Insights from industry

Features and Applications of the Nicolet iN10 FT-IR Microscope

In this interview, AZoM talks with Dr. Mike Bradley from Thermo Scientific about their exciting iN10 FT-IR Microscope.

Infrared microanalysis offers some unique research and analysis opportunities. How do you feel the Thermo ScientificTM NicoletTM iN10TM FT-IR microscope meets the needs of today’s scientists and laboratories?

The Thermo Scientific Nicolet iN10 microscope was designed from the ground up to be a general user’s microscope rather than a microscopist’s microscope. By which I mean, if you look at it, it doesn’t look like a traditional microscope at all. It’s very clean on the outside. There’s no knobs and dials and things like that. You don’t even see the barrel that you associate with traditional microscopes.

It was designed to be integrated into a single unit. The infrared spectrometer, all of the optics and everything were optimized to work together as efficiently as possible. This turns it into more of a productivity tool than just a microscope.

It’s still a fully-fledged microscope but it’s a tool where people can easily walk up to it and not be intimidated by it; they simply just start using it. The operation is done by computer icons for added familiarity. There are no eyepieces on the unit, it has been designed so the person uses camera images on a computer screen. It’s almost like you’re playing a video game as you’re working with your science.

Nicolet iN10 microscope with Nicolet iZ™10 FT-IR module.

Image 1. Nicolet iN10 microscope with Nicolet iZ™10 FT-IR module.

The basic need of a scientist is to solve a problem, that’s what they’re interested in. They’re not necessarily interested in high-power microscopy. The target audience for this product was really the people who had chemical problems they wanted to solve. They wanted to identify something. They wanted to be able to look at a pile of powder and identify the different components present in the power. To look at a pharmaceutical tablet and be able to analyze the different regions of that tablet.

The microscope is a tool just like a screwdriver to get you to the end goal. In other words, the microscope isn’t what they’re after, they’re after answers, and they want to know what’s going on. That’s really the way this tool was designed – to answer questions and find solutions.

To further optimize the iN10 microscope, it was designed with specialized optics to allow you to use a non-liquid nitrogen cooled detector for your analysis.

Most of the time users can get down to 50 microns without using a liquid nitrogen cooled detector, so in other words you can put the Nicolet iN10 in the back of a truck and analyze samples on the road without needing liquid nitrogen.

There were a number of tools supplied to improve productivity. As I said the key points are that the spectrometer and all the pieces of the microscope are integrated into one instrument with a very innovative software interface, including some wizardry that we’ll talk about a little bit later in the interview, and then all of this extra power through these multiple detectors we’ll also discuss later.

What specific features of the iN10 enable enhanced analysis of specimens?

In order to understand the features of the iN10, you have to understand the problems that we were trying to solve.

A customer may come to us with an electronic circuit board and there are fibers which they can see embedded in the wiring, those finely laid down wires on the board, or there may be a component or solder or something that’s contaminated. In order to analyze these items, you need to use a device that samples a very localized area. We have something called a micro tip ATR which allows you to sample from a very small area, a few microns in size, yet the surface can be highly irregular, it doesn’t have to be smooth to do that. You can analyze those very small areas simply by engaging the pressure device to push that ATR down onto the sample in a specific location you have visualized on the screen.

Software Wizardry

Thermo Scientific OMNIC™ Picta™ software provides the full picture from particle and multi-compound analyses.

Image 2. Thermo Scientific OMNIC™ Picta™ software provides the full picture from particle and multi-compound analyses.

There’s also a large number of software wizards to help achieve the desired analysis. We worked with customers who have specific problems, like they have a powder and they want to identify the different components of that powder. They lay the powder out onto a microscope slide, and they analyze it with the spectrometer. This wizard does everything for you. The iN10 1.) locates the particles, 2.) it puts the aperture or the focusing point of the microscope onto those particles, 3.) it collects the data, 4.) it collects the background data correctly based on the size of those apertures, 5.) it does the spectral searching, and 6.) it gives you chemical and component identification on screen and in a final  report. Basically you go from having a pile of powder on the microscope slide to a report which you can pass onto your superior, all with very minimal interaction.

Detector options offer flexibility to meet sampling needs.

Image 3. Detector options offer flexibility to meet sampling needs.  

We also have an ultrafast, wide-area mapping capability where the instrument can basically sweep across the sample very quickly and give you a large area chemical view of samples. One of our favorites is the eyeball on the US $20 bill. One can analyze that specific area, the ink and everything in it. That would be considered a fairly large sample; it’s several millimeters in size. You can scan across that very quickly, get the data and analysis into a report fast, without much user manipulation.

Coupled with this analysis, the instrument has a very high infrared throughput, meaning you get lots of the light through the instrument, allowing the use of a room temperature detector, which I pointed out earlier. We also offer two other detectors on the iN10, one of which is a high-sensitivity liquid nitrogen detector, allowing you to detect things very quickly or to do intense investigations of small area samples.

Finally, there is the array detector that allows us to sweep across the sample very quickly. Imagine a broom sweeping across the sample. So we have several features to probe the customer samples. Maybe they’re looking at inks on paper or the electronic circuit board, so we have this imaging array or we can touch it with the ATR.

The key mission of the iN10 design was to match up our customers’ requirements, their questions, and apply the capabilities of the instrument to directly access different sample areas and answer those questions.

This really is an instrument that’s designed for the working scientist. It’s great to see a product developed from that standpoint, helping people meet their own requirements and needs in industry.

You always have two approaches to it. You can imagine when you’re driving an automobile, what does the extra horsepower buy for you? Now I will admit that I want an Aston Martin DB9.  I also know good and well that my little car does a very good job of getting me to the grocery store. What a user wants in the lab out of a scientific instrument is to solve problems. You’ve got the high-end users who want the fancy stuff and yeah you’re right, they want more horsepower and more tools, but this tool’s designed with the scientist, the person at the bench who works in a polymer factory who wants to solve a problem, in mind - that’s who this is for.

The Nicolet iN10 has been designed to seamlessly integrate with a range of other analytical techniques; could you tell us a bit more about the configurable options that are available on this tool?

The Nicolet iN10 microscope can be interfaced to a unit that’s called the Nicolet iZ10. It’s a module that sits on the side of the instrument. Previous microscopes and the vast majority of those that are available in terms of infrared microscopes required a spectrometer to be attached.

In order to be able to access these other techniques, the iZ10 uses the beam that comes out of the microscope. This unit allows us to do things such as bulk sampling, attenuated total reflection for larger size samples, or very interestingly, something called thermogravimetric analysis (TGA) infrared, where you can de-formulate a sample!

In a polymer lab for instance, you would get a sample in and you want to understand the contaminations or the defects that are present in that polymer, so you may examine those under the microscope. But then if you want to probe the chemistry of that polymer defect, then you need to de-formulate. You take the sample, you put it in this TGA, which heats the sample up. The TGA does a quantitative measure of the gases that are evolved as the sample heats up. But then those gases can be sent out to the infrared side unit, this iZ10 sitting next to the spectrometer, and analyzing those gases tells us what they are.

Now I’ve got the microanalysis tool, where I’ve analyzed the defects or the localized imperfections in the material as best as I can using the microscope and spectrometer, and then I can also do a bulk analysis, where I’m looking at the overall content of the material using TGA.

The germanium Slide-On Micro ATR accessory expands analytical capabilities to the smallest samples.

Image 4. The germanium Slide-On Micro ATR accessory expands analytical capabilities to the smallest samples.

This gives you an analytical workstation where you can analyze a wide range of problems. The bulk ATR, the thermogravimetric analysis, and the microscopy.

The real point of any of these labs as we understand it is to solve problems, that’s what they’re after. You realize that more than half of the time a single tool is not going to do it.

You’re going to need to bring a battery of tools there and that’s what we’ve got here; the ability to add these extra tools to the iN10. Of course there’s a blizzard of other analytical techniques but that’s one defined example of how we’ve adapted the iN10 to give us more of this kind of complementary information.

Do you find that your application engineers get involved heavily, early in the buying process to help your clients spec the iN10 or do you see it as an off the shelf product?

One of the key things in the selling process is how we generate a relationship with the customer. You will find that there are broadly two kinds of customers; you have experienced customers who understand very well the FT-IR technique, and they will come in, and they will define for you the instrument they want, “I need to do near-infrared and mid-infrared and far-infrared, and I need this kind of microscope, and I need this spatial resolution.”

More times than not, however, you’re working with customers who, as I’ve said again and again, have a problem they want solved, yet are not spectroscopists nor microscopists.

In that case, the selling process is more consultative, where we will sit down with them and listen, “I have this problem where I’ve got dimples forming on the dashboard of my automobile, and I need to get rid of those dimples. I need to understand the origin of the dimples and then obviously how to eliminate them.” At which point you, now as a consultant to them, begin to help them define the instrument they really need, “What are the polymers, what are the things you’re looking at, how might you prepare your sample?” Once we know their problem, we can explore the different ways of configuring the perfect instrument to answer their questions.

We’re the experts on the technology. They are the experts in the problem they need to solve. We help them find the solution.

We have already touched on a few of them Mike, but are there any specific industries that you’re aiming the iN10 instrument at?

As an instrument manufacturer and designer, you would really like to strive towards covering all bases. If you focus too much on a given industry, you become tied to that industry and the market fluctuations that occur there. If you’re tied to the pharmaceutical industry and suddenly they go into a recession, you’re in a slump. Fortunately FTIR microscopy has extremely wide applications as an analytical tool.

Polymers is a very obvious industry. Polymers ever since the beginning of FTIR has been a very important market for us because of the chemical compositions and processes used to make these raw materials. But we also look at paints and coatings, packaging materials, etc.

Transmission image of a polymer laminate film on a salt window (BaF2)

Image 5. Transmission image of a polymer laminate film on a salt window (BaF2)

The potential applications of the Nicolet iN10 are extremely diverse. For example if you look at the seal on a bag of potato chips, the way the chip bag is sealed at the top by that hot seal; it forms a multilayer film. If you cut away a sample of that, you can actually see the layers in it; you can see the tie layers and the bulk polymer layers. Again, you can analyze for defects or imperfections in your packaging material – by refining the sealing process and you may improve packaging performance! Microelectronics I touched on earlier.

We do a lot with inks and pigments, fibers or embedded fibers. A large user of tools to help identify the make-up of these types of samples would be the forensics industry. We sell both of our microscope solutions into forensics because they’re interested in everything from the age of bloodspots to the embedded fibers in a piece of evidence to who knows, it’s very interesting! They never know what sample they’re going to have to analyze, but a lot of times it’ll be micron-sized samples.

Pharmaceuticals is also a huge market for the Nicolet iN10. We’re helping clients look at tablets, their formulations and the homogeneity of a tablet. If you look close at like a cold / flu tablet, three main ingredients are usually there: a painkiller, something like aspirin or acetaminophen, something for decongestion and then maybe caffeine. As you look at the sample, these samples are not homogeneous within the tablet itself.

What you’ve got are little domains, almost like sand particles, or little crystalline regions of each one of these ingredients. As you look at the sample, it’s a mosaic of all these different components intertwined. It’s not like the three things are perfectly homogeneous, they’re distributed in these little domains throughout the tablet, and you can see those under the microscope using visible and then the infrared spectrum.

We’ve also worked with cement companies; we’ve worked with tires or rubber, and cosmetic companies. We’ve worked with people doing LEDs and laser technology.

We’re beginning to see more applications even in medicine, where they’re imaging thin biopsy tissue samples, looking for chemical aberrations, maybe even distribution of a drug treatment.

What specific features of the Nicolet iN10 really do you think make it perfect for this diverse range of applications?

One of the key pieces as I stated at the outset was the efficient movement from a sample to an answer or solution. The customer is not really interested in a squiggly line that might mean nothing to the untrained eye. In the pharma example, customers want to visually and chemically identify those domains present in the tablet. They want to know what they are, they want to know where they are, and they want to know how big they are. They want to find out if their manufacturing process is consistent or not. They want to see if a raw material is degrading under certain process conditions or not. They want the whole solution!

These are the tools that are available through the software wizards. The iN10 can give you a map at the end, showing you not spectral points, but actually identifying which compounds are present, where they’re present in the mapped area. It can even ratio the total area of one particular component to the total area of the map, which gives you a semi-quantitative measurement of the concentration of those materials present in the tablet.

The idea here is that with the wizardry as a major feature of the system, you can move from the sample all the way to the analysis report, which provides the answer you want to pass onto your superiors.

In the forensics lab they might get a sample in and they want to quickly examine it under the microscope. Without requiring liquid nitrogen, they can put it under there, run it with the room temperature detector, get a first pass, and then if they need more information, they can move on to the more sensitive analysis.

That high speed detector I mentioned earlier is able to give you a wide area of image to really look at a large amount of your sample in one pass. You may not know where the defect is, you may not know where the problem is, this helps you narrow down your search quickly.

An interesting example of this is in some of the counterfeiting fields. If the counterfeiter actually tries to erase or change a number or a signature, you can actually still find traces or images of the ink that were left behind. Or even flakes of skin or other materials that are embedded in it. You wouldn’t have known where to look for this initially. By being able to scan it quickly, you find this information quickly and efficiently.

It’s really cool because if you look at ink on paper, there's a multilayered set of answers. If you examine for the cellulose, you can actually see the underlying fibers in the paper without seeing anything else. It’s like looking through the ink at the paper. Then you can change what you’re looking for and look at the inks and now you get this image of the different colored inks on the paper without seeing the paper! That’s the advantage of these wide area images, you can pick out what you want to look for and then get the images that are very specific to particular pieces.

The idea as I’ve kind of been stressing since the beginning is moving from having a pile of samples on a microscope slide to getting a true answer. The integration of the software and the hardware make that happen, this is the magic of the Nicolet iN10.

What we have done is translate a diverse range of data gathered efficiently and rapidly into actionable information.

As the efficiency and cost of laboratory analysis is increasingly focusing on cost and  budget, how does the Nicolet iN10 help to streamline microanalysis workflows in the lab?

The information content and the transition of that information into true actions often required the involvement of an expert, someone who could interpret for you, almost like sending your x-rays off to the radiologist to get an interpretation of them. What we’re trying to do here with the iN10 is help you need that radiologist, that expert, on a less frequent basis because we’re now giving you more of the answer that you’re aiming for in one fell swoop.

What we’ve done is add the high throughput infrared so that you’re getting more signal, to enable you to take data more rapidly and then help you remove as much as possible the need for an expert to analyze it.

About Dr. Mike Bradley

Dr. Michael Bradley received his B.S. degree in Chemistry from the University of South

Carolina and his Ph.D. in Physical Chemistry from the University of Illinois.

Dr. Mike Bradley

He taught graduate and undergraduate chemistry for 15 years, prior to becoming a field

applications scientist with Thermo Nicolet – subsequently Thermo Fisher Scientific – in 2002. In 2008, he helped launch the Thermo Scientific Nicolet™ iN™10 microscope and Nicolet iS™10 spectrometers, while also completing his M.B.A. in management.

As a Product Manager, Mike worked intensely developing the Thermo Scientific iS™50 FT-IR spectrometer, which joined the Nicolet iN10 as an R&D 100 Award winning product. He is now Marketing Manager for FT-IR and FT-IR Microscopy products.

Mike enjoys fishing from his kayak, camping and building models. Mike and his wife have two children (both entering science).

 

 

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