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Iron Ore Analysis

Using RIGAKU Correction Method


by RIGAKU XRF

Hisashi HOMMA
SBU-WDX
RIGAKU Corporation
1
Contents
1.   Fusion bead method for iron ore analysis using RIGAKU bead correction
・ Introduction of RIGAKU bead correction
・ Analysis of T.Fe2O3 using CRMs
・ Analysis using Vale calibration standards
・ Our proposal for Vale

2.   Pressed pellet method for iron ore analysis using the Compton
scattering ratio method with theoretical alpha
・ Introduction of the Compton scattering ratio method with theoretical alpha
・ Analysis of T.Fe2O3 using CRMs
・ Analysis using Vale calibration standards
・ Our proposal for Vale

Summary
2
1. Fusion bead method for iron ore
analysis using RIGAKU bead correction

3
Fusion bead method

Analytical Error Factors in Powder Samples

Powder Sample Heterogeneity Effect

Grain-size Effect Error


factors
Mineralogical Effect for bead

Fusion Bead Weighing Error

Loss on Ignition

Gain on Ignition

Evaporation of Flux

4
Fusion bead method

Error Factors in Fusion Method

Weighing Fusing Bead

Weighing error (1) GOI (3) Flux LOI (2)


(4)
O2 evaporation
CO2 H2O
Sample FeO
Fe2O3

Flux(Li2B4O7 etc)
Pt crucible

1000-1200 degC

The four error factors can be corrected.

5
Fusion bead method

Calibration Formula for Matrix Correction


Corrected for LOI/GOI, weighing error (Flux ratio) and flux
evaporation Only Rigaku software
can correct flux
Formula evaporation
Wi  (aIi 2  bIi  c)(1   αjWj  αLOIWLOI  αFRF  KF )
Correction term for flux ratio

aj : Theoretical alphas for correcting components


aF : Theoretical alphas for LOI(GOI)
aF : Theoretical alpha for flux ratio
RF : Flux ratio
KF : Constant (for flux ratio)

The term of aLOIWLOI can be eliminated by assigning LOI/GOI as balance.

RIGAKU bead correction is available in


Simultix10,11,12.14 and ZSX software
6
Fusion bead method

RIGAKU Bead Correction and Required


Information on the Sample Preparation
RIGAKU bead correction
LOI and flux ratio Flux evaporation
correction correction
Weighing error V V
Corrected error
GOI&LOI V V
factor
Flux evaporation - V
Flux ratio input at measurement F/S B/S-1
Required Sample weight (S) Required Required
information on Flux weight (F) Required -
sample
preparation Bead weight (B) - Required
on Calc. of Balance
Set “Ig” Set Flux
theoretical alpha component
Correction Use “calculated
Calibration Set “-1”
constant K value”

7
Fusion bead method

Improvement of Calibration Curve by


Bead Correction
page 1/2
Measurement
page 1/2
component : page
2010- 8-16 11:44
T.Fe 1/2 2O3 2010- 8-16 13:47

Empirical Calibration Empirical Calibration Empirical Calibration


Uncorrected Application Without corr Matrix correctionApplication Fe-ore_3rd_print
Flux evaporation +Application
600 600
Component
Element line
Fe2O3
Fe-KB1
only 600
Component
Element line
Matrix
Fe2O3
Fe-KB1
correction Comp
Eleme

X = AI 3+ BI 2 + CI + D X = AI 3 + BI 2 + CI + D X=A
Linear(straight) Linear(straight)
A= A=
B= B=
400 400 400

Intensity
Intensity

C= 2.21630e-001 C= 1.38143e-001
Intensity
D= -4.87844e-001 D= -5.74283e-001
Intensity(kcps)

Intensity(kcps)

Intensity(kcps)
Accuracy 2.11054e+000 Accuracy 2.32364e-001 Accur
Corr. factor 9.91576e-001 Corr. factor 9.99898e-001 Corr. f
Inter. std No Inter. std No Inter. s
Fixed point No Fixed point No Fixed
200 Weighting
200 Normal Weighting
200 Normal Weigh

Accuracy : Accuracy : Accuracy :


1.5mass%(T.Fe) 0.16mass%(T.Fe) 0.08mass%(T.Fe)
0 0 0
0 50 100 0 50 100 0 50 100

Std. Value (Fe2O3)


Std. value(mass%)
Std. Value (Fe2O3)
Std. value(mass%) Std. Value (Fe2O3)
Std. value(mass%)
No. Sample Intensity Std. value Calculated
No. Sample Deviation Apparent
Intensity Std. value No.Calculated
Sample Deviation Apparent
Intensity Std. value Calculate
1 JSS 804-1 431.46408 94.73 95.13745
1 JSS 804-1 0.40745 431.46408 94.73 194.69402
JSS 804-1 -0.03598 59.05185
431.46408 94.73 94.6638
2 JSS 805-1 439.81267 97.28 96.98775
2 JSS 805-1-0.29225 439.81267 97.28 297.20327
JSS 805-1 -0.07673 60.23023
439.81267 97.28 97.1503
3 JSS 814-1 423.42292 93.93 93.35529
3 JSS 814-1-0.57471 423.42292 93.93 393.80539
JSS 814-1 -0.12461 57.99553
423.42292 93.93 93.9615
4 JSS 820-2 390.22711 81.50 85.99811
JSS 820-2 4.49811
5 JSS 831-1 356.93926 81.54
4
78.62053
5 JSS 831-1-2.91947
390.22711
356.93926
81.50
81.54
481.96730
JSS 820-2 0.46730 53.02878
390.22711 8
81.50 81.5582
581.27356
JSS 831-1 -0.26644 48.89411
356.93926 81.54 81.4748
6 JSS 850-4 427.86248 93.89 94.33923
6 JSS 850-4 0.44923 427.86248 93.89 693.93297
JSS 850-4 0.04297 58.50511
427.86248 93.89 93.9214
Fusion bead method
Conditions for Experiments Using CRMs
Spectrometer
Rigaku sequential spectrometer ZSX PrimusII (WDXRF)
Data processing
Fusion bead correction and generation of
scattering ratio alphas

Measurement conditions
X-ray tube : End-window Rh target (4kW)
kV-mA : 50kV-50mA ZSX PrimusII
Calibration standards
Hematite ore, Magnetite ore, Limonite, Iron sand, Sinter, Pellet,
Pure iron oxide
29 certified reference materials of JSS, BAS, BCS, NBS, LKAB,
CSMI
Sample preparation (duplicated bead)
Sample / Flux(Li2B4O7) / Oxidizer(NaNO3) : 0.4g / 4.0g / 0.24g
Releasing agent : 50% LiI solution 50l
Fusion : RIGAKU HF fluxer at 1150 degC
9
Fusion bead method
Components and Concentration Range of
Samples Used (29CRMs)
Concentration Range Concentration Range
Component Component
(mass%) (mass%)
T.Fe2O3 35.3 – 101.6 V2O5 0.005 – 0.82
(T.Fe) (24.7 – 71.1) BaO – (0.16)
SiO2 0.47 – 20.0 Cr2O3 (0.003) – 0.041
CaO 0.01 – 22.0 Co2O3 – 0.005
MnO 0.02 – 1.31 NiO (0.003) – 0.057
Al2O3 0.27 – 7.24 CuO – 0.013
TiO2 0.02 – 7.77 ZnO (0.002) – 0.13
MgO 0.01 – 3.45 As2O3 0.001 – 0.044
P2O5 0.018 – 1.35 PbO (0.001) – (0.56)
SO3 0.005 – 2.1
Analyzed components cover the elements
K2O 0.002 – (0.72) described in JISM8205 and ISO9516-1
except for Sn. 10
Fusion bead method

Schematic Procedure of Fusion Bead Making


in RIGAKU Laboratory
3. Weighing
2. Drying Weigh 0.4g sample and 4.0g
Dry 2hours at 105degC flux and record their weight
of sample and exactly (catch weight)
675degC of Li2B4O7
1. Grinding
4. Addition of Additive
Add 0.24g oxidizer
Na2CO3 and 50ul
releasing agent LiI in
50% solution by
micropipette

6. Weighing
Record bead weight 5. Fusion
Fuse at 1150degC
exactly
Measurement using HF fluxer

11
Fusion bead method
page 1/2 2010- 8-16 09:38

T.Fe2O3 Calibration Curve of 29CRMs Using


Empirical Calibration
RIGAKU Bead Correction
600
Application Fe-ore_3rd_print

Component Fe2O3
Element line Fe-KB1

X = AI 3+ BI 2 + CI + D
Linear(straight)
A=
B=
400
C= 1.37747e-001
D= -3.29235e-001
Intensity(kcps)

Accuracy 1.11135e-001
Corr. factor 9.99977e-001 ZSX PrimusII
Inter. std No
Fixed point No
200 Weighting Normal

T.Fe Accuracy : 0.078(mass%)


Components for correction: Fe2O3, SiO2,
Al2O3, P2O5, MgO, SO3, CaO, K2O, MnO,
V2O5 , Cr2O3 , NiO , CuO , ZnO , BaO , Pb
0 O , As2O3 , Co2O3
0 50 100
Bead correction : Flux evaporation correction
Std. value(mass%)
Number of samples : 58(29x2)
Whether
No. the matrix correction requires
Sample Intensity traceStd. value Calculated Deviation Apparent

element component or not depends on the 94.73


1 JSS 804-1 431.46408 Sample
94.67629 preparation
-0.05371 : RIGAKU
59.13724 Lab
2 JSS 805-1 439.81267 97.28 97.16654 -0.11346 60.32405
standard set. This CRM set requires at least Equipment : ZSX
3 JSS 814-1 423.42292 93.93 93.94589 0.01589 PrimusII
57.98625 12
V2O5 4and JSS
BaO in
820-2
the matrix correction
390.22711 81.50 81.52483 0.02483 53.40716
Fusion bead method

Evaluation of T. Fe2O3 Calibration Curve


Using RIGAKU Bead Correction

unit : mass%
Certified XRF value
CRM Error
value (T.Fe) (T.Fe)
IPT-123 Bead1 65.10 65.001 -0.099
Bead2 ↑ 65.040 -0.060
IPT-146 Bead1 65.51 65.542 0.032
Bead2 ↑ 65.560 0.050

13
Fusion bead method
Conditions for Experiment Using Vale
Samples
Spectrometer
Rigaku multi-channel simultaneous spectrometer Simultix14 (WDXRF)
Data processing
Fusion bead correction and generation of
scattering ratio alphas

Measurement conditions
X-ray tube : End-window Rh target (4kW)
kV-mA : 50kV-50mA Simultix14

Calibration standards
Vale calibration standard
14(7x2) samples
Sample preparation (duplicated bead)
Sample / Flux(Li2B4O7) / Oxidizer(NaNO3) : 0.4g / 4.0g / 0.24g
Releasing agent : 50% LiI solution 50l
Fusion : RIGAKU HF fluxer at 1150 degC
14
Fusion bead method
T.Fe2O3 Calibration Curve Using Vale
Calibration Standards : Simultix14

Simultix14

T.Fe Accuracy : 0.053(mass%)


Components for correction : Fe2O3,
Vale standard set does SiO2, Al2O3, P2O5, MgO, SO3, CaO,
K2O, MnO
not required additional
trace component in the Bead correction : LOI and flux ratio
correction
matrix correction
Number of samples : 14(7x2)
Sample preparation : RIGAKU Lab
Equipment : Simultix 14 15
Fusion bead method
Calibration Curves Using Vale Calibration
Standards : Simultix14
SiO2 CaO MnO Al2O3 TiO2
Intensity

Accuracy Accuracy Accuracy Accuracy Accuracy


= 0.044 = 0.018 = 0.007 = 0.028 = 0.004
0 4 8 12 0 2 4 0 1 2 0 1 2 3 0 1 2
Std.Val.(mass%) Std.Val.(mass%) Std.Val.(mass%) Std.Val.(mass%) Std.Val.(mass%)

MgO P2O5 SO3 K2O


Intensity

Accuracy Accuracy Accuracy Accuracy


= 0.014 = 0.001 = 0.002 = 0.002
0 1 2 0.0 0.1 0.2 0.3 0.0 0.008 0.016 0 0.1 0.2
Std.Val.(mass%) Std.Val.(mass%) Std.Val.(mass%) Std.Val.(mass%) 16
Fusion bead method
Compiled Results Using RIGAKU Bead
Correction
Number
Calibration Standard T.Fe range Bead
Accuracy of Equipment
Set (mass%) correction
samples
Flux
CRMs 0.078 24.7 - 71.1 58 PrimusII evaporation
correction
Flux
Steel company 0.064 56.4 – 67.9 38 PrimusII evaporation
correction
LOI and
Vale 0.053 50.4 – 68.3 14 Simultix14 flux ratio
correction

Sample preparation for all standard set were performed at Rigaku laboratory.
Calibration standard set of steel company includes the Australian iron ores
(Marra Mamba or Brockman and CID)
17
Fusion bead method
Schematic Procedure of RIGAKU’s Approach
for Fusion Bead Method in Vale
3. Weighing Save time
2. Drying Only record sample
Dry 2hours at 105degC and flux weight exactly
of sample and (catch weight)
500degC of flux
1. Grinding without LiI 4. Addition of Additive
Add releasing agent
in solution by
micropipette

e.g. 50ul of
LiI in 50%
sol.
6. Measurement using LOI
and flux ratio correction
Reduce
Set fused bead 5. Fusion interference
and register flux of residual
ratio and then iodine and
“Start” save cost

18
2. Pressed pellet method for iron ore
analysis using the Compton scattering
ratio with theoretical alpha

19
Pressed pellet method

Compton Scattering Ratio Correction Method


Scattering Line Internal Standard Correction

Equation
Wi = A Ii/IRh-K Compton+B
Rh-K Compton line
Assumption
IRh-K Compton  1/Rh-K Compton
Rh-K Compton  i
: Mass absorption coefficient
Problem
Applicable only when all heavy
elements including analyte are
trace amount. That is, above
assumptions are not always
true.

20
Pressed pellet method
Mass Absorption Coefficients for Coexisting
Elements Normalized at Rh-K Compton
Relationship of absorption coefficients is proportional ?

Analyzing line :Fe-K

(analyzing line)
coefficient m to Rh-K Compton

60 O Al
Ratio of mass absorption

Cu absorption edge
Zn absorption edge
O
50 Al Si
Pb absorption edge

Si

Fe-K
Rh-K Compton

40
Ca Ca
30

20 Fe-K
(analyzing
10 Pb line)
Fe Zn
Cu
0
0.05 0.1 0.15 0.2 0.25 0.18 0.2
Wavelength (nm) Wavelength (nm)
Rh-K Compton  i We need additional correction!
21
Pressed pellet method

Compton Scattering Ratio Correction with


Theoretical Alphas
Calibration equation
Wi  ( A I 2R  B I R  C)  (1    j W j)
Ii
IR 
ICompton
This method corrects for the errors of Compton
ratio method by adding matrix correction term.
Alphas are generated by using FP method calculating
theoretical intensities of Compton x-ray scattering and
fluorescent x-ray lines.
This FP function is available in Only Rigaku
Simultix 14 and ZSX software software has this
FP function 22
Pressed pellet method

Calibration Curve of T.Fe


page 1/2 page 1/2 2010- 6-15 18:55 2010- 6-15 16:31
Compton ratio with
page 1/2

Without
Empirical Calibration Correction EmpiricalCompton
Calibration ratio only Empirical Calibration

30
Application
theoretical alphas
30.0
CRM-EMP_prn1 Application CRM-EMP_prn1 Application

Component Fe 30.0
Component
30 Fe C

Intensity ratio (IFe/ICompton)


Intensity ratio (IFe/ICompton)
Element line Fe-KA Element line Fe-KA E

60
600
X = AI 3+ BI 2 + CI + D X = AI 3+ BI 2 + CI + D X
Fe Intensity (a.u.)

Quadratic(curved) Quadratic(curved)
A= A=
B= -9.81336e-005 B= -3.27393e-002
20
20.0
C= 1.80256e-001 20
20.0
C= 2.86926e+000
D= -3.99940e+000 D= 1.76733e+001
Intensity(kcps)

40
400
Int. ratio

Accuracy 1.00216e+000

Int. ratio
Accuracy 2.21132e+000 A
Corr. factor 9.66789e-001 Corr. factor 9.93269e-001 C
Inter. std No Inter. std Rh-KAC In
Fixed point No Fixed point No Fi
10.0
Weighting 10 Normal Weighting
10.0
10 Normal W
20
200

Accuracy = Accuracy = Accuracy =


2.2mass% 1.0mass% 0.14mass%
0020.0 40.0 60.0 80.0
0
0.0
20.0 40.0 60.0 80.0 0
0.0
20.0 40.0 60.0 80.0
20 40 60 80 20 40 60 80 20 40 60 80
T.Fe conc. (mass%)
Std. value(mass%) Std. value(mass%) Std. value(mass%)

No. SampleT.Fe conc. (mass%)


Intensity Std. value No. Sample Deviation
Calculated
T.Fe conc. (mass%) Int. ratio
Apparent Std. value CalculatedSample Deviation
No. Apparent
Int. ratio Std. value Calc
1 JSS 804-1 556.38760 66.26 1 JSS 804-1 -0.34637
65.91363 23.01014 66.26 66.36105
1 JSS 804-1 0.10105 23.01014 66.26 66.
2 JSS 805-1 565.47146 68.04 2 JSS 805-1 -1.48901
66.55099 24.13532 68.04 2 JSS 805-1-0.18725
67.85275 24.13532 68.04 67.
3 JSS 814-1 537.48925 65.70 3 JSS 814-1 -1.16424
64.53576 22.34365 65.70 3 JSS 814-1-0.26165
65.43835 22.34365 65.70 65.
4 JSS 820-2 526.42765 57.00 4 JSS 820-2 6.69674
63.69674 18.41738 57.00 4 JSS 820-2 2.41242
59.41242 18.41738 57.00 56.
5 JSS 831-1 430.94680 57.03 5 JSS 831-1 -1.57373
55.45627 16.51450 57.03 5 JSS 831-1-0.90122
56.12878 16.51450 57.03 57.
6 JSS 850-4 548.08700 65.67 6 JSS 850-4 -0.35293
65.31707 22.60310 65.67 6 JSS 850-4 0.13100
65.80100 22.60310 23 65.67 65.
7 JSS 852-2 546.16535 66.83 7 JSS 852-2 -1.65296
65.17704 23.01046 66.83 7 JSS 852-2-0.46852
66.36148 23.01046 66.83 66.
8 BAS 676-1 291.67065 39.76 8 BAS 676-1 0.46746
40.22746 8.62906 39.76 8 BAS 676-10.23456
39.99456 8.62906 39.76 39.
Pressed pellet method
Comparison of Theoretical Alphas with and
without Compton Ratio
Theoretical alpha for Fe-K
Component
w/o Compton ratio with Compton ratio
MgO 0.0158 0.0018
Al2O3 0.0180 0.0019
SiO2 0.0220 0.0026
P 0.0568 0.0064
S 0.0700 0.0081
K2O 0.0956 0.0107
CaO 0.0967 0.0110
Ba 0.271 0.0266
TiO2 0.0955 0.0104
V 0.1770 0.0193
MnO 0.0350 -0.0034
Fe 0.0537 -
The coefficients with Compton ratio are smaller by one order of
magnitude. Although matrix effect still can not be ignored, it can reduce
influences from analytical error of coexisting elements
21/04/13 24
Pressed pellet method

Conditions for Experiments Using CRMs


Spectrometer
Rigaku sequential spectrometer ZSX PrimusII (WDXRF)
Data processing
Fusion bead correction and generation of
scattering ratio alphas
Measurement conditions
X-ray tube : End-window Rh target (4kW)
kV-mA : 50kV-50mA ZSX PrimusII

Calibration standards
Hematite ore, Magnetite ore, Limonite, Iron sand, Sinter and Pellet
26 certified reference materials of JSS, BAS, BCS, NBS, LKAB,
CSMI
Sample preparation
Grinding : Vibrating mill using WC container (10min., No binder)
Pelletizing : 250kN with aluminum ring (32mm dia.)
25
Pressed pellet method
Components and Concentration Range of
Samples Used (26CRMs)
Concentration Range
Component
(mass%)
Fe (total) 36.0 - 71.1
SiO2 0.47 - 16.5
CaO 0.01 - 19.6
MnO 0.02 - 1.07
Al2O3 0.27 - 6.81
TiO2 0.02 - 7.77
MgO 0.01 - 3.45
P 0.008 - 0.59
S 0.002 - 0.85
K2O 0.003 - 0.52
V 0.003 - 0.46
Ba - (0.14) 26
Pressed pellet method

Schematic Procedure of Pressed Pellet


Making in RIGAKU Laboratory
2. Drying
Dry 2hours at
105degC
1. Grinding
Grind about 10g sample 3. Press
with WC container Press with aluminum
ring at 250kN

Measurement

27
Pressed pellet method

page 1/2
T.Fe Calibration Curve Using 26CRMs 2010- 8-11 19:03

Applied Rigaku’s Compton scattering ratio correction with


Empirical Calibration
theoretical alpha
Application method
CRM-EMP_prn1
30.0 Component Fe
Element line Fe-KA

X = AI 3+ BI 2 + CI + D
Cubic(curved)
A= 9.90250e-004
B= -6.85117e-002
20.0
C= 3.68961e+000
D= 4.73864e+000
Int. ratio

Accuracy 1.41067e-001
Corr. factor 9.99873e-001
Inter. std Rh-KAC ZSX PrimusII
Fixed point No
10.0 Weighting Normal

T.Fe Accuracy : 0.14(mass%)


Theor.alphas : calcurated by ZSX software
with FP function
0.0 Components for correction.: SiO2, Al2O3, P,
0.0 20.0 40.0 60.0 80.0
MgO, S, CaO, K2O, MnO, TiO2, V, Ba
Std. value(mass%) Sample preparation : RIGAKU Lab
No. Sample Int. ratio Std. value Calculated Deviation Apparent
1 JSS 804-1 23.01014 66.26
Equipment
66.28235
:
0.02235
ZSX Primus II
65.40460
28
2 JSS 805-1 24.13532 68.04 68.01247 -0.02753 67.82898
Pressed pellet method
Conditions for Experiments Using Vale
Samples
Spectrometer
Rigaku multi-channel simultaneous spectrometer Simultix14 (WDXRF)
Data processing
Fusion bead correction and generation of
scattering ratio alphas
Measurement conditions
X-ray tube : End-window Rh target (4kW) Simultix14
kV-mA : 50kV-50mA
Calibration standards
Vale calibration standard
7 samples
Sample preparation
Grinding : Vibrating mill using WC container (10min., No binder)
Pelletizing : 250kN with aluminum ring (32mm dia.)
29
Pressed pellet method
T.Fe Calibration Curve Using Vale
Calibration Standards : Simultix14

Simultix14

T.Fe Accuracy : 0.063(mass%)


Theor.alphas : calcurated by Simultix14
software with FP function
Components for correction.: SiO2, Al2O3,
P, MgO, S, CaO, K2O, Mn, TiO2
Sample preparation : RIGAKU Lab
Equipment : Simultix14

30
Pressed pellet method
Calibration Curves Using Vale Calibration
Standards : Simultix14
SiO2 CaO Mn Al2O3 TiO2
Intensity

Accuracy Accuracy Accuracy Accuracy Accuracy


= 0.18 = 0.018 = 0.007 = 0.049 = 0.005
0 4 8 12 0 2 4 0 1 2 0 1 2 3 0 1 2
Std.Val.(mass%) Std.Val.(mass%) Std.Val.(mass%) Std.Val.(mass%) Std.Val.(mass%)

MgO P S K2O
Intensity

Accuracy Accuracy Accuracy Accuracy


= 0.032 = 0.002 = 0.001 = 0.002
0 1 2 0.0 0.1 0.2 0.3 0.0 0.003 0.006 0 0.1 0.2
Std.Val.(mass%) Std.Val.(mass%) Std.Val.(mass%) Std.Val.(mass%) 31
Pressed pellet method

Compiled Results Using the Compton


Scattering Ratio with Theoretical Alpha
Correction

Calibration Standard T.Fe range Number of


Accuracy Equipment
Set (mass%) samples
CRMs 0.14 36.0 – 71.1 26 PrimusII
Steel company 0.12 56.4 – 67.9 19 PrimusII
Vale 0.063 50.4 – 68.3 7 Simultix14
CRMs2 0.093 39.8 – 69.8 6 Simultix14

Sample preparation for all sample set were performed at RIGAKU laboratory.

CRMs2 is subset of CRMs but both are discrete set.


32
Pressed pellet method
Binder Test on Sample Preparation of
Pressed Pellet Method
Std. dev. of intensities of both
Accuracy of sides of pelletsB ( kcps )
Standard Number of
Binder T.Fe calib.
samples samples
curve Rh-K-C Fe-K

ValeA 3 Ceridust 0.101 0.0222 7.03


Vale 7 Ceridust 0.139 0.0149 3.02
Vale 7 None 0.063 - -
CRMs 6 Ceridust 0.197 0.0078 1.75
CRMs 6 S-blend 0.172 0.0213 2.98
CRMs 6 Boric Acid 0.193 0.0096 0.60
CRMs 6 None 0.093 0.0049 0.37
Binder : Sample is 1 : 9. Pressed with Aluminum ring at 250kN.
All of sample except ValeA were prepared in Rigaku laboratory.
B   1/ d2  R
:
Pressed pellet method
Schematic Procedure of RIGAKU’s Approach
for Pressed Pellet Method in Vale
Save time
and cost
2. Drying
p
Dry 2hours at Ski
105degreeC
1. Grinding
Grind to fine 4. Press
grained particle Press with sample cup

5. Measurement
Set pressed 5’. Measurement by
pellet and other equipment
then “Start” Cover pellet by polymer
thin film, then measure

34
Summary of RIGAKU Correction Method and
ZSX & Simultix Software

Fusion bead Pressed pellet


Bead correction (with
Compton scattering ratio
flux evaporation
with theoretical alpha
correction)
Simultix10, Unable to generate
V
Applicable 11,12 scattering ratio alphas
equipment Simultix14 V V
ZSX series V V
Remarks Rigaku Only Rigaku Only

All advanced correction methods of both fusion bead


and pressed pellet for iron ores can be applied in only
RIGAKU XRF.
35
Obrigado por sua atenção !
Thank you for your attention !

36

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