Industrial production of iron ore

Example featuring:

Range statistics for estimation

of sampling uncertainty

Uncertainty in Sampling
Nordtest Workshop
12th – 13th April 2007
Hillerød, Denmark

Presented by Bertil Magnusson, SP, Sweden

 Background
LKAB is in every sense a high-tech processing industry.
The iron ore from the underground mines in Kiruna and Malmberget
is upgraded step-by-step in a long process
LKAB’s main product range, iron ore pellets, is produced from finely
ground highly concentrated iron ore mixed with additives (one or
more of dolomite, olivine, quartzite and limestone) and a binder
before rolled into 10-15mm balls prior to oxidizing sintering at
1250°C.

The industrial site at Kiruna,

with the KK3 pelletizing
plant in the foreground.
The sampling target is one day
(24h) of pellet production

Uncertainty in sampling - iron ore 2007-04-11 2

Measurand & Uncertainty estimation
Measurand
Analyte & Unit Sector & Sampling target
technique matrix
Total iron % Fe dried Mining Lot – 24 hours
XRF sample iron ore production

Uncertainty estimation
Purpose Design Statistics
Uncertainty Empirical Range
of sampling replicates (standard dev. can also be used)

Uncertainty in sampling - iron ore 2007-04-11 3

Nordtest uncertainty guide – 10 steps

1. Scope
2. Scenario and sampling target
3. Sampling procedure
4. Study design – double split replicates
5. Sample preparation and analysis
6. Results
7. Comments
8. Assessment of fitness for purpose
9. Reporting and interpretation
10.Summary

Uncertainty in sampling - iron ore 2007-04-11 4

Scope & Sampling target

• What
– Sampling uncertainty for iron content in the produced highly
upgraded iron ore pellets
• How
– Sampling according to the ISO protocol 3082 for iron ores
– Evaluation of duplicates

• Sampling target
– One day (24 h) of pellet production

Uncertainty in sampling - iron ore 2007-04-11 5

Sampling procedure ISO 3082:2000. Iron ores – Sampling
Process step Form of material Description of process step

Sampling Target Collection of increments into

Sampling a production day (24h)
15 0000 tons 24 (1 h) composite samples (24 • 300 kg)

Primary Sample Automatically grinding and comminution of

7.2 tons (24 • 300 kg) each composite samples to 30 g

Sub-samples Automatically mixing into

24 • 30 g three 8 h 240 g shift samples
Physical sample
preparation
Laboratory sample Mixing into one 720 g sample and
3 • 240 g mechanical splitting to 150 g

Test sample Drying 105 °C 2h

150 g

Test portion Fusion for XRF

0,5 g
Analysis
Test bead – XRF Analytical determination of iron
content
Uncertainty in sampling - iron ore 2007-04-11 6
Study design - double split replicates

LOT – production day

3 gross samples
8h shift –
2 400 kg A B C

3 laboratory samples A B C

6 test portions
X111 X2112 X121 X2122 X131 X2132

Design also to ISO 3085 Iron ores — Experimental methods for checking the
precision of sampling, sample preparation and measurement

Uncertainty in sampling - iron ore 2007-04-11 7

Comment on the design
No true sampling replication
• Use the three shifts as replication of sampling
• Sampling different in time!

Drawback
• IF variation in production – too high sampling
uncertainty

Benefits
• Can use production sampling without any changes in
production

Uncertainty in sampling - iron ore 2007-04-11 8

Sample preparation and analysis
• Sample split using mechanical splitter
• Test portion (0,5 g) fused into a glass bead
• Analysis with X-Ray Fluorescence (XRF)

Data from analytical laboratory

• Within laboratory reproducibility
s = 0,07 % Fe
• Standard analytical uncertainty
uc = 0,10 % Fe

Uncertainty in sampling - iron ore 2007-04-11 9

 Raw data – iron in iron ore

Lot date Lot Sample 1 Sample 2 Sample 3

xi xi11 xi12 xi21 xi22 xi31 xi32
% Fe % Fe % Fe % Fe % Fe % Fe % Fe

2005-12-14 68,11 68,03 68,15 68,09 68,11 68,16 68,14

2005-12-15 68,07 68,13 68,01 68,05 68,07 68,08 68,05

2005-12-16 68,06 68,05 68,08 68,09 68,04 68,05 68,06

2005-12-17 68,03 68,06 68,05 67,99 68,02 68,06 68,02

Uncertainty in sampling - iron ore 2007-04-11 10

Results - Analysis
Parameter Comment
% Fe
Mean range from duplicates 0.046
Stand dev. Estimated from range 0.041 s = range/1.128

Results - Measurement
Parameter % Fe Comment
Mean range from –triplicates 0.050
Standard dev. estimated from range 0.030 s = range/1.693

Uncertainty in sampling - iron ore 2007-04-11 11

 Results - Sampling

Parameter % Fe Comment
Measurement
Measurement – standard dev. 0.030 (sampling + analytical, n=2)
Analysis – standard dev. 0.041 Analytical part (n=1)
2
= 0.030 2 −  0.041 
Sampling– standard dev. < 0.01  2

Uncertainty in sampling - iron ore 2007-04-11 12

Comments

Very low sampling uncertainty!

Yes – sampling designed for more inhomogeneous

parameter like particle size distribution

Uncertainty in sampling - iron ore 2007-04-11 13

Nordtest uncertainty guide – 10 steps

1. Scope
2. Scenario and sampling target
3. Sampling procedure
4. Study design – double split replicates
5. Sample preparation and analysis
6. Results
7. Comments
8. Assessment of fitness for purpose
9. Reporting and interpretation
10.Summary

Uncertainty in sampling - iron ore 2007-04-11 14

 Assessment of fitness for purpose

YES - With this low sampling uncertainty this sampling

procedure for determining Fe in iron ore pellets is

fit for purpose

If a lower uncertainty is required it is the analytical part

that needs to be improved

Uncertainty in sampling - iron ore 2007-04-11 15

Reporting and interpretation
Standard measurement uncertainty from the laboratory is
uc = 0,10 % Fe

An analytical result in production can be reported e.g.

68,0% Fe ± 0.2% Fe
The results is given with an expanded uncertainty
(95 % confidence interval, k=2)

The measurement uncertainty based on only this

study will be only 0,08! – Only repeatability

Uncertainty in sampling - iron ore 2007-04-11 16

Laboratory ladder for iron ore pellets with Fe about 68 %
– uncertainty at 95 % confidence level (k=2)

Sampling < 0,02 % Fe

< 0,08 % Fe

< 0,14 % Fe

< 0,20 % Fe

Uncertainty in sampling - iron ore 2007-04-11 17

Summary

Expanded Uncertainty Target variability

Sampling Analytical Measurement Typical production
variation
< 0.02% Fe 0.20% Fe 0.20% Fe 0.32% Fe
measured under within
lab reproducibility
conditions

From this study

• Repeatability, analytical is 0,08 % (2s)
From laboratory
• Within-laboratory reproducibility is 0,14 % (2s)

Uncertainty in sampling - iron ore 2007-04-11 18

Conclusion

For the determination of iron in iron ore the

sampling uncertainty is:
low and fit for purpose

The low sampling uncertainty is due to a:

sampling design for more
inhomogeneous parameters

Lots of thanks to LKAB and personnel for support

of this project

Uncertainty in sampling - iron ore 2007-04-11 19