Are you fully aware that many essential physicochemical properties of an Active Pharmaceutical Ingredient (API) depend on its solid-state structure? Solubility, bioavailability at desired levels, shelf-life stability, hygroscopicity, compressibility, tableting ability, electrostatic charging, plus many others, can be crucial properties. And the decision is not trivial, which kind of solid-state form should be produced or selected for an API and which data are required by patent lawyers. Sophisticated analytical tools and the right expertise are essential for successful evaluations. 

Inolytix AG represents now SOLID-CHEM GmbH in Switzerland
By working together on analytical projects, it became clear that SOLID-CHEM GmbH, Bochum, Germany possesses special equipment of instruments and the right expertise – especially for the pharmaceutical industry but also for others. Customers reacted very positively, for example, “…now my favorite CRO for ssNMR….”.  
Therefore, we are pleased to announce that Inolytix AG is now an exclusive partner in Switzerland for services offered by SOLID-CHEM GmbH. 

Offering a comprehensive service of solid-state analysis
Exploring suitable solid-state forms (amorphous, polymorphs, salts, co-crystals, or solvates) requires a diverse methodological portfolio plus the expertise and the compounds for (co ) crystallization. Moreover, you need to precisely define all the appropriate analytical tools when matching your API with the final formulation.
Many methods exist for determining solid-state forms because the intermolecular interactions responsible for the solid-state have a very subtle character. Diffraction- and thermochemical methods, particle determination, ssNMR, humidity determination, etc. - all this requires collaborating specialists overviewing such cross-networking analyses. Finally, they have to understand the different languages when speaking to organic, bio, theoretical, and technical chemists, to pharmacists, formulation specialists, and, last but not least, with patent lawyers. 

​It will be our pleasure and ambitious task to provide you with the best analytical services for solid solutions for the solid-state of pharmaceutical products ranging from 

•    pure APIs to complement tablet formulations
•    screening procedures of solid forms, 
•    data for patents or stability tests

Any questions about your solid product form? 
Contact us, and let’s discuss it! 

​Please find below two supporting documents: 

1. ​A one-page overview by SOLID-CHEM about Screening Procedures of different solid forms, e.g. polymorphs and characterization methods
2. A detailed presentation of the different characterization methods and applications with examples created by SOLID-CHEM and Inolytix 

Inolytix, Aargau (Switzerland) - Inolytix is a startup launched in 2014 with the focus on accelerating product development and true understanding for the chemical and pharmaceutical industry. Through new and innovative analytical methods delivered by reliable and experienced partners such as SOLID-CHEM, Inolytix offers a customer-friendly service for R&D departments: providing the customer with a clear expert view and access to effective, but less known analytical methods, Inolytix manages the whole process from quotation to the industry- oriented report on the results. 
Contact: Dr. Ralf Dümpelmann (for Switzerland),  Founder and Managing Director
ralf.duempelmann@inolytix.com, phone: +41 79 312 9327, www.inolytix.com 

SOLID-CHEM GmbH (Germany, Bochum) - Founded by Prof. Boese and Dr. Schauerte as a spin-off from the University of Essen, SOLID-CHEM GmbH has become an expert center of solid solutions for the solid-state of pharmaceutical products. The philosophy is, to support customers with expert opinions based on experimental, scientific, carefully retrieved data and on precisely documented experiments. Results and reports from investigations can be potentially used for litigations, and therefore, scientific integrity is our absolute priority.
Contact: Dr. Carsten Schauerte, Managing Director and Co-founder, 
schauerte@solid-chem.com, phone: +49 234 936 90610, www.solid-chem.de

Surface analysis of solids as particles, fibers and plats can be very tricky. Dynamic gas adsorption with 15+ different gas probes, also known as Inverse Gas Chromatography (IGC), delivers very detailed information about surface energies, nanoroughness, polarity, acid/base properties (Lewis) and surface heterogeneity.  

Adscientis has 20 years of experience of analyzing samples by IGC with now over 800 different projects for the industry. Recently, Adscientis made a great step forward in IGC with a new automated system (neuronicIC) of high flexibility, accuracy and transparency of all process conditions overcoming thereby many shortcomings of existing instruments.  
Inolytix, founded in 2014, is an enthusiastic promoter of innovative analytical techniques and IGC in particular from the beginning. Analytical challenges of the chemical and pharmaceutical industry are successfully solved especially of solid and surface properties. With respect to IGC, the focus is on the german-speaking market, i.e. Germany, Switzerland and Austria. The annual organization of the International IGC-Symposium is one of the examples of community support and expert network. 

Inolytix and Adscientis start a global cooperation
Now, with the new IGC instrument, both experienced companies decided to join forces for a global collaboration. This involves common communications about the use of IGC, the new instrument properties, application notes, webinars and an extension of the IGC Symposium worldwide. “It is exciting to work so closely together and to use our mutual understanding of surface characterization on a global scale”, says Ralf Duempelmann, Managing Director and Founder of Inolytix. Eric Brendle, CEO of Adscientis adds “After six years of some cooperation with Inolytix, it is now just the right time for a closer cooperation. We share the same spirit and enthusiasm to move IGC towards the next level”.  

Interested in surface and solids characterization?
Having issues with qualities, batch-to-batch properties or understanding product modifications? Don’t hesitate to contact either one of the companies! Our expertise and their our willingness to characterize difficult surfaces will bring you forward – either using IGC or complementary analytical techniques.  

Adscientis, Wittelsheim (France) - Adscientis, founded in year 2000, is today recognized as the most reliable IGC specialist. With over 800 customer projects, the company acquired a unique set of skills and know-how on IGC techniques for the surface characterization of powders ranging from carbon black to pharma products, fibers and flat surfaces. The art of using dynamic adsorption and 15+ gas probes is refined continuously to deliver reproducible and quantitative values of surface energy, nanoroughness, polarities, acid/base properties, surface heterogeneity, specific surface areas and even HSP values. The results address crucial challenges as quality issues, product development and application behaviors. The development of an automated and highly flexible IGC instrument is based on customer needs and a result of the long-term practical experience.   
Contact: Dr. Eric Brendle, CEO, e.brendle(at)adscientis.com,
phone: +33 389 4800042, www.adscientis.com 

Inolytix, Aargau (Switzerland) - Inolytix is a startup launched in 2014 with the focus on accelerating product development and true understanding for the chemical industry. Through new and innovative analytical methods delivered by reliable and experienced partners such as Adscientis, Inolytix offers a customer-friendly service for R&D departments: providing the customer with a clear expert view and access to effective, but less known analytical methods, Inolytix manages the whole process from quotation to the industry- oriented report on the results. 
Contact: Dr. Ralf Dümpelmann,  Founder and Managing Director, 
ralf.duempelmann@inolytix.com, phone: +41 79 312 9327, www.inolytix.com 

​I have worked for 20 years in the R&D of global chemical companies and I always appreciated their own, in-house analytical services. They are fast, have known methods, all costs are budgeted and best: costs appear only somewhere in the depths of SAP. Great!
 
Today, I’m running Inolytix Ltd and we bring innovative, less known analytical tools as external services into chemical companies. Why? It’s my believe and experience that many opportunities in understanding your F&E or quality issues are missed, simply because the known analytical methods are too often not the best. Or to quote Donald Rumsfeld “…there are also unknown unknowns, things we do not know we don't know.” 
 
In this article, I’d like to discuss the advantages of in-house analytical services, the advantages of external analytical services and how to balance both in the best possible way. To be a bit provocative, I’m stating some common believes as myths and explain the truth behind. Are your experiences different or do you share similar stories? Would be great to know !
 
Myth #1:  in-house analysis is the cheapest option
Yes and no. For standard analysis like HPLC, being used on a daily basis, hardly anything can beat your own analytical laboratory. It is not only comparable in costs to the cheapest external laboratory (even though some outsourcing labs argue on price), but also fast and results can be easily discussed with the experts in-house. 
But for analytical methods not being used every day (like e.g. Raman-FTIR, XPS or IGC), things look very different: These analytical services (if available in-house) seem cheap too but in fact, they are not.
 
Truth #1: a lot of in-house costs are hidden
Three factors seem to hide some of the true costs:
First, service, maintenance and repair of analytical equipment is a considerable cost factor especially if not used on a regular basis. And these are cash-out costs.
Second, method development for rarely used instruments are often difficult and time consuming. However, the analytical department needs to promote special methods, otherwise they will never be used – so costs are distributed. 
Least obvious, but very important is the third point: the value of expertise. Experts need exercise, many different samples and challenges. This is easy with daily analysis, but difficult with less used ones. Either the expertise is not very high or regular practice is costly – either way, this is not satisfying.  
 
Myth #2:  new analytical instruments amortize easily
NO – at least in many cases. We all know this justification: the new instrument costs e.g. EUR 150’000.  With 150 samples over 2 years, costing EUR 1’000/sample externally pay-back time would be 2 years only: a convincing argument! But really?? Before coming to Truth #2, I would like to mention a fact which makes it indeed easy to invest into new equipment – regardless of any follow-up costs. The investment budget for a new instrument is simply a different “box” than the operational budget. It is common sense to allocate some money for new instruments. However, this investment budget is often being fully used, irrespective of whether or not the new instrument is indeed useful and cost efficient. 
 
Truth #2: operation, maintenance and expertise are expensive
A true pay-back time calculation needs to incorporate all operating costs such as working time plus maintenance, method developments, amortization and the development of the required expertise to actually use the given instrument. The more underutilized the instrument is the worse becomes the calculation due to an increasing part of fixed costs. Let’s assume the in-house operating costs of the case mentioned above can be brought down to EUR 500 /sample. In this case, pay-back time doubles to 4 years! Some details are provided in an example including an FTIR instrument of USD 20’000 investment and external costs of USD 10’000. In conclusion, realistic pay-back times of analytical instruments are often much higher than anticipated. External services appear costly at first sight but in fact, they are often highly cost-efficient if compared on a 1:1 basis. 
 
Myth #3: in-house experts are the best
Surely, in-house experts are often very good, especially with methods they always use. But what about the other methods? Last year, I have visited a company sophisticated on rheology using rotary viscosimeters. But they did not know about micro-rheology offering new possibilities in their case. It needs a good balance between the NIH-syndrome (not-invented-here) and curiosity plus openness for new methods.  
 
Truth #3: really good experts know when to ask for advice
 The solution for your analytical challenge may be in-house, but it might be also outside. Your experts are really good if they are curious, reach out to other experts and help to find the best analytical solution for you– and not just the one available. The first steps of external expertise are often free anyway. A short email or a phone call and you have more options to evaluate already. Surprisingly, I’m receiving these requests more often from development chemists than from analytical people. 
 
In conclusion, there are many rational arguments to be more open towards external analytical services – to save money and to increase the understanding of the product properties. 

When we had decide because of Covid19, if the annual IGC Symposium should take place in 2020, we did not expect this successful outcome. Instead of doing it onsite in person, we took the opportunity to offer it online. And suddenly the number or registrations increased rapidly. At the end we had more than 150 registrations from all over the world.

Another benefit of going online are the recordings that you can now watch afterwards, even if you did not attend the symposium. We published all those that we are allowed to publish on youtube. If you are interested in learning more about the applications and special details of inverse gas chromatography, you find the recordings below.

If you are interested in the slides you can download them here:

If you have any questions or requests, please contact us.

Our first online webinar "Introduction to Inverse Gas Chromatography (IGC) and Best Practice" on 8th June 2020 was a great success. More than 45 participants participated and actively engaged in the Q&A session. The initial objective of the webinar was to give newcomers in IGC a first understanding in this technology as a preparation for to 9th Int. IGC Symposium, 16th June 2020, see IGC Symposium website.

However, it seems, it was the beginning of an open, almost global dialogue about how to characterize powder and other surfaces by dynamic gas adsorption. 

The Q&A session after the presentation highlighted many open questions and uncertainties around IGC as a technique. You find the questions and some of the answers below. We plan to answer them in a separate blog post. ​Follow us and stay tuned.

Do you know, that highly quantitative values for diffusion coefficients, adsorption isotherms of methanol on zeolites and energy distribution functions, as well as detailed characterization of recycled and artificially aged catalysts can all be performed by perfectly controlled adsorption and desorption processes?
​We have entirely redefined an instrument also known under the name “Inverse Gas Chromatography”, short IGC. Today, our setup is the most versatile instrument to study all kind of physisorption processes – not only for catalysts, but for many other powders, fibers and plates too. 

We were so much looking forward to showing our poster (download below) about catalyst applications at the “53. Jahrestreffen Deutscher Katalytiker” scheduled for 11-13 March in Weimar – usually attracting around 600 experts! But: Due to the Corona crisis, this conference was cancelled. Now we are taking the online opportunity to explain the key features of our unique setup and explain the use by three very different applications. 

Key feature of our IGC instrument is very flexible injection of any kind of volatile “probe” substance into the gas stream – either at very low concentrations, ideally “infinite dilution”, or at high concentrations at defined p/p0, e.g. 0.3, to allow a saturation of the surface. In IGC terms, these two regions are called IGC-ID and IGC-FC (finite concentration). An autosampler and a most accurate dosing system allows up to 48 different probe substances. We usually use 15 different apolar and polar molecular probes to characterize surfaces in its different dimensions. 

A standard IGC characterization (IGC-ID) is done by using different n-alkanes at infinite dilutions to determine the disperse (apolar) surface energy 𝛾sd. Usually, we are adding seven different polar molecules ranging from chloroform to diethylether thereby covering electron acceptor (acidic) and donor (basic) probes. In the example, the customer wanted to characterize the changes of catalysts from fresh to used and the processes of recycling and artificially aging.  The analysis revealed very clearly, that the recycling process is not only far from restoring the original surface properties but also increasing apolar properties far beyond those of fresh or used catalysts. 

The ability to saturate the entire surface at a given p/p0 (IGC-FC) with any kind of probe molecule and to interpret the desorption isotherm in detail was used in a study of zeolites and methanol adsorption. The IGC-FC setup determines the adsorption isotherm, the specific surface area (BET), any irreversible adsorption and the Adsorption Energy Distribution Function (AEDF). The zeolites are very close in performance, but the adsorption of methanol and subsequent desorption revealed significant differences in the amount of irreversible bound methanol and in the distribution of the high energy sites. This way, it enabled a better selection and further optimization of the zeolites for application. 

Also, saturation at a given p/p0 and desorption allows the determination of diffusion coefficients (D) in porous systems. In a setup called Zero Length Column (ZLC), a very small amount of sample is exposed to a given p/p0 and the sudden desorption front interpreted using a ln(c/c0) plot to obtain D by fitting the desorption curve. In the given example, the diffusion coefficients of toluene, cyclooctane and n-octane were determined for two different alumina beads. 
​
These examples show the power of the experimental setup by injecting any kind of volatile probes at different concentrations and accurately determine the physisorption behavior. The IGC framework provides a solid background to determine disperse surface energies but many more values can be obtained, like diffusion coefficients or adsorption energy distribution functions. 

«Yesterday was a very good event!!!! Thanks for all the effort in organizing it!” – something must have been right, when you receive such an email after an event. It was a trial. For the first time, the companies Inolytix and Novitom together with SLS Techno Trans AG, the technology transfer of the Swiss Light Source, organized an event at the Paul Scherrer Institute (PSI). Around 25 people found their way to Villigen and discovered the fascinating possibilities in 3D imaging for industry. 

Stefan Müller, SLS Techno Trans AG, introduced the whole PSI with some facts and figures, namely mentioning the 2100 employees and the 1’400 publications annually. But not only this. For SMEs, there is a special funding available called CALIPSOplus, which provides some (but not all…) services free of charge – a great possibility to try some new analytical tools! For more information see the link at WayforLight.eu. 

The collaboration of Inolytix, Novitom and SLS Techno Trans AG is supporting many of the unknown steps towards an effective and most easy access of companies. This includes efficient project management and reports, which can be used for the management too, as  Ralf Dümpelmann, CEO and founder of Inolytix, explained. 

Many practical examples from different industries as cosmetics, food and composite materials were provided by Barbara Fayard, CEO and cofounder of Novitom. One example was the change of the microstructure of a composite material over time in-situ at 300°C. It becomes clearly visible how the polymer matrix penetrates into the fibres and reduces the porosity to an acceptable level. 
 
Margie Olbinado, a scientist at PSI, explained the differences of microtomography and the nanotomography, as well as ptychographic X-ray nanotomography. The microtomography is very fast within seconds or minutes and objects of a few mm can be measured with resolutions up to 10 micrometers or  1 micrometer, respectively. While the ptychographic nanotomography achieves resolutions down 15 nm but requires beam times of several hours and very small samples. 

Additive Manufacturing, or more easy 3D-Printing, is not easy to optimize in terms of speed. Christian von Burg, CEO and founder of Sintratec AG, an innovative producer of 3D Printers for polymeric structures in Brugg, illustrated, how the microtomography and the 3D imaging helped them to optimize their operating conditions.  How accurately can be measured? This question was answered by Benjamin Bircher in high talk “Industrial high-resolution CT for metrology”.  It was fascinating to learn, that Metas, the Swiss institute for metrology, provides a very solid basis to produce and to measure accurately – definitely a Swiss speciality!

The experimental setups of micro- and nanotomography were in detail explained by the PSI researchers during a fascinating tour through the large hall of the Swiss Light Source, the only synchrotron facility in Switzerland. 
Do you have 3 dimensional objects – and the need to optimize and understand the inner structure? Contact us! We want to make you more successful. 

Visualization in 3D for new insights

Sometimes a good visualization helps to understand the problem. Like an x-ray image or even much better: like an MRI scan - a 3D image of a human brain or a tumor in an organ.

In material science, today's micro- and nanotomography goes a step further in terms of resolution. 3-dimensional structures below one micrometer and even in the nanometer range are possible. The beam lines of the Paul-Scherrer-Institut (PSI) at the Swiss Light Source (SLS) take advantage of extremely coherent x-ray sources and high energy levels. As part of the ETH-Zürich, this federal institute has all the capabilities to produce not only high resolution images, but also high speed images if required. 

Easy access for the Industry
Inolytix is committed to make the use of valuable and innovative analytical techniques as easy as possible for industrial customers. The need of the industry is discussed and translated into actual measurement plans together with the academic researcher. And not only this.

The best visualization requires excellent software and the experience to quantify for example pores and coatings in a stack of many hundreds of images for a full 3D analysis. That is the reason, why we work together with Novitom, a small industry-oriented company in Grenoble, France, with just the right skills for excellent interpretations. 

Discover the possibilities of Micro and Nanotomography on 7th November 2019

You can learn more about the possibilities of Micro and Nano Tomography and 3D imaging at this symposium. It will be held at the PSI in Villigen, where you will visit the SLS and see different analytical methods for 3D analysis and 3D imaging.

When you have questions about your 3D properties, e.g. the inner properties of 3D printed materials, foams or aerogels, cements, ceramics, catalysts or batteries, this symposium will provide you with answers. 

Date:                  7 November 2019
Time:                 13:00 - 17:00
Location:            PSI, Forschungsstrasse 111, 5232 Villigen

When you click on the 'Register' button below, you will see the detailed program.

BASF is using more and more Inverse Gas Chromatography (IGC) to characterize surface properties of particles of batteries, catalysts, building materials and many others. “IGC as a one-fits-all technique gives great – but hardly explored – details” Dr. Matthias Kellermeier, BASF, Material Physics, Ludwigshafen, Germany, summarized it perfectly during his talk “Characterizing complex surfaces of industrial relevance by inverse chromatography”. 

Ten speakers from industry and academia exchanged their experiences with IGC during the 7th International IGC Symposium, 19.06.2018 in Cologne – with participants from 8 countries. The basic principle is quite easy: “15-20 different gas probes are used like AFM-tips to explore the surface properties” Dr. Ralf Dümpelmann, Inolytix AG, Switzerland, explained. “Many polar, apolar, cyclic and branched molecules are used to provide surface energies, nanoroughness, polarities and electron donor and acceptor properties”. Picture: Steven Abbott with results of the discussion group. 

Practices & applications of IGC
However, the practices itself and the applications are very different, as the presentations showed. Dr. Peter Schiffels, Fraunhofer Inst. Bremen, showed the different surface qualities of lignin intended as precursor for bio-based carbon fiber production. Another practice was a good differentiation of industrial TiO2 samples shown by Sven Böhm, Kronos International, Leverkusen. In addition, the effect of different mills and grinding conditions on the mineral attapulgite was explained by Rachel Calvet, Ecoles des Mines, Albi, France. Other speakers provided examples about carbon black particles and zeolites.  

Current limitations of IGC
The principles of IGC as such are very useful, but often there seemed to be limitations in terms of instrumental setup (concentration range, non-symmetric peaks, number of probes) and also controversial methodologies (“nominal” surface coverage treated as “real”, no operation under “ideal diluted” conditions). As a result, the true potential of IGC often seems not fully explored – with BASF as a positive exception, as mentioned above.  

A new, automated and flexible setup
​Therefore, Dr, Eric Brendle, Adscientis SARL, France, complemented this challenge by explaining not only the requirements of an ideal setup but also the advances towards an automated and fully flexible IGC. Controlled and highly accurate syringes for the injection of gases and liquids provide not only “ideally diluted” conditions, but also exact p/p0 settings for desorption isotherms. Altogether an excellent step towards reliable, industrial applications.  

Finally, an interactive session and wrap-up presentations provided everyone a great picture of all the experiences, some limitations and many opportunities. Looking forward to see you next year in June... exact date and location to be announced!