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Sampling, Sieving, Imaging, &
Correlating the Data Between the Two
Presenters:Kyle James – Verder Scientific Inc.
Gert Beckmann – Retsch Technology
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Areas of DiscussionTOPICS
2© Retsch GmbH
1.) Sample Acquisition: Sampling Methodology & Techniques
2.) Sieve Analysis: Principles / Techniques / Concerns
3.) Dynamic Image Analysis: Methodology / Technique / Correlation
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Quality Control / R&DApplications
3© Retsch GmbH
Defined product properties
Detected product properties
Agreement
Certain properties are to be achieved when products are manufactured.These depend on the particle size and the particle distribution.
Particle size/distribution = product property
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Particle Sizing ExampleWhy it Matters
4© Retsch GmbH
Example: CoffeeThe particle size determines important taste properties
Too coarsely ground coffee: the brewing process is accelerated and gives a watery cup of coffee
Too finely ground coffee: too many aromatics, acids and bittering agents are dissolved, the filter could be blocked
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Sample Acquistion
5© Retsch GmbH
The bigger the particle size, the more difficult it is to attain the representative part sample
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Sampling Process
6© Retsch GmbH
Transports(belt,container, train and truck)
Accumulation(filling, feeding)
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Sample Amount
7© Retsch GmbH
Qmin = 0.07 * dmax / ρ
Qmin = mass of a single sample [dm3]
dmax = maximum particle size [mm]
0.07 = factor [kg/mm]
ρ = bulk density [kg/dm3]
Minimum volume (Qmin) of a single samplewith grain sizes (dmax) < 120 mm
DIN 51701 part 2 - Sampling of solid fuels -
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Standard Deviations of Various Sample Divisions Methods
8© Retsch GmbH
qualitative variation
Sample divider PT 100
Random sampling
Sample splitter
Cone and quartering
qualitative variation0 1 2 3 4 5 6 7 8 9 10 %
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Coning and Quartering
9© Retsch GmbH
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Stream of material
Single sample
Sample Extractor Chute
10© Retsch GmbH
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Sample Extractor Bucket
11© Retsch GmbH
Stream of material
Single sample
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Sample Extractor
12© Retsch GmbH
Stream of material
Single sample
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Sample Dividers from Retsch
13© Retsch GmbH
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Sample Splitters
14© Retsch GmbH
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Rotary Tube Divider PT 200
15© Retsch GmbH
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Laboratory Sample Divider PT 100
16© Retsch GmbH
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4 accurate particle size analyses= 4 different results!
Importance of sample divisionSample division
17© Retsch GmbH
xc_min [mm]0.5 1.0 1.5 2.0 2.5 3.00
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Q3 [%]
randomsampling
sample material: standard sand
*,* = nominal values of standard sand
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xc_min [mm]0.5 1.0 1.5 2.0 2.5 3.0 3.50
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Q3 [%]
Importance of sample divisionSample division
18© Retsch GmbH
sample splitter
sample material: standard sand
*,* = nominal values of standard sand
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Importance of sample divisionSample division
19© Retsch GmbH
xc_min [mm]0.5 1.0 1.5 2.0 2.5 3.00
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Q3 [%]
rotating sample divider
PT 100
4 accurate particle size analyses= 4 similar results!
sample material: standard sand
*,* = nominal values of standard sand
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Sieveability of particlesSieving
20© Retsch GmbH
Free flowing particles
Van-der-Waals forces
Fluid bridges
Electrostatic Forces
Agglomerated particles
+ -
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Sieving aidsSieving
21© Retsch GmbH
• Aerosil
• talcum powder
• aluminum oxide
solid
• wet sieving
• degreasing:
benzinealcohols
liquid
• chain rings
• brushes
• cubes
• rubber balls
• agate balls
• steatite balls
mechanical
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Test sievesthat comply with standards Test sieves
22© Retsch GmbH
If sieve analysis is used for quality controlwithin the context of DIN EN ISO 9000:2000
then both the sieve shaker and thetest sieves must be subjected to
test agent monitoring.
w = mesh widthd = wire diameter
w
w
Ø d
Ø d
Tolerance for mean value (Y):The mean value of the mesh widthmust not differ from thenominal value w by more than thetolerance ± Y.
Technical requirements & testingaccording to ISO 3310
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100 200 300 40040 50 60 70 80 90particle size x[µm]
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Q3 [%]
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Q3 [%]
44%
+Y 66,4
36%
-Y 59,6
Importance of mesh widthConsequences of tolerances Test sieves
23© Retsch GmbH
63 µmtolerance ± Y = 3,4 µm
40%
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Real Mesh WidthReal Mesh
24© Retsch GmbH
x [µm] 200 400 600 800 1000 1200 0
10
20
30
40
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60
70
80
90 Passing [%]
Sample-1__xc_min_002.rdf Sieving-upper-range-S1.ref
Excellent correlation
when using the real mesh opening sizes
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Influence of Mesh WidthMesh measurements
25© Retsch GmbH
1400µm 1400µm 1429.5µm
Nominal Sieve Mesh = 1400µm Real Sieve Mesh >1400=1455
only beads < 1400µm
will pass the sieve mesh
beads > 1400µm will not pass the sieve mesh
Upper mesh size range ~1455µmsieve No. 03033531 (nominal 1400µm)
Theory: Reality:
Mesh sizes warp Mesh sizes weft
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Calibrationcertificate
26© Retsch GmbH
Nomial mesh width
Tolerances
Number ofmeasured apertures
Mean mesh width
Standard deviation σ
Wire diameter
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Sample AmountSieve Analysis
27© Verder Scientific Division
4 mm2 mm1 mm
500 µm250 µm125 µm
63 µm45 µm
collecting pan
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Sieving Methods forparticle size determination Basics
28© Retsch GmbH
Horizontal sievingVibratory sieving Air jet sievingTap sieving
dry wet
vibratory
horizontal
tap
air jet
AS 200 jet AS 200 tap AS 200 AS 300 AS 400 AS 450 control
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Selection of amplitudeVibratory sieve shakers
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0
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90
100
Q3(
x) /
%
10 50 100 500 1000 5000Particle size / µm
Quartz,sieving time: 5 min.
AMP- 2 mmAMP- 0.5 mmAMP- 1.2 mm
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Statistical resonanceVibratory sieve shakers
30© Retsch GmbH
T = periodic time of sieve bottom vibration
particle
sieve bottom
t
A
T T
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Sieve analysis procedureProcess
31© Retsch GmbH
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Potential Concerns & IssuesSampling & Sieving
32© Retsch GmbH
1.) Sampling problems:Sampling Technique (pouring and “spooning“)Material Behavior & Composition
2.) Sieving problems: Sieve OverloadSieving Technique / Technology UsedNominal Size Real Mesh SizeMaterial Behavior & Composition
3.) Scale Problems:Low Resolution (0.1g of sample)Not Sensitive Enough (sieves vs actual)
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Digital Imaging SievingImage Analysis
33© Retsch GmbH
x [µm]200 400 600 8000
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90
Q3 [%]
RT669_3993_Z_LB_05%_xc_min_001.rdfRT669_RT_3993.ref
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Particle SizeMorphology
34© Retsch GmbH
xcmin
xc min
“width”
A
A‘ = Ax a
rea
“diameter overprojection surface”
xarea“length”
xFe max
xFemax
CAMSIZER results are
compatible with
sieve analysis
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Digital Image ProcessingComparison
35© Retsch GmbH
x [mm]0.1 10
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
Q3
Tinovetin-B-CA584A_BZ_xc_min_002.rdfSyngenta-1mm-2min-Sieb.ref
--- width measurement
-*- Sieving
comparisonCAMSIZER-measurement xc min (red)and sieving * (black)
xc min
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Ellipsoid ParticlesComparison
36© Retsch GmbH
x [mm]1.0 1.25 1.5 1.75 2.00
10
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Q3 [%]
rice
xcmin
A‘ = A
x are
a
A
Red CAMSIZER curve of particle width gives excellent correlation
at the black sieve points
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Lenticular ParticlesComparison
37© Retsch GmbH
x [mm]0.2 0.4 0.6 10
10
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50
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Q3 [%]
Sample A_BZ_0.2%_xc_min_001.rdfSample A_.ref
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Digital Imaging SievingLenticular Particles
38© Retsch GmbH
x [mm]0.2 0.4 0.6 10
10
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Q3 [%]
Sample A_BZ_0.2%_xc_min_001.rdfSample A_.ref
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Digital Imaging SievingCubes / Angular
39© Retsch GmbH
x [µm]200 400 600 8000
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Q3 [%]
RT669_3993_Z_LB_05%_xc_min_001.rdfRT669_RT_3993.ref
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Angular ParticlesCoal, Sand, Sugar
40© Retsch GmbH
x [µm]200 400 600 8000
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Q3 [%]
RT669_3993_Z_LB_05%_xc_min_001.rdfRT669_RT_3993.ref
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Angular ParticlesShell Limestone
41© Retsch GmbH
xc_min [mm]0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.80
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Q3 [%]
Muschelkalk_xc_min_001.rdfRT3204_Muschelkalk_Sieb.ref
*Sieve Analysis -CAMSIZER
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Digital Imaging SievingAngular
42© Retsch GmbH
x [µm]200 400 600 8000
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Q3 [%]
RT669_3993_Z_LB_05%_xc_min_001.rdfRT669_RT_3993.ref
x [µm]200 400 600 8000
10
20
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Q3 [%]
RT669_3993_Z_LB_05%_xc_min_001.rdfRT669_RT_3993.ref
angular particles without fitting
CAMSIZER-measurement xc min (red)sieve analysis * (black)
angular particles with Q3-fitting
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Digital Imaging SievingDistribution
43© Retsch GmbH
Two samples with different width of distributionbut …
… with similar shape
(= same product type)
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Limitations of Old ProceduresOld vs New
44© Retsch GmbH
xc_min [mm]1.0 1.5 2.0 2.5 3.00
0.1
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0.3
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0.5
0.6
0.7
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Q3
CAMSIZER Elementary – Fittingxc_min [mm]1.0 1.5 2.0 2.5 3.0
0
0.1
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0.3
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0.5
0.6
0.7
0.8
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Q3
xc_min [mm]1.0 1.5 2.0 2.5 3.00
0.1
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0.5
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0.7
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0.9
Q3
Old fittingmethods
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Digital Imaging SievingElementary Fitting
45© Retsch GmbH
Single class:Taken from the sieve stackand measured in CAMSIZER
For creating a CAMSIZER Elementary
fitting file use the more narrow sample
(green)
Elementary fitting with single (narrow) sieve class.It can be the sieve with the highest amount, one above or one below
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Digital Imaging SievingElementary Fitting
46© Retsch GmbH
xc_min [mm]1.0 1.5 2.0 2.5 3.00
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Elementary - Fitting
New elementary fitting with single (narrow) sieve class and entire distribution
{
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Measurement of Single ClassSingle Size
47© Retsch GmbH
xc_min [mm]1.0 1.5 2.0 2.5 3.0 3.50
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Try to geta single sieve class
as narrow as possiblein the middle
of the distributionof the sample
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Elementary Fitting in PracticeSet-up
48© Retsch GmbH
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Elementary Fitting in PracticeSet-up
49© Retsch GmbH
Try to get a singlesieve class as narrowas possible ~ in the
middle of thedistribution of the
sample
Try to get a sample ofyour product as
narrow as possible
Try to get a sample ofyour product as
narrow as possible
Try to get a single sieve classas narrow as possible
in the middle of the distributionof the sample
![Page 50: Sampling, Sieving, Imaging, Correlating the Data Between ... · If sieve analysis is used for quality control. within the context of DIN EN ISO 9000:2000. then both the . sieve shaker](https://reader034.vdocuments.us/reader034/viewer/2022042110/5e8a465f50e3f233a656303c/html5/thumbnails/50.jpg)
Elementary Fitting in PracticeSet-up
50© Retsch GmbH
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Shell LimestoneExample
51© Retsch GmbH
xc_min [mm]0.4 0.6 0.8 1.0 1.2 1.40
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Muschelkalk_xc_min_001.rdfRT3204_Muschelkalk_Sieb.ref
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Multimodal DistributionExample
52© Retsch GmbH
x [mm]0.2 0.4 0.6 0.8 1.0 1.2 1.40
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SU_Demo02-05_Standaard_BZ_LB_Gl15_03%_xc_min_001.rdfStandaard.ref
x [mm]0.2 0.4 0.6 0.8 1.0 1.20
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SU_Demo02-05_Mix_BZ_LB_Gl15_03%_xc_min_001.rdfMix-Opzak-and-stMG4502.ref
Excellent sievecorrelation evenwith bimodal or
multimodal distributions
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SummaryCorrelation Wrap-Up
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CAMSIZER® Elementary Fitting:• For samples with similar shape• Fitting of different width of distribution possible
(even multimodal distributions)• Applications: Sand, Sugar, Fertilizer, Minerals, Plastics,
Foodstuffs ... and many more• Creating a CAMSIZER® correlation method
only takes 20 minutescompared to 3 hours with competitive instruments
Samples with varying particle shape, e.g. abrasiveswill need different fitting files or CAMSIZER Meta-Fitting®
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Thank you for yourattention !