U_MOOC_Countries_of_Participants_2018On Tuesday, March 27, 2018 the web course Estimation of Measurement Uncertainty in Chemical Analysis was launched the fifth time as a MOOC (Massive Online Open Course)!

Currently more than 450 participants from 70 countries are registered! As was the case in the previous years, the majority of participants are from analytical laboratories. This once again demonstrates the continuing need for training in measurement uncertainty estimation for practicing analytical chemists.

The full course material is accessible from the web page https://sisu.ut.ee/measurement/uncertainty. As is usual, some developments and improvements have been made to the course material. in particular, the description of course organisatsion was improved; more explanations and examples were added on random and systematic effects within short and long term; the typical requirements for determining repeatability and within-lab reproducibility have been clearly outlined; more explanations on the main principles of modifying a model in a modelling approach have been given, together with an example. Some changes are still in the pipeline.

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 pass six graded tests and get higher than 50% score from each of tehm. These tests are available to registered participants via the Moodle e-learning platform.

 

LCMS Method Validation online course offered by UTOn Feb 16, 2018 the on-line course (MOOC) LC-MS Method Validation finished successfully.

Altogether 424 (303 last year) people were registered from 71 (61 last year) countries. 236 (224 last year) participants actually started the course (i.e. tried at least one graded test at least once) and out of them 159 (168 last year) successfully completed the course. The overall completion rate was 37% (55% last year). The completion rate of participants who actually started the studies was 67% (75% last year). As can be seen, almost all these statistics are worse than they were the year ago. But then in the last year’s edition both completion rates were all time highest that our group has seen in any of our MOOCs. Thus we probably can be reasonably happy with the completion rates that we have now.

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 and in several cases led to improvements in the course. This active participation made teaching this course a great experience also for us, the teachers! The discussion threads gave a lot of added value to the course and some of them triggered making important modifications to the course materials.

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

We plan to repeat this course again in Autumn 2018.

 

It was the spring of 2011 when I decided to apply to the AMS programme. If I remember correctly, the decision was based on my gut feeling and it was a right one. AMS was related to “perceived” world more than many other programmes in the faculty of science and technology as was also stated in the slogan “bridging the gap between measurements and society”.

5 years after the graduation I am still thankful for taking the journey, and I wanted to remind to myself and to others the three aspects that distinguished the programme from many others.

1) Combination of science and society. If you have the opportunity to combine your own favourite scientific topic (in my case biochemistry and measurement science) with knowledge about requirements related to law, regulations, and standards one has the possibility to give your thoughts a new perspective. It was beneficial for me in the labour market – there are not many people who know both of these aspects simultaneously which makes an AMS graduate a valuable specialist, mostly in private sector, but also in “pure” science. (I am currently working as a quality assurance specialist at Kevelt AS, which is a pharmaceutical manufacturing company in Estonia.)

2) Improvement of communication skills. There was a lot of group work during the studies, which improved my social skills. There is nothing more important than human relations! We had the possibility to study with people from Uzbekistan, Latvia, China, United Kingdom, Ukraine, Jordan, Romania, France, Turkey, and many more. This enabled to study about other cultures, but also how to communicate with people from other cultures.

3) The inspiring (!) lecturers. Their eyes were sparkling when they spoke about their topics so vividly. I believe that people are best at what they really love to do and I aim for the same in my professional career.

I could not thank Prof. Ivo Leito more for such an important contribution to our (students´) lives as leading the AMS programme. He is passionate about what he is teaching and sincerely interested in answering the endless questions, giving us the opportunity to find our better selves in the progress of studies.

 

The_Winning_C_Team_and_the_Baby_Boss_InstrumentThe winner of the student team work of the EACH Winter school 2018 is team C – Snežana Đorđević, Kenneth Arandia, Lydia Man, Mohan Ghorasaini!

They built an instrument for controlling Baby food temperature – the Boss Baby Bottle Sensor. The instrument senses the temperature of a baby food container and indicates with LED lamps whether the temperature is too low, suitable or too high. In the latter case the system runs a fan for cooling the food. Nice instrument and nice presentation!

Baby_Boss_Instrument_in_Operation

 

Photos (Ivo Leito): Up: Kenneth, Lydia, Snežana and Mohan with the instrument and the prize (sweets). Right: Baby Boss Bottle Sensor in operation – cooling a too hot drink.

 

Turbidimeter lab at EACH Winter School 2018

Turbidimeter lab at EACH Winter School 2018

Possibly the most exciting activity at the EACH Winter School 2018 is the teamwork aiming at building some simple instrumentsusing the Arduino Integrated Development Environment (https://www.arduino.cc, see also https://en.wikipedia.org/wiki/Arduino).

The instruments built were thermometer, light intensity meter and turbidimeter (!). All are small and simple, but highly useful devices. The Arduino motherboard is programmed and the obtained data are managed using laptops and a dedicated software. So, instruments can be built at very low cost and virtually everywhere.

 

Measuring with self-made turbidimeter

Measuring with self-made turbidimeter

It is quite a joy to generate analytical data (even if not the most accurate) using an instrument that the student has built his/herself!

Photos (by Ivo leito) show students working in the improvised “instrument manufacturing lab”.

Let there be light! The LED source of the turbidimeter

Let there be light! The LED source of the turbidimeter

Prof_Jerome_Randon_Explaining_Organization_of_EACH_Winter_School_2018On Jan 22, 2018, the third Winter School of the EACH programme started in Valpré (Lyon, France). Altogether 36 students from more than 20 countries participate.

The Winter School offers a diverse set of activities to the participants. There are lectures on advanced analytical chemistry topics (Smart sensors, high-resolution NMR, etc) by top experts, group works and entertainment. Several sessions are presented by practitioners from reserach labs and industry. The intense working is counterbalanced by social activities.

EACH_Lyon_team_explaining_their_thesis_work_and_life_in_LyonTraditionally an important activity in the Winter school is selecting first year students to study tracks. In order to give one more piece of information what the study tracks are about, there was a session of presentations on the first day by second year students on their master thesis topics (see photos).

EACH_Uppsala_team_explaining_their_thesis_work_and_life_in_UppsalaAnother exciting session planned in the Winter school is related to Do-it-yourself activities – building a sensor-based control system prototype and a simple turbidimeter.

EACH_Abo_Turku_team_explaining_their_thesis_work_and_life_in_Abo_Turku

 

 

Full information about the Winter School activities is available at the EACH Winter School web page.

Photos (Jayaruwan Gunathilake): Prof. Jérôme Randon explaining the organization of the Winter School (upmost photo); Groups of second year students from Lyon (up right), Åbo (right) and Uppsala (up left) explaining the life and master thesis work at their universities.

We wish all the participants enjoyable experience!

 

 

Measurements and computations of acidity and basicity of strong and superstrong acids (superacids) and bases in organic solvents is among the core research topics at the UT Chair of Analytical Chemistry. In a recent works (Chem. Sci. 2017, 8, 6964-6973.,    J. Phys. Org. Chem. 2013, 26, 162-170.,    J. Phys. Chem. A 2015, 119, 735–743.,    J. Phys. Chem. A 2016, 120, 3663–3669.) the behavior of a number of acids – ranging from weak to strong and superstrong acids (superacids) was examined in three solvents (water, acetonitrile, 1,2-dichloroethane) and in the gas phase. Acidities (pKa values) of a number of different acids including the well-known superacids trifluoromethanesulfonic (triflic) acid, bis-trifylimide (Tf2NH), etc as well as the carborane superacids (closo-carborane superacids), but also weaker acids (HCl, acetic acid, phenol) etc are examined in the above mentioned solvents. pKa of superacids are not easy to find in literature. Trends of acidity changes on moving from water to the gas phase depnding on the on the nature of the acidity centre and the molecular structure are analyzed. The acidity orders are different in water, MeCN, DCE and the gas phase. In some cases – notably, the hydrohalogenic acids HCl, HBr and HI – the differences are dramatic. These three acids are among the strongest known acids in water but have modest acidity in the gas phase. In contrast, 9‑C6F5‑Octafluorofluorene, a weak acid in water (approximately of the strength of phenol) is quite strong acid in the gas phase, beating any of the hydrohalogenic acids.

It is demonstrated that the decisive factor for behavior of the acids when transferring between different media is the extent of charge delocalization in the anion and that the recently introduced WAPS parameter in spite of its simplicity enables interpretation of the trends in the majority of cases. The acidity data together with references to specific publications are collected in the Table below.

Table of pKa valuesa of acids in different solvents.

 

 

 

 

 

 

Acid

H2O

MeCN

DCEb

GP

GP

 

pKa

pKa

pKa

pKa

GA

 

 

 

 

 

 

Fluoradene

11.1

23.90

12.5

238

324.9

Para-Toluenesulfonamide, 4-CH3-C6H4-SO2-NH2

10.21

26.87

15.6

245

334.0

9‑C6F5‑Octafluorofluorene

10.1

18.88

9.0c

220

300.6

Phenol

10.00

29.14

19.6

251

342.3

(C6F5)2CHCN

9.5

21.10

10.3

229

312.4

C6F5CH(CN)COOEt

5.89

17.75

7.5c

230

313.5

2,4-Dinitrophenol, 2,4-(NO2)2-C6H3OH

4.09

16.66

4.7

226

308.6

(CF3)3COH

5.40

20.55

9.2

238

324.0

Acetic acid, CH3COOH

4.76

23.51

15.5

250

341.1

(4-CF3-C6F4)2CHCN

4.4

16.13

6.0

221

302.1

4-NO2-C6H4-CH(CN)2

2.3

11.61

0.3

220

299.5

Saccharin

1.80

14.57

5.5

232

315.9

Picric acid, 2,4,6-Trinitrophenol

0.40

11.00

0.0

219

299.0

(4-NO2-C6H4-SO2)2NH

<-1

8.19

-3.9c

213

291.1

(CF3SO2)3C6H2OH

-2.0

4.48

-6.6c

208

284.2

(CF3SO2)2NH

<-2

0.3d

-11.9c

210

286.9f

(C2F5SO2)2NH

<-2

-0.10

-12.4c

208

283.7

Cyanoform, (CN)3CH

-5.1

5.1

-6.4c

216

294.8

Triflicid, trifluoromethanesulfonic acid, CF3SO2OH

-14.7g

0.70

-11.3c

215

292.7g

Hydrochloric acid, hydrogen chloride, HCl

-5.9g

10.30

0.2c

241

328.1g

Hydrobromic acid, hydrogen bromide, HBr

-8.8g

5.5

-4.4c

233

318.3g

Sulfuric acid, H2SO4

-9e

8.7d

-2.2c

221

301.2f

Pentacyanopropene

-9.02

-2.80

-15.3c

196

267.2

Hydroiodic acid, hydrogen iodide, HI

-9.5g

2.8

-7.3c

227

309.3g

CB11H12H, unsubstituted closo-Carborane superacid

-25h

-17h

-25f

195

266.5f

B12H12H2, unsubstituted closo-Dodecaborate superacid

-17h

-9h

-17f

196

267.5f

CB11F12H, perfluoro-closo-Carborane superacid

-47h

-39h

-47f

156

212.8f

B12F12H2, perfluoro-closo-Dodecaborate superacid

-45h

-37h

-45f

156

213.4f

 

 

 

 

 

 

a Values from http://dx.doi.org/10.1002/poc.2946 unless noted otherwise. There are numerous comments and details to these values. Please see the original articles for details and comments. GA values are given in kcal mol-1. pKa values in the gas phase are approximate and have been obtained from the GA values by dividing with 1.364 kcal mol-1. b Ion pair pKa values relative to picric acid in 1,2-dichloroethane. c Values from https://doi.org/10.1039/c7sc01424d. d Values from http://dx.doi.org/10.1021/jo101409p. e Value from E. V. Anslyn, D. A. Dougherty, Modern Physical Organic Chemistry, University Science Books, Sausalito, 2006. f Values from http://dx.doi.org/10.1021/jp506485x. DCE values have been recalculated from absolute to relative, in order to be comparable with the rest. g Values from http://dx.doi.org/10.1021/acs.jpca.6b02253. h Crude estimates from DCE data by considering that bulk water is by 53 kcal mol-1 more basic than bulk DCE and bulk acetonitrile is by 42 kcal mol-1 more basic than bulk DCE.

 

(This post was initially posted on Feb 2, 2013. On Jan 15, 2017 a number values in the table have been replaced by more reliable values from more recent publications. In addition, some compounds were added to the in order to give a fuller picture. The changes concern only the table. The image has not been changed and should be viewed as illustrative)

_END_

Huian_Liu_in_lab_with_GC_instrumentThe master theses of the EACH programme have usually high practical value. However, this does not prevent them to lead to cutting edge scientific results.

The master thesis of Huian Liu – EACH 2017 graduate from the Lyon study track – titled Gas separation by high pressure gas chromatography using monolithic columns is a good example. At its core the thesis was devoted to investigating the behavior of monolithic GC columns in separation of small hydrocarbons for achieving high efficiency and short analysis time – an important issue in oil refineries.

As an additional value, however, it involved experimenting with a novel detector – vacuum UV absorption detector (VUV detector). VUV detector is an emerging detector in GC, enabling simultaneous detection, identification and quantitation of analytes.

In chromatography there are detectors of two response types – concentration-sensitive and mass-sensitive detectors. The response type is important in planning separation, and especially in quantitation. As a result of Huian’s work it was firmly established that VUV detector is a concentration-sensitive, not mass-sensitive detector. This result was considered scientifically so significant that it was accepted for publication by the number one chromatography journal in the world – Journal of Chromatography A (!): Huian Liu, Guy Raffin, Guillaume Trutt, Jérôme Randon J. Chrom. A, 2017, 1530, 171–175. Congratulations to Huian and the team!

Huian is continuing his studies as a PhD student at UCBL.

 

(Photo: Huian Liu in lab with the GC instrument)

 

Monika_Sandy_Rudolf_MarkoThis June and September, the first intake of students graduated successfully from the EACH programme (See the graduation blogposts at Uppsala, Lyon and Åbo).

Just few months later, 14 out of our 17 fresh graduates have already obtained positions! Some work in the professional/industrial field, some in academic field. Their jobs range from research assistant at a university to project manager at an international corporation. Several have chosen to continue their studies as PhD students. The reflections of some of our graduates on the programme are here:

Marko_Jovanovic

 

Marko, working as project leader in the Industrial Development at Servier (France), writes:
I have spent amazing 2 years in EACH Programme, that represents a perfect balance between studying and travelling. Throughout this period, we had the opportunity to be educated by the experts in the field of Analytical Chemistry. The study track – Industrial Analysis held in France gave me an important insight into the field that I was not so familiar with before I had the opportunity to spend 6 months of the Programme among well-educated and highly-skilled professionals in the company Axel’One, where I was doing my internship. Since Axel’One is a collaborative research platform, I was engaged in several different projects with different companies. This enabled me not only to enrich my knowledge and skills in applied analytical chemistry, but also to significantly expand my professional network. In the end, I was offered a job in France, within a company Servier, as a Project Lead in the Industrial Development.

Monika

 

Monika, working as research assistant at the University of Exeter (United Kingdom), writes:
The Excellence in Analytical Chemistry program was an extremely valuable experience that increased rapidly the course of my career. Taught by highly competent and respected professors it gives the opportunity to gain all the necessary skills in modern analytical techniques. It has been a pleasant, exceptional experience and honor to be a part of EACH!

Monika is simultaneously pursuing doctoral study at Exeter.

 

Sandy

Sandy, now working in the laboratory of the Akademiska sjukhuset hospital in Uppsala, Sweden, writes:
EACH program was so fruitful. It provided me with the skills needed to kick off my career path by providing a wide range of courses delivered by passionate tutors who really care about your success. Moreover, EACH has wonderful activities like a winter school where you can get knowledge and unforgettable social activities. Thanks to everyone who contributes to the success of EACH!

Rudolf

 

 

Rudolf, now a doctoral student at the Örebro University (Sweden), focusing on analytical chemistry of environmental pollutants, adds:
EACH program exposed us to new (study) environments and without doubt provided an invaluable experience. This project offered me a chance to study a specific field in depth. The obtained skills were crucial for pursuing of third cycle studies. All in all, I got more out of the program than I expected in the beginning.

 

 

The success of our graduates is also the success of the EACH programme! This has also been recognised by the European Commission who has decided to extend the funding of Erasmus Mundus scholarships for the EACH programme.

 

Agnes Heering successfully defended her PhD thesis on experimental realization of the unified pH scale

On December 6, 2017 Agnes Heering, an alumna of AMS, the sister programme of EACH, successfully defended her PhD thesis titled Experimental realization and applications of the unified acidity scale.

Her work literally redefines the way the pH of non-aqueous and mixed aqueous solution is understood and measured. The main focus of the experiments was on validating the measurement approach and measuring the unified pH values, i.e. pHabs values, of HPLC mobile phases (eluents). Her work introduces a conceptually new approach of measuring pH of mixed-solvent liquid chromatography (LC) mobile phases and has been published in the Analytical Chemistry journal: Unified pH Values of Liquid Chromatography Mobile Phases. Anal. Chem. 2015, 87, 2623–2630.

Mobile phase pH is very important in LC, but its correct measurement is not straightforward and all commonly used approaches have deficiencies. The new and fundamentally correct approach developed by Agnes enables direct comparison of acidities of solutions made in different solvents, based on chemical potential of the proton in the solutions.

The work by Agnes represents the first experimental realization of the pHabs concept using differential potentiometric measurement for comparison of the chemical potentials of the proton in different solutions (connected by a salt bridge), together with earlier published reference points for obtaining the pHabs values (referenced to the gas phase) or pHabsH2O values (referenced to the aqueous solution). The liquid junction potentials were estimated in the framework of Izutsu’s three-component method.
She determined the pHabs values for a number of common LC and LC-MS mobile phases and formed a self-consistent pHabs scale. This scale enables for the first time direct comparison of acidities of any LC mobile phases: with different organic additives, different buffer components etc. Agnes has developed a possible experimental protocol of putting this new approach into chromatographic practice and has tested its applicability. She has demonstrated that the ionization behavior of bases (cationic acids) in the mobile phases can be better predicted by using the pHabsH2O values and aqueous pKa values than by using the alternative means of expressing mobile phase acidity. Description of the ionization behavior of acids on the basis of pHabsH2O values is possible if the change of their pKa values with solvent composition change is taken into account.

The defence was successful in every respect. Agnes presented very well, answered questions confidently and convincingly demonstrated to everyone that she is really on top of this whole matter.

(Photo: Agnes Heering and prof. Peeter Burk, the chairman of the defence committee, during defence)