FUSIONS HOW TO IMPROVE THROUGHPUT AND

CONCENTRATION RANGE OF ANALYSIS BY ELIMINATING

THE LOSS ON IGNITION PROCESS STEP, USING DIFFERENT
DILUTION RATIOS AND MAINTAINING ACCURACY AND
PRECISION OF RESULTS

Laura Oelofse (Rigaku Americas) and Yoshijuro Yamada (Rigaku

Corporation )

Abstract
The use of fusions for XRF in industrial process monitoring is common
practice and there are several time consuming steps to complete in
order to render a sample fusion ready.
This paper details a method that would eliminate the need to carry out
the Loss on Ignition, Gain on Ignition step thus eliminating 2 hrs from
the preparation time and it also details the ability to use different
dilution ratios of sample and flux for materials on the same calibration
curve in order to increase the scope of materials that can be included in
a universal calibration curve using both naturally sourced certified
reference materials and synthetic pure chemicals as calibration
standards

Analysis Schemes in Various

Industry Sectors
Composition
varies in
narrow range

Widely
varying
composition

Incoming Raw
Materials

Product

XRFs Role in High Throughput

Solutions
Results

Analysis

Sample
Introduction

Sample
Preparation

Sample
Loading

Fusions Flux + Sample

All compounds changed to oxide form

Eliminate Particle Size Effect
Eliminate Mineralogical Effect

Some Typical Fused Glass Beads

Why Preparation of Fused Glass Beads

Particle size and mineralogical effects are removed or diminished

by fusion of the sample with a suitable flux to form a glass bead.
Synthetic calibration standards can be made by mixing pure oxides
at concentration levels to suit the analytical range.
Depending on sample type, fusion can even be quicker than
pressed powder procedure.
Generally accuracies and reproducibility are superior with fusion
procedure.
Only drawback is possible dilution of trace elements and therefore
inferior LLD. Low dilution fusions are possible.

Preparation of
Fused Glass Beads
Melting method
Heat for
Melting

Weigh out
and mix
Flux + Specimen

Cast & Cool

1000 -1100 C

To standard holder
Glass disk
specimen

Platinum crucible

Remove bubbles
9499D00500

3 - 7 mins

8 - 15 mins
5 mins
8

Preparation of Fused Glass Beads

Preparation of powder as fused glass bead involves weighing out

sample and flux, placing in Gold/Platinum crucible, heating to 1000
1200 degrees and casting as a flat glass bead by pouring melt
into a heated Gold/Platinum mould and cooling under controlled
conditions.
Newer alternative is moldable where melt remains in crucible and
bead is formed in situ.
DEPENDING ON NATURE OF SAMPLE LOSS ON IGNITION
MAY BE NECESSARY. ( CEMENTS, LIMESTONE, DOLEMITE)

In reality there are three types of samples

Type 1 Sample is stable, no loss or gain during fusion process
Sample

Flux
F

Type 2 : Sample loses CO2 or Intrinsic Waters during fusion, known as Loss on Ignition
LOI

Sample

Flux
F

Type 3: Sample loses CO2 or Intrinsic Waters during fusion, known as LOI and changes oxidation state and
pick up oxygen, gaining on ignition, known as GOI
LOI

Sample
S

Flux
Replaced with flux
B

GOI

Analytical Error Factors in Fusion Method

The errors can be removed by Rigaku Bead Correction method
Powder Sample

Heterogeneity Effect
Grain-size Effect
Mineralogical Effect

Fusion Bead

Weighing Error
Loss on Ignition

Gain on Ignition
Evaporation of Flux

Error factors
for Bead

Error Factors in Fusion Method

Fusing

Weighing

Weighing error(1)

GOI (3)
O2

Sample

FeO

Flux(Li2B4O7 etc)

Bead

(4)
Flux
LOI
evaporation

(2)

CO2 H O
2

Fe2O3

Pt crucible

1000-1200 C

The four error factors can be corrected.

Strategy for the Corrections of LOI, GOI and Dilution Ratio

Model 1 : Use of Ratio of flux to sample weight ( F/S)
LOI

Sample

Flux
F

Definition of LOI
: Imaginary component with no x-ray absorption
Correction LOI(GOI) : Concentration is manually input or calculated as balance
Dilution ratio : Corrected by manual input of F/S

Model 2 : Use of Ratio of bead to sample weight( B/S)

LOI

Sample
S

Flux
Replaced with flux
B

Definition of LOI
: Imaginary component of flux
Correction : LOI(GOI) : Concentration is manually input or calculated as balance
Dilution ratio : Corrected by manual input of B/S
(Note) Flux evaporation can be corrected

Analysis in Fused Beads

Use of fusion bead correction
Software generates theoretical alphas for LOI/GOI and dilution ratio
Calibration equation

Wi (aI 2 bI C)(1 K jWj LOIWLOI FRF)

The alphas correct for

LOI/GOI
Dilution ratio
and Flux evaporation during fusing
The alphas are generated by using a fundamental parameter software and it
generates variety of models.

Dilution ratio models : Flux weight to sample

weight(F/S) or bead weight to sample weight(B/S)
LOI/GOI : Loss eliminated or manual input

Rigaku Fusion Bead Correction Software

Allows for varying flux : sample ratios and the use of

catch weights
Allows calculation of the Loss on Ignition /Gain on
Ignition and flux loss component by balance or ratio input

BCS376

LOI 0

LOI 10

SiO2

67.1

67.42

60.68

TiO2

0.02

0.02

0.02

Al2O3

17.7

17.79

16.01

Fe2O3

0.10

0.10

0.09

CaO

0.54

0.54

0.49

MgO

0.03

0.03

0.03

Na2O

2.83

2.84

2.56

K2O

11.2

11.25

10.13

LOI

0.35

0.00

10.00

Total

99.87

99.99

100.01

Sample (g)

0.3000

0.2700

Li2B4O7 ( g)

3.0000

3.0000

60

50

40

LOI XRF

Oxides

30
LOI CHEM
Liner (LOI CHEM)

20

10

0
0

20
LOI CHEM

-10

40

60

Fusion Bead Correction for LOI in Various Kinds of Materials

BCS393
(Limestone)

Chem.
XRF
Diff.
NBS69b
Chem
(Bauxite)
XRF
Diff.
NBS697
Chem
(Bauxite)
XRF
Diff.
NBS97a
Chem
(Clay)
XRF
Diff.
JDo 1
Chem
(Dolomite)
XRF
Diff.
BCS375
Chem
(Feldspar)
XRF
Diff.
R801
Chem
(Pyrophyllite) XRF
Diff.
BCS314
Chem
(Silica brick) XRF
Diff.

SiO2 TiO2 Al2O3 Fe2O3 MnO MgO

0.70 0.01
0.12
0.05 0.01
0.15
0.77 0.02
0.16
0.03 0.00
0.13
-0.07 0.01
0.04 -0.02 -0.01 -0.02
13.57 1.92 49.29
7.21 0.11
0.09
13.68 1.92 49.28
7.25 0.11
0.14
0.11 0.00
-0.01
0.04 0.00
0.05
6.84 2.53 45.99 20.09 0.41
0.18
6.88 2.51 45.98 20.15 0.42
0.25
0.04 -0.02
-0.01
0.06 0.01
0.07
44.00 1.91 39.06
0.45 0.00
0.15
43.89 1.93 38.72
0.45 0.00
0.09
-0.11 0.02
-0.34
0.00 0.00 -0.06
0.21 0.00
0.01
0.02 0.01 18.58
0.28 0.01
0.06
0.01 0.00 18.87
0.07 0.01
0.05 -0.01 -0.01
0.29
67.15 0.38 19.82
0.12 0.00
0.05
67.80 0.38 20.05
0.10 0.00
0.07
0.65 0.00
0.23
0.02 0.00
0.02
78.64 0.10 16.76
0.17 0.00
0.04
78.62 0.10 16.71
0.17 0.00
0.08
-0.02 0.00
-0.05
0.00 0.00
0.04
96.40 0.19
0.77
0.53 0.01
1.81
96.47 0.20
0.79
0.49 0.00
1.86
0.07 0.01
0.02 -0.04 -0.01
0.05

CaO Na2O
55.46 0.03
55.78 0.00
0.32 -0.03
0.13 0.03
0.17 0.00
0.04 -0.03
0.71 0.04
0.78 0.00
0.07 -0.04
0.11 0.04
0.13 0.01
0.02 -0.03
33.94 0.01
33.95 0.00
0.01 -0.01
0.89 10.41
0.87 9.95
-0.02 -0.46
0.04 0.22
0.08 0.16
0.04 -0.06
1.81 0.05
1.86 0.01
0.05 -0.04

K2O
0.02
0.01
-0.01
0.07
0.07
0.00
0.06
0.06
0.00
0.50
0.58
0.08
0.00
0.00
0.00
0.79
0.74
-0.05
0.18
0.19
0.01
0.09
0.08
-0.01

P2O5
0.01
0.00
-0.01
0.12
0.11
-0.01
0.97
0.97
0.00
0.36
0.37
0.01
0.04
0.03
-0.01
0.00
0.01
0.01
0.00
0.02
0.02
0.00
0.01
0.01

LOI
43.44
43.10
-0.34
27.46
26.99
-0.47
22.18
22.00
-0.18
13.42
13.83
0.41
47.18
46.79
-0.39
0.39
0.03
-0.36
3.86
3.88
0.02
0.10
0.01
-0.09

Results are obtained by using theoretical alphas and LOIs are

obtained as balance. The accuracy of the calculated LOI across the
range of 0 % - 50% is 0.5%

Quantification and
Correction of Gain
on Ignition
Synthetic mixtures of SiO2 and
FeO were blended to yield
30%, 50% and 70% FeO
During fusion the FeO is
oxidized to Fe2O3 and there is
a weight gain of
(Fe2O3 2FeO)/ 2FeO
The mass absorption
coefficient of GOI is set to zero
and the value is considered as
a negative LOI in the FP
calculation.
The WFe2O3 = WFeO + W GOI

SiO2

FeO

calc.
Recalc.
FP value

70.00

30.00

calc.
Recalc.
FP value

50.00

calc.
Recalc.
FP value

30.00

Fe2O3

32.27
32.48
50.00
52.64
52.84
70.00
72.17
72.15

Determination of GOI from Standard Iron Ore

Fe2O3

Diff

Chem

XRF

JSS 803-2

89.57

89.71

0.14

JSS830-3

84.18

84.16

-0.02

Euro 680-1

86.33

86.31

-0.02

ASCRM 004

89.43

89.51

0.08

Method applied to iron ore with high Fe content and

shown to be suitable

Dilution Ratio Correction

STD
S:F 1:5
JB-2

UNK
S:F 1:10
JG-1

Lit.

FP

Lit.

SiO2

52.83

73.06

72.75

TiO2

1.18

0.28

0.26

Al2O3

14.57

14.02

14.29

Fe2O3

14.24

2.13

2.21

MnO

0.20

0.06

0.06

MgO

4.63

0.71

0.75

CaO

9.82

2.18

2.19

Na2O

2.02

3.38

3.41

K2O

0.43

4.10

3.97

P2O5

0.10

0.09

0.10

Application of LOI, GOI and dilution ratio correction to

Empirical Calibration Methods
Matrix correction coefficients were theoretically calculated for LOI,
GOI and dilution ratio correction components
The matrix correction expression including the dilution ratio
correction is shown on the next slide
Using the Theoretical Alpha Correction model where the base
component is considered to be the LOI/GOI/D.C then these are
eliminated in the De Jongh calculation and are calculated as a
balance component.
The accuracy for Fe2O3 in a regression of geological standards for
an uncorrected calibration was 0.161%, for a calibration with
conventional matrix corrections 0.066% and for theoretical matrix
correction coefficients with LOI and GOI correction an improved
accuracy of 0.056%

Rigaku Theoretical Alphas for Fusion Bead

Correction equation of T.Fe
Wi = (aiIi2+biIi +c)*(1+SajWj + aFRF - KF)
Factor Coefficient
K
0.910900
a(T.Fe) 0.002392
a( SiO2) 0.001413
a(Mn)
0.002923
a(CaO) 0.006793
a(MgO) 0.000967
a(Al2O3) 0.001128
a(TiO2) 0.006700
a(P)
0.003929
a(S)
0.004874
a(K)
0.008125
a(FLUX) 0.089130

1. The correction coefficients a j for inter-elements and flux

are calculated theoretically by Rigaku/FP software. These
alphas depend on the optics of spectrometer.
2. K corresponds to the standard dilution ratio.
3. When the actual dilution ratio RF ( Bead weight/ sample
weight ) is input for the each sample manually, all error
factors are automatically corrected. ( LOI, GOI and Dilution
Correction)
4. Calibration constants (a,b,c) are calculated using the nonlinear regression equation , after standard samples are
measured.

Dilution Ratio Correction

Calibration equation with dilution ratio correction

Wi b I i c 1 a j Wj a F R F K F
j L

K F aFR F
General calibration equation

Wi b I i c 1 a j Wj a F R F

R F R F R F
aFRF + KF is the correction term for
the difference between the actual and
standard dilution ratio.

RF : Difference between the actual

and standard ratio
RF

: Actual dilution ratio

Matrix Correction Model

Correction model
Lachance-Traill

Uncorrected
component
Analyte

Notes
Correction by all the components except the
analyte.
The calibration curve is linear.

de Jongh

Base component

Correction by all the elements except the base

component.
The calibration curve is linear.

JIS

Base component
and analyte

Correction by all the elements except the base

component and the analyte.
The calibration curve is linear or quadratic.

When a significant amount of LOI (GOI) is contained, it is advisable to use de Jongh or JIS
model.

SiO2 Calibration Curve

Analysis sample: rock fusion disk (dilution ratio 5:1)
de Jongh model

X-ray intensity (a. u.)

X-ray intensity (a. u.)

JIS model

Accuracy: 0.18
mass%
Standard value (mass%)

Accuracy: 0.17
mass%
Standard value (mass%)

considering self-absorption
by the analyte

CaO Calibration Curve

Analysis sample: rock fusion disk (dilution ratio 5:1)
de Jongh model

X-ray intensity (a. u.)

X-ray intensity (a. u.)

JIS model

Accuracy: 0.17 mass%

Standard value (mass%)

Accuracy: 0.14 mass%

Standard value (mass%)

considering self-absorption
by the analyte

Comparison of Matrix
Correction Coefficients
between Several Materials by
the Fusion Method
Analysis of Refractories

Calibration Range of the Major Components and

Dilution Ratio for Each Material
Material

Major component (mass%)

SiO2

Al2O3

Fe2O3

MgO

649

Silica

8497

10

10

44

4794

10
8199

Chrome-magnesia

27

Zircon-zirconia

45

Alumina-zirconia-silica

42

Alumina-magnesia
The whole range

(Flux/Sample)

3786

Magnesia

ZrO2

Clay
High alumina

Cr2O3

Dilution ratio

10
253

1082
1093

97

1052

94

22.16
4892

10

1248

10

379
27

99

Wide calibration range

Different dilution ratio

10

10
53

92

1022.16

Flux: Li2B4O7
LiNO3 was used just
for Chrome-magnesia.

Comparison of Matrix Correction

Coefficients for Each Material (1)
Clay

Alumina-Zircon-Silica

SiO2

Analyte
Correcting comp.
Al2O3
Fe2O3
TiO2
MnO
CaO
MgO
Na2O
K2O
P2O5
Cr2O3
ZrO2

High alumina

1.38E-03
1.02E-03
2.44E-04
8.65E-04
6.91E-05
1.33E-03
1.04E-03
-5.41E-05
-1.88E-05
6.06E-04
8.76E-04

Si-Ka
1.38E-03
1.01E-03
2.41E-04
8.62E-04
6.60E-05
1.33E-03
1.04E-03
-5.75E-05

1.37E-03
1.02E-03
2.43E-04

6.81E-05
1.33E-03
1.04E-03
-5.49E-05
6.07E-04
8.68E-04

Correction model: Lachance-Traill

Correction coefficients are almost identical for each
material.

SiO2 Calibration Curve

Magnified
Magnesi
a
X-ray intensity (a. u.)

X-ray intensity (a. u.)

Accuracy:
0.25 mass%
Silica
Clay
AZS

AZS

10 : 1
22.16 : 1

Chrome-magnesia

(Chrome-magnesia)

Standard value (mass%)

Standard value (mass%)

AZS: Alumina-zirconia-silica

Comparison of Matrix Correction

Coefficients for Each Material (2)
Clay

Alumina-Zircon-Silica

Fe2O3

Analyte
Correcting comp.
SiO2
Al2O3
TiO2
MnO
CaO
MgO
Na2O
K2O
P2O5
Cr2O3
ZrO2

High alumina

-1.88E-03
-2.19E-03
3.93E-03
-1.94E-04
4.03E-03
-2.37E-03
-2.62E-03
3.94E-03
-1.65E-03
7.27E-03
1.09E-03

Fe-Ka
-1.87E-03
-2.18E-03
3.95E-03
-1.93E-04
4.04E-03
-2.36E-03
-2.61E-03
3.96E-03

-2.06E-03
-2.37E-03
3.64E-03

3.72E-03
-2.54E-03
-2.79E-03
3.64E-03
6.91E-03
1.30E-03

Correction model: Lachance-Traill

Correction coefficients are almost identical for each
material.

Fe2O3 Calibration Curve

Magnified

Chrome-magnesia

Accuracy:
0.029
mass%
10 : 1

X-ray intensity (a. u.)

X-ray intensity (a. u.)

Magnesi
a

Chrome-magnesia

22.16 : 1

Zircon-zirconia

(Chrome-magnesia)

Standard value (mass%)

Standard value (mass%)

AZS: Alumina-zirconia-silica

Dilution Ratio Correction

+ Matrix Correction
Rock sample
Analyte

GSJ:

dilution ratio 10:1 and 5:1

: SiO2

Analysis sample
CCRMP: SY-2, SY-3
JA1, JA2, JA3, JB2, JB3, JG1a, JG2, JG3, JGb1, JR1, JR2, JLs1, JCp1

Dilution Ratio Correction

Rock sample
Analyte

dilution ratio 10:1 and 5:1

: SiO2

No correction
X-ray intensity (a. u.)

X-ray intensity (a. u.)

Accuracy: 11 mass%

5:1
10:1
Standard value (mass%)

Dilution ratio
correction
Accuracy: 3.6
mass%

5:1
10:1
Standard value (mass%)

The dilution ratio correction improves

the accuracy; however, the fitting is
still not excellent due to matrix effect.

Dilution Ratio Correction

+ Matrix Correction
Dilution ratio
correction
Accuracy: 3.6
mass%

5:1
10:1
Standard value (mass%)

dilution ratio 10:1 and 5:1

: SiO2

X-ray intensity (a. u.)

X-ray intensity (a. u.)

Rock sample
Analyte

Dilution ratio
cor.
+ Matrix cor.
Accuracy:
0.33 mass%

5:1
10:1
Standard value (mass%)

The combination of the dilution

ratio and matrix corrections enables
an excellent fitting.

LOI Correction (1)

Test sample: rock sample with 50 mass% LOI

(the bead was made with the dilution ratio

10:1, and then treated as the dilution ratio 5:1,
which results in the sample with 50 mass%
LOI.)
Analyte: SiO2

LOI Correction and

Matrix Correction Coefficients
Correction model: de Jongh
Element line: Si-Ka
Without LOI cor.

With LOI cor.

Base component

SiO2

LOI

Na2O
MgO
Al2O3
SiO2
P2O5
K2O
CaO
TiO2
MnO
Fe2O3

-4.79E-04
-6.32E-05

5.15E-03
5.81E-03
5.91E-03
2.78E-03
2.74E-03
2.67E-03
2.94E-03
3.35E-03
4.76E-03
5.11E-03

-1.97E-03
-1.99E-03
-2.03E-03
-1.87E-03
-1.61E-03
-7.21E-04
5.03E-04

Matrix Correction
(without LOI Correction)
Analyte

: SiO2

Accuracy: 2.5
mass%

w/o LOI
with LOI
Standard value (mass%)

X-ray intensity (a. u.)

X-ray intensity (a. u.)

No correction

Matrix
correction
Accuracy: 3.5 mass%

w/o LOI
with LOI
Standard value (mass%)

LOI Correction and Matrix

Correction
Matrix
correction
Accuracy: 3.5 mass%

w/o LOI
with LOI
Standard value (mass%)

: SiO2

X-ray intensity (a. u.)

X-ray intensity (a. u.)

Analyte

LOI correction
+ Matrix cor.
Accuracy:
0.26 mass%

w/o LOI
with LOI
Standard value (mass%)

Wide Analysis Range in XRF

Analysis of Diverse Natural
Minerals
by the Fusion Method
(Synthetic Fusion Bead Added)

Purpose of This Test Analysis

To obtain a good fitting for calibration curves with wide
concentration range of diverse natural minerals by the fusion
method
To obtain a good fitting for calibration curves with synthetic
standard fused beads

Reference Materials for Calibration (1)

Sample

Material

Dil. ratio

Sample

Material

Dil. ratio

BAS203a

Talc

10

NBS688

Basalt rock

10

BCS313-1

High purity silica

10

SRM 1c

Limestone

10

BCS314

Silica brick

10

SRM 69b-1

Bauxite

10

BCS315

Fire brick

10

SRM 696

Bauxite Surinam

10

BCS319

Magnesite

10

SRM 697

Bauxite Dominican

10

BCS368

Dolomite

10

SRM 698

Bauxite Jamaican

10

BCS369

Magnesite-Chrome

22.167

SRM 70a

Potash feldspar

10

BCS370

Magnesite-chrome

22.167

SRM 99a

Soda feldspar

10

BCS375

Soda feldspar

10

R-603

Clay

10

BCS376_1

Potash feldspar

10

R-701

Feldspar

10

BCS358

Zirconia

10

R-801

Pyrophyllite

10

BCS388

Zircon

10

JSS009-2

Pure iron oxide

10

BCS389

High purity magnesium

10

JRRM511

Chrome-magnesia

22.167

BCS393

Limestone

10

JRRM602

Zirconia

10

BCS394

Calcined bauxite

10

JRRM701

AZS

10

BCS395

Bauxite

10

RM-611

Portland cement

10

NBS98a

Plastic clay

10

RM-612

Portland cement

10

NBS120c

Florida phosphate rock

10

RM-613

Portland cement

10

Reference Materials for Calibration (2)

Sample

Material

Dil. ratio

Notes

ECISS782-1

Dolomite

10

ECISS776-1

Fire brick

10

BCS348

Ball clay

10

NIST 81a

Glass sand

10

NIST 278_1

Obsidian rock

10

NIST 1413

Glass sand

10

NBS694

Phosphate rock

10

BAS 683-1-(1)

Iron ore sinter

10.13

BAS 683-1-(2)

Iron ore sinter

10.13

BCS315_Co1

Fire brick with Co AA standard sol.

10

For analysis of Co from the WC container

BCS315_W1

Fire brick with W AA standard sol.

10

For analysis of W from the WC container

NIST278_1_Co05

Obsidian rock with Co AA standard sol.

10

For analysis of Co from the WC container

NIST278_1_W05

Obsidian rock with W AA standard sol.

10

For analysis of W from the WC container

TiO2_10

TiO2 reagent

10

To extend TiO2 calibration range

P2O5_25

LiPO3 reagent

10

To extend P2O5 calibration range

K2O_50

K2CO3 reagent

10

To extend K2O calibration range

CaO_100

CaCO3 reagent

10

To extend CaO calibration range

Na2O_25

Na2CO3 reagent

10

To extend Na2O calibration range

Calibration Range
Unit: mass%

Analyte

Calibration range

Analyte

Calibration range

Na2O

25

Fe2O3

99.84

MgO

96.7

Cr2O3

52.51

Al2O3

88.8

ZrO2

92.7

SiO2

99.78

HfO2

1.63

P2O5

33.34

SO3

6.07

K2O

50

SrO

0.28

CaO

100

Co2O3

1.407

TiO2

10

WO3

1.261

MnO

0.596

Li2B4O7

10

22.167
Dilution ratio
(flux/sample)

Na2O calibration

MgO calibration

Na2CO3
Synthetic bead

Accuracy: 0.048 mass%

Standard value (mass%)

X-ray intensity (a. u.)

X-ray intensity (a. u.)

Accuracy: 0.40 mass%

BCS370
Mg-Cr

BCS369
Mg-Cr
Standard value (mass%)

SiO2 calibration

X-ray intensity (a. u.)

X-ray intensity (a. u.)

Al2O3 calibration

Accuracy: 0.23 mass%

Standard value (mass%)

Accuracy: 0.35 mass%

Standard value (mass%)

P2O5 calibration

SO3 calibration

Phosphat
e rock

Accuracy: 0.017 mass%

Standard value (mass%)

X-ray intensity (a. u.)

X-ray intensity (a. u.)

LiPO3
Synthetic bead

Portland
cement

Accuracy: 0.056 mass%

Standard value (mass%)

K2O calibration

CaO calibration
CaCO3
Synthetic bead

X-ray intensity (a. u.)

X-ray intensity (a. u.)

K2CO3
Synthetic bead

Accuracy: 0.021 mass%

Standard value (mass%)

Accuracy: 0.27 mass%

Standard value (mass%)

TiO2 calibration

Fe2O3 calibration
Fe2O3
Synthetic bead

X-ray intensity (a. u.)

X-ray intensity (a. u.)

TiO2
Synthetic bead

Accuracy: 0.027 mass%

Standard value (mass%)

Iron ore

Accuracy: 0.067
mass%
Standard value (mass%)

Summary
By applying the dilution ratio correction, LOI correction and matrix
correction (theoretical alphas), it is possible to obtain a good fitting for
calibration curves with wide concentration range for diverse natural rocks
and minerals by the fusion method.
With a few calibration standards, it is necessary to use the de Jongh or
Lachance-Traill models, where calibration curves are linear in theory. In this
test, de Jongh model was used because some samples contain significant
LOI content.
With a large number of calibration standards, it is possible to use the JIS
model, where calibration curves can be quadratic.
With synthetic fused beads to extend the calibration range, it is possible to
obtain a good fitting for calibration curves.

Conclusion
The fusion bead method is useful sample preparation for eliminating
hetrogeneity effects, particle size effects, however chemical
reactions can cause the sample weight to decrease or/and increase
during fusion because of volatilization of H2O, CO2 and oxidation.
It is possible to correct error factors in fusion for either the FP
method or the Empirical Calibration method.
It is possible to skip the lengthy independent LOI step in preparing
the samples for fusion, by incorporating the step into the fusion
process and correcting for the associated losses and/or gains via
the correction methods just detailed
It is possible to weigh catch weights and have them recorded in the
dilution correction.
The time savings realized by eliminating the LOI step and supporting
varying dilution ratios improves throughput and cuts the analysis
cost per sample

 Thank you for your attention