X'Press 3/2016

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X'Press 3/2016

Our periodical X'Press, the customers' voice, contains news items, reports of trips and conferences and customer stories.

'How to develop?' is the central theme of the third and last issue of X’Press in 2016. Many of our customers, be it in industry or in research institutions, are involved in developments of new processes or products. In this phase they often approach our specialists for advice on how to get quick feedback on intermediates, easy verification of materials or a quality check of end products.

20 years and still powering on

When performing high-precision X-ray fluorescence (XRF) analysis, people tend to equip their laboratory with highquality detectors or robust software. However, the core element of X-ray analysis – a reliable X-ray tube – is often taken for granted. A high-power XRF tube is a high-vacuum product operating under the most demanding conditions. It must maintain its vacuum for 10 years and more, be stable at voltages up to 90 kV, handle 3-4 kW of power and cope with anode and cathode temperatures above 800 ºC. Material purity, geometric accuracy and high-vacuum joining technology determine a tube’s quality and reliability.

Yara’s mine in Siilinjärvi (Finland) is the only apatite mine in Western Europe and ca. 3 km long, 1 km wide and with a deepest point of 240 m.

In the heart of Sydney’s University of New South Wales, the team of the X-ray Fluorescence Laboratory, comprising Sarah Kelloway, XRF Technical Officer and led by Senior Technical Officer, Irene Wainwright, conducts materials analysis on minerals, cements, glass and more. They use PANalytical’s PW2400 XRF spectrometer equipped with a Rh X-ray tube as well as an Axios Advanced XRF spectrometer with the SST R-mAX tube. PANalytical’s Customer Support team was recently on-site tocertify a clean bill of health for UNSW’s instruments and tubes.

The PW2400's X-ray tube celebrates an unprecedented 20-year tube life which breaks the record of a 13-year old PANalytical tube also found in Australia.

PANalytical is the only major analytical X-ray instrumentation supplier with its own X-ray tube factory. Located in Eindhoven, the Netherlands, the tube factory has a history of more than 40 years. It offers a wide range of X-ray tubes for X-ray fluorescence and X-ray diffraction analysis in addition to other industrial applications like inspection, non-destructive testing (NDT) and gauging.

The factory is able to customize X-ray tubes according to specific demands, for instance, tailoring to many anode types from Sc, Ti, Cr, Mn, Fe, Co, Cu, Mo, Rh, Ag, Gd, W to Au and more.

True to PANalytical’s value of restless innovation, the company continues to improve tube functionality (power, intensity, soft X-ray output, spectral purity), stability (shortand long-term drift, flash frequency), reliability and lifetime. Development of new material combinations and design geometries has further optimized important properties such as thermal expansion, thermal conductivity, vapor pressure and adhesion increasing both cathode and anode lifetimes to more than 10 years.

Physical ageing and cathode evaporation have been reduced to the point that the initial X-ray output remains constant during the entire tube lifetime achieving optimal reproducibility, minimum (re)calibration and maximum uptime. This has been realized with the patented ZETA technology in all SST-mAX tubes and new robust anode technology in all SST R-mAX tubes.

“By having X-ray tube development and manufacturing under our control, we ensure continuous innovation and performance improvement of our tubes at competitive prices for our end users” says Maarten van Andel, director of PANalytical’s X-ray tube factory. “PANalytical’s newest Zetium XRF spectrometer, launched in 2015, features the revolutionary SST R-mAX tube whose performance remains consistent and drift-free even after 12,000 hours and beyond.”

Gjalt Kuiperes, regional director for PANalytical's Asia Pacific region, adds “This is an important feature for our end users – to be able to trust in our instruments in delivering reliable results throughout the tube’s entire lifetime”.

We are very happy with the tube’s performance especially since we’re still getting consistent good results after 20 years of tube life Irene Wainwright, Senior Technical Officer, University of New South Wales

The University of New South Wales

The University of New South Wales (Australia) is a public research university located in a suburb of Sydney.

Established in 1949, it is regarded as one of the country’s leading universities. Its nine faculties provide an inspiring environment for research and education for more than 50,000 students.

Redefining benchtop XRD

PANalytical’s new Aeris X-ray diffractometer

During the last months, PANalytical continued to spread rumors about a new product to be launched. The customers’ curiosity was finally satisfied in November with the introduction of Aeris, the new benchtop X-ray powder diffractometer. The editors of X’Press asked two of the major players in the development of the new system about the ideas that have driven the development of Aeris and their experiences during this process.

Jan van Rijn, general manager X-ray systems and Harald van Weeren, product manager X-ray difraction about ‘How to develop’

Harald, can you explain why PANalytical has chosen to develop a benchtop XRD system while there are already a few of those on the market?
It is simple; the demand for compact or benchtop analytical systems in general is increasing. We see this with our own X-ray fluorescence instruments, but also outside of PANalytical’s market there is an increasing demand e.g. for compact electron microscopes. It is in fact the need for everyday and simple routine analysis that is increasing. Although we always deliver best-inclass performance, this has not been the main focus of the development of Aeris. Instead we focused on simple routine analysis – we wanted to create a benchtop XRD instrument that is extremely easy to use. Insert your sample, press a button and get the results. Additionally, Aeris is the first benchtop XRD that can be automated with a robot or a belt, which facilitates routine analysis even more.

Could you elaborate on the ease of use?
I would rather call this term intuitiveness. Apps are a good example of this intuitiveness. You see kids picking up an iPad and just using it without any preceding instructions. Current X-ray diffraction instruments can, especially for new users, be rather daunting with their many different optical components and the wealth of options in the software. That’s something we wanted to overcome with Aeris. Its ease of use can be traced back to both the hardware and software design. For basic operation, you just put your sample on the external sample platform or sample changer without worrying to have to enter the optical path. For the software design we have worked closely together with an interaction designer. Together with a broad set of people, from XRD specialists to those completely new to analytical instrumentation, we have created a user interface for Aeris that is truly intuitive and focused on learning while doing.

Jan, you are responsible for the technical development process. Could you tell our readers how such a process is set up?
The development of such an instrument always involves a large number of people from various departments who need to act as one team. In order to achieve this we made use of LEAN techniques, which had been successfully rolled out in our R&D department during the last year. We also created a review group of enthusiastic pragmatic users whose input was fed back to our architects to generate a system design in which all stakeholders from users to service engineers, supply chain and manufacturing were heavily involved. Personally I see the alignment of software and system development as the highlight of the innovation. It resulted in early-stage First-Time- Right design concepts, which could be validated quickly in real applications.

I see the alignment of software and system development as the highlight of the innovation. Jan van Rijn, general manager X-ray systems at PANalytical

Harald, Aeris is an interesting product name. Can you tell us how this was ‘invented’?
Aeris is Latin for air or atmosphere. Both are pretty essential for life on earth and our benchtop XRD instrument is the essential tool for materials research. Additionally it is an essential tool to make the production of metals or cement as well as mining of minerals more efficient and environmentally friendly.

Not all of our readers might be familiar with X-ray diffraction. Could you explain the benefits of this technique?
X-ray diffraction gives information about the three-dimensional arrangement of atoms in crystalline materials. It is that crystal structure that defines the physical properties of a material. For example graphite and diamond are both made up of carbon atoms, yet their physical properties are completely different because of their different crystal structure. Graphite in a pencil easily leaves material on a piece of paper when you write, but diamond is extremely hard. Similar examples can be found in pharmaceuticals, building materials and in the metals industry. XRD easily identifies the different crystalline phases and gives precise information about the analyzed compound.

Jan, even though Aeris is very easy to use, there might be customers who need a bit of extra help with their application. Can PANalytical provide assistance?
Users will experience a clever user interface and an easy-to-use system. Besides that, every user, for every system, can rely on our comprehensive support network. The support we can deliver varies from training to addressing new applications with Aeris. In particular we see standardization in customer (multi-site) PC/QC (process control/quality control) as an increasing trend in which we can develop multi-site SOP’s (standard operating procedure) and operator training in which systems perform according to strict internal performance requirements.

A ‘Christmas tree’ for the Imperial College London

The Department of Materials at Imperial College London (UK) is the oldest department of its kind in the United Kingdom and is currently ranked 3rd in the world for material science (QS World University Rankings 2016). Over the years it has earned a reputation for excellence in teaching at all levels to both undergraduates and postgraduates alike. The Department’s six research themes cover biomaterials and tissue engineering, ceramics and glasses, alloys and functional materials, nanotechnology and nanoscale characterization and the theory and simulation of materials with activities in all themes applied in a wide range of commercial sectors.

To be able to deal with the challenges of such a wide variety of research themes, the Department of Materials decided in December 2015 to purchase an Empyrean X-ray diffractometer from PANalytical. Since its installation, the instrument is being used extensively within a multi-user environment made up of a large number of research staff and students. They primarily investigate thin films and particularly epitaxial layers by high-resolution measurements, rocking curve, X-ray reflectivity (XRR), reciprocal space maps (RSM), texture, residual stress, in-plane, glancing incidence measurements (GI-XRD and GI-SAXS), small- and wide-angle scattering (SAXS/WAXS) as well as nonambient in situ studies.

Left to right: Terry Soteriou (PANalytical), Richard Sweeney (Imperial College London) & Dr. Paul O’Meara (PANalytical) by the Empyrean conducting a thin film experiment

To satisfy these numerous requirements the Empyrean has what is known as a ‘Christmas tree’, configuration including three- and five-position programmable cradles, various monochromators, the Bragg-BrentanoHD optical module for high-speed generation of high-quality data, the ScatterX78 SAXS/WAXS attachment, and the Domed Hot Stage DHS1100 for non-ambient experiments. PANalytical’s PIXcel3D detector is taking care of recording the data, which can then be processed by one of the eight different software applications purchased with the instrument.

Mr. Richard Sweeney, Senior Research Officer at the Department of Materials X-ray Diffraction lab was impressed by the outstanding professionalism and thoroughness of the installation team. He stated: “The quality of the data produced by PANalytical from the Empyrean at the tender evaluation stage was very impressive and I’m happy to say that the Empyrean has certainly lived up to expectations. Switching between modes is straightforward and the ultra-fast reciprocal space mapping is truly remarkable, enabling us to quickly select only the best films for more detailed measurements”.

Mr. Richard Sweeney is particularly happy with the ScatterX78 attachment, which enables them to “easily obtain good-quality SAXS and WAXS data to characterize a range of nanomaterials without the need for a separate SAXS instrument”.

I’m happy to say that the Empyrean has certainly lived up to expectations. Mr. Richard Sweeney, Senior Research Officer at the Department of Materials X-ray Diffraction

Mars rover operational strategies testing at terrestrial analog sites

An extraterrestrial application for ASD’s field-portable VNIR spectrometry

Returned Mars rover data can help us to attempt to reconstruct the geologic history of a region and identify biosignatures reflecting past life. The approaches used to robotically explore planetary field sites are an outgrowth of geologic fieldwork on Earth. A NASA-sponsored project seeks to test modes of rover operations and determine which mode provides maximum science return from a time- and resource-limited robotic mission on Mars. Real rovers are not used given the cost and technical /logistical constraints and because the tests are solely to test rover science methodologies and protocols; terrestrial analog rover simulations are used instead, and as a tool in refining Mars rover operational strategies.

Sarah Black, a University of Colorado PhD student in the Department of Geological Sciences participated in Mars rover analog field tests in remote Utah (US). In these tests, Sarah acted as a ‘human rover’ using an ASD TerraSpec Halo Mineral Identifier to simulate functionally-equivalent instruments available to the current rovers on Mars.

‘Human rovers’ were commanded by a separate science backroom (Mission Control). Mission Control told the rovers where to go and what data sets to collect at each stop. The data was then ‘downlinked’ to Mission Control, who used that data to plan the next targets of interest, and which data to acquire at those sites.

Visible near-infrared (VNIR) spectroscopy provides a wealth of compositional information, and is a valuable tool in planetary exploration. The portable spectrometer allowed for rapid data acquisition of in situ outcrops, similar to those data gathered Mars rovers, and allowed the instrument operator to rapidly traverse the field site, maximizing the number of data points gathered for the science teams.

The use of field-portable VNIR as an analog for rover instrumentation was sufficient for science team operations; the teams were able to efficiently conduct their site investigation and analysis of operational methods using terrestrial analog instrumentation. The result of this study will feed directly into the Mars rover Curiosity’s operational planning to maximize the science return from Mars.

Collecting spectra directly from a sectioned femoral diaphysis. Diffusion of light through the cortex is clearly visible. The PMI for this sample was short (<6 months).

Figure A. A ChemCam Remote Micro Imager (RMI) scene (CR0_439663426PRC_F0240312CCAM02475L1; NASA/JPL-Caltech/LANL) superimposed on a MastCam image (0475MR0018870000302888E02_DXXX; NASA/JPL-Caltech/MSSS) of the base of Mount Sharp, Gale Crater – acquired on sol 475 of the Curiosity Rover mission. VNIR reflectance of the area within the circle was sampled via ChemCam’s passive function.

Figure B. Sampling site with the field-portable VNIR spectrometer. Sampled area is within the circle. Inset: The ASD TerraSpec® Halo fieldportable spectrometer in action.

Reference: Black, S.R., Yingst, R.A., Hynek, B.M. (2016). Spectroscopy, 31, 29-35

New developments in the fight against Zika and Dengue

Zika and Dengue are viral diseases that infect well over 400 million people each year. In humans, infection by the Dengue virus results in fevers, headaches, rashes and severe joint and muscle pains. Infection by the Zika virus typically causes a mild illness known as Zika fever. More significantly, prenatal Zika infection has been associated with microcephaly and other serious birth defects. Both viruses are transmitted by mosquitoes of the Aedes species.

Numerous studies have shown that infecting these mosquitoes with a targeted strain of the Wolbachia bacterium greatly reduces the likelihood that the mosquitoes carry the Zika or Dengue virus. Wolbachia-infected mosquitoes spread rapidly and can infect over 80 percent of the local mosquito population.

In order to judge the effectiveness of a release program of infected mosquitoes, wild mosquitoes must be trapped and screened for the presence of the Wolbachia bacterium. Dr. Maggy Sikulu-Lord, from QIMR Berghofer Medical Research Institute in Brisbane, Australia, and colleagues have developed a method for rapidly screening Wolbachia infection in mosquitoes based on near-infrared (NIR) spectrometry. Using ASD’s field portable LabSpec NIR analyzer, the researchers have been able to distinguish between infected and uninfected mosquitoes with 85-95% accuracy, enabling them to rapidly determine the effectiveness of the program.

Dr. Sikulu-Lord states: “A study nominated for an award by Combating Zika and Future threats, funded by USAID, and led by Dr. Sikulu from the University of Queensland, will investigate the ability of NIR as a rapid technique to detect Zika and Dengue infections in the principal mosquito vector Ae. aegypti in Rio de Janeiro, Brazil. We will use a Labspec 5000 NIR instrument from ASD PANalytical to develop models that can be used to rapidly detect Zika and Dengue transmission hotspots in Brazil. This non-destructive technique is faster than the standard polymerase chain reaction diagnostic techniques. It requires little sample processing and does not consume any reagents.”

Brent Olsen, VP & GM of ASD is pleased that “our solutions have the ability to help make a difference in the fight against Zika and Dengue. This is well in line with PANalytical’s mission to create a better world by helping people to analyze materials that matter to them and the environment.”