EDXRF Analysis of Pressed Powder Nickel Ore

Nickel has been produced from two very different ores, sulfidic and lateritic. The origin of lateritic ore is mainly in tropical countries such as Indonesia and is mined from several depths below the surface, while sulfidic ore is generally discovered jointly with copper ore and is mined underground.

The demand for nickel production has been increasing recently as nickel is a main component in lithium-ion batteries utilized in electric vehicles. A rapid, accurate, and precise technique is required for the assessment of these ores both in the mining and refining processes.

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

Instrumentation

The Thermo Scientific™ ARL™ QUANT’X EDXRF Spectrometer has been fitted with a Silicon Drift Detector (SDD) and a 50 Watt Rh or Ag target X-Ray tube, which is air cooled with a maximum excitation voltage of 50 kV.

A set of nine primary beam filters have been developed to improve the peak-to-background signals for all elements from F to Am. The 10-position auto-sampler with spinner enables neglected analysis of several samples. Its SDD remains the performance benchmark for all energy-dispersive detectors. The large active area of 30 mm² allows efficient capture of characteristic element X-Rays discharged by the sample.

Excitation Conditions

As far as EDXRF is concerned, sensitivity and accuracy are obtained by targeted excitation of the sample to fluoresce only the elements of interest. The ARL QUANT’X EDXRF Spectrometer provides a virtually limitless combination of excitation voltages (4 to 50 kV) and several main beam filters for optimal background control.

As displayed in Table 1, spectra were gathered on every nickel ore sample for a total live time of 5 minutes. Measurement time could be fine-tuned as per the specific applications. The analysis is performed in the air.

Table 1. Analytical conditions. Source: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

Condition Voltage Tube Filter Medium Live Time (s) Elements
Low Za 4 No Filter Air 180 Mg, Al, Si
Low Zb 8 C Thick Air 60 S, Ca, K
Mid Za 16 Ag Thin Air 60 Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn

 

Sample Preparation

Calibration was performed with the help of 17 nickel ore Certified Reference Materials (CRM) from OREAS®. Samples were made to press into pellets without binder at around 20 tons. Table 2 displays the concentration ranges of the various oxides covered by the calibration and the R² and RMSE (root mean square error) values achieved for the various compounds.

Table 2. Concentration ranges and calibration parameter values for the analysis of nickel ore. Source: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

Element Min % Max % R2 RMSE
MgO 0.7 27.3 0.9986 0.4
Al2O3 1.6 17.5 0.9985 0.2
SiO2 22.8 48.0 0.9896 0.8
SO3 0.03 0.19 0.9897 0.007
K2O 0.069 0.228 0.9935 0.006
CaO 0.13 3.11 0.9995 0.019
TiO2 0.02 1.36 0.9998 0.003
Cr2O3 0.17 1.75 0.9971 0.02
MnO 0.11 1.94 0.9997 0.008
Fe2O3 12.7 46.0 0.9986 0.4
Co 0.023 0.090 0.9839 0.003
Ni 0.05 2.94 0.9993 0.02
Cu 0.007 0.05 0.9999 0.00014
Zn 0.007 0.035 0.9968 0.0005

 

Calibration

Calibration curves have been derived concerning element characteristic X-Ray intensity to oxide concentration. X-Ray fluorescence quantifies elements, but the outcomes could be related directly to the oxide forms of such elements when only one single form of oxide is present in the sample. Figures 1 to 14 display the calculated versus provided concentration plots achieved for Ni, MgO, Al₂O₃, SiO₂, SO₃, K₂O, CaO, TiO₂, Cr₂O₃, MnO, Fe₂O₃, Co, Cu, and Zn.

Ni Calculated versus Given Concentrations.

Figure 1. Ni Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

MgO Calculated versus Given Concentrations.

Figure 2. MgO Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

Al2O3 Calculated versus Given Concentrations.

Figure 3. Al2O3 Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

SiO2 Calculated versus Given Concentrations.

Figure 4. SiO2 Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

SO3 Calculated versus Given Concentrations.

Figure 5. SO3 Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

K2O Calculated versus Given Concentrations.

Figure 6. K2O Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

CaO Calculated versus Given Concentrations.

Figure 7. CaO Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

TiO2 Calculated versus Given Concentrations.

Figure 8. TiO2 Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

Cr2O3 Calculated versus Given Concentrations.

Figure 9. Cr2O3 Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

MnO Calculated versus Given Concentrations.

Figure 10. MnO Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

Fe2O3 Calculated versus Given Concentrations.

Figure 11. Fe2O3 Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

Co Calculated versus Given Concentrations.

Figure 12. Co Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

Cu Calculated versus Given Concentrations.

Figure 13. Cu Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

Zn Calculated versus Given Concentrations.

Figure 14. Zn Calculated versus Given Concentrations. Image Credit: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

Validation

Two nickel ore reference materials (192 and 199) were utilized to validate the calibration. Table 3 displays the analysis outcomes for such reference materials. CRM reference values are made to compare with the average of 10 replicate analyses of the two CRMs while Tables 4a and 4b display the repeatability outcomes for every CRM.

Table 3. Accuracy of results for standards 192 and 199 using ARL QUANT’X Spectrometer. Source: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

  MgO
%
Al2O3
%
SiO2
%
SO3
%
K2O
%
CaO
%
TiO2
%
Cr2O3
%
MnO
%
Fe2O3
%
Co
%
Ni
%
Cu
%
Zn
%
192 Reference 21.32 2.76 43.58 - - 0.313 0.036 0.9129 0.277 18.1 0.0404 1.77 - 0.0176
192 Analysis 21.86 2.61 43.97 0.03 0.0104 0.308 0.034 0.8854 0.269 18.2 0.0376 1.80 0.0060 0.0164
199 Reference 0.742 17.47 24.93 0.08 0.069 0.208 0.842 0.686 1.94 41.01 0.0554 0.0995 0.0189 0.0198
199 Analysis 0.880 17.94 24.58 0.07 0.0724 0.213 0.840 0.695 1.95 40.68 0.0566 0.0984 0.0189 0.0206

 

Table 4a. Repeatability results for standards 192 using ARL QUANT’X Spectrometer. Source: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

  MgO
%
Al2O3
%
SiO2
%
SO3
%
K2O
%
CaO
%
TiO2
%
Cr2O3
%
MnO
%
Fe2O3
%
Co
%
Ni
%
Cu
%
Zn
%
Repeats 01 21.853 2.574 44.171 0.032 0.0104 0.307 0.034 0.885 0.269 18.187 0.036 1.803 0.0060 0.0164
Repeats 02 21.992 2.565 43.843 0.031 0.0104 0.309 0.032 0.882 0.266 18.175 0.038 1.803 0.0060 0.0158
Repeats 03 21.785 2.633 44.018 0.032 0.0104 0.307 0.034 0.886 0.268 18.174 0.039 1.802 0.0060 0.0164
Repeats 04 21.843 2.625 43.916 0.029 0.0104 0.308 0.033 0.886 0.270 18.202 0.037 1.800 0.0060 0.0164
Repeats 05 21.448 2.712 44.334 0.033 0.0104 0.308 0.038 0.886 0.270 18.209 0.036 1.807 0.0060 0.0167
Repeats 06 21.950 2.589 43.882 0.032 0.0104 0.307 0.034 0.888 0.268 18.188 0.037 1.800 0.0060 0.0162
Repeats 07 21.901 2.607 43.973 0.030 0.0104 0.307 0.030 0.886 0.270 18.173 0.039 1.804 0.0060 0.0167
Repeats 08 21.958 2.586 43.913 0.028 0.0104 0.306 0.034 0.886 0.270 18.199 0.038 1.803 0.0060 0.0165
Repeats 09 21.950 2.626 43.707 0.031 0.0104 0.308 0.038 0.888 0.269 18.185 0.038 1.802 0.0060 0.0163
Repeats 10 21.964 2.581 43.964 0.030 0.0104 0.310 0.035 0.882 0.271 18.198 0.040 1.804 0.0060 0.0166
                             
Average 21.864 2.610 43.972 0.031 0.0104 0.308 0.034 0.885 0.269 18.189 0.038 1.803 0.0060 0.0164
1-Sigma 0.160 0.043 0.175 0.002 - 0.001 0.002 0.002 0.001 0.013 0.001 0.002 - 0.0003
% RSD 0.73 1.65 0.40 4.86 - 0.32 6.95 0.23 0.51 0.07 3.34 0.12 - 1.62
Minimum 21.448 2.565 43.707 0.028 0.0104 0.306 0.030 0.882 0.266 18.173 0.036 1.800 0.0060 0.0158
Maximum 21.992 2.712 44.334 0.033 0.0104 0.310 0.038 0.888 0.271 18.209 0.040 1.807 0.0060 0.0167

 

Table 4b. Repeatability results for standards 199 using ARL QUANT’X Spectrometer. Source: Thermo Scientific-Chemical Analysis-Spectroscopy Solutions

  MgO
%
Al2O3
%
SiO2
%
SO3
%
K2O
%
CaO
%
TiO2
%
Cr2O3
%
MnO
%
Fe2O3
%
Co
%
Ni
%
Cu
%
Zn
%
Repeats 01 1.009 17.750 24.609 0.069 0.074 0.213 0.845 0.696 1.943 40.653 0.056 0.098 0.0191 0.0212
Repeats 02 1.053 17.755 24.563 0.073 0.071 0.213 0.839 0.693 1.945 40.680 0.058 0.099 0.0192 0.0205
Repeats 03 0.981 17.827 24.559 0.077 0.073 0.215 0.847 0.694 1.942 40.698 0.056 0.098 0.0190 0.0209
Repeats 04 0.773 18.055 24.612 0.074 0.073 0.213 0.838 0.694 1.950 40.683 0.057 0.099 0.0186 0.0208
Repeats 05 0.887 17.903 24.685 0.074 0.073 0.214 0.841 0.690 1.950 40.651 0.058 0.098 0.0189 0.0208
Repeats 06 1.203 17.767 24.359 0.073 0.071 0.213 0.838 0.697 1.940 40.669 0.055 0.098 0.0188 0.0196
Repeats 07 1.024 17.885 24.488 0.078 0.074 0.211 0.848 0.690 1.939 40.656 0.057 0.098 0.0190 0.0209
Repeats 08 0.389 18.263 24.756 0.074 0.073 0.213 0.836 0.698 1.953 40.693 0.058 0.099 0.0188 0.0202
Repeats 09 0.746 18.160 24.516 0.076 0.072 0.215 0.835 0.699 1.941 40.687 0.055 0.099 0.0190 0.0210
Repeats 10 0.737 18.040 24.614 0.075 0.071 0.213 0.836 0.695 1.948 40.688 0.058 0.098 0.0186 0.0204
                             
Average 0.880 17.941 24.576 0.074 0.072 0.213 0.840 0.695 1.945 40.676 0.057 0.098 0.0189 0.0206
1-Sigma 0.229 0.181 0.109 0.002 0.001 0.001 0.005 0.003 0.005 0.017 0.001 0.001 0.0002 0.0005
% RSD 26.03 1.01 0.44 3.28 1.56 0.49 0.56 0.43 0.25 0.04 2.29 0.62 1.06 2.27
Minimum 0.389 17.750 24.359 0.069 0.071 0.211 0.835 0.690 1.939 40.651 0.055 0.098 0.0186 0.0196
Maximum 1.203 18.263 24.756 0.078 0.074 0.215 0.848 0.699 1.953 40.698 0.058 0.099 0.0192 0.0212

 

Conclusion

This article discusses the suitability of the ARL QUANT’X EDXRF spectrometer for studying nickel ores samples.

This compact instrument enables quick and trustworthy analysis of nickel ores. Precision and repeatability outcomes show that satisfactory results are achievable for an analysis of pressed powders in air. This is a considerable benefit for nickel ore mines which frequently tend to function in remote areas.

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.

Citations

Please use one of the following formats to cite this article in your essay, paper or report:

  • APA

    Thermo Fisher Scientific - Elemental and Phase Analysis. (2023, February 07). EDXRF Analysis of Pressed Powder Nickel Ore. AZoM. Retrieved on July 23, 2024 from https://www.azom.com/article.aspx?ArticleID=22384.

  • MLA

    Thermo Fisher Scientific - Elemental and Phase Analysis. "EDXRF Analysis of Pressed Powder Nickel Ore". AZoM. 23 July 2024. <https://www.azom.com/article.aspx?ArticleID=22384>.

  • Chicago

    Thermo Fisher Scientific - Elemental and Phase Analysis. "EDXRF Analysis of Pressed Powder Nickel Ore". AZoM. https://www.azom.com/article.aspx?ArticleID=22384. (accessed July 23, 2024).

  • Harvard

    Thermo Fisher Scientific - Elemental and Phase Analysis. 2023. EDXRF Analysis of Pressed Powder Nickel Ore. AZoM, viewed 23 July 2024, https://www.azom.com/article.aspx?ArticleID=22384.

Ask A Question

Do you have a question you'd like to ask regarding this article?

Leave your feedback
Your comment type
Submit

While we only use edited and approved content for Azthena answers, it may on occasions provide incorrect responses. Please confirm any data provided with the related suppliers or authors. We do not provide medical advice, if you search for medical information you must always consult a medical professional before acting on any information provided.

Your questions, but not your email details will be shared with OpenAI and retained for 30 days in accordance with their privacy principles.

Please do not ask questions that use sensitive or confidential information.

Read the full Terms & Conditions.