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Sampling methods. Problems and solutions

Article · January 1991

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 Chapter 16

SAII{PLING METIIODS: PROBLEMS AI{D SOLUTIONS

Ralph J. Holmes

CSIRO, Division of Mineral- and Process Engineering

P.O. Box 312, Clayton, Victoria , 320'7, Australia

INTRODUCTTON SAI\4PLING BASICS

Although sampling: techniques used by Tt 'i.s crenera l I v ar:cerlf ed that

s v v v r e v s e the
the mineral industry continue to discharge point of an ore or
improve, sampling is stil-I an area concentrate stream is the most suitabl-e
which is often neglected. Frequently, sampling' .l-ocation. The stream can be
sampling and sample preparation intersected at regular intervaJ-s, and
requirements are l-eft to personnel who representative samples, referred to as
do not fully appreciate the increments, can be obtained by taking a
significance and importance of complete cross-section of the ore
sampling. Consequently, plant stream. On the other hand, sampling
evaluations are often based on devices that take part of the stream on
seriously biased samples, leading to an intermittent or continuous basis,
mass balance problems and incorrect €.9., a bleed from a piper frdy
assessments of pJ-ant performance. introduce serious bias, and shoufd be
avoided at all cost.
The basic rule for correct sampling
is that each particle of ore or Increments may be taken at
concentrate must have an equal completely random times or tonnages
probability of being col-lected and during the sampling operation, in which
becoming part of the final sample for case it is cal-Ied "random sampling".
analysis. If this is not t.he case, However, as shown below, random
bias is easify introduced and the sampling results in the largest
sample is not representative. For sampling variance, so it. is preferabfe
example, when ore is travelling on a to divide the ore or concentrace srream
conveyor belt, the lumps may come to up into strata of equal- time or mass
the surf ace. ConsequentJ-y, a grab and take one incremenL from each
sample taken from the top layers only stratum. This operation is call-ed
wil-l- contain a greater proportion of stratified sampJ-ing and may be either
lumps, i.e., the sampl-e is biased. systematic sampling, in which
There seems little point in making, increment.s are taken at the same point
major investments in precise analytical- in each stratum/ or stratified random
equipment, if the sample provided to sampling in which t.he increments are
the analytical laboratory is not taken at random within each stratum.
representative in the first place. Systematic sampling results in t.he
smallest sampling variance, provided
This paper describes the sources of periodic variations in quality or
plant sampling errors, reviews the quantity are not present which may
methods of estimatingi their variance, coincide with, or approximate to, any
presents some worked examples, and multiples of the proposed sampJ-ing
provides some practicaf advice for interval. fn such cases, it is
reducing' sampling errors and their strongly recommended that st.ratified
variance. random sampling within fixed time or
mass intervals be carried out.
157
I58 EVALUATION AND OPTIMIZATION OF METALLURGICAL PERFORMANCE

The increments are subsequentlY o'o, = o'r.r + .... + otru, +

combined into subsamples or a gross * o'ruu-, 1 o2a: (3)
sample and then crushed and divided as
necessary in a number of "sampling" where o'r* sampling error varj-ance
stages to produce various test samples for stage 1
according to the user's requirements. o'ru, sampling error variance
The aim always is to reduce the overall- for stage I
variance to an acceptable fevel while o'r",., : samPling error variance
aL the same time eliminating anY for stage u-1,
ci an j f i n:nf ] ^ ' ia S e S . In thiS reSpegt, the second fast staqe.
moisture samples require sPecial
attention. To minimise any change in This method is particularly usefuf for
moisture content, moisture samples must designing, optimising and assessing
be extracted as soon as possible with sampling schemes. However' Lo obcain
minimum handling and test portions maximum benefit, it is necessary to
weighed immediately. If this is noL collect data at each sampling stage.
possible, samples should be stored in Note that the sampling error variaqce
impervious air-tight containers with a for the last stage is included in Lhe
minimum of free air space. measurement variance o'ou.

The second method, which is found in

OVER,AI.L VARIA}ICE most existing national and internat-
.:^-^1 ^---r r-- qf anclarris. is tO break
I(rlldf JarttPrIIrY vusrrsqrsrt

The overall variance of t.he final up the overall- variance into the
qamnl qamn
measurement, denoted by o'"u consists of nri m: rrr i na lo nr-a

the variance of samPling Plus the 1: l <n r o € o r r o r l- - - LU dJ JalttPlg

variance of measurement (chemical preparation) and measurement variances

analysis, moisture determination, as follows:
determination of particle size
distribution, etc. ) as follows: o2o, : G', * o2, + o2ou (4)

o'o" o'r" * o'^r ( 1) where o'. prrmary samptl-ng' varrance

o" variance due to all sub-
where 6'," error sequent sampling and
:v:a: ?r rl _asnacm
e pling sample preparation sLeps,
ot* measurement error i .e . , sample processing,
variance. cxcent selecfion of the
test portaon.
fn equation (1), the total samPling
error variance includes the variances Note that the primary sampling variance
due to all sampling stages from primary 02, is identicaL to the sampling error
sampling down to selection of the test variance f or sLage 7-, i.e., o"rr in
portion. However, as assumed below, equation (3) . The rel-ative magnitudes
the variance due to selection of the of the variance components in equacion
test. portion is usually included in the (4) indicaLe where additional effo:t
"measurement" varianc€ o2asr because it needs to be focussed to reduce the
is difficult to separately determj.ne overal-I variance.
the "true" measurement variance.
FinaIIy, as described by Merks
n,,..i +^
\f|LIILE
^1cran
U! LEll
llrrr
! lr sol n/ rl r u q L ei ^2f A (1985), the overalf variance can be
measurements are carried out to reduce estimated experimentaf Iy by collecting
the overall variance, in which case: "interpenetrating" duplicace samples .
This method gives valuable information
6'o, o'r, * o 2* / r (2) at no additionaf cost on the overal-l
variance actually achieved for a given
The estimation or measurement of the sampling scheme. The odd and even
overall variance can be carried out in numbered increments from two adjacent
a number of ways, dePending on the Iots are separately combined to give
purpose of the exercise. In many samples A and B for the two lots.
respects the different approaches are After repeating this procedure a number
complementary. nf t-imcq- thc overafl t
variance for the
e . . v \

Iot is given by:

The first method is to break uP the
sampling variance into its components o 2 o "= ( 0 . 8 8 6 E l x ^ . - x u , l / N ') (5)
for each sampling stage (1, 2, ...., L,
\r-1, u) as described by Gy where x^, and xB. are the analyses for
(1982a). The overall variance is then each pair of samples, and N is the
a i tron Frrr . number of pairs.
 SAMPLING METHODS: PROBLEMS AND SOLUTIONS 159

SAMPLTNG ERRORS particles in a crusher due to excessive

air flow in the dust extraction svstem.
Considering sampling errors first of
all, according to Gy (1-982a, 1982b) the Deli:nitation and Extraction Errors
sampling'error TE, for a given sampling
stage can be broken up into a number of The del-imitation and extraction
independent components as folLows: errors arise from incorrect sample
cutter design and operation. The
TEi : FEi + GEi + QE2i + QE3i del-imitation error can be el-iminated if
+ wEi + DEi + EEi + PEi (6) aIl parts of the stream cross-section
are diverted by the sample cutter for
where FEt fundamental error arising the same length of time. The
from the constitution extraction error can afso be el-iminated
heterogeneity of the ore by ensuring that the increment is
or concentrate particles completely extracted from the st.ream
GEr grouping and segregation without any material rebounding or
error arising from qroup- beinq lost from the cutter. t
ing and segregation of
the particles Cutter Desiqn. Sample cutters must be
QE2i : long-range quality located at a point which provides
fluctuation error arising access to the complete stream.
from long-range quality Normally the cutter is driven through
f l-uctuations the stream being sampled. However,
nE? periodic quality when sampling slurries, a flexibl-e hose
fl-uctuation error discharging the slurry can be driven
wEi weighting error across a fixed cutter. Both
DEr increment delimitation arrangements are equivalent. To ensure
error that both the delimitation and
increment extraction extract.ion errors are eliminated. the
error foll-owing design rul-es must be
PEi = preparation error. observed.

A number of these error components, . The sample cutter must be

such as delimitation, extraction and nonrestrictive and self-cleaning,
preparation, can fead to bias, which discharging completely each
can be reduced to insig,nificant J-eveIs increment without any rebounding,
by using correct sampling practices. overflowing or hang-up in the
These errors are considered first in cutter. The cutt.er throat should be
the fol-lowing discussion. The I arcrer 1 -h a n thc r-rtf 1-Fr ^nerLure
-F- and
remainder can be minimised or reduced must be designed to give the lowest
to an acceptabfe level by careful possible resistance to fl-ow to
design of the sampling system. prevent choking or plugging. To
prevent hang-up, minimum valley
Preparation Error angles of 60o are required. For
sticky materials such as wet mill-
In this context, preparation is a feed, stainfess steel or
nonselective operation without change polyethyfene lined chutes are
of mass, such as sample transfer, recommended.
drying, crushing or mixing. Typical
preparation errors include sample . No material-s other than the sample
contamination, sample Ioss, afteration must be introduced into the cutter,
of the chemical or physical composition €.9., dust or slurry must be
of the sample or operator mistakes. prevented from accumulating in the
These errors can aII be eliminated by cutter when in the parked position.
use of correct sampling practices and
staff training. For example, cutters . The cutter must col-l-ect a complete
should have dust caps to prevent entry cross-section of the stream, both
of dust when the cutter is in the the leading and trailing edges
^^-^rarar.,,:leer.i
parked position. As mentioned above, uvlltPrgLEry v r 9 o ! r r r y n c r fuhr res rs ut r e a m at
the moisure sample should afso be the t$ro l-imits of the cutter path.
prepared quickly to avoid change in
moisture content. In addition, . The cutter should intersect the
excessive vertical drops shoufd be stream either in a plane normal to,
avoided, because breakage of coarse or al-ong an arc normal t.o, the mean
particles wiIl alter the physical trajectory of the stream. Verticaf
characteristics of the sample. Such cutter lips shoul-d be avoided,
drops will- also result in loss of because particles striking the
moisture content. Another example of a inside of the cut.ter J-ips are
preparation error is loss of the finer usually defl-ected down and away from
160 EVALUATION AND OPTIMIZATION OF METALLURGICAL PERFORMANCE

the cutter aperture by gravitY.

. The cutter must travel through the

stream at a uniform speed. Electric
drives are best in this resPect. Nt'
Special care needs to be taken when
samplinq high capacity streams. The
cutter drive must have sufficient
power to ensure that the cutter does
not sfow down as it enters the
stream and speed uP as it leaves the
stream. Because of the mass of the
moving parts of the cutter, there (a) CORRECT (b) TNcoRRECT
must al-so be sufficient sPace at
both sides of the stream for the
cutter to accelerate to its cutting
t
speed prior to entering the stream
and to sfow down and stoP after
Qrmnl ina nf qIrrrrrz f rnm
exiting the stream. f l.LrUKli l- e r s ! ! _ ) '

a pipe
. The geometry of the cutt.er opening
. q:mnlc drre t-9
must be such that the cutting time R i eqsr i n+ cr r rY
uf of fhc

at each point in the stream is defl-ection and/or rebounding of the

equaI. Hence, for finear-Path Iarger particles.
cutters, the cutter edges (cal-Ied
Iips) must be parallel, while for . Shock load problems and difficulties
cutters travelling in an arc or a in maintaining constant speed while
circfe (e.9., a Vezln cutter) , the cutting the material- stream.
cuLter Iips must be radial.
Experimental work undertaken by Gy and
. The cutter aperture must be not Iess Marin (1978) shows that to avoid
than 3 times the nominal toP size of significant bias the cutter sPeed
the ore or concentrate being shoufd not exceed 0.6 m/s for a cutter
sampled. For dry materials, this aperture of 3 times the nominal toP
rule hofds down to 3 mm nominal toP size of the material- being sampled.
size, bel-ow which a fixed cutter For cutters where the aperture (w) is
aperture of 10 mm is recommended. in excess of 3 times the nominal toP
For damp or wet materials, a minimum size, the maximum cutter speed al-lowed
cutter aperture of 50 mm is \/ r. cz / I marr l-re i nr-reasecl in accordance
recommended to prevent bridging. with the fol-Iowing equation:

. The cutter must have sufficient vc 0.3(1 * w/wr) (7)

uaPourLy
. : r . . fu^v a c c o n r m O d a t e t h e
increment mass obtained at the where vc maximum cutter speed, in
maximum flow-rate of the stream. metres per second
w acLual widt.h of cutLer
. If a belt-scraper is required Lo aPerture
remove ore or concentrate adhering w1 3 times nominal- top size.
f n t-ha
u r r v
l-rel f -
v e ! e t
thc sr-renpr
v v ! s r v +
muSt
r , ' be
located so that the scraped material Cutter l.4aintenance. The cutter must be
fal-1s within the area traversed by sufficiently robust to withstand the
the cutter. impact of Lhe particles in Lhe stream
without being distorled. It must be
. For slurries, Ioss of sample regularJ-y cleaned and inspected for
material- due to dribbles must be deformation and wear. The cutter lips
avoided. eipes must be bent down- should be constructed of impact and
wards to prevent slurry flowing back wear resistant material which can be
along the outside of the PiPe (see easily replaced.
Fig. 1), and the sloPe at the end of
a faunder must be sufficient to Weighting Error
prevent slurry flowing back
mL^ ..^: -L! i -n o
g rl !r vn !r
underneath the launder. frlg wE19rrLfrly rr so os ur rr lut !5 f fOm

f.l-uctuations in the flow-rate of the

Maximum Cutter Speed. In designing a stream. The consequences of these
mechanicaf sample cutLer, one of the f]uctuations are that increments do not
mosL important design parameters is the have the same mass for mass-basis
cutter speed. Too high a cutter speed sampling and che tonnage represented by
will lead to: an individual increment for time-basis
sampling is uncertain. The best
 SAMPLING METHODS: PROBLEMSAND SOLUTIONS l6r
sol-ution is to regulate the flow-rate quality fluctuation error variance is
prior to sampling, thereby making the often referred to as the distribution
weighting error insignificant. variance ( M e r k s , 1985) .
However, practical experience and
computer simul-ations by Robinson (1988) Estirnation of Fundamental Error
show that the weighting error is stil_l Variance and Minimum Sample l4ass
negligible, even when there are
significant variations in flow-rate. The fundamental error variance o2ou
results from the constitution
Periodic Qual.ity Fluctuation Error heterogeneity of the ore or concentrate
particles. According to Gy (I9B2a,
Periodic variations in quality can 1982b), it. is given by:
arise from crushing and grinding
circuits, centrifugal pumps, bucket.- o'ou cd3a2 /m, (11)
wheel- reclaimers, etc. Difficulties
mainly occur when the sampling interval- where C the sampling constant of a
approaches that of the periodic given ore or concentrate
variation. The most noted example is fnr : rvirzon n : r l - e +i n
v rl au Jc ri -- ag
slurry sampling after centrifugal and critical component
pumps, where cavitation can cause nominal- top size of the
strange effects. This particular concentrate, in centi-
sampling l-ocation shoul-d therefore be mararq
avoided. ms sample mass at a given
sampling stage, in grams
a : fractional- concent.ration
SAII{PLING VARIAI{CE of the component under
consideration.
Assuming that the weight.ing,
del-imitation, extraction and preparat- The sampling constant f- iq airran l.rrr.
ion errors have been etiminated or are
j-nsignificant, and that periodic vari- ( ' n 1 € n
(12)
ations in quality are not a problem,
the sampling error TE, for each where c minera.logical composit ion
sampling staqe given by equation (6) factor defined befow
reduces to: I liberation factor
f (arla) if the ore or
TEi : FEi + GEi + QE2i (8) concentrate is not fully
rI r vi sh! aqrua 9f u , orl .lI
u vl -g. af ri r g^ ^ + x^
LtrE:
Hence, the sampling error variance nomina] top size at which
for sampling stage rrirr is given by: c^ o^ m
* ^pt-^Lre^t e r. ll _* D e r a t ] - o n ocCurs
1 if the ore or
o'r", : o'""t + o2cei * o'o"r, (9) concentrate is ful-lv
Iiberated
where o'"", fundamental- error - - * r i ^ l ^
lJq! L ture
^ L ^ n A
Jllclr _ f a a l a r

variance which can usualfv be t,aken

o'"t, seEregation and grouping to be 0.5
error variance si zo randa f anl. nr
t
rqruc qr qr rr 'r l l 1 , ,
o'o"r.,. long:-range quality between 0 .25 and 1.0 .
fluctuation error
variance. If dr is unknown, a conservative
assumption is to set dr : d.
As pointed out before, the sampling
error variance for the first stage o2ru, The mineralogical composition factor
is identical to the primary sampling is given by:
variance 02, . Hence, equat j - o n ( 9) can
also be used to estimate 02. in c: (1-a)[(1-a)pr + ap2]/a (13)
equation (4).
where P, density of the particles
Alternatively, the fundamental error of the critical component,
varj-ance o2"", and the segreqation and. in grams per cubic
grouping error variance o2cEi in centimeter
equation (9) can be combined into the pz density of the gang-ue
short-rang'e quality fluctuation error particles, in grams per
variance o2qerir giving the following cubic centimeter.
equation:
The sj-ze range fact.or g can be
O'r", O2geri * o2oezi (10) estimat.ed from the rat.io of the nominal
top size d to the lower size }imi_t d,
In equation (10), the long-range (about 5% undersize) as foll-ows:
162 EVALUATION AND OPTIMIZATION OF METALLURGICAL PERFORMANCE

Large size range (d/d' > 4): This exceeds the mass of test portion
usually used for chemical analysis.
g : 0.25 However, if the sample is pulverised to
a nominal top size of 75 pm, m" is
Medium size range (2 < d/d' reduced to 0. 44 g, thereby enabling
test portions of 0.5 to 1.0 g to be
g : 0.50 used for the above ZnS concentrate.

Small size range (d/d' < 2): Exampfe 2. Consider the case of
sampling a porphyry copper ore with
S: 0-75 d : 2.5 cm, dt : 200 pm (0.02 cm) and a
Iarg:e particle size rangre. Assume the
Uniform size (d/d' : l-) : mineral is CuFeS, with a particle
density : 4.2 gcm-3, and that the
Pr
g: 1.00 gang'ue consists of silicates with a
particle density Pz : 2.6 gcm-3. In
A fundamental- characteristic of o2"" addition, assume the CuFeS, t
is that it diminishes very quickly when concentration is 1% (i.e., d : 0.01) .
d is reduced and not so quickly when mt This corresponds to a copper
is increased. However, it can never be concentration of about 0 .35% Cu, so
eliminated no matter what crushing and assume that the fundamental error must
homog'enisation procedures are used, not exceed 0.02e" Cu or 0.06% CuFeS"
althougrh for fine fl-otation (i.e., o." : 0.0006).
concentrates the fundamental- error
variance is negligible when the sample c : 0.99(0.99x4.2 + 0.0l-x2.6)/0.01
mass exceeds about 100 g. A 1 A
A L A . L
'

Equation (10) can be transposed to r : 1(0.02/2.5) :0.089

give the minimum sample mass m, for a
desired fundamentaf error variance o'." C 4L4.2x0.089x0.5x0.25: 4.6I
as f o]Iows:
'x (0.01)']
ms [4.61x (2.5) / (0.0006)'z
nk : Cd3a'/Ct", (14) 20,0099:20k9

Hence there is an absolute mimimum Thus the minimum sample mass for a
sample mass required to achieve a given nominal top size of 2.5 cm is 20 kg.
fundamental error variance at any stage The sample must be crushed to a smal-l-er
of sampling. The sample mass cannot be nominal top size before the sampl-e mass
reduced bel-ow this minimum until- the can be reduced any further. For
sample is crushed to a smaller particle example, if the 20 kg sample is passed
size. This is one of the most through a jaw crusher to reduce the
important sampling rules, which nominal top size to 1 cm, repeating the
unfortunately is often ignored, J-eading above cafculation shows that the sample
to poor sampling precision. mass can then be safelv reduced to
2 kg.
Example 1. Consider the case of
sampling a zinc concentrate with Segregation and Grouping Error Variance
d:160 pm (i.e., 0.016 cm), dr:50 pm
and a J-arge particle size range. The segregation and grouping error
Assume the mineral is ZnS with a variance cannot be easil-y calculated,
particle density : 5.0 gcm-3, and but it can be determined experimentally
Pr
that. the gangue consists of sificates together with t.he fundamental- error
with a particle density Pz : 2.6 gcm-3. variance by preparing and analysing
In addition, assume the ZnS repJ-icate samples (B or more) of a
concentration is 50? (i.e., a : 0.5) given sample mass and calculating the
and that the fundamentaf error must not variance bet.ween samples o2ur. Af ter
exceed 0.022 zn or 0.03% ZnS (i.e., repeating this procedure for a range of
one: 0.0003) . different sampJ-emasses, the variance
can be expressed in terms of the
c : 0.5(0.5 x 5.0 + 0.5 x 2.6)/0.5 replicate sample mass ms as f oll-ows:
3.8
o'u, so * sr/m, (1s)
r : {tso/reol: 0.s6
C 3.8 x 0.56 x 0.5 x 0.25:0.21 where So and S, are const.ants determin-
ed from a .l-east-squares fit to the
3 x( 0 . 5 ) ' ? 1 ( 0 . 0 0 0 3 )' z
ms 1 . 0. 2 ' 7 x( 0 . 0 1 6 ) / experimental dat.a.
= 3.1 g
 SAMPLING METHODS: PROBLEMS AND SOLUTIONS r63

The variance So in equation (15)

incl-udes the segregation and grouping
error variance o2o, and the sample
processing and measurement variance,
and is independent of sample mass. The
second term is the fundamental error pv
variance, i.e.,
e*?
eB'gt
o'., so - o', - o'o, (16) -

#"*
(17)

Al-ternatively, according t.o Gy

(I982a, 1982b), the segregation and
grouping error variance is either
Ac
smaller or about t.he same magnitude as
the fundamentaf error variance.
Consequently, i t is always safe to
assume that it is equal to the LAG (t)
fundamental error variance, i.e.,

o'"" o'uu (18)

Long-range Quality Fluctuation Error FIGURE 2. Experimental- and

Variance corrected variograms.

The long-range quality fluctuation In most cases it is found that.

error variance o2o", can be estimat.ed by variograms which occur in pract.ice can
extracting a large number of successive be adequately approximated by a
increments (say 30-50) at a given qf r: iahJ- I i no nrrar l- ha r^nda f rnm rzorrr

sampling stage and anal-ysing them small values of t to at l-east twice the
individually. There are two principal- spacing between increments (Saunders et
methods of analysing the resultant dl., 1989). Thus it can be assumed
i ^ ! ^ +L-r.
u a L a . L l l a L .

The better method is to cal-culate v.(t) A. + Bt (20)

the variogram, which examines the
differences between increments at where A" random component of
increasing intervals (called lagrs) variance of the correct.ed
apart. The variogram approach all-ows variogram
for seria.l- correfation between B gradient (or slope) of the
increments, and enables the separate varrogram.
contributions of the variances o2qs1 dnd
o2ou, to be determined. The sampling error variance o2.. for
a- g- ] r- v, ^e- .r r s- - a- ^r rn. lP- -r r n g ' s t a g e at ^ 5 t! Ln^ e n glven
The value of the variogram V.(t) at by:
Iag t is given by:
(a) Systematic sampJ-ing

-z -4" BQ (2r)
E [xi*, - xif , V T d -

= (19) n 6nz
Ve (t)
2Nt
(b) Stratified random sampling

-2 An Be
where xt is the analysis for increment A-o-= ---: + - (22)
i, x,r. is the analysis for increment n 3nz
i+t, and N. is the number of pairs of
increments at lag t apart. The (c) Random sampling
resultant variogram is call-ed the
"experimental" variogram, and includes -2 A" -B Q
the variance of sample processing and O-oo= -----: + (23)
n3n
analysis as well as the sampling
variance. Subtraction of the sample
processing and analysis variance gives where O : tonnage or time interva.l-
the "corrected" varioqram V.(t), which over which sampling takes
provides information on the sampl-ing place
errors only (see Fig. 2) . n - number of increments.
164 EVATUATION AND OPTIMIZATION OF METALLURGICAL PERFORMANCE

Clearly, the sampling variance depends n : o2r/c'ru (28],

on the sampling-scheme chosen, random
sampling being the l-east precise. When Example. Consider the case of sampling
there are no periodic variat.ions in a copper concentrate sl-urry stream.
quality, systematic sampling is also The stream was sampled at 7 . 5 m in
more precise than stratified random intervals g"iving the resul-ts shown in
sampling. the Table befow.

In equations (21), (22) and (23), Sample No. % Cu Sample No. % Cu

the first and second terms on the left
hand side correspond to the short- and L Z9.L 16 30.1
long-range quality fluctuaLion error 2 28.5 L7 30.0
variances respectively. Thus for 3 29.3 1B 3 0 .s
systematic sampling: 4 29.6 19 29.5
5 29.4 20 29.r
6 30.1 2I 29.3
A" 1 29.5 22 2B'.5
o'nr, = (24l'
n B 29.2 23 2 1. 9
9 29.4 24 28.I
10 3 0. 0 25 2 8. 0
11 30.9 26 28.I
=
O'On (2s) L2 29.8 21 2 8. 8
ffi 13
14
2 9. 6
29.0
2B
29
2 9. 9
28.1
15 2 9. 4 30 29.2
The alternative method of estimating The variance of sampJ-e processing and
the sampling error variance is a analysis was 0.01. The experimentaf
simplified approach invoJ-ving variogram is shown in Fig. 3. Fitting a
cal-culation of the variance between sf raiohf Iine to the first forrr noinf s
increments, referred to as the nf f lro ovnarimanl- rl rr:ri n a r :-m* ^ . .
: gaves :
increment variance o2b. whil-e this
method tends to overestimate the A" 0.0510
- . . ^ r . :! , - !rl 1 . . ^ - . - a t i O n errOr varianCe when B
Y U q r r L y u L L q c 0.0146
there is significant correlation
between increments, it errs on the safe IJan^a

side and is much easier to apply than

the variogram method. However, the A. 0.0510 - 0.01
separate contributions of the variances 0.0410
o 2 q p 1d n d o 2 q s 2 c d n n o t b e d e t e r m i n e d . The
increment variance o2b can be estimated
for a given sampling sLage using the
f ol-lowing equation:
0.8

'V;: o.7
o ' o= (26)
{)'
0.6
(l)
0.5
where X: analysis for increment )
ui
()
x mean analysis for all 0.4
z
increments
n number of increments. (r 0.3

Again the variance of sample processing o.2

and anal-ysis shou.l,d be subtracted to
obtain a better estimate of o2o. Thus, 0.1
if n increments are taken, the sampling
error variance o2r, for the sample
obtained by combining aII increments 30 45
does not exceed:
LAG (min)
o'ru : o2 o/ n ( 2 7\

Rearranging equation (21) enabl-es

the number of increments required to
achieve a given sampling error variance FIGURE 3. Experimentaf variogram
to be cal-cul-ated as f ol-l-ows: for copper concentrate stream.
 SAMPLING METHODS: PROBLEMSAND SOLUTIONS 165

Assume that eight successive increments r_ncrement mass, provided the increments
are combined to form hourly composites. are extracted in such a manner that the
For systematic sampling, equation (2I) particles in the stream have an equaJ-
gives: probability of beingr selected and
becoming part of the final sampJ-e for
o2r" : 0 . 0 4 1 0 / B + ( 0 . 0 1 4 G x 6 0 )/ ( 6 x g r ) anal-ysis. fn fact it is generalty
0.00513 + 0 .00228 preferabl-e to take a J-arge number of
0.00741 :-ncrement of smal-l_ mass than a smalf
number of increment.s of larqe mass.
This is the primary sampling variance.
Adding the varj-ance of sample Correct increment extraction for a
processing and analysis in accord.ance cross-stream cutter is det.ermined by
with equation (4) gives the fol-Iowing the minimum cut.ter aperture and the
overall variance for hourly composites: maxlmum cutter speed. Hence, the
increment mass required. to obtain an
o'ou: 0.00741 + 0.01 unbiased sample for a given nomina.l top
0 -0174 size is essentially determined ny ff,e
flow-rate of the ore or concentrate
Thus, stream and is given by:

oou 0.13? cu mr GA/3.6v. (29\

For comparative purposes, if the where ml mrmlmum mass of
simplified method is used, the variance in(:remenf - 'i n lli'l r n a - ^r- oq l r L D
vY
of the Cu analyses in the above Tabl_e - flow-rat.e of concentrate
given by equation (26) is 0.532. stream, j-n tonnes per hour
Subtracting the sample processing and A minimum cutt.er aperture,
anal-ysis variance of 0.01 gives I n maJ- raa
o2o : 0.522. For hourly coirposites, vc maximum cutter speed, in
equation (27 ) t.hen gives : metres ner seCOnd.

otru: 0'522/B
0.06s3 !{.ASS-BASIS AIVD TIME-BASIS SAMPLTNG

Adding the variance of sample Mass-basis Sanpling

processing and analysis gives the
fo.l-l-owing overall_ variance for hourlv In mass-basis sampling, increments
composites: are taken at fixed tonnage intervals AT
given by:
o'ou: 0.0653 + 0.01
0.0753 aT < Q/n (30)
Thus, where AT : mass intervaf between
primary increments, in
Oou 0-212 Cu tonnes
mass of lot, in tonnes
The overa.l-l standard deviation is twice n number of increments.
the value obtained using the variogram
method, demonstrating that. the The increment.s must be taken in
simplified method can overestimate the such a manner that t.hey have al_most
sampling variance. As a consequence, uniform mass r €.g. r by using a variabfe
equation (28) will over-estimate the speed cutter, the speed of which is
number of increments required to proportionaf to t.he f_l-ow-rate at the
achieve a desired sampli-ng: error time of taking' the increment.
variance by a considerable margin.
Time-basis Sampling
Further detai]s on the use of
variograms for the estimation of fn time-basis sampling, increments
sampling variance, including case are taken at. fixed ti-me interva.l_s qiven
studies, are given by Gy (I982a) and by:
Royle (1983) .
ar. (3r1
M.I\SS OF INCREMENT where At time interval between
primary increments, in
whil-e there is an absolute minimum minutes
sample mass required to achieve a given O mass of lot, in tonnes
fundamental- error variance, there is no maximum flow-rate, in
similar fundamental_ lower limit on tonnes per hour
166 EVALUATION AND OPTIMIZATION OF METALLURGICAL PERFORMANCE

n nurnlf,er of increments. difficul-t to crush is usually different

in composition from t.he remainder of
The mass of each increment must be the sample and cannot be satisfactorily
proportional- to the fl-ow-rate of the mixed back into the sampl-e.
stream at the time of samplinq. For
this purpose, a fixed speed cutter is Sample mixing
required. The relative masses of the
individuaL increments or subsamples The sampling error variance can be
must be preserved throughout sample reduced by thorough mixing of the
processing to obtain the correct. sample prior to division. The need for
weighted mean for the final analysis. mixing is particularty important when
samples from more tharr one source are
combined. Exampfes of mixinq methods
METHODS OF REDUCTTON, MTXTNG are as f o]Iows:
A}ID DIVISION
. Passing the sample through a riffl-e
i
Particle Size Reduction or preferably a rotary sample
divider three times in succession,
Partic.l-e size reduction can be recombining the portions after each
carried out using comminution machines pass.
such as jaw crushers, rol-l- crushers,
cone crushers, hammer mil-l-s, plate . Forming and reforming the sample
mill-s and ring mil-ls. They shoul-d be into a linear strip three times in
easy to clean and shoul-d be cleaned succession by careful- distribution
between each sample to prevent cross- of the material along the Iength of
ql-rin qhar;ol
contamination. tha v e r + r
rs rv rq. ir Yn n :

Those parts of the apparatus which . Pu]verisation in a rino mill-.

come into contact with the sample
should be of wear-resistant material to It should be noted that some
minimise contamination. This is methods of hand mixing, for example
particularly important for samples in forming and reforming a conicat pi1e,
which trace e]ements are to be can have the clnnrlsi f e ef f er-f to that
determined, and every ef fort shoul-d be intended, and can in fact lead to
made to use equipment. which does not increased segregation.
contain any of the el-ements to be
determined. Division

According to Pl-owman ( 1985) , jat Suitabl-e methods for division

crushers are mainly suitable for innlrrrla r^l- er\r qrmnlo r'li-tiqinn riff la

crushing dry hard material-s. The division and manual increment division.
reduction ratio is reasonably high, but Of these rotary sample division is the
it is difficult to crush to a very fine most rel-iabl-e method for dividing
particle size. RolI crushers can have chemical- analysis samples, but moisture
smooth or toothed ro1fs. For sampling loss can be a problem for moisture
applications, smooth rol-l-s are samples. The variance of rif f l-e
preferred, because they can be scraped division is generalJ-y larger t.han for
to prevent build-up of material, rotary sample division, particularly in
thereby preventing' cross-contamination the hands of unskil]ed operators. Loss
between samples. Hammer mill-s have a of moisture can al-so be a problem.
high reduction ratio and high Manua.l- increment division, when
throughput, but the hiqh airflow can correctl-y applied, can be quite precise
ji
cause dust loss. Loss of moisture from :nrl l.ranarrca nf f he h icrh rzi 5 jgp

moisture samples is also a problem. ratio, is suitable for division of

moi.strrre samnles with minimum Ioss of
Some mills such as rinq mill-s and moisture. The method consists of
plate mills tend to become heated, so spreading the sample out on a smooth
samples that are susceptibl-e to heat, srrrface- marki no out a matri x of at
e.9., some concentrates, must not be least 20 parts on the surface of the
allowed to remain in them long enough sample, and taking an increment from
to become affected. If a mil-l- is used each part with an increment scoop.
for a series of samples, it should
either be water cooled or al]owed to
cool- between each operation. CONCLUSION

During preparation of the chemicaf The discharge point of an ore or

analysis sample, screening to remove concentrate stream is the most suitabfe
oversize particles for re-crushing is sampling focation. The stream can be
not permitted. Material which is intersected at reguJ-ar intervals, and
 SAMPLING METHODS: PROBTEMSAND SOLUTIONS L67

representative samples can be obtained Gy, P.M. , I9B2b, "Sampling f rom High-
by taking a complete cross-section of Capacity Streams", Proceedings,
the stream. Sampling devices that take First Australian International Bul-k
part of the stream on an intermittent Materials Conference, Sydney, pp.
or continuous basis may introduce 401-423.
serious bias and therefore are not
recommended. There is l-ittle point in Saunders, I.W -, Robinson, G.K.,
having precise analytical equipment if Lwin, T.t and Holmes. R.J., 1989,
the sample provided to the analytical "A Simplified Variogram Method for
l-aboratory is not representative in the Determining the Estimation Error
first place. Variance in Sampling from a
Continuous Stream" I International-
The components of sampling'error Journal- of MineraL Processing, Vol-.
have been described in detail-. Some 25, pp. 175-198.
can be reduced to insiglnificant level-s
by correct sampling practices. The Merks, J.W., 1985, Samp)ing and
remainder can be minimised or reduced Weighing of Bul-k SoJids, Trans Tech
to an acceptable leve1 by design of the Publications, Cl-austhaL-Zel-l-erfeld.
sampling system. To assist in this
task, ways of estimating the overall- PIowman, P.M., 1985, "PracticaJ- Aspects
variance and the sampling variance have of Samp1ing", Bufk Soljds HandJing,
been described- Vol-. 5, No. 6, pp. 1259-1265,

Royle, A.G., 1983, "SampJ-ing f rom

REFERENCES Moving Streams", Department. of
Mi n i nc :nd Mi nar: l F.nai npori nn 'f ha

Gy, P.M., and Marin, L-, I9'7B, TIn i rrorq i I rr LeedS .

"Unbiased Sampling from a Falling

Stream of Particulate Material", Rnhi nqnn C
v . L \ .
K 1 qAA
L r e v t
nri rrat. a
y ! a v q u v
f t

International- Journaf of Mineral- communication.

Processing, VoI. 5, pp. 29'l -3I5 -

Gy, P.M., 1,982a, Sampling of

ParticuJ-ate l"lateriaLs - Theory and
Practice, Second Edition, Elsevier,
Amsterdam.

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