477

GOLD,PALLADIUM IN SOUTH
AND TELLURIUM AFRICAN,
CHINESE
AND JAPANESEGEOLOGICAL
REFERENCE
SAMPLES

E. KONTAS, H. NISKAVAARA and J. VIRTASALO

Chemical Laboratory, Geological Survey of Finland,

P.O. Box 77, SF-96101 Rovaniemi, Finland

Reliable rock reference materials for Au, Pd and Te are detection limits were 0.2,0.4 and 1 ppb for Au, Pd and Te,
scarce. We report here our analytical data on these respectively.
three elements in 46 NIM, IGGE and GSJ reference
samples in order to accumulate analytical data on these RESULTS AND DISCUSSION
samples.
Three independent analyses have been done on each
sample and the averages and standard deviations are pre-
The analytical method employed is based on aqua sented in Tables 1 to 3. Some literature values have been
regia digestion of samples at room temperature overnight. found for Au and Te but none for Pd. Therefore the accu-
Weighing may vary from 0.1 g up to 20 g depending on racy of results can be only estimated.
sample type and metal to be determined. If the determina-
lion of Au is of primary interest larger weighing would be Table 1. Au, Pd and Te in the six NIM reference samples, in
necessary. However, for reference samples only restricted ppb. Average of three determinationsf standard deviation
amount of material is available and hence smaller weigh- This work Reported values
ings must be used. Au, Pd andTe have been separatedfrom Au
matrix solution by reductive co-precipitation using SnCl2
Sample Au Pd Te Ref. 3 Ref. 4
as rcductant and mercury as coprecipitant. Centrifuging
has bccn used in the separation of the Hg precipitate from NIM-G 1.0f0.0 <0.4 7fl 1.07 8
NIM-S 0.7 f0.3 ~0.4 2f0.2 0.29
the solution. For the analysis, the Hg-(Au-Pd-Te) precipi- NIM-L 1.7f0.3 <0.4 9fl 0.64 4
tate is dissolved in aqua regia and diluted with 3M HN03 NIM-N 1.5k0.3 1.1 50.1 1f0.5 0.76 4
NIM-P 1.1 fO.l 18.2k0.4 3f0.5 0.82
(1-2). NIM-D 0.7rt0.2 <0.4 1 +0.5 0.41

In this work 1.OO g sample weight was used. Because it

is possible that some Te can be lost during roasting at
70O0C,only graphite bearing samples were roasted before
digestion for the determination of gold while Pd and Te
were determined in unroasted samples. Pd has been deter-
mined using pyrocoated tube and peak height integration
wilh Perkin-Elmer Model 2280 AAS equipped with HGA
500 graphite furnace and D,-background corrector; Au and
Te have been determined with Perkin-Elmer Model 3030
Zeeman graphite furnace AAS using pyrocoated L’vov
platform tube and peak area integration. For Te, indium
solution (1000 ppm) was used as a matrix modifier (2). The
Some Au contents in the NIM samples (Table 1) ob-
tained in this study are in good agreement wilh
Terashima’s values (3) but some are not. The values pre-
sented by Steele et al. (4) are much higher than ours; no
reliable data for Pd and Te exists in the literature.
Au and Te contents in IGGE samples (Table 2) ob-
tained in this work are generally lower than the reported
values (5). Some Te values deviate Len fold from our
values. The deviations between some analytical methods
used in the Chinesc work (5) are so large that apparently

Geostandards Newsletter, Vol. 14,N o 3 , Octobre 1990,p . 477 cf 478

478

nificantly from our values. This may be due to heterogene-

Table 2. Au, Pd and Te in 18 IGGE reference samples, in ous occurrence of gold in these samples.
ppb. Average of three determinations f standard deviation
This work Reported values Generally, the precision for Au, Pd andTe is excellent.
Sample Au Pd Te Au (5) Te (5)
The detection limit of 0.4 ppb for Pd is too high for most
GSR-1 0.2fO.I
sample types to obtain accurately their contents.The disso-
4.4 7 i I 0.55f0.18 21 f 3
GSR-2 0.9 f 0.1 4.4 1 f0.5 0.95f0.32 17f3 lution of Te in aqua regia digestion is a matter for discus-
GSR-3 0.5 f 0.1 4.4 15~0.5 0.66i0.20 22f9 sion. The hydrobromic acid-brominedigestion is adequate
GSR-~ i.afo.3 4.4 s +-2
_. 1.8fo.6
_. - 3_ _a-t 7
GSR-5 0.4 f 0.1 4.4 12fl 1.Of0.5 22f8 to dissolve tellurium in most geologic samples (7). How-
GSR-6 0.6 f 0.1 4.4 15f2 0.94f0.45 23f8
GSS-1 0.3 f 0.1 4.4 34f3 0.55f0.1 51 f 3 4 ever, if tellurium minerals are occluded in or protected by
GSS-2 1.4f 0.1 4.4 20f2 1.7f0.3 35f17 silicates or siliceous materials, decomposition involving
GSS3 '4.7 f 1.4 4.4 23fl __ 40f9
GSS-4 3.6 f 0.2 4.4 21 + 3 5.5*1 6 lfiOt70 hydrofluoric acid may be beneficial (7). Aqua regia is a
GSS-5 216f9 4.4 3960 I 2 0 0 266f 4 4066c2300
GSS-6 4.5 f 0.2 4.4 24ofii 9+5 420iiao solvent similar to hydrobromic acid-bromine and therefore
GSS-7 0.4 f 0.1 4 4 ll+l 0 ..8 f 0 2
~
._
aqua regia digestion may be regarded as adequate.
GSS-8 0.9 f 0.1 k.4 2521 1.4f0.4 46f8
GSD-9 0.3f0.1 4.4 28fl 1.3f0.8 40f20
GSD-10 0.5f0.2 4.4 77fl -- 90 + 40
GSD-11 2.7f0.3 4.4 46OI10 3.6f0.9 38OI150 RESUME
GSD-12 2.6f0.6 4.4 250f10 5.6f2.3 290f5
'one outlier content of 46 ppb Au rejected. Tres peu d'echantillons de reference, bien caracterises
pour leurs teneurs en Au, Pd et Te sont disponibles.
Aussi, presentas-nous nos rbultats sur ces trois
Table 3. Au, Pd and Te in 22 GSJ reference samples, in ppb.
Mments dans 46 khantillons de reference afin d'ac-
Average of three determinations f standard deviation croitre les donnkes analytiques sur ces Cchantillons.
This work Reported
REFERENCES
values
Sample Au Pd Te Au (Ref. 6)
(1) E. Kontas, H. Niskavaara and 3. Virtasalo (1986)
JG-1a c0.2 c0.4 3 f 0.5 0.14 Flameless atomic absorption determination of gold and
JG-2 <0.2 10.4 3 f 0.5 palladium in geological reference samples, Geostandards
JG-3 <0.2 e0.4 2f0.5
JR-1 0.2 f 0.1 c0.4 1 f0.5 Newsletter, 10: 169-171.
JR-2 0.2 f 0.1 c0.4 1 f0.5
JA-2 0.2 f 0.1 ~0.4 1 f0.5 (2) H. Niskavaara and E. Kontas (1990)
JA-3 0.6 f 0.1 0.9 f 0.2 3 f 0.5 Reductive co-precipitation as a separation method for the
JB-la 0.4 f 0.1 c0.4 1 f0.5 0.7 determination of Au, Pd, Pt, Rh,Ag, Se and Te in geologi-
JB-2 *3.7 f 0.1 5.6 f 0.3 4 f 0.5 6
JB-3 1.6f0.2 2.8f0.2 2 f 0.5 2.1 cal samples with graphitefurnace atomic absorptionspec-
JGb-1 0.9 f 0.1 c0.4 llfl I trometry, Analytica Chimica Acta, 231: 273-282.
JP- 1 0.2 f 0.1 1.4 f 0.3 1 f 0.5 0.1
JF-1
JF-2
<0.2
<02
<0.4
<0.4 <1
<l .
(3) S Terashima (1988)
JLk-1 0.5 f 0.1 1.1 f 0.3 113f2 6
Deterrnination of gold in sixty geochemical reference
JLs-1 c0.2 <0.4 1 f 0.5 samples by flameless atomic absorption spectrometry,
JDO-1 <0.2 ~0.4 2 f 0.5 Geostandards Newsletter, 12: 57-60.
JSI-1 0.3 f 0.1 0.7 f 0.5 65f3
JSI-2 <0.2 0.5 0.1 45f1 (4) T. W.Stele, A. Wilson, R. Goudvis, P. J. Ellis and A. J.
JSd-1 0.7 f 0.1 <0.4 21 f 1
JSd-3 2.9 f0.2 0.9 f 0.1 264f6 Radford (1978)
JCh-I t0.2 0.5 f 0.1 22f 1 Trace element data (1966-1977) for the six NIMROC
reference SamDles. Geostandards Newsletter, 2: 71-106.
"one outlier content of 26 ppb Au rejected
(5)X.Xie,M.Yan,C.Wang,L.LiandH.Shen(1989)
Geochemical standard reference samples GSD 9-12, GSS
all those methods are not reliable for the determination of 1-8 and GSR 1-6, GeostandardsNewsletter, 13: 83-179.
low Te contents in geological samples. All Pd contents are
(6) K. Govindaraju (1989)
below the detection limit (0.4 ppb) of the method used in and sample descrip-
this work. Newsletter, Spe-

Only some reported values for Au for the GSJ samplcs (7) R. M.O'Leary and A, L. Meier (1984)
(Table 3) have been found in the literature (6). The re- Analytical methods used in geochemical exploration, U.S.
ported values €or the samples JB-2 and JLk-1 deviate sig- Geological Survey Circular 948,39 pp.