Quo Vadis work package 4

1. Quo Vadis work package 4 Sampling and sample preparation By Geert Cuperus (Tauw) TAUW VTT INFA INSTITUTE

2. Contents • Background • The new standard • Validation of sampling and sample preparation • Ruggedness testing

3. 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

4. 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 Mass reduction Size reduction Analysis

5. The new standard – EN 15442 • Lot size (period of production) • Number of increments • Size of increments • Distribution of increments • Sample size

6. The new standard – EN15442

7. The new standard – EN 15442 • Minimum sample size:

8. 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

9. Sampling at 5 sites Sampler 1 Sampler 2 Sampler 3 Sampler 4 Sampler 5 A A A A A B B B B B Validation of sampling

10. 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

11. Validation of sampling Sample preparation Quartering

12. Validation of sampling Sample preparation Splitting

13. Sample 5 sites Primary splitting or quartering Subsample Subsample Secondary splitting or quartering A1 A2 A3 A4 Validation of sampling

14. 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

15. Validation of sampling

16. Validation of sampling Validation of sampling => total standard deviation Validation of sample preparation => minus sampling Therefore:

17. Validation testing on sample preparationShare sampling in total repeatability

18. 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

19. Ruggedness testing • Several method parameters affect the reliability of EN15442 • Of these, the lot size and the number of increments are considered most important

20. 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

21. Ruggedness testing Sampling at 4 sites 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 5 samples A-E

22. Ruggedness testing Sampling at 4 sites 500 ton 1.500 ton 2.500 ton 3.500 ton 5 samples A-E 5 samples A-E 5 samples A-E 5 samples A-E

23. Ruggedness testing on sampling Results repeatability versus number of increments

24. Ruggedness testing on sampling Results repeatability versus lot size

25. 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

26. Conclusion • Much work has been done now • Go and try the standard for yourself!! THANK YOU