Borate fusion is known to be one of the best sample preparations for analysis with XRF. However, it can be a complex preparation to work with and different parameters have an impact on the analytical results. This presentation will focus on understanding these parameters, before and during the fusion, to help the users achieve a stable method that gives good results.

This talk presents a comprehensive approach to sample preparation for a variety of samples, prior to elemental analysis.  The methods involve the use of microwave digestion and auto-dilution techniques to achieve reliable and accurate results. Prior to analysis, samples are reduced using Retsch Jaw crushers, ensuring efficient and consistent sample preparation. Samples can then be subsampled and digested via our Milestone microwave systems.  Once digested, automated dilution provides accurate and precise results for a range of sample matrices, including environmental and geological samples. By utilizing tools such as Teledyne Cetac’s Simprep, you can reduce human error and increase the efficiency of the analysis sequence.

This process provides a reliable and efficient solutions for sample preparation to streamline your analysis process for metals analysis, providing accurate and reliable results.

Iodine is a micronutrient essential for human health. Dietary supplementation, by means of iodised salt, is commonly used to address global prevalence of iodine deficiency (ID) disorders. However, efforts to reduce salt consumption to alleviate other chronic health diseases such as high blood pressure and other heart complications could impair the effectiveness of such preventive measures. On the other hand, biofortification is an alternative strategy to address ID, as iodine stored in food is readily bioavailable. Therefore, it is important to understand the iodine-soil-crop dynamics, which demands the need for efficient and sensitive analytical methods for the determination of iodine in soil. 

Available methods for the determination of iodine in soil are primarily based on reaction catalysis, spectrophotometry, neutron activation analysis, pyrohydrolysis-ICPMS, etc. which are time consuming, labour intensive, prone to interferences, and of poor sensitivity. Based on microwave digestion with Tetra Methyl Ammonium Hydroxide (TMAH), we have developed a rapid extraction method, followed by sensitive measurement with ICPMS following direct dilution of the digestate. Method was validated using certified soil reference material (NIST SRM2709) with a limit of detection 0.016 ppm (16 ppb) in the dry solid.

ISO/IEC 17025:2017 is the international standard for testing and calibration laboratories, and it provides guidelines for the management of laboratory activities. Accreditation to this standard indicates that a laboratory is competent and operates under a well-defined management system, ensuring the reliability and accuracy of its results. Mineral testing labs can benefit from accreditation to this standard in several ways, including mitigating risks associated with their testing activities.

Here are some ways in which accreditation to ISO/IEC 17025:2017 can help mineral testing labs mitigate risks:

Ensuring accuracy and reliability of test results: ISO/IEC 17025:2017 requires laboratories to have a quality management system that ensures the accuracy and reliability of test results. This includes ensuring that the test methods used are valid, that equipment is calibrated and maintained, that staff are trained and competent, and that records are maintained.

Reducing the risk of errors and mistakes: Accreditation to ISO/IEC 17025:2017 requires laboratories to have procedures in place to identify and manage risks associated with their testing activities. This includes identifying potential sources of errors or mistakes and taking steps to reduce or eliminate them.

Improving customer confidence: Accreditation to ISO/IEC 17025:2017 is a globally recognized symbol of competence and reliability. Customers can be confident that the test results provided by an accredited laboratory are accurate and reliable, which can help to build trust and confidence in the laboratory's services.

Complying with regulatory requirements: Accreditation to ISO/IEC 17025:2017 can help mineral testing labs demonstrate compliance with regulatory requirements. This can be particularly important in industries such as mining, where accurate testing of mineral samples is essential for complying with safety and environmental regulations.

Facilitating international trade: Accreditation to ISO/IEC 17025:2017 can facilitate international trade by providing a recognized standard for laboratory competence. This can help to remove barriers to trade and reduce the need for additional testing or certification.

Control charting is an essential tool for quality management in assay laboratories. Control charting techniques in current use are geared for single analyte tests, when applied to multianalyte tests such as ICP-OES, XRF the Type I inference error increases as the number of analytes increases, resulting in very high numbers of QC failures. Current practice is to chart only a few selected “important” analytes for control charting, resulting in minimal, if any, QC for most analytes tested.

The Euclidian Distance approach for charting multianalyte tests has been shown to have the same Type I inference error regardless of the number of analytes tested. In this presentation the Type II inference error properties of the Euclidian Distance approach is shown. The experimental situation examined is 50 analytes for a control sample on 500 test runs, a total of 25,000 test results. The data matrix was populated with Gaussian distributed random numbers. Bias was added from 0.1 z units to 5.0 z units to selected analytes ranging from all 50 analytes biased to only one analyte biased.

This approach simulates commonly encountered situations such as dilution error, calibration error, contamination, selective analyte extraction errors during sample digestion / dissolution.

In this presentation, I will make the case for the need to better include Women and Girls in STEM, especially in domains related to sustainability.¹ There are many reasons why women deserve to have access to STEM-related jobs. For instance, how gender inequity leads to economic disparity and explains in part the gender salary gap. On the other hand, I will also make the argument including women in these positions is central to developing better research, because of the blind spot that can emerge from a lack of diversity when addressing sustainability questions. I will finish by presenting some solutions to empower more women in the field. I will also use this time to introduce a couple of vignettes on the research effort of my group, including in waste valorization of biomass with mechanochemistry and our efforts to integrate toxicology in nanodesign.

1. Cannon, A. S., Carrier, D. J., Engelberth, A. S., Garcia, J. M., Heath, E., Kuok Hii, K., Kerton, F. M., Makhubela, B., Moores, A., Rossi, L. M., Vidal, J. L., Voutchkova-Kostal, A., & Wilson, K. (2022). Women in Green Chemistry and Engineering: Agents of Change Toward the Achievement of a Sustainable Future. ACS Sustainable Chemistry and Engineering, 10(9), 2859–2862.

In January 2023 ColdBlock Technologies published its new Strong Acid Digestion method. This method was developed to provide laboratories with a faster, safer alternative to traditional 4-acid digestion methods, while still providing the same accuracy and repeatability across sample types and matrices.

We will be presenting this new method and sharing results from our in-house testing of a 10 different CRM's. With ColdBlock’s new Strong Acid Digestion method, digestion cycle time is reduced from >1.5hrs to just 30 minutes. Of note, this is accomplished without the use of dangerous perchloric acid.

This new method utilizes ColdBlock’s new Pro Series CBM digester – a 16-sample digester that can be scaled up into a 32/48/64-sample platform. It also utilizes ColdBlock’s new test tube liners that permit the use of hydrofluoric acid.

Results demonstrate high recoveries relative to stated CRM expected values, and well within acceptable ranges for each CRM type. The results show potential for use with base metal, lithium, and uranium samples and wide range of matrices.

This new method is currently being rolled out for use at several commercial laboratories.

Identifying deposits of rare earth elements (REE) that are economically viable to extract has become increasingly important. REEs have some desirable magnetic, luminescent and electrochemical properties that are desirable in high-tech industries from TV and computer screens to aircraft engines and high-power magnets. These properties are dependent on purity of the element. However, the same properties that make them desirable to industry can also make them difficult quantify analytically due to their ability to form oxides and double charges, causing interferences on other REE and other impurities such as arsenic and selenium respectively. The NexION 5000 multi-quadruple ICP-MS is perfectly suited to the analysis of such difficult elements due the unique powered interface and universal cell technology, making it ideal for reaction mode analysis necessary for REE analysis. Here we describe advanced ICP-MS techniques for accurately quantifying REE elements and removing the interferences caused by utilizing multi-quad ICP-MS and advanced reaction cell technology, and describe how these are utilized in applications.

The mining of Rare Earth Elements (REE) is an important industry and the high value of these REEs makes it even feasible to mine for trace values. Due to their genesis, REEs are usually find all together in specific geological formations like carbonatite, clays, sediments and even Coals.

Determining if a location is worth for mining extraction is important due to financial but also ecological considerations. ED-XRF can be a quick and accurate method to measure indicator elements like Yttrium to determine the total REE concentration (TREE) in a sample. Unlike low power ED-XRF system, a benchtop system can easily determine ppm levels of Y, and at the same time does not require and extensive set up like a floor standing WD-XRF model.

How does new technology and innovation reach Canada and the savvy mineral analyst?

The mining cycle (with its massive cash flow droughts) and (ever crushing industry) consolidation are 2 critical barriers to entry.

Four technical marketing case studies are discussed with key learning points presented.

Proper maintenance scheduling for critical engine and field machines should be considered to minimize cost, extend lifetime, and maximize performance. A regular maintenance schedule can be hard to implement based on the amount of service hours required in remote locations.

Radom MICAP-OES 1000 is a microwave inductively coupled atmospheric plasma which operates on industrial grade (99.9%) nitrogen and 1000 W power.  The technology to create the stable plasma is called Cerawave™ which replaces the traditional electric water-cooled coil coupled to an RF generator. The result is no argon and no chiller required. The benefits are a light-weight, compact instrument with the lowest carbon footprint and lowest cost per sample. This design can perform critical analyses for elements which indicate engine performance.

Lithium ion batteries are state-of–art power sources and widely used in variety of applications such as portable electronic devices, electric vehicles, and bikes. Precise and accurate determination of major elemental content is very important for performance and quality control of these Li-Ion batteries. This presentation will discuss the analytical requirements and challenges of cathode materials analysis, common methods, continuous real-time simultaneous internal standardization (CRTSIS approach), and analysis results.

Neutron Activation Analysis is a referee technique for trace elements analysis which gives a total elemental analysis based on the nuclear properties of the elements in a sample independent of their chemical states. As such, NAA is a referee technique for accuracy, and especially important for the certification of reference materials. Nuclear proliferation concerns have led to the closure of most nuclear reactors historically used for NAA, with resulting decline in its awareness and use. Use of Neutron Activation Analysis (NAA) for certification of reference materials has declined from > 50% of all results used for certifications in the 1970’s to < 20% in the last decade.¹ Examples are discussed of bias in reference materials certified values from over-reliance on popular methods of analysis based on chemical vs. nuclear properties.

1. The role of NAA in securing the accuracy of analytical results in inorganic trace analysis. R.S. Dybczyński, Institute of Nuclear Chemistry and Technology, Warsaw, Poland, presented at 2^nd International Conference on Radioanalytical and Nuclear Chemistry, Budapest, May 2019.

In 2012, Agilent forever changed ICPMS with the introduction of the first ever commercial ICP-MS/MS platform, the Agilent 8800. The unique mass-analyser consisted of two full-sized quadrupoles, one in front and one behind the octupole reaction/collision cell. The performance of the MS/MS mass analyzer was driven by the patented 5-stage vacuum system, which houses each quadrupole in a dedicated high vacuum region to provide low abundance sensitivity (<1x10^-10), low backgrounds (<0.2cps), mass resolution of <1u (both quadrupoles) and thus allowed for a full exploitation of reaction modes in MS-MS mode. This unique design afforded a unique instrument platform that combined the ease-of-use and scan speeds of quadrupole based ICPMS with interference handling capabilities outperforming high resolution sector-field ICPMS systems, providing unmatched ICPMS performance. The ICP-MS/MS technology was quickly adopted into laboratories across the globe, resulting in a strongly growing number of research publications and new ICPMS applications. Taking the lessons learned from the 1^st ever ICP-MS/MS, Agilent introduced a new, more powerful, generation of ICP-MS/MS systems, the Agilent 8900, in 2016. Join us for a 10^th anniversary celebration of ground-breaking ICP-MS/MS technology and a brief history of Agilent’s ICP-MS/MS technology.

As a key raw material in the production of high density and rechargeable batteries, Lithium has been heavily sought after in recent years. The two major sources for lithium are 1) lithium brines, which includes salt-lake brine, seawater, geothermal brine etc., and 2) lithium bearing minerals, most commonly spodumene, petalite and lepidolite from pegmatite deposits. Both sources have respective advantages when it comes to mining, with Lithium brines accounting for over 70% of the total lithium reserve, while hard rock pegmatite mines having much higher grade of LiO2 at around 1~4%. Meanwhile, exploration and extraction for both types of resources face technical challenges that require information on the chemical compositions of the brines/ores, demanding effective analytical solutions for these sample types. However, lithium brines and mineral fusion digests have heavy and complex matrices with high total dissolved solids (TDS) which promote deposition and clogging in the sample introduction systems while introducing spectral and non-spectral interferences. These samples require robust atomic spectroscopy instrumentation and appropriate methods for routine analysis on an operational basis. Agilent Technologies have developed several methods for fast and accurate analyses of lithium and other major and minor elements in lithium brines and spodumene digests, using the Agilent 5800 VDV ICP-OES and Agilent 240 FS AAS. These methods focus on sample preparation, speed, detection limit, carryover management as well as ease of use, providing a complete suite of solutions for the lithium mining industry. 

Metal leachate and acid rock drainage (ML/ARD) are common issues at mine sites and at other industrial sites, such as metal plating operations. When such sites are situated in the vicinity of surface water bodies, or the groundwater plumes extend to property boundaries, this can pose environmental risks to aquatic life and/or can result in significant regulatory or legal liability. The long-term presence of ML/ARD at such sites requires an equally long-term solution.

Recent developments have allowed the design and long‑term performance of passive treatment barriers for groundwater plumes containing heavy metals to be assessed.

This talk will present:

• ML/ARD related contaminants of concern that can be treated via these passive treatment barriers;
• Recent advances in barrier design, installation and validation techniques that make the performance of these barriers more certain and better than ever; and
• Case studies on an:
  • Arsenic plume site; and
  • Antimony, cadmium and zinc plume site

The case studies will include a presentation of site characteristics, remedial approach and post-remediation groundwater monitoring data demonstrating that remedial targets were achieved and maintained.