CHAPTER - 6

Rapid solvent extraction of gpld(III)

with high molecular weight amine

from organic acid solution

 191

CHAPTER-6

Rapid solvent extraction of gold(III) with high molecular weight

amine from organic acid solution.

6.1 Introduction

The importance of gold in human life as well as its fascination for

scientists has been appreciated right from alchemist times until the present
day. This metal is found in about 3.5 ppb in the earths crust, often as 75-
90% pure native gold that has been released by the weathering of
sedimentary and igneous rocks. Gold is one of the most ancient metals used
in the arts and jewellery, and it is of growing importance in technology
because of its resistance to corrosion, ft commands a premium price
because of its low abundance in nature. Hie economy of a nation depends to
a significant extent on the size of its gold reserves.

Many alloys used in dentistry contain gold, silver and copper, often
with small amounts of platinum and palladium. The utility of gold or gold
salts has been recognized since the time of Ayurveda, the ancient Indian
medical science (1500-1000 BC). In ancient Indian philosophy many
remedial uses of gold in curing patients were described.

It is worthwhile here to stress the advantages of organic acid media

over mineral acid media. One of the distinct advantages of the organic acid
media is the facility of controlling the concentration of complexing ligand,
the ease of adjustment of pH and the wide difference in pH at which various
metals form anionic complexes. The comparative ease of stripping of the

This work has been published in Gold Bulletin 34(2001) 50.

 192

complexes from the organic phase can be achieved by fully exploiting the
difference in reactivity of various metals to extraction back into the aqueous
phase by mineral acid. It is known that organic acid media offer better
separation of metals possibly due to high stability of metal-organic acid
complexes.

6.2 Summary of methods for solvent extraction of gold(III)

The preconcentration of metals from complex matrices of natural

samples obtained by using high molecular weight amine (HMWA)
extractants is well known [1] but little work has been reported on the
extraction of gold, particularly by secondaiy amines. However, the solvent
extraction technique using HMWA and ammonium salts is effective for
extracting gold. It is also effective for the separation of gold from other
associated elements. Some HMWA have been used for extraction
separation and determination of gold(III) from real samples.

Pohlandt has reported the effectiveness of n-octylaniline [2-6] as an

extractant for noble metals. The extraction depends upon the method of
preparation of the reagent. Some of the drawbacks of the method are
(i) emulsion formation, (ii) requirement of more equilibration time (30 min),
(iii) higher reagent concentration and (iv) the need of multiple extraction.
Before extraction of gold(IH), the base metals Cu, Ni, Co and Fe must be
removed from the 3M hydrochloric acid solution of gold(m) and platinum
group elements. The extraction of gold(HJ) from hydrochloric and
hydrobromic acid with 5% tri-iso-octylamine (TIOA) solution in carbon
tetrachloride has been studied [7]. The coextracted Fe(III) was masked with
potassium dihydrogen phosphate. The method suffers from interferences of
anions like thiocyanate, cyanide, sulphide, sulphite, thiosulphate, EDTA,
bromide, nitrite and iodide and cation Ag(I) seriously interfere. The
extraction of gold(III) with trioctylamine (TOA), trioctyl methyl ammonium
 193

chloride [TOMA(Cl)J. trioctylmethyl ammonium bromide [TOMA(Br)]

from hydrochloric or hydrobromic acid solution by using diluents as
kerosene or carbon tetrachloride has been carried out in combination with
atomic absorption spectrometry [8-10]. A preconcentration step was
required since as low concentration of gold and chemical separations are
usually necessary to avoid a matrix effect. The extraction of gold(III) from
hydrochloric acid solution with N-bemyl aniline in chloroform was
investigated and stripped with thiourea [11]. Gold(IH) from alkaline
cyanide solution was extracted by primary amine N 1923 and was studied
using radioactive tracer method [12]. Aggregations were formed above
gold(III) concentration 10 gL'1. NN’-Diphenylbenzamidine in chloroform
was used as an extractant for gold(IQ) from 0.3 M hydrochloric acid
medium [13]. Method was extended for analysis of geological samples.

Gold(QI) was extracted into chloroform from an aqueous solution

over the range 4M hydrochloric acid to pH 11 containing zephiramine and
potassium iodide [14], which followed determination by atomic absorption
spectrometry. Cu(II), which interferes was masked with 1,10-
phenanthroline. Tervalent gold was extracted as HAtiCU from hydrochloric
acid medium into 1,2-dichloroethane-kerosene with NN-di-s-octylglyeine
[15]. NN-di-(l-methyl heptyl)glycine in 1,2-dichloroethane-kerosene was
used to extract gold(m) from aqueous hydrochloric acid medium [16]. Sub­
microgram amount of gold(IH) was extracted with 1,4-butylenebis-(N-
hexadecyl-NN-dimethyl-ammonium bromide) in chloroform from an
aqueous phase in hydrochloric acid and potassium iodide [17]. Such method
can be used to determine > 0.02 ppm of gold(IH) in rocks, ores and flotation
tailings. Gold(III) from pulverized geological material was extracted and
determined with Aliquat 336 in di-isobutyl ketone in combination with
graphite-fomace atomic absorption spectrometry [18]. Tertiary amine
 194

Hostarex A 327 in n-decane was found an effective extractant for goId(III)

from hydrochloric acid solution [19]. The extraction reaction was found to
exothermic and the extraction equilibrium depends on the ionic strength.
Solvent extraction of gold(UI) with 1,2,3-benzotriazole in n-butanol was
studied at pH 3.0 [20]. Extraction of gold(HI) from solution of ores into
2-hexylpyridine in xylene was studied, for subsequent determination by
AAS [21]. Gold(HI) was extracted from aqueous hydrochloric acid medium
with an equal volume of chloroform containing N-tolyl-2-picolinethioamide
and determined radiometrically with use of tracers. But the method suffers
from interference by KI and thiourea [22].

Methods have been developed for the extraction of gold(IH) with

sulphur containing extractants. Ideal conditions for the extraction of
goldpt) with 2-mercaptobenzothiazole into butyl acetate and chloroform
have been established, but foe methods suffers from interference by large
number of anions and cations [23,24]. Dioctyl sulphoxide in various diluents
was used as an extractant for gold(IH) from hydrochloric or hydrobromic
acid medium and determined gold(III) by AAS [25,26]. Down to 20 ppb of
gold(IQ) in 3M hydrochloric acid medium was extrcted into dioctyl sulphide
in xylene for atomic absorption determination [27]. The extraction of
gold(HI) with petroleum sulphides in toluene was achieved from
hydrochloric acid medium, foe method did not suffer from interference of a
1000-fold excess of other metals [28,29]. Fire-assay extraction pre-
concentration of gold(Ql) with petroleum sulphides-alkylaniline
hydrochloride was studied and analytes were determined in foe organic
phase by flame or electrothermal AAS [30]. The simple and rapid method
was developed for extraction of gold(HI) with bis-(2,2,4-trimefoylpentyl)
sulphide-sulphonated kerosene but Pd(II) and Hg(I) coextract, Sb and Sn
interfere [31]. The extraction of gold(III) was carried out from aqueous acid
 195

solution with dibutyl sulfide and compared with dibutyl selenide and
telluride [32]. It was found that 7,10-dithia-hexadeeane and 2,5,9,12-
benzotetrathiacyclopentadecane (thioethers) were powerful extractants for
gold(I) [33]. The thioethers in combination with a reducing agent efficiently
extract gold(III). Solvent extraction of gold(III) using thionalide in ethyl
methyl ketone or isobutyl methyl ketone at pH 5.0 was studied [34]. In this
method citric acid tartaric acid was added as masking agent for natural
matrices.

The method has been developed for rapid and selective extraction of
gold(III) with ethyl thioacetoacetate into chloroform at pH 4.0 [35]. The
method suffers from interference by ions like cyanide, sulphide,
thiosulphate, Ag(I), Hg(H) and Cu(D). The extraction method has been
developed for gold(III) with benzothiazole-2-thiol into chloroform and
portions of organic and aqueous phases were measured by y-activity [36].
Bromate and sulphur containing anions strongly interfered in this method
and were decomposed with nitric acid. A solution was made 0.5 M in NN’-
di-o-tolyl-2-thiourea and the gold(m) was extracted into butyl acetate for
direct atomic absorption spectrometric determination [37]. Nonyl-benzyl and
dodecyl-thiourea were prepared as novel extractants for gold(m) and found
- 1 — -

highly selective in very acidic solution containing CT and m the presence of

Cu(H) and Fe(III) [38]. The extraction of gold(m) with N-substituted
benzoylthioureas as N-benzoyl-N’N’-diphenyl-, N-benzoyl-N’phenyl-, N-
benzoyl-N’-hexyl- and N-benzoyl N’N’-dihexylthiourea in toluene from
hydrochloric acid medium was investigated [39]. Selective liquid-liquid
extraction of gold(m) from aqueous chloride media into cumene by thiourea
derivatives namely 2a-c (N-thiocarbamoylbenzamidine derivatives), 3a-f (N-
benzoylthiourea derivatives) has been investigated in detail [40]. The lack of
interference from even appreciable amounts of base metals may be
considered an outstanding advantage of the method. The extraction
 196

properties of the sulphide podand l,l2-di-2-thienyl-2,5,8,l 1-

tetrathiadodecane (TTD) in 1,2-dichloroethane, chloroform and methyl
isobutyl ketone for goId(III) in acid media have been examined [41]. Basic
studies for extraction of gold(III) with dibenzylammonium
dibenzyldithiocarbamate (DBADBDC) into chloroform were conducted at
pH more than 4 [42]. The extraction mechanism of complex was examined
in the presence of chloride ion in an aqueous solution, and extraction
reactions and extraction coefficients were proposed and calculated
respectively. The solvent extraction of gold(in) from hydrochloric add
medium with bis (n-octylsulfine) ethane (BOSE) in butyl acetate was studied
[43] . It provides a rapid and highly selective method for separation of
gold(HI) from common and noble metal ions. The composition of extracted
complex and 1he mechanism of the extraction of gold(IQ) are discussed.
Oxygen containing solvents acts as an extractants, metals are
extracted by these solvents by the process known as oxonium extraction
system where metal ion gets solvated by the solvent interacting the oxygen
from solvent with metal ion. The extraction of gold(HI) from nitric acid
solution by means of various oxygen containing solvents has been discussed
[44] . The most effective solvents are di-isopropyl ether and diethyl ether.
Isobutyl methyl jcetone (MIBK) was used as an extractant for gold(QI) [45-
51]. These methods are useful for (i) separation of traces of gold(III) from
macro amounts of iron [46], (ii) determination of gold(IH) in wood sample
[48], (iii) human urine [50] and (iv) in geological matrix [51]. The solution
of gold(III) in hydrochloric acid medium was extracted with 4-methyl-1,3-
dioxolan-2-one in chloroform [52]. The composition of extracted species
was AuCLf. The use of 3-methylbutanol as an extractant for gold(m) from
aqueous hydrochloric acid medium is discussed [53]. Interference by Fe and
Cu was overcome by using the standard addition technique. The gold(III)
was separated by double extraction with ethyl methyl ketone-chloroform
from hydrochloric acid or nitric acid media [54]. Gold(III) was extracted
 197

selectively from 10% acid solution into ethyl ether [55]. Ethyl acetate has
been used as an extractant for gold(III) from hydrochloric acid medium and
analysed gold(III) by y-ray spectrometry with high purity Ge detector [56].

Organophosphorous reagents are most important for the extraction

separation and recovery of noble metals from very dilute solution. The
gold(III) can be extracted only in alkline thiosulphate solution with alkyl
phosphorus ester [57]. The additioin of ammonia to thiosulfate solution has
a strong influence on the mechanism of the extraction of gold(Hl). A
solution of 0.1 M trioctylphosphine oxide in isobutyl methyl ketone extracts
gold(m) from equal volume of aqueous solution containing hydrochloric
acid, potassium iodide and ascorbic acid [58]. Trioctylphosphine in isobutyl
methyl ketone has been used as an extractant for gold(III) and determined
gold by AAS [59]. The use of tris-(2-ethylhexyl) phosphate in toluene for
extraction of gold(m) has been discussed [60]. Thiocyanate and thiosulfate
interfere seriously and must be absent. Tributyl phosphate has been used as
an effective extractant for gold(III) [61]. GoldflIII extraction from .
hydrochloric acid media was studied in detail by using tetra-buty1-1,3- (I

xylylenediphosphonate [62]. The selectivity of extraction, stripping and

extraction kinetics were evaluated in relation to the recovery of gold(lH)
from acidic waste solutions. Small amounts of gold(HI) can be completely
extracted with bis (methylheptyl) methylphosphonate from hydrochloric
acid media [63]. The effectiveness of cyanex 471 X as extractant of gold(UI)
from hydrochloric acid solution is demonstrated [64], The extraction system
is endothermic and experimental variable influence it. The partition of
gold(m) from hydrochloric acid solutions by the phosphine oxide Cynex
921 has been studied [65]. The extraction system is exothermic, the
extraction being influenced by several variables. Stripping of gold(III) was
achieved effectively with water and the reaction is endothermic. Extraction
of gold(I) with Cyanex 923 in xylene was studied and selectivity of system
was also investigated [66,67]. The extraction of gold(III) from hydrochloric
 198

acid solutions by l-(dodecyloxy)-3-methyl-l-oxo-A3-phospholen, l-(2-

ethylhexy-loxy)-3-methy1-1 -oxo-A3-phospholen and 1 -(2,6-dimethylhept-4-
yloxy)-3-methyl-l-oxo-A3 phospholen dissolved in cumene, kerosene and

toluene have been studied [68].

The sample solution containing gold(M), upto 3M hydrochloric acid

was extracted with 2 mL 0.5M solution of alkylaniline (alkyl = Cg to Ci0) in
toluene and determined gold(III) in toluene phase by atomic absorption
spectrometry [69]. The extraction of gold(IH) from sulphuric acid medium
into chloroform in the presence of potassium ethylxanthate was studied [70].
Highly selective extraction method for gold(UI) from sulphuric acid-
potassium cyanide media into dichloroethane in presence of 1,1-
| | --------------- 1ir_rrr_,1,Ti-a*—■'Trtrimiiri wnmiiin-11r111*n fii -—--irr

diantipyrinyl butane has been discussed [71,72]. The same extractant in the
dichloromethane was applied for extraction of gold(IH) from cyanide
solution of leaching of raw materials [73]. Dicyclohexyl-18~crown-6 in
isobutyl methyl ketone was used as an extractant for gold(m) [74].. Mercury
interfered in the extraction procedure, the complexing conditions and the
selectivity of 3,5-dimethylpyrazole for gold(ni) have been studied in the
presence of large number of cations at pH 4.0 [75], The extraction procedure
can be completed in 30 min. The competitive exfraction of golden) and
other metals from aqueous solutions into chloroform was performed using
derivatives of p-t-butylcalix [4] arenes [76]. The introduction of amide
functional groups into the extractant improved the extraction of gold(IH).
Studies have been conducted on the equilibrium distribution of goid(m)
between hydrochloric acid media and chlorinated organic solvents with
nonionic surfactants, polyoxyethylene nonyl phenyl ethers (PONPES) [77].
The selective solvent extraction agent DBC extract gold(UI) to the extent of
99.99% [78]. The advantages of this process are reasonable separation
procedure, high selectivity of extraction, 5 min needed for loading,
continuous operation. A method for the separation of bromide complex
anions of gold(IH) with liquid-solid extraction system of
 199

polyvinylpyrrolidone-salt-water was investigated [79J. In the medium of

hydrobromic acid, gold(IIl) can be separated from Fe(III), Co(II), Ni(ll),
Al(IIl), Ca(II), Mg(II) and Cu(II) and method was used for analysis of real
samples. The extraction of goId(III) from aqueous chloride solutions into
non-desulphurized fraction of crude oil distillates, especially paraffin oil is
described [80]. 2,2’-dipyridyl-2-pyridylhydrazone (DPPH) was used as an
extractant for gold(III) from 0.2% SCN~ at pH 6.0 - 8.0 followed by
determination with atomic-absorption spectrometer [81]. The test solution
was made 0.5-3.0M in hydrochloric acid and the gold(in) was extracted into
a solution of triphenylguanidium chloride in dichloroethane [82]. NN-bis-(l-
methylneptyl) acetamide was used for the separation of gold(IH) from
Fe(III), Ni(H) and Cu(II) with kerosene as extraction solvent and £ 0.1M in
hydrochloric acid medium [83]. Adogen-464 in carbon tetrachloride extracts
gold(m) from 1.2M hydrochloric acid medium, with the method requiring
5 min for equilibration [84].

N-n-octylaniline has been used in this laboratory for quantitative

extraction of some platinum group metals [85-88]. The use of this reagent is
found to be advantageous as it can be synthesized at low cost, with high
yield and of best purity. The present investigation describes its use in
establishing the conditions for the quantitative extraction of gold(m) and the
development of a rapid and selective method for the separation of eoldfim
from associated elements. The method has been evaluated for the separation
and determination of gold(III) from alloys and pharmaceutical samples.
The various extraction methods for gold describing the nature of the
aqueous phase, organic phase, interference and special feature have been
summarized in Table 6.1.
 200

Table 6.1
Summary of methods for solvent extraction of gold(III)

System Aqueous Organic Interference Specific feature Ref.

phase phase No.
rn [21 [3] [4] m r«i
n-octyla- HC1,3M Toluene • Noble metals extracted 103- 2-6
niline 104 times better than base
HC1,3M DIBK Ni, Cu, Co, metals.
Fe coextract’ • Equilibration time 10-15
min.
HC1, 3M DIPK • Back extraction by 7M
HCIO4
• Troublesome emulsion
formation.. .
Tri-iso- HC1,2 M CCh Thiocyanate, • Iron co-extracts but could be 7
octylamine cyanide, sul­ masked with potassium
(TIOA) phide, thio­ dihydrogen phosphate.
sulphate, • Separation of gold from
EDTA, bro- palladium and platinum.
mide,Nitrite,
iodide, Ag
Trir-odyl- HC1 Kero­ • Selective transport and 8-10
amine (TOA) sene recovery of gold through a
supported liquid membrane
impregnated with tri-
octylamine on the basis of
differences in extraction
equilibria and kinetics.
HC1 CCI4 • The mechanism of extraction
belong to ion-association.
N-benzyl HC1,3M CHCfe - • 80% extraction of gold. 11
aniline • Stripping by thiourea.
i—
*
111

Primary
ii

• Synergistic attraction 12
amine N • Aggregation formed in gold-
1923 loaded organic phase when
concentration of gold
reaches 10 g L'1.
NN’- HC1, CHCI3 • Stripping with 1% thiourea 13
diphenylben- 0.5M in 0.5M H2SO4
zamidine • Extraction of gold from ores,
geological samples.
• Determination by
electrothermal AAS.
Zephiramine HC1.4M CHCI3 Cu(H) • Detection limit for gold 14
pH=ll interferes, 0.21 ng/ml
Pt • Method applied in the
coextracts analysis of silver alloys.
NN-di-s- HC1, 0.1- 1,2-di- • Back extraction by Na2S03 15
octylglycine 9.0M chloro- or thiourea
ethane,
ke­
rosene
 201

Table 6.1 contd...

rn [21 [3J KI rsi [61

NN-di-(l-me HC1, 0.1- 1,2-di- • Back extraction by Na2S03 16
thylheptyl) 9.0 M chloro- or thiourea
glycine ethane
kerosene
1,4-butylene HC1,1M, CHC13 • Large amount of Cu, Zn, Pb, 17
bis-(N-hexa- KI, 1M Co, Ni, Al, K, Na, Ca and
decyl-NN- Mg tolerated.
dimethyl • Method useful for
ammonium determination of > 0.2
bromide) ppm gold in rocks, ores,
flotation tailings.
Aliquat 336 di-iso- • Method not suitable for 18
butyl determining interstitial gold
ketone in silicates, but could be
applied for free gold.
• The large sample capacity
overcome problems of
sample inhomogeneity.
Hostarex HC1 n- - • Extraction reaction is 19
A 327 decane exothermic
1,2,3-benzo- pH=2.0 to n- • Extraction recovery 98% 20
triazole (1H- 7.0 butanol • Maximum extraction at
benzotri- pH=3.0.
azole)
2-hexyl- Xylene • Method applicable for deter 21
pyridine -mination of 0.01 to ig t'1 of
gold in ores and tailings.
N-tolyl-2- HC1 CHCI3 KI, thiourea 22
picolinethioa
mide
2-mercapto- butyl Sb, Pd 23,
benzothia- acetate interfere, 24
zole PH=2.0 Chloro­ bromate, Back extraction by ammonia.
form cyanide,
sulphide,
thiocya­
nate, thio­
sulphate,
thiourea,
Se, Ag,
Pd,Hg
interfere.
Dioctyl HBr, 8M benzene • Separation of gold from 25,
sulphoxide HC1- 3-meth­ palladium. 26
HNOs yl buta­ • Method useful for determin­
nol ing gold in geological
butyl samples down to 0.8 mg t"1
acetate
Dioctyl HC1, 3M Xylene • Method applied for 27
sulphide determining ppb concentra­
tion of gold in ores.
 202

Table 6.1 contd....

Ill 121 [31 14] - [5j |6|

Petroleum HC1, 1M Toluene • No interference from 1000 28,
sulphides fold excess of silver. 29
• Determination by atomic
emission method.
Petroleum HC1 Toluene • Determination by electro 30
sulphides thermal atomic absorption
alkylaniline sepectroscopy.
hydro­
chloride
Bis-(2,2,4- Sulpho- Pd, Hg • Method was simple rapid 31
trimethyl- nated coextract and the precision was ~ 3%
pentyl) Kero­
sulphide sene
Dibutyl HClor • Determination by AAS in 32
sulfide and hno3 acetylene-air flame
Dibulyl
selenide
7,10-dithia- 1,2- • Thioethers in combination 33
hexadecane, dichloro with a reducing agent as
2,5,9,12- ethane hydroxylammonium
benzotetrathi and sulphate efficiently extract
acyclopentad toluene gold(m).
ecane
(thioethers)
Thionalide K-H Ethyl or • Method could be used for 34
phthalate isobutyl £ 25 pg of gold.
(pH=5.0) methyl
ketone
ethyl thio- pH-1.0- Chloro­ Cyanide, 35
acetoacetate 3.6 form sulphide,
thiosulphate,
Ag, Hg, Cu
interfere
Benzothiazo- pH=2.0 Chloro­ Thiourea, • >10% Sb(V), Cr(VI), 36
le-2-thiol form Br0 3, S2-, W(VI), Mo(VI), Se(VI) co­
SCIST, S202-3 extract
interfere
NN’-di-O- HC1,1M Butyl • Determination by AAS (air- 37
tolyl-2- acetate acetylene flame)
thiourea
Nonyl- Acidic • Method was highly selective 38
benzyl- and in presence of Cu(II), Fe(III)
dodecyl- and veiy acidic solutions
thiourea containing Cl'.
Table 6.1 contd....

•m 121 [3] 14] 15] r«i

N-benzoyl- HC1, ‘ Toluene • Separation of gold from 39
N’N’-diphe- 0.01M platinum group metals
nyl-, N-ben- except palladium
zoyl-N’-phe
nyl-, N-ben-
zoyl-N’-hex-
yl- and N-be
nzoyl-N’N’-
dihexyl
thiourea
2a-c(N-thio- Chloride • Lack of interference from 40
carbamoyl- media appreciable amounts of
benzamidine Cu(U), Zn(II) and Fe(III).
derivatives),
3a-f(N-ben-
zoyl thiourea
derivatives)
Sulphide HC1, 1> • Combined use of a reducing 41
podand 1,12- 0.001-1M dichloro agent with TTD enhances
di-2-thienyI- ethane the extractioinof gold(ni) in
2,5,8,11-te- 1,2-dichloroethane.
trathiado-de-
cane (1TD)
Dibenzyl- pH=2-10 Chloro­ 42
ammonium form
dibenzyl- •
dithiocarba-
mate (DBA -
DBDC)
Bis (n-octyl HC1,0.1- Butyl • Spectrophotometric 43
sulfine) 6MKBr acetate determination with crystal
ethane violet.
(BOSE) • Rapid and highly selective
method for separation of
goldOII) from common and
noble metal ions.
• Method successfully applied
for determination of gold in
ores.
Oxygen • Separation of gold from 44
containing HNOs, most elements.
solvents- Di­ 5.5-10M • U(VI), Th(IV), Ce(IV) and
isopropyl HNOj, Cr(VI) were extracted but
ether Diethyl 4-10M are less effective than that of
ether goldOII)-_______________
 204

Table 6.1 contd....

Ill F21 13] [41 [5]

Isobutyl HC1,6M • Method successfully applied 45-
methyl to a converter matte. 51
ketone • Separation of microgram
(MIBK) HC1 amounts of gold from macro
amounts of iron.
• Detection limit 1 ppb.
HCI,2M • Method applicable for rocks
and concentrates.
HCI • Method applicable for
determination of gold in
vegetation.
• Thirty co-existing ions did
not interfere.
• Determination by flame
atomic-absorption
spectrophotometry.
pH=4 • Successful application for
determination of gold from
human urine.
• Detection limit 70 ng L"1
HCI, 3M • Analysis of geological
materials and determination
by a.a.s.
4-methyl- HCI, 0.5- Chloro­ • Method could be used to 52
1,3- 0.1M form separate gold(III) from a
dioxolan-2- solution containing other
one metals.
(propylene
carbonate)
3-methyl HCI, 1M Fe, Cu • Method applicable for 53
butanol interfere determining gold in dunites,
basalts, gabbros, diorites and
granites.
Ethyl methyl HCI, 1M • Double extraction 54
ketone- orHNOs,
chloroform 1M
Ethyl ether Acid, Sb coextract • ICP-AAS determinatioin. 55
10% • The method applicable in the
certification analysis of gold
standards.
Ethyl acetate HCI, 3M • Back extraction by 2-amino- 56
2-hydroxymethyl-1,3-
propanediol
• Gold tracer with carrier were
prepared with these
separations.
Alkyl Thio­ Aliphat­ • The addition of ammonia to 57
phosphorus sulphate ic hydro aqueous phase strongly
esters carbon influences extraction.
diluents
 205

Table 6.1 contd....

rn [2] [3] [41 [51 [6J

Trioclyl HC1, 1M M1BK • 98% extraction. 58
phosphine KI,0.25M • Determination by atomic
oxide Ascorbic absorption spectroscopy
acid,
0.1M
Trioctyl MIBK • Precision and accuracy were 59
phosphine good for samples of metal
containing 3.2-83.0 |xg g'1 of
gold.
Tris-(2-ethyl HC1, Toluene Thiocyanate, • Stripping with water. 60
hexyl) 4.0M thisulfate
phosphate interfere
Tribulyl 61
phosphate
(TBP)
Tetra-butyl- HC10.1- 1,2- • Selective recovery of gold 62
1,3-xylylene 5.0M dichloro
diphospho- ethane
nateand
tetra-butyl-
alkylene-di-
phosphonate
Bis(methyl HC1, 6M Ben­ • Analysis of anode mud for 63
heptyl) zene gold.
methyl-
phosphonate
Cyanex471x HC1,1- “ “ • Stripping by sodium 64
3M thiosulphate.
Cyanex921 HC1, - “ « Extraction system is 65
5-7M exothermic
Cyanex 923 “ Xylene • Stripping by NaCN or 66,
NaOH 67
Hdodecylo- HC1 Cumene 68
xy)-3-methyl , kero­
-1-oxo-A3- sene
phospholen, and
l-(2-ethyl- toluene
hexyloxy)-3-
methyl-1- -
oxo-A3-phos-
pholen and
l-(2,6-dime-
thyl-hept-4-
yloxy)-3-me­
thyl-1-oxo-
A3-phospho-
lene
Alkylaniline HC1, Toluene • No interference with 50 fold 69
(alkyl=C8 to 2-3M excess of any of the other
Cio) metal.
 206

Table 6.1 contd....

m 121 PI W I5J 16]

Potassium II2SO4, Chloro­ • Degree of extraction was 70
ethyl 0.1-8M form determined by spectrophoto-
xanthatc metric & a.a.s. methods.
u- H2SO4- Dichl- Cu, Ni, Pb, • Highly selective extraction- 71-
diantipyrinyl KCN oro- Ag inter­ a.a.s. method. 73
butane ethane fered • Method applicable to
*
determination of gold in
cyanide solution from
leaching of raw materials.
Dicyclohex- MIBK Hg • Method useful to determine 74
yI-18-crown- interfered gold in sand, urine, sea­
6 water.
3,5-dimethyl pH=4.0 • Selective extraction and 75
pyrazole concentration of gold(IH)
from solution of salts of
copper, iron and other
elements.
Calix[4] Chloro­ • Presence of large excess of 76
arenes (p- form sodium ions decreases
ter-butyl- exactibility of gold.
calix [4]
arenes)
Polyoxy HC1 Chlori­ • Successfully applied to gold 77
ethylene nated leach liquor from a printed
nonylphenyl organic substrate
ether’s solvent
(PONPE’s)
DBC • Reasonable separation 78
procedure, high selectivity
of extraction
Polyvinylpyr HBr • Method applied in separation 79
rolidone- of gold from real samples.
salt-water
Paraffin oil Chloride • Method applied for gold in 80
auriferous rocks and ores
containing 0.018 g per ton.
2,2’-dipy- SCN-, • Determination by air- 81
ridyl-2-pyri- 0.2 % acetylene flame
dylhydrazo- pH=6.0 — ■
ne(DPPH) 8.0
Triphenylgu HC1,0.5- Dichl- 82
anidhim 3.0 M oro
chloride ethane
NN-bis-(l- HC1, Kero­ • Back extraction by excess of 83
methyl- 0.1M sene oxalic acid solution in
heptyl)aceta presence of tin(IV) at pH
mide 6.0.
Adogen-464 HC1, Carbon 84
1.2 M tetra •
chloride
 207

6.3 Experimental

6.3.1 Apparatus

An Elico digital spectrophotometer, Model SL-171, with 1 cm quartz

cells was used for absorbance measurements, pH measurements were carried
out using an Elico digital pH meter model LI-120.

6.3.2 Reagents

A stock solution of gold(in) was prepared by dissolving lg HAuC14

(Johnson Matthey, UK) in 250 mL of double distilled water and was
standardized gravimetrieally [89]. A working solution was made therefrom
by appropriate dilution.

N-n-octylaniline was prepared by the method of Gardlund [90] and

its solution (0.1M) was prepared in xylene.

A 10% solution of stannous chloride dihydrate in 1M hydrochloric

acid was used. A fresh solution should be prepared weekly.

All chemicals used were of A.R. grade. Double distilled water was
used throughout.

6.3.3 Extraction procedure for gold(III)

A aliquot of 2 mL of gold(III) solution (100 pg/mL) was mixed with

a sufficient quantity of sodium malonate (0.11 lg) to make its concentration
0.03M in a total volume of 25 mL of the solution. Then the pH of the
solution was adjusted to 1.0 using dilute hydrochloric acid and sodium
hydroxide. The solution was transferred into a 125 mL separation funnel and
shaken with 10 mL of 0.1M (2.303%) N-n-octylaniline in xylene for 1 min.
After equilibration, the mixture was allowed to separate and the metal was
stripped from the organic phase with two 10 mL portions of ammonia
solution (7M). The extracts were evaporated to moist dryness. The residue
was dissolved in 5 mL aqua regia, evaporated, then 2 mL of 2% sodium
chloride solution [89] and concentrated hydrochloric acid were added and
 208

the mother liquor again evaporated. The procedure of evaporation was

repeated to remove oxides of nitrogen, taking care not to evaporate to
dryness and so avoid loss of gold [91]. The residue was dissolved in 0.05M
hydrochloric acid and the gold(III) determined spectrophotometrically by
stannous chloride method [92] at 400 nm.

6.4 Results and discussion

6.4.1 Extraction as a function ofpH

The extraction of gold(m) was carried out from 0.03 M sodium

malonate at pH varying from 0.1-10.0 (Table 6.2). The extraction
commenced at pH 0.1 (42%) and was quantitative between pH 0.5-2.0. This
shows that the equilibrium in the pH range 0.5-2.0 is favourable for the
formation of an ion pair complex (Fig.6.1). If a higher pH is used for the
extraction there is the possibility of hydrolysis. This indirectly promotes
competing equilibria with the formation ofan ion pair complex, resulting in
a decrease in extraction effectiveness. Therefore pH 1.0 was used throughout
this work.

6.4.2 Extraction as afunction oforganic acid concentration

The extraction of gold(m) was carried out at pH 1.0 with 0.1M N-n-
octylaniline in xylene in the presence of varying concentrations of sodium
malonate and sodium succinate as weak acid media (Table 6.3). The
extraction commenced with 0.005 M sodium malonate and became
quantitative in the concentration range 0.02M - 0.04M sodium malonate.
■-■-■niiii --- r —inn i I,,

With an increased concentration of sodium malonate there is a decrease in

the efficiency of extraction of gold(HI) (Fig.6.2). The decrease in extraction
at high acid concentration is presumably due to preferential formation of the
malonate of the N-n-octylaniline . A 0.03M concentration of sodium
malonate was therefore used throughout this work. Extraction was found to
be incomplete in sodium succinate media.
 209-

6.4.3 Extraction as a function ofN-n-octylaniline concentration

The go!d(III) was extracted at pH 1.0 with vaiying concentrations of

N-n-octylaniline at constant (0.03M) sodium malonate concentration. The
concentration was varied from 0.005 to 0.15M of extractant in xylene (Table
6.4). The extraction was 49% with 0.005M of extractant but was quantitative
in the range of 0.08M-0.15M of N-n-octylaniline . With increased
concentration of extractant there was a decrease in the proportion of
gold(ffl) extracted and this might be due to the dissociation of the complex
(Fig.6.3). We used 0.1M of the extractant for routine work.

6.4.4 Choice ofdiluents

Keeping all of the other variables constant, the gold(IH) was extracted
with 0.1M N-n-octylaniline with various diluents. The extraction was
quantitative with xylene, amyl acetate, amyl alcohol and n-butyl alcohol as
the diluents. It was incomplete with benzene (34%), toluene (28%),
chloroform (36%), carbon tetrachloride (30%) and methyl isobutyl ketone
(MDBK) (36%) as given in Table 6.5. An inert diluent such as xylene does
not participate in the actual extraction process as do the oxygenated solvents.
N-n-octylaniline causes ion-pair formation of a gold-malonate complex and
thus promotes extraction. However, a definite correlation between diluent
and its dielectric constant could not be established.

6.4.5 Nature ofthe extracted species

The probable composition of extracted species is ascertained by

plotting graphs of log D[Au(ni)] against log C [N-o-octyimto \ at fixed sodium
malonate concentration (0.03M) (Fig.6.4). The plots were linear, having the
slopes of 1.24 and 1.04 respectively (at pH 0.75, 1.0). Also, plots of log
D[Au(m)] against log C[Maionate] at fixed N-n-octylaniline concentration
(0.1M), were linear and with slopes of 2.05 and 1.87 respectively (Fig. 6.5).
The probable composition of the extracted species is calculated to be 1:2:1
 210

(metal:acid:extractant). The possible mechanism for the extracted species

appears to be protonated N-n-octylaniline which forms cationic species as
RR’NH2+ while malonate combines with gold(IQ) to form anionic species as
Au (C3H2C>4)‘2 and both of them associate to form an ion pair of the type
[RR’NH+2 .Au(C3H204)'2]org and since these are neutral they are extractable
species.

6.4.6 Effect ofshaking period

Variation of the shaking period showed that a 15 s equilibration time

was adequate for quantitative extraction of gold(m) from malonate media.
But in this work, 1 min equilibration time was recommended in order to
ensure the complete extraction of gold(III). However, a prolonged
equilibration period (>5 min) was found to have an adverse effect on the
extraction and should be avoided (Table 6.6).

6.4.7 Loading capacity ofN-n-octylaniline

The concentration of gold(IH) was varied to determine the loading

capacity of N-n-octylaniline (Table 6.7). The loading capacity was found to
be 5 mg of gold(m) with 10 mL of 0.1M N-n-octylaniline in xylene at
0.03M sodium malonate concentration.

6.4.8 Effect ofaqueous to organic phase volume ratio

The results of contacting different volume ratios of aqueous to

organic phases have been studied. It was found that the extraction of
gold(III) was quantitative when the aqueous to organic phase volume ratio
was in the range 1:1 to 5:1, while it decreased when the ratio changed from
5:1 to 20:1 (Table 6.8). Hence, the aqueous to organic volume ratio
recommended in the procedure is 2.5:1.

6.4.9 Effect ofstripping agents

Gold(III) was stripped from the organic phase with various stripping
agents such as acids, bases, salts and buffer solutions. It was then found that
 211

with > 3M ammonia the stripping was quantitative because beyond this
molarity the optimum conditions of extraction were reversed (Table 6.9).
Hence 7M ammonia was used as the stripping agent. Whereas gold(lII) did
not recovered with other strippants.

6.4.10 Effect offoreign ions

Gold(m) was extracted in the presence of other ions and substances

(Table 6.10). The tolerance limit was set as the amount of foreign ion
required to cause less than ±2% error in the recovery of gold. The only
species showing interference in the procedure were thiourea, ascorbate and
thiosulphate. Of the cations examined, only Pd(H), Rh(III) and Pt(IV)
interfered. The interference of Pd(H) and Rh(M) was eliminated by masking
with tartaric acid and that of Pt(IV) with oxalic acid.

6.5 Applications

6.5.1 Separation ofgold(III) from associated metals

Gold(m) was separated from commonly associated metal ions by

taking advantage of the difference in the extraction conditions between
metals.

Gold(III) was separated from Ir(III), Os(Vm), Ru(m), Se(IV), J

Te(IV) and base metals such as Fe(JII), Co(II), Ni(II), Cu(II) by its
extraction with 0.1M N-n-octylaniline in xylene at pH 1.0 from 0.03M
sodium malonate media. Under these conditions all added metal ions remain
quantitatively in the aqueous phase in which they are determined
spectrophotometrically by standard methods (Table 6.11). Gold(III) from the
organic phase was stripped with (2x10 mL) 7M ammonia and estimated
spectrophotometrically by applying with stannous chloride method.

Gold(III) is separated from Pd(II) and Rh(III) by masking with each

of 20 mg of sodium potassium tartarate and that of Pt(IV) with 20 mg of
 212

oxalic acid respectively. The masked metal ion from the aqueous phase is
subsequently demasked and estimated by following a standard procedure.

The determination of small amounts of gold in mineral containing

large amounts of base metals is difficult, hence it was decided in the present
work to evaluate the effectiveness of N-n-octylaniline as an extractant for
the gold from the variety of the minerals and processed solutions. It was
found that gold(m) was separated from comparatively large amounts of
iron(HI), cobalt(II), nickel(II) and copper(n) by its extraction with 0.1 M
N-n-octylaniline in xylene at pH 1.0 from 0.03M malonate media. Under \i
these conditions, all the base metals remain quantitatively in the aqueous
phase, where they were determined using spectrophotometric methods.

6.5.2 Determination ofgold(III) in a synthetic mixture

A solution containing 200 jig of gold(!Il) was taken and known

amounts of other metals were added. Extraction of gold(IH) was carried out
using the method developed here. The results obtained were in good
agreement with the amounts added (Table 6.12).

6.5.3 Determination ofgold(III) in real alloys

Dissolution ofcopper-silver-gold alloy

About Ig of sample was transferred into a 250 mL conical flask

i

covered with a short-stem funnel and dissolved in 10 mL aqua regia. The i

solution was then treated with 10 mL of concentrated hydrochloric acid,
added in 2 mL portions, the solution was evaporated almost to dryness on a
steam bath after each addition. The residue was dissolved in dilute
hydrochloric acid and the precipitated silver chloride filtered off and washed
with dilute hydrochloric acid. The filtrate and washings were collected in a
250 mL standard flask and made upto volume with distilled water.
 213

An aliquot of the sample solution was taken and gold(III) was

determined using the procedure described above. The results of analysis are
given in Table 6.13.

6.5.4 Determination ofgold(IIl) from Ayurvedic sample

The sample (one tablet) was dissolved in 10 mL aqua regia. The

solution was slowly evaporated to moist dryness, the residue dissolved in
dilute hydrochloric acid, and the solution filtered if necessary. The filtrate
was diluted to 25 mL with distilled water. An appropriate aliquot of the
solution was used for analysis. The amount of gold(lH) found in the tablets
is in agreement with the certified value given (Table 6.14). The accuracy of
the results was confirmed using atomic absorption spectroscopy (AAS).
 214

Table 6.2

Extraction behaviour of gold(III) as a function of pH

Gold(HI) = 200 jig Sodium malonate = 0.03 M

N-n-octylaniline = 0.1 M in xylene Strippant = 7M NH3 (2 x 10 mL)
Aq: Org = 2.5 :1

pH Percentage Distribution
extraction, % E ratio, D
0.10 42.0 1.81
0.25 80.0 10.00
0.50 100 OO

0.75, 100 oo

1.00 100 OO,

1.25 100 oo

1.50 100 OO

1.75 100 OO

2.00 . 100 OO

2.50 85.0 14.16

3.00 60.0 3.75
4.00 42.0 1.81
5,00 27.0 0.92
6.00 16.0 0.48
7.00 0.00 0.00
 215

Table 6.3

Extraction behaviour of gold (III) as a function of organic acid

concentration

Gold(III) = 200 pg pH = 1.0

N-n-octylaniline = 0.1 M ift xylene Strippant = 7M NH3 (2x10 mL)
Aq: Org = 2.5 : 1

Concentration Sodium malonate Sodium succinate

of acid, M Percentage Distribution Percentage Distribution
extraction, ratio, D extraction, ratio, D
%E %E
0.00 0.00 0.00 0.60 0.00
0.005 42.0 1.81 10.8 0.30
0.010 76.0 7.92 14.8 0.44
0.015 90.0 22.50 16.0 0.48
0.020 100 OO 18.0 0.55
0.025 100 OO 19.5 0.60
0.030 100 oo 22.8 0.74
0.035 100 oo 23.0 0.75
0.040 100 oo 24.8 0.83
0.050 92.0 28.75 22.4 0.72
0.060 77.5 8.61 20.0 0.63
0.070 68.0 5.31 16.8 0.50
0.80 60.0 3.75 15.6 0.46
0.90 51.0 2.60 12.0 0.34
0.100 45.0 2.05 0.00 0.00
0.150 0.00 0.00 0.00 0.00
 216

Table 6.4

Extraction behaviour of gold(III) as a function of N-n-octylaniline

concentration

Gold(III) = 200 jig Sodium malonate = 0.03 M

pH = 1.0 Strippant = 7M NH3 (2x10 mL)
Aq : Org = 2.5 :1

N-n-octylaniline Percentage Distribution

concentration, M extraction, % E ratio, D
0.00 0.00 0.00:,.
0.005 49.0 2.40.,
0.010 59.0 3.60 :
0,020; 70.5 5.97 ,
0.030 80.0 10.00
0.040 85.5 14.74
0.050 88.2 18.69
0.060 90.5 23.82
0.070 92.0 28.75
0.080 100 OO

0.090 100 00
0.10 100 OO

0.12 100 OO

0.14 100 OO

0.15 100 OO

0.16 86.0 15.36

0.18 57.0 3.31
0.20 31.0 1.12
0.22 16.0 0.48
0.24 10.5 0.29
0.25 0.00 0.00
 217

Table 6.5

Extraction of gold(III) with various diluents

Gold(HI) = 200 pg pH = 1.0

Sodium malonate = 0.03 M Strippant = 7MNH3 (2 x 10 mL)
N-n-octylaniline =0.1 M Aq: org = 2.5 :1

Diluent Dielectric Percentage Distribution

constant, e extraction, % E ratio, D
Benzene 2.27 34.0 1.29
Toluene i 2.38 28.0 0.97
Xylene 2.30 100 oo

Chloroform 4.80 36.0 1.41

Carbon tetrachloride 2.24 30.0 1.07
Amyl alcohol 13.9 100 oo

n-butyl alcohol 17.8 100 oo

Amyl acetate 4.8 100 00

Methyl isobutyl ketone 13.10 36.0 1.41

4T
 218

Table 6.6

Effect of shaking period on extraction

Gold(III) = 200 pg pH = 1.0

Sodium malonate = 0.03 M Strippant = 7M NH3 (2 x 10 mL)
N-n-octylaniline = 0.1 M in xylene Aq: org = 2.5 :1

Time Percentage Distribution

extraction, % E ratio, D
10 sec 48.0 2.31
15 sec 100 00

30 sec 100 00

1.0 min 100 00

2.0 min 100 00

3.0 min 100 00

4.0 min 100 00

5.0 min 100 00

6.0 min 88.0 18.33

7.0 min 82.0 11.39
8.0 min 70.0 5.83
9.0 min 60.0 3.75
10.0 min 47.0 2.22
15.0 min 22.8 0.65
20.0 min 0.00 0.00
 219

Table 6.7

Loading capacity of N-n-octylaniline

Sodium malonate = 0.03 M pH = 1.0

Strippant = 7M NH3 (2 x 10 mL) Aq : org = 2.5 :1
N-n-octylaniline = 0.1 M in xylene

Concentration of Percentage Distribution

Au(ffl), pg extraction, % E ratio, D
50 100 OO

100 100 00

200 100 OO

400! • 100 OO

800 100 OO

1200 100 oO

1600 100 OO

2000 100 OO

3000 100 OO

4000 100 OO

5000 100 OO

6000 84.0 13.13

7000 78.8 9.30
10,000 46.0 2.13
 220

Table 6.8

Effect of aqueous to organic phase volume ratio

Gold(ffl) = 200 pg pH = 1.0

Sodium malonate = 0.03 M Strippant = 7M NH3 (2 x 10 mL)
N-n-oclylaniline = 0.1 M in xylene

Aqueous: Organic Percentage Distribution

volume extraction, % E ratio, D
10:10 100 OO

20:10 100 OO

25:10 100 OO

30:10 100 OO

35:10 100 OO

40:10 100 oo

50:10 100 oo

75 :10 90 . 22.5

100:10 86.0 15.36

200:10 51.2 2.62

Table 6.9

Effect of strippant concentration

Gold(ffl) = 200 pg pH = 1.0

Sodium malonate = 0.03 M Strippant = NH3 (2x10 mL)
N-n-octylaniline = 0.1 M in xylene Aq : org = 2.5 :1

Concentration of Ammonia, Percentage

M Recovery
0.05 2.5
0.1 13.0
0.5 27.0
1.0 50.8
2.0 74.0
3.0 100
4.0 100
5.0 100
6.0 100
7.0 100
8.0 100
9.0 100
10.0 100
 Table 6.10
Effect of foreign ions on the extraction of200 jig gold(III) at
pH 1.0 in 0.03m sodium malonate with 0.1m N-n-octylaniline
dissolved in xylene

Ratio of ions Amount Foreign ion

(Gold: ions) tolerated (mg)

1:125 25 U(VI), citrate, iodide, bromide, fluoride

1:100 20 . Ni(H), Ca(II), Ba(II), tartrate, oxalate

1:75 15 Mn(II), Mg(H), Cu(E)j Be(fl), Al(ffl),

EDTA

1:50 10 Fe(III), Cd(II), Pb(II), V(V), Ti(IV),

In(III), acetate

1 :25 5 Fe(H), Bi(ffl), Mo(VI), Ce(IV), Te(IV),

Sr(II), Sb(III), Cr(VI), thiocyanate

1:10 2 Hg(II), T1(I)

1:5 1 Ir(IV), Rh(m)a, Os(Vm), Se(TV)

1:2.5 0.5 Pd(n)a,Pt(IV)b

T 0 Thiourea, ascorbate, thiosulphate

a = masked with tartrate

b = masked with oxalate
Tabe 6.11
Separation of gold(HI) from multicomponent mixtures

Metal ion Amount Average Chromogenic Reference

taken, (ig % Recovery* ligand number
Au(lII) 200 99.9
Pda(II) 100 99.8 4’-chloro PTPT 93
Au(ni) 200 99.9
Ptb(IV) 300 99.8 SnCl2 92
Au(in) • ;2oo 99.9
Ir(IV) 100 99.8 SnCl2 + HBr 92
Au(III) 200 99.8
Os(Vm) 300 99.8 Thiourea 92
Au(IH) 200 98.9
Rha(III) 300 99.7 SnCl2 + KI 92
Au(HI) 200 99.7
Ru(ffl) 300 99.7 Thiourea 92
Au(ffl) 200 99.8
Se(IV) 300 99.8 4’-bromoPTPT 94
Au(ffl) 200 99.9
Te(IV) 100 99.7 4’-bromo PTPT 95
Au(III) 200 99.9
Fe(III) 10,000 99.8 Thiocyanate 92
Au(III) 200 99.8
Cu(II) 15,000 99.9 4’-chloro PTPT 96
Au(III) 200 99.9
Co(II) 15,000 99.8 Thiocyanate 97
Au(ffl) 200 99.7
Ni(II) 20,000 99.9 DMG 97

* = average of six determinations

a = masked with tartrate
b = masked with oxalate
 224

Table 6.12
Separation of gold(III) from synthetic mixtures

Composition, pg Gold(III) Mean Recoveiy RSD

found, pg % %
Au, 200; Pda, 200; 199.9
Pt*, 200 199.8
199.9 199.88 99.94 0.06
199.9
199.9
Au, 200; Pda, 200; 199.8
Co, 1000; Ni, 1000 199.8
199.7 199.78 99.89 0.11
199.8
199.8
Au, 200; Pda, 200; 199.9
Ptb, 200; Ag, 200 199.9
199.8 199.86 99.93 0.07
199.8
199.9
Au, 200; Se, 300; 199.8
Te, 100 199.9
199.9 199.88 99.94 0.06
199.9
199.9
Au, 200; Fe, 1000; 199.9
Cu, 1000 199.9
199.8 199.86 99.93 0.07
199.9
199.8

a = masked with tartrate

b = masked with oxalate
Table 6.13
Analysis of alloys

Composition of Gold(m) Gold(ffl) Recovery RSD

Alloy found by found by % %
AAS % proposed
method* %
Cu, 49.35; Ag, 7.25; 43:3 43.2 99.8 0.23
Au, 43.4
Cu, 35; Ag, 5; 59.9 59.7 99.7 0.33
Au, 60

* Average of five determination

 226

Table 6.14
Analysis of gold(DI) in Ayurvedic samples

Amount Amount found

Name of Medicine found by by proposed . RSD %
AAS, method*
pg/mL pg/mL
Vita-Ex-Gold 80 79.8 0.25
(Shree Baidyanath, Nagpur)
Suvama Sootashekhar 40 39.8 0.50
(Ayurveda Rasashala, Pune)
Makardhwaja Vati 36 35.9 0.28
(Ayurveda Rasashala, Pune)

* Average of five determinations

Fig. 6.1. Extraction behaviour of gold (Hi) as a function of pH
from 0.03 M sodium malonate solution with 0.1 M
N-n-octylaniline in xylene
0.9- /

0.8- /
0.7-

-1.8 -1.7 -1.6 -1.5 -1.4 -1.3 -1.2 -1.1 -1

Log Cpj-n-octylaniline]

Fig. 6.4. Log-log plot of Log D [mm against Log C [N-n-octyiamiine]

at fixed sodium malonate concentration (0.03 M)
Log D[Au(lll)]

Fig. 6.5. Log-log plot of Log D [AU(tii)] against log C [mai0natei at fixed
N-n-octylaniline concentration (0.1 M)
 227

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