Chapter – 3 Sampling and Analytical Techniques

Sampling and sample preparation

Sampling is a scientific, selective process applied to a large mass or group or a

population is defined by investigator in order to reduce its bulk for interpretation
purpose. This is achieved by identifying a component part a sample which reflects the
characteristics of the parent population within acceptable limits of accuracy, precision
and cost effectiveness. In the mineral industry the average grade of a tonnage of
mineralized rock (the population) is estimated by taking samples which are either a few
kg or tones in weight. These samples are reduced to a few grams (the assay portion)
which are analyzed for elements of interest.

Homogeneity and heterogeneity

Homogeneity is the property that defines a population whose constituents units are
strictly identical with one another. Heterogeneity is the reverse condition. Sampling of
the former material can be completed by taking any group of these units such as the
most accessible fraction. Mineralization is composed of dissimilar constituents and is
heterogeneous, it is rarely homogenous and correct sampling of mineralization is
heterogeneous. Material has to ensure that all constituent units of the population have a
uniform probability of being selected to form the sample and the integrity of the sample
is respected (this is the concept of random sample).

Sampling Error: sampling consists of the main steps, and errors can occur in one or
more .

 (I) actual extraction of the sample(s) from the insitu material comprising the
population

 (II) the preparation of the assay portion which involves a mass reduction from a
few kg(or tones) to a few grams for chemical analyses

 (III) the analysis of the assay portion

 When sampling care has to be taken: Geological heritage is the only record of
the earth history and processes and need to be preserved for research and
enjoyment of present and future generations.
Sample collection and preparation

 Sample should be collected in non metallic containers to avoid contamination

 Kraft paper bags are best suited for sampling soil and stream sediments because
the bags retain their strength if the samples are wet and the samples can be
oven dried without removing them from their bags

 Thick gauge plastic or cloth are preferred for rock sampling

 All samples should be clearly labeled by pens containing non metallic ink

 Most sample preparation is carried out in the field, particularly when it involves
the collection of soil and stream sediments. The aim of the sample preparation is
to reduce the bulk of the samples and prepare them for shipment.

 Soil and stream sediments are generally dried either in the sun, in low
temperature ovens, or freeze dried, the temperature should be below 65 degree
centigrade so that volatile elements such as mercury are not lost

 Drying then is generally followed by gentle disaggregation and sieving to obtain

the desired size fraction

 Preparation of rocks and vegetation is usually carried out in the laboratory and
care should be taken in the selection of crushing material.

 For example- in rock geochemical program, a company searching for volcanic

associated massive sulfides found manganese anomalies associated with hard
amphibolites. They were encouraged by this and took it as a sign of exhalative
activity , however manganese highs were related to pieces of manganese steel
breaking off the jaw crusher and containing the amphibolite samples.

 Contamination can also be eliminated by cleaning crushing equipment thoroughly

between samples

Sampling in Reconnaissance technique

1. Stream sediment sampling

Widely used reconnaissance techniques in residual area undergoing active weathering

is stream sediment sampling. The simplicity of the method allows the rapid evaluation of
the areas at relatively low cost. Interpretation of stream sediment data is carried out by
comparing the elemental concentrations of catchment as there is only a poorly defined
relationship between the chemistry of the catchment. In stream sediment sampling the
whole stream sediment or a particular grain size or mineralogical fraction of the
sediment, such as heavy mineral concentrate can be collected. In temperate terrains
maximum anomaly/background contrast for trace metal is obtained in the fine fraction of
the sediments as this contains the majority of the organic material, clay and iron and
manganese oxide. The coarser fractions including pebbles are generally of more local
origin and depleted of trace elements. Usually the size cut-off is taken at 80 mesh (˂
177μm) however, the grain size giving best contrast should be determined by an
orientation survey. For base metal analysis and geochemical mapping 0.5kg sample is
sufficient, but for gold due to its very erratic distribution 8-10kg of -2mm is sampled.
Common sample collection method is grab sample of active stream sediment 20-30m
apart, 10-15 cm depth to avoid excessive iron and manganese oxide. In addition
contamination should be avoided by sampling upstream from roads, farms, factories
and galvanized fences.

Orientation survey- Evaluating which techniques are effective for the commodity
sought and in the area of search. In orientation survey the following things are
considered and decided:-

 Clear understanding of the target area

 Understanding of surfacial environment of the search area.

 Nature of primary and secondary dispersion

 Sample types available

 Sample collection procedures

 Sample size requirements

 Sample interval, orientation and areal density

 Field observation required

 Sample preparation procedures

 Sample fraction for analysis

 Analytical method required

 Elemental suit to be analyzed

 Data format for interpretation

Stream sediment preparation

Wet samples are sieved in the field and 0.15mm fraction will air dried and sent to
sample preparation laboratory. In the lab, Samples will be dried at 40 degree
centigrade, ground manually in a porcelain mortar and re-sieved to 0.15mm. Dried
samples are disaggregated by hand using a mortar and pestle sample homogenization
is then carried out using an agate planetary ball mill until 95% is finer than 53μm.
Quartering- quantity required depends on analytical method and it will be collected by
coning and quartering method. The ˂ 0.15 mm fraction then split into two portions using
rotary divider and one of the portion is archived for further studies. The other portion is
pulverized to a grain size ˂0.063mm, homogenized and divided into bottles to be
submitted to the analytical laboratories

2. Lake Sediments

In glaciated areas of northern Canada and Scandinavia access to rivers is difficult on

foot, but the numerous small lakes provide an ideal reconnaissance sampling medium.
A sample is taken by dropping a heavy sampler into the lake sediment and retrieving it.

3. Overburden Geochemistry (Soil sampling)

In areas of residual overburden, overburden sampling is generally employed as a follow

up to stream sediment surveys. This depends on the nature of the overburden, if the
chemistry of the near-surface soil reflects that at depth, then it is safe to use the cheap
option of sampling soil, if not then samples of deep overburden must be taken.

The main areas where surface soil don’t reflect the chemistry at depth are:

 Glaciated area where the overburdens has been transported from another media

 In areas of wind blow sands

 In areas of lateritic weathering, where most trace metals have been removed
from the near surface layer.

(a) Surface Soil Sampling

o The major problem is to decide which layer of the soil to sample as the
differences between the layers are often greater than that between sites.
But generally the most effective samples are from a zone as around 30 cm
depth.
o Usual method of soil collection in temperate terrains is to use a soil hand
auger up to 1m, at 30 cm depth. 100-200 g masses sample collected for
base metals, and 500 g-2 kg for gold.
 o There are of influence of a soil sample is relatively small and should be
determined during an orientation survey.
o The spacing is dependent on the size of the primary halo expected to
occur across the target and the type of overburden.
o Spacing in the search for veins may be as little as 5m between samples
but 300m between lines, but for more regularly distributed disseminated
deposits may be as much as 100m by 100m
o Sample spacing may also be dictated by topography, in flat land or
subdued topography, rectilinear grids are ideal choice and in mountainous
ridge, spur sampling
(b) Transported Overburden

 In areas of transported overburden, such as glaciated terrains, sandy desserts or

gravel covered areas sampling problem is sever.
 In glaciated area, chemistry of till must be examined. Basal till sampling can only
be accomplished by drilling (light percussion drills).
 In sandy areas -80 mesh fraction of overburden is enriched in wind blown
material, therefore we use coarse fraction 2-6mm reflecting locally derived
material.
 Example:- Kimberlite of Botswana in Jwaneng area, samples taken at 0.5 km
grid, heavy minerals separated from +0.42mm fraction. Kimberlite indicator
minerals such as picro-ilmenite counted anomalies shown displaced from sub-
outcrop due to wind.

4. Hydro geochemistry

Use water as sampling medium

Water is restricted to very specific circumstances because not all elements show equal
dissolution rates, indeed many are insoluble, contents of trace elements are very low
and have been different to measure. Water samples are highly dependents on weather
and easily contaminated by human activity. Uses when hydro geochemistry becomes
useful in exploration of arid areas with poor outcrop, like exploring fluorite as fluoride is
easily measured in the field using a portable single ion electrode. If water wells are
drilled for irrigation and tap deep aquifers, they can be used to explore in the
subsurface. Water sample has been used for uranium exploration although it has not
been very successful as the uranium concentration is dependent on the age of ground
water, the amount of evaporation and its source which are extremely difficult to
determine.
5. Gases

Gases are potentially an attractive medium to sample as gases can diffuse through thick
overburden. Example:- Mercury is the only metallic element which forms a vapor at
room temperature and it is widely present in sulfide deposits particularly volcanic
associated base metals deposit. Gas radon- is generated during the decay of uranium
and has been widely used with some success. In general results has been
disappointing because of the large variation in gas concentration caused by changes in
environmental condition, particularly changes in biometric pressure and rainfall.

6. Vegetation

Vegetation is used in two ways in exploration geochemistry. Firstly the presence,

absence or condition of a particular plant or species can indicate the presence of
mineralization or a particular rock type called Geobotony. Elemental content of
particular plant can also be measured, this is known as biogeochemistry.
Biogeochemistry have higher application than Geobotony and found particular
application in the forest regions where surface sampling is difficult.

Geobotony- is all about identifying plants in particular flowers associated with

mineralization.

Example:- small mauve copper flower, Zambian copper belt. The flower require a soil
copper content of 50-1600ppm Cu to thrive, known as indicator plant.

But can flourish under other conditions and are not very reliable. A more reliable
indicator of metal in soil is the stunting of plants or yellowing (chlorossis). This condition
is particularly amenable to remote sensing from satellites.

II. Follow-up Sampling

Once an anomaly has been found during reconnaissance sampling and a possible
source identified, it is necessary to define that source by more detailed sampling. If
reconnaissance phase was stream or lake sampling, this will probably involve
overburden sampling. In the case of soil or overburden sampling it means increasing
the density of sampling until the source of an anomaly is found, proving the source by
deep overburden sampling and sampling rocks at depth or at surface when there is
outcrop.
Rock Geochemistry

 It is recommended that 30-40 samples are taken from each pluton to eliminate local
effects.
  In general 1 kg sample is sufficient for base metal, 5 kg for precise precious metal
determination if present as discrete grains.

 Surface weathering products should be removed with a steel brush.

Rock sample preparation:

 Cutting of specimens to required size using diamond saws.

 Mounting the specimen- place the specimen face down in epoxy casting cup.

 Labeling the specimen- use a tungsten carbide scriber or engraving tool to mark
the back or side of the sample once it is hardened.

 Grinding the specimen- ground on 15 micron cast aluminum lap for about 2-10
minutes or until the surface is free of excess epoxy and irregularities.

 Initial polish (0.3 micron alumina on cloth)

 Final polish

Field observation when sampling

 Description of site locality, preferably with regard to a fixed permanent feature or

land mark

 Grid reference

 Date and Identity of collector

 Catchment geology from map (stream sediment sampling)

 Clast and bed rock geology at site.

 Heavy minerals seen in concentrate

 Land use- contamination, sediment color and composition

 Precipitates in stream, whether condition, stream flow condition

 Summary of application of various sampling techniques

Planning Drainage Lake Water Soil Deep Rock Vegetation Gas

Scale Sediments Sediments over Sample Sample Sample
burden

Reconnaissance 1:10,000- Common Glacial Arid Common Laterite, Good forest

1:100,000 area Glacial out crop

Detailed 1:2,500- Common - Common forest Arid

1:10,000

Drilling ˃1:1000 Common

 Analytical Method

 Most analysis is aimed at the determination of the elemental concentrations in a sample and usually of trace metals.
 The difference between these methods is cost, the detection limits of analysis, speed of analysis and the need to make
material into solution.
The major methods are the following:-
Capital Multi Precision Sample Cost per Comment and Sample
Cost (USD) Element Type Sample
(USD)

Colorimetery 8,000 No Poor Solution 2-10 Good for field use and W, Mo

Atomic absorption 60,000 No Good Solution 1-5 Cheap and precise

Spectrophometry

X-ray flouresence 200,000 Yes Good Solid 20 God for refractory elements (Nb,
Mo, Ta, W, Ru)

ICP-ES (Inductive 150,000 Yes Good Solution 10 Good for transition metals (Nb, Zr,
coupled emission Mn, Co, Ni, Zn, Sr, Ba)
Spectrometry)

ICP-MS Inductive 150,000- Yes Good Solution 10 Good for heavy metals, high
Coupled mass 1000,000 resolution instrument, very low
spectrometry detection limit