Analyzing Nickel Ore with Wavelength-Dispersive XRF (WDXRF)

Two very different ores, lateritic and sulfidic, are used in nickel production. Lateritic ore is seen in tropical countries, such as Indonesia, and is mined from several depths below the surface, while sulfidic ore is generally found with copper ore and mined underground.

In the past few years, nickel production has witnessed a high demand; it is a major component in lithium-ion batteries and is utilized in electric vehicles. Therefore, a quick, precise, and accurate technique is required for quantifying such ores in the refining and mining processes.

X-Ray fluorescence spectrometry (XRF) is considered a well-established analytical technique to identify chemical composition in materials exhibiting high precision and the least sample preparation. It is a favored method in process and quality control throughout several industries.

Instrumentation

The Thermo Scientific ARL OPTIM’X™ WDXRF Spectrometer has been developed for easy use with the least operation and maintenance charges. The instrument is equipped with a Thermo Scientific SmartGonio™ Goniometer spanning elements from fluorine (9F) to uranium (92U). Two power versions exist, either 50 W or the new 200 W version. The 50 W version has been utilized for the tests displayed in this report.

The instrument does not need internal or external water cooling and executes 10 times better spectral resolution compared to a conventional EDXRF instrument as well as excellent stability and accuracy. It displays good performance for magnesium (12Mg), sodium (11Na), and fluorine (9F).

Analytical Conditions

As displayed in Table 1, spectra were gathered from every nickel ore sample for a complete analysis time of just 10.4 minutes with the help of the ARL OPTIM’X WDXRF Spectrometer at 50 W power. Measurement time could be further fine-tuned as per the particular applications.

All counting time can be reduced by a factor of 2.5 using the 200 W version of the ARL OPTIM’X WDXRF Spectrometer while still enabling the same precision and accuracy. Therefore, a complete analysis time would reduce to around four minutes

Table 1. Analytical conditions. Source: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Name Component type Analysis
time(s) kV mA
Ni Ka 1,2 Gonio XRF 36 30 1.67
Zn Ka 1,2 Gonio XRF 60 30 1.67
Cr Ka 1,2 Gonio XRF 36 30 1.67
Ti Ka 1,2 Gonio XRF 36 30 1.67
Si Ka 1,2 Gonio XRF 36 30 1.67
S Ka 1,2 Gonio XRF 36 30 1.67
P Ka 1,2 Gonio XRF 60 30 1.67
Mg Ka 1,2 Gonio XRF 60 30 1.67
K Ka 1,2 Gonio XRF 60 30 1.67
Ca Ka 1,2 Gonio XRF 36 30 1.67
Al Ka 1,2 Gonio XRF 36 30 1.67
Mn Ka 1,2 Gonio XRF 36 30 1.67
Co Ka 1,2 Gonio XRF 60 30 1.67
Fe Ka 1,2 Gonio XRF 36 30 1.67

 

Sample Preparation

Calibration was carried out with the 18 nickel ore CRMs. Samples were made to fuse into beads in the absence of ignition with a sample-to-flux ratio of 1:20. Ammonium nitrate oxidizer was added to the fusion mix.

Table 2 displays the concentration ranges of the various oxides covered by the calibration. The R2 and SEE (standard error of estimate) values were achieved for the various compounds.

Table 2. Concentration ranges and calibration parameter values for the analysis of nickel ore. Source: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Elements Calibration R2 SEE
N Min % Max %
Al2O3 17 1.599 17.470 0.9998 0.0813
CaO 18 0.133 3.106 0.9999 0.0096
Cr2O3 17 0.170 1.750 0.9980 0.0204
Fe2O3 15 12.728 45.990 0.9998 0.1521
K2O 5 0.069 0.228 0.9831 0.0089
MgO 17 0.742 27.306 0.9998 0.1551
MnO 18 0.109 1.940 0.9996 0.0096
NiO 18 0.066 3.740 0.9996 0.0214
SiO2 16 22.790 47.970 0.9993 0.2415
TiO2 13 0.035 1.360 0.9998 0.0063
Co3O4 16 0.031 0.123 0.9921 0.0027
P2O5 7 0.005 0.173 0.9847 0.0099
SO3 7 0.004 0.189 0.9763 0.0108
ZnO 18 0.009 0.044 0.9504 0.0023

 

Calibration

Calibration curves were derived relating element characteristic X-Ray intensities to oxide concentration. X-Ray fluorescence quantifies elements, but the outcomes could be directly related to the oxide forms of such elements when only one single form of oxide is present in the sample. Figures 1–10 display the calibration curves achieved for NiO, MgO, CaO, Al2O3, Cr2O3, MnO, Fe2O3, K2O, SiO2, and TiO2.

NiO calibration graph.

Figure 1. NiO calibration graph. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

MgO calibration graph.

Figure 2. MgO calibration graph. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Al2O3 calibration graph.

Figure 3. Al2O3 calibration graph. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

SiO2 calibration graph.

Figure 4. SiO2 calibration graph. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

K2O calibration graph.

Figure 5. K2O calibration graph. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

CaO calibration graph.

Figure 6. CaO calibration graph. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

TiO2 calibration graph.

Figure 7. TiO2 calibration graph. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Cr2O3 calibration graph.

Figure 8. Cr2O3 calibration graph. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

MnO calibration graph.

Figure 9. MnO calibration graph. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Fe2O3 calibration graph.

Figure 10. Fe2O3 calibration graph. Image Credit: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Validation

To validate the calibration, three nickel ore reference materials (181, 184, and 198) were utilized. Table 6 displays the analysis outcomes for such reference materials. CRM reference values are compared with the average of 10 replicate analyses of the three CRMs, while Tables 3–5 display the repeatability of the 10 replicates for every CRM.

Table 3. Repeatability results of nickel ore using the ARL OPTIM’X WDXRF Spectrometer for sample 181. Source: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Elements Sample 181: all values are %
Al2O3 CaO Co3O4 Cr2O3 Fe2O3 K2O MgO MnO NiO P2O5 SO3 SiO2 TiO2 ZnO
Rep 1 11.65 2.37 0.060 1.26 35.71 0.129 2.07 0.164 0.664 0.034 0.184 33.52 0.320 0.009
Rep 2 11.33 2.37 0.060 1.26 35.70 0.133 2.04 0.168 0.669 0.039 0.173 33.48 0.326 0.009
Rep 3 11.56 2.37 0.061 1.25 35.57 0.131 2.16 0.169 0.658 0.031 0.181 33.40 0.341 0.009
Rep 4 11.46 2.36 0.064 1.24 35.61 0.139 2.07 0.169 0.657 0.026 0.211 33.50 0.330 0.010
Rep 5 11.49 2.36 0.059 1.25 35.65 0.132 2.14 0.169 0.661 0.032 0.191 33.35 0.329 0.012
Rep 6 11.57 2.35 0.060 1.25 35.68 0.138 2.07 0.165 0.658 0.026 0.166 33.66 0.333 0.007
Rep 7 11.37 2.35 0.059 1.26 35.62 0.130 2.05 0.163 0.666 0.035 0.184 33.73 0.326 0.011
Rep 8 11.31 2.35 0.062 1.27 35.70 0.128 2.02 0.168 0.666 0.021 0.207 33.62 0.336 0.010
Rep 9 11.63 2.39 0.059 1.26 35.68 0.126 2.05 0.166 0.664 0.027 0.180 33.51 0.343 0.009
Rep 10 11.59 2.35 0.061 1.26 35.69 0.132 2.11 0.168 0.656 0.028 0.170 33.43 0.335 0.014
AVG 11.50 2.36 0.060 1.26 35.66 0.132 2.08 0.167 0.662 0.030 0.185 33.52 0.332 0.010
SD 0.124 0.013 0.002 0.008 0.047 0.004 0.045 0.002 0.005 0.005 0.015 0.119 0.007 0.002

 

Table 4. Repeatability results of nickel ore using the ARL OPTIM’X WDXRF Spectrometer for sample 184. Source: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Elements Sample 184: all values are %
Al2O3 CaO Co3O4 Cr2O3 Fe2O3 K2O MgO MnO NiO P2O5 SO3 SiO2 TiO2 ZnO
Rep 1 4.58 0.215 0.121 1.760 39.14 0.011 3.04 0.667 1.280 0.036 0.032 42.22 0.055 0.033
Rep 2 4.47 0.211 0.121 1.760 39.20 0.011 2.92 0.670 1.290 0.033 0.037 42.35 0.071 0.033
Rep 3 4.51 0.216 0.120 1.770 39.22 0.012 3.07 0.666 1.290 0.030 0.043 42.41 0.062 0.033
Rep 4 4.53 0.216 0.121 1.760 39.20 0.011 3.11 0.665 1.290 0.045 0.042 42.27 0.062 0.028
Rep 5 4.49 0.218 0.121 1.770 39.27 0.012 3.06 0.674 1.290 0.050 0.050 42.62 0.059 0.032
Rep 6 4.58 0.209 0.120 1.760 39.12 0.010 3.07 0.660 1.280 0.045 0.032 42.64 0.066 0.034
Rep 7 4.48 0.214 0.124 1.750 39.09 0.014 3.15 0.667 1.300 0.038 0.031 42.32 0.058 0.034
Rep 8 4.60 0.217 0.124 1.750 39.13 0.009 3.05 0.666 1.290 0.040 0.049 42.51 0.065 0.031
Rep 9 4.50 0.224 0.120 1.780 39.27 0.014 3.02 0.657 1.290 0.031 0.056 42.26 0.066 0.031
Rep 10 4.42 0.228 0.125 1.760 39.14 0.012 3.05 0.674 1.300 0.032 0.061 42.37 0.059 0.030
AVG 4.51 0.217 0.122 1.760 39.18 0.012 3.05 0.667 1.290 0.038 0.043 42.40 0.062 0.032
SD 0.057 0.006 0.002 0.009 0.063 0.001 0.060 0.005 0.007 0.007 0.010 0.148 0.005 0.002

 

Table 5. Repeatability results of nickel ore using the ARL OPTIM’X WDXRF Spectrometer for sample 198. Source: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Elements Sample 198: all values are %
Al2O3 CaO Co3O4 Cr2O3 Fe2O3 K2O MgO MnO NiO P2O5 SO3 SiO2 TiO2 ZnO
Rep 1 15.75 0.350 0.106 0.285 46.18 0.100 0.807 1.53 0.085 0.167 0.105 22.83 1.35 0.022
Rep 2 15.74 0.345 0.106 0.281 46.15 0.099 0.841 1.51 0.088 0.170 0.115 23.04 1.36 0.022
Rep 3 15.83 0.348 0.109 0.281 46.08 0.098 0.808 1.52 0.081 0.179 0.124 22.84 1.37 0.024
Rep 4 15.79 0.357 0.106 0.269 46.09 0.103 0.820 1.51 0.090 0.179 0.119 22.91 1.36 0.021
Rep 5 15.89 0.368 0.105 0.271 46.07 0.106 0.882 1.52 0.086 0.179 0.132 23.05 1.36 0.020
Rep 6 15.72 0.349 0.108 0.273 46.12 0.100 0.829 1.52 0.091 0.170 0.132 22.89 1.36 0.024
Rep 7 15.67 0.357 0.112 0.279 46.18 0.101 0.797 1.51 0.092 0.179 0.128 22.85 1.36 0.023
Rep 8 15.88 0.342 0.109 0.281 46.01 0.099 0.870 1.51 0.088 0.171 0.119 22.90 1.38 0.024
Rep 9 15.90 0.355 0.111 0.283 46.04 0.107 0.861 1.51 0.089 0.186 0.117 23.01 1.36 0.026
Rep 10 15.65 0.345 0.112 0.275 46.22 0.106 0.817 1.51 0.089 0.172 0.126 23.13 1.37 0.024
AVG 15.78 0.352 0.108 0.278 46.11 0.102 0.833 1.51 0.088 0.175 0.122 22.95 1.36 0.023
SD 0.091 0.008 0.003 0.005 0.068 0.003 0.029 0.007 0.003 0.006 0.008 0.104 0.008 0.002

 

Table 6. Analysis results of nickel ore using the ARL OPTIM’X WDXRF Spectrometer. Source: Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers

Element Sample 181 Sample 184 Sample 198
CRM AVG Difference CRM AVG Difference CRM AVG Difference
Al2O3 11.55 11.50 0.050 4.622 4.510 0.112 15.81 15.78 0.030
CaO 2.372 2.360 0.012 0.216 0.217 -0.001 0.346 0.352 -0.006
Cr2O3 0.061 0.060 0.001 0.123 0.122 0.001 0.110 0.108 0.002
Fe2O3 1.241 1.260 -0.019 1.75 1.76 -0.010 0.285 0.278 0.007
K2O 35.944 35.66 0.284 39.298 39.180 0.118 45.99 46.11 -0.120
MgO 0.132 0.132 0.000 NA NA NA 0.101 0.102 -0.001
MnO 2.054 2.08 -0.026 3.045 3.050 -0.005 0.798 0.833 -0.035
NiO 0.168 0.167 0.001 0.676 0.667 0.009 1.53 1.51 0.020
SiO2 0.652 0.662 -0.010 1.295 1.290 0.005 0.088 0.088 0.000
TiO2 0.017 0.030 -0.013 0.017 0.038 -0.021 0.161 0.175 -0.014
Co3O4 0.189 0.185 0.004 0.060 0.043 0.017 NA NA NA
P2O5 33.785 33.52 0.265 42.252 42.400 -0.148 22.79 22.95 -0.160
SO3 0.339 0.332 0.007 NA NA NA 1.36 1.36 0.000
ZnO 0.012 0.010 0.002 0.035 0.032 0.003 0.026 0.023 0.003

 

Conclusion

This article has reviewed the ARL OPTIM’X WDXRF Spectrometer's suitability for studying nickel ore samples. This compact instrument enables rapid and trustworthy analysis outcomes integrated with outstanding repeatability.

A complete analysis time of 10.4 minutes was utilized with the ARL OPTIM’X WDXRF Spectrometer at 50 W power. Measurement time could be fine-tuned as per specific applications.

All counting time could be reduced by a factor of 2.5 while utilizing the 200 W version of the ARL OPTIM'X WDXRF Spectrometer while still enabling the same precision and accuracy. In this context, the total analysis time would be around four minutes.

This information has been sourced, reviewed and adapted from materials provided by Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers.

For more information on this source, please visit Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers.

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