Widiastuti Setyaningsih

European Master in Quality Analytical in Laboratory
Gdansk University of Technology
E­mail widiastuti_setyaningsih@yahoo.com
Mobile +48889664465 or +6287878121767

AM0801-DESIGN OF SAMPLE STRATEGIES

AND SAMPLING TECHNIQUES

Date : February 17, 2009

Sampling course. Assessment work

1. Hands-on PC seminar (EXCEL work. Use of Gy’s formula and replication experiments)
2. Mass reduction. Biased and unbiased sampling devices.
3. Case study 1-D (gas production plant)

1. Case study 0-D (waste container). Describe briefly the sampling procedure to obtain 30 g of
representative sample out of 10 tons of heterogeneous material from a waste container. Write
the sequence of SUOs used in the sampling procedure.

Answer :
Sampling Procedure
Objective
to Obtain 30 g of Representative Sample Out of 10 Ton Lot

Definition
Lot = Heterogeneous Material from a Waste Container
Increment = Group of heterogeneous material fragment from each waste container
sampling

StepsProcedures

SUO1 Since the lot was huge as 3-Dimensional, we need to reduce the dimension with
put it into a conveyor belt.
“Let assume that our conveyor belt transporting (Vc) 60 ton per hour”

SUO6 Do the composite sampling by take the increments from conveyor belt with cross
section samplers to reduce the effect of distributional heterogeneity.

“ Assume that cross section belt velocity (Vs) is 10 cm/s

Vs = 10 cm/s
and sample container width = 10 cm”
X = 10 cm

Vc =60 Ton/Hr
The minimum increments weight Mi-min as much as
Mi-min = 10 000 000 gram x 10 cm = 16666.67 gram
10 x 60 s x 10 cm/s
 If the waste material consists of crushed sandstone, it might have C : 1370g/cm3
(ref. http://www.simetric.co.uk/si_materials.htm); assume d (Average) = 2 cm,
So we can calculate Absolute Minimum Sample Weight Ms-min, which is tied to
tolerated primary fundamental error (assume S (FSE1) 10%)
Ms-min = Cd3 = 1370 g/cm3 x 23 cm3 = 1096000
S2 (FSE1) (10/100)2

Therefore, this minimum sample (Q) should be made of :

Q = Ms-min = 1096000 = 65.7599  66 increments
Mi-min 16666.67
If the sample should be representative of 10 Ton waste material (or 10 minutes
in the conveyor belt), then we shall collect 1 increment every 9 seconds.

Collect the increments into a composite which known as Primary Sample

(Considering for the sampling strategies which might applied. It might stratified
randomized during 9 seconds).
Primary Sample should be taken as much as
S1 = 10 cm x 2 cm x 2 cm x 1370 g/cm3 = 54800 gram

SUO4 Particle Size Reduction (Commutation) is needed since the material have constitutional
heterogeneity. It might done with solid waste shredder.
“Assume that the waste material will be crushed to 0.5 cm before reaching the
secondary sampling”

SUO5 Blend the shredded waste material to reduce distributional heterogeneity.

SUO7 Split it into parts with the same size to obtain Representative Mass Reduction.

So, we can have Ms-min as below

Ms-min = Cd3 = 1370 g/cm3 x 0.53 cm3 = 17125 gram
S2 (FSE2) (10/100)2
Sampling Ratio = 17125 gram = 0.3125 or  33.33 %
54800 gram

Allot the primery sample into 3 same part then we will get secondary sample
as much as 54800/3 gram = 18266.67 gram

SUO4 Refined the tertiary sample to make it closer to homogeneous level with grinder.
“Assuming that we are grinding the secondary sample to 16 mesh (0.10 cm)”

SUO5 Blend again to make it distribute well.

SUO7 Split it into parts with the same size to obtain Representative Mass Reduction.
So, we can have Ms-min as below
Ms-min = Cd3 = 1370 g/cm3 x 0.103 cm3 = 137 gram
S2 (FSE2) (10/100)2
Sampling Ratio = 137 gram = 0.00749 or  0.75 %
18266.67 gram
 Since the sample was very fine and mixed well. We can split into the desired
sample size for the analysis (or weigh it as much as 30 gram)

Keep the rest in a good storage location (for retain sample).

RESUME

LOT
10 Ton, Heterogeneous Material from a Waste Container

SUO1-Dimensional Reduction
conveyor belt transporting (Vc) 60 ton per hour

SUO6-Composite Sampling
collect 66 increments; 1 increment in range 9 seconds
Primary Sample : 54800 gram

SUO4-Particle Size Reduction

crushed to 0.5 cm

SUO5-Blend/Mix

SUO7-Representative Mass Reduction

Allot the 1st sample into 18266.67 gram for each 2nd sample

SUO4-Particle Size Reduction

grinding into 16 mesh (0.10 cm)

SUO7- Representative Mass Reduction

SUO7- Representative Mass Reduction

Weighing as much as 30 g for 3rd sample for analysis needs

Store the Retain Sample

2. Hands-on PC seminar (EXCEL work. Use of Gy’s formula and replication experiments)
1. Given a lot of C = 540 g/cm3, and lot mass ML = 100 Kg,
a) calculate the fundamental sampling error if the particle size, d = 0,1 cm, and the sample
mass, MS = 50 g. How big would be the absolute error if the lot grade (aL) is 0,05%?
Answer :

(Reference : M H Ramsey and S L R Ellison. (2007). Measurement uncertainty

arising from sampling : a guide to methods & approaches. From
135.196.210.195/images/EURACHEM1_tcm18-102815.pdf )

C = 540 g/cm3 σa =?
d = 0.1 cm
Ms = 50 g
ML = 100 Kg = 100 000 g
aL = 0.05%

σr2 = (540 g/cm3)(0.1 cm)3((1/50 g)-(1/100000 g))

σr2 = 0.0107946
σr = (0.0107946)½
σr = 0.103897064

σa = σr . aL = (0.103897) (0.05) % = 0.519 %

b) calculate the total fundamental sampling error if the particle size, d = 0,1 cm, and we
perform a primary sampling taking sample mass, MS = 1000 g followed by a reduction of
particle size, d =0,05 g, and a secondary sampling, taking MS = 50 g.
Answer :
s2 (FSET) = s2 (FSE1) + s2 (FSE2)  1 1 
s2 (FSE ) = Cd 3  − 
 MS ML 
3
C = 540 g/cm Ms1 = 1000 g
d1 = 0.1 cm Ms2 = 50 g
d2 = 0.05 cm ML = 100 Kg = 100 000 g
s2 (FSET) ??

s2 (FSE1) = (540 g/cm3)(0.1 cm)3((1/1000 g)-(1/100000 g)) = 0.0005346

s2 (FSE2) = (540 g/cm3)(0.05 cm)3((1/50 g)-(1/1000 g)) = 0.0012825
s2 (FSET) = 0.000534 + 0.0012825 = 0.0018165
s (FSET) = 0.042620418 = 4.26 %
 c) For a lot of the same material and d = 0,1 cm, how much sample mass should be taken to
reach a fundamental sampling error of 2 %? And 1%, 5%?
Answer :
In Gnumeric File (Spreadsheet of Linux)
Widiastuti.Setyaningsih_assessment_material >> Sheet 1

d) For a lot of the same material and taking a sample size of 500 g, how small should be the
particle size to attain fundamental sampling errors of 1%, 2%, 5%?
(Use the SOLVER tool for parts c) and d))
Answer :
In Gnumeric File (Spreadsheet of Linux)
Widiastuti.Setyaningsih_assessment_material >> Sheet 1

e) For a lot of the same material, plan sample strategies that allow for having a fundamental
sampling error of 2 % (particle size range allowed: 0,01 cm - 0,1 cm; sample mass range
allowed: 20 g – 200 g). Build a contour plot representing CV (%) (z) vs. particle size (x) and
sample mass (y) to detect the possible ranges of particle size and sample mass that can
provide the desired error level.
i) Can we work with a sample mass equal to 20 g? Which particle size range should be
used?
Answer :
In Gnumeric File (Spreadsheet of Linux)
Widiastuti.Setyaningsih_assessment_material >> Sheet 1

ii) How low the error can get if the particle size is 0,1 cm?
Answer :
In Gnumeric File (Spreadsheet of Linux)
Widiastuti.Setyaningsih_assessment_material >> Sheet 1

2. Study the effect of the factors that modify the fundamental sampling error according to Gy’s
formula. Make plots in a), b) and c) for a lot where the critical particles are mixed with the
gangue, i.e., β = 1, α = 100, and for a lot where the critical particles are fully integrated in the
lot, i.e., β = 0.03, α = 30.
Sheet: Gy’s formula liberated particle, Gy’s formula integrated particles.
a) Effect of particle size. Represent the variation of CV (%) vs. particle size (particle size
range from 0.01 cm to 0.5 cm).
Answer :
In OpenOffice File (Spreadsheet of Linux)
Widiastuti.Setyaningsih_assessment_material
Sheet : Gy's formula liberated particle and Gy's integrated particles

b) Effect of sample mass. Represent the variation of CV (%) vs. sample mass. (sample mass
range: from lot mass to 10-5 times lot mass). You can use a sample mass logarithmic scale
for a better visualization.
Answer :
In OpenOffice File (Spreadsheet of Linux)
Widiastuti.Setyaningsih_assessment_material
Sheet : Gy's formula liberated particle and Gy's integrated particles
 c) Effect of lot grade. Represent CV (%) vs. lot grade. (lot grade range: from 10% to 10-6 %).
You can use a lot grade logarithmic scale for a better visualization.
Answer :
In OpenOffice File (Spreadsheet of Linux)
Widiastuti.Setyaningsih_assessment_material
Sheet : Gy's formula liberated particle and Gy's integrated particles

3. Calculate the GEE, TSE, PSE, SSE and TAE errors (%) from the data of the replication
experiment.
Answer :
In OpenOffice File (Spreadsheet of Linux)
Widiastuti.Setyaningsih_assessment_material
Sheet : Replication experiment

EXCEL file: lot0D.xls

Sheet: Gy’s SOLVER and contour plot (exercise 1 c), d) and e))
Sheet: Gy’s formula liberated particle, Gy’s formula integrated particles (exercise 2).
Sheet: replication experiment (exercise 3).

4. Mass reduction. Biased and unbiased sampling devices. Reading material: L. Petersen, C.K.
Dahl and K.H. Esbensen. Chemom. Intell. Lab. Sys. 74(2004)95-114.
a. Which are the main causes of biased mass reduction in the design of riffle splitters?
Answer :
The main causes of biased mass reduction in the design of riffle splitters are :
1. Riffle Splitters Model (Closed riffle splitters provide lower bias than opened model in
term of bouncing materials)
2. Feeding Tray Size (To reduce the bias, feeding tray must have exactly the same width
as the rectangular receiving region of splitter)
3. The Chutes Characteristics
• The width of the chutes (To reduce the bias, it must be minimum 5 mm or 3 times
the largest particle diameter and must all have the same size and form)
• The number of the chutes (The larger number of chutes makes the bias smaller
because the device provide better result to split the sample. And to reach the lowest
bias, it have to be an equal number of chutes)
◦ Compromises an even number, but not less than a total of eight (usually between
12 and 20)
◦ The number of the chutes have to be an equal number for the both sides
(adjacent chutes discharging at opposites sides)
• Wall dimension of chutes (it must be thin in relation to the wall-to-wall dimensions
of the chutes themselves to get the low bias).
• The Chutes Slope (to provide material flow down properly to depress the bias)
◦ Range between 45o until 60o
4 Material feeding
• The material that will be split have to spread evenly on a rectangular scoop designed
so as to fit splitter width.
• The scoop open end covers the set of chutes exactly and the scoop edge is placed in
the middle of the chutes
 •The material must be fed perpendicularly to the longitudinal axis
•The scoop must be discharged slowly and evenly to allow the materials flow freely
down the chutes.
5 Equipments Cleaning
• It is required to clean and brush both the chutes and scoop to remove the adhered
fine particles to their surface in order to make the materials flow properly
• To minimize the decontamination effort, disposable drying trays are recommended.
6 Split Replication
• Implement an even better than an odd number of riffling stage.
• When sampling for technical purposes, it should be alternated the choice of the
right and left sample
• When sampling for commercial purpose, the split sample must be chosen at random

b. Describe an unbiased procedure/device for representative mass reduction.

Answer :
Unbiased Procedures/Device for representative mass reduction of “Vario Divider” as
describe bellow.

A. Vario Divider Description

▪ The splitting principle which same as riffle splitters and Boerner divider, is that
every second chute contributes to one of two alternative collecting reservoir – or to
more than two, resulting in variable split rations.
▪ The revolving feeding funnel distributes the sample material equally (in time) over a
number of radial chutes (assuming constant rotational speed). It provide equally
reliable mass reduction.
▪ In this journal, they used 1 G/1-4 Model . The specification of this Vario Divider i.e.
• It designed for grains samples, 1 sample, 4 outlets of which 1, 2 or 3 can be
covered to obtain larger dividing ratios

B. Vario Divider Precision and Accuracy

▪ The precision of this device depend on the rotating speed as the influx velocity of the
material through the feeding funnel and the grain-size contrast of the material.
▪ The accuracy of the dividing depends on the number of subsamples. To obtain the
greatest accuracy, the time taken for dividing must be never be less than 20 seconds.

C. Vario Divider Advantages

▪ It require very little maintenance
▪ The method was very easy and fast to use, so has no user-dependency
▪ It is possible to get a mass reduction ratio as small as 1:100 (dependently particle
size of samples)

D. Vario Divider Disadvantages

▪ Splitting the samples in many streps result higher error since every single step is
error generating.
▪ The loss material caused by rebounding of the rape seeds from the sample boxes.
▪ Set-back would appear to be difficulty to cleaning sticky materials and immobility
when needed in fieldwork.
E. Operational Procedures
For the example 4 kg samples should be divided into 2 samples of 1 kg each (e.g. 1
sample and 1 copy sample)
1. The handle (10) is moved to position (4) on the scale
2. Sample trays (7) and (8) are placed in position.
3. Check the hopper is of the correct size then start the divider by
turning the switch on.
4. The sample to be divided poured through a hopper (1) It must
be fed perpendicularly to the longitudinal axis to led it down
into a revolving feeder (2). Wait approximately 15 seconds.
With sample less than 4 kg, it is necessary to use an inlet
hopper with a smaller outlet hole. The sample have to divided
in at least two steps for a realistic testing of vario dividing
principle.
5. Material continued to a chute opening (11) or to the bottom as left-over material (9). In
order to make it flow properly, the chutes must be cleaned well and free form sticky
materials.
6. The machine gives two equivalent samples (7) and (8). The number of subsamples can
be calculated by multiplying the number of rotations of revolving feeder (40 rpm) with
the number of outlet. Considering the purpose of the sampling (technical or
commercial) to define which sample should be taken.

(1) Hopper
(2) Revolving Feeder
(3) Motor
(4) Chute Closer
(5) Sample Outlets
(6) Sample Outlets
(7) Sample
(8) Sample
(9) Left-over material
(10) Chute Opening Handle
(11) Chute

E. Summary of The Characteristics for Vario Divider

Characteristics Score Note
Composition + Standard Deviation (); Relative Bias (); Representativeness ()
Mass + Standard Deviation and Relative Bias of the Final Sample Mass ()
Loss + Total Loss of Material ()
Cleaning - Easiness to clean ()
Initializing + Simplicity Initializing Procedures () and Initialing Time ()
User-dependency + User-dependency ()
Time + Operating Time ()
Score 5 Defined in Very Good (Sum=5) Method/Device
c. Describe a biased procedure/device for mass reduction. Identify the source of bias.
Answer :
Biased Procedures for representative mass reduction of “Alternate Shoveling” as describe
bellow.
A. Alternate Shoveling Description
▪ The method is based on the principle that all
extracted shovelfuls from the original sample are
deposited sequentially in two alternative heaps as
illustrated in the right picture .
▪ The mass is reduced into two samples with almost
equal weight and (hopefully) equal composition.
▪ This is an example of correct an incorrect shovel
design
Incorrect Design Correct Design

Round shape : material at the top of a Square Shape : all material has the same
flattened sample has more chance to be chance to be part of the increment
part of an increment than the material at
the bottom

B. Alternate Shoveling Precision and Accuracy

▪ The precision of this device depend on the consistently of the samplers while taking
the increments.
▪ The accuracy of the dividing depends on the number of scoops. The larger number
of scoops, the better reduction. Increasing the number of increments should
minimize the effect of the grouping and segregation error.

C. Alternate Shoveling Advantages

▪ More reliable and accurate than coning and quartering
▪ The method is quick and cheap in operation

D. Alternate Shoveling Disadvantages

▪ The equality of the final samples will be highly dependent on the nature of the lot.
▪ Some sample loss was observed due to the practical handling of shovelfuls
▪ Different Operators will have unequal quality of the final reduced samples.
▪ Each scoop tends to select particles adjacent to each other, maintaining much of the
naturally occurring grouping and segregation error.
▪ The analyst must balance the extra time required for small scoop sizes to achieve a
lower grouping and segregation error with being able to accomplish all the
shoveling steps in the time available for sample processing.
▪ The procedure may need to be repeated until the sample is reduced to the mass
required for chemical or physical analysis.
 E. Operational Procedures
▪ Extract the material to be sampled one shovelful at a time and place it in two
alternating distinct heaps.
▪ All shovelful should be approximately have the same size and each heap should
consist of the same number of shovelfuls.
▪ One heap should contain only odd increments and the other only even increments.
▪ The increments should be the same size and the minimum number of increments
should be around nine (9) for each pile.
▪ One pile is then randomly chosen and subsequently shoveled into two new smaller
piles and so forth.
▪ Sample selected at random to preserve the sampling equity.

E. Summary of The Characteristics for Alternate Shoveling

Characteristics Score Note
Composition - Standard Deviation (); Relative Bias (); Representativeness ()
Mass - Standard Deviation and Relative Bias of the Final Sample Mass ()
Loss 0 Total Loss of Material (can not be defined)
Cleaning + Easiness to clean ()
Initializing + Simplicity Initializing Procedures () and Initialing Time ()
User-dependency - User-dependency ()
Time - Operating Time ()
Score -2 Defined in Poor (Sum < 2) Method/Device

5. Case study 1-D (gas production plant). In a biogas production plant, the formation of the
major product (methane, CH4) and some contaminant by-products, such as hydrogen sulphide
(H2S), must be controlled. To do so, the yield of these two compounds is determined daily as a
part of a systematic quality assurance program. Since the complete process of biogas
production takes around two-three weeks, a daily control is considered to be sufficient.
Previous studies showed that the yield of CH4 and H2S is not correlated at all and, therefore, an
independent variographic analysis of each compound should be carried out. The results are
represented in Figure 1 and 2.

Figure 1. Variogram and error map for H2S.

a) Describe the H2S variograms. Try to estimate the nugget effect, sill and range
Answer :
The Variogram of H2S describe bellow.
A. Origin Data of Variogram
▪ Variogram data consists of H2S concentration in produced biogas.
▪ The data have taken in 3 months (January to March, 2005) to obtain 90 samples. By this
means the concentration of H2S was recorded daily as primer data.
B. Variogram Type
▪ The type of the variogram is cyclic.
▪ The graph is cyclic in every 7 days.
▪ The cyclic period is related to the premix capacity per week, which will be restricted
during weekend when there is lag of industrial waste being mixed in bioreactors that can
change the profile of raw material of biogas. The amount of Industrial waste which
consist of iron chloride will reduce the H2S content and makes the concentration of H2S
drop centered on the weekend.
C. Variogram Characteristics
▪ Nugget Effect,
• The value is around 0.005
• By this means, the H2S concentration
is still relatively heterogeneous.
▪ Sill
• The estimated of overall sill is around
0.075; or to different ± 0.070 between
the overall sill and the nugget effect.
▪ Range
The distance at which variogram reaches the sill (Range) is ± 14 days

Figure 2. Variogram and error map for CH4.

a) Describe the CH4 variograms. Try to estimate the nugget effect, sill and range in each case.
Answer :
The Variogram of CH4 describe bellow.
A. Origin Data of Variogram
▪ Variogram data consists of CH4 concentration in produced biogas.
▪ The data have taken in 3 months (January to March, 2005) to obtain 90 samples. By this
means the concentration of CH4 was recorded daily as primer data.
▪ But the data of increments No. 2 and 56 are outliers that fatally influenced the Variogram
analysis.
 B. Variogram Type
▪ After remove the significant outliers (increments number 2 and 56), the type of the
variogram appear as cyclic.
▪ The graph is periodically cyclic in 20±2 days (~ 3 weeks)
▪ The cyclic period is related to the transportation of animal manure in which small farm
deliver raw manure weekly while larger farm per 3 weeks.

C. Variogram Characteristics
▪ Nugget Effect,
• The value is not negligible (± 0.001)
• It is mean that the variability of the CH4
concentration is still big since all the
type of waste are heterogeneous
(consists of 60% cow manure, 20% pig
manure, 20% organic industrial food
processing waste)
• Pre-mixing with collect and deliver the
the type of manure to plant, will help to bring constant overall raw material
composition.
▪ Sill
• The estimated of overall sill is around 0.009; or to different ± 0.008 between the
overall sill and the nugget effect.
▪ Range
• The unclear range display on the variogram. But it may around ~ 6-8 days.

b) Design a sampling strategy valid to control simultaneously the yield of H2S and CH4.
Answer :
Valid Sampling Strategies Design to control simultaneously the yield of H2S and CH4
(1) It need composite sampling because both of the the nugget effect is not negligible.
(2) Use Stratified Random for sampling
◦ The cyclic variogram indicate that there were found heterogeneity of H2S and CH4
concentration within one period (dissimilar population).
◦ Stratified random sampling is most appropriate when the entire population from which the
sample is taken is heterogeneous.
◦ To obtain representative sample, increment must be taken randomly per stratum (a period
which is defined based on H2S and CH4 sharing a specific attribute or characteristic).
(3) Sampling Rate, The Sample must be taken below range
◦ For controlling H2S concentration, the range is ± 14 days. This means, sample may took
per 2 weeks. Since composite sampling is needed, increments should be taken. It is
recommended to take sample within a periodic cycle (variogram cyclic in every 7 days)
◦ Range in CH4 controlling is ~ 6-8 days. So, the increments should be taken bellow 6 days.
◦ Concerning in efficiency, sampling may done in two purpose (H2S and CH4). Because of
the range of CH4 is lower than H2S (but nearly with the H2S cyclic), the sampling should
be taken below 1 week with increments. The number of increments may calculated based
on defined target error (usually 10%).
◦ From figure 2. Increments may take bellow the range 7 (lag 2) as much as 2 increments to
achieve Total Sampling Error bellow 10% (9.33% of error)
c) Comment on possible options to perform the sampling operation to determine the CH 4 yield
achieving a Total Sampling Error below 15%. Answer :
Possible options to perform the sampling operation to determine the CH4 yield to achieve TSE
< 15% mentioned bellow.
Option 1. Option 6.
Number of Increment : 1 Number of Increment : 8
Lag J : 2 TSE achievement : 13.198 % Lag J : 10 TSE achievement : 8.383%
Comment. Comment.
The number of increment is not enough to This option reduce TSE of option number 5
get the representative sample because the by take more increments in the same lag, but
nugget effect is not negligible and needs still not applicable to control the yield of
composite sampling. CH4 since the sampling done > range.
Option 2. Option 7.
Number of Increment : 2 Number of Increment : 4
Lag J : 2 TSE achievement : 9.333% Lag J : 24 TSE achievement : 14.523%
Comment. Comment.
It is sufficient to collect increments as much Regarding to the sampling rate, increments
as 2 increments per 2 days. Moreover if must be taken < range (range for CH4 is ~6-
tightened sampling is applied (< 10%) to 8 days). Although this scheme has sufficient
control CH4, this scheme is useful. number of increments, it can not be applied
to control CH4 yield (lag > Range).
Option 3. Option 8.
Number of Increment : 4 Number of Increment : 8
Lag J : 2 TSE achievement : 6.599% Lag J : 24 TSE achievement : 10.269 %
Comment. Comment.
Higher increments take in the same lag will Same with option 7, this scheme is not
reduce the TSE. Another concern is the suitable to control CH4 yield in terms of
availability of sampler and sampling sampling rate (must be < range) although
equipments for this increments. they reduce the TSE with take more
increments in the same lag.
Option 4. Option 9.
Number of Increment : 8 Number of Increment : 4
Lag J : 2 TSE achievement : 4.666% Lag J : 43 TSE achievement : 14.838 %
Comment. Comment.
This is the best sampling scheme in terms of This is the most simple and practical one to
TSE achievement. But the increments that have composite samples since only 4
should be taken are enormous and run out increments per 43 days. But, when it come
from efficiency if (far away or) not suitable into CH4 discussion which sampling must be
on the defined target (<<< 15%). taken bellow range (~6-8 days), this scheme
is not applicable.
Option 5. Option 10.
Number of Increment : 4 Number of Increment : 8
Lag J : 10 TSE achievement : 11.855 % Lag J : 43 TSE achievement : 10.492%
Comment. Comment.
TSE of this scheme still bellow 15% with Not suitable to obtain representative sample
adequate increments. But It is not suitable to because the Lag is very high (>>> Range)
apply to control CH4 since the Lag > Ratio.
Conclusion
To obtain the representative sample to control CH4 yield with TSE target as much as 15%, we have
to concern about the sampling strategy requirements (Number of increments, and sampling rate
(range > lag)). So we have 3 rules which must be obeyed to get the representative sample, i.e.
1. Number of increment > 1 increment
2. Lag < Range (~6-8 days)
3. Total Sampling Error (TSE) < 15 %
From mentioned options, it can be defined the most suitable scheme for sampling to control CH4
yield. Option 2 is recommended as a guide of sampling scheme since it fulfill all of the requirement
of 3 rules listed in above. It is quite adequate for the number of increments (2 increments) and no
need many samplers or sampling equipments to take the increments (relatively no need higher cost
than other options which have more increments). The sampling rate also meet the rule which must
be done bellow the range. The only disadvantage is it may have tightened sampling scheme since
the TSE relatively quite far from target error, but it can be re-evaluated in the future based on
sampling history. If this sampling scheme success to control CH4 properly, the lag should be re-
calculated in between 2 until ~6-8 days to come closer with TSE 15%.

ANNEX -Useful formula-

 1 1  (1- aL/α)2
s (FSE ) = Cd 
2 3
−  C = cfgβ c= ρc + (1- aL/α) ρm
M
 S ML  aL/α

CV   = 100 × s 2  FSE  For more than one source of error: CV total  = 100 × ∑ s
i
2
i

EXCEL HINTS
SOLVER tool
To optimize a parameter of Gy’s equation in order to reach a certain error level for FSE, you
may use the SOLVER tool. You should introduce the Gy’s formula in the objective cell and ask for
an optimization varying the suitable parameter (particle size, sample mass,…) in the changing cell.
The goal of the optimization is making the value of the objective cell equal to the desired error
level by modifying the parameters in the changing cell. After running the SOLVER tool, the result
of the objective function will get close to the error level desired and the changing cell will adopt the
optimized value.
 Objective cell: it should contain the equation to be optimized (the Gy’s formula in this case).
When writing the equation, the cell containing the parameter to be modified should be called.
 Changing cell: it should contain a number, an initial guess of the parameter to be optimized.
Syntax: Tools –SOLVER
Dialog box: objective cell (mark cell with Gy’s formula)
Objective cell value: equal to s2(FSE) (numerical value)
Changing cells: (mark cell with parameter to be optimized)
Resolve
CONTOUR PLOTS
Represents a flat plot of z values (with contour lines) vs. x/y pairs. A table with the z values
for the different x/y pairs should be calculated (WARNING!!! values in x and y axes should be
equispaced).
Select the whole table of x,y,z values
Syntax: plot wizard icon – Surface – contour plot
To modify intervals among contour lines, click legend and change scale values (may vary according
to EXCEL version).