
msotts* Pigar© 9 ehowe thr* variiitiwi of K^ vpltie witte the RCIO^
eonomtr^ tiofi«
(li) Sfperttti^ng aehlpvitt Pov«»rrl binary •{»i»ijr»ti jn« w«r© t r i t ^

Qsiiiff £^ eolnnm eontf^lnfng 2 r of ttie fixehfttiger (100»800 ««iiti)
in nt-form tt'k^n in r. glti»« tabc* of mi i«d«/<-' 0«6 om* tbe enititl
ion» «»r0 eltit«<9 nt ti f loir reitc of'^^ 0«i nl/niiift titiiiir ultitnits
MlcetoA on th« 1iii«l» of W^ wnlvrnti obtained. Vhe notai icm* tn
tli» effluent• w#r» Aotominta »« Aeveribott nboirt* fli« tnrportaat
••l>«r«tiont •ehlowd on ttfe ootttwns «r«ftbcvMSin FijûrtP iO to i3»
o i
i S 8 8 S 8 S 8 8 « 9 ^ ft IR r:
's
V
n 8 g S 1^ 8• S •8 •S• $^• $• 9 IS• 8• 8•
e*e* O 1^ O O O O
tJ
o o w^
s
f 8 S K » « S S « « S «« &• 8« l:•
s © © © © e© o
« «
<< © © « » o rk © ^
's •I
1
SS8S888S8gSS&^
IT
€ ©©©©oo©o«^©©<4©a
tfj 8 8 8 8 S $ 3 S g 9 a^ 8 {^ S
© © © I ' * © © © © © © © *• ©
g^ 8 8 8 S 8 8 8 S 8 ;t 8 » 8 8
© © © i ^ © © © © v \ © « 4 n © ^
s
g 8 ^S 8• R• « 3• 8• i:• S S 8 S 1^ S
8 I 8
^
© © © O © V\ M © © © r\ «i
I 1^^
ss
1^^
fi« IM IM H
^^
e&1^^ l^'
1^
asffi8:tfss<fftS3
0 0
tutel font Dtstrtbtstloa oo«ffloi«tit«

(K^ St 10-*)
«b(t) 9*16
nm 1.51
lii(tt) 0.95
T(ni) 5«.50
»(in) 7.50
Cr(m) %%.9o
89
FIG-9-EFFECT OF HCIO4ON Kd VALUES OF Cs*

ON TIN ( I V ) ARSENOSiLICATE 10 N-E XCHAGER
90
O.OiN HCIO4 I.ON HCIOA
• Cd HI )
•z. • Hgdl)
ID /
cr
<
^V. X. 1 (^
2:
o !. ON HCIO4
<
h-
2
UJ Hg i l l )
O
O
o
± J
8 10 12 14 16 18 2 0 2 2 24
EFFLUENT VOLUME ( m l )
FIG-.IO. SEPARATION OF Hq ( I D P R O M Cd ( i l ) AND Z n ( l l )

ON TIN ( I V ) ARSENO-SILICATE COLUMNS
1
0.01 N HCiq^ ONHC104
5 • CodI)
4
h- 3
>
2
(X
<
cc
0#—# » .. o I' t q..- <^.
z
o * - O . O I N HCIO4 1. 0 N HCIO^,
<
a:
i-
2:
UJ
O
z Ydll)
o
u
6 8 10 12 14 16 18 2 0 22 24
EFFLUENT VOLUME I m I )
FlG-11. SEPARATION OF Co (H) FROM C r (111) AND Tb (IIDFROM

Y Clll) ONTIN (IV) ARSENO-SILICATE COLUMNS
92
O.OtNHClOA \ ONHCIO^, ->
liil)
2)
>
cc
tcc ^ •'%—M,^ „ q » ,,„ ^^—I %- .1' i^ ^
cc
•z.
o
<
O
ou
0 2 4 6 8 10 !2 14 16 !8 2 0 22 24 26
E F F L U E N T VOLUME (ml )
FIG.12.SEPARATION OF T l Cl ) FROM Hq (II) AND Co(ll)
FROM Fe (111) ON TIN (IV) ARSE NO-SILICATE COLUMNS
1.2 0.01M
HCIOA
• Ba (ID
o 0.8
<
UJ
~J
uJ 0.4
a:
if)
•z.
o 0
<
u.
o
if)
tu 0.6
_j
O
Ba I U )
0.2
0 20 40 60 80
VOLUME OF EFFLUENT ( m l )
FIGJ 3. SEPARATION OF B a d O F R O M C a d i )
AND S r t i O ON TIN(IV) ARSENO-SILICATE
COLUMNS
PISCIBSIOW
Vb« naln f««ttifl«» of tbi« •to^jr ar^t

!• Tli« •ytitHasit of « i}«« itmêsetisiig* «at«riel beted on tin(IV),
erseiiie(V) and ail loon (XV)» allowing a irarr high tharaal
atahilltF*
8* Saperettcm of fietal tone toportant fron the enolytleol and
pollottoo point of •tew »aing liqnid eojlotmn ebrosîtogrophy,
8n(IV) artanoBilleeta shoira o eation-exohcnge hehevioor

aifflilar to other niatartalo of thie elaaa praperod earlier* the
tn apectmai (Pig. 7) ahowa aoaia sharp end strons Iwmde at fre^nonoiea
- ^ 6O0|-''\îlO0,/^1800,.-^ K>00 and 33OO-37O0 <wo • Vhe firet two
hende indloate (85) the praoenee of arsenate to the atrootare*
in edditioii to the {!ietal.oxjên atretctiing vlhrettona (1I-0) whtoh
alao ahaort» in thia ranfê* The preaenee of 8i<»0»8t open eheina
or ringa tn the atmettira and the 81-0!! atretohtng vihrattone ere
evtdeneed by the abaorptton bands nepr the 1100 o«* and 5500 «§**
rangea reapaetlTely* nie freqn^ney band at 530O»5700 en alao
rapraaenta the region tn whioh external vater noleetilea abaoifi.
The TOA ennrea of thia aalt (rtg* 9) ahow that the pereant
weight loaa tn the aaiiple tn B^«.fom ta greater than that tn
Na^-fomi* It la obvioua baeaoae of the preeenoe of more protono
in the •tmetore of the for«er Material, ffie weight loaa tn the
anbatanee npto 5%0 6 tnelndea the renoral of external water nolo-
eitlea and •xe9B9 of AagOv (8^) fôv the atmetnre* The oondaaaatlon.
93
whtoh ttlubt have t>«ffBO oft«r ttil« toarpcmttsre pro^nblr oonttBiMt

^ t 9 'xy500 e e» t« •vtaftst froM ilie f«et that tin vetfijtit beeoK»»
eoBSti^fit fitter tht« tMip«rataf«* OB tHe 1bii«lc of i t s ^tsite^l ase.
l y t t e , then«>^rrvttietfT «n<! tnfr«rttf •taditi tli« follow tog foraols
m&y t«iiti^ttv«ly bo proposed for tbe ttetorlolt
Ôg.nuAod^.StOg .n BgO
ftie valoe of o (nesfeier of oxtenial ^cter noleeulee per «oleonlo

of tbo exobrtêr) eonee o»t to be 5«% bjr tbc Albertl*e metbc^ (S9)f
if i t te eesiiiied tbet iipto SOO 6 OBIIK exteni®! water isoieotilee
ere reisoired* A f«rtlM»r beetitte opto 3^ G tilf,bt ivetove tbe «itf»
Ae„0« froii tbe totol itfita of tbe exebciigcr« tbtte eoootrntiiis for
ea edditioar.l 5# wetgbt loeo*
Vttble 3C? illuetretee tbe KM voluee of i% wetrl iime in Wti^

mif W^m (m^ 1IC10|« Sone K^ walnee were eieo oibtainea aeiii^
rediotreeere • • ebowB i« teble X?X« Rffeet of BOlOj^ eonoentretioB
on tbe dittribotioa beberioor for Ci(X) ion io eboim in Hsore %
wbiob i s • Qeoal pbeaoneBon* Beeed on tbese obeervetiono eoae
taiporte»t binary neperetiano beve been eebieved on tbe oolmno
of titt(TY) aroeno oilioete (rige. 9 to i5)«
36
lEFBIBBHCES
!• H.Haoifmny K«rtB«i?|l«« ^ 17% (1969)*

&• l»T«B&r6tilcova ood 6*lf«Redloii9Vet lS*dto Chtote,' SOy 8% (I960)*
22^ W 7 («97t),
%« 0*AIt>«rtl« UtCoitcntitiot r«niOr«gorlo cmd B«forveoe«, tbid^
26^ e3%t (196%K
9* M«Qi!f«ifbiy B.tiMtr aa«i ft«B»Riiibor«t ^«Cli«««8oo*(A)9 878 (1970)*
S» MtQiirettity n*KfMmw ^nA I!»f»»Hatli9r«« tbtdt 1986 (t970K
7* NvQiireBbt, V«iri»i»r and H^SSahra^ ^•Chroeetc^r** £2^ 991 (1978)*
8* !f«Qiir«8lil end <l«p*llîitf J*Ioofi«Ktiol«€Sicis«» ^ 909 (196S)«
9* fl.^Nresbi m& Km^mV^rBhmyt ^^^^v 2 ^ 9081 (1968).
to. M.QQrethly 6*A«Nabi and !l»ISelire» Caned«J»Ghe@«, Jg^ 1667
C1977).
11. K«0«Veratuiey una A»A«Kh«tt, J*tn9ng«Ktwl«eii«i«» fkl^ 2%1 (1979)*
18« X.G.Varatmey and A.A^Khattf ¥alAttt«t ^ 989 (1978)*
19. lf.Qiirtatii and fi»e.iCiia«t)litt Aaal.Chaii.y 2S» ^^' (t977).
!%• f»8*flilnd« s.s.sandlitt and J«1P«8«w«t« Ohlii.Anal* (ir«r»inr)»
8%^ 69 (1979).
19* N.îir«alil» 8.Vinar and R.C.iCaaalilkt 8t|in.8el. ft Vrebnol.t
12^ 189 (1978).
16. N.Qiira»lil, fl.KiMar« •.Sliania and T.XIian, J.îromatoir.,
118, 179 (1976).
17. K.O.Vlirflhnay and A.Fr»«adaa« ^.Ll<|itld ClifiMiati»8«» f||, 919
(1981).
97
19* A«t«f^«lf *A f»st l«o!c of QaiBttt«tlir« ImmiiBte il8at9r»ls%
fltl* f«H»?!:oltfioff mitf ii*fi»ii»ti»r* ^ o l o M t r t e Misiyvts*, v ^ l * 5^

pp* i96» 3sci«>82» ikit«tiitti«ft««| mw ti>nc«
tl» 8«ll*Ftti»i!iit •StmitSArd MstHoas of UhceilesI Aii«ty»ti%
6tli #«•« vol* i« |}|»» t i 7 « i f t fOn HO«tf©iidt prlnoefOBy
ntm fOft (t969)*
iS« ll«l«f^}|» ena K«V«p»|i^r, ^vaioaîloott 11299 <t9l9)»
99* 0«ll«lteOt «di«itlo«l i^plloailflas of Hifi^rea lôtrooeo|^«
{»• SSSy AoiMtiîo PvtoOt lHOtt !*«« VOfli Ct969)«
&%• e«I)ar«l» •DiOf««iito fttomofrflvteotrte Molfvto** ^ a 1l»«ra*»
p* S»>9» Eloovlor fitl^lltttitai Go«» »•« Toft (i9$9)*
if* G«All»«rtt« Btforrotton ana ^•eoato^ <l»Iiioti*1ta«l»ai««*«
Ion E <change Method for the Detection of Aliphatic and
Aromatic Aldehydes
taklul Z«l«r Ouf*«hl, M. 8. RalM, and Shahan* Bafl«
On/tf rtn^nnr of CfnmtUn' Aitggrh Uv^l-m UmvtrMily Aiigmh imit
l<(<c,,i|». inn exi-hjmtc r''«in« hov* h w n tm»d (or the er lest pven bv I''eigl ( / ' I was ba.»iHl on iai.«K«>d aurlor
«J»lp<'»'n «nd fipdnmnBtinn "( ntRHnk (tinrtinniil gTT»i|>f> ation of the omdation <•' p pbeiiyU'iidiamine bv h ^ i ' i|c ri
{t 4\ h% "Ri-"!!! Spilt T " ! rpchniif"i ' pr'Mxidc However, compininds like c\«noh\drii|i a H - ' .df-
piiirmiiti' r t ili'iI'lnfWf) lhi» Iprhnmn? «nd eniplovprt it ammonia, and aliphatic and aromatic oxim" iiuittcd'd
to imrcnw th( I'.isivitv "f thr l e t for Ihp d f l r r l i o n of in with tht» test
ofpj/inK I'lti" (A ^1 Sotin" tr<>t.<( liavp dlno been rtt'Trihcd for In the present connminicatii ••» describe a new lout
the drtKtKin nl ort^ntiic i<im|w)uri(t« mirh SR phowili. nli for 111"' lietpclioii •>( nliphniir ' aromatic alih-hviles
phfltic nminM, primiirv nrnmntir nmiMPo, «I<lphv<lo«, «nd using ion exchange r e m bends as i l ' (ectimi m'-iliiim
m i M i d i t f d hsdnii?mps ( 9 - / / I All ih<^p t c i t i arc Ihe
m"Hi(i<«ti<in of thpir c l o r rcii-Iions dlrffldy known. How l-.XrFRIMKNTAl,
pvfr. rrmn tipnds can also \K ii«cd to develop new color Resxeots All (hpoiitnU nued wfrcof ffSKeni (trs*i^
tt'fldion Bi' wan dpurriHed bv îiri's-lii for diphpnylnmine Test Sotiilinns, SoUi'ifinn of ftlileln <le-* wcrt> prcptirfil i'ith»'f lii
(12) Ion pxchongc rt'sin sets ai sn pffxient ontalvil. They W^ nicohni iiT in watoi (trte from ainmi"nuin KMWI
Rrsini. Dnwcx WW Xrt (20 Ml mesh) and Amlinlil. (!«' M r»«
CHn hrinR shixit hydrolvif iindrr n-lBtively mild condi-
in« were ii.ipd ofler ihe uiiial regenrriui(»n aod ("MvyrMt.ti to ilie
tionn without the introduction of anv new ions They IV U'ftn The resin» wi're wftshed witli dpinmeriili/ed v.itivr until
should, therefore, prove «dv«nt«(!eoiiR in all these reac- wivolor wsBiitilniiii'd liv NCSSIIT'S rciiKPnl
tions where hvdrolvHis in [H-rfornied prior to detection. Mixture of aaluraled Solution of llvdroRen tysnide «n<l .So
Such methods can be developed for other orgnnio func- dium Cyantde. A to ml saturated solution of soduun i \H0idi 'vns
tional ((roups as well, added to a 50 ml ^fparating funnel luntaming I fi ^tam* "I dry
AmlMTlile IR IZ<i in H ' form The lumwl wa« priAi'l<i' «iili a
A number of testi (or the detection of aldehydes are glasswonl plup The contents were "hakeii and Ih"" rp'.jii »«•< «l
based on the formation of colored Schiff bases when al lowed to settle down The suiicrnstanl liqiiH l» n<i«iiio- nl
dehydes are condensed with primary amines Feigl (13) N»CN HC'N) was used directly in the form of ilnijis hy '|M ning
described a method for the detection of aromatic al- the stopcocks For better results, it is advisitilc In u*v the loiier
dehydes. The aldehydes formed Schiff bases with A'.A'- natant liquid within 4 hours.
dimethylphenylenedianiine in the presence of acid The Procedure, Place ahoul 5- Id ion cxihimge beads in H ' fiirm in
test covered a number of aromatic aldehydes but it gave a a micro (cstlube, add I drop (0 05 ml) of the test •<olutiun, i drops
of a saturntcd mixture of HCN and NaCN solution, and I drop of
positive test with aliphatic unsaturated with tnore than coned sulfuric acid. Heat the contents to hoil'OK USHIK a low
one double bond conjugate with carbonyl group. Anotbei flame (Caution: Take precaution aitainst harnifnt vspor** of Ht'N
Schiff base test for the detection of aliphatic and aromatic gas which comes out during heatitifi ) Wash Ihp o in l>ertdi. uiih
aUJfhydes was de.scribed by Wasioky (/•/) using 0-dianisi- dominera!i«'d water, blot them dr\ with a (luahtfOiu- ttliei (iftper
dine as condensation reagent. Certain ketones, alicylic (QuantitatiNe filter papt^r contains ammontuni ion,,) Add a drop
conipoiindi- such a-s pinenes and caniphenes interfered of Nessler's reagent A reddish pink color is developed at cm e on
the besd surface if the teal .solution coiusins ildftivdf Tli" .ep-i
with the test, A spot test was given by Anger ()5) for tl-p tivity cj( the test may be miprovcH if fre^hlj rcmii»fr«!»-d tesm in
detection of aromatic aldehydes along with polysar wet form is used
cimrides, pentose, hexiwes. celluloses, ethers, and e-slcrs of
cell'ilnses and N-arvlidene compounds. A general test RESIJMS
bas(»d upon the characteristic yellow color between chlo Detection nf Aldehydn's. To find the most suitable
rite m neutral or acidic medium was described by Hs.shnii re-in for Hie deU'ction of aldehvdfs, thi lidiiming resins
t'l o/,, (/6) but aldehydes such as anisaldehyde, vanillin, were tried: Ambeilite IK('-.'iO and iJowex vW > ' ! OO 'n
iH'Tolcin, p-dimelhylamirobenialdehydc, glucose, vpra- niorth^.
ivaldelivde. and glvceraldehyde gave negative tests Anoth- It was found that the carbosvltc resin, Aiiiberlut' IKC-
•SO gaie neRalive te^ts with croton.sldehvde, ciuruuoal-
(II M Oure»hl, S Z Ouieahl, and S C Slnghal, Anal ChBm , 4 0 t7S1
(1968) rielivde, nod f dimethjlaniinoben/aldrhvdt As a result of
(?) M Oureshi nn/J S i Oumshl, ;4n»/ Chim Ada 34,108(1966) this stiid\ it was concluded that U^vex 5<)V\ Xi^ was (he
(31 P W Wa^l M Ouroshi, aiH) S Z UursshI, Anal Chim Acta 36, he*.! lesin for the detection of iildehvdes
9 ' 11966)
(4) M OurMt.1, .S Z OuresMi and N /niva. Anal Chi,n Arta 47,189
I'hi- following aliphatic and aroninlic aldebvdes giof a
(1966) positive test bv the resin tiead?, ineth'id' aceiindchvdf, o\
(51 M fujlmolo, Cham:sl Analym 4 0 . 4 11960) iaahU'hyde, ben/iddehvdv, (roton«i''i'hvrte, i i o n n i i ' i l
(6) M Fii]imiM.OtillChern Soc Jaii ,?0, W ( I ' l S ' i
(7) M ^^|lm<l(^> flu'l Chwi Soc .Ian 30, 283 i »«(>
dehvdes. p diinellivliiTniooli(u,Hldclo(le. f<"inHldel!,i(<'
(8t H K«b(fi3n,T, V Mnrl, a'ld > ^ amrtsoki Nip^'f^n f aq^k'i /-"ftl^ 71 pnipionnldohyde. pHinldehN dc. and sijluvlaldohydc
90V 118«<) A negative lest was obtaiiicil f " i the ("llowoii; "I
(9) A U u ) ! , N'Bpf>n(<»q4l(ii7aiiSW, » 1 , I »• I19«01
(10) W Oodonliftinier, B Krtson, end *j »»f)n. Anal Ch>in At-, ?9
deh\di"i: t,4,fi nie(bi'X\hi'n.,':ildihMli' i liiitsi il li''i, I-
5112 (1!)63) \ i i n ' I ' u i (v>diuc^ a \ellM-.\ toitodit', ntttr kot pi. . i
( I I T A I'.gil N'Cm>n>(«9»liu?,iMh', »«, 9 1 » ( 1 9 t i M (11 MM.N
(1.?. M Ouo*<h'sod S 7 Qviethi, Anai Chem . 36. I'l'^s ( f f t R l
lt3» F l-*Kjl. 1 prt'i Do* .-»nd 6 JunuÂis, Ch*tiTl flpn-ysf 5?. 1 M
f l f h i i v i o r of Misc*d.4tM'oUH t'oinpound'
('Or.l, tvpii.'ii or^'HiiK (iti'U"'lilwN "t-ri t ^ ' ' i i
no n W.<,!L-kvsndO Pr«»id»n MIkfKiTi Ac>a I ! , 6 ( I 4 . U |
05l J /ny<»f . i . d S Otfl. f/K*i/);.;s / 4 - s , r'.'i«'-»i 'VOft, 4?? iÔ(,il
.'h M H M i ' n m i A A Av 17 .,'ifi A AtwniHl .1 , ( n^c, tit î'"<
T«M» t. l-«»nlt of W«- 'i J l t o n of AHphntie HIMI
Amfn*t)<- Ald»hjf<t 1*
».
Ma«w Vf*«» AaMiHK
AM»»-r*» •VI*M« UkM. twt) ^>M'V'<, <jl«)
Vrtit'xmVhh.ik 0 (m 0 05 17 »
Ai»ilwM''iti!' 0m 0 ts» 40 «
lJ#l)rÎd''livi)» 0 01 0 m ,11 8
l'<)rin«)<l<"liv<I<" n 01 0 oa »» 0
SdlirtsHi-hy'lr 0 Ot 0 in .<M «
Cinnnnmldcht'l'i 0 01 ^ 0,1 ^1» «
PTOpiciimliicl'i 1 0 01 f) 03 n 44
i»(i*«l>'Milr)fh>. '•• n 01 0 fll ?B B
A<-«t«)<l«hy<ii- 0 01 0 01 1» 2
p-I)im(*tlivl*iniii(>-
hrnaidfhvdt 0 01 (1 03 U 7
Table II. D«>lect(im of Pormnldehrdp Jn th^

Prc««nee of ForelRt Suhxtanoea
AnHmot i<^
(bmlitii
wtrtUnc^
Aiwûi* >>f
Hcmi
lilll
FoMlcn lUthitMw* tMtd, mn dttt«Ct«t, Ml
Acetic acid SM 30
Biilaitol 324 30
Oioxan 776 an
Ethvl methyl ketone 60-i 30
Piwnol 482 30
Triraethylamme 231 30
Xylene 487 80
I
Table III. Uetootionof Benzaldehydein the
Fresenvt' of Foxeign Substances
i
At> 'iiatof
f-rwiltn Amount of
Buhstanoo 1 .j).i;!»o
I'nn^ltn mxbBt«nc« ndtfed, mK <l«i(«to(i, ^tt
Acetic acid 167 30

Uutnnol 666 .TO
Uioxan 207 30
Ethyl imitliyl ketone 8U 30
Truuethylamune 165 30
Phenol 107 30 .S A J
Table IV. Testa for Aldehydes. Amides, and

Nitrili-8 and Other Organic Compounds •r
lon-KKchnnRe If.n-ejtrlmivrp Ion ort hatiKQ
OimpnuiMl
Arnmoiic and aliphatic

nmide teAt lutrjlp t««1 Hlflnfiytie tont
II
aldehydoo Negative Negative Positive
Nil riles Positive Positive Posit live
Unetilietituted amides
and imidea Positive Positive Positive
Other organic com- I i%
pouniis Negative Negative Negative
mended procedure and were found not to intertere (vith

the (est The following corn pounds were tested
H\dii>inrhoni nnd their dirwativen Benzene, toluene,
broniobeniene. nitrobenzene. catfconteirachlorKle
II
Amiw*. Aniline, ditnethvlflmiiie, trimelhylamine
Almhoh Methanol cthanol bolanol S
Artds Formir acid, H< etic »cid •3
A'''((in.'s At clone, acetdphpiio.tf ethvl tnethvl Itttone
ii fsi
ill
h'ther-, Dionan.elhei J 3 •3 s
I'h'^niA Phenol < 5
IMn . AMMYTlCAL Ctll *<IMnv »iOl 4fi l>4'
A number of ketone* were teoted by this method an't
l'nrhth\<h<iif- Glueow. fructito" .irt<!<«. gave a negative test The reason is that in tho ' <4'ê of Vi-
Umtl of lil'^'itificmlnn. The limil .if idrntificiKioti for • tones. WBCtion (ti^ above is generallv revp-r^tlile. whweax
numhrr <>( sliphnlir nnd uromstir (ildfhvftw «•«« dttcr- in the rase of aldehydes and most non lii-.îirrrl kflones,
minrd Th»r»«ull«»f»nimmiiriitH in Tnhle I the formation of cvanhydriiw is e'lenlially qoandtativ* if
iMwtlon of Aldehvdp* In the PrB»HHse of for«lni strr.ng acid is added to the miitiire containing sodium cy-
HvbuUnr**. Thr- (iftottion of nldehyde* in the prmencf of anide (/A)
» lurff amount of fon-lKn nulwUnce was studied Formal- As wa' expected, a p"eitiv» test obtained with ni-
<li ti\df and bcnrBlflchvde wprc taken an the itprenenta- triles, unsaturated ami-if^. and \n\\ n's. To dintingulah
liie i>f the aliphatK and aromatic aldehyde* The multa amortg the three functional groups, three tests are rerom-
are aummarized in Table* II and III mended- i ». the ion exihange amide tut ! C. Hv i'îi r\
change nitrite test (-», and the preteitt i''i> f\i tm-iKi" "ilrte
DISCUSSION hyde test Results given by the three teslji arc nuninvsti/ed
When aqueoua {lolution* of aldehydes are heated with in Table IV.
Maturated NafN containinft HON, together with a alight A comparison of different testa for aldehydes has been
exreta of aulfuric acid and beada of cation-exchange renin, summarized in Table V which proves the merits of the
ryanhydrina ate formed. The resin in the hydrogen form "Ion Exchange Test" in terms of factors such us limpliei-
cat4ilyzei the hydrolyaia of the cyanhydrins to carhoiylic ty, sensitivity, and specificity over the available aldehydes
acida and ammonium iona. The ammonium ions are re- testa mentioned in tlie literature.
tained by the reain and are later detected in the ben - by
Nensler'o reagent. The reaction sequence is the following:. ACKNOWLEDGMENT
We thank W. Rahman, Head, Department of Phe-îstry
for providing research facilities and Mohsin Qure«hi for
his helpful suggestions.
RCHO + CN" » * R CHCN «)
Received for review April 9, 1973. Accepted Derember 17,
I
RCHCN + HiO —• R CH<OH)CN + OH <ii)
1973.
(18) J D. Bobetts and M C Caserlco. 'Bas'r Prioclple-i o' Orgsnlo
RCH(OH)CN + H/3 + Rea'H* — Chemlttrir.' Jnd ed W A Benlainln. Uv. N»* "-ork >i » \''Si.
R CHfOHKXWH + Rffl~NH/ (iii) P 439
(19) M Ouraslll S Z Oureshl. and S C Pmoâl AnnI , «'»i dr's ,
Rea'NH, -t- Neasler's reagent (alkaline) —» red colored beads 13,361 (1971)
Talania Vol 26 pp 883 lo 884 0039 9140/79/0901 0883S02 00/0
® Pergamon Press Lid 1979 Printed in Great Britain
SELECTIVE ROLE OF OXIDANTS IN THE PRESENCE OF

CATION-EXCHANGE RESINS IN Na+-FORM FOR THE
DETECTION AND DIFFERENTIATION OF ACIDIC,
BASIC AND NEUTRAL AMINO-ACIDS
SAIDUL ZAFAR QURESHI and SHAHANA ANWAR

Department of Chemistry, Aligarh Muslim University, Aligarh, India
{Received 26 April 1978 Revised 5 February 1979 Accepted 22 February 1979)
Summary—A test for detection and differentiation of acidic, basic and neutral amino-acids is based
on use of a sulphonic acid cation-exchange resin in Na"'"-form, in the presence of various oxidants
(permanganate, dichromate, chromate, lod-'te, peroxide) and final detection with Nessler's reagent
Atninocarboxylic acids (a and fi) are usually detected chromate, bromate and lodate and a 0 2-vol hydrogen per-
with ninhydnn,' which is the most sensitive reagent oxide solution were used
and can even be used for their deamination However, Dowex 50W x 8 (20-50 mesh) resin was used in Na*-
form after washing with demineralized water until no
primary and secondary aliphatic amines, simple fis- colour was obtained with Nessler's reagent
sion products of proteins such as polypeptides, and
ascorbic acid also give a positive test with ninhydrin General test
Another test^ for a-aminocarboxyhc acids is based on To one drop of test solution in an ignition tube add
treatment with hypochlorite or chloramine-T,' the one drop of 1% potassium permanganate solution and
aldehyde formed being detected with fuchsin-sul- 5-10 ion-exchange beads (Na*-form) Heat in a boiling
water-bath for 2-3 mm Decant, leaving the resin beads
phurous acid but the sensitivity is poor and the test Wash the beads by decantation with 3 or 4 portions of
fails with compounds which are oxidized by the re- demineralized water Transfer the beads to a white spot-
agent, such as thiols, p-aminophenol, nitroso com- plate and dry them by blotting with fiher paper Add one
pounds and inorganic reductants drop of Nessler's reagent An immediate light pink colour
on the surface indicates the presence of amino-acid(s)
Feigl* described a test for salts of aliphatic and
aromatic amines based on their fusion with dry 'potas- Detection of acidic and neutral ammo-acids
sium thiocyanate and detection of the hydrogen sul- Perform the previous test, but replace the permanganate
phide produced This test was extended to a general solution by any of the other oxidants Basic amino-acids
test for amino-acids having carboxylic, sulphur, and give a negative test
imido groups ' According to Feigl, aminocarboxylic
acids, aromatic aminosulpho acids and compounds Detection of basic ammo-acids
If acidic and neutral amino-acids are absent, perform
containing both an acidic hydrogen atom (NH2,
the general test but replace the permanganate by one drop
-OH, -COOH, ASO3H2 groups) and (in another pos- each of 4M hydrochloric acid and 1% potassium bromate
ition) a basic nitrogen atom, also behave like salts solution
of amines The test can be applied for amino-acids
in presence of free amines, but amine and ammonium Differentiation between acidic and neutral amino-acids
salts interfere This test is not applicable in the pres- Perform the general test but replace the permanganate
by one drop of 0 005M sodium hydroxide followed by one
ence of organic compounds which form water during drop of 1% potassium dichromate solution A positive test
fusion and thereby evolve hydrogen sulphide from the IS given by acidic amino-acids only
potassium thiocyanate
Ion-exchange resin beads have been used exten-
sively for detection and determination of organic
functional groups ' " ' ' Here we describe theiiûse for RESULTS AND DISCUSSION
detection and differentiation of aminocarboxylic
acids The amino-acids in Table 1 all give positive results
in the general test and so do cystine, cysteine, valine,
EXPERIMENTAL
asparagine and glycylglycine Negative tests are given
Reagents by tyrosine, phenylalanine and tryptophan Isoleu-
Amino-acid solutions were prepared in water free from cine, valine, asparagine and glycylglycine fail to give
ammonia Aqueous 1% solutions of potassium dichromate, the test for neutral amino-acids
883
884 SHORT COMMUNICATIONS
Table 1 Limits of identification phonic acid group, weakly acidic resins do not give
the test
Molar Amounts
concentration detected, R-CH-COOH -f- O '^"°*
Feebly
R-C-COOH + H2O
Amino-acid of amino-acid MS oxidative
NH, NH Imino acid
a-Alanine 0 005 22
^-Alanine 0050 222
L-Proline 0010 23 Resin(Na'' + H + ) -1- M n O ; ^ Resin(Na+) + H*
Glycine 0005 19 + MnOi"
Methionine 0 010 30 Selective oxidant
Threonine 0005 30
Leucine 0010 104 R-C-COOH + H , 0 * R-C-COONH4
DL-Serine 0005 26 Selective
oxidant
Aspartic acid 0020 133 NH
Glutamic acid 0005 59 o
Lysine 0100 730 Keto-acid ammonium salt
Arginine 0100 870 Resin(Na-') + NH^ ;^ ResinCNH^) -I- Na"'
Histidine 0100 757
Resin(NH4) + Nessler's reagent —• Pink beads
No interference is given by hydrocarbons, alcohols,

When an aqueous solution of amino-acid is heated ethers, carboxylic acids, phenols, heterocyclic bases,
with potassium permanganate in the presence of amides, nitnles, amines and ketones Aldehydes are
cation-exchange resm beads in the H'^-form, de- easily sorbed on resin beads and give a reddish pink
amination takes place with evolution of ammonia A colour which finally changes to black (depending
positive test is given by one drop of Nessler's reagent upon the concentration) when the beads are directly
on the resin beads This test cannot be applied to treated with Nessler's reagent However, if the resin
the detection of amino-acids, as other organic func- beads are thoroughly washed with water before addi-
tional groups, such as amines, amides, imides and tion of the reagent no pmk or black precipitate is
nitnles, also give a positive test because of the oxi- obtained
dation of the amines or acid hydrolysis of the amides,
imides and nitnles Acknowledgement—We thank Prof W Rahman, Head of
Department of Chemistry, for providing research facilities
Surprisingly, if the resin beads are used in Na"^-
form, a positive test is obtained only with amino-
acids We suppose that in conversion of the resin into REFERENCES
Na"^-form, a small fraction of the H"^ ions will be 1 S Ruheman, J Chem Soc, 1910, 97, 1438, 2025, 1911
left and the resultant very low concentration of H"^ 99, 792, 1486
ions in the beads will be sufficient to make potassium 2 O Frehden and L Goldschmidt, Microchim Acta,
1937, 2, 186
permanganate a selective oxidant for amino-acids, but 3 F Feigl, Spot Test m Organic Analysis, 7th Ed, pp
insufficient to bring about acid hydrolysis or oxi- 295-296 Elsevier, Amsterdam, 1966
dation of other organic functional groups 4 F Feigl and H E Feigl, Mikrochim Acta, 1954, 85
The same will apply to the other oxidants tested, 5 M Qureshi, S Z Qureshi and S C Singhal, Anal
but as these have lower oxidation potentials than per- Chem, 1968, 40, 1781
6 M Qureshi and S Z Qureshi, Anal Chm Acta, 1966,
manganate the test becomes still more selective, with 34, 108
basic amino-acids failing to react The reason for the 7 P W West, M Qureshi and S Z Qureshi, ibid, 1966,
negative test for basic amino-acids is not known but 36,97
may be further reduction of the H*-ion concentration 8 M Qureshi, S Z Qureshi and N Zehra, ibid, 1966,
by protonation of the amino-acid This view is sup- 47, 169
9 S Z Qureshi, M S Rathi and S Bano, Anal Chem,
ported by the fact that when a basic amino-acid solu- 1974, 46, 1139
tion IS acidified with a drop of 4M hydrochloric acid 10 S Z Qureshi and M S Rathi, ibid, 1975, 47, 1424
It gives a positive test in the presence of potassium 11 M Qureshi and S Z Qureshi, ihid, 1966, 38, 1956
bromate (E° 1 45 V), but not in the presence of potas- 12 S Z Qureshi and I^zatuUah, Anal Chim Acta, 1977,
sium dichromate {E° 1 33 V) or chromate or potas- 99, 201
sium lodate or hydrogen peroxide (£" 1 23 V) 13 Idem, Z Anal Chem, 1977 285,265
14 S Z Qureshi and M S Rathi, Mifcrocîm Acta 1977
The following tentative mechanism is proposed 1, 11
This method depends on the use of resins with a sul- 15 S Z Qureshi and Izzatullah, Talanta, 1977, 24, 529
46 Fresenius Z. Anal. Chem., Band 298 (1979)
Abb. 1 a und b
Gas-Chromatogramme von
Barbital.
a Aus einer bei pH 1 mit Alher
perforierten Harnprobe;
b aus Harn nach Abtrennung als
Quecksilberverbindung; jeweils
eingesetzte Harnmengen: 20 ml
mit 0,3 mg Barbital; injizierte
Mengen/2 (JI Losung in
r^ r—.
0
' ' ' '
10
•-
Essigsaureethylester
Retentionszeit (min)
bj Gas-Chromatographie. Gas-Chromatograph HP 5835 A; Literatur

Detektor FID; Detektortemperatur 300"C; Injektortempe-
ratur 250° C; Trennsaule: 2 m Glassaule, 3 mm ID, 1 % OV 17 1. Hoeltzenbein, P., Bohn, G., Riicker, G.: Fresenius Z.
auf Chromosorb G-AW, DMCS 80/100mesh; Saulenofen: Anal. Chem. 292, 216-218 (1978)
Temperaturgrogramm 150-280°C, 87min, Tragergas 50 ml 2. Poethke, W., Fiirst, W.: Pharm. Zentralhalle 98, 171
He/min; Brenngase: 30 ml H2/min und 250 ml synthe- (1959)
tische Luft/min; Abschwachung 1:256, Papiervorschub 3. Reinert, M.: Arch. Exp. Pathol. Pharmakol. 130,49 (1928)
0,5cm/min. Eingegangen am 17. Mdrz 1979
Fresenius Z. Anal. Chem. 298,46 (1979) - © by Springer-Verlag 1979
Selective Detection of Fructose and Sucrose Procedure. Place about 4—6 beads of Dowex 50WX8
by. means of l-Chloro-2,4-dinitrobenzene (20 —50 mesh) (H"^ form) impregnated with l-chloro-2,4-
dinitrobenzene (saturated solution in chloroform) in a micro
and Ion-Exchange Resin test tube. Add 1 dropof the test solution followed by 1 drop of
50 % sulphuric acid and heat for 2 — 4 min on a boiling water
bath. An orange colour on the resin indicates the presence of
fructose or sucrose. The sensitivity of the test is enhanced, if
S. Z. Qureshi and Shahana Anwar freshly prepared resin is used while still moist.
Chemistry Department, Aligarh Muslim University, Glucose, lactose, xylose, rhamnose and arabinose gave
Aligarh 202001, U.P., India negative tests. Other characteristic colours were developed
with the following compounds: aniline (red), salicylaldehyde
SeJektiver Nachweis von Fructose und Saccharose (red), cinnamaldehyde (orange), diphenylamine (red),
mit l-Chlor-2,4-dinitrobenzol und lonenaustauscherharz methyl-n-propyl ketone (red).
The limit of identification was 14.4|.ig for fructose and
Key words: Nachw. von Fructose, Saccharose; lonenaus- 3.2 |ig for sucrose. In the detection of 14.4 |ig of fructose the
tausch; 1 -Chloro-2,4-dinitrobenzol following amounts of foreign compounds can be tolerated:
803 mg of acetophenonc, 1.9 mg of glycine, 24,6 mg of
A selective test for the detection of fructose and sucrose is nitrobenzene, 39.6 mg of acetic acid and 35.6 mg of aniline.
based on the reaction with 1-chloro-2,4-dinitrobenzene in the
presence of a cation-exchange resin in the H"^ form. Received February 19, 1979; revised April 17, 1979
Kurye Mitteilungen 45
Fresenms Z Anal Chem 2 9 8 , 4 5 - 4 6 (1979) - © by Spnnger-Verlag 1979
Abtrennung von Barbitursaurederivaten rederivate ohne den Zusatz von Barbitursaure unter 40 % Bei
Zusatz von Barbitursaure erhohen sie sich auf bis zu 80 % mit
und Phenytoin aus Harn als schwerlosliche ciner Standardabweichung von 4—7% (Tabellel)
Quecksilber-Verbindungen
zur gas-chromatographischen Analyse Tabellel. Gas-chromatographischer Nachweis einigei Arz-
neistoffc aus Harnproben nach Fallung als Quecksilberver-
bindungen Emgesetzte Harnmenge 20 ml, Arzneistoffkon-
P Hoeltzenbein*, G Bohn** und G Rucker zentration 1 (ig/ml
Institut fur Rechtsmedizin, von-Esmarch-Str 86**
und Institut fur Pharmazeutische Chemie, Arzneistoff a h a/b X i \
Hittorfstr 58, Westf Wilhelms-Universitat, D-4400 Munster
Barbital 60 9,2 6,5 70 4,15 1,84
Isolation of Barbiturates and Phenytoin Pentobarbital 84 4,5 18,6 73 5,84 2,38
from Urine Samples as Insoluble Mercury Compounds Secobarbital 88 24,9 3,5 67 6,70 2,73
for Gas-Chromatographic Analysis Hexobarbital 102 19,2 5,3 75 5,72 2,33
Key words: Best von Barbituraten, Phenytoin m Harn, Phenobarbital 56 14,1 4,0 80 4,44 1,81
Chromatographie, Gas, Hg-Verbmdungen v Barbituraten 11,0 74
Phenytoin 97 8,8 5,98 2,44
Bei der Abtrennung von Barbitursaurederivaten aus Harn aHohe der Arzneistoffbande (mm) 6Mittlere Hohc der
nach Stas-Otto gelangen auch zahlreiche korpereigene Sub- storenden Banden (mm) 0,5 min vor und nach der jeweiligen
stanzen, insbesondere Carbonsauren, in die Extrakte Diese Arzneistoffbande xMitdere Wiederfindungsrate (%) aus 6
interferieren bei der anschlieBenden gas-chromatographi- Emzelmessungen s Standardabweichung ( %) der Einzelmes-
schen Analyse nut den Substanzbanden der Barbitursaurede- sungen von Mittelwert x i^ Abweichung (%) des Mittelwer-
nvdte und deren Metaboliten BCurzhch benchtetcn wir uber tes X vom wahren Mittelwert
ein chromatographisches Verfahrcn an Extrelut" (E Merck,
Darmstadt) zur Abtrennung der Sauren aus Harnproben [1]
Nach Reinert [3] bilden Barbiturate mit HgCl2 schwer- Die Mittelwerte von jeweils 6 Einzelbestimmungen wei-
losliche Saize, aus welchen sich m salzsaurem Milieu chen vom wahren Mittelwert durchschnitthch nur um ± 2 %
die Ausgangsverbindungen wiedei freisetzen lassen [2] ab In alien Fallen war das Verhaltms der Intensitat der
Auf der Grundlage dieser Reaktion wurde ein Verfahren Arzneistoffpeaks A (MeBwert a, Tabelle 1) zur Intensitat der
zur Abtrennung der Barbitursauren und des Phenytoins aus storenden Peaks korpereigcner Substanzen (Blindweit h)
Harn zum Zwccke der gas-chromatographischen Analyse groBer als 2 Deutlich veranschaulichen dies die Gas-Chro-
erarbeitet Fur die Fallung dei Quecksilberverbindungen matogramme (Abb 1) von jeweils 0,3 mg Barbital in 20 ml
wuide der Harn mit 0,1 N KOH auf pH 12 eingestellt und mit medikamentcnfreiem Harn nach Stas-Otto-Extraktion bei
5%iger waBngci HgClj-Losung versetzt Unter diesen pH 1(a) und nach Fallung mit Quecksilberchloiid (b) Das
Versuchsbcdingungen bilden korpereigene Carbonsauren Chromatogramm b enthalt neben der Bande dcs Barbitals nur
keine schwerloslichen Quecksilbersalze, wie Untersuchungen noch gcnngfugig storendc Signale
nach Zusatz von Benzoesaure, Phenylessigsauie, Phenoxyes-
sigsaure, Hippuisaure, Lavulinsaure und Homovanillinsaure
zu medikamentcnfreiem Harn zeigten Arbeitsvorschrift
a) Aufbeieilung der Hainpi ohen Zu 20 ml Harn wurden unter
Zur quantitativen Ausfaliung von Barbitursaurederivaten Ruhren 10 mg Barbitursaure (1 % in Accton) gegebcn Mit
und dcs Phenytoins crwies sich dor Zusatz von Barbitursaure 0,1 N KOH wurde der Harn sodann auf pH 12 eingestellt und
als »Spurenningei« notwendig Diese biidct einerseits eine unmittelbar danach mit 10 ml 5 %igci HgClj-Lo-
schweiloslichc Quccksilberverbindung, andercrseits interfe- sung veisetzt Der gelbbiaun gefaibtc Niedeischlag wuide
iiert ihr Peak im Gas-Chromatogramm nicht mit denen der 20min bei 3500 U/min zentrifugieit, der Niedeischlag 3mal
Bai bitursauredcrivdte und des Phenytoins ErfahiungsgemaB mit H2O ausgewaschen und jeweils zentnfugiert Der nun
muflein furklinisch-bzw forensisch-toxikologische Analysen farblosc Ruckstand wurde in 10ml 6N NH4OH aufgenom-
anwcndbaies Vcitahren noch den Nachweis von weniger als menundmitkonz HCl auf pH 1 eingestellt Dieklaie Losung
1 mg Wirkstoff/1 Harn ermoghchen In diescm Konzentra- wurde nach Sattigung mit NaCl 3mal mit je 10 ml Essigsauie-
tionsbereich lagcn die Wiedcifindungsraten fui Barbitursau- ethylester mittels Vortex Mixer extiahieil "Die abgetrcnnten
organischen Phasen wurden vereinigt, ubci Na2S04 ge-
* Teil del Dissertation, Univcrsitat Munster, 1978 trocknet, cingedampft und der Ruckstand sodann in 100^1
** Koriespondcnzanschrift Essigsaureethylester aufgenommen

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Studies On The Detection and Spectrophotometric Determination of Organic Compounds and The Synthesis of A New Inorganic Ion-Exchanger

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studies on the Detection and

A THESIS SUB vIITTED FOR THE DEGREE OF

«tMi«i«l Xiitro4MtiMi* glvlag •> •««oait •f tli» i«|^rt«a«« ftf tli«

CSiaptar I I sonaariaaa tba aa loot I r a rola af oxldanta ia

^* i—«^> taati To ana drop of tha tast aolation takan in an

f i l t e r iMH>*r tb«y mtn t i « a t « « v i t l i • dmp o f 1l«»«l«r*s r««(4mt*

iM i M W d l a t * pink o o l v r en tb« •arf«o« l i i d l e a t « a t h * prttwno* ^ f

B* Petacttca of a e t d l c and mantra 1 tnwAno aetdat f » a t A wa»

p a r f o n w d by t a k i n g 1 ^ tBTO^/Kjflrj^O^/KlO^/nj^OQ i n plaoa of tha

IMmmmaiiata a o l n t i w i * Baale aaino aelda geva a aegatiTo t a a t .

e« patootlon o f baa to a«ljio aotdai I f a e i d i c and n a u t r a l aaino

aoida ara abaant tha t e a t aay ba perfomad by repleelng pamangaaata

by one drop aaeb of %M hydroehlorlo aoid and t% potaaatna broaato

D* P l f f a r a n t l a t l o p botwaaw a c t d l c and n a u t r a l awtno aetdat I n tha

ganeral t a a t Aaaertbad aboira tha pamaaganato vaa replaead by a

drop of 0«005N aodiim hydroxlda follawod by a drop of 1 ^ potaaalim

dlohrcmata a o l n t l m i * A poaltiira t a a t I n d i e a t e a tha praaanoa of

r a b l a X givoa tha I t a l t of I d o n t l f l o a t i o n of a e l d i e , baalo

•ad a o n t r a l aaiao aetdsvblla t a b l a o I I - X T anaaartoo t t e o f f a o t of

foroiga oAotaaooa on tho dotootioa of o i l tha throa typoo of aalao

aotdo* A t o a t a t t v o aeohoaioa haa alao boea proposed f o r t h e

Cbapter XXI gtvoo aa aoooiait of a aonottlya «ad opoelf to

raata bead t o o t f o r t i t o t i d i a a aad I t a opoetropliotoaetrio dotomtaotii

no lag t B r O j • • a laagoat* The aothod f o l l o w e d f o r the dotootioa off

A* m»»qtion »roe»<«f f»r titttldlBai A f«v re* in beadt (Va^^fom)

B* Psteriination of hietldinot A s a a l l aaotmt ('-^O.i • ! ) of tho

I f f o o t s of ^ 9 roagstttOf t i a e aad toaporaturo have boon

UNIT or HKMTIF:EOATIOIf <NP ACIDIC. BASIC AKD

RBtDTRAt AJflNO ACXDB

JL -Alan In* 5s 10-5 0.05 22.8

UMIT OF TOIBHAWCE OP VAaiOPS rOBEI«m SUBSTAHCTS

' • I " '" t '' I

erotfmaidehyd* 2 a 10"^ 0*t B«3

SttoroMi 1 x 10*' 0.2 1.4

At«ton« 1 X toT^ O.t e*9

iU«ti9 aei« 1 m iST^ 0.9 IS.O

rfil41ii« 1 X to** 0*5 2«4

Bmstno 1 X 10** 0*5 2.3

u m r <y TOUIKMICE or TAmopg roHEigK BmstmcBB

' ' I ' I ' 't

ett» ton A1 dehydd 2 X 10"* 0,2 2.t

8«eros« 1 JE 10*^ 0.3 1«0

M«t<MI« 2 X 10** 0.2 2.3

Fyrldlne 1 X to** 0.2 l.«

Aalsidlne 1 X 10"* 0,3 2.9

A««it« aeid 1 X 10"* 0.3 it.o

ilC»t«Bi«* i X 10"* 0.3 l.t

BthF^mia* l.« 0.% 19.0

UMn OF TOUMIAIICB OF •AMOPS FOBEIOM SOaSTAMClS

Ao«toii« 2 X 10*^^ 0.4 4.€

JUMtMlidO 1 X 10*^' 0.5 3.0

•MIS«II« t s ur^^ 0.5 3.5

fhnmtwu 1 X 10*^^ 0.5 9.0

W^Kfl • • t t l F l IC«tQM« 1 X tO*^^ 0.6 4.3

FFTitfln* 1 X 10"^^ 0.5 3.5

IIBFIKMDOeiiXUTT AND nOEOISlON DATil m

1. 1.0 ©•30 0,38 0.33 0.94 0.30 0.98

f i l t e r iMH>r tb«y mtn t i « a t « « v i t l i • dmp o f 1l«»«l«rs r««(4mt*

About 46 tim«4»xeli«iig« rmniM lb««d» imprtgiiat*4 v l t l i tii«

Irfntf 9w$mvwi9tm eatf cttt««ft«« t^l» wofle ««• eoii|plt«i fli« ! •

fr«»«nto» 2:Aiial«€fe«»t j ^ 89S Ct9t9)*

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how t h * S!!f>«ti»nc«e Ti»«»hfiv«» imtfer th« eanrtttlons f»!lfh |cov*»ni the

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