SAMPLE PREPARATION AND
ANALYTICAL METHODS
GEOCHEMISTRY, EXPLORATION AND MINING
Sample preparation and analytical methods
Geochemistry, exploration and mining
SAMPLE PREPARATION
4
BASE METAL ANALYSES
10
11
12
13
14
15
PRECIOUS METAL ANALYSES
16
19
20
21
ADDITIONAL ASSAYS
22
PETROLOGICAL ANALYSES
24
INDUSTRIAL MINERAL ANALYSES
28
CHARACTERIZATION OF WASTE
29
SAMPLE MANAGEMENT AND STORAGE
30
ABBREVIATIONS
REFERENCES
31
Rock samples
Automated Sample preparation
Sample preparation schemas Sample preparation methods Soil and sediment samples
Sample preparation methods Geochemical analyses Exploration analyses (non-mineralised samples)
Geochemical analyses Rare earth and other trace elements Base metal assays Ore grade analyses
Base metal assays One element assays
Base metal assays Oxide ore package for Iron and Uranium ores
Precious metal assays Geochemical analyses ( non-mineralised samples)
Precious metal assays Ore grade analyses
Special analyses for gold
Whole rock analysis Precious metals
Rare earth elements Individual determinations for whole rock analysis
Determination of hydrochloric acid soluble elements Determination of hydrochloric acid soluble elements and insoluble residue of the sample
Leaching tests
Acid Generation Potential Evaluation 3
4
6
7
8
9
9
25
25
26
27
28
28
29
29
32
SAMPLE PREPARATION
Rock samples
The objective of a precise sample preparation scheme is to produce a representative and meaningful test sample (regularly about 100 - 150 g) from a large bulk sample. The grain size of the prepared sample must be so
fine that the element of interest (or host mineral) can be properly liberated from the bulk matrix and distributed
in the pulp to produce a homogeneous distribution to ensure sufficient representativity for the following analytical methods. This is particularly important for low-concentration ores (e.g. Au and PGE’s) where the number of
mineral particles producing ore concentration is always low.
Different minerals behave differently during pulverisation – most (brittle) minerals will easily break down to
small particles while some (e.g. native gold) will just change their shape if proper sample preparation methods
are not used.
It is commonly accepted that poor sample preparation is, next to poor sampling, the largest source of bias in
an exploration or resource evaluation project. Sample preparation methods should therefore be selected as
carefully as the actual analytical methods.
Drying
All samples are always dried no matter what the earlier sample preparation history is (Method 10). Exceptionally wet and large samples (RC-, chip-samples etc.) require longer drying in elevated temperature (Method 14).
For routine sample preparation we recommend our automated sample preparation system.
Conventional, manual sample preparation (crushing, splitting, pulverizing) is available in our laboratories in
Rovaniemi, Kuopio, Espoo and Sodankylä
Crushing
The standard scheme consists of direct one–stage fine crushing using a special type jaw crushers (nominal
particle size > 70 % < 2 mm), precision riffle splitting (Method 31) and pulverising the split subsample of 100
–150g. This is a suitable method if crushed reject is needed for future work. The use of this method is meaningful to maximum size of 2000 g samples, because if more than 3 - 4 splittings are required the representativity
of the split subsample can not be assured. If larger than 2000 g samples are prepared using this procedure an
extra pre - crushing (Method 30) is invoiced.
For samples containing visible gold and/or for unusually big or heterogeneous samples, (max. 3,5 kg) we
recommend standard crushing to 5-10mm (Method 30) and followed by pulverising the entire test sample
(Methods 50) using Essa LM5 mills.
If crushed reject is required for future work the crushed material can be split to two (e.g. 1-2 kg) splits (riffle
splitting Method 35) – the other for storage and the other for pulverising (Method 50).
Pulverising
Pulverising will always cause unavoidable contamination of wear metals at trace level from the grinding surfaces. This contamination may vary depending on material of the bowl, hardness of the sample material,
4
SAMPLE PREPARATION
Some examples of bowl materials used at LABTIUM and expected contamination:
- carbon steel (< 0.2 % Fe, no base metals)
- hardened steel (< 0.2 % Fe, low Mn, Ni, Cu, Cr, Co)
- chrome steel (up to 200 ppm Cr, < 0.2 % Fe, traces Mn, Cu, Co)
- tungsten carbide (W, Co)
- agate (Si)
To minimise cross-contamination, cleaning of pulverising bowls between samples (pulverising with
barren quartzite) is included in the price in all Labtium pulverising methods. The pulverisers and jaw
crushers are cleaned with compressed air and brushes between every sample.
The standard scheme consists of direct one–stage fine crushing using a special type jaw crushers (Method 31
nominal particle size > 70 % < 2 mm), precision riffle splitting (Method 35) and pulverising the split subsample
of 100 –150g (Method 40).
For samples containing visible gold and/or for unusually big or heterogeneous samples, (max. 3,5 kg) we
recommend standard crushing (Method 30) and followed by pulverising the entire test sample (Methods 50,
hardened steel bowl) using Essa LM5 mills, avoiding any sample splitting which may deteriorate representativity of large samples. The pulverising takes place in large bowl and provides a large homogenised test sample
for representative subsampling directly from the bowl without any further sample handling. The grinding action
in LM5 is based on impact and hence smearing of gold particles (which are a problem with ring and disc mills)
on bowl surfaces is minimised, which is an addition advantage of the technique. The Method 50 is also suitable for pulverising RC (reverse circulation) samples and for percussion drill chip-samples, making crushing
and splitting unnecessary. If sample size exceeds 3,5 kg the sample must be pulverised by separate millings
and homogenised before subsampling to analytical sample. In this case additional charge is invoiced for each
kg exceeding 3,5 kg.
For high – precision whole rock analysis tungsten carbide pulverising must be used.
5
SAMPLE PREPARATION
Rock samples
Rock samples
Automated
Sample Preparation
Automated Sample Preparation
Labtium offers as a routine method for sample preparation of rock samples a totally automated sample
Labtium offers
routine method
for sample preparation of rock samples a totally automated sample prepapreparation
lineas
in a
Rovaniemi
laboratory.
ration line in Rovaniemi laboratory.
Through the use of a totally automated sample preparation system several benefits are attained. The
Through the (accuracy/repeatability)
use of a totally automated
sample
preparation
system that
several
areattained
attained.inThe
conconsistency
of the
process
is something
can benefits
never be
manual
sistency preparation
(accuracy/repeatability)
of the process
is something
thatcarrying
can never
manual
sample
sample
where a number
a different
people are
out be
theattained
work. in
Even
though
the
preparation
where
a
number
a
different
people
are
carrying
out
the
work.
Even
though
the
procedures
are
well
procedures are well documented and regulated the individuals do not carry out tasks exactly the same way
documented
and regulated
individuals
notcritical
carry out
tasks
exactly
theprocess,
same way
and humanthe
errors
are
and
human errors
are still the
possible.
The do
most
thing
in the
whole
maintaining
sample
still
possible.
The
most
critical
thing
in
the
whole
process,
maintaining
the
sample
representativity
during
the
representativity during the reduction of particle and sample size is carried out state-of –the-art rotary splitters.
reduction of particle
and
sizeissue
is carried
–the-art
rotary splitters.
Contamination
control
is a
Contamination
control
is sample
a profound
in theout
QCstate-of
of sample
preparation.
Also this
can be carried
out more
profound issue
in the QC ofinsample
preparation.
this
be segregation
carried out more
precisely
consistently
precisely
and consistently
automated
systems.Also
Loss
ofcan
fines,
of materials
byand
density,
shape
in automated
systems.
Losscross
of fines,
segregation of
materials
by density,
and size
of the particles,
cross
and
size of the
particles,
contamination
from
previous
sample shape
etc can
be minimized
by sealed
contamination
from
previous
sample
etc can
be
minimized
by
sealed
compartments
and
optimizing
the
system
compartments and optimizing the system parameters of e.g. slitters, controlled dedusting, cleaning of the
parameters
of e.g.surfaces.
slitters, controlled
dedusting,
cleaning
machine
working
Labtiumofconmachine
working
The Labtium
concept
utilizesofathe
unique
glass
bead surfaces.
blasting inThe
cleaning
the
cept
utilizes
a
unique
glass
bead
blasting
in
cleaning
of
the
pucks
and
bowls.
The
quality
of
the
cleaning
propucks and bowls. The quality of the cleaning procedure can also be monitored by human eye which is not
cedure can
also be monitored
by human eye
which
not possible
in flow-through
pulverizers. Surely
the
possible
in flow-through
type pulverizers.
Surely
theisincreased
capacity
will affecttype
the turn-around
times and
increased
capacity
will
affect
the
turn-around
times
and
also
cost-efficiency.
However
still
the
most
important
also cost-efficiency. However still the most important benefits are the improved working conditions - by
benefitsthe
areequipment
the improved
working
conditions
- by sealing
noise
exposure
to mineral staff
dust
sealing
noise
and exposure
to mineral
dust the
canequipment
be controlled
andand
minimized
. Laboratory
can
be controlled
andphysically
minimizedhard
. Laboratory
staff
is liberated
the physically
hard repetitive
work
to more
is
liberated
from the
repetitive
work
to more from
challenging
and versatile
work. The
benefit
of
challenging
and versatile
work.for
Thethe
benefit
sample preparation
the client
is shorter
robotized
sample
preparation
clientofisrobotized
shorter turnaround
time andforbetter
quality
control turnaround
in sample
time
and
better
quality
control
in
sample
preparation.
preparation.
The sample
sample preparation
preparationline
lineincludes
includes
The
- sample
logging
and recording
the sample
- sample
logging
and recording
the sample
weightweight
fine crushing
thesample
rock sample
to >70%
- fine- crushing
of theofrock
to >70%
<2mm<2mm
particleparticle
size size
- splitting
- splitting
with
a
rotary
splitter
to
a
1
1,5
kg
subsample
and a crushed
with a rotary splitter to a 1 - 1,5 kg subsample and a crushed
reject reject
- bagging
andcode
bar code
labelling
the crushed
- bagging
and bar
labelling
of the of
crushed
reject reject
- pulverizing
thesubsample
split subsample
bymills
LM2tomills
to >90%
<100µm
grain
sizelowusing
low- chrome
- pulverizing
the split
by LM2
>90%
<100µm
grain size
using
chrome
bowls bowls
- subsampling
the sample
to one
or ampoules
two ampoules
bar code
labelling
Assay
sample
if requested
- subsampling
the sample
to one
or two
withwith
bar code
labelling
andand
FireFire
Assay
sample
if requested
- cleaning
- cleaning
pulverizing
bowl
and
puck
with
efficient
glass
bead
blasting
after
every
sample
pulverizing bowl and puck with efficient glass bead blasting after every sample
- adding
theAssay
Fire Assay
the FA-subsample
and mixing
the mixture
- adding
the Fire
flux toflux
theto
FA-subsample
and mixing
the mixture
Maximum weight
weight of
of the
the sample
sample that
that can
can be
be prepared
in the
the unit
>4kg are
are
Maximum
prepared in
unit is
is 10
10 kg.
kg. However
However samples
samples weighing
weighing >4kg
subject
to
additional
charge.
Minimum
weight
of
the
sample
is
1
kg.
subject to additional charge. Minimum weight of the sample is 1 kg.
Additional ampoule
ampoulesubsample
subsamplecan
canbe
berepresentatively
representatively
split
e.g.
send
a second
laboratory.
Additional
split
e.g.
to to
bebe
send
to atosecond
laboratory.
Automated sample
preparation
Sample preparation of drill cores and rock
samples. Crushing , splitting, pulverizing
and subsampling
1 – 10kg
ROBO1
Sample preparation of percussion
samples (<5mm). Splitting, pulverizing
and subsampling
1 - 10kg
ROBO2
6
SAMPLE PREPARATION
Rock samples
Rock
samples
Sample
preparation schemas
Sample Preparation Schemas
Standard sample preparation
of rock samples (max 2000g)
Storing half
of original
sample
“Total” sample preparation of
rock samples (max 3500g)
ROCK SAMPLE
DRILL CORE
RC-SAMPLE
CHIP SAMPLE
ROCK SAMPLE
DRILL CORE
RC-SAMPLE
CHIP SAMPLE
Splitting by sawing
Splitting by sawing
o
Storing
coarse reject
Storing half
of original
sample
o
Drying at 70 C
Drying at 70 C
Labtium method code 10
Labtium method code 10
Jaw crushing (max 2.0 kg).
Fine jaw crusher.
Nominal > 70 % < 2 mm
Jaw crushing
Coarse jaw crushing.
Labtium method code 31
Labtium method code 30
Subsampling by riffle splitting
Pulverising the entire sample.
(max 3,5 kg);
LM5 mill; hardened steel
bowl.
Nominal > 90 % < 100 µm
Quartzite cleaning after every
samples
Labtium method code 35
Storing pulp
Labtium method code 50
Pulverising the split subsample
Ring mill; carbon steel bowl
Subsampling from the bowl
(100-150g)
Nominal > 90 % < 100 microns
(or by mat-rolling if requested
Quartzite cleaning after every
sample
(Labtium method code 36)
Labtium method code 40
Test sample in vial (100 – 150 g)
Test sample in vial (100 – 150 g)
Additionally riffle
rifflesplitting
splitting(35)
(35)can
canbebe
included
after
crushing
to
Additionally
included
after
crushing
to retain
retain
of the crushed
reject. However
coarse (30)
crushing
50%
of 50%
the crushed
reject. However
coarse crushing
has to(30)
be rehas to be
by fine
crushing (31).
placed
by replaced
fine crushing
(31).
7
SAMPLE PREPARATION
Rock samples
Sample
Sample preparation
preparation methods
methods
Preparation Method
Drying in forced air ovens
In stainless steel/aluminium
trays
Crushing by jaw crusher
Pulverising in ring mill
Quartzite cleaner included
Grain size of the pulp
> 90 % < 100 m
Maximum
weight
Labtium
method
Drying at 70 C
4000 g
10
Drying at < 40 C
o
4000 g
11
Sorting and drying of exceptionally large
o
or wet samples at > 100 C
(e.g. RC -or chip samples)
8000 g
14
Standard coarse crushing the whole
sample using Mn-steel jaws
4000 g
30
Fine crushing the whole sample using Mnsteel jaws to nominal > 70 % < 2 mm
2000 g
31
Pulverising the split sample in carbon
steel bowl
150 g
40
Pulverising the split sample in tungsten
carbide bowl (petrological samples)
150 g
43
3500 g
50
20 kg
51
Description
o
Pulverising the entire sample in hardened
steel bowl (LM5)
(e.g. Drill cores, RC - or chip samples)
Pulverising the entire sample in
continuous flow chrome steel bowl,
splitting by rotary splitter included
(e.g. RC-, chip or feasibility samples).
Cutting of drill cores and
rock samples
Sawing to two equal halves by diamond
saw, returning the other half to original
core case, packing the other half to plastic
bags or aluminium trays for further
processing
Core-logging facilities can be leased in Sodankylä for exclusive use on daily basis.
8
SAMPLE PREPARATION
Preparation Method
Miscellaneous Sample
Preparation
Maximum
weight
Description
Labtium
method
Separate splitting /subsampling by riffle
splitter (max 5 splittings) to 100 - 150 g
subsample.
4000 g
35
Separate homogenisation / subsampling
by mat-rolling to 100 - 150 g subsample.
4000 g
36
Separate splitting / subsampling by rotary
splitter.
4000 g
37
Wet sieving to 100 m, (QC for
pulverising) and weighing the +100 m
200 g
28
Compositing / homogenising large pulps in
rotary mixer
50 kg
Soil and sediment samples
Sample preparation methods
For soil samples (e.g. till), we recommend drying at 110 °C (Method 10) and sieving to < 0.06 mm fraction
(Method 24). If mercury or other volatile components are to be determined, lower drying temperatures must
be used. High drying temperatures may also cause oxidation of some minerals. Other sieve fractions (<
0.125, < 0.25, < 0.5 mm) can be used upon client’s request. When requesting sieving, please indicate the
fraction to be analysed. If coarse sieve fractions are used for analysis, additional pulverizing is regularly
required (Method 40).
For some purposes, the entire soil sample (weathered bedrock) or a coarse sieved fraction of the sample
can also be crushed and/or pulverised.
Preparation Method
Description
Drying in permeable
bags* in forced air
ovens
Drying at 70 C
Sieving with nylon
sieves
Pulverising in ring mill
Maximum
weight
Labtium
method
o
2000 g
10
Drying at 40 C
o
2000 g
11
Sieving to < 0.06 mm fraction
1000 g
24
Sieving to a fraction selected by the
client
1000 g
27
150 g
40
Pulverising the split sample in carbon
steel bowl
9
BASE METAL ANALYSES
SAMPLE ANALYSIS
Base metal assays
analyses
To obtain the best quality and cost-efficiency in a particular geological project it is important to decide the
strategy of analysis by selecting the appropriate analytical methods (element suit, digestion / pretreatment
method, detection limits, optimum measurement area etc.) to fit the objectives of the project. Selecting a
wrong method may end up in attaining optimised results in wrong concentration levels and introducing
problems in laboratory
(contamination, additional sample dilutions) which may deteriorate accuracy and
precision.
Methods
The specialists of laboratory will also assist you in selecting the optimised methods of analysis for your project.
For geochemical exploration for the base metals, we recommend aqua regia digestion of the sample and multielement analysis by ICP-OES (Method 511P). The package can be upgraded by ICP-MS- analysis to include
larger set of elements and lower detection limits (Method 511PM).
Although aqua regia is a powerful leaching agent, it still produces a partial dissolution for many elements. The
dissolution of silicates and refractory minerals (e.g. baryte, chromite and other spinelles, zircon, cassiterite,
tourmaline) varies depending on various factors. Most of the sulphide and oxide minerals (ore forming minerals)
are, however, dissolved. The data will also give information on alteration and weathering of rock and till samples.
Method 510P is an economic choice when only ore forming base elements are of importance. The method is
suitable for mineralised samples with moderate grades. There are limitations in the solubility of Ag and Pb at
high concentrations, and samples expected to contain more than 5 % of sulphur should be analysed for sulphur
using an alternative method (e.g. by combustion technique, S-analyser, Method 810L).
Rare elements including rare earth elements can be analysed using multi-acid total digestion and ICP-OES and
ICP-MS –analysis (307P/M).
Refractory ore minerals (e.g. chromite, magnetite, ilmenite, columbite, cassiterite etc.), high-grade base
metal ores (e.g. Ni ores) and concentrates can also be analysed using alkaline peroxide fusion and multielement analysis by ICP-OES (720P) or XRF-analysis (179X).
When high quality assays of base metals is required more representative subsamples and traditional highprecision procedures either by ICP-OES (514P) as a multi-element package or by FAAS (514A) using single
element methods can be used. Single-element (or selected multi-element) assays using a total analysis by
sodium peroxide fusion is carried out using the method 721P. Results close to total are obtained also for
major elements (except Si). Methods 720P and 721P can be applied also to mineral samples and
concentrates.
10
BASE METAL ANALYSES
Geochemical analyses.
Exploration analyses (non-mineralised samples).
Decomposition
pretreatment
method
Aqua Regia
Digestion
Determination
ICP-OES
The basic package of
511P using ICP-OES
can be upgraded by
ICP-MS analyses to
package 511PM
ICP-MS
Sample
weight
0.15 g
Elements
Detection
limit (ppm)
Ag
Al
As
B
Ba
Be
Ca
Cd
Co
Cr
Cu
Fe
K
La
Li
Mg
Mn
Mo
Na
Ni
P
Pb
S
Sb
Sc
Sr
Ti
V
Y
Zn
Zr
1
20
10
5
1
0.5
50
1
1
1
1
50
200
1
1
50
1
2
50
3
50
10
20
20
0.5
0.5
1
1
0.5
1
1
Ag
Be
Bi
Ce
In
Mo
Sb
Se
Te
Th
U
W
Yb
0.01
0.05
0.01
0.02
0.02
0.01
0.03
0.05
0.006
0.05
0.05
0.05
0.02
11
Labtium
method
511P
31 elements
511PM
Combined
40 elements
BASE METAL ANALYSES
Geochemical analyses.
Rare earth and other trace elements.
Determination
Decomposition
pretreatment method
HF-HClO4-digestion
ICP-MS
Sample
weight
0.2 g
Package A
Package B
0.2 g
Elements
Detection
limit (ppm)
As
Ba
Be
Bi
Cd
Co
Cr
Cu
Li
Mo
Ni
Pb
Rb
Sb
Sn
Sr
Ti
Tl
V
Zn
0.5
2
0.5
0.1
0.1
0.2
4
2
6
0.6
4
1
0.2
0.1
2
3
10
0.1
0.5
10
Ce
Dy
Er
Eu
Gd
Ho
La
Lu
Nd
Pr
Sm
Sc
Tb
Th
Tm
U
Y
Yb
0.15
0.1
0.15
0.05
0.15
0.05
0.1
0.05
0.25
0.05
0.2
0.3
0.05
0.4
0.05
0.1
0.1
0.1
.
12
Labtium
method
307P/M
BASE METAL ANALYSES
Base metal assays
Ore grade analyses
Decomposition
pretreatment method
Aqua Regia Digestion
Decomposition
pretreatment method
Sodium peroxide
fusion
Determination
ICP-OES
Determination
ICP-OES
Sample
weight
0.15 g
Sample
weight
0.20 g
Elements
Ag
As
Cd
Co
Cr
Cu
Fe
Mn
Mo
Ni
Pb
S
Sb
Zn
Elements
Al
As
Ca
Co
Cr
Cu
Fe
K
Mg
Mn
Mo
Ni
P
Pb
S
Sb
Ti
V
Zn
13
Detection
limit (ppm)
1
10
1
1
1
1
50
1
2
3
10
20
20
1
Detection
limit (%)
0.01
0.01
0.01
0.001
0.003
0.002
0.01
0.05
0.02
0.001
0.005
0.005
0.05
0.01
0.02
0.01
0.01
0.005
0.005
Labtium
method
510P
14 elements
Labtium
method
720P
19 elements
BASE METAL ANALYSES
Base metal assays
One element assays
Decomposition
Determination
pretreatment method
Aqua Regia
Digestion
Sodium peroxide
fusion
Sample
weight
Elements
Detection
limit (%)
Labtium
method
FAAS
1.0 g
Ag
As
Cd
Co
Cu
Ni
Pb
Zn
1 ppm
0.05
1 ppm
0.01
0.01
0.01
0.01
0.01
514A
ICP-OES
1.0 g
Ag
As
Cd
Co
Cu
Ni
Pb
S
Zn
1 ppm
0.05
1 ppm
0.01
0.01
0.01
0.01
0.01
0.01
514P
(Package of
8 elements)
0.2 g
Al
As
B
Ba
Be
Ca
Co
Cr
Cu
Fe
K
La
Li
Mg
Mn
Mo
Nb
Ni
P
Pb
S
Sb
Sc
Sr
Ta
Ti
U
V
Y
Zn
0.01
0.01
0.01
0.05
0.001
0.01
0.001
0.003
0.002
0.01
0.05
0.003
0.005
0.02
0.001
0.005
0.02
0.005
0.05
0.01
0.02
0.01
0.002
0.001
0.01
0.01
0.01
0.005
0.002
0.005
ICP-OES
721P
Analyses of processed samples (concentrates and other metallurgical products etc.) on request.
Check also sulphide selective leaches for Ni-ores (additional assays).
14
BASE METAL ANALYSES
Base metals assays
Oxide ore package for Iron and Uranium ores
Decomposition
pretreatment method
Determination
Pressed powder pellets
XRF
Sample Elements Detection
weight
limit (ppm)
7.0 g
Al
Ba
Ca
Cd
Ce
Cl
Cr
Cu
F
Fe
K
La
Mg
Mn
Na
Nb
Ni
P
Pb
Rb
S
Si
Sr
Ta
Th
Ti
U
V
Y
Zn
Zr
15
100
20
30
30
30
60
30
20
200
100
30
30
200
30
500
7
20
60
30
10
60
100
10
30
10
30
10
30
7
20
10
Labtium
method
179X
(31 elements)
PRECIOUS METAL ANALYSES
Precious metal analyses
To obtain the best quality and cost-efficiency in a particular geological project it is important to decide the strategy of analysis by selecting the appropriate analytical methods (element suit, digestion / pretreatment method,
detection limits, optimum measurement area etc.) to fit the objectives of the project. To help this selection a
description of different strategic levels of analysis applied at is given. Selecting a wrong method may end up in
attaining optimised results in wrong concentration levels and introducing problems in laboratory (contamination, additional sample dilutions) which may deteriorate accuracy and precision.
Methods
In gold and PGE-exploration, both the careful selection of sample preparation method and the choice of analytical method (including the weight of analytical sample) are critical. Figure 2 shows the effect of the grain size of
nugget gold on sample weight for obtaining acceptable precision in gold analysis. We recommend carrying out
a pilot study with selected, typical samples of the specified mineralization at an early stage of a large resource
evaluation program. The mode of occurrence of gold can be studied using the so-called diagnostic leach and
screen fire assay. Replicate analyses of samples can be carried out to study which of the available analytical
techniques (and subsample weight) will give acceptable precision (e.g. < 5 %) for reliable resource evaluation.
Based on this data, a scheme of sample preparation and analysis can be selected for optimum accuracy and
precision. A tailored QA/QC-protocol for the project can be planned. The study will also provide information to
be used as baseline data for more thorough metallurgical tests.
Different pretreatment and preconcentration /separation methods are available (aqua regia digestion, fire assay, cyanide leach) combined with different methods of determination (FAAS; GFAAS; ICP-MS; ICP-OES;
gravimetric), each method having its benefits and limitations. Our specialists will assist in the selection of a
suitable analytical method.
In the geochemical exploration for the precious metals (Au, Pd and Pt), we recommend aqua regia leach,
followed by pre-concentration by Hg co-precipitation and analysis by GFAAS (Methods 520U and 521U; 5
g subsample) (Kontas et al.1990). Sub-ppb detection limits can be attained for Au and Pd giving meaningful
anomaly contrasts. Alternatively a larger sample weight of 20 g can be used (Method 522U). The methods are
subsample)
et al.1990).
Sub-ppb
can be
attained
for Au and
Pd rock).
giving meaningful
applicable to(Kontas
non-mineralised
samples
(till, detection
weatheredlimits
bedrock,
stream
sediments,
humus,
anomaly contrasts. Alternatively a larger sample weight of 20 g can be used (Method 522U). The methods
are
to non-mineralised
(till, weathered
streamforsediments,
humus,
rock).
Theapplicable
use of pathfinder
elements in samples
geochemical
prospectingbedrock,
– particularly
gold is known
to give
more information of element dispersion in secondary environments and assist in the classification of the type of mineraliThe
useMany
of pathfinder
elements
in geochemical
prospecting
– particularly
gold is known
to givetomore
zation.
studies have
been carried
out at LABTIUM
to study
the elementfor
associations
connected
gold
information
of
element
dispersion
in
secondary
environments
and
assist
in
the
classification
of
the
type
mineralizations (e.g. Nurmi et al.1991, Eilu 1999). Nurmi et al. concluded that the most important elements of
in
mineralization.
Many studies
have beengold
carried
out are:
at Au,
LABTIUM
to Ag,
study
the Se.
element
exploration for Precambrian
mesothermal
deposits
Te, Bi, As,
W and
Figureassociations
3 shows the
connected
to gold
mineralizations
Nurmi to
et 41
al.1991,
Eilu
Nurmi Australian
et al. concluded
that themesomost
most important
pathfinder
elements(e.g.
connected
Finnish
and1999).
11 selected
and Canadian
important
elements
in exploration
mesothermal
deposits are: Au,offers
Te, Bi,forAs,
Ag,exploraW and
thermal gold
deposits
representedfor
asPrecambrian
enrichment factors
relativegold
to basalt. LABTIUM
gold
Se.
Figure
3 packing
shows the
most Au,
important
connected
41 Finnish
tion a
unique
including
Bi, Sb, pathfinder
Se and Te elements
(520U) with
ultra low to
detection
limits.and
This11setselected
can be
Australian
and Canadian
mesothermal
gold deposits option
represented
as enrichment
factorsusing
relative
to basalt.
complemented
by Methods
511P or 511PM. Another
is a multi-element
package
ICP-OES
and
LABTIUM
offers for
gold exploration
a unique
packing
Au, Bi,
Sb, Se Au,
andPd
Teand
(520U)
withultra-trace
ultra low
ICP-MS analysis
(515PM).
This package
will give
totallyincluding
42 elements
including
Pt with
detection
limits.limits.
This set can be complemented by Methods 511P or 511PM. Another option is a multilevel detection
element package using ICP-OES and ICP-MS analysis (515PM). This package will give totally 42 elements
including Au, Pd and Pt with ultra-trace level detection limits.
Note that these methods are not suitable for mineralised samples.
60
16
Se. Figure 3 shows the most important pathfinder elements connected to 41 Finnish and 11 selected
Australian and Canadian mesothermal gold deposits represented as enrichment factors relative to basalt.
METAL
LABTIUM offers for gold exploration a unique packing includingPRECIOUS
Au, Bi, Sb, Se and
Te (520U)ANALYSES
with ultra low
detection limits. This set can be complemented by Methods 511P or 511PM. Another option is a multielement package using ICP-OES and ICP-MS analysis (515PM). This package will give totally 42 elements
including Au, Pd and Pt with ultra-trace level detection limits.
Note that these methods are not suitable for mineralised samples.
Number of deposits
60
50
40
30
20
10
0
Au Te S As W Bi Ag Se Sb B Mo Cu U Hg Pb Sn Cr Co Tl Ni Zn
Enrichment relative to basalt
> 1000
1000 - 100
100 - 0
Figure 1. Frequency and contrast of concentrations (relative to background) of elements enriched in
mesothermal gold deposits (Nurmi et al.1991).
The Method
using
20 g subsample,
is best
suited
for prospecting or for preliminary ore assay. In some
Method
521U522U,
or 522U
is a
recommended
for low
level
Au-analyses.
cases, depending on the mineralogy of the sample, the aqua regia leach may give slightly lower recoveries
for Au
as compared
with fire
(Juvonen is& best
Kontas
1999).
Information on
highpreliminary
graphite content,
which
The
Method
522U, using
a 20assay
g subsample,
suited
for prospecting
or for
ore assay.
In
interferes
in the
aqua regia
procedure, should
be conveyed
to theregia
laboratory.
of some
some
cases,
depending
onleach
the mineralogy
of the sample,
the aqua
leach Also
may dissolution
give slightly
lower
PGE-minerals
to aqua
recoveries
for isAunotascomplete
compared
with regia.
fire assay (Juvonen & Kontas 1999). Information on high graphite
content, which interferes in the aqua regia leach procedure, should be conveyed to the laboratory. Also
Ore grade assays
gold and the is
platinum
metalstoare
performed
dissolution
of someofPGE-minerals
not complete
aqua
regia. by a high-precision classical Pb fire assay
method using either 25 g or 50 g subsamples (704/705), combined with alternative finishes (FAAS, ICP-OES,
gravimetric). If only Au (or Pd/Pt) is to be analysed, we recommend the Method 704A (or 705A) where Au is determined by FAAS. If, however, Au, Pd and Pt are to be analysed we recommend the Method 704P (or 705P).
When Rh content is required, Method 708P (or 708A) can be applied. Combined with method 705A (Au) – Au,
Pd, Pt and Rh can be analysed. Request for a quotation. Special precautions need to be taken if samples
contain appreciable amounts of graphite, S, As, Te, Se, Ni, Cu. For sample with high concentrations of these
metals smaller subsample weight may have to be used deviating from the original request.
Gravimetric determination after the fire assay (705G) gives the best precision and accuracy for high-grade (50
–1000 ppm) gold samples and low-level concentrates. For high-level concentrates use the methods 741G and
742G.
When all six of the PGE are to be analysed, the method of choice is the NiS fire assay (714M). Our method
includes Te coprecipitation for better Au recovery (Juvonen et al. 1994). Detection limits at the ppb range are
obtained by our ICP-MS determination. Osmium is an optional element in this method and should be specified
in the request for analysis. The routine method sample weight is 15 g, but alternative sample weights can be
used.
17
PRECIOUS METAL ANALYSES
As a routine method for cyanide soluble gold we recommend Labtium method 236A which involves the use
of PAL1000 –machine. The method enables the simultaneous pulverizing and cyanide leach of crushed rock
samples, percussion samples or soil samples. A 0,500 kg subsample can be used. The leaching is very effective due to aggressive leaching conditions which promote the liberation and breaking of gold nuggets. Graphite, organic matter (humus) and sulphides interfere in the cyanide leach, lowering the recovery of gold.
The concentration of cyanide soluble free gold may also be evaluated using the sodium cyanide leach method.
The traditional 3 hour tumbling with the LeachWELL accelerator (235A). A large, representative subsample
(0.5 kg) can be used. Combined with pulverising of total sample (sample preparation Method 50) the method
is the best possible routine method in the case of coarse-grained gold for grade control and resource evaluation samples (e.g. RC-samples, chip samples). The results attained by this partial extraction are comparable to
technical CIP- and CIL- extraction techniques and are of benefit in the metallurgical testing of the mineralisation. The method is not suitable when the total content of gold is needed.
Additional methods for gold analysis include screen fire assays for coarse grained gold, diagnostic leaches to
evaluate mode of occurrence of gold in different mineralogical phases and analysis of the ”total gold”, which
includes cyanide leach and analysis of the tailing (and head, if requested) sample by fire assay.
The most suitable analysis method for silver is by acid digestion with aqua regia and finish with FAAS
(511A/514A) or ICP-OES (510P/514P; see base metals). However, there are potential limitations in the solubility of Ag in high concentrations (Ag > 100ppm). Fire Assay and gravimetric finish (705G) with a more representative sample and better precision can be used for ore grade samples (Ag > 50ppm). In addition metallic
silver can be analysed with cyanidation methods 235A and 236A as gold.
PAL1000 for simultaneous pulverising and cyanide leach of 0,5 kg subsample
18
PRECIOUS METAL ANALYSES
Precious metal assays
Geochemical analyses (non-mineralised samples)
Decomposition
pretreatment method
Determination
Aqua Regia Leach
GFAAS
Sample
weight
Elements
Detection
limit (ppm)
5g
Au
Bi
Sb
Se
Te
0.5ppb
2ppb
5ppb
5ppb
2ppb
520U
5g
Au*
Pd*
Te
0.5ppb
0.5ppb
2ppb
521U
5g
Ag
Al
As
Au
B
Ba
Be
Bi
Ca
Cd
Co
Cr
Cu
Fe
K
La
Li
Mg
Mn
Mo
Na
Ni
P
Pb
Pd
Pt
S
Sb
Sc
Se
Sn
Sr
Te
Ti
Th
Tl
U
V
W
Y
Zn
Zr
Hg-coprecipitation
Aqua Regia digestion
ICP-OES and
ICP-MS
0.01
15
0.05
0.5ppb
5
1
0,5
5ppb
50
0.01
0.1
1
1
50
100
1
1
10
1
0.01
50
1
50
0.01
0.5ppb
0.5ppb
20
2ppb
0,5
5ppb
0.1
1
2ppb
1
0,01
5ppb
0.01
1
0.05
0.5
1
1
Labtium
method
515PM
42 elements
*Analyses of Au, Pd and Pt at sub-ppb levels in organic samples (vegetation, humus etc.) based on quotation.
19
PRECIOUS METAL ANALYSES
Precious metal assays
Ore grade analyses
Determination
Decomposition
pretreatment method
Aqua Regia Leach
Sample
weight
Labtium
method
20 g
Au
Pd
Pt
Te
0.01
0.01
0.02
0.01
522U
FAAS
25 g
Au
Pd
Pt
0.05
0.05
0.1
704A
50 g
Au
Pd
Pt
0.02
0.02
0.05
705A
50 g
Rh
0.01
708A
25 g
Au
Pd
Pt
10 ppb
10 ppb
10 ppb
704P
50 g
Au
Pd
Pt
5 ppb
5 ppb
5 ppb
705P
50 g
Pd
Pt
Rh
5 ppb
5 ppb
5 ppb
708P
15 g
Au
Pd
Pt
Rh
Ir
Ru
(Os
0.5 ppb
1 ppb
0.1 ppb
1 ppb
0.1 ppb
2 ppb
1 ppb)
714M
ICP-OES
NiS-Fire Assay
Detection
limit (ppm)
GFAAS
Hg-coprecipitation
(Preroasting
Included)
Pb-Fire Assay
Elements
ICP-MS
Te-coprecipitation
Optional
PAL1000-analysis.
Pulverizing of <2mm
sample and Cyanide
Leach
FAAS
0.5 kg
Au
Ag
Cu
0.05
0.1
1
236A
Cyanide Leach
3 h accelerated
FAAS
0.5 kg
Au
Ag
0.05
0.1
235A
20
PRECIOUS METAL ANALYSES
For the analyses of high grade ores and low-level concentrates ( > 50 ppm – 1000 ppm) we recommend Pb-Fire
Assay with gravimetric finish. High level Ag can be combined with FAAS/ICPOES determination of Au. Analyses
of Ag see also Base Metals (methods 510/514P).
Pb-Fire Assay
Gravimetric
50 g
Au
or
Ag
Pb-Fire Assay
Gravimetric
and
FAAS/ICPOES
50 g
Ag
and
Au
2 ppm
5 ppm
705G
2 ppm
705G
0,01ppm
705A/P
Special analyses for gold
Concentrates (e.g flotation concentrates)
Pb-Fire Assay (sample weight varies 5 - 30 g) with gravimetric finish.
Includes sample preparation and representative subsampling using
precision rotary splitter.
Concentration range 100 – 100 000 ppm .
740G
High grade concentrates
Pb-Fire Assay (sample weight varies 5 - 30 g) with gravimetric finish.
Includes sample preparation and representative subsampling using
precision rotary splitter.
Concentration range >10% Au
741G
Commercial assays, bullion and umpire assays
742-743G
Screen Fire Assay for coarse gold
Sieving of a 0.5 kg subsample with a 125 µm (120 mesh) sieve.
Weighing each fraction.
Fire assay ( Method 705A ) of the entire + 125 µm fraction.
Duplicate Fire assay ( Method 705A ) of - 125 µm fraction.
Calculation of weighted concentrations of gold (total and fractions).
Total gold
Cyanide leach of a 0.5 kg subsample ( Method 235A or 236A ).
Washing, neutralising and homogenising the tailing.
Duplicate Fire Assay ( Method 705A ) of the tailing.
21
ADDITIONAL ANALYSES
ADDITIONAL ASSAYS
Additional analyses
When the ore forming mineral is exceptional or when total concentrations for geochemical or petrological studies
When the ore forming mineral is exceptional or when total concentrations for geochemical or petrological stud(trace levels of elements) are required, please contact the laboratory for assistance in selecting the best possible
ies (trace levels of elements) are required, please contact the laboratory for assistance in selecting the best
digestion/
pretreatment
method formethod
your purpose
total (e.g.
digestion
307P/M,
Method
175X;
see
possible digestion/
pretreatment
for your(e.g.
purpose
totalMethod
digestion
MethodXRF
307P/M,
XRF
Method
Whole
RockWhole
Analysis;).
175X; see
Rock Analysis;).
The XRF
a versatile
tooltool
in the
of theof
base
(Method(Method
175X). For
moreFor
informaThe
XRF technique
techniqueisisalso
also
a versatile
in analysis
the analysis
themetals
base metals
175X).
more
tion on the XRF technique see the section on Petrological Analyses.
information on the XRF technique see the section on Petrological Analyses.
In addition to classical geochemical methods, a selection of selective leaches (using water extraction, ammoIn addition to classical geochemical methods, a selection of selective leaches (using water extraction,
nium acetate, pyrophosphate etc.) combined with ICP-MS-analysis is also available for geochemical exploraammonium acetate, pyrophosphate etc.) combined with ICP-MS-analysis is also available for geochemical
tion of buried ore deposits. The set of elements is comparable to method 511MP or 515MP.
exploration of buried ore deposits. The set of elements is comparable to method 511MP or 515MP.
Elements in specific mineral phases of the sample can also be determined, such as Ni in the sulphide phase
or elements
in the carbonate
phase of
of the
the sample
sample. Elements
in specific
mineral phases
can also be determined, such as Ni in the sulphide phase or
elements in the carbonate phase of the sample.
Special methods are available e.g. for the determination of mercury, total sulphur and carbon (Combustion;
Method 810L) or sulphur and carbon mineral phases.
Special methods are available e.g. for the determination of mercury, total sulphur and carbon (Combustion;
Method 810L) or sulphur and carbon mineral phases.
Volatiles
Decomposition
pretreatment
method
Determination
Combustion
technique
Hg -Analyzer
Ignition
Combustion
technique
Sample
weight
0.1 g
Gravimetric
S/C-Analyzer
1g
0.2 g
Elements
Hg
Loss on ignition
o
at 1000 C
S
C
Detection
limit
Labtium
method
0.005 ppm
822L
0.01 %
813G
0.01 %
0.01 %
810L
811L
Determination of carbonate carbon and non-carbonate carbon
Combustion
technique
Treatment with HCl
C-Analyzer
0.5 –
1.0 g
C-tot.
C-carb.
C-noncarb.
22
100 ppm
100
100
811L
816L
ADDITIONAL ANALYSES
Base metals in sulphides
Decomposition
pretreatment
method
Determination
Ammonium CitrateH2O2 - leach
ICP-OES
Bromine-Methanolleach
FAAS
Sample
weight
Elements
Detection
limit
Labtium
method
0.15 g
Cu
Ni
Co
Fe
S
10 ppm
10 ppm
10 ppm
100 ppm
50 ppm
240P
0,15 g
Cu
Ni
Co
Fe
5 ppm
250P
Comparison of the leaching efficiency of different digestion methods in the analysis of ultramafic
rock samples with varying contents of sulphide- and silicate-Ni.
2500
2000
Ni (ppm)
Ammonium citrate+H2O2-leach
Ascorbic acid+H2O2-leach
1500
Digestion w ith 7M nitric acid
Aqua regia digestion
Peroxide fusion
1000
Bromine+methanol
500
K
J
I
H
G
F
E
D
C
B
A
0
Other parameters
Specific gravity
Gas
pycnometer
Magnetization
Satmagan
3
SG
0,01g/cm
830G
Fe3O4
0,01%
891G
23
PETROLOGICAL ANALYSES
Petrological analyses
PETROLOGICAL
ANALYSES
Whole rock analyses are carried out using high precision methods applying state-of–the-art instrumentation
(XRF, ICP-OES, ICP-MS).
Major, minor and many trace elements are determined by XRF. Determinations are made on pressed
powder pellets (Method 175X). The XRF analysis can be supplemented by determination of the rare earth
elements (Method 307M, package B) and other trace elements by ICP-MS and/or ICP-OES after the total
digestion of the sample (package A). PGE at low concentration levels (Method 714M) can be included for
petrological studies. Carbon (Method 811L) and loss on ignition (Method 813G) are recommended for
complete whole rock analysis. Individual determinations, which are often required in whole rock analysis,
+
such as iron (II), fluoride, H2O and H2O , are also available.
The XRF method is applicable to rocks and soil samples, such as sand, gravel, till and sediments. Technical
products and ash of similar composition can also be analysed. The prerequisite for applicability of the XRF
method is that the chemical composition of the sample remains unchanged during the fine grinding (< 10 m)
as the pressed powder pellet is prepared. Samples containing > 20 % S cannot be analysed by this method.
24
PETROLOGICAL ANALYSES
Whole rock analysis
Decomposition
pretreatment method
Determination
Pressed powder pellets
XRF
Sample Elements Detection
weight
limit (ppm)
7.0 g
Determination of
carbon is also
recommended
(Method 811L).
Al
As
Ba
Bi
Ca
Ce
Cl
Cr
Cu
Fe
Ga
K
La
Mg
Mn
Mo
Na
Nb
Ni
P
Pb
Rb
S
Sb
Sc
Si
Sn
Sr
Th
Ti
U
V
Y
Zn
Zr
100
30
20
30
50
30
100
30
20
200
30
50
30
200
40
10
500
10
20
60
30
10
100
30
30
100
30
10
10
30
10
30
10
20
10
Labtium
method
175X
Precious metals
Determination Sample
Decomposition
weight
pretreatment method
NiS-Fire Assay
Te-coprecipitation
ICP-MS
15 g
Elements
Au
Pd
Pt
Rh
Ir
Ru
(Os
25
Detection
limit (ppb)
0.5
1
0.1
1
0.1
2
1)
Labtium
method
714M
Optional
PETROLOGICAL ANALYSES
Rare earth elements
Decomposition
pretreatment method
HF-HClO4-digestion
Lithium metaborateSodium perborate
fusion
Determination
ICP-MS
Sample
weight
0.2 g
Elements
Detection
limit (ppm)
Ce
Dy
Er
Eu
Gd
Ho
La
Lu
Nd
Pr
Sm
Tb
Tm
Yb
Sc
Y
U
Th
0.1
0.1
0.15
0.1
0.15
0.1
0.1
0.1
0.2
0.1
0.2
0.1
0.1
0.15
0.5
0.1
0.2
0.5
Labtium
method
308M
Additional elements:
Co
Hf
Nb
Rb
Ta
V
Zr
0.5
0.5
0.2
0.2
0.2
0.5
0.5
308M
For other elements contact laboratory
26
PETROLOGICAL ANALYSES
Individual determinations for whole rock analysis
Decomposition
pretreatment method
Ignition
Combustion
technique
Acid digestion
Determination
Sample
weight
Elements
1g
LOI
Loss on
ignition
o
1000 C
0.01
813G
0.01
0.01
815L
Gravimetric
Detection
limit (%)
Labtium
method
H2O analyzer
0.5 g
Moisture
Cryst.water
Titrimetric
0.5 g
Fe
0.02
301T
Potentiometric
0.1 g
F
-
0.01
725I
2+
HF - H2SO4
NaOH-fusion
27
INDUSTRIAL MINERAL ANALYSES
INDUSTRIAL MINERAL ANALYSES
Determination of hydrochloric acid soluble elements
(Recommended method)
Decomposition
pretreatment method
Hydrochloric acid
digestion
Determination
ICP-AES
Sample
weight
0.1 g
Elements
Al
Ca
Mg
Fe
Mn
Detection
limit (ppm)
200
600
150
150
2
Labtium
method
407P
Determination of hydrochloric acid soluble elements and
insoluble residue of the sample
Decomposition
pretreatment method
Hydrochloric acid
digestion
Determination
Sample
weight
ICP-AES
1.0 g
Gravimetric
1.0 g
Elements
Al
Ca
Mg
Fe
Mn
Insoluble
residue
28
Detection
limit (ppm)
Labtium
method
200
400
100
100
1
406P
0.3 %
406G
CHARACTERISATION OF WASTE
CHARACTERISATION OF WASTE
Leaching tests
Compliance test for leaching of granular waste materials and sludges
EN 12457-1
EN 12457-2
EN 12457-3
EN 12457-4
Leaching behaviour test. Up-flow percolation test
CEN/TS 14405
pH and EC
EN 12506
Element analyses by ICP-OES and ICP-MS
EN 12506
Hg
EN 17852
Anions
EN 12506
EN 13370
TDS
EN 15216
DOC
EN 13370
Acid Generation Potential Evaluation
Acid–Base Accounting (ABA). Static test for sulfidic waste.
Neutralisation Potential, NP
Draft:
CEN/TC WI292053
Acid Potential, AP
Neutralisation Potential Ratio, NPR
Net Neutralisation Potential, NNP
Net Acid Generation (NAG)
AMIRA
ARD Test Handbook
Single NAG
Australia
Sequential NAG
pH
EN 12506
Total Sulfur (pyrolysis)
ISO 15178
Total Carbon (pyrolysis)
CEN15104
Carbonate Carbon
EN 13137 (Mod.)
29
SAMPLE MANAGEMENT AND STORAGE
SAMPLE
MANAGEMENT
STORAGE
Sample management
andAND
storage
Systematic and well-organised sample archiving is not always thought to be included in the quality
management of an exploration project. Good archiving helps the future retrieval of samples for e.g. feasibility
testing and replicate or umpire analysis. During future audits of the project, well organised archiving is one of
the fundamental issues. At Labtium special attention is paid on labelling and storing of all materials. The
laboratory samples are placed in plastic ampoules and stored in impact resistant styrofoam cases. Pulps and
/or rejects are stored in sealed plastic bags in pallets. All the packing materials except for pallets are
included in the prices.
Sample batch reception (901) includes checking the sample numbering, sorting etc. and packing materials.
The cost for long term storage of drill cores, rejects and pulps (906) and laboratory samples in vials (907)
can be negotiated.
If the client does not want the rejects and pulps to be returned a waste management levy is invoiced (902).
The disposal of hazardous materials is invoiced on costs (903).
If sample batches are arriving in the laboratory highly disorganised the laboratory is forced to invoice also the
reorganising of the field samples (904). Also if the sample bags or containers are damaged, the replacement
of the samples to new containers has to be invoiced (905).
Reception fee for a batch of samples
901
902
Waste disposal fee for reject sample materials
Disposal fee of hazardous wastes
903
Organising received disorganised samples
904
Removing samples from damaged/unsuitable containers to
new containers/bags
905
Storage of pulps/rejects after 1 months from reporting
906
Storage of laboratory samples after 1 months from
reporting
907
30
ABBREVIATIONS
Abbreviations
ABBREVIATIONS
Analytical
Analytical
technique
technique
Description
Description
GFAAS
GFAAS
Atomic
Atomic Absorption
Absorption Spectrometry,
Spectrometry, electrothermal
electrothermal atomisation
atomisation
U
U
FAAS
FAAS
Atomic
Atomic Absorption
Absorption Spectrometry,
Spectrometry, flame
flame atomisation
atomisation
A
A
CVAAS
CVAAS
Atomic
Atomic Absorption
Absorption Spectrometry,
Spectrometry, atomisation
atomisation by
by
Cold
Cold vapour
vapour generation
generation
H
H
XRF
XRF
Wavelength
Wavelength Dispersive
Dispersive X-ray
X-ray Fluorescence
Fluorescence Spectrometry
Spectrometry
X
X
ICP-OES
ICP-OES
Inductively
Inductively Coupled
Coupled Plasma
Plasma Optical
Optical Emission
Emission Spectrometry
Spectrometry
P
P
ICP-MS
ICP-MS
Inductively
Inductively Coupled
Coupled Plasma
Plasma Mass
Mass Spectrometry
Spectrometry
M
M
S/C-ANALYZER
S/C-ANALYZER
Combustion,
Combustion, IR-detection,
IR-detection, Sulphur
Sulphur or
or Carbon
Carbon analyser
analyser
L
L
Units
Units
-9
Labtium
Labtium code
code
-9
ng
g
ng =
= 10
10 g
-6
-6
g
g=
= 10
10 -3g
g
-3
mg
g
mg =
= 10
10 g
ppb
ppb =
= ng/g
ng/g =
= g/kg
g/kg =
= mg/t
mg/t
g/g
=
mg/kg
ppm
=
ppm = g/g = mg/kg =
= g/t
g/t
References
REFERENCES
Juvonen
Juvonen R.,
R., Kallio
Kallio E.
E. and
and Lakomaa
Lakomaa T.
T. (1994)
(1994) .Determination
.Determination of
of precious
precious metals
metals in
in rocks
rocks by
by inductively
inductively
coupled
coupled plasma
plasma mass
mass spectrometry
spectrometry using
using nickel
nickel sulphide
sulphide concentration.
concentration. Comparison
Comparison with
with other
other prepretreatment
treatment methods.
methods. Analyst119
Analyst119 (1994),
(1994), p.
p. 617
617 -- 621.
621.
Juvonen
Juvonen R.
R. and
and Kontas
Kontas E.(1999).
E.(1999). Comparison
Comparison of
of three
three analytical
analytical methods
methods in
in the
the determination
determination of
of gold
gold in
in
six
Finnish
gold
ores,
including
a
study
of
sample
preparation
and
sampling,
Journal
of
Geochemical
six Finnish gold ores, including a study of sample preparation and sampling, Journal of Geochemical
Exploration
Exploration 65
65 (1999)
(1999) 219
219 -- 229.
229.
Kontas
Kontas E.,
E., Niskavaara
Niskavaara H.
H. and
and Virtasalo
Virtasalo J.,
J., (1990).
(1990). Gold,
Gold, palladium
palladium and
and tellurium
tellurium in
in South
South African,
African, Chines
Chines
and
and Japanese
Japanese geochemical
geochemical reference
reference samples,
samples, Geostandards
Geostandards Newsletter,
Newsletter, 14(1990),
14(1990), 477
477 -- 478.
478.
Kontas
Kontas E.
E. (editor)(1993).
(editor)(1993). Analytical
Analytical methods
methods for
for determining
determining gold
gold in
in geological
geological samples,
samples, Geological
Geological Survey
Survey
of
of Finland,
Finland, Report
Report of
of Investigations
Investigations 114
114 (1993),
(1993), pp
pp 41.
41.
Niskavaara
Niskavaara H.
H. (1990).
(1990). Reductive
Reductive coprecipitation
coprecipitation as
as a
a separation
separation method
method for
for the
the determination
determination of
of gold,
gold,
palladium,
platinum,
rhodium,
silver,
selenium
and
tellurium
in
geological
samples
by
graphite
furnace
palladium, platinum, rhodium, silver, selenium and tellurium in geological samples by graphite furnace atomic
atomic
absorption
absorption spectrometry,
spectrometry, Analytica
Analytica Chimica
Chimica Acta,
Acta, 231(1990),
231(1990), 273
273 -- 282.
282.
Nurmi
Nurmi P.A.,
P.A., Lestinen,
Lestinen, P.
P. and
and Niskavaara,
Niskavaara, H.
H. (1991).
(1991). Geochemical
Geochemical Characteristics
Characteristics of
of mesothermal
mesothermal gold
gold
deposits
deposits in
in Fennoscandian
Fennoscandian Shield
Shield and
and a
a comparison
comparison with
with selected
selected Canadian
Canadian and
and Australian
Australian deposits.
deposits.
Geological
Geological Survey
Survey of
of Finland,
Finland, Bulletin
Bulletin 351,
351, Espoo
Espoo 1991,
1991, 101
101 pp.
pp.
31
ACCREDITATION
ACCREDITATION
Labtium Ltd. (formerly The Geolaboratory of the Geological Survey of Finland), is an
accreditaded testing laboratory. The accreditation according to ISO/IEC 17025 was
received
originally
1994 from the
Finnish
Accreditation
Service isFINAS
at the MIKES
Labtium
Ltd. (formerly
TheinGeolaboratory
of the
Geological
Survey of Finland),
an accreditaded
testing
(The
Centre
for
Metrology
and
Accreditation).
The
accreditation
code
of
Labtium
is
FINAS
laboratory. The accreditation according to ISO/IEC 17025 was received originally in 1994 from the Finnish
T025. Service
The FINAS
up-to-date
scope(TheofCentre
thefor Metrology
accreditation
can be The
found
in
Accreditation
at the MIKES
and Accreditation).
accreditahttp://www.finas.fi/Scopes/T025_M17_2008.htm
and
then
FINAS
service.
tion code of Labtium is FINAS T025. The up-to-date scope of the accreditation can be found in http://www.
finas.fi/Scopes/T025_M17_2008.htm and then FINAS service.
The FINAS accredited bodies may state in their reports and certificates that they are
accredited by FINAS, which is a signatory of the EA (European co-operation for
The FINAS accredited bodies may state in their reports and certificates that they are accredited by FINAS,
Accreditation),
ILAC
(International
Laboratory
Accreditation
Cooperation
which
is
a
signatory
of
the
EA
(European
co-operation
for
Accreditation),
ILAC
(International
Laboratory
http://www.ilac.org/) or IAF (International Accreditation Forum Inc.; http://www.iaf.nu/)
Accreditation
Cooperation
http://www.ilac.org/)
or IAF (International
Accreditation
Forum
Inc.; http://www.
recognition
agreement.
Thus a global acceptance
and recognition
of the
accreditation
and
iaf.nu/)
recognition
a global
acceptance and recognition of the accreditation and quality
quality
systemagreement. Thus
of Labtium Ltd is
achieved.
system of Labtium Ltd is achieved.
Labtium Ltd is continuously participating in independent, international proficiency tests in
the Ltd
mineral
sector runparticipating
by e.g. Geostats
Pty Ltd, international
Australia and
the GeoPT
by the
Labtium
is continuously
in independent,
proficiency
testssponsored
in the mineral
secInternational
Association
of
Geoanalysts
(IAG).
In
addition
Labtium
participates
in
tor run by e.g. Geostats Pty Ltd, Australia and the GeoPT sponsored by the International Associationaof
proficiency
testInfor
Canadian
accredited
mineral
testing laboratories
(CANMET
PTP-MAL).
Geoanalysts
(IAG).
addition
Labtium
participates
in a proficiency
test for Canadian
accredited
mineral
These
tests
are
used
to
evaluate
the
performance
and
validity
of
our
methods
in
testing laboratories (CANMET PTP-MAL). These tests are used to evaluate the performance and validity
comparison to other international mineral testing laboratories. The reports are available to
of our methods in comparison to other international mineral testing laboratories. The reports are available
clients on request.
to clients on request.
Juha Virtasalo
JuhaQuality
Virtasalo
Manager
Quality Manager
Labtium Oy / Betonimiehenkuja 4 FIN- 02150 Espoo FINLAND/ Tel: +358 10 653 8000
Labtium Oy / Betonimiehenkuja 4 FIN- 02150 Espoo FINLAND/ Tel: +358 10 653 8000
32
STANDARD SERVICE AGREEMENT 31.1.2008
1. APPLICABILITY AND DEFINITIONS
1. These terms apply to the services ordered by the client and provided by Labtium Oy (hereafter “Labtium”),
unless otherwise agreed in writing.
2. Hereafter “written” and “in writing” shall include
traceable / verifiable e-mails and other electronic communications.
2. TENDER
1. Labtium’s written tender is valid for one (1) month
from the date of issue, unless otherwise stated in
the tender.
3. AGREEMENT, ORDER AND ORDER
CONFIRMATION
1. An agreement comes into force when the client
and Labtium have signed a separate agreement,
when Labtium has confirmed an order or when the
client informs Labtium in writing that they accept the
binding tender submitted by Labtium.
2. Labtium shall at all times confirm orders in writing
and shall act according to order specifications, unless the client suggests changes to the order in writing and the parties agree on said changes before
assignment work is begun.
3. The agreement can’t be transferred to a third
party without the written consent of the other party.
This does not limit the right of Labtium to use the
services of subcontractors.
4. Any changes or additions to this agreement are
subject to approval, in writing, by both parties.
5. In the event that two or more contractual documents show conflicting or contradictory terms, their
order of precedence shall be: 1) written agreement,
2) order confirmation, 3) order, 4) tender, 5) general
terms and condition and 6) invitation to tender.
4. SAMPLE MATERIAL
1. Samples shall be delivered at the client’s expense
to a unit specified in the Labtium order confirmation or otherwise indicated in writing by Labtium.
Labtium is responsible for shipping samples between Labtium units, unless otherwise agreed. 2. The client is under an obligation to inform Labtium
of any potential health or safety hazards inherent
in the samples (radiation, particles that constitute
a health hazard etc.). Labtium reserves the right to
suspend sample processing and, if necessary, terminate this agreement, if any such hazard becomes
evident during the work.
3. The client is responsible for ensuring that sample shipments are properly marked and shipped in
appropriate packaging. Labtium reserves the right
to present a separate bill at an hourly rate for extra
work arising from damaged sample packages and/
or mixed up sample codes.
5. The parameter and uncertainty limits for the results of analyses and measurements reported by
Labtium are valid for the typical application areas
of the method in question as applied in Labtium’s
process work. Clients must check, to their own satisfaction, the applicability of said limits to their own
problem configuration or testing scheme.
6. Labtium shall keep the assay/test reports and
other material of the agreed assignment for a period
of three (3) years after termination of the agreement.
6. OWNERSHIP AND RIGHT OF USE
9. OTHER RIGHTS AND RESPONSIBILITIES
OF THE PARTIES
1. The client shall furnish Labtium with the necessary basic information and, for each separate assignment, such equipment and other resources as
agreed.
1. Any documentation given to Labtium in connection with sample material is the property of the client and shall be returned to them or destroyed on
instructions from the client after one (1) month of the
date of the assignment report. The cost of shipping
or disposal is borne by the client. Any storage in excess of one month is subject to agreement and a
separate charge.
2. The client has a right to monitor the progress of
the assignment.
2. When the assignment is completed and paid for
in full, the reports, assays and other documentation
become the exclusive property of the client.
4. The parties shall inform each other without delay
of anything that may jeopardise the carrying out of
the assignment or cause unforeseen costs.
3. Labtium use mainly their own methods for analyses, assays and tests. The methodology is the
exclusive property of Labtium. The client does not
have the right to divulge to a third party anything in
connection with assignment reports, apart from a
general description of the methodology.
5. Labtium shall complete the assignment in the
agreed period of time. Where no delivery time has
been agreed, the assignment shall be completed
without undue delay.
4. Where Labtium makes use of the client’s methodology, this is the exclusive property of the client and
the relevant documentation shall be returned to the
client or destroyed. Use of the client’s methodology
is always subject to a written agreement. Labtium
takes no responsibility for the applicability of the
client’s methodology. Labtium reserves the right to
decline to use methodology that they deem unsuitable for the assignment or unsafe.
5. Where Labtium pays part of the assignment
costs, Labtium’s rights to the results shall be determined in advance and separately in each case.
6. The expertise gained from assignments that form
part of research and development projects is the
property of the client and Labtium reserves the right
to use the professional skills and experience gained
from assignments in their business operations.
7. The ownership of any equipment procured for an
assignment and financed by the client, shall be subject to a separate agreement.
7. CHARGES AND BILLING
1. Unless the cost or service price has been otherwise agreed, Labtium shall charge the client for
the assignment or product as set out in the order
confirmation.
2. The cost estimate of the assignment is stated in
the order confirmation and is binding, unless sample
quantities or assignment parameters are changed
4. Unused sample material is the property of the cli- or the assignment is accepted on the basis of billing
ent and shall, as the client chooses, be returned to at an hourly rate. A separate bill shall be presented
them or destroyed after one (1) month of the date of for travel costs and other assignment-related costs.
the assignment report. The cost of shipping or disposal is borne by the client. Any storage in excess 3. Overtime shall be subject to a separate agreeof a month is subject to agreement and a separate ment. Where overtime or special arrangements are
charge.
necessary for reasons outside of Labtium’s control
or due to changes in assignment or additional work
5. Appropriate packaging materials, designed to ordered by the client, Labtium shall present a sepaprotect the client’s samples, are subject to a sepa- rate bill for added costs.
rate charge, unless otherwise agreed.
4. Should the nature of the assignment or the sched6. Labtium shall not be held responsible for dam- ule be changed, the assignment cost estimate and
age to the client’s samples stored on the premises of bill shall be reviewed correspondingly.
Labtium or their subcontractor unless the damage is
demonstrably caused by neglect on Labtium’s part. 5. In the event that the client and Labtium together
perceive material changes in the cost level during
5. REPORTS
an agreement period, the cost estimates and charges shall be correspondingly reviewed from that date.
1. All assignments include a written and signed report. Reports or parts thereof can be communicated 6. Payment is due on the due date given on the bill.
by e-mail, subject to separate agreement in each Overdue payment shall be subject to interest as set
case.
out in the Interest Act of Finland. Labtium reserves
the right to suspend work on the assignment if pay2. For reasons of confidentiality, reports will be sent ments are overdue and, if significantly overdue, to
to only one mailing address and one e-mail address terminate this agreement.
given in writing by the client.
8. CONFIDENTIALITY
3. Reports on assays and analyses produced by
Labtium may not be copied or used in whole or in 1. The parties undertake to treat as confidential any
part for the purpose of presenting said reports as information as well as business and trade secrets
issued by an accredited laboratory.
received from or learned about the other party.
4. Where a sample is not taken by Labtium, the results of the analysis concern only the specific sample, or part thereof, delivered to Labtium.
3. The client may not divulge any confidential information or business or trade secrets received from
or learned about Labtium in connection with the
assignment, nor use such information in their own
business operations.
2. Labtium may not release the results of an assignment or material connected thereto to a third party
unless so instructed in writing by the client.
3. The parties may establish a project organisation
for carrying out the assignment. The composition,
tasks and responsibilities of such a group, as well
as any changes, are subject to a separate agreement in writing.
6. Labtium shall assiduously and professionally perform the assignment as defined in the agreement
and shall take care that competent personnel is assigned to the work. Labtium takes full responsibility
for the work of a subcontractor.
7. Labtium reserves the right to extend the processing time of the assignment in the event that work is
delayed for reasons beyond the control of Labtium
or due to the action or neglect of the client.
8. If the performance of an assignment is altered,
delayed or interrupted due to the action or neglect of
the client, Labtium reserves the right to bill the client
for costs and damages arising thereof.
9. As an employer, Labtium is responsible for the
statutory social security, insurance and other costs
of their personnel, as well as industrial safety, wherever the assignment work is carried out.
10. Labtium is liable for any direct damage or loss
to the client arising from Labtium’s deliberate or
consequential mistakes or neglect. The client shall
be liable for any damage or loss suffered by a third
party as an unavoidable consequence of adherence
to the agreement and which, even with the exercising of all possible care and diligence, is outside the
control of Labtium.
11. The liability of Labtium, their representatives
and personnel, shall at all events be limited to the
amount paid to Labtium for the assignment. Labtium
shall not be liable for any indirect or consequential
damage or loss.
12. The expert opinions expressed by Labtium are
based on comparing the observations and materials at their disposal, as well as generally known
laws, regulations and instructions. Expert opinions
expressed by Labtium must not be taken out of context and must always be quoted in whole. Labtium
takes no responsibility for interpretations of expert
opinions or conclusions drawn from such opinions,
or for the actions taken by others on the basis of
such opinions.
13. Any claims on Labtium must be submitted in
writing within one (1) month from delivery of the assignment report or material to the client.
10. LIABILITY FOR RISK
1. The liability for the risk of accidental damage to
the assignment results is transferred to the client
at the time of delivery. If delivery is delayed by the
client, the liability for risk is transferred to the client
at the latest time delivery should have taken place.
11. QUALITY ASSURANCE, AUDITS
AND THIRD PARTY COMPARISON TESTS
1. Labtium is a FINAS-accredited test laboratory
(T025), which conforms to the ISO 17025 quality
system standard. Test and assay reports are issued
with the accreditation symbol and the report identifies which results have been gained using accredited process methods. When assay and test reports
are used as reference material, this information may
not be altered or omitted.
33
2. Labtium is audited by an official accreditation
organ. Audits of the client shall always be subject
to a written agreement and Labtium shall be given
the opportunity to comment the report. The audit
report may not be released to a third party without
Labtium’s written consent.
3. The results of comparison tests performed by
third parties may not be published without Labtium’s
written consent.
12. USING THE CLIENT’S NAME
AS A REFERENCE
1. Labtium reserves the right to use the client’s
name as a commercial reference, unless permission is expressly denied by the client. Such references shall not present information on the location
of the sample find or assignment volume data.
13. FORCE MAJEURE
1. A party shall be released from the obligations under this agreement and the liability to compensate
for damages in the event that the contractual obligations have been breached or neglected for reasons
beyond the control of the party. Sufficient grounds
for release from obligations under this agreement
arise in circumstances that are such that they could
not be foreseen when this agreement was concluded and are beyond the control of the parties and
the effects of which can’t be avoided or overcome
by reasonable means. Such circumstances include
war, insurrection, requisition or confiscation, embargo, natural disaster, suspension of transport or energy distribution, industrial dispute, fire, interrupted
communications or circumstances of a similar and
unusual nature beyond the control of the parties. A
delayed sub-contractor delivery or the bankruptcy of
a sub-contractor is also defined as force majeure.
2. If an obligation under this agreement is delayed
for any of the reasons given in 13.1, the time limit
given to perform the obligations is extended as far
as is reasonable in the circumstances.
14. TERMINATING THE AGREEMENT
1. Either party may terminate this agreement if the
other party materially fails to meet the obligations of
this agreement.
2. Should the client fail to meet the obligations of
this agreement, Labtium has the right to suspend
assignment work until it is determined whether the
breach of agreement shall be grounds for termination.
3. Labtium has the right to terminate the agreement
in the event that the client is obviously insolvent or
has entered into bankruptcy proceedings.
4. Both parties have the right to terminate the agreement in the event that the obligations under the
agreement become impossible to perform or are
delayed for more than six months by reason of force
majeure. Labtium reserves the right to terminate
the agreement, regardless of the aforementioned
time limit, if the delay is of material significance to
Labtium.
5. If the agreement is terminated, the client shall pay,
at the agreed rate, for such parts of the assignment
that have been completed and approved or, if the
parties consent to continue with the assignment
after the agreement is terminated, until the assignment work is completed.
6. If this agreement is terminated as a consequence
of the client’s action or neglect to perform an obligation, Labtium is entitled to compensation for the
costs and damage arising from termination of the
agreement.
15. DISPUTES
1. Any disputes arising from this agreement that the
parties are unable to settle by negotiation, shall be
tried in the Espoo District Court.
2. The interpretation of provisions of this agreement
and the settlement of disputes shall be based on
Finnish law in force at the time the agreement was
signed.
Labtium Oy/Ab/Ltd.
Business ID 2128301-1
tel. +358 10 65 38000
www.labtium.fi
E-mail: firstname.lastname@labtium.fi
Contacts:
Heikki Niskavaara
Lea Hämäläinen
Business area director. Geology, Exploration and Mining. +358 10 65 38601 Business Area director
Environment and Industry.
+358 10 65 38301
Espoo Raahe
Hanna Kahelin, Laboratory manager
+358 10 65 38103 Anitta Massinen, Laboratory supervisor
+358 10 65 38901
(Betonimiehenkuja 4)
PL 57 02151 ESPOO Rantakatu 4
92100 RAAHE
Kuopio Outokumpu
Susanna Arvilommi, Laboratory supervisor +358 10 65 38319 Pekka Parvinen, Laboratory supervisor
+358 10 65 38501
(Neulaniementie 5)
PL 1500
70211 KUOPIO (Tutkijankatu 1)
PL 45
83501 OUTOKUMPU
Rovaniemi Sodankylä
Auli Ojala, Laboratory supervisor +358 1065 38607
Anja Autio, Laboratory supervisor +358 10 65 38801
(Raidetie 1) (96900 SAARENKYLÄ)
PL 8601
96101 ROVANIEMI
(Poikajuntintie 34)
PL 97
99601 SODANKYLÄ