There are several key meetings and conferences each year which might concern material scientists in general, but there’s only one exclusively dedicated to analytical X-ray techniques. The Denver X-ray Conference (DXC) has been organized by the International Center for Diffraction Data (ICDD) for the past 64 years! I don’t get to attend as often as I’d like, but I’ve never regretted making the trip. It’s not always in Denver, but The Westin Hotel in Westminster, CO played host yet again this year which makes everything very convenient and relatively inexpensive. I was fortunate enough to merit an invitation from our good friends at Materials Data, Inc. this year and attended as their guest.

The main draw for me is the educational sessions. Classes taught by legends in the industry on everything from basic XRF and XRD theory to advanced structure determination and pair distribution function (PDF) analysis. Topics vary year to year, but this time I sat in on mainly XRD courses. Instructors are usually prominent university professors or industry experts. ICDD has a strict policy against overt advertising in these sessions which means information is presented in “platform neutral” terms and is beneficial for all attendees. The exhibit hall is full of vendors promoting everything from complete XRF and XRD systems (PANalytical, Bruker, Rigaku, Thermo etc) to sample preparation equipment (Chemplex, Spex, Claisse, Mikron, Angstrom). One of the most interesting products I saw was the latest D2 Phaser from Bruker with a new LynxEye PSD capable of eliminating Cu KB1 peaks without the need for a Ni filter. This doesn’t sound like that impressive of a feat until one considers that this will triple the intensities with an inverse effect on data collection times.

Proto has expanded their offerings to include a benchtop XRD with some impressive capabilities. Most notably, it is the only benchtop I’m aware of which offers independent control of the Theta and 2Theta axes. Grazing incidence and rocking curves are valuable data collection techniques which have thus far been unavailable to small XRD users. It’s always going to be hard for a small instrument to match the data quality of a true, research grade XRD such as the D500, D5000 and D8 lines, but they’ve certainly upped their game in this area.

Oxford was onhand to show off some of their very impressive low temperature stages. The more elaborate offerings are capable of cooling a sample to 12K… You read that correctly, 12 Kelvin. They do this with a regenerative He-based cooling system. I installed a D8 last year at Johns Hopkins which was purchased as nothing more than a base for one of these stages.

I spend most of my time bouncing between industrial, academic and government laboratories maintaining and upgrading their hardware so I see many of the attendees throughout the year though it’s rare to spend time with them casually. It’s always a good time with laughs, enlightenment and education.

We’ve been using additive fabrication (3D printing) and traditional subtractive methods (CNC machining) for years so when we started looking for a fun item to give away at the AAPG conference, we decided that a special Texray/KSA billet Aluminum microsplitter would be a great way to show our prospective clients that we’re not just in the business of chemical analysis, we’re passionate about it.

It is often quipped that sampling technique is the first and most important step toward accurate results. It’s easy to get carried away focusing on instrumental repeatability and analytical error, but these can only ensure accurate results for the aliquot measured. Some of our clients are only producing materials in mg batches, but we got to talk to the users on the other end of the spectrum at AAPG last month. These geologists are concerned with the chemistry of huge formations so getting a representative analysis is critical. They’ll take thousands of samples and combine the results into extremely complicated data sets. Many of the companies exhibiting there were selling data and data representation tools and nothing else. One company specialized in moving massive quantities of data over existing internet infrastructure. Apparently many of these outfits are generating so much data that the only way to move it rapidly enough is to ship boxes of hard disk drives from the exploration site to the central lab.

Those are extreme cases and require exotic solutions. The more common situation is that a client will ship 1kg of material for us to analyze. Sampling at this scale is still an important part of getting accurate results so while it would be very easy to simply spoon a measurable aliquot from the bag, we prefer a more precise and elegant solution. Microsplitters (also referred to as “rifflers”) are a great way for labs to reduce larger bulk materials with reasonable certainty that the they’ll retain a representative sample. These indispensable little devices consist of a top section (the funnel), a splitting mechanism (I call it the comb), and two or three receptacles (bins). The comb is not simply a series of straight slits, each one has a ramped bottom which alternates between one bin or the other. In this way, the sample is divided between the two bins more or less evenly. The contents of one bin are discarded and the contents of the other bin are dumped into the funnel to be split again until the desired volume is reached. This is why it’s best to have three bins on hand.

The gallery below includes a few pictures from the initial rapid prototyping through the finished product. In the end, I added some fancy legs to the side to make it easier to use. Note that the slits are cut with a slitting saw on out CNC milling machine. This allowed for slots which have rounded edges at the top and bottom. This is critical to avoid clumping and makes a very smooth transition at the top and bottom of the comb. We may offer these as a regular product if there is enough interest to justify a production run. If that happens, customized engraving would be an option. Contact us if you’re interested.

We had a great time at AAPG 2015. Many of our existing customers were there including some from overseas. The oil industry is in a bit of a slump, but it didn’t stop the big players (Baker Hughes, Weatherford Labs, Core Labs, Saudi Aramco, etc) from putting together very impressive booths and lots of extra activities.