The range of geological samples includes soils, silts, lake and stream
sediments, rock, rock chips, drill core, percussion drill samples, panning
concentrates and vegetation. Many of these sample types may be large, wet and
heterogeneous. The purpose of sample preparation is to produce a smaller, dry
and manageable sample suitable for laboratory scale analysis while at the same
time ensuring that the prepared sample is homogeneous and fully representative
of the original field material. A reduction of particle size through crushing
and pulverizing is required for rock and drill core materials whereas it is
usually sufficient to sieve soil and sediment samples to obtain suitable
material for analysis.
It is essential that a geological sample be properly prepared prior to analysis.
At ALS we have always maintained that a poorly prepared sample is simply not
worth analyzing.
The risk of sample contamination is greater in the sample preparation process
than in any other section of the laboratory. It is essential that a clean work
environment be maintained through the enforcement of good work practices.
Routine cleaning of workstation surfaces and crushing and grinding machinery is
essential as is the use of a comprehensive dust control collection system.
Over the years ALS has developed its
exclusive, patented Dustbox technology to ensure efficient extraction of dust
during the sample preparation process. This technology provides sufficient
extraction to avoid cross contamination of samples, while at the same time
avoiding over-extraction of fine material. You can see the Dustbox in operation
at all of our sample prep laboratories around the globe.
One essential feature of ALS operations is our insistence on sample
classification and sorting according to sample type and expected metal
concentrations. In this way we can separate high grade and low grade samples and
reduce chances for cross contamination. Separate process lines are also
maintained for high and low grade samples to minimize the effects of carryover
within the sample preparation machinery. You, the client can help this process
further by making note of any expected high grade material in the relevant boxes
on the Sample Submission Form
Introduction
Geological samples are highly variable and encompass a broad range of sample
types that includes soils, silts, drill core, rocks and panning concentrates.
The purpose of sample preparation is to produce a small, dry and manageable
sample suitable for laboratory scale analysis while at the same time ensuring
that the prepared sample is homogeneous and fully representative of the original
field material. Experience has shown that the potential risk for contamination
is greater in the sample preparation process than in any other part of
laboratory operations. For this reason particular care and attention must be
paid to sample handling and there must be strict adherence to standard operating
procedures and good work practices. The physical plant facilities must be
designed for an orderly workflow, possess sufficient crushing and grinding
equipment to allow for specialized usage, and have a comprehensive dust control
system.
Sample Tracking System
ALS has developed a unique sample
tracking system that is an integral part of the company s new Laboratory
Information Management System (LIMS). This system utilizes bar coding and
scanning technology that provides, for the first time by any laboratory,
complete chain of custody records for every stage in the sample preparation and
analytical process.
Upon receipt of samples at any of the ALS worldwide locations, a bar code label
is attached to the original sample bag. This label is then scanned and the
weight of sample recorded together with information such as date, time,
equipment used and operator name. The scanning process is repeated for each
subsequent activity performed on the sample from sample preparation to analysis
through to the storage or disposal of the pulp and reject material. Sample
labels are also scanned at the shipping and destination locations whenever
samples are transported locally or internationally between ALS facilities. The
system has also been designed to accept client supplied bar coded labels that
are attached to the sample bags in the field.
The benefits to our clients of this system are:
- Complete traceability of the sample through the entire laboratory process.
- Sample integrity is guaranteed by scanning the sample label at every stage.
- Record of every sample weight submitted to the laboratory from the field.
Contamination Control during Sample Preparation
We take many steps to minimize the risk of cross contamination between samples
during the preparation process. One of the most important steps is to sort and
classify samples according to matrix type and expected metal concentrations as
soon as they enter the laboratory. The samples will then be routed through the
laboratory in different batch streams. Physically separated areas are maintained
as much as possible so that, for example, concentrates and vegetation samples
would never be processed in the same area.
Once samples are classified, they are prepared using equipment that has been
designated for certain matrix types and expected metal concentration ranges.
Equipment is color-coded and numbered so that it is clear for which sample type
it is intended to be used.
In addition, our routine operating procedures call for the use of barren wash
material to clean out sample preparation equipment between batches of submitted
samples, drill holes (if identified) and samples that appear to be of a
substantially different type than those submitted in the same batch. However, if
the client expects significant mineralisation, we recommend that they identify
the samples and request a clean wash between samples. The wash material is
tested for the elements of interest prior to use in the laboratory, and on a
routine basis once in use.
Our Dustbox dust extraction system is a key component of our sample preparation
laboratories. The Dustbox ensures that crushing and grinding equipment is
virtually completely enclosed. Our experience has shown that the fine dust,
which can otherwise collect, will invariably
contain trace amounts of gold and base metals. The end result is an improved
dust control system which reduces the risk of sample contamination and provides
a healthier workplace environment for our employees.
It is unfortunate that all grinding surfaces impart some degree of metal content
to samples during pulverisation. As a result, there will always be some degree
of contamination when crushing and grinding procedures are used. However, at ALS
we have a great variety of grinding surfaces that vary widely in their chemical
composition. We offer equipment made of hardened manganese steel, chrome steel
or carbon steel as well as non-ferrous materials such as zirconia and tungsten
carbide. Hence an Explorer can choose one of these options in such a way as to
eliminate the possibility of contaminating a sample with an element of potential
exploration significance. In the following table is a typical chemical
composition for a Chrome Free and Chrome Steel Pulveriser bowl. More information
on this topic follow in the Contamination Introduced by Sample Preparation
Equipment section.
Sample Preparation Equipment
The main equipment in use at ALS consists of:
- Drying ovens • Crushers (roll, traditional jaw and oscillating jaw)
- Pulverisers (small ring, large ring, flying saucer style puck)
- Ball mills • Screens
- Riffle splitters, and Rotary splitters
Drying Ovens
The sample drying process is more critical than may appear at first. Many
samples arrive at the laboratory sopping wet. Drying time for these samples is
invariably a major contributor to lengthened turnaround times. Hence it would be
tempting to improve turnaround time by using blast furnace drying techniques.
However there is a considerable risk to sample integrity by taking such an
approach in that some samples will appreciably oxidize at higher temperatures
(especially sulfides) and some potentially volatile elements (arsenic, antimony,
mercury; all key pathfinder elements for gold exploration will be lost at
elevated drying temperatures. Of course, even if these elements are not of
immediate interest, the samples will be rendered useless for any future
analysis.
At ALS we use two different drying temperatures and once again the choice of
temperature depends on the sample classification. For rocks, rock chips, drill
core and other "coarse" material with a relatively low surface area, we employ a
drying temperature in the range of 110-120 C (230-250 F). Independent studies of
these sample types have shown that the potentially volatile elements will not be
lost at this temperature. However for soils, silts, sediments and other "fine"
materials with a proportionately higher surface area, we limit the drying
temperature to 60 C (140 F).
Our ovens are all large, gas-heated forced air furnaces; samples are pre-loaded
onto moveable drying racks before being rolled into an oven. This avoids the
potential contamination risk that is inherent in fixed shelving units. Large
samples are placed into stainless steel trays to ensure efficient heat transfer
and minimal drying times.
Crushers
In recent years improvements have been made to the traditional jaw crusher by
the introduction of the oscillating jaw crusher. These new crushers, built
specifically for laboratory usage, provide enhanced crushing by ensuring that
the sample receives continuous grinding as it passes between the plates. The end
result is a finer product in a single step, typically >50% is -1mm whereas only
about 10% is -1mm in the traditional jaw crusher. These new crushers are also
much easier to clean and therefore chances of cross contamination between
samples are reduced.
Pulverisers
At ALS we use ring pulverisers. Ring
pulverisers have become the industry standard in recent years. Basically they
consist of a bowl that contains either a small puck and one or more rings, or a
large saucer. Crushed samples are added to the bowl, the bowls are sealed and
then subjected to centrifugal force by mechanical action. The puck and/or
ring(s), being free to move inside the bowl, subject the sample to considerable
grinding action, resulting in a very fine sample. Bowls are manufactured in
different sizes ranging from 50 g capacity to 4 kg capacity. At ALS we use two
sizes primarily, 250 g and 3 kg. The bowls themselves are made of different
materials including manganese steel, chrome steel, zirconia and tungsten carbide
so that it is easy to avoid contaminating a sample with an element of potential
interest.
Screens
Screens are used to sieve soil samples in order that the fine fraction can be
analyzed. At ALS we use stainless steel screens with stainless steel or nylon
mesh depending on the application. Brass screens are a potential source of
contamination for both copper and zinc, especially if the sample contains hard,
abrasive particles.
Contamination Introduced by Sample Preparation Equipment
The intense grinding action produced by crushers and pulverisers results in wear
metals being added to the samples being ground. The elements that are added will
depend on the composition of the grinding surfaces. The concentration of the
elements added is harder to determine as it will depend on a number of factors
including the hardness of the grinding surface, the hardness of the sample and
the length of grinding time.
Before putting any new sample preparation equipment into use we perform tests
using ultra trace methods to ensure no significant amounts of elements are
imparted to the samples being prepared.
The table below shows typical levels of elements that can be carried over for
each type of grinding medium. It must be stressed that these are typical ranges
that may not apply to exceptional samples.
|
Element |
Manganese steel (ppm) |
Chrome steel (ppm) |
Carbon steel (ppm) |
Zirconia (ppm) |
Tungsten carbide (ppm) |
|
Chromium |
2-10 |
20-500 |
5-25 |
<1 |
|
|
Iron |
0.2-1.5% |
0.1-0.5% |
0.2-1.5% |
<10 |
|
|
Manganese |
10-100 |
5-50 |
10-125 |
<1 |
|
|
Molybdenum |
<1 |
<1 |
1 |
<1 |
|
|
Nickel |
1-2 |
1-5 |
6 |
<1 |
|
|
Lead |
|
2 |
3 |
<1 |
|
|
Vanadium |
|
1 |
<1 |
<1 |
|
|
Tungsten |
|
|
|
|
30-300 |
|
Cobalt |
|
|
|
|
10-100 |
|
Zirconium |
|
|
|
30-300 |
|
|
Hafnium |
|
|
|
1-5 |
|
Sample Preparation Procedures
Crushing
Samples that require crushing are dried at 110-120 C and then crushed with
either an oscillating jaw crusher or a roll crusher. Note that if the whole
sample is required to be pulverized, then this condition becomes irrelevant.
Crushing charges are based on the sample weight. The entire sample is crushed,
but depending on the method only a portion of the crushed material may be
carried through to the pulverizing stage. That amount, typically 250 g to 1 kg,
is subdivided from the main sample by use of a riffle splitter. If splitting is
required, a substantial part of the sample (the "reject" or spare ) remains.
Pulverising
A whole or split portion derived from
the crushing process is pulverised using a ring mill. The size of the split is
determined by the client based on the pulverising procedure that is selected.
Split sizes for manganese or chrome steel rings are typically 250 g to 4 kg;
however split sizes for zirconia rings are 100 g and those for tungsten carbide
rings are only 75 g. Because of the relative lightness of these latter two
materials, the size of the sample to be pulverized must necessarily be reduced
to these weights in order to achieve the ALS QC specification for final
pulverizing, namely that >85% of the sample be less than 75 microns (200 mesh)
(see graph below ).
For those samples which require enhanced homogeneity, such as samples which are
known to exhibit coarse gold behavior, intermediate pulverization of the entire
sample (or a representative split) is also available.
Screening
Soil and sediment samples are typically sieved through a 180 micron ( -80 mesh)
screen and the fine fraction is retained for analysis. This procedure is
satisfactory for smaller (i.e. 500 g or less) samples where the exploration
target is base metals. However, when gold is the exploration target, we
recommend that the particle size of the minus fraction be further reduced using
ring mill pulverization to > 85% - 75 microns (150 mesh) in order to obtain more
reproducible gold data.
For gold exploration, many "soil" samples weigh in at several kilograms or more.
In this latter case, the samples often contain larger components such as pebbles
or agglomerations of clay and other material. For samples like this, we
recommend that after disaggregation the sample is sieved through a -2 mm (10
mesh) screen to remove the coarse material. Following this intermediate
screening, the -2 mm (10 mesh) material is then split to about 500g using a
riffle screen and then sieved through a standard -180 micron (80 mesh) to obtain
a minimum of 150 g of fine material. We still recommend further pulverization if
gold is the exploration target, for the reasons outlined above.
Special Procedures
Vegetation and humus samples require special procedures because they are easily
contaminated, difficult to reduce in particle size and awkward to homogenize.
This type of sample tends to be highly variable, ranging from well-rotted humus
to bits of tree trunk. Vegetation sample preparation is done in our Vancouver
and Brisbane laboratories because we have special facilities available. Samples
submitted to
regional offices will be shipped to the Vancouver or Brisbane laboratories and
this may result in some extra shipping charges to the client if the weights or
volumes are judged to be excessive.
Composites
Composite samples are normally prepared on a volumetric basis and the composite
is homogenised either by: repulverisation, or; mixing the samples in vials which
are mounted in dual orbiting mixers. Composites can be prepared on a weight
basis if desired but the charges are greater because the labor costs are
significantlyore higher.
Quality Control Procedures for Sample Preparation
QC Specifications for Crushing and Grinding
As mentioned in the Crushing and Pulverising sections, ALS does sizing test to
ensure specifications for these procedures. A range of specifications are
available for crushing and pulverising so that clients can select protocols that
best meet their project needs. Statistics are maintained for each sample
preparation workstation, permitting an assessment of all pieces of machinery.
Not only does this data ensure sample preparation specifications are being met,
but it also allows us to optimise the sample preparation process and helps us in
the purchase of new equipment.
Sample Sequence Logs
For any sample preparation activities we maintain sample sequence logs at all
workstations. These logs detail which samples have been prepared in what order
and are very helpful for investigative purposes.
Pulp and Reject Policy
Materials that have been submitted for analysis are retained at our laboratories
for a limited time only. The prepared master pulps are stored free of charge for
90 days from the time that we issue the final certificate of analysis. Coarse
and fine reject fractions are stored free of charge for the first 90 days,
except for large reject fractions (>3 Kg) which are stored for a nominal charge
from day one. Monthly charges will be levied for storage of all sample types
beyond the first 90 days. Instructions for pulp and reject handling can be
placed in the relevant boxes of the Sample Submission Sheet as per the
accompanying illustration:
We can provide reports about your pulps and rejects at any time upon request.
These reports will include information about ALS workorder numbers, your project
name or number, and numbers of samples. Please note that when local tipping fees
are significant, we reserve the right to bill clients for the cost of disposing
rejects to landfill.