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Preparation and certification of high-grade gold geochemical reference

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DOI: 10.1007/s00769-006-0179-8

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Accred Qual Assur (2006) 11: 329–335
DOI 10.1007/s00769-006-0179-8 GENERAL PAPER

V. Balaram
M. L. Patil
Preparation and certification of high-grade
A. K. Agrawal gold geochemical reference material
D. V. Subba Rao
S. N. Charan
M. Satyanarayanan
Ramavati Mathur
K. Kapilavastu
D. S. Sarma
M. Sankara Gowda
S. L. Ramesh
P. Sangurmath
K. V. Anjaiah
B. Dasaram
R. K. Saxena
Zahida Begum

Received: 3 March 2006

Accepted: 29 May 2006
Published online: 5 July 2006


C Springer-Verlag 2006
V. Balaram (
) · D. V. S. Rao ·
S. N. Charan · M. Satyanarayanan ·
R. Mathur · S. L. Ramesh ·
K. V. Anjaiah · B. Dasaram · Z. Begum
National Geophysical Research
Institute,
Hyderabad 500 007, India
e-mail: balaramv1951@yahoo.co.in
M. L. Patil · K. Kapilavastu ·
M. S. Gowda · P. Sangurmath
The Hutti Gold Mines Company
Limited,
Hutti-584115, Karnataka, India
e-mail: patil hgml@yahoo.com
A. K. Agrawal · R. K. Saxena
National Physical Laboratory,
New Delhi 110 012, India
e-mail: aka@nplindia.ernet.in
D. S. Sarma
University of Western Australia,
Perth 6009, Australia
Abstract One high-grade gold
geochemical reference material-BND
3401.01 has been prepared by the
National Geophysical Research
Institute (NGRI), Hyderabad in
collaboration with the Hutti Gold
Mines Company Limited (HGML),
Hutti and National Physical
Laboratory (NPL), New Delhi, in
India. The sample is a sheared
gold-sulphide-bearing quartz vein
emplaced in a sheared acid volcanic
rock that was collected at the
2400-foot level from the middle reef
of Hutti deposit located in the
north-western periphery of the
late-Archaean Hutti-Maski
greenstone belt, Karnataka, India.
Fifteen institutions in India, Canada,
China and Tanzania having
experience in geochemical analysis
had participated in this collaborative
analysis programme. The sample was
extensively characterized for its
major, minor, trace and ultra-trace
element composition by using a
variety of analytical techniques.
Usable values were provided for
major, minor and several trace
elements including all rare earth
elements (REE). The certified value
for the gold concentration in BND
3401.01 gold ore is 12.1 ± 0.7 mg/kg.
Keywords Gold reference material .
BND 3401.01 . REE . Trace
elements . International collaborative
analysis . Certified value

Introduction concentration of gold in rocks, minerals, ores and soils. In

Exploration for gold is a challenging task due to its char-
acteristic heterogeneous levels of concentration, nugget ef-
fect, and distribution in rocks, ores and soils. Exploration
for locating gold deposits is typically characterized by a
large-scale and systematic sampling effort over a suspected
mineralized region in a gridded pattern in order to establish
regional distribution and background anomalous concen-
tration contour maps, describing the nature of occurrence
of economically profitable zones in association with en-
velopes of relatively low-grade areas within a given region.
Consequently, analytical methods developed for the deter-
mination of gold must have sufficient sensitivity, accuracy,
and robustness to detect and determine even the lowest
addition, quality control protocols involving measurement
against appropriate and traceable certified reference mate-
rials (CRMs) are also required for testing the reliability of
each batch of data produced in the laboratory. Such refer-
ence materials are prepared from rock matrices that contain
gold with a uniform distribution throughout the pulverized
rock powder and are extremely valuable in the routine es-
timation of gold in geological samples and data quality
monitoring, especially, in gold exploration studies. One of
the most important features is that the CRMs must be of the
same lithological type as the test material in a given batch
to eliminate/minimize various interference associated with
analytical methods.
330
Due to the complex variety and broad variability in the
chemical compositions and petrological characteristics of
the naturally occurring auriferous materials, it is essen-
tial that analytical geochemists have access to a variety of
CRMs in order to accurately assess the nature and distri-
bution of gold in a given area. In order to meet such an
important requirement of gold exploration studies and the
mining industry in the country, it is proposed to prepare a
series of gold geochemical reference materials covering a
wide range of gold concentration ( ∼ 50 ng/g–15 mg/kg),
comprising of natural geological materials encompassing
different lithological types including ores, host rocks and
soils. As a first step in this national endeavour, a high-grade
gold reference material BND 3401.01 is prepared and char-
acterized using an international collaborative study, the re-
sults of which are presented here.
Sample collection and preparation
Approximately 350 kg of a sheared, gold-rich sulphide-
bearing quartz vein emplaced in a sheared acid volcanic
rock was collected at the 720-m level from the middle reef
of Hutti deposit located in the north-western periphery of
the Hutti-Maski greenstone belt, Karnataka. Ore material
was manually chipped to 2.5-cm size sample splittings and
the whole material was crushed to 0.5 cm size by Labora-
tory Jaw Crusher and Rolls Crusher. After crushing the raw
sample, it was repeatedly mixed manually. The ore mate-
rial was then ground to 63 µm by a Disc Pulverizer and
screened through a 75-µm sieve and the screened materials
thoroughly mixed manually by repeating standard mixing
procedures such as coning and quartering several times.
After a full homogeneity test, 500 g of this finely powdered
material was packed in wide-mouth polyvinyl plastic jars
of 500 ml capacity. An announcement was published in the
Journal of Geostandards and Geoanalytical Research for
Fig. 1 Error bar chart for gold 12.80
determination of 25 replicates of
BND 3401.01 gold ore sample
by F-AAS. The precision is of 12.60
about 1.54% RSD, which is
well within the acceptable range
12.40
c(Au)/(mg/kg)
12.20
12.00
11.80
11.60
11.40
1 2
Mean = 12.3; SD = 0.19; CV = 0.04
collaborative analysis of this sample [1], as such interna-
tional collaborative analysis programmes are found to be
extremely useful in this kind of studies [2].
Petrography
Petrographic studies were carried out on thin sections of
the sample. The productive gold sulphide bearing quartz
reef consists of recrystallized quartz ribbons, calcite veins,
gold, arsenopyrite, pyrite, minor chlorite/biotite, sericite
and scheelite, constituting the high-grade Au ore.
Homogeneity testing
About 500 bottles were filled with 500 g of sample pow-
der and were divided into ten batches. To comply with the
criterion required to confirm with primary certified refer-
ence materials [3], 25 sub-samples (5% of the total bottles)
of the sample was taken at random for replicate analyses.
Care was taken to select at least 2–3 samples (20–30%
from each batch) from all batches. Ten duplicate samples
were analyzed within a single bottle and the results agreed
within 2% RSD. Each 10-g BND 3401.01 gold ore sample
was transferred to a porcelain crucible along with 1 g of
ammonium nitrate, then mixed thoroughly, and roasted for
1 h in a muffle furnace at 650◦ C. After roasting, the samples
were transferred to 250-ml glass beakers and 30 ml freshly
prepared aqua regia was added to each sample. One gram
of NaCl was added to stabilize gold chloride complex dur-
ing evaporation on a hot plate. Heating was continued for
at least 4 h with the addition of aqua regia at regular inter-
vals to maintain the free acid level at about 1 cm above the
sample level. The watch glasses were then removed and the
contents evaporated slowly until the residue became nearly
dry. Then 40 ml of 3 M HCl was added to each beaker
3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25
Sample nos.
 331

Table 1 List of participating Country Institute Name of the scientist

Laboratories
Canada i) Lab. Geochemie L. Paul Bedard
Universite du Quebec a Chicoutimi, G7H 2B1
ii) Department de geologie et de genie geologique, Universite Laval, Marc Constantin
Sainte-Foy Quebec, G1K 7P4
China i) Institute of Geophysical and Geochemical Exploration, Langfang Chi Qinghua
Hebei 065000
India i) Geological Survey of India Central Region Nagpur S. N. Girhe
T. K. Pal
R. J Gajbhiye
ii) Ore Dressing Division S. R. Bhaisare
Indian Bureau of Mines, Nagpur – 440 016
iii) Geological Survey of India Kerala Unit Kurian V. Kunnath
Thiruvananthapuram-695 014
iv) Geochemistry Division J. B. Ghosh, C. Saha
Geological Survey of India P. Roy Chowdhury
Kolkata – 700 016 N. K. Banerjee
v) The Hutti Gold Mines Co. Ltd M. Shankar Gouda
Hutti – 584 115, Karnataka
vi) National Centre for Compositional Sunil Sai Kumar
Characterisation of Materials (CCCM)
Hyderabad – 500 062
vii) Bhaba Atomic Research Centre M. Sudersanan
Mumbai – 400 085
viii) Shiva Analyticals (India) Ltd Sitaram
Bangalore
ix) Ashco Analytical Services Padma
Andheri (E)
Mumbai – 400 093
x) Geochemistry Division T. Gnaneshwar Rao
National Geophysical K. Krishna
Research Institute
Hyderabad – 500 007
xi) Osmania University
Hyderabad – 500 07
Tanzania i) Geological Survey of Tanzania A. Nyalusi
(GST), PO Box 903
Dodama, Tanzania
East Africa

and the solutions were warmed until clear solutions were Table 2 Concentrations∗ (%) Concentration
obtained. These sample solutions were cooled and filtered of trace elements in the
high-grade gold geochemical Major oxide (%)
using Whatman No.1 filter paper. The residue was washed reference material BND
with a minimum amount of 3 M HCl. The final residue was SiO2 80.4 ± 0.8
3401.01 gold ore (information
discarded and the filtrate was used for the determination values) Al2 O3 4.0 ± 0.1
of gold by flame atomic absorption spectrometry (F-AAS) TiO2 0.25 ± 0.002
after methyl iso-butyl ketone (MIBK) extraction [4]. In Fe2 O3 4.1 ± 0.05
our laboratory, international gold certified reference mate- MgO 1.7 ± 0.03
rials obtained from Rocklabs, New Zealand (Ox-15, S-8, CaO 4.3 ± 0.09
S-6, S-9, etc.) and Canadian Certified Reference Material Na2 O 0.91 ± 0.02
Project (CANMET, Canada) (WMG-1, WMS-1, etc.) were ∗
Average of 6 replicates K2 O 0.65 ± 0.01
also treated in a similar way and the resulting respective MnO 0.07 ± 0.002
Accuracy is <6% RSD (relative
solutions were used for calibrating the instrument and also standard deviation) P2 O5 0.03 ± 0.001
to check the accuracy and precision of the measurements. LOI Loss on ignition LOI 2.7 ± 0.05
Figure 1 presents the results of the determination of gold
in 25 replicates of BND 3401.01 gold ore sample. It can be
seen that the coefficient of variation of homogeneity testing
 332

0.13 ± 0.01
0.15 ± 0.01
0.40 ± 0.02
0.39 ± 0.02
0.12 ± 0.01
0.09 ± 0.01
0.18 ± 0.01
Concentration

0.5 ± 0.03
is very small and within the error range of the analytical
50.4 ± 3.0

82.5 ± 4.9
16.4 ± 0.9
5.2 ± 0.3

68.8 ± 4.1
50.0 ± 2.9
method. Since the coefficient of variation of homogeneity
testing was very small and within the error range, inhomo-
geneity of the sample was not included. It was also found
that good representativeness of sub-sampling is guaranteed
when each sub-sample weight is 10 g or higher.
Element

International collaborative analysis of BND 3401.01

Tm

Yb
Tb

Th

Zn
Zr
Ta

Te
Sr

W
Tl

U
V

Y
Fourteen laboratories in India, Canada, China and Tanzania
Serial number
Concentrations∗ (mg//kg) of trace elements in the high-grade gold geochemical reference material BND 3401.01 gold ore (information values)

have participated in the analytical programme; they are

listed in Table 1. All these laboratories have had expertise
in the analysis of gold for over a decade and have credible
43
44
45
46
47
48
49
50
51
52
53
54
55
56 record in the form of publications in reputed international
journals. One pack, containing 250 g of material, was
0.08 ± 0.005

0.53 ± 0.03

0.83 ± 0.05
0.61 ± 0.04
Concentration

sent to each participating laboratory, the analyst being

1901.0 ± 114
6.6 ± 0.4
1.6 ± 0.1
1.4 ± 0.1
41.5 ± 2.5
29.2 ± 1.8

17.2 ± 1.0

3.1 ± 0.2
10.0 ± 0.5

2.0 ± 0.1

requested to submit three replicate analyses for as many

elements as possible. Though a few analytical methods
such as Pb-fire assay, MIBK F-AAS and di-ethyl iso-butyl
ketone (DIBK) F-AAS methods were specified for the
estimation of gold, other well-proven methods can also
be employed. Since many geochemical laboratories do
not have facilities for gold analysis, only 14 laboratories
Element

(Table 1) responded and submitted data. Surprisingly,

Mo

Sm
Nb
Nd

Rb
Lu

Pb

Sb

Sn
Pr
Ni

Sc
Se

there was no response from the chemical laboratories of

S

the mining companies in the private sector. Individual

Element Concentration Serial number

laboratories have adopted procedures similar to the one

adopted in our laboratory for calibration.
29
30
31
32
33
34
35
36
37
38
39
40
41
42

Major, minor, trace and rare earth element (REE) data

0.79 ± 0.04
0.56 ± 0.03
0.23 ± 0.02

0.83 ± 0.05
0.10 ± 0.01
0.26 ± 0.02

0.18 ± 0.01
263.0 ± 15.8

1.2 ± 0.07
5.6 ± 0.3

10.4 ± 0.6

Information values were calculated from the data obtained

< 0.0006
< 0.12

by different participating laboratories. From the cluster,

< 0.1

outliers were removed and the mean was calculated. Out-

liers were identified by their isolated position in the cluster.
Care was taken to include as many values that fall un-
der stable cluster, while calculating the mean. Sufficient
Gd
Ga

Hg
Ho
Eu
Dy

Ge

La
Er

Hf

Li
Ir

care was also taken to see that data from at least two
F

reliable analytical methods based on different principles

Element Concentration Serial number

were included, when the data is in agreement with each

other.
The majority of the laboratories used XRF (both WD and
ED) for the determinations of major and minor elements.
15
16
17
18
19
20
21
22
23
24
25
26
27
28

F-AAS, ICP OES and colorimetric methods were also uti-

lized. Usable data of major and minor element composition
214.1 ± 11.8
7403 ± 440

0.33 ± 0.02
0.29 ± 0.02
7800 ± 462
1.0 ± 0.05

15.0 ± 0.8
99.3 ± 5.8

17.4 ± 1.0
35.1 ± 2.1

for the high grade reference material, BND 3401.1 gold ore
3.9 ± 0.2

2.0 ± 0.1
2.7 ± 0.2

1.3 ± 0.1

sample are presented in Table 2.

Popular analytical techniques such as ICP-MS, ICP OES
Average of 6–10 replicates

and INAA were used by most of the participating labo-

ratories for the generation of trace and REE data. Other
Accuracy is <6% RSD

analytical techniques like emission spectrometry (ES), ion

Cd

Cu
Ag

Co
Ba

Ce

Cr
As

Be

Cs

Cl
Bi
C
B

selective electrode (ISE) were also used. Acid digestion

(both open as well as closed using acid mixture) as well
Serial number

as fusion digestions were used. Concentrations for several

trace elements including all 14 REE obtained from different
Table 3

participating laboratories were very consistent (Table 3). A

10
11
12
13
14

plot of REE content normalized to chondritic abundances

1
2
3
4
5
6
7
8
9

∗
 333

Fig. 2 Chondrite-normalized 100.0

REE pattern of the high-grade
gold reference material

REE/Chondrite
10.0

1.0
La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu

Fig. 3 Values with uncertainty 17

range reported by participating
laboratories. Uncertainty was 16
calculated by the formula σ
 =
(standard 15

 deviation)
[(n x 2 ) − ( x 2 )]/[n(n − 1)]. 14
Solid and dotted lines indicate
mean and standard deviation 13
c(Au)/(mg/kg)

(4σs) respectively
12

11

10

6
10 04 07 03 11 02 05 01 06 08 09 12
Lab Code

Table 4 Z-score values calculated for the gold concentrations obtained from different laboratories
Z-score between the Z-score within the Sample weight
Lab code Au∗ (mg/kg) laboratories Zbi laboratory Zwi (in g) Technique used
01 12.3 ± 0.3 0.4 0.06 10 Pb-Fire Assay F-AAS finish
02 12.0 ± 0.2 –0.01 –0.4 10 Pb-Fire Assay F-AAS finish
03 11.6 ± 0.1 –0.5 –0.3 20 MIBK – F-AAS method
04 10.8 ± 0.7 –1.6 0.9 20 MIBK – F-AAS method
05 12.0 ± 0.3 0.01 0.04 20 K-Tellurate – F-AAS method
06 12.4 ± 0.03 0.5 –0.4 20 Pb-Fire Assay F-AAS finish
07 10.9 ± 0.1 –1.5 –0.4 50 Pb-Fire Assay F-AAS finish
08 12.6 ± 1.0 0.8 1.6 20 Polyurethane foam extraction – F-AAS method
09 13.0 ± 0.2 1.4 –0.2 5 MIBK – F-AAS method
10 8.5 ± 1.7 –4.6 3.0 0.1 Instrumental Neutron Activation Analysis
11 11.9 ± 1.2 –0.1 1.9 2.3 Instrumental Neutron Activation Analysis
12 16.5 ± 0.01 5.9 –0.471 0.1 Instrumental Neutron Activation Analysis
13 11.0∗∗ – – 20 MIBK – F-AAS method
14 Not reported – – – –
15 Not reported – – – –
∗
Average of six replicates
∗∗
Only one value provided
F-AAS Flame atomic absorption spectrometry
334

Fig. 4 Z-score within the 4.0

laboratory

3.0

2.0

Z Score wi
1.0

0.0
1 2 3 4 5 6 7 8 9 10 11 12
-1.0

-2.0
Participating Laboratories

Fig. 5 Z-score between the 6.0

laboratories
5.0

4.0

3.0

2.0
Z-score bi

1.0

0.0

-1.0 10 4 7 3 11 2 5 1 6 8 9 12

-2.0

-3.0

-4.0

-5.0

-6.0

Participating LaboratoryCode Number

should yield a smooth curve. Such plots provide informa-
tion on the formation environment, fractionation of differ-
ent REE, etc. [5]. The chondrite-normalized REE plot of
the high-grade gold reference material gave a smooth curve
(Fig. 2) suggesting that the data possessed the required ac-
curacy and precision.
laboratories provided data forms with replicate analysis
(Table 4). Except laboratories no. 10 and 12, all other lab-
oratories provided values within the expected target mea-
surement range (4σ) (Fig. 3). Uncertainty was calculated as
standard deviation based

on  (n − 1) method
the non-biased
by the formula SD = [(n x 2 ) − ( x 2 )]/[n(n − 1)].

Gold concentration Criteria followed for the assignment of certified value

for gold
Established methods such as (i) MIBK extraction and F-
AAS, (ii) DIBK extraction and F-AAS, (iii) Instrumental The procedure for certification of a reference material, for
Neutron Activation Analysis (INAA), (iv) K-tellurate pre- example, at Mintek [6] requires that the following criteria
concentration and F-AAS, (v) Pb Fire-assay and F-AAS, must be met before a certified value can be assigned to a
and (vi) preconcentration by polyurethane foam and F- constituent in a geological sample.
AAS, were used to generate highly precise concentration I. There must be a minimum of ten bottle means after the
for gold in this sample. Samples of 10–50 g were used to gross outliers have been rejected.
overcome problems associated with the heterogeneous dis- II. The robust relative standard deviation (robust Sr ) must
tribution of gold in geological samples. All participating be smaller than 33%.
 335

III. The distribution of the data must not be bimodal (i.e., it samples. Hence, a value of 12.1 ± 0.7 mg/kg (expanded un-
must not have two peaks when plotted as a histogram). certainty K = 2, 95% confidence level) has been assigned
IV. There must be good agreement between the four indi- for gold to this high-grade gold reference material, BND
cators of central tendency (mean, median, mode and 3401.01 gold ore.
standard deviation).
In addition, it is preferable for the results to be obtained
Conclusions
by the use of more than one analytical method and there
must be no obvious bias between the results obtained by
The certification of gold concentration value in this new
the different analytical techniques.
high-grade gold geochemical reference material, BND
To evaluate the quality of the data quantitatively, two
3401.01 gold ore was achieved successfully after the In-
types of Z-score values have to be calculated viz., Z-score
ternational Interlaboratory Comparison Programme on the
within the laboratory (Zwi) and Z-score between the labora-
analysis of gold in Au-sulphide-bearing quartz vein em-
tories (Zbi). Values of the Z-scores have been calculated by
placed in sheared acid volcanic rock from Hutti-Maski
integration of the seven summary statistics – number of the
greenstone belt, Karnataka, India. The certified value as-
laboratories, median, normalized interquartile range (IQR),
signed is 12.1 ± 0.7 mg/kg (expanded uncertainty K = 2,
robust coefficient of variation (CV), minimum, maximum
95% confidence level) and tests indicated that this sample
and range [7]. Z-score within the laboratory indicates the
had a high degree of homogeneity. This reference sam-
variance in the data produced in the laboratory itself and
ple is available at cost with the Co-ordinator, Indian Ref-
Z-score between the laboratories indicates the variance in
erence Materials Programme, National Physical Labora-
the data (median value) produced at different participating
tory, Krishan Marg, New Delhi 110 012, India (E-mail:
laboratories. Values of concentration of the gold reported
aka@mail.nplindia.ernet.in).
by the participating laboratories along with Z-score val-
ues are given in Table 4. The values of Z-score are com- Acknowledgements The authors are thankful to Dr. V.P. Dimri, Di-
pared in Figs. 4 and 5. For certification of the concentration rector, National Geophysical Research Institute, Dr. Vikram Kumar,
of gold in high-grade gold geochemical reference sample, Director, National Physical Laboratory, Mr. Ashok V. David, Chair-
data of the laboratories whose Z-score values are within man and Managing Director and Mr. B. S. Gangal, General Manager,
The Hutti Gold Mines Company Limited for their active support for
± 2 had been taken into account for statistical computation this study. The authors are grateful to Dr. Kishan Lal for initiating the
[8]. Arithmetic mean of the values, after rejecting the data Network Project on SRMs in India and Dr. Paul De Bievre for for-
of outliers laboratories, was taken as the certified data. Re- mally releasing this high-grade gold geochemical reference material
cently, Yan et al. [9] also adopted the similar method for during January, 2006 at NPL, New Delhi.
providing certified values for gold geochemical reference

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4. Ramesh SL, Sunder Raju PV, Anjaiah KV,
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Dasaram B, Nirmal Charan S, Subba Rao
DV, Sarma DS, Ram Mohan M, Balaram
V (2001) At Spectrosc 22:263–269
5. Taylor SR, McLennan SM (1988)
In: Gschneidner KA, Erving L (eds)
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(1995) Geostand Newsl 19:125–133

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