quo vadis work package 4
DESCRIPTION
Quo Vadis work package 4. Sampling and sample preparation By Geert Cuperus (Tauw) TAUW VTT INFA INSTITUTE. Contents. Background The new standard Validation of sampling and sample preparation Ruggedness testing. Background. Inhomogenity is the issue Shape Variability in shape and size - PowerPoint PPT PresentationTRANSCRIPT
Quo Vadis work package 4
Sampling and sample preparation
By Geert Cuperus (Tauw)TAUWVTTINFA INSTITUTE
Contents
• Background• The new standard• Validation of sampling and sample preparation• Ruggedness testing
Background
• Inhomogenity is the issue• Shape
•Variability in shape and size
• Occurance of substances•Many elements occur concentrated in particles•“99% of a substance in 1% of the SRF”•Subsamples keep containing such particles
Background
• Many types of SRF exist• Fluff as complex example• Sampling from static lots and stockpiles mostly occur• Sampling consists of a series of steps
Sampling Mass reduction Size reduction AnalysisMass reduction
The new standard – EN 15442
• Lot size (period of production)• Number of increments• Size of increments• Distribution of increments• Sample size
The new standard – EN15442
The new standard – EN 15442
• Minimum sample size:
pVC
pgDsM
2g
395m )(
)1(
6
π
Validation of sampling
• Procedure:•Five production sites•Samplers (5) apply EN15442 to draft a sampling plan•Sampling (duplicate) of selected batches•Evaluation of plans and sample performance by Tauw•Analysis of elements by one laboratory•Statistical analysis
Validation of sampling
Sampling at 5 sites
A B
Sampler 1 Sampler 2 Sampler 3 Sampler 4 Sampler 5
A B A B A B A B
Validation of sampling
SAMPLE PREPARATION• Samples to laboratory: < 5 kg.• Particle size < 30 mm.• Sample preparation = subsampling + comminution• WP4 investigated size reduction by
•Quartering•Splitting
Validation of sampling
Sample preparationQuartering
Validation of sampling
Sample preparationSplitting
Validation of sampling
Sample
SubsampleSubsample
Primary splitting or quartering
Secondary splittingor quartering
A1 A2 A3 A4
5 sites
Validation of sampling
• Field experience:•EN15442 was easy to understand and practicable•Some samplers indicated the standard is too extensive•Useful comments resulted•Proper sampling plans were drafted
Validation of sampling
Net calorific value Repeatability 2,3%
Reproducibility 3,1%
Chlorine Repeatability 20,5%
Reproducibility 23,4%
Antimony Repeatability 40,4%
Reproducibility 41,8%
Copper Repeatability 123%
Reproducibility 123%
Validation of sampling
2,
2,
2samplingextmeasurementotaltmeasurementotalsampling sss
Validation of sampling => total standard deviationValidation of sample preparation => minus sampling
Therefore:
Validation testing on sample preparationShare sampling in total repeatabilityParameter Site 1 Site 2 Site 3 Site 4
Dry matter 100% 86% 64% -826%
NCV 100% 97% -40% -150%
Chlorine -22675637% 52% -460% -1313%
Antimony -79900% -1500% -1018% -567%
Arsenic -602% -1393%All values equal
detecion limit 86%
Lead -1764% -272% -308% 87%
Cadmium -49640% 46% -133% -351%
Chromium 40% -336% -2350% 100%
Cobalt -6411% -2067% -843% 97%
Copper -1430 0 -2% 0
Manganese 52% -5114% 71% 80%
Nickel 94% -400% -1339% 100%
Mercury -4733628% 7%All values equal
detecion limit 100%
ThalliumAll values equal
detecion limitAll values equal
detecion limitAll values equal
detecion limitAll values equal
detecion limit
Vanadium 100% -247% 61% 96%
Validation of sampling
• Results were used to adjust EN15442• Practicable recommendations resulted• Errors of repeatability frequently higher than errors of
reproducibility• Repeatability variation frequently negative or >100%• Other sources of error therefore have larger influence
Ruggedness testing
• Several method parameters affect the reliability of
EN15442• Of these, the lot size and the number of increments
are considered most important
Ruggedness testing on samplingStructure of the investigation
• Preparation • Research topics
•Parameters: Cl, Hg, Cu, Cr •Sampling focused on influence number of increments
(12, 24, 36, 48 and 60)•Sampling focused on influence lot size (500, 1500, 2500,
3500)
• Field work at 4 sites (Italy, Norway, Germany, Belgium)
• Sample preparation & analysis• Calculation results and reporting
Ruggedness testing
Sampling at 4 sites
5 samples
A-E
12 increments 24 increments 36 increments 48 increments 60 increments
5 samples
A-E
5 samples
A-E
5 samples
A-E
5 samples
A-E
Ruggedness testing
Sampling at 4 sites
5 samples
A-E
500 ton 1.500 ton 2.500 ton 3.500 ton
5 samples
A-E
5 samples
A-E
5 samples
A-E
Ruggedness testing on sampling Results repeatability versus number of increments
0%
50%
100%
150%
200%
250%
300%
350%
400%
0 12 24 36 48 60
Number of increments
Rep
eata
bili
ty
Chlorine
Mercury
Copper
Chromium
Average Cl, Hg, Cu and Cr
Ash
Ruggedness testing on sampling Results repeatability versus lot size
0%
50%
100%
150%
200%
250%
300%
350%
400%
450%
500%
0 500 1000 1500 2000 2500 3000 3500 4000
Lot size
Rep
eata
bili
ty
Chlorine
Mercury
Copper
Chromium
Average Cl, Hg, Cu and Cr
Ash
Ruggedness testing
• Optimum lot size is 2.500 ton (based on Cl, Hg and
Cr)• Optimum number of increments is 36• However: neither of these parameters dominate the
quality of a sample• Therefore 24 increments and lot size 1/10 of annual
production can well be applied
Conclusion
• Much work has been done now• Go and try the standard for yourself!!
THANK YOU