TITAN LE LIMESTONE/CEMENT/GYPSUM

Application

Michelle Cameron, Alexander Seyfarth

June 2013

August 25, 2015

XRF in the Cement Industry

More and more it is required to get

faster results and work “at line”
in the plant to troubleshoot an
issue or to make decision in the
quarry or silos

Innovation in ED XRF hardware,

resulted in smaller, compact
instruments with an increasing
performance to measure “light”
elements such as Na2O and MgO.

ED XRF both as HH (HAND HELD)

and BT (Bench Top) has grown to
fill more and more applications
previously limited to the “BIG”
WDX units

December 14, 2010 2

Cement Production Locations
Handheld XRF & Bench top EDX

1. Quarry 5. Raw-mill 9. Cooler

2. Crusher 6. Filter 10. Clinker
3. Conveyor 7. Pre-heater 11. Silo
4. Mixing bed 8. Kiln 12. Cement mill
13. Logistics
Cement Production Materials
XRF Application Areas

Saving time by being “AT LINE “or in the “FIELD”

• Raw materials from Quarry : elemental analysis of samples from exploration

or blast hole drilling (LIMESTONE)

• Feed stream: limestone, clay, quartz sand, fuel, gypsum, pozzolana and fly
ash

• Raw material (GYPSUM, SAND, FERRIC)

• Raw mix control

• Finished Clinker and Cement to “ID” material

• Cured Cement/Concrete to “ID” material and compare

FUTURE : COAL and FUEL analysis for receiving inspection

25 August 2015 4
Cement Production
Handheld APPLICATION areas

1. Quarry 5. Raw-mill 9. Cooler

2. Crusher 6. Filter 10. Clinker
3. Conveyor 7. Pre-heater 11. Silo
4. Mixing bed 8. Kiln 12. Cement mill
13. Logistics
Calibration of the analyzer

HH XRF

BT XRF

WD XRF

25.08.2015 6
The story of standard Geological
Calibrations (or Mining Calibrations)

• Standard Geochem calibrations are for a wide variety of

matrices, but perform the best on Silicate and
Aluminosilicate-type matrices.
• Many Mining (ore) applications are focused on either oxide or
sulfide ore with high metals content
• If Matrices far from these tend to have more uncertainty and
measurements become semi-quantitative at best for divergent
matrices.
• For cement applications, the matrix is carbonate vs. oxide, so
a separate application was developed to get good results on
limestone rich matrices.

December 14, 2010 7

HH and Benchtop Have Different Uses in
Cement Applications

Advantages of HH:
• Little or no sample preparation -
can be used on rocks and on
coarse or fine powders
• Can be easily taken to the field
and brought to the samples
• Quick screening tool

Limitations of HH:
• Large uncertainty – mainly
used for estimating raw material
content
• Light element analysis is
difficult due to no vacuum and
poor sample quality (cannot see
Na)
December 14, 2010 8
Measurement Approach

Loose powder in a
BT or DT stand

2 Min to 3 Min
measurement …

The longer the

better
Field or Rock-face measurement
LIMESTONE Application

• The Limestone application is designed with 3 USER SELECTABLE

calibrations”

• LIMESTONE (Carbonate bearing material)

• GYPSUM (GYPSUM bearing material)

• CEMENT (Ca,Al – Silicate bearing material)

• The calibration set is based on the same reference material set, but each
individual calibration uses different corrections and has the calibration line
optimized. Reporting is done as shown in next slides

25 August 2015 14
Calibration Setup

• Certified reference Material (NIST, ECRM, ,IPT, GBW) as well as RM

provided from various limestone quarries(EU,US,Canada,Chile) with
traceable fused bead XRF (S8 TIGER) analysis

• Prepared as loose powders with 4 micron Prolene™ foil

• 180 sec measurement time at 15kV with optimized current for the BRUKER
SDD detector electronics rate of 120 000 cps

• Instrument power level is <1 WATT to achieve this performance using the
SHARPBEAM™ technology including the patented TITAN DETETCOR
SHIELD™ to protect the detector

August 25, 2015 15

 Calibration MgO and CaO
Limestone matrix

80

50
70

60
40

XRF Concentration (%)

XRF Concentration (%)

50

30
40

30
20

20

10
10

0
0
0 10 20 30 40 50 60 70 80 90 100 0 10 20 30 40 50 60 70 80 90 100

Concentration (%) Concentration (%)

Conc. XRF Conc. XRF
 Calibration SO3

40

30

XRF Concentration (%)

20

10

0
0 10 20 30 40 50 60 70 80 90 100

Concentration (%)
Conc. XRF
 Calibration Info Limestone

Limestone/Raw Mix
Compound MgO CaO Al2O3 SiO2 P2O5 SO3 K2O TiO2 Mn3O4 Fe2O3
Range 0-81% 0-51% 0.02-28% 0.02-99% 0-20% 0-44% 0-3% 0-1.5% 0-1% 0-13%
SEC 1.1 0.8 0.5 0.8 0.2 0.06 0.05 0.01 0.01 0.2
LLD (pure SiO2) 0.5 0.003 0.06 0.02 0.003 0.01 0.003 0.002 0.002 0.002
Reported As MgCO3 CaCO3 Al2O3 SiO2 P2O5 SO3 K2O TiO2 MnO Fe2O3
SEC 2.2 1.4
LLD (pure SiO2) 1.05 0.01
 Calibration Info
GYPSUM and CEMENT

Gypsum
Compound MgO CaO Al2O3 SiO2 P2O5 SO3 K2O TiO2 Mn3O4 Fe2O3
Range 0-81% 0-51% 0.02-28% 0.02-99% 0-20% 0-44% 0-3% 0-1.5% 0-1% 0-13%
SEC 1.1 0.8 0.5 0.8 0.2 0.06 0.04 0.01 0.01 0.17
LLD (pure SiO2) 0.6 0.003 0.08 0.02 0.02 0.01 0.003 0.002 0.002 0.001
Reported As MgO CaSO4 Al2O3 SiO2 P2O5 SO3 K2O TiO2 MnO Fe2O3
SEC 1.9
LLD (pure SiO2) 0.01

Cement /Clinker / Raw Mix

Compound MgO CaO Al2O3 SiO2 P2O5 SO3 K2O TiO2 Mn3O4 Fe2O3
Range 0-81% 0-51% 0.02-28% 0.02-99% 0-20% 0-44% 0-3% 0-1.5% 0-1% 0-13%
SEC 1.1 0.8 0.4 0.8 0.2 0.06 0.04 0.01 0.01 0.17
LLD (pure SiO2) 0.7 0.003 0.08 0.02 0.02 0.01 0.003 0.002 0.002 0.001
Reported As MgO CaO Al2O3 SiO2 P2O5 SO3 K2O TiO2 MnO Fe2O3
 Typical Repeatability (60s)

Measurement Scan Time MgCO3 Al2O3 SiO2 P2O5 SO3 K2O CaCO3 TiO2 MnO Fe2O3
1 60 3.03 0.51 3.23 0.08 0.17 0.08 92.31 0.02 0.01 0.56
2 60 5.03 0.69 3.22 0.16 0.19 0.09 90.05 0.02 0.01 0.54
3 60 3.17 0.73 3.21 0.09 0.17 0.08 91.97 0.02 0.02 0.54
4 60 3.47 0.66 3.27 0.12 0.19 0.08 91.65 0.01 0.01 0.53
5 60 3.66 0.67 3.32 0.17 0.18 0.08 91.35 0.01 0.02 0.54
6 60 4.37 0.64 3.32 0.18 0.21 0.09 90.63 0.02 0.02 0.52
7 60 3.30 0.67 3.27 0.19 0.19 0.09 91.71 0.02 0.02 0.54
8 60 3.82 0.57 3.30 0.13 0.19 0.08 91.33 0.02 0.02 0.54
9 60 3.86 0.59 3.31 0.20 0.19 0.09 91.20 0.01 0.02 0.53
10 60 4.71 0.44 3.19 0.17 0.17 0.08 90.68 0.02 0.02 0.52
Average 3.84 0.62 3.26 0.15 0.19 0.09 91.29 0.02 0.02 0.54
Stdev 0.67 0.09 0.05 0.04 0.01 0.00 0.68 0.00 0.00 0.01
Reference 4.25 0.69 3.34 0.26 0.22 0.09 90.50 0.02 0.02 0.55
 Typical Repeatability (120s)

Measurement Scan Time MgCO3 Al2O3 SiO2 P2O5 SO3 K2O CaCO3 TiO2 MnO Fe2O3
1 120 4.61 0.58 3.37 0.20 0.20 0.09 90.37 0.02 0.02 0.53
2 120 5.01 0.67 3.28 0.19 0.19 0.08 90.03 0.02 0.02 0.52
3 120 5.65 0.59 3.20 0.14 0.20 0.09 89.59 0.02 0.02 0.50
4 120 4.05 0.50 3.13 0.12 0.18 0.08 91.38 0.02 0.02 0.53
5 120 4.34 0.72 3.28 0.06 0.18 0.08 90.79 0.02 0.01 0.53
6 120 5.99 0.65 3.19 0.15 0.20 0.09 89.18 0.02 0.02 0.51
7 120 3.36 0.64 3.42 0.18 0.20 0.09 91.54 0.02 0.02 0.54
8 120 4.72 0.69 3.36 0.12 0.20 0.09 90.28 0.02 0.01 0.52
9 120 2.84 0.59 3.28 0.08 0.18 0.08 92.36 0.02 0.02 0.55
10 120 3.71 0.52 3.42 0.09 0.20 0.09 91.39 0.02 0.02 0.54
Average 4.43 0.62 3.29 0.13 0.19 0.09 90.69 0.02 0.02 0.53
Stdev 0.99 0.07 0.10 0.05 0.01 0.00 0.98 0.00 0.00 0.01
Reference 4.25 0.69 3.34 0.26 0.22 0.09 90.50 0.02 0.02 0.55
Typical Repeatability (180s)

Measurement Scan Time MgCO3 Al2O3 SiO2 P2O5 SO3 K2O CaCO3 TiO2 MnO Fe2O3
1 180 2.7607 0.6134 3.3729 0.0605 0.1817 0.0848 92.341 0.0189 0.0155 0.5506
2 180 5.6655 0.6525 3.3008 0.1601 0.205 0.0887 89.3813 0.0169 0.0173 0.512
3 180 4.7933 0.5359 3.2878 0.1901 0.1974 0.0877 90.3585 0.0168 0.0143 0.5183
4 180 5.4103 0.5915 3.2512 0.1475 0.196 0.0848 89.7784 0.0164 0.0153 0.5086
5 180 4.1467 0.6736 3.3589 0.1364 0.2036 0.0883 90.8404 0.0195 0.0182 0.5146
6 180 5.4217 0.6872 3.2723 0.1584 0.1948 0.087 89.6355 0.0151 0.0152 0.5127
7 180 5.1799 0.6164 3.3619 0.1728 0.2054 0.0884 89.8243 0.0195 0.0173 0.5142
8 180 3.9286 0.5988 3.2728 0.0872 0.1812 0.0817 91.2907 0.0164 0.0174 0.5252
9 180 5.3484 0.5342 3.273 0.1699 0.1951 0.0866 89.8224 0.0199 0.0151 0.5352
10 180 4.3439 0.6165 3.2699 0.1538 0.2075 0.0903 90.7666 0.0178 0.0158 0.5181
Average 4.70 0.61 3.30 0.14 0.20 0.09 90.40 0.02 0.02 0.52
Stdev 0.91 0.05 0.05 0.04 0.01 0.00 0.92 0.00 0.00 0.01
Reference 4.25 0.69 3.34 0.26 0.22 0.09 90.50 0.02 0.02 0.55

August 25, 2015 22

Conclusion

• The new LIMESTONE application expands the capabilities pioneered by the

S1 TURBO LE unit and provides more sensitivity as well as flexibility

• Already we have fielded units for grade control in the field !

August 25, 2015 23

Availability

• Available on all LE units 730.0087 starting June 1st

• Price USD 1500.-

August 25, 2015 24

Suggested Bundling
Suggested Accessories
TDS!

• Make sure to ADD the TITAN

DETETCOR SHIELD to avoid
accidental puncture of the detector!

August 25, 2015 26

Consumables(buy locally or via Internet!)
FOIL

• www.chemplex.com

NO Waste
NO Static Cling
NO Contamination
NO Experience Necessary

3018 Prolene® 4.0 µ (0.16 mil); 3.0"; SpectroMembrane® $37.50

August 25, 2015 27

Sample cup (100 pieces)

430 Single 1.22" 0.88" 0.97" $50.00

(31.0mm (22.4mm (24.6mm
) ) )
Luggable Mill
57 kg to 90 kg
aterial soft, medium-hard
Size reduction principle impact, shearing
Material feed size* < 15 mm
Final fineness* < 80 µm
Speed at 50 Hz (60 Hz) 2,850 min-1 (3,420 min-1)
Rotor peripheral speed 20.4 m/s (24.5 m/s)
Types of rotors rotor beater
Material of grinding tools cast iron: grinding
chamber - stainless steel:
rotor / ring sieves /
retaining frame -
chromium plated:
retaining frame
Sieve sizes trapezoid holes 0.08 /
0.12 / 0.20 / 0.25 / 0.50 /
0.75 / 1.00 / 1.25 / 1.50 /
2.00 mm
round holes 3.00 / 4.00 /
10.00 mm
Collector capacity 5 l / optional: 30 l
Drive 1-phase motor / 3-phase
motor
Electrical supply data different voltages
Power connection 1-phase / 3-phase
Protection code IP 54
Power consumption 1.1 kW
W x H x D closed 560 x 1150 x 700 mm
(with base frame)
Net weight ~ 57 kg (with base frame)
August 25, 2015
Feed material soft, medium-hard
Material feed size* < 15 mm
Final fineness* < 50 µm
Speed at 50 Hz 8,100 min-1 (9,700 min-
1)
(60 Hz)
Rotor peripheral 58 m/s (69.5 m/s)
speed
Types of rotors rotor beater / standard /
distance
Material of stainless steel: grinding
grinding tools chamber / ring sieves /
retaining frame -
chromium plated:
retaining frame
Sieve sizes trapezoid holes 0.08 /
0.12 / 0.20 / 0.25 / 0.50 /
0.75 / 1.00 / 1.25 / 1.50 /
2.00 mm
round holes 3.00 / 4.00 /
10.00 mm
Collector capacity 5 l / optional: 30 l
Drive 3-phase motor
Electrical supply different voltages
data
Power connection 3-phase
Protection code IP 54
Power 2.2 kW
consumption
W x H x D closed 560 x 1200 x 890 mm
(with base frame)
Net weight ~ 95 kg
29
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