TEXRAY LAB » Datascan

Big changes in the Jade ecosystem from MDI

Posted by: Ken Stauver In: Uncategorized 18 Feb 2019 0 comments Tags: crystallography, Datascan, Diffraction, Diffractometer, Jade, Jade 2010, Jade 9.5, Materials Data Inc, MDI, powder XRD, PXRD, XRD

MDI Jade has been our goto analysis suite for powder XRD data for decades now. Powerful, versatile, and well supported, it’s earned a following second to none in the industry. What began as a simple suite of MS-DOS-based programs in the early 1990s has blossomed into a full-featured toolset for just about any kind of powder XRD analysis one could need. As computer hardware and software platforms evolved, Jade grew right alongside them with more powerful features, faster processing, and even greater flexibility.

Several years ago it became apparent that the core programming of Jade was going to become a limiting factor in its development. Enter Jade 2010. Built from scratch on next-generation architecture, Jade 2010 freed up the developers at MDI to implement many of the changes they’d been wanting to add for several years. The result was a beautiful new interface with streamlined and reorganized menus that greatly improved the user experience. The new structure allowed for much more integration between features that had once been modular, making them easier to use as well as more powerful. The original Jade suite (now on version 9.8) became Jade Classic and it became clear that there was a sunset coming for the venerable program. The only complaint we ever received about Jade 2010 was that it was only available as an annually-licensed product. Each year the users would need to renew their subscription to continue using the software. This gave me pause just as it did many of our clients, but the rapid pace of development almost necessitated this as new changes and updates were taking place monthly rather than yearly as they had in the past.

Fast forward a few years and we’ve had another big change. Jade Classic (9.8) has been discontinued and Jade 2010 has become Jade Pro. It’s still all-inclusive with all the advanced capabilities available on every license. It’s also still an annually licensed program. Development will continue free from the limitations of the old core programming and the distraction of maintaining two completely separate products.

This alone wouldn’t be such big news, but there is a new option that we’ve been waiting for years to see. Jade “Standard”. We now have four additional products available to users with more limited needs and budgets.

Jade Standard level 1 includes all the basic pattern analysis and manipulation tools that users would need for many of the more common projects as well as some of the more advanced features that were only offered on the premium Jade+ (plus) program before.

Jade Standard level 2 includes all the level 1 functionality, plus Search/Match (2a) or Whole Pattern Fitting/Rietveld (2b).

Jade Standard level 3 includes both Search/Match and Whole Pattern Fitting.

All Jade Standard products are perpetually licensed (One-time purchase, lifetime license).

Several of the ancillary tools offered by MDI are still available as always including Ruby, ClaySim, and RIQAS.

We’ve been waiting a very long time to be able to make this announcement and I must say that the way this has been implemented couldn’t be better for ourselves or our clients.

Please contact KS Analytical Systems for more information and upgrade pricing.

Flexibility, versatility and adaptability

Posted by: Ken Stauver In: Uncategorized 14 Oct 2013 0 comments Tags: crystallography, D500, D5000, D5005, Datascan, Diffraction, Diffractometer, Energy-dispersive detector, Jade, Jade 9.5, KS Analytical, Materials Data Inc, MDI, PXRD, Siemens, Thin-film, X-ray, XRD, XRD data collection, XRR

A large part of our business at KS Analytical Systems is refurbishing and reselling WDXRF and XRD instrumentation. We specialize in Siemens and Bruker models because, and I can’t stress this enough, they last. Siemens was 20 years ahead of their time with features like full computer automation, interlocked radiation housings (not just an enclosed beam path) and independent axis control coming standard on most systems. The D500 may well be the most reliable powder diffractometer ever built and for most of our history, it’s outsold all other models of XRD and XRF combined. Most users are simply performing basic powder scans with many running the optional 40-position sample changer, but I always get excited when I find someone pushing the limits of the platform.

Several years ago I was approached by a new professor at a major American university about purchasing a refurbished Siemens D500 XRD. He’d been seriously considering a new instrument from one of the big-three OEMs, but chose to focus on the D500 due to its reputation for low cost of ownership, versatility and nearly identical resolution/intensity to the new system he’d been looking at. It’s been a few years since that unit was delivered and I’ve been very impressed with the improvements that have been made.

The first step was to bring the software up to date with a complete package from Materials Data Inc. (MDI). This included Datascan 5.0 for instrument control and data acquisition as well as the flagship Jade 9.5 analysis package. Whole pattern fitting (Rietveld), semi-automatic phase ID (Search/Match) and a host of other advanced quantitative and modeling options are included. Jade 9.5 is modular and can be purchased with any combination of these options. I’d estimate that 70% of the XRD systems we sell go out with some level of MDI package. We’ve been working with them for 20 years now and have never heard anything other than glowing praise for their excellent products and support. One key feature of Jade is that it was designed to be a universal analysis solution from the ground up so there’s never a problem opening any of the OEM file formats. It’s much easier to justify the cost to upgrade your software when you know it will integrate seamlessly with any other data or instruments you may encounter. Contact KSA if you’d like more information on this.

This is Jade 9.5. You’ll notice that it’s a much different interface than the Jade 2010 program I usually use. This option is modular with available plug-ins for all the higher level functions of Jade 2010, but 9.5 is perpetually licensed.

This is actually the VirtualXRD program that comes along with Datascan. I don’t use it often, but some of my users run extremely long count times and predicting the affect of a parameter change could save them days of experimentation. It’s a great tool even for users running simple 1 hour scans.

The next step was more hardware based than anything else. The independent axis control of the D500 (in Theta/Theta or Theta/2Theta configurations) allows for both rocking curves and grazing incidence scans. With the goal of analyzing thin-films in mind, we upgraded the D500 with a grazing incidence attachment. These are designed to minimize scatter while the sample is held at a shallow (usually 3 degrees) incident angle and the scan is performed with the detector alone. The attachment consists of a long collimator coupled with a simple monochromator just before the detector. We’ve performed some rather intense studies with one of these at Texray and were very impressed with its performance. In fact, we use it whenever practical even though we have a dedicated parallel beam optics system in the lab as well. It was about time for a new tube so a new, ceramic Cu long, fine focus tube was included in the upgrade.

Some additional software solutions were developed on-site to facilitate XRR (X-ray Reflectivity) measurements around the same time. I confess that this is not something I’m personally very familiar with, but it seems fascinating. It involves scans at extremely low angles which can require caution since one is working with a very nearly direct beam.

The last upgrade he made is actually the one that most impressed me and the one I had absolutely nothing to do with. In an effort to further expand the capabilities of his instrument, he purchased and installed an energy dispersive detector with an integral digital pulse processor (DPP). Clever mounting and some experimentation allowed him to perform EDXRF elemental (qualitative AND quantitative) analysis on samples while using the D500s X-ray tube as the primary emission source. The flexibility of the D500 platform even allowed him to control the effective layer depth by adjusting the incident beam angle. Since his application involved analysis of a thin film coating, he set the goniometer to a low angle to minimize penetration depth and substrate interference. After seeing how well this worked, I immediately started working on a similar upgrade that we could offer to all our current and future XRD users. I’ll detail my early progress in the next post.

Phase ID

Posted by: Ken Stauver In: Uncategorized 23 Sep 2013 0 comments Tags: AMCSD, Bruker, crystallography, D500, D5000, D5005, D8, Datascan, Diffraction, Diffractometer, ICDD, Jade, Jade 2010, Jade 9.5, JS Technical, KS Analytical, Materials Data Inc, MDI, NIST, Phase analysis, Phase ID, PXRD, Siemens, X-ray, XRD, XRF

XRD work is categorized into two major groups. Single crystal and powder analysis. While single crystal work is usually highly customized to particular applications and involves a largely unique hardware set, powder (PXRD) work covers a broad range of applications. Many of which can be performed without any special hardware at all. Perhaps it would be more accurate to call it “Randomly oriented small particle” diffraction. Somehow I think “ROSPXRD” would be slow to catch on. At the risk of oversimplifying the options, I’d like to take a few posts to showcase some of the more common analyses which can be performed with a basic PXRD system and perhaps a few that require minimal additional attachments.

This is an example of a Bruker D8 Advance configured in its most basic PXRD state with only a scintillation counter, sample stage and source.

This is the same D8 base instrument configured for single crystal XRD. Note the Chi, phi, XYZ stage, area detector (2D) and Goebel focusing mirrors.

My last post involved a basic phase identification and this seemed like a great place to start. Most PXRD users are asked to identify some unknown bit of corrosion, rock or contaminant at some point. I once took a shot at something which later turned out to be sewage sludge ash. I have no idea what they hoped to find in that. Exotic, mundane or distasteful, the most basic XRD can collect the necessary data to perform this analysis. Phase ID is usually the first step most users take toward more advanced software. In addition to the simple pattern analysis features that usually come standard, you’ll need an engine designed to search one of the many commercial or open-source databases available. The ICDD, NIST and AMCSD are probably the most popular with several others on the fringe. There are even user-developed databases which are usually compiled in a particular lab to cover the range of phases they expect to see based on their product or application.

Limiting the search to categories of phases which are likely to be present greatly improves the relevance of the results list. There’s obviously no reason to search through a huge list of minerals when trying to identify a metallic oxide coating. Hit lists can also be refined based on data from other sources such as qualitative elemental analysis. We use our WDXRF systems and the built in elemental filter in Jade to trim the options substantially.

Any good search/Match engine will have support not only for multiple databases, but also offer the option to limit your search to certain subfiles which are group my material categories.

Semi-quantitative or simple qualitative elemental data can be used to eliminate a large percentage of erroneous hits so the analyst can focus on only pertinent options. We prefer to bundle an XRF scan with any Phase ID project.

Isolating the valid hits from erroneous is where experience comes into play. Non-ideal particle size, preferred orientation and crystallographic imperfections can make the process quite difficult. Relative peak intensity ratios, peak width and sometimes even the complete absence of a particular peak which would theoretically be present all present opportunities to gain additional insight. Sometimes this is relatively easy as in the case I presented in the previous post, but other situations are not so simple. These difficulties are amplified in the case of low concentrations and complex mixtures.

This is a great example of Phase ID the way we all wish it came out. The peaks are sharp, intense and located right on their theoretical angle.

This is an example of something a little harder to nail down. Overlapping peaks, several additional phases and a highly imperfect sample. Refining the options based on external measurements and in depth sample prep make the difference between success and failure in cases like this.

XRD pattern analysis has come along way in the last 40 years and most of the major improvements have come on the heels of increased computing capability which enables us to perform exhaustive iterative calculations on complex patterns quickly and at comparatively low cost. However, there is nothing on the market as of now which has made an experienced analyst obsolete.