During 24-26.02.2019 the Suprachem 2019 conference took place at University of Würzburg (Germany). The UT Analytical chemistry chair was represented by two posters: Optimization of the reaction pathway for the synthesis of substituted 1,3-bis(carbazolyl)urea anion receptors by Alo Rüütel and Mihkel Ilisson and From receptor-anion binding ladder to ion-selective electrode by Kerli Martin, Sandip A. Kadam, Ulriika Mattinen, Johan Bobacka and Ivo Leito.

The presentation from Alo and Mihkel focused on optimization of the synthesis route of anion receptors (ionophores) based on the 1,3-bis(carbazolyl)urea building block, augmented with additional amide functionalities (see the poster). The developed synthesis route is very valuable for the synthesis of a wide variety of analogous receptors (ionophores) that have previously been demonstrated to bind carboxylates with high affinity (see K. Martin et al, Eur. J. Org. chem. 2017, 5231-5237).

Kerli Martin et al present the first practical application of such receptors: a solid-contact acetate-selective electrodes. For acetate anion the electrodes show linearity over the activity range of 10-4.50 – 10-1.10 with a sub-Nernstian slope of -51.3 mV per decade and a detection limit of 10-5.00. The anion-selectivity pattern of these electrodes deviates markedly from the pattern found in DMSO solution and from the Hofmeister pattern. The selectivity coefficients of SCN, I, NO3 and Br decrease by 3-5 orders of magnitude when adding the studied ionophore to the membrane. The selectivity coefficients of hydrophilic anions such as Cl, F, HPO42–, and SO42– are significantly lower than in case of the ionophore-free control membrane. All in all, it is clear that a lot of work is still needed for improving the selectivity of the electrode.
This work has been accepted for publication: K. Martin et al Electroanalysis 2019 (the link will work soon).

The combined contributions from our group stood out from the majority (the conference altogether had 27 oral and 111 poster presentations) by a clear line of development from fundamental research (receptor design) to highly practical application (ion-selective electrode).

(Photos: above left: Mihkel Ilisson explaining his work to Dr Diane Smith from Wiley; right: Poster by Kerli Martin et al)

 

LCMS Method Validation online course offered by UTOn Feb 15, 2019 the on-line course (MOOC) LC-MS Method Validation finished successfully!
Altogether 426 (424 in 2018, 303 in 2017) people were registered from 70 countries (71 in 2018, 61 in 2017) countries. 227 (236 in 2018, 224 in 2017) participants actually started the course (i.e. tried at least one graded test at least once) and out of them 125 (159 in 2018, 168 in 2017) successfully completed the course. The overall completion rate was 29% (37% in 2018, 55% in 2017). The completion rate of participants who actually started the studies was 55% (67% in 2018, 75% in 2017). As can be seen, almost all these statistics have been getting worse year after year. We are working n analysing the situation. On the positive side it can be said that the completion rates more than 0% of those who started can be considered very good by any measure. Thus we probably can be reasonably happy with the completion rate that we have this time.

As has been the usual case with our online courses, the questions from the participants were often very interesting, often addressed things that are really important to analysts in their everyday work. Such discussions made teaching this course a great experience also for us, the teachers!

We want to thank all participants for helping to make this course a success!

We plan to repeat this course again in Autumn 2019.

 

 

The 2019 edition of the web course (MOOC) Estimation of Measurement Uncertainty in Chemical Analysis will be running during Mar 26 – May 7, 2019. Registration is open!

The full course material (as well as the registration link) is accessible from the web page https://sisu.ut.ee/measurement/uncertainty. The course materials include videos, schemes, calculation files and numerous self-tests (among them also full-fledged measurement uncertainty calculation exercises). In order to pass the course, the registered participants have to take six graded tests and get higher than 50% score in every graded test. These tests are available to registered participants via the Moodle e-learning platform. Participants who successfully pass the course will get a certificate from University of Tartu. A digital certificate of completion is free of charge. A certificate of completion on paper can be requested for a fee of 60 euros.

You are welcome to distribute this message to potentially interested people!

We are pleased to announce that the 2019 Eurachem general Assembly and the scientific workshop Validation of targeted and non-targeted methods of analysis will take place in Tartu!

The Workshop will take place on May 20th and 21st; the General Assembly will take place on May 23rd to 24th. The preliminary programme of the workshop, as well as registration and abstract submission are available at the event website:
https://eurachem2019.akki.ut.ee/

Compact overview of the workshop can be obtained from the First Circular.

The workshop addresses the current status of analytical method validation in general and specifically validation of the non-targeted methods (i.e. ones where the analyte is not defined beforehand). Non-targeted methods are an especially noteworthy part of the programme, because their validation involves specific issues (since analyte is not known it is not possible to make validation experiments with it) and their validation is significantly less developed than validation of targeted methods (i.e. the “normal” analytical methods, where the analyte is known beforehand). At the same time non-targeted methods are becoming increasingly important in environmental protection, food safety, different omics areas, etc.
Some example topics of the workshop are: Validation of targeted methods: where are we? Validation of non-targeted methods – differences from targeted methods. Detection of a multitude of (unknown) components in complex samples: criteria for identification. Managing the huge amounts of complex data from non-targeted methods. Software solutions for validation.

These events also mark the 30th anniversary of Eurachem.

These events are jointly organized by Eurachem and ECAC (University of Tartu, Tallinn University of Technology and the Estonian Environmental Research Centre).

 

Recently the Analytical chemistry group of University of Tartu participated in a cutting-edge research endeavor: characterizing the acidity of some extremely efficient strongly acidic organocatalysts. In the case of the Mukaiyama aldol reaction the best of them (1) worked at low ppm to sub-ppm level, (2) gave excellent yields and (3) high enantiomeric selectivity as well as (4) turnover numbers (TON numbers) of hundreds of thousands (Nature Chemistry 2018, 10, 888-894).

The extent to which these four features occurred together in the same catalyst was so remarkable that the results were published in one of the most prestigious journals in chemical sciences: Nature Chemistry.

The extremely demanding acidity measurements were performed by Dr Karl Kaupmees using the unique non-aqueous acid-base chemistry facility that the group is running. The whole research project was led by the group of professor Benjamin List – a worldwide known guru in the field of strongly acidic catalysts working at the Max-Planck-Institut für Kohlenforschung.
These results are expected to open new avenues in development of powerful new organocatalysts.

(Photo by Andres Tennus: Karl doing acidity measurements in a glovebox under anhydrous conditions)

Validation_of_LC-MS_Methods_Online_CourseIn one week – on Nov 27, 2018 – the online course LC-MS Method Validation will start again! Registration is still open at the address https://sisu.ut.ee/lcms_method_validation/!

Whoever is interested, please hurry!

The course will run during Nov 27, 2018 – Feb 08, 2019.

This is a practice-oriented on-line course on validation of analytical methods, specifically using liquid chromatography-mass spectrometry (LC-MS) as technique, mostly (but not limited to) using the electrospray (ESI) ion source. The course will also be of interest to chromatographists using other detector types. The course introduces the main concepts and mathematical apparatus of validation, covers the most important method performance parameters and ways of estimating them. The course is largely based on the recently published two-part tutorial review:

The course materials include lectures, practical exercises and numerous tests for self-testing. In spite of being introductory, the course intends to offer sufficient knowledge and mathematical skills for carrying out validation for most of the common LC-MS analyses in routine laboratory environment. The real-life analysis situations for which there are either examples or self-tests are for example determination of pesticides in fruits and vegetables, perfluoroalkyl acids in water, antibiotics in blood serum, glyphosate and AMPA in surface water, etc. It is important to stress, that for successful validation practical experience – both in analytical chemistry as such and also specifically in validation – is crucial and this can be acquired only through hands-on laboratory work, which cannot be offered via an on-line course.

Participation in the course is free of charge. Receiving digital certificate (in the case of successful completion) is also free of charge. Printed certificate (to be sent by post) is available for a fee of 60 EUR. Registration is possible until the start of the course. The course material is available from the above address all the time and can be used via web by anyone who wishes to improve the knowledge and skills in analytical method validation (especially when using LC-ESI-MS).

 

Today, On Nov 16, 2018 the General Conference on Weights and Measures (CGPM) unanimously decided to fundamentally remake the SI system of measurement units. Perhaps the most important change is that the kilogram will not be defined via a physical artefact – the platinum-iridium cylinder – but in terms of the Planck constant. As a result, for the first time the entire SI system will be defined entirely on the basis of fundamental constants, which has been the aim for decades!

The change will become effective on the 2019 World metrology day – May 20, 2019.

More information can be found in the post CGPM votes unanimously to change the SI by Dr Steve Ellison at the Eurachem website.

(Image: Wikipedia)

 

On Nov 05, 2018 Ivo Leito gave a presentation Unified pH about the pan-European research network of fundamental pH Research UnipHied (www.uniphied.eu) at the 7th Baltic Electrochemistry Conference organized by the University of Tartu.

The presentation started with explaining the need for the experimental realization and measurement capability of unified pH (pHabs). Thereafter the current state of art of measuring pHabs values was described and finally some first exemplary results were highlighted.

The presentation created a lot of interest from the participants and roughly as many questions were asked as for the other four presentations of the same session put together!

As of now, it is not possible to compare pH values of solutions made in different solvents, as every solvent has its own pH scale. This situation is highly unfortunate, since it causes confusion and inaccuracies into many fields, extending far beyond the specific field of acid-base chemistry. Examples are industrial catalytic processes, food chemistry, liquid chromatograpy, etc.

The central aim of the UnipHied network is to establish at international level measurement capability of pHabs values that would be applicable also at routine laboratory level. The two key activities for achieving that are creating a reliable method for the experimental or computational evaluation of the liquid junction potential and between aqueous and non-aqueous solutions and developing a coherent and validated suite of calibration standards for standardizing routine measurement systems in terms of pHabs values for a variety of widespread systems (e.g., industrial mixtures, soils/waters, food products, biomaterials).

The partners of the UnipHied network are LNE (France, coordinator), BFKH (Hungary), CMI (Czech Republic), DFM (Denmark), IPQ (Portugal), PTB (Germany), SYKE (Finland), TÜBITAK-UME (Turkey), Freiburg University (Germany), ANBSensors (United Kingdom), FCiencias.ID (Portugal), UT (Estonia, initiator).

UnipHied is funded from the EMPIR programme (project 17FUN09) co-financed by the Participating States and from the European Union’s Horizon 2020 research and innovation programme.

 

On Oct 26, 2018 Ivo Leito gave a presentation titled Analytical chemistry education activities at University of Tartu at the EcoBalt 2018 conference in Vilnius (Lithuania).

The presentation contains information about the on-line courses LC-MS Method Validation and Estimation of Measurement Uncertainty in Chemical Analysis, as well as the recently published tutorial reviews (Validation I, Validation II, LoD I, LoD II) that form the basis of the LC-MS Method Validation course.

The presentation also addresses the international master’s programmes Applied Measurement Science and Excellence in Analytical Chemistry at University of Tartu.

The last part of the talk is devoted to the Eurachem 2018 General Assembly and Workshop that will take place in Tartu on May 20-21, 2018. The topic of the workshop is “Validation of targeted and non-targeted methods of analysis”.

 

Validation_of_LC-MS_Methods_Online_CourseWe are glad to announce that the third edition of the online course LC-MS Method Validation is open for registration at the address https://sisu.ut.ee/lcms_method_validation/ !

The course will be offered as a Massive Open On-line Course (MOOC) during Nov 27, 2018 – Feb 08, 2019.

This is a practice-oriented on-line course on validation of analytical methods, specifically using liquid chromatography-mass spectrometry (LC-MS) as technique, mostly (but not limited to) using the electrospray (ESI) ion source. The course will also be of interest to chromatographists using other detector types. The course introduces the main concepts and mathematical apparatus of validation, covers the most important method performance parameters and ways of estimating them. The course is largely based on the recently published two-part tutorial review:

The course materials include lectures, practical exercises and numerous tests for self-testing. In spite of being introductory, the course intends to offer sufficient knowledge and mathematical skills for carrying out validation for most of the common LC-MS analyses in routine laboratory environment. The real-life analysis situations for which there are either examples or self-tests are for example determination of pesticides in fruits and vegetables, perfluoroalkyl acids in water, antibiotics in blood serum, glyphosate and AMPA in surface water, etc. It is important to stress, that for successful validation practical experience – both in analytical chemistry as such and also specifically in validation – is crucial and this can be acquired only through hands-on laboratory work, which cannot be offered via an on-line course.

Participation in the course is free of charge. Receiving digital certificate (in the case of successful completion) is also free of charge. Printed certificate (to be sent by post) is available for a fee of 60 EUR. Registration is possible until the start of the course. The course material is available from the above address all the time and can be used via web by anyone who wishes to improve the knowledge and skills in analytical method validation (especially when using LC-ESI-MS).