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Sampling and Sample

preparation Module

Sampling and Sample Preparation Module

Sampling and Sample


preparation Module

BASIC SAMPLING AND PREPARATION


1. INTRODUCTION
Importance of Sampling
A sample is a small amount of material that contains all the
components in the same proportions in which they occur in the original
bulk material. This means that if there is 20%A, 10%B and 70%C in the
original bulk material then every sample will also contain 20%A, 10%B
and 70%C.
In mining it is important to sample and assay continuously. Borehole
samples are taken from places where it is suspected that the ore body
is. Therefore the analyses of the borehole samples help the mine
planner to decide where to blast. Separate holes are drilled along the
ore body and are set with explosives. The samples taken from these
holes are called blast hole samples. Therefore the analyses of the blast
hole samples tell the people on the mining site the amount of pgms
and gold to expect and what the grades of the material blasted are. By
knowing what grade of ore it is, it is then decided if the blasted
material will be sent to the concentrator or to the waste dump.
Knowing the grade of ore also helps decide how the ore should be
blended before being sent to the concentrator. In concentrating plants
such as flotation plants and smelters it is very important to sample and
analyze the products of every process (e.g. feeds and tails) to find out
if the process is efficient. Truck composites are the final material
obtained after concentration of the pgms and gold. Truck composite
samples are analyzed so that the mine knows the amount of precious
metals produced. The whole process of sample preparation is therefore
very important and should be done correctly by everybody involved.
Importance of Sample Preparation
Basically, sample preparation is used to convert the sample into a
homogeneous state and to a state where it can be used in fire-assay. A
sample that is not properly prepared would give wrong results about
the amount of precious metals contained in the sample. Therefore all
the results that follow will be incorrect and all the work done would be
done for nothing. This results in both wasted time and money.

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Sampling Terminology
Lot: For purpose of defining the sampling procedure, the total amount of material from
which a sample is to be taken.
Increment: The quantity of sample taken in one cut.
Sample: A sample is a small portion removed from a large quantity of material in such a
way that the portion has the same characteristics and properties as the original material.
Sub-sample (laboratory): A representative portion of the sample, of convenient mass,
delivered to the laboratory.
Analysis sample: The ultimate sample of the series, subjected, as a whole, to the
analytical procedure.
Particle size: The size (m) of each discrete unit of the material assumed, during the
sampling process, to be indivisible.
Top size: The maximum particle size of the material being sampled determined by the
screen size on which less than 5% of the material is retained.
Continuous sampling: The process by which the increments are taken, manually or
automatically, at regular intervals.
Intermittent sampling: A non-continuous process in which increments are taken at
irregular intervals.
Replicate sampling: The procedure in which the same number of
increments, as in continuous sampling, is transferred in turn to
different containers as the contents of each container submitted
separately for analysis.
Sampling error: The difference between the experimental results and the true values.
Random error: An error leading to results, which are sometimes higher and sometimes
lower than the true values. The mean of a number of results subject only to random error
will approach the true value as the number of results increases.

Sampling and Sample


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Systematic error (bias): An error leading to results, which are
consistently higher or lower than the true value.
Homogeneity: Describes the condition of the material being sampled
or prepared, in terms of the distribution of components in that
material. A homogenous material has all its components randomly
distributed within it.
Random sample: Composites of cuts taken at random, at several
places in the material being sampled.
Stratified sample: Sample composed of cuts or increments taken at
regular intervals throughout the material being sampled.
Systematic sampling: Samples collected at specified time intervals
or a weight delivery interval.

Principal Stages in Chemical Analysis


The main steps in a complete analysis are:
Collecting the sample (Sampling)
Deciding what analytical data are required
Making a preliminary analysis of the sample e.g. (scanning by
XRF or ICP)
Selecting the most appropriate analytical method
Converting the sample or component in question into the state to
which
the analytical method can be applied
Performing the actual determination, and
Calculating the results in a form that answers the questions
asked
The reasons for sampling and analysis
It is essential that a reliable system of sampling and analysis be
maintained. The process is of great importance since; if it is not
satisfactorily done the labour and time spent in making a careful
analysis of the sample may be completely wasted. If the material is
more or less homogeneous, sampling is comparatively simple. If,
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however, the material is bulky and heterogeneous, sampling must be
carried out with great care.
Samples must be truly representative of the whole that it represents, in
other words, samples have to meet the requirements of a specified
sampling program and be handled in a manner that does not cause
deterioration of the sample or introduce contamination to it before it
reaches the laboratory.
Sampling is done in order to obtain analyses, which will be used:
To control the metallurgical extraction process.
To obtain the data required for metallurgical accounting.
To obtain data used for planning future development.
The reliability of the results obtained depends on
The quality of the sample is the extent to which the final (analytical)
sample represents the lot.

The quality of the analysis.


Methods of Sampling
There are no general sampling methods applicable to all types of
material. Specialized methods depend on whether a gas, liquid or solid
is involved. In the sampling of solids, particle size is an important
variable and the problem can be much more difficult than for liquids or
gasses, in which a uniform, homogeneous condition usually - but not
necessarily- exists. Mechanical devices are available for sampling
large volumes of material; in many industrial processes continuous
sampling or monitoring may be possible e.g. of the cyanide or mercury
level in a waste effluent or of radioactive substances in a nuclear
reactor coolant. Exact procedures of sampling are specified by various
professional societies for sampling many types of materials. These
methods are based on careful studies and long experience. Although
some materials may be relatively easy to sample, some are not.
Difficulty may be encountered, for instance, in obtaining a
representative 25g sample from a 25 ton mill feed. To sample properly
substances that are bulky and inhomogeneous, such as ore, a large
gross sample must first be taken. A good way of doing this is to grab
pieces at random as the substance is being unloaded from a conveyor
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belt. Then the gross sample is crushed to a smaller particle size.
Portions of the crushed sample are taken and the rest is discarded.
Further reduction, particle size of a sample is accomplished by passage
through a disk pulverizer. Sieves may be used to see if the final
sample is of the proper mesh size. In general large quantities of
materials are best sampled while in motion. Metal and solid materials
are sampled by drilling, sawing, or milling (the sawdust, shavings, etc.
constitutes the sample). Inhomogeneous liquids or soft solids can be
sampled by sticking a pipe into the full depth of a substance and lifting
out the core inside the pipe. Gas samples are usually obtained by
allowing the gas to displace a confining liquid in a bottle equipped with
a suitable stopcock.
Hand Sampling
There are various forms of hand sampling, each of which requires a
different degree of skill. Precision and accuracy may vary considerably
from one technique to another, and hand sampling should only be used
if no other more accurate machine sampling technique is possible.
Grab Sampling:
This particular form of sampling is the least accurate of hand sampling
techniques. The accuracy is largely dependent on the discretion of the
sampler. It basically entails taking lumps of material, of proportional
sizes over equal distances. It requires great care and judgment on the
part of the sampler. This technique is used solely to get an idea of the
composition of material; it is quick and cheap to carry out.
In the picture below is an example of manual sampling, a shovel is
used to sample the material discharged from the conveyer belt. The
shovel is pushed directly underneath the discharged material till the
whole cup has passed through the material and is then pulled back
through the material.

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Sampling and Sample


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Sampling Equipment
Slurry Sampling
Manual sampling of slurry (a mixture of liquid and powder) streams is
generally not satisfactory due to their being no guarantee against bias,
and precision is generally poor compared to recent automatic sampling
systems. Manual sampling however is still important to serve as a
guide in the day to day running of plants, for example the use of
manual sampling to determine stream pulp densities.
Mechanical samplers may be of two general types, namely
Cross -stream cutters
Arc or Rotary type cutters
Cross-stream cutters:
The cross-stream cutter system consists of a stilling box, which
reduces turbulence in streams in order to extract a reasonable sample.
A sample cutter is designed to travel at right angles to the flow of the
slurry, to take a sample increment. The cutter length should have a
minimum length of three times the thickness of the stream, from which
an increment is taken. This should ensure that the cutter could handle
the full flow of the stream. The stream should be directed to the top
part of the blades preferably a third in length from the top of the
blades, so that when the strength of the steam is weaker it will still be
able to cut. When the cutter is not physically taking an increment the
cutter should park beyond the reach of the stream. The slurry flow rate
and the largest particle size determine the cutter traveling speed and
gap. As indicated below the yellow arrows show the direction of the
slurry on to the cutter. The cutter normally consists of a motor that
drives the chains inside the guarding box, and the chain controls the
movement of the cutter. The cross cutter must be cleaned every shift
to prevent build ups that may cause it to choke and to minimize
contamination. The chain must be greased regularly and fastened to
ensure that it doesnt derails from its path, which will cause the motor
to trip. Regular inspections must be done to identify any faults daily.
Lock-out is required if you are going to be working on the cross cutter
since it has moving parts or can start automatically. The cross cutter is
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used mostly as a primary sampler cutter with the vezin cutter as the
secondary sampler cutter.

Cross cutter laundry

Motor
Gear
Belt/chain
the vezin cutter
box

Direction of the flow

Direction of the cutter movement

Sample outlet to

sample

blade/cutter
Rotary or Arc Sample Cutters: These types of sample cutters are
generally used for smaller process flow streams or for sub-sampling.
Rotary cutters used on large flow streams generally have only one
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cutting arm, while rotary cutters used for sub-sampling or on smaller
flow streams may have two or even four cutting arms. The cutters
may operate continuously or intermittently, as is the case for arc-type
cutters. Rotary sample cutters are designed to remove a percentage
of streams, depending on the cutter open area to that of a circle it
makes. The same rules for determining cutter gaps and speeds for
cross-stream cutters apply to rotary cutters. Like mentioned before this
vezin cutter (diagram below) below act as the secondary sample cutter
by further reducing the amount of slurry from the cross cutter into the
sample container and discarding the rest.

Motor
Gear box
Cutter
Blades

Sample inlet from


Cross cutter

Sample to the container

Rejected sample Shaft


General notes regarding sample cutters:
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Cutter gaps are set according to the following basic rules:
If the top particle size is > 3mm then the critical cutter width is = 3
times the top particle size. If the top particle size is < 3mm then the
critical cutter width is = 10mm.
The top particle size is the top size class (or screen) on which 5% of the
material is retained.
The critical cutter speed has been established to be 0.6 m/s at the
critical cutter width. Cutter speeds less than or equal to this value
would be feasible. For cutters of width n times the critical cutter
width, the critical cutter speed may be determined by the following
relationship
Critical cutter speed = 0.3 (1 + n) m/s
The length of the cutter plates should be at least 3 times the thickness
of the stream, from which a sample is taken.
Other types of sampling equipment:
Due to the costs
involved
with
installing
sample
cutters, particularly
in older plants where
modifications
to
existing process flow
sheets need to be
made, other means
of obtaining samples
may be required.
These
sampling
systems often do not
conform
to
the
accepted sampling
practices, but may
be to some extent
been justified.
Vezin
to
vezin
sampler cutter

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Slurry inlet

Cutter blades

Cutter motor
Sample out let to the second vezin cutter
Slurry returns to the
Process

Sample material from


primary vezin cutter
Cutter motor

Sample

cutter

blades

Sample rejected from


the cutter

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Sample to the container

Because of the nature of the material flowing it sometimes becomes


necessary to use two vezin cutters, like we are doing with our primary
cleaner tails. Since the cross cutter takes flat streams, the vezin can
take steams from round pipes and also the stream flow rates
contributes in this choice of sample cutter. The material /slurry get
reduced from the primary vezin cutter by the rotating blades into the
secondary vezin cutter which cuts into the sample container. This kind
of sample cutters in this configuration they choke easily when not
constantly cleaned, so it is important to clean it regularly and do
inspections on it.

The Hammer Cutter


Conveyer
belt

Ore
Cutter with a
brush

Motor

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Direction of the flow

Sample in to the rotary splitter

Splitted to waste
Rotating direction of the splitter
sample to the container

split

Ore from the hummer cutter


Splitting blades

Splitter motor

Since it has become dangerous to manually sample over a moving


conveyer belt, the hummer cutter makes it convenient to sample under
those conditions. It normally set at periodical time interval e.g. every
hour it will make a cut. This hummer cutter is incorporated with a
brush at the end/tip of the sample cutter blades to also brush the fines
into the sample container after it has been splitted. Since the ore will
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be flowing in a certain direction the hummer cutter will cut at a right
angle to the flow. The rotary slipper is there to reduce the size of the
sample about 75 % of the material is splitted to waste and the rest as a
sample.

Barrell type filter press

T- Bar
Compressed air inlet
Pressure release valve

Barrell
Filter clamp

Filter Base

Drained water

Filtering (de-watering)
Liquid as well as slurry samples to be filtered are received. Analyses
are required for some samples on the liquid portion only, for others on
the solid portion only and for some on both portions. All apparatus
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must be clean and if analysis on the filtered portion is needed, then all
apparatus must be dry as well. Samples are filtered either under
pressure or vacuum. A potential source of error is loss of solids under
the edges of the filter paper. This may be avoided by taking adequate
precautions in the design and operation of the filter. Filtrates should be
tested regularly for the presence of significant quantities of solids.

Drying ovens

Drying of samples.
Drying is effected in a well-regulated and ventilated oven, set at a
temperature of 105 C to 110 C. Other methods such as infra red
heaters or hot plates may be used for rapid control analysis. They are
not recommended for accurate work. At temperatures above 110 C,
chemically combined moisture may be lost. The resultant error may be
appreciable in the determination of moisture. Ovens must be inspected before
use and cleaned after use. Racks normally lose their paths inside the ovens and this must
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be reported and get fixed. When starting it is advisable for the ovens to reach the desired
temperatures before anything can be inserted.

Jones riffler splitter


Rifflers
chute/dish
Rifflers grating
Sample dish
Waste dish
Waste bin
Rifflers feet
stand

The Jones riffler is used for splitting coarser material to reduce the
sample size; it is helpful when using it on side e.g. near hummer
cutters that are not incorporated with splitters. As the material is
poured inside the chute the gratings will divide the material almost
equally into both the sample dish and waste dish. Any material that
doesnt pass through must be collected and get broken to be able to

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fit. The Jones riffler is not one of the most accurate splitters due to the
fact that the sample will not be homogeneous when splitted.

10 way rotary splitter

Splitters cone
feeder
Sample divider
Sample cup holders
Vibrator feeder
Vibrator motor
Sample cup holder
rotation switch
Rotation speed
control switch
Vibration switch
Rifflers stand
Vibrator switch
The 10 way jones riffler is efficient for splitting the sample. When the
sample is poured into the sample cone the vibration must be set to
release the sample slowly onto the rotating sample cups. The purpose
is for the sample to be equally distributed into the ten sample cups.
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The cascades splits the sample as in enters the cups while the cups are
rotating. The rotational speed and vibration rates can be controlled by
the speed control switch to 30 rotations before the sample is
completely distributed.

Laboratory tumble mixers.

Tumbler mixers
motor
Sample steel
container

Sample
container
clamp
Tumblers
switch
Timer
Base stand
The function of the tumbler mixer is to homogenize the sample. When
operating the tumbler always insert the two containers even if youre
only using one container to balance the other one. The timer is set to a
desired time for mixing the sample. Before stating the equipment
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ensure that the sample containers lids are properly closed not to spill
any sample. It mixes the sample by making rotation on the sample
containers. The sample containers must be cleaned inside before
putting in the sample and ensures that the containers are used for a
specific grade only. Example concentrate sample containers must not
be used in the tail section to avoid contamination. The tumbler has
moving parts when in rotation so when starting it make sure you take a
safe position and the in nothing obstructing the path of the rotation.
Always keep the tumbler clean when not in use and the surrounding
are must also be clean.

The V-blender
Sample inlet
lid
V-blender
shaft
V-blender
motor
Display and
timer
Sample out
let
Sample
containers
V-blender stand

The V-blender is normally designed to homogenize larger bulk of


material such as preparation of quality control material. It also has a
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timer to control the blending period. The blender is normally housed in
a cage since it has moving parts and the door of the cage is equipped
with a trip switch for the blender not to switch on when the door is
open. The V-blender normally has a weight capacity that it can handle
depending on it size and that weight must not be exceeded to prolong
the life span of the motor and the shaft. The load ratio is that for a
blender of 1 dm3 capacity the optimum sample volume is 300 to 500
cm3 with a 20 rotations per minute velocity. The ideal mixing time
under these conditions is 10 to 30 minutes depending on the type of
material.
Mixing by bottle rolling
The practice of mixing samples by paper bottles or cylindrical cans
gives rise to gross segregation and should never be used.

Mixing by paper rolling


This classical procedure is carried out on a glazed paper. A corner of
the paper is drawn toward its opposite corner so that the sample is
made to roll over upon itself. Care should be taken to ensure that the
sample does not merely slide along the surface. Each corner is drawn,
in turn, towards its opposite corner until the sample is thoroughly
mixed. The method is rapid and requires no mechanical aids. But it
restricts the sample to smaller volume and particle size and is prone to
bias arousing from loss of fines. This is aggravated by rough handling
and the method requires a certain amount of operator experience and
care.

Laboratory jaw crusher

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Crusher
primary
switch
Crusher
chute
V-belt
guard

Secondary switch
Crusher motor
Sample dish slot
Waste bin cabinet

The primary jaw crusher, with an opening of approximately 200 X 125


mm, reduces the sample to < 8mm. The product from the jaw crusher
is passed through a roll crusher (200 X 125 mm). The product from the
roll crusher should be < 3 mm. Surfaces of jaws should be examined
frequently and worn parts replaced. Settings should be checked daily,
and the particle size of the product should be re-established at regular
intervals. The crusher primary switch is incorporated with a lock slot to
enable lock out and the secondary switch has a start stop button only.
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The V-belt should always be guarded not even for a finger to go in. The
crusher is normally inspected for loose bolts and nuts, gap size, proper
guarding and cleanness. When not in use the crusher must be switched
off.

LM-5 Pulverizer Mill

Mill open
cover
Air bag
Sample
container
lid
Sample
container

Emergency/stop button
Start button
Pressure
Display

The LM-5 pulverizer has the capacity to mill samples fairly bigger than
what can be milled using a vertical spindle pulverizer. Inside the
sample container is a milling disc that actually crushes the sample into
smaller pieces, depending on the nature of material being milled it
should be able to mill material to a particle size of 80 % that should
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pass through a 75 microns sieve. The mill must be operated with the
cover closed and the pressure gauge should show 400 kpa or slightly
above for the equipment to have sufficient pressure to operate. The
green start button is pressed and holds to start the equipment. To stop
the equipment we can use the stop button. The principle it uses is it
shakes or vibrates randomly with the sample and disc inside, forcing
the disc to crush the samples as it counteracts the movement of the
mill.

Vertical spindle Pulverizer


Primary switch
V-belt guard
Adjusting wheel
Motor
Stop/start switch
Sample inlet chute
Pulveriser side door
Sample cup holder
Pulverizer discs
Waste tray

The function of the pulverizer is to reduce the particle size of the


sample from < 3 mm to < 150 m. The danger of contamination is
greatest during pulverizing. Varying amounts of fine material become
lodged on the grinding surfaces and, more especially, on the central
area of the disc. If the material is not removed it will contaminate the
next sample to be pulverized. The equipment should therefore be
cleaned out after each sample.

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Lump breaker
Primary Switch
Chute lid
Sample input
chute
Lump breaker
motor
Sample
container handle
Sample
container
Secondary
switch
Sample container stand.

In dried slurry there is sometimes lumps that preventing the sample to


be homogeneous. The lump breaker becomes critical in breaking those
lumps and leaving the samples in a fairly equally size particles. The
lump breaker must not be used as homogenizing equipment as that is
not its co function. On the safety issue hands must not be inserted into
the chute as they are rotating parts within the machine that can catch
your hands.

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3 Pots Swing Mill


Seep mill holder
Pot holder
Sample pot
Sample pot
handles
Spring holder
Swing pot clamp

Start switch for


forward rotation
Start switch for
backwards
rotation
Swing mill doors
Swing mill cover
Swing mill
spongy floor

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The swing mill shakes with the samples inside the pots, inside the pots
there steel rings and a central puck in the middle. The rings have
spaces between then where the sample will occupy those spaces in
between. During vibrations the pucks crushes the sample as they try to
close the spaces in between. The particle size of the sample is hence
reduced in this way. The swing is housed with a spongy floor to reduce
the noise and absorb some of the fine dust materials. It rotates with a
forward rotation first and a backward rotation thereafter. The swing
must always be operated with three pots inside even if only one pot is
the only one with a sample. The equipment must be operated with the
door closed for safety reasons. Always clean the equipment before and
after use.
General
Over the years numerous samplers and designs have been proposed
for sampling process streams. Many of such samplers have however
not met the criteria required in taking unbiased samples and hence
have found little practical use. The costs, relative importance of
samples and the general degree of precision required from samples
have dictated the type of installation often used. Where samples are
required for metal accounting purposes, a high degree of precision is
required and therefore better sampling methods have to be used.
What information does the laboratory require?
What sample is it? (Name and place of origin)
What analysis is required? (Gold, PGMs, grading, etc.)
Is any special treatment required? (Acid, washing, wet screening,
drying, etc.)
What are the approximate values expected? (High grade/Low
grade)
What is the priority rating i.e. how soon do you need the results?
Will a composite analysis be required at a later date?
How long the sample should be kept for analysis that may be
repeated?
May the sample be discarded or must it be returned to its place
of origin?
To whom must the results be reported?
Is there any, safety or health risk associated with the sample?
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Problems encountered with the identification and handling of
samples.

Bad handwriting/Wrong date/Wrong shift


Labels not tied on properly
Labels put into wet samples
No labels
Too much sample in too small a packet
Sample not properly dried
Specifically colored bottle or bucket labeled incorrectly
Same shifts on tickets
Two different labels in one sample
Label on outside of sample different to label on inside
Sample sheet does not correspond to samples sent i.e. ID or No.
Paper bags used for wet samples (Plastic bags)
Insufficient sample for analysis required
Large wet samples (Results required urgently)
Analysis required not marked on sample ticket or packet.

Contamination
Contamination is the spoiling of one sample by allowing small portions
of
another sample (or samples) to become mixed with it.
Contamination from other sources is also possible. For example - small
amounts of iron from pulverizer discs. This type of contamination
would only be a problem if one were analyzing for the element
concerned - in this case iron.
To avoid contamination:
Containers and equipment should never be interchanged
between different
grades of samples.
Containers and equipment should be thoroughly cleaned before
use.
Plastic bags, paper packets or disposable plastic cups which are
used only once reduce the risk of contamination, but are not
suitable for all stages of preparation.
Bias

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Bias results from systematic errors, which produce consistently positive
or negative results. In sampling, two major areas where bias exists
are:
Sampling:

Increments coinciding with cyclic events


Only a portion of a stream being sampled
Cutter specifications not adhered to
Overfilling of sample containers
Sampling increments too infrequent

Sample Preparation

Inadequate mixing
Insufficient material during intermediate stages
Not crushing prior to further sample reduction
Dust losses
Drying temperatures too high

Why Evaluation?
Evaluation is precisely what the name implies, the evaluation of data
obtained from a sampling system. Evaluation is an integral part of any
mine. Metal accounting is based on figures produced by the evaluation
department. Process evaluation consists of the following basic
components.
Sampling - obtaining of representative samples
Sample preparation - drying, crushing, sub-sampling, sizing etc.
Measurement of process streams - mass flow rates, densities etc.
Sample analysis - grade, size analysis, ash etc.
Construction of metallurgical balances
Safety & Housekeeping

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In all cases the safety of the sampler (person) is of the utmost
importance. Belts should be stopped when sampling manually. Fast
and heavy streams should be sampled with care.
When taking
samples, ensure that the sample site is well lit, and the sampler is not
off-balance when taking the sample. Safety equipment must be worn
where appropriate and proper sampling equipment used, especially
when dealing with chemicals or toxic streams. In dusty environments,
ensure that proper respiratory gear is available, and used. Ensure that
the sampling equipment is always in a good and clean condition. The
area where sampling takes place must be demarcated. When working
with automatic samplers stay clear of all moving parts. Should any
adjustments to the equipment be necessary, ensure that the
equipment is locked out, and that the working area is safe. Avoid
wearing loose clothing especially when near moving parts.
Auditing the Sampler
Was the sample taken in the demarcated area?
Was the sampling equipment in good working order, free of
visible damage?
Was the sample container clean?
Was the proper sampling equipment used to take the sample?
Was the equipment clean?
Was the proper amount/mass of sample taken?
Was the sample promptly delivered to the lab?
Was the sampling procedure carried out safely and responsibly?
Did the person use his proper Personal Protective Equipment?
Was there any deviation from the relevant Work Instructions?

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