Talanta 62 (2004) 489495

Spectrofluorimetric determination of iridium(IV) traces

using 4-pyridone derivatives
Vinka Drukovic a , Vlasta Vojkovic a, , Slobodan Miko b
a

Laboratory of Analytical Chemistry, Faculty of Science, University of Zagreb, Strossmayerov trg 14, 10000 Zagreb, Croatia
b Institute of Geology, Sachsova 2, 10000 Zagreb, Croatia
Received 12 March 2002; received in revised form 7 August 2003; accepted 20 August 2003

Abstract
A new spectrofluorimetric determination of iridium(IV) with 3-hydroxy-2-methyl-1-phenyl-4-pyridone (HX) or 3-hydroxy-2-methyl-1-(4tolyl)-4-pyridone (HY) is reported. Iridium(IV) react with HX or HY and chelates were extracted into chloroform or dichloromethane. The
organic phase showed fluorescence. The fluorescence measurements to quantify iridium were carried out in its fluorescent band centred at
ex = 373 nm and em = 480 nm. Under optimal conditions, the calibration graphs were linear over the concentration range of 0.17.6 g ml1
of iridium for Ir(IV)HX and 0.15.8 g ml1 for Ir(IV)HY with a correlation coefficients of 0.999 and 0.992 and relative standard deviation
of 1.1%.
The method is free from interference by Rh(III) and Pt(IV), which normally interfere with other methods. Iridium can be determined in the
presence of 300-fold excess of rhodium(III) and 10-fold excess of platinum(IV).
The method was applied successfully to the determination of iridium in some synthetic mixtures and mineral sample gave satisfactory results.
2003 Elsevier B.V. All rights reserved.
Keywords: Chromite; Extraction; Fluorimetry; Iridium(IV); 4-Pyridone; Rhodium

1. Introduction
Iridium occurs as osmiridium alloy and one of the minor constituents in most platinum metal deposits. It is commonly used in various jewellery, dental alloys, electrical
equipments, corrosion-resistant chemical wares, crucibles
for high temperature reactions and extrusion dyes for high
melting glasses. Therefore, highly selective, sensitive, rapid
and economical methods are needed for its trace and ultra
trace determination. The most widely used methods for the
determination of iridium are spectrophotometric methods
[110]. The technique is tedious time consuming because
the reactions were only at high temperature developed [14].
These methods have shown some drawback as regards selectivity when iridium(IV) is in the presence of rhodium(III)
[13,58]. So, in most of these system, the preliminary separation of platinum metals were necessary before applying
these methods.

Corresponding author. Fax: +385-1-48-18-458.

E-mail address: vlastavojkovic@yahoo.com (V. Vojkovic).

0039-9140/$ see front matter 2003 Elsevier B.V. All rights reserved.
doi:10.1016/j.talanta.2003.08.031

Recently, it has been shown that spectrofluorimetric

method is more versatile than spectrophotometric for solving analytical problems. The spectrofluorimetric methods
are preferable to the other methods as graphite furnace or
inductively coupled plasma atomic emission spectroscopy,
because they are much easier to apply and have a lower
cost. It leads, not only to an increase in selectivity, but also
in many cases to an increase in sensitivity [11]. Moreover,
literature data have been scarce for a luminescent method
for the determination of iridium. Fink and Ohnesorge have
described a spectrofluorimetric determination of iridium(III)
with 2,2 ,2 -terpyridine, but the procedure involves reaction
on a high temperature and suffered from interferences by
rhodium(III) and ruthenium(III) [12].
Liquidliquid extraction of the same metal ions with 3hydroxy-2-methyl-1-phenyl-4-pyridone (HX) or 3-hydroxy2-methyl-1-(4-tolyl)-4-pyridone (HY) as complexing agents
has been performed by spectrophotometry [1320]. Spectrofluorimetric methods for the determination of these ions
on the basic metalHX(HY) complexes were not described,
anyway. A previous paper presented an experimental study
of the liquidliquid extraction and spectrophotometric de-

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V. Drukovic et al. / Talanta 62 (2004) 489495

termination of iridium(IV) with HX or HY [21]. On the fact

that the extracted organic layer exhibited fluorescence properties, a detailed study of the iridium(IV)HX(HY) system
has been carried out and a method was proposed for the
spectrofluorimetric determination of traces of iridium.
Described fluorimetric assay is simple and sensitive
enough to be useful for determining iridium in synthetic
and mineral sample.

2. Experimental
2.1. Materials and reagents
The stock solution of iridium(IV) chloride (5 103 M)
was prepared by dissolving 0.02195 g of (NH4 )2 IrCl6
(Aldrich, Milwaukee, USA) in 10 ml 0.2 M solution of
hydrochloric or sulphuric acid. The resulting solutions
was standardised gravimetrically [22]. A working solution
was prepared daily by diluting the standard solution with
deionised-distilled water.
HX and HY were synthesised as described previously
[23]. Solutions of the HX or HY were prepared by dissolving weighted amounts of HX(HY) in redistilled chloroform
(Fluka, Buchs, Switzerland) or dichloromethane (Merck,
Darmstadt, Germany).
Other standard solutions of different cations used to
study the effect of various ions were prepared by dissolving
suitable quantities of their salts (Merck, Fluka) in deionised
water or in dilute hydrochloric acid. Solutions of anions
were prepared by dissolving the respective alkali metal salts
in water.
Cation exchanger resin Dowex 50 W X8, 200400 meshes
(Fluka) in the hydrogen form was used. All the chemicals
used were of AR grade.
2.2. Apparatus
Fluorescence intensity was measured with a Perkinspectrofluorometer, Model Perkin-Elmer LS50, furnished
with a xenon lamp, and connected to a HP ColorPro Graphics
Plotter. Fused quartz cells, 10 mm 10 mm 45 mm, were
used throughout the study. The instrument was calibrated
by using a standard fluorescence band equivalent to yield
of a 1 ppm solution of quinine sulphate in 0.05 M H2 SO4 .
The fluorescence meter at ex = 373 nm, em = 480 nm,
and excitation and emission slit width of 2.5 and 6.0 nm.
FT-Raman spectra of crystalline solids in capillary tubes
were recorded at room temperature using a Bruker Equinox
55 with FT-Raman Module-106/S, equipped with a Raman
accessory (1064 nm excitation) at 1 cm1 resolution. Magnetic measurements were carried out at room temperature
using Gouy method.
A Griffin flask shaker with a time switch served for extraction. The pH of the aqueous phase was measured with a
Radiometer PHM 85 precision pH-meter.

2.3. Extraction procedures

To an aliquot of solution containing 3.8 g ml1 iridium(IV), sulphuric, hydrochloric or perchloric acid was
added in the amount to have the selected acidity, pH = 3,
at constant ionic strength = 0.2 M for sulphuric acid
solutions and = 1 M for hydrochloric or perchloric acid
solution, and the volume was made up to 5 ml. The solution
was equilibrated with 5 ml HX(HY) dissolved in chloroform
or dichloromethane, and both phases were shaken with a
mechanical shaker in a 50 ml conical flask for 25 min. After
the phases were separated by gravity the relative intensity of
fluorescence of the organic phase was measured at 480 nm
(ex = 373 nm).
2.4. Isolation of iridium(IV) extracted species
The iridium complex was obtained by shaking a chloroform solution of HX (4 104 M) with an equal volume of
water phase containing ammoniumhexachloro iridate (4
104 M), sulphuric acid (1 103 M) and 0.2 M Na2 SO4 ,
or 4 104 M (NH4 )2 IrCl6 , hydrochloric acid (5 103 M)
and 1 M NaCl. The organic phase was separated and the solvent evaporated in vacuum. The remaining solid products
were recrystallised from chloroformligroin (1:2) and magnetic measurements were carried out.
2.5. Analysis of synthetic mixtures
Different amounts of metal salts including those of iridium
were mixed in such a way that the metal content of resultant
mixtures corresponded to that of standard reference samples
such as alloys. The mixture (0.040.1 g) was dissolved in
aqua regia with heating and evaporated nearly to dryness
[24]. Concentrated hydrochloric acid (2 ml) was added and
the solution was warmed. After cooling to room temperature
it was diluted and then filtered and the filtrate was diluted to
100 ml in a calibrated flask. An aliquot of the sample solution
was adjusted to pH 3 and treated similarly as described in
Section 2.3.
2.6. Analysis of real sample
A weighed portion of sample of chromite (Alb-121) was
placed in a heat-resistant (Pyrex) vessel, and conc. HClO4
was added in small portions. The vessel was covered by
a watch glass and the mixture was heated to fuming on a
hot plate. Heating was continued for as long as the precipitate at the bottom of vessel did not become dark red. After
evaporation of excess HClO4 , the residue was treated with
37% (v/v) HCl. In this case, most of the chromium was
removed in the form of volatile chromyl chloride. The insoluble residue was separated and the analysis carried out
(Scheme 1) [25].
A solution obtained with treatment of salts with 0.1 M
HCl, was passed through a column (length 10 cm, diame-

V. Drukovic et al. / Talanta 62 (2004) 489495

500

SAMPLE about 1 g

Relative intensity of fluorescence

Treatment with HNO3 + HClO4

(with addition of HCl or NaCl)
Evaporation to dryness
Treatment with HCl
Filtration

FILTRATE

491

INSOLUBLE RESIDUE

400

Excitation

Emission

c(Ir) x 10 / M
1) 0.0
2) 0.6
3) 1.0
4) 2.0
5) 3.0
6) 5.0
7) 7.0

200

3
2

100

300

0
300

350

400

450

500

550

600

Incineration

Wavelenght / nm
Evaporation to
moist salts

Fusing with 4:1 mixture

of Na2O2 + Na2CO3
Leaching fusion cake
with H2O + HCl

Evaporation to
moist salts
Treatment of salts with
concentrated HCl
Evaporation of moist salts
Treatment of salts with 0.1 M HCl
Ionic exchange (0.1 M HCl)
Extraction of Ir with HX
(procedure 2.3), method of standard addition

Fig. 1. Excitation and emission spectra of Ir(IV)HX complex in

chloroform layer. c(HX) = 4 104 M, c(HCl) = 1.0 M 102
c((H,Na)Cl) = 1.0 M.

3.1.1. The optimum conditions

The influence of the medium acidity on the formation
Ir(IV)HX(HY) complex and its extraction into chloroform
was studied using sulphuric, perchloric, or hydrochloric
acid (Fig. 2). The optimum pH range for a constant emission signal in the organic layer was at pH 2.5 (pH adjusted with H2 SO4 , at constant ionic strength = 0.2 M)
and pH 2.0 (pH adjusted with HCl or HClO4 , at constant ionic strength = 1 M), regardless of the reagents
using in the organic phase. Accordingly, 1 103 M
H2 SO4 , at c((H,Na)2 SO4 ) = 0.2 M, or 1 102 M
HClO4 , at c((H,Na)ClO4 ) = 1 M, or 1 102 M HCl, at
c((H,Na)Cl) = 1 M, were used in further work.
The signal emitted in the organic phase was found to be
maximal and it remained virtually constant between 0 and

Fluorimetric measurement
240

ter 19 mm) of 30 ml (10 g) of cation exchanger in hydrogen

form. Iridium was not adsorbed on the resin [26]. The solution which passed through a column was diluted to 25 ml
and used for extraction and fluorimetric determination of Ir
with HX, as described in Section 2.3.

3. Results and discussion

3.1. Fluorescence spectra
The fluorescence spectra of Ir(IV)HX and Ir(IV)HY
complex in chloroform or dichloromethane layer exhibited
the excitation maximum at 373 nm, and emission maximum
at 480 nm, whereas the blank probe did not show a fluorescence (Fig. 1).

Relative intensity of fluorescence

Scheme 1. Determination of iridium in chromite.

200
160
120
80
Ir(IV)-HX
Ir(IV)- HY

40
0
-4.0

-3.5

-3.0

-2.5

-2.0

-1.5

-1.0

-0.5

0.0

0.5

log(acid)initial
Fig. 2. Effect of medium acidity in the aqueous phase on the
fluorescence intensity of iridium(IV)HX(HY) complexes in chloroform layer: c(Ir(IV)) = 2.2 105 M, c(HX) = 4 104 M, or
c(HY) = 1.3 103 M. (, ) c((H,Na)2 SO4 ) = 0.2 M, H2 SO4 is
varied; (, ) c((H,Na)ClO4 ) = 1.0 M, HClO4 is varied; (, )
c((H,Na)Cl) = 1.0 M, HCl is varied.

492

V. Drukovic et al. / Talanta 62 (2004) 489495

Relative intensity of fluorescence

240
200
160
120
80
40

Ir(IV)-HX
Ir(IV)-HY

0
0

20

40

60
IV

c(HX or HY) / c(Ir )

Fig. 3. Effect of HX or HY on the fluorescence intensity of iridium(IV)HX(HY) complexes in chloroform layer: c(Ir(IV)) = 2.2 105 M. (,
) c(H2 SO4 ) = 1 103 M, c((H,Na)2 SO4 ) = 0.2 M; (, ) c(HClO4 ) = 1 102 M, c((H,Na)ClO4 ) = 1.0 M; (, ) c(HCl) = 1 102 M,
c((H,Na)Cl) = 1.0 M.

120 min after the separation of two phases. Fluorescence

intensity of the extract was found stable and constant after
shaking time longer than 15 for Ir(IV)HX and 20 min for
Ir(IV)HY complex, so the shaking time was kept to 25 min.
Effect of the HX and HY concentrations on the fluorescence intensity is shown in Fig. 3. Reagentschloroform solutions of the various concentrations were added to the solution containing 2.2105 M of iridium(IV) at optimum conditions. It was found that the fluorescence intensity showed
a constant value for more than 0.1 mM of HX and more than
0.5 mM of HY. Thus, the concentration of HX was adjusted
to 0.4 mM and of HY to 1.3 mM, respectively.

The extraction was performed from aqueous phase of a

given composition using HX in various solvents as diluents.
The extraction was non-reproducible with isobutyl methyl
ketone and incomplete with isoamyl alcohol as diluents for
HX. The extraction becomes quantitative with chloroform
and dichloromethane. Chloroform is recommended for further extraction procedures.
3.2. Calibration graph, precision and accuracy
The calibration graph for the determination of iridium(IV)
was constructed using the optimum conditions. The mea-

Table 1
Detection limit of foreign ions to the spectrofluorimetric determination of iridium(IV) with HX
Tolerance limit ([ion]/[iridium(IV)])

5000
2500
1000
500
300
250
100
50
10
5
<1

Ion
Sulphate solutiona

Chloride solutionb

Sulphate, chloride, perchlorate, Na(I), K(I)

Oxalate
Phosphate, citrate
Bromide, Ni(II), Mn(II), Cd(II)
Rh(III)
Tartarate, acetate,
Thiocyanate, Co(II)
Carbonate, Cu(II)
Pt(IV)

Na(I), K(I), perchlorate

Oxalate
Ni(II), Cd(II), Mn(II), Cu(II), phosphate, citrate
Bromide
Rh(III)
Tartarate
Co(II), carbonate

Os(VIII), Os(IV), Pd(II), Ru(III), Mo(VI), Fe(III), Ag(I)

Conditions: 2.0 105 M Ir(IV); 4.0 104 M HX.

a 1.0 103 M H SO , c((H,Na) SO ) = 0.2 M.
2
4
2
4
b 1 102 M HCl, c((H,Na)Cl) = 1.0 M.

Pt(IV), Ag(I)
Ru(III), Pd(II), Os(VIII)
Os(IV), Os(VIII), Fe(III), Mo(VI)

V. Drukovic et al. / Talanta 62 (2004) 489495

surement was carried out at excitation (2.5 nm) and emission

slit width (6 nm). Linear calibration graphs were obtained
in the range 0.17.6 g ml1 of iridium(IV) for Ir(IV)HX
complex and 0.15.8 g ml1 of iridium(IV) for Ir(IV)HY.
The calibration lines for Ir(IV) determination fit the equations RIF = 4.64+45.58C (R = 0.999) for Ir(IV)HX complex and RIF = 13.84 + 27.96C (R = 0.992) for Ir(IV)HY
complex (where C presented Ir(IV) in g ml1 ). The relative standard deviations evaluated from 10 independent determinations of 1.92, 3.84, and 7.68 g ml1 of iridium(IV)
were 0.9, 1.1, and 0.6%, respectively.
3.3. Interference studies
All results previously presented indicated the difference
in fluorescence intensity for Ir(IV)HX and Ir(IV)HY
complex. The organic layer which contained Ir(IV)HY had
about 40% smaller fluorescence intensity than Ir(IV)HX
complex. Iridium(IV) can be extracted with less excess
of HX. From this point of view we assumed that the
Ir(IV)HX complex is more stable than Ir(IV)HY complex.
Therefore, in further studies the Ir(IV)HX complex was
used.

493

marised in Table 1. The smaller interferences of foreign ions

were detected when extraction of the Ir(IV)HX complex
was carried out from chloride solutions. Most metal ions
and anions did not interfere. The most serious interferences
were observed with iron(III), osmium(IV), osmium(VIII)
and molybdenum(VI).
3.4. Composition of the extracted species
Previously we have investigated the ratio of iridium(IV)
to HX(HY) in the extracted species, which are determined
spectrophotometrically, by Jobs and the mole ratio methods [21]. The results were indicated that the metal and the

3-hydroxy-2-methyl-1-phenyl-4-pyridone (HX)

3.3.1. Cations and anions

The effects of various ions on the determination of Ir(IV)
with HX were studied. Fixed concentration of iridium(IV)
(3.8 g ml1 ) was taken with different amounts of foreign
ions and the recommended procedure was as follows. Metal
ions were added as the nitrate, chloride, or sulphate, while
the anion were added as ammonium, potassium, or sodium
salts. The limiting value of the concentration for each ion
was taken as that value, which caused an error, not higher
than 3% in the fluorescence intensity. The results are sum-

Ir(IV)-HX complex
isolated from sulphate medium
128

Relative intensity of fluorescence

400

300
Ir(IV)-HX complex
isolated from hydrochloric medium

100

200

133

100

0
0.0

0.2

0.4

0.6

0.8

1.0

c(Ir)
c(Ir) + c(HX or HY)
Fig. 4. Determination of Ir(IV) to HX(HY) ratio by Jobs method:
(, ) c(H2 SO4 ) = 1 103 M, c((H,Na)2 SO4 ) = 0.2 M; ()
c(Ir) + c(HX) = 1.2 104 M; () c(Ir) + c(HX) = 9.0 105 M;
(, ) c(HClO4 ) = 1 102 M, c((H,Na)ClO4 ) = 1.0 M; ()
c(Ir) + c(HY) = 2.0 104 M; () c(Ir) + c(HY) = 9.0 105 M.

500

400

300

200

100

-1

Raman Shift (cm )

Fig. 5. Raman spectra of HX and IrHX complex isolated from sulphuric
and hydrochloric acid media.

494

V. Drukovic et al. / Talanta 62 (2004) 489495

ligand, in the extracted species, were present in the ratio

Ir(IV):HX = 3:2.
The results of the Jobs method applied fluorimetrically
are presented in Fig. 4. A broad maximum has got an option
for formation mixture of complexes or polymeric species.
We have isolated IrHX complex in the solid form (see
Section 2.4) in order to confirm the formation of the extracted species. The isolated complex was again dissolved in
CHCl3 and the solution gave fluorescence spectra identical
to that obtained by direct extraction. This proves further that
during the isolation neither decomposition nor any change
occurred. The magnetic susceptibility was measured, and
the data showed that the isolated complex is diamagnetic.
Very few analytical methods are based on measurements
of luminescence intensity for the determination of transition metals because most complexes of these metal ions are
paramagnetic and thus do not fluorescence in fluid solution
[12]. Octahedrally co-ordinated Ir(IV) has a t52g configuration with one unpaired electron [27]. On the other hand,
Soroka et al. [28] have examined the fluorescence properties
of iridium(IV)8-hydroxyquinoline-5-sulfonic acid (HQS)
complex. Authors concluded that iridium(IV) is a strong oxidising agent, and that the fluorescence is due to the HQS
oxidation product rather than the metal chelate. The diamagnetic property of iridium polynuclear complexes some

authors attributed to strong spinspin interactions by direct metalmetal (MM) bonding. In the absence of the
metalmetal interactions, on the other hand, complex containing iridium(IV) (d5 ) would be paramagnetic (high-spin)
[29,30].
A large number of complexes containing MM bonds are
known. In general, (MM) in vibrational spectra appear in
the low-frequency region (200100 cm1 ) [31,32]. Raman
spectra of HX and IrHX complex isolated from sulphuric
and hydrochloric acid media are shown in Fig. 5. The complex line at 128 cm1 (isolated from sulphuric media) and
two shoulder at 100 and 133 cm1 (isolated from hydrochloric media), were attributed to MM bond. Our results (Job,
Raman, and magnetic susceptibilities) could be accounted
for by postulating formation of a polymeric type complex
with a metalmetal bridge.
3.4.1. Comparison with the other methods
Iridium(IV) and iridium(III) react with different ligands,
which reactions can be used in spectrophotometric determination of iridium [110]. Only two papers described fluorimetric method for determination of iridium(III) [12,28].
Therefore, we compare the proposed method for fluorimetric determination of iridium as an Ir(IV)HX(HY)
complex with spectrophotometric methods described earlier

Table 2
Comparison of the present method for the determination of iridium with some of the methods reported in literature
Reagent

Medium

Temperature
(heating time)

Linear range
(g ml1 of Ir)

1,5-Diphenyl carbazide
1-Phenyl-4,4,6-trimethyl-(1H,4H)pyrimidine-2-thiolate
Bis(thiopheno-2-aldehydo)-thiocarbohydrazone
N--Pyridyl-N -benzoyl thiourea
Difurfuryl thiocarbohydrazone
Piperazine dimalonate
5-(5-Nitro-2-pyridylazo)-2,4-diaminotoluene
2-Methyl-1,4-naphthoquinone monooxime
2,2 ,2 -Terpyridine
3-Hydroxy-2-methyl-1-phenyl-4-pyridone
3-Hydroxy-2-methyl-1-(4-tolyl)-4-pyridone

CHCl3
CHCl3

100 C (45 min)

60 C (5 min)

0.533.00
3.842.0

<1
40

[1]
[2]

Ethyl acetate
CHCl3
Ethyl acetate
Aqueous
Aqueous
1-Butanol
Aqueous
CHCl3 , CH2 Cl2
CHCl3 , CH2 Cl2

100 C (30 min)

100 C (45 min)
No heating
No heating
No heating
No heating
100 C (120 min)
No heating
No heating

1.24.2
0.818.16
0.933.73
0.024.0
0.00.7
0.013.7
210
0.17.7
0.54.8

<1

2
10
<1
<1
5
300
20

[3]
[4]
[5]
[6]
[7]
[8]
[12]
This work
This work

Tolerance limits
(c(Rh)/c(Ir))

Reference

Table 3
Determination of iridium in some synthetic mixtures
Composition of the synthetic mixture (, g ml1 )

Speciality

Amount of iridium
found (, g ml1 )

R.S.D. (%)

Sample 1
Ir(28)Pt(55)Rh(7)Cu(3)Pd(3.5)

Alloy

28 2

1.3

Sample 2
Ir(20)Pd(10)Pt(15); Rh(15)Os(2)Mn(50)

Alloy

19 1

0.7

Sample 3
Ir(3.5)Rh(7.6)Ni(30)Mn(100)Cd(60)Pb(20)Cr(1)Mg(150)

Geological sample

Sample 4
Ir(20)Rh(15)Os(10)Pt(200)
Average of four determinations. Conditions: 4.0

Geological sample
104

M HX, 1.0

103

3.4 0.9
19 1

M H2 SO4 , c((H,Na)2 SO4 ) = 0.2 M.

0.8
1.1

V. Drukovic et al. / Talanta 62 (2004) 489495

495

Table 4
Determination of iridium in mineral sample

Acknowledgements

Sample

Found Ir (ppb)
INAA

Proposed method

R.S.D. (%)

This work was supported by the Ministry of Science and

Technology of Croatia Project Nos. 119410 and 0181006.

Chromite Alb-121

300

306 12

3.9

Average of six determinations. Conditions: 4.0 104 M HX, 5 103 M

HCl, c((H,Na)Cl) = 1.0 M, INAA was performed at ACTLABS (Ancaster,
Ontario, Canada).

(Table 2). In comparison with previously reported timeconsuming procedures for determination of iridium [14]
the proposed procedure is much simpler, because no heating is required, and the method is more sensitive. On the
other hand, rhodium ions interfere in previously described
methods [1,35,7,8,12], but this method allows possibility
in the presence of 300-fold excess of rhodium(III).
3.5. Analytical applications

References
[1]
[2]
[3]
[4]
[5]
[6]
[7]
[8]
[9]
[10]
[11]

The method was applied to a set of synthetic samples and

to the mineral sample (chromite Alb-121) in order to validate it. Synthetic concentrates with Ir(IV) contents similar
to those typically found in some industrial alloys and geographical samples were prepared. As can be seen in Table 3,
the results obtained were highly consistent with the added
amounts.
Sample treatment of natural mineral sample (chromite
Alb-121) is described in Section 2.6. At least the sample
solution was determined spectrofluorimetrically by the standard additions method. The result of analysis was in good
agreement with the value obtained by instrumental neutron
activation analysis (INAA) method (Table 4).

[12]
[13]
[14]
[15]
[16]
[17]
[18]
[19]
[20]
[21]
[22]

4. Conclusion

[23]

The present work describes the determination of iridium

by measuring the intense luminescence of the Ir(IV)HX
chelate in solution. The proposed methods have the advantages of being simple, reproducible, selective and more
sensitive over many other methods. Iridium was thus determined in the range 0.17.6 g ml1 . The relative standard deviations were 0.9, 1.1, and 0.6 % for 1.92, 3.84,
and 7.68 g ml1 of iridium(IV), respectively. HX can be
used for the determination of iridium at room temperature even in the presence of platinum and rhodium. The
method can be applied for simultaneous determination of
iridium in synthetic mixtures, corresponding to some standard reference samples such as alloys, and in natural mineral
sample.

[24]
[25]
[26]
[27]
[28]
[29]
[30]
[31]
[32]

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