ALUMINUM TRACE ELEMENTS ANALYSIS BY EPSILON 1 FOR SMALL SPOT ANALYSIS

Authored by Hussain Al Halwachi. Hussain has published a lot of researches in XRD and XRF filed related to aluminum smelting technology. He has a wide experience in industrial laboratories. He is specialized in X-ray fields and Carbon analyses. He developed many alternative methods in the X-ray filed to replace wet chemical procedures. He is holding B.sc in Chemistry from the University of Bahrain, and MBA from Arabian Gulf University in collaboration with ESSEC University – France.

The amount of alloying materials and trace elements in aluminum metal are usually measured by Optical emission spectroscopy (OES) technique, which is an accurate and reliable method applied in most aluminum smelters and downstream industries. In the absence of an OES machine, it is extremely difficult to decide the amount of alloying materials required for each aluminum alloy, and certification of final aluminum product cannot be carried out.

Recently, a new analytical application was developed by Hussain Al Halwachi, a researcher from Aluminum Bahrain Alba, using the Epsilon 1 EDXRF machine for small spot analysis. The application was successfully capable to generate a backup for OES to measure the trace elements in aluminum metal with very high accuracy. In spite of known factors and difficulties in measuring a few of the light elements in Energy-dispersive X-ray fluorescence (EDXRF) in the lower range, Epsilon 1 for small spot analysis was able to measure the low ranges of Silicon and Manganese, which are crucial elements in aluminum alloys.

 

Omnian calibration was modified by adding six reference materials certified by Rio Tinto Alcan (RTA). Further an aluminum in-type standard was generated as TAG to measure aluminum samples. Repeatability and reproducibility tests performed, revealed the reliability of the application. The beauty in the new application is that it can assist in measuring even irregular shapes of aluminum pieces and analyze them without sample facing, which help heavily in metal recycling.

The research was recently published in Light Metals 2020, which is the annual book gathering the technical papers for the annual international conference conducted by the minerals, metals & materials society (TMMS) and attended by 4000 worldwide researchers.

Epsilon 1 for small spot analysis is able to measure most of trace elements in aluminum metal samples with very high accuracy, repeatability and precision. Tests showed confidently that the machine is able to produce accurate results

HUSSAIN AL HALWACHI

Useful links:

References:

Al Halwachi H. (2020) Aluminum Trace Elements Analyses Using Epsilon 1 Meso EDXRF Technique. In: Tomsett A. (eds) Light Metals 2020. The Minerals, Metals & Materials Series. Springer, Cham- DOI: https://doi.org/10.1007/978-3-030-36408-3_27

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Originally Posted by: Malvern Panalytical (www.malvernpanalytical.com) on 7 May 2020

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VALUE OF MINERALOGICAL ANALYSES FOR BASE METAL MINING AND BENEFICIATION – COPPER

In the blog about “Value of mineralogical monitoring” series, we discussed the value of tracking the mineralogical composition for efficient ore beneficiation on the examples of copper and nickel ore. This blog elaborates on copper ore application in more detail.

Complex mineralogy of copper ore

Copper, being a transition metal, is part of many mineralogical phases. Over 150 copper minerals were identified, however, only a few are of economic importance. Copper minerals can be divided into three groups: (i) primary sulphide minerals (e.g. chalcopyrite, bornite, and enargite); (ii) oxides, formed by weathering of primary sulphides (e.g. cuprite, malachite, chrysocolla and covellite); and (iii) secondary sulphides (e.g. chalcocite and covellite) formed from copper leached from near-surface primary sulphides.

The complex mineralogy of copper ore deposits presents a challenge for effective mine planning and further beneficiation steps. Every mineral behaves differently during the flotation or leaching; therefore, mineralogy analysis will help to select correct reagents and efficiently use them. Apart from accurate quantification of economically valuable copper sulphides and oxides, the presence of gangue minerals, like quartz, talc, clays, pyroxenes, or amphiboles has a huge influence on processing and recovery rate.

Failure to adequately monitor copper ore mineralogy can result in reduced recovery rate due to significant variance of the feed and wrong calculation of oxide/sulphide ratio, reduced grinding, and pumping efficiency due to the presence of soft and hard minerals or increased acid consumption due to alteration minerals such as clays.  The combined impact can lead to tens of millions of losses, which can be prevented if accurate and frequent mineralogy checks are in place.  

Earlier we summarised established that X-ray diffraction (XRD) is fast, versatile and accurate mineralogy probe, which can be easily implemented in the process flow at mine operation and processing plant. In the following case study, we evaluate the accuracy of XRD for resolving mineralogical composition of copper ore using 100 samples from a drill core of a Northern American copper ore deposit.

Accurate characterization of copper ore mineralogy by XRD

One hundred samples were prepared as pressed pellets and measured on Aeris Minerals benchtop diffractometer with a scan time of 10 minutes, followed by an automatic quantitative phase analysis. Figure 1 shows the result of XRD analysis using Aeris Minerals tabletop diffractometer of copper ore sample.

Figure 1. Quantitative phase analysis of complex copper ore using Aeris Minerals tabletop diffractometer. Measurement time per sample is 10 minutes.

Any XRD pattern is a set of diffraction peaks of different intensities, located at certain diffraction angles (2q), specific to a certain mineralogical phase. Peak positions enable identification of present phases. The relative intensities of each mineral contribution to the XRD pattern allows us to quantify the relative amount of each present mineral using full-pattern Rietveld refinement [1].

The analyzed sample set is characterized by a very complex mineral composition, varying from sample to sample (Figure 2, top). In total 23 different minerals were identified in the analyzed sample set. Main copper-bearing minerals are a mix of sulphides and oxides: chalcopyrite CuFeS2, cuprite Cu2O, tenorite CuO, brochantite Cu4[(OH)6(SO4)] and serpierite Ca(Cu, Zn). The complex mineralogy of Cu-bearing phases should be considered in the planning of the next processing steps. Oxides and sulphides should be separated and concentrated. Based on the relative phase amounts, the type and quantity of active agents for flotation and leaching should be identified.

Figure 2. Quantitative phase analysis of complex copper ore (top); comparison of total copper and iron content, calculated from mineral composition (black squares), and bulk chemical analyses using (red cycles).

The majority of the analyzed samples are very high in quartz (Figure 2, top).  Quartz is a hard mineral, which will increase wear and tear of the crushing and milling equipment. A significant amount of talc and clay minerals also a reason for concern. These soft minerals are known to cause issues during flotation, increase consumption of acid used for leaching, finally, soft minerals lead to tubes clogging and blockage, reduce milling and pumping efficiency, etc.

Performed quantitative mineralogy analysis (Figure 2, top) allows us to take several decisions to optimize mine planning, further downstream processing, and allows fast counteractions.  But how accurate are the presented results?

Using the identified mineral quantities, the total oxides can be calculated, which can be compared with the bulk chemical analyses. In the bottom graph in Figure 2 the comparison of total iron and copper content, calculated from the mineralogical composition, with that measured by x-ray fluorescence (XRF) is shown.

We see a very good agreement between XRD and XRF results. Even very small amounts of copper minerals can be monitored, and the respective Cu-content can be accurately predicted using 10 minutes measurement of a complex copper ore on a tabletop XRD instrument.

Added-value of XRD monitoring throughout the whole process

In the above section we analyzed mineralogy of 100 drill-core samples of copper ore and identified points of attention for the next processing step. The efficiency of the following steps can also be monitored using X-ray diffraction. In addition to the classical quantitative phase analysis, XRD offers several other tools to simplify day-to-day process monitoring. In our blogs on iron ore and heavy mineral sand processing (published shortly) we will give an example of cluster analyses [2,3] being used for quick and easy monitoring of ore grade definition and mineral separation efficiency. A similar approach can be used to monitor the separation and concentration efficiency at copper processing plant. Mineralogy of tails and waste products can also be controlled using XRD.

On-line control of clay content in copper ore

In the introduction blog we discussed the advantages of near-infrared spectroscopy (NIR) for online mineralogy monitoring. Not all minerals, commonly present in copper ore, are visible for NIR spectroscopy.  however, talc and clay minerals are, and therefore can be easily identified and quantified using on-line NIR over-the-belt analyzer or laboratory NIR spectrometer. Real-time monitoring of clay and talc content in the run-of-mine will improve the efficiency of flotation and leaching processes, prevent possible equipment blockage and other common issues, associated with the presence of large quantities of soft minerals in the ore.

NIR spectrometers can also be part of completely automated laboratories, operate standalone in a laboratory, or assist mine geologists as handheld devices in the field.

To summarize, copper ore mineralogy is very complex and has a major impact on the beneficiation process. To run it efficiently, not only the copper oxide/sulphide ratio should be considered, the adequate and timely control over mineral impurities should part of the process monitoring. A moderate investment in fast, accurate, and reliable mineralogical probs upstream helps to save millions of dollars downstream.

Written By: Dr. Olga Narygina – Malvern Panalytical (www.malvernpanalytical.com)

Join Live Webinar On Practical Tips for Efficient Grinding in Laboratory Ball Mills

 

Our partner RETSCH will be conducting a live webinar on “Practical Tips for Efficient Grinding in Laboratory Ball Mills” provides valuable information which will help to facilitate your daily work and discusses new possibilities for ball milling.

Webinar will include following topics:

  • Ball mills: technology and models
  • Grinding tools: selection of the material, number and size of grinding balls
  • Tips & Tricks for the milling process

At the end of the webinar, you will have the chance to download a package containing all relevant information.

Webinar Information

For your convinience the webinar will be held on the following dates:

  • Date 1: 8th June 2020 – Monday
  • Date 2: 9th June 2020 – Tuesday

At each date there will be two sessions to cover for your convinience

  • Time ( Option 1): 10:00 AM – 11:00 PM (Arabian Standard Time)
  • Time ( Option 2): 17:00 PM – 18:00 PM (Arabian Standard Time)
  • Language: English
  • Speaker:
    Dr. Tanja Butt, Product Manager RETSCH GmbH
    Dr. Gerhard Beckers, Application Specialist RETSCH GmbH
CLICK HERE TO REGISTER

Posted By: Retsch (www.retsch.com)

Focus on Pharma – XRD Masterclass 2: In situ Stability Studies

Stability studies often precede patient studies and registration stability studies, as advised by the International Conference on Harmonisation (ICH) guideline Q1A (R2). Such testing is mandatory to regulatory filing and approval of the drug products for the market.

As per Q1A(R2) ICH guidance on Stability testing of new drug substances and products, “stability studies should include testing of those attributes of the drug substance that are susceptible to change during storage and are likely to influence quality, safety, and/or efficacy. The testing should cover, as appropriate, the physical, chemical, biological, and microbiological attributes. Validated stability-indicating analytical procedures should be applied.” The same principle should be applied to drug products.

The guidance specifies the storage conditions for long term, intermediate and accelerated studies and the frequency with which these studies should be performed. If a significant change is observed, stability studies should be carried out more frequently.

Even if the stability characteristics of the API/drug product are fully understood, stability behavior should be continuously monitored and verified.

To gain a better understanding of stability performance and to avoid unnecessary studies, in situ X-ray powder diffraction experiments as a function of temperature and relative humidity can be implemented.

These provide a direct means of characterizing the polymorph stability of a pharmaceutical material at high temperature and the occurrence of hydration/dehydration processes. Within such an approach, the experimental conditions required for long term, immediate or accelerated stability studies (as defined per ICH Q1A(R2)) can be easily achieved. More extreme conditions can be established in order to speed up stability investigations. Such non-ambient X-ray diffraction testing can be performed at any stage of the drug development process.

In this webinar we will give an overview of the accessories that are required for in situ stability testing, discuss prerequisites for such studies and provide a few examples of successfully performed investigations.

Summary

Date:
May 07 2020 – May 07 2020
Time:
18:30 – 19:30 Arabian Standard Time
Event type:
Webinar – Live
Language:
English
Industry:
Pharmaceuticals

Speakers

Natalia Dadivanyan Ph.D. – Field Application Specialist – Pharma Sector

More information

  • Who should attend?

– Anyone involved in stability studies
– Anyone who is developing pharmaceutical formulations
– Anyone engaged in chemical development or support of scale up activities
– Anyone engaged in polymorph screening activities as part of lead optimization activities

  • What will you learn?

– You will learn about in situ X-ray diffraction testing and respective experimental set-up
– You will learn how these studies can assist in making pharmaceutical development more efficient

Posted by: Malvern Panalytical (www.malvern panalytical.com)

The Analytical Chain: Value of Smart and Easy Sample Preparation for Elemental Monitoring in Mining and Ore Processing

The concept of the analytical chain includes all the steps necessary to take a sample from its raw state to analytical data. As with all chains, this process is only as strong as its weakest link and sample preparation is of vital importance for the quality of data needed for elemental monitoring in the mining industry. For example, ensuring that impurity levels of mineral concentrates fulfill product specifications and quality standards thereby avoiding penalties or reprocessing requires full control of the sample preparation process for XRF analysis.

Based on customer feedback requests, this webinar will show you how a complete solution from Malvern Panalytical can simplify and speed up the necessary sample preparation steps and enhance the quality of the results. It is a fact that preparing mineral samples as fused beads enhances the accuracy and precision of XRF analytical results, and for this reason this webinar will focus on the technique. Root causes of problems or errors commonly encountered in the fusion sample preparation technique and how to avoid them will also be discussed. Finally, we will illustrate how Malvern Panalytical covers other links in the chain, such as integrated sample tracking capabilities, quality monitoring, simplified fusion methods, usage of high-quality chemicals, automated weighing and certified calibration standards.

Summary

Date:
May 05 2020 – May 05 2020
Time:
18:30 – 17:30
Event type:
Webinar – Live
Language:
English
Industry:
Mining

Speakers

Chantal Audet – Product Manager Sample Preparation & Calibration

More information

  • Who should attend?

Professionals working for mining, minerals and metals companies, researchers and technical associations searching for knowledge and new sample preparation solutions for X-ray fluorescence analysis.

  •  What will you learn?

You will learn the latest with regard to sample preparation techniques, from an expert with over 16 years of experience.

Posted by: Malvern Panalytical (www.malvernpanalytical.com)