How to Measure Nickel Ore?

Nickel is derived from two extremely different ores; lateritic and sulfidic. Lateritic ore is typically found in tropical countries, such as Indonesia and mined from multiple depths beneath the surface, while sulfidic ore is generally found in combination with copper ore through underground mining.

As nickel is an essential component of the lithium-ion batteries that are used in electric vehicles and other everyday devices, there has recently been a significant surge in demand for nickel production.

Resultingly, a rapid and accurate analysis method is necessary for the precise quantification of these ores across both the mining and refining processes.

X-Ray fluorescence spectrometry (XRF) is a long-established, high accuracy analytical method that has the ability to establish chemical composition in materials with minimum sample preparation, making it the preferred technique in process and quality control across a number of industries.

Instrumentation

The Thermo Scientific™ ARL OPTIM’X™ WDXRF Spectrometer has been developed with easy operation in mind and with maintenance costs completely minimized.

The instrument includes a Thermo Scientific SmartGonio, which is able to cover elements from fluorine (9F) to uranium (92U). Two different versions exist, either in 50 W or the new 200 W version. The 50 W version was employed for the tests outlined in this article.

External or internal water cooling is not necessary with this instrument which possesses 10 times better spectral resolution than a traditional EDXRF instrument as well as best-in-class precision and stability. It has an outstanding performance for sodium (11Na), magnesium (12Mg) and fluorine (9F).

Analytical Conditions

As Table 1 demonstrates, spectra were taken from each Nickel Ore sample for an overall analysis time of 10.4 minutes utilizing the ARL OPTIM’X at 50 W power. Measurement time can be better calibrated as required for each specific application.

Table 1. Analytical Conditions. Source: Thermo Fisher Scientific – Materials & Structural Analysis

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

 

Overall counting time can be reduced by a factor of 2.5 when using the 200 W version of ARL OPTIM’X while still achieving equivocal accuracy and precision. Thus, overall analysis time would decrease to around 4 minutes.

Sample Preparation

Calibration was conducted with 18 Nickel Ore CRMs. Samples with a sample to flux ratio of 1:20 were consolidated into beads without ignition. Ammonium nitrate oxidizer was then introduced into the fusion mix.

Table 2 displays the concentration ranges of the various oxides the calibration covers. The R2 and SEE (Standard Error of Estimates) values were acquired for each of the different compounds.

Table 2. Concentration ranges and calibration parameter values for the analysis of Nickel Ore. Source: Thermo Fisher Scientific – Materials & Structural Analysis

Element 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 derive from associating element X-Ray intensity characteristics to oxide concentration.

X-Ray fluorescence measures elements, but the results may directly correspond to the oxide forms of these elements when there is only one single form of oxide present in the sample. Figures 1 -10 exhibit the calibration curves acquired for NiO, MgO, Al2O3, CaO, Cr2O3, Fe2O3, K2O, MnO, SiO2 and TiO2, respectfully.

NiO Calibration Graph.

Figure 1. NiO Calibration Graph. Thermo Fisher Scientific – Materials & Structural Analysis

MgO Calibration Graph.

Figure 2. MgO Calibration Graph. Thermo Fisher Scientific – Materials & Structural Analysis

Al2O3 Calibration Graph.

Figure 3. Al2O3 Calibration Graph. Thermo Fisher Scientific – Materials & Structural Analysis

SiO2 Calibration Graph.

Figure 4. SiO2 Calibration Graph. Thermo Fisher Scientific – Materials & Structural Analysis

K2O Calibration Graph.

Figure 5. K2O Calibration Graph. Thermo Fisher Scientific – Materials & Structural Analysis

CaO Calibration Graph.

Figure 6. CaO Calibration Graph. Thermo Fisher Scientific – Materials & Structural Analysis

TiO2 Calibration Graph.

Figure 7. TiO2 Calibration Graph. Thermo Fisher Scientific – Materials & Structural Analysis

Cr2O3 Calibration Graph.

Figure 8. Cr2O3 Calibration Graph. Thermo Fisher Scientific – Materials & Structural Analysis

MnO Calibration Graph.

Figure 9. MnO Calibration Graph. Thermo Fisher Scientific – Materials & Structural Analysis

Fe2O3 Calibration Graph.

Figure 10. Fe2O3 Calibration Graph. Thermo Fisher Scientific – Materials & Structural Analysis

Validation

To validate the calibration values, three Nickel Ore reference materials (181, 184 and 198) were used.

Table 6 exhibits the results of the analysis for each of these reference materials. CRM reference values are contrasted against the average of 10 replicate analyses of the three CRMs, while Tables 3-5 demonstrates how repeatable each of the 10 replicates is relating to each CRM.

Table 3. Repeatability results of Nickel Ore using ARL OPTIM’X Spectrometer for sample 181. Source: Thermo Fisher Scientific – Materials & Structural Analysis

Sample 181– all values are %
Elements 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 ARL OPTIM’X Spectrometer for sample 184. Source: Thermo Fisher Scientific – Materials & Structural Analysis

Sample 184 – all values are %
Elements 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 ARL OPTIM’X Spectrometer for sample 198. Source: Thermo Fisher Scientific – Materials & Structural Analysis

Sample 198– all values are %
Elements 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 ARL OPTIM’X Spectrometer. Source: Thermo Fisher Scientific – Materials & Structural Analysis

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 outlines the aptitude of the ARL OPTIM’X spectrometer for the accurate analysis of nickel ore samples. This instrument facilitates reliable and rapid analysis results in combination with exceptional repeatability in a compact housing.

An overall analysis time of 10.4 minutes was employed with the ARL OPTIM’X at 50 W power. Measurement time can be calibrated further in line with each specific application.

All counting time may be reduced by a factor of 2.5 when the 200 W version of ARL OPTIM’X is used and accomplishes equivalent accuracy and precision. Thus, the overall analysis time required would decrease to around 4 minutes.

This information has been sourced, reviewed and adapted from materials provided by Thermo Fisher Scientific – Materials & Structural Analysis.

For more information on this source, please visit Thermo Fisher Scientific – Materials & Structural Analysis.

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