Eligible authors at German institutions may publish open ... · 3, 2020. A 4hour workshop in which...

56 13

2

VOLUME 24MARCH

2020

1

Your accepted OA article is then published under a Creative Commons license on Wiley Online Library.

Corresponding authors who submit their work from participating Projekt DEAL

institutions may:

• Publish research articles in Wiley gold OA journals without charge to authors

(beginning 2019)

• Publish OA in Wiley hybrid journals without an author fee (from 1st July 2019)

Projekt DEAL and Wiley have partnered to support institutions and researchers

to advance open research, drive discovery, and develop and spread knowledge.

• Eligible authors at participating German institutions may publish OA and benefit from

full reading access to Wiley’s journals

• Authors from Projekt DEAL institutions may publish primary research and review articles

OA in Wiley journals, and retain copyright of their works, at no charge to the author

• All Projekt DEAL institutions have access to read Wiley’s academic journals back

to the year 1997

19 - RM000125

Eligible authors at German institutions may publish open access (OA) and benefit from full reading access to Wiley’s journals

If you have questions on your OA publishing eligibility, reach out to us: [email protected]

For more information and to check eligibility, visit: bit.ly/DEALAuthor

Another Year - So What’s New?For me it apparently becomes a tradition to write the first editorial of the year about things that have changed. Change is necessary, but only seldomly easy. So, please find below an update of things that have happened so far and a preview of things to come.

New Website - New Look and Feel

The last year has brought about quite a change for the G.I.T. Laboratory Journal. For those who are subscribers to our newsletter, you will have noticed that the layout has changed and that the online presence has moved to a new home named analyticalscience.wiley.com. The new webpage unifies the resources of SeparationsNOW, SpectroscopyNOW, Imag ing & Micrcoscopy, Microscopy & Analy sis, and G.I.T. Laboratory Journal. That way the users can find the information in one place, rather than having to scout several sites. If you haven’t looked at the site yet, please do so now and I am sure you will enjoy the new layout.

Less Issues - More Focus!

For the G.I.T. Laboratory Journal in print, we decided to publish 4 issues this year. We will have a stronger focus on the special topic of the magazine (Spectroscopy in this issue). The next focus topics are Chromatography and Separation, Laboratory IT & LIMS, and Laboratory Equipment. I am confident that this selection of

topics reflects what you as readers want to see in our publication.

Meet us at the Fair!

This year we will also be at selected conferences and trade fairs, starting with Pittcon, which will unfortunately be already over when you get this issue. Due to the uncertainty introduced by the COVID19 outbreak, I am somewhat hesistant to write about where our team will be present. We are monitoring the situation and hope the fairs will not be cancelled. I have planned to be at the Paperless Lab Academy. The rest of our schedule is not yet fixed, but we will keep you updated as to where you will be able to meet us in person.

Mini-series “Digital Laboratory”

During this year, we will also have a miniseries about Digitalization in the laboratory. The emphasis will be put on things that are already on the market and things that have been implemented. However, to add a little spice, there will also be a few ‘science fiction’ scenarios. As always, we will offer a mix of authors from the industry and academia so you can get the most complete picture about what’s what in the field.

Is that all? - Not quite yet!

One last thing: We have created the Wiley Analytical Science Award. This award is

for new and innovative products and solutions. We will have a jury of experts from the field who will select a shortlist of all entries. Then, we hand this shortlist over to a very diverse and unbiased, as well as very critical jury, namely you, the readers. Once the shortlist has been selected, you will have the opportunity to cast your votes. Then the three winning entries in each category are presented with the award. The deadline for the submission of your product or solution is April 30th, 2020. For all further informations, including the web based submission tool, please refer to this website: https://www.pro4pro.com/en/specials/was_en.html

Dr. Martin Graf-UtzmannEditor-in-ChiefG.I.T. Laboratory Journal

www.hahnemuehle.com

Protect what matters

Food & BeverageEnvironment Diagnostic

The OriginalFilter Papers since 1883

Meet us atAnalytica 2020

stand 323hall A2

Magazine

The Bot on the Bench 24Cooperative Robotics and the Routine LabT. Teutenberg et al. Cobots in the Analytical Laboratory 26Useful Tool or Gadget?K. Thurow

Chemical Syntheses Molecular Electronics 28Building Organometallic Chains Molecule by Molecule A. Vladyka et al.

Mass Spectrometry European Proteomics Infrastructure Consortium – Providing Access 32A European Proteomics InitiativeM. O’Flaherty

Identification of the Fluorescent Photoproducts 36Analysis of Two Phenylureas by Photo-Induced Fluorescence (PIF) and GC-MSP. A. Diaw et al.

ProductprofileYMC: Innovative UHPLC/HPLC Solutions for BioLC 39

ShowcaseWITec: Find, Classify and Identify Microparticles 40

Products 40

Index/Imprint Inside Back Cover

Cover StoryMisa – A New, Portable Food Analysis System 12Protecting Consumers with the Latest in Food Testing Technology

SpectroscopySingle Cell Technologies in Modern Core Facilities 14Complementary Technologies Are Underpinning Single Cell ResearchD. Davies et al.

The Epigenome: Illuminated One Cell at a Time 16Using scATAC-Seq to Study the Impact of Epigenetic VariationK. Simonyi

UV-Vis and FTIR Instruments in Regulated Environments 18An Innovative Solution for Molecular SpectroscopyJ. Hesper

Multivariate and Multiway Calibrations 20What Analytical Chemists Would Ask From Aladin’s LampA. C. Olivieri

Laboratory Automation The Digital Laboratory 23A Short IntroductionM. Graf-Utzmann

EditorialAnother Year - So What´s New? 3M. Graf-Utzmann

Events Paperless Lab Academy 6

News 7

Read & WinGenomic Approaches in Earth and Environmental Sciences 9G. Dick

20 Minutes 10

Congratulation!

The winner of Read&Win issue 4/19 is T. Garrett from Newberry, Florida.

The winner of Read&Win issue 5/19 is S. Gunstrup from Denmark.

The next prize draw is on page 9

A human’s inherited DNA sequence remains relatively consistent across healthy cells throughout life. But over time, epigenetic modi-fications accrue and influence the way those genes are expressed and, in turn, how the cells function. The challenge with understanding how these changes impact human develop-ment and disease is that there is no single epi-genome to decode – it differs across individual cells. Below we discuss the technological ad-vances that are now allowing scientists to piece together the impact of epigenomic modifica-tions at a single-cell level and at scale.

More on page 16

Preview Issue 2/20Coming out 27th May, 2020

Special: Chromatography & SeparationTopics: Mass Spectrometry, Omics, Food

Magazine Articles Marketplace

Spectroscopy

©A

rtem

Gor

ohov

- st

ock.

adob

e.co

m

4

Contents

G.I.T. Laboratory Journal 1/2020

Good Products deserve an Award –our Wiley Analytical Science Award.

Do not think twice, submit now!Where? was-award.com

Until when? 30th April 2020

Who? Every company whose product from the laboratory sector convinces with an innovative approach.

We are looking for the best products or solutions within the following categories:

A – SpectroscopyB – Lab AutomationC – SeparationD – MicroscopyE – Lab Equipment

Your Contact: Isabel Brenneisen [email protected]+49 6201 606 716

APPLYNOW!CLOSING DATE

APRIL 30, 2020

was-award.com

© K

zeno

n - s

tock

.ado

be.c

om

WileyAnalytical

ScienceAward

Foster Digital Revolution in your LABThe Paperless Lab Academy is ready to run its 8th European Edition, supported by more than 25 laboratory solutions and services providers.

Once again, the stage is set for discussions on strategies and implementations of 21stcentury technologies for your laboratory and quality processes. The program is an agile combination of future horizon views already running in some industries and tangible real users’ cases on how to solve today’s concerns.

Along with keynotes speakers from different industries sharing their digital transformation experiences, 15 interactive workshops and enjoyable networking sessions are planned.

A training opportunity on vendor selection and risk management is also offered on the precongress day, Wednesday June 3, 2020. A 4hour workshop in which Mr. Mark Newton will take you through his best practices in software implementation and as such in vendor selection management. Mark brings his 35 years of experience in the pharmaceutical industry in QC Labs, computer systems validation and lab informatics at Eli Lilly. The Paperless Lab Academy, owned and organized by industry domain experts, is the ideal learning platform for all companies that own a laboratory, involved in run

ning, consolidating, integrating or simplifying scientific data management and laboratory processes.

»At the Paperless Lab Academy, We Challenge the Status Quo.«

Keynote speakers and solutions providers are very vocal about the fact that companies should really consider investing in exploiting the quality data for performance evaluation, in stimulating process improvements and in simulating scenarios that may lead to predictive quality.

From Keynotes to Interactive Work-shops, These Topics, Among Others, Will be Covered:

▪ Rapid transfer of raw data to a shared environment in the cloud allowing the immediate use of this data at all levels

▪ Easier integration of any laboratory instruments through the Internet of Lab Things #IoLT to complete traceability of sample management and full data integrity compliance

▪ How Standard formats are simplifying the use and access to the data, even in GxP environments.

▪ Big Data being the new state of the evolution and Artificial Intelligence the real

driver to predictions, recommendations, classification and automatic recognitions.This new concept is destabilizing the organizations, not only IT departments which were focused on process enablement but also laboratories and R&D departments that are trying to learn how to embrace this new concept.

▪ The use of structured and unstructured data in realtime which is quickly replacing the use of oldfashion approaches to evaluate and solve “afterthefact” problems. This approach will allow the use of largely underutilized data to predict rather than correct. It is also changing attitude at all company levels and real case studies will be presented at the PLA2020.

▪ Broad ELN and LIMS implementation project

The Paperless Lab Academy 2020 is your place to be for answers relating to those topics and discussion with those who have already gone through it.

Everything you always wanted to know about Scientific Data Management, Laboratory Informatics, Paperless Processes and latest news from the industry.

Announcement

Registration https://www.paperlesslabacademy.com/registration

6 News

Wiley Science SolutionsHelping laboratories build abetter future

sciencesolutions.wiley.com

Advantages of using a Wiley spectral library in thetoxicology field

Positively identifytrace compounds

Seamless integration Create efficient workflows

Complete both untargetedand targeted analysis

ISBN: 978-1-119-41223-6 ISBN: 978-3-527-34685-1 ISBN: 978-3-527-34327-0

Secrets of the Foot Many of us take our feet for granted, but they have a challenging job in the bio-mechanics department. When we push off with the ball of the foot, the force we apply exceeds our body weight, causing the middle of the foot to bend. Yet the foot maintains its shape be-cause it is stiff enough to withstand this force. Re-searchers have long de-bated what gives the mid-foot its stiffness. Now, a new study, published in Na-ture, has shed light on the importance of a little-studied structure called the transverse arch (TA), which runs across the foot. The researchers theorized that the TA contributes even more to this effect, much like how rolling a floppy piece of paper makes it harder to bend. Using a protocol developed with the help of computer simulations, and experi-ments on plastic and mechanical models, the researchers found that about half of the stiffness in human cadaveric feet is controlled by the TA.Original publication: https://bit.ly/GLJ0120-N1

Clever Pathway to Branched OlefinsHydroformylation, or oxo synthesis, is an industrial process for obtaining aldehydes from olefins. Current catalytic processes yield both linear aldehydes, which are key in-termediates for the detergent and polymer industry, and branched ones, which are

considered a powerful tool for the fine chemical industry because of their possible use in producing enantioen-riched products, that is, products fea-turing a greater proportion of a given enantiomer of a chiral substance. The researchers first screened several catalytic conditions to maximize the yield of the branched product that could be obtained with homogeneous catalysis. They then showed how they could go beyond this limit and achieve much higher branched selectivity by adding MOFs to the reaction mixture. They also tested different MOF topolo-gies to understand the role of the MOF environment in such a change in selectivity. The group was able to show that the mi-cropores of MOFs push the cobalt-catalyzed hydroformylation of olefins to kinetic re-gimes that favor high branched selectivity, without the use of any directing groups. The addition of MOFs allowed branched selectivity of up to 90% in these cases, a feat that cannot be achieved with existing catalysts.Original publication: https://bit.ly/GLJ0120-N2

New Subtype of SchizophreniaPenn Medicine researchers are the first to discover two distinct neuroanatomical subtypes of schizophrenia after analyzing the brain scans of over 300 patients. The first type showed lower widespread volumes of gray matter when compare to healthy controls, while the second type had volumes largely similar to normal brains. The findings, published Thursday in the journal Brain, suggest that, in the future, ac-

The longitudinal arch has been well studied when it comes to foot stiffness, but this research found that the transverse arch may be more important.

© O

IST Micropores of MOFs with certain topo-

logies increase the density of the ole-fins while partially preventing the ad-sorption of the synthesis gas.

© @

PSI

Magazine


counting for these differences could inform more personalized treatment options. Schizophrenia is a poorly understood mental disorder that typically presents with hallucinations, delusions, and other cognitive issues - though symptoms and re-sponses to treatment vary widely from patient to patient. Up until now, attempts to study the disease, by comparing healthy to diseased brains, has neglected to ac-count for this heterogeneity, which Davatzikos says has muddled research findings and undermined clinical care. Original publication: https://bit.ly/GLJ0120-N3

Gut Microbe Could Cause CancerCancer mutations can be caused by common gut bacteria carried by many people. This was demonstrated by researchers from the Hubrecht Institute (KNAW) and Princess Máxima Center in Utrecht, the Netherlands. By exposing cultured human mini-guts to a particular strain of Escherichia coli bacteria, they uncovered that these bacteria induce a unique pattern of mutations in the DNA of human cells. This mutation pattern was also found in the DNA of patients with colon cancer, implying that these mutations were induced by the ‘bad’ bacteria. It is the first time that researchers establish a direct link between the microbes inhabiting our bodies and the genetic alterations that drive can-cer development. This finding may pave the way to prevention of colorectal cancer by pursuing the eradication of harmful bacteria. This study may have direct implications for human health. Individuals may be screened for the presence of these genotoxic bacteria; it is reported that 10-20 percent of people can harbor the ‘bad’ version of E. coli in their intestines. Antibiotic treatment could eradicate these bacteria early on. In the future it may be possible to catch colorectal cancer development very early or to even prevent tumors from developing.Original publication: https://bit.ly/GLJ0120-N4

Believing in Conspiracy Theories Could Increase Non-Normative ActionsConspiracies abound in society and can have real world impacts when it leads some people to act, whether that means becoming more engaged politically, or less engaged. Previous research linking conspiracy beliefs and political actions provide mixed results. Some studies show people with a conspiracy worldview are more likely to disengage politically, while others show they are more engaged. The re-searchers conducted two experiments, one in Germany (194 people) and another with Mturk workers based in the United States (402 people). In both experiments, people were assigned to imagine being in a particular type of society. Some were assigned a conspiracy-focused description that suggested a few powerful groups controlled the fate of millions, others read an intermediate scenario where people wondered if the media and politicians could be trusted, and another group read about a world view that governments and the media were trustworthy and trans-parent. Each person was then asked a set of follow-up questions about what politi-cal actions they’d be willing to engage in, from “normative” actions like voting, participating in rallies, or contacting media or politicians, to “non-normative” ac-tions such as destroying property, harming others, or other illegal behaviors. In both studies they found people who were presented with a high conspiracy scenario were more likely to engage in the non-normative political actions than those pre-sented with a low conspiracy scenario. Political engagement for normative actions.

Was higher for those reading about low conspiracy scenarios compared to the other two groups.Original publication was not yet available at the time of printing. It is pub-lished in the Journal: Social Psychological and Personality Science

Quantum Entanglement

The CAS key lab of quantum information makes a significant progress in quantum ori-enteering. Researchers enhanced the performance of quantum orienteering with en-tangling measurements via photonic quantum walks. Thanks to quantum entangle-ment, quantum information processing is much more efficient than its classical counterpart in many tasks, like quantum computation, quantum communication, quan-tum metrology, and so on. Quantum entanglement can manifest itself in both quantum states and quantum measurements. On contrast to the extensive research of entan-gling states, there are few experimental studies of entangling measurements because entangling measurements are difficult to realize. Their work demonstrated a truly non-classical phenomenon that is owing to entanglement in quantum measurements in-stead of quantum states. Meanwhile, it offers an effective recipe to realizing entangling measurements in photonic systems. These results are of interest not only to founda-tional studies of quantum entanglement and quantum measurements, but also to many applications in quantum information processing. Original publication: https://bit.ly/GLJ0120-N5

Social Media and Vaccine Scepticism in ChinaIn July 2018, Chinese government inspectors determined that Changchun Changsheng Biotechnology, a prominent manufacturer of vaccines in China, had violated national regulations and standards when producing 250,000 rabies vaccine doses. The violation might have undermined the effectiveness of the involved vaccines. News began slowly escalating on Chinese social media platforms not long after the incident. Researchers have analysed the impact social media had on the debate. They warn about the dan-gers of public perception of even a single vaccine safety incident. The team also be-lieves the possible emergence of vaccine opposition in China is a potential cause for concern, especially considering the density of several large Chinese population centers.Original publication: https://bit.ly/GLJ0120-N6

Ultrasonic Attack on Siri and GoogleUltrasonic waves don’t make a sound, but they can still activate Siri on your cellphone and have it make calls, take images or read the contents of a text to a stranger. All without the phone owner’s knowledge. However, new research from Washington Uni-versity in St. Louis expands the scope of vulnerability that ultrasonic waves pose to cellphone security. These waves, the researchers found, can propagate through many solid surfaces to activate voice recognition systems and, with the addition of some cheap hardware, the person initiating the attack can also hear the phone’s response. The team suggested some defense mechanisms that could protect against such an attack. One idea would be the development of phone software that analyzes the re-ceived signal to discriminate between ultrasonic waves and genuine human voices. Changing the layout of mobile phones, such as the placement of the microphone, to dampen or suppress ultrasound waves could also stop a surfing attack. Their final hint is to put the telephone on a tablecloth to filter out the Ultrasonic waves.Original publication: http://bit.ly/GLJ0120-N7

© P

enn

Med

icin

e

Schematic diagram and experimental setup for optimal orienteering with parallel and antiparallel spins.

© T

AN

G J

unfe

ng e

t al

.

8 News

Magazine


Other book presentations: https://bit.ly/WAS-RNW

What is your main focus in research, what is your main scientific interest?The main focus of my research is on how microorganisms influence their environment, ranging from questions about how and why they produce toxins that are a concern for the health of drinking water and ecosystems, to understanding the history of Earth’s oxygenation through the lens of microbial mats that are functionally analogous to those that were prevalent in deep geological time. Much of my research draws on “omics” approaches – genomics, transcriptomics, proteomics – to track the activities of these microorganisms as they exist in communities in the environment.

What was the reason to write the book?The field of environmental omics has emerged and advanced very quickly. The goal of this book was to provide a reference and a starting point for researchers who wish to get familiar with this field.

What is the target audience for the book?Microbiologists and geoscientists in academica, industry, and government agencies who want to learn about this rapidlyemerging field.

What knowledge is prerequisite for the book?Basic microbiology and/or earth and environmental sciences.

What is the structure of the book?The book is structured to first provide an overview of the applications of omicsbased approaches to the earth and environmental sciences, as well as background on the architecture of microbial genomes and the ecological and evolutionary forces that shape it. Then the book goes through the various omics approaches, including metagenomic assembly and binning, functional annotation, metatranscriptomics and metaproteomics, and downstream approaches.

What is the - in your opinion - most surprising discovery?Geomicrobiology has provided many surprising discoveries in the past few decades. To me the most surprising is the staggering diversity of microorganisms in the environment – most organisms in the environment have not been cultured, and contain genes of unknown function. Thus there is a preponderance of microbial “dark matter” that is poorly understood, and plenty of room for discovery in the future!

Also available in electronic formats

Gregory J. Dick

Dick, G.Genomic Approaches in

Earth and Environmental SciencesSeries: Analytical Methods in

Earth and Environmental Science2018.

Hardcover.ISBN: 978-1-118-70824-8

Genomic Approaches in Earth and Environmental SciencesThe past 15 years have witnessed an explosion of DNA sequencing technologies that provide unprecedented insights into biology. Al-though this technological revolution has been driven by the biomedical sciences, it also offers extraordinary opportunities in the earth and environmental sciences. In particular, the application of “omics” methods (genomics, transcriptomics, proteomics) directly to environmental samples offers exciting new vistas of complex microbial communities and their roles in environmental and geochemical processes. Genomic Approaches in Earth and Environmental Sciences begins by covering the role of microorganisms in earth and environmental pro-cesses. It then goes on to discuss how omics approaches provide new windows into geobiological processes. It delves into the DNA se-quencing revolution and the impact that genomics has made on the geosciences. The book then discusses the methods used in the field, beginning with an overview of current technologies. After that it offers in-depth coverage of single cell genomics, metagenomics, metatran-scriptomics, metaproteomics, and functional approaches, before finishing up with an outlook on the future of the field.

is an Associate Professor in the Department of Earth and Environmental Sciences at the University of Michigan. He is a geomicrobiologist, mean-ing that he studies how organisms influence their environment. He current focus in on (i) production of toxins by cyanobacteria in lakes and (ii) under-standing controls on oxygen production in cyanobacterial mats.

Win

this

book

see p

age 1

0

Read & Win 9

Magazine


© pict rider - Fotolia.com

Weird Science

Happy birthday to you and washing hands

☛ The Center for disease control in the US has published a guide that shows how to wash your hands

correctly. This may sound odd, but there are things that can and usually do go wrong. I, for one, did not

know that humming the “Happy Birthday” song twice while scrubbing the hands is a good timer for the

20 seconds needed for proper cleaning. Further details (including the science behind it all) can be found

under this link:

https://bit.ly/GLJ0120-WS1

Smile, you’re on camera!

☛ A team of scientists have deployed a large number of camera traps in the Bukit Barisan Selatan

National Park in Sumatra. They detected 39 species, including such endangered species as the Sumatran

tigers and Sunda pangolins. The original publication can be found here:


Super urinating fish and the mangrove

☛ Researchers from the University of Michigan have tracked tropical fish in a mangrove estuary on the

Bahamas. Their analysis shows that the most active individuals of the grey and cubera snappers provided

disproportionally large amounts of Nitrogen (in the form of Ammonia). Subsequent simulations showed

that the Nitrogen introduced by the two snapper populations is roughly equivalent to all other Nitrogen

sources. The study was published in Science Advances.


Web-Tip!Monty Hall and the GoatThere are probably not too many people out there that have not come across the so-called Monty Hall Problem. The simplified descrip-tion is the following: The player is presented with three doors, behind two of which there is a goat. Behind one door is the great prize: a car. After the first choice, the host of the ga-me-show opens one of the doors that were not chosen and presents the player with the choice to change the original choice or to stay with it. Which strategy is more likely to get the main prize? Here is a link to a simulating tool that lets you try and find out. Have fun with this one!

https://bit.ly/GLJ0120-MH

Read and Win!To have a chance of winning the book find the origi-nal figure in this issue from which the image below is taken. Send the title of the article to [email protected] with the subject Read & Win!

All correct answers will be entered in a prize draw and the lucky winner will receive a copy of “Ge-nomic Approaches in Earth and Environmental Sciences”, which is featured on page 9.

Closing date: May 6th, 2020

10 20 Minutes

Magazine


Look closely is the task in this puzzle. We manipulated the right image. Find all eight mistakes we have hidden for you. Send the image with the marked errors to [email protected] with subject line “Picture Puzzle”. Among the correct submissions, the lot decides the winner of a small sur-prise. Closing date is 6th of May, 2020. !Picture Puzzle

Sudoku! Fillomino!

ww

w.c

raus

wor

th.c

om

ww

w.c

raus

wor

th.c

om

©skypicsstudio - stock.adobe.com

20 Minutes 11

Magazine


The Basics of SERS

SERS is a Raman spectroscopic technique that transforms moderately sensitive Raman spectroscopy into a trace analytic method. The discovery of SERS in 1977 was a serendipitous result from attempting to observe Raman spectroscopy from monolayers of molecules adsorbed onto roughened silver electrode surfaces. To date this initial discovery has expanded to surfaces as variant as free floating

nanoparticles to sophisticated nanomachined silicon structures. Regardless of the surface state of the material, SERS results from special optical properties of silver and gold and the size of the surface structures.

The SERS effect stems from a unique property of these particular metals that, unlike other materials, create a resonance with the electric field of the laser light and the Raman scattering. This resonance creates large electric fields at the

metal’s surface that enhance Raman scattering by as much as 107. The electric field enhancement is located only at the surface of the SERS active materials. This is an important limitation to the technique the target material must be extremely close (< 3 nm) to the surface. Generally, nitrogen and sulfur containing compounds are the strongest materials to adsorb to these noble metals and exhibit the greatest SERS effect. Fortunately nitrogen and sulfur containing compounds includes most food adulterants and most active pharmaceuticals (legal and illegal).

The SERS effect can be summarized by: ▪ Million plus fold enhancement of Ra

man signals due to nanostructured surfaces.

▪ Selective adsorption of materials at these surface.

This combination creates a useful technique of trace sensitivity for food contaminants.

Misa – A New, Portable Food Analysis SystemProtecting Consumers with the Latest in Food Testing Technology

Industrial dyes used in brightly colored candies, pesticide residues on fruits and vegeta-bles, pharmaceuticals illegally added to herbal medicines - Contamination of food prod-ucts is a global problem, whether it is done intentionally for profit or accidentally through negligence, the end result is the same – consumers pay the price. The problem of food contaminations can be addressed with complex analytical laboratory techniques such as GC-MS and HPLC, but time, skill, and cost requirements limits their usage to the confines of well-equipped laboratories. Surface Enhanced Raman Scattering (SERS) – an extension of Raman spectroscopy - permits detection and identification of analytes in concentrations as low as parts per billion. Food analysis with SERS can be fast, con-venient, and inexpensive.

12 Advertisement

Cover Story


Advantages of SERS over Tradi-tional Trace Analysis Technologies

Food samples are normally a complex matrix consisting of proteins, fats, starches, sugars, and many other materials. Contaminants – when presented, are usually at trace levels. Analytical techniques that carry the claim of “trace” detection inevitably involve separation of the analyte from an overwhelming matrix. Terms such as part per million (ppm) or part per billion (ppb) can be easily understood when related to populations of people. A part per billion means that you can find a single person in a country of one billion. To a chemist this is a doable challenge – in less than an hour! But what does it require to make these measurements?

The key is to use features of the target analyte to distinguish it from its matrix. This concept of separation lays the foundation to differentiate various trace analytical techniques and leads to the advantage of SERS.

Mass spectrometry is the most common trace analytical technique. The name mass spectrometry stems from its ability to identify materials through their molecular mass. For example, the fungicide Thiram has a molecular mass of 240.42. However, if a dilute sample of Thiram in a solvent is placed in a mass spectrometer, the more abundant solvent will hinder the detection of Thiram. As a result, mass spectrometric methods require a separation method prior to the analysis. This is most often a chromatographic method such as gas chromatography (GC), liquid chromatography (LC), or Ion Mobility Spectrometry (IMS). These separation methods require time and skill to produce the separation. For example, GC requires a column of material that selectively adsorbs the matrix materials and passes the analyte. This can require up to 30 minutes for a separation and detection. Faster separations are achievable with methods like IMS, but then the detection can be very limited to a small class of materials.

SERS detection also involves separation. But in this case the separation occurs much faster as the analyte adsorbs to the nanostructured surface. SERS can determine in seconds that a specific material is present. SERS identification of a molecular fingerprint is equivalent to the identification of a mass fingerprint and in the case of chemical isomers it is superior. SERS is an extremely attractive technique as it retains all of the appealing features of Raman – portable equipment, multianalyte detection capabilities, and rapid analysis.

Misa to the Rescue!

Misa from Metrohm is a dedicated instrument for performing SERS measurements. It was developed with the focus for a simple, efficient and green testing solution to address food safety threats. Easily swappable attachments allows flexibility of testing using different types of SERS materials. Metrohm also provides targeted ID Kits that include test materials as well as detailed stepbystep instructions for measurement of common contaminants in various food matrices. The advantages at a glance ▪ A mobile app provides simple, intui

tive, guided workflows ▪ Automated analysis quickly and accu

rately identifies trace contaminants ▪ Intelligent mobile platform enables re

mote sharing of results, location, and hazard alerts

▪ Dedicated applications to inform sample analysis methods

User Groups of Misa and Different Use Scenarios

With these advantageous in mind, Misa is an excellent mobile platform for the rapid identification of food contaminants at the point of sample.

Usage Scenario #1 – Mobile Food Inspection Laboratories

Food inspectors play an important role in securing the safety of consumers. At every point along a food supply chain, there is potential for fraud and contamination. The ability to detect harmful contaminants and additives immediately means that no time is lost before vital information about the substance can be shared

and immediate steps can be taken by public authorities to protect consumers.

Usage Scenario #2 – Inspection of Incoming Raw Materials and/or Finished Products

At a food processing facility, raw ingredients e.g. agricultural produce, may be sourced from several different farms. The ability to quickly verify that the incoming materials are free of contaminants or adulterants can reduce factory down time and wastage. Similarly, products can be quickly inspected atline during manufacturing to ensure no accidental introduction of contamination. In both of these situations, rapid and efficient detection technology like Misa can lead to significant cost savings for the business.

Usage Scenario #3 – Preliminary Analysis in a Traditional Laboratory

While Misa cannot replace a “gold standard” analysis instrument like GCMS in a wellequipped lab, it can work in tandem with these traditional analysis technique to speed up laboratory workflow. A positive presumptive result using the Misa can help guide the laboratory scientists to configure settings on more resource intensive instruments to specifically confirm analytes of interest, cutting down on analysis time, reducing wastage of reagents and saving on valuable resources.

ContactDr. Wei YuMetrohm [email protected]

Advertisement 13

Cover Story


The explosion of information that can be derived for specifically defined cells has great possibilities in biomarker discovery, therapeutic intervention and personalised medicine.

But to determine the function, genotype, and phenotype of an individual cell, it is essential to integrate several technological approaches. No one approach will fit all as it may depend on whether simple single cell information is needed (suspensionbased methodologies) or whether there also needs to be a relational aspect i.e. the context of the cells in a tissue (tissue or slidebased methodologies). This allows to gain a greater understanding of the complex nature of cells reactions to stimuli, cell to cell interactions and cell fate.

Cells are still identified based on some a priori knowledge of the cell system and its response to, for example, drug treatment. True discovery needs a high throughput mode that is not present in most of the single cell technologies discussed here. There are a number of techniques available and the one used will depend on the question asked and, more and more, researchers rely on integrated results from several approaches.

Suspension Technologies

Flow cytometry is a wellestablished technique that uses fluorescence (labelled antibodies, fluorescent probes or proteins) to enable researchers to specifically identify subpopulations within a heterogeneous population. It has been established for almost 50 years and has been embraced particularly by the field of immunology. The ability to measure structural parts of a cell (protein, DNA, RNA) and cell function (pH, calcium flux, apoptosis) on a cellbycell basis makes it an extremely powerful technology. Additionally, any subpopulation identified by its fluorescence characteristics may be retrieved using a cell sorter. Sorted cells may be passaged,

transplanted, put into functional assays or may be subject to downstream genetic, proteomic or metabolomic analysis.

Flow cytometry is still considered to be the gold standard of high parameter single cell analysis technologies [1]. Throughput is high – 10k/second is relatively easy to achieve, but can be high cost given the amount of reagents needed. Currently, it is not easily possible to examine more than 30 parameters per cell which can be limiting and challenging in looking at highly heterogeneous populations. Cells have traditionally been sorted using electrostatic drop deflection but given the high pressures often used, low pressure microfluidics system such as the Miltenyi Biotec Tyto or the Cytonome microfluidic sorter can have advantages where subsequent functional studies are dependent on cells being as little stressed as possible. Single cell sorting for subsequent genomic, transcriptomic or proteomic analysis is also possible using an electrostatic drop deflection cell sorter.

Recently suspension mass cytometry (Fluidigm Helios) which uses metaltagged antibodies to identify cells of interest has emerged. Although throughput here is slower, the number of analytes is increased compared with flow cytometry so allowing even greater subdivisions of heterogenous populations.

Also, in recent years, imaging flow cytometry has allowed the positional information of fluorescence and the shape of cells to be captured as well as whole cell

fluorescence. This is especially useful when looking for translocation or localisation of fluorescence, and because it is flowbased also allows thousands of cells per second to be analysed making it suitable for rare cell analysis.

Tissue Based Assays

Most single cell suspension approaches do not reveal spatial information either at the subcellular level or between cells as they need to be disaggregated. The Laser Scanning Cytometer was introduced in the late 1990s as a way of deriving subcellular information from single cells on a substrate, and recent iterations of this technique has been used to analysis tissue sections but have a limited number of targets. To address tissue cytometry needs, in recent years there has been an expansion of new techniques each with their own advantages, that are compatible with standard tissue sectioning techniques i.e. cryopreserved or formalin fixed paraffin embedded (FFPE), material which is critical for their adoption.

Nanostring Digital Spatial Profiling (DSP) can analysis tissue sections using a panel of either antibody or oligonucleotide probes that are marked with unique photocleavable oligonucleotide identifiers. Regions of interest down to a single cell are targeted with UV light releasing identifying oligonucleotides, which are collected and identified using either a multicoloured fluorescent bar code system (up to 800 plex) or next generation sequencing (NGS) (kilo plex).

The Akoya Codex system can analysis tissue sections using a panel of antibodies that are labelled with an oligo duplex with unique 5’ overhangs. Antibody identity can be determined using iterations of single base extension to sequential identify oligo duplexes from the panel. Three antibodies can be identified per iteration by the addition of fluorescent nucleotides and their

Single Cell Technologies in Modern Core FacilitiesComplementary Technologies Are Underpinning Single Cell Research

▪ Derek Davies1, Grant Calder2, Peter O’Toole2

Being able to make measurements on a single cell level allows us to link genotype, phe-notype and function. Several single cell technologies exist and there is now more of a need to integrate several of these into an analysis workflow. The complementary nature of flow cytometry, single cell sequencing and genomics platforms allows researchers to make more measurements than ever before. However, to do this knowledge of the ad-vantages and disadvantages of each approach is vital especially as there is, of neces-sity, more of a link-up between these technological approaches.

Fig. 1: Looking at cell division using the Amnis ImageStream. Using a combination of Propidium iodide staining (for DNA; red) and mpm2 staining (for mitotic cells; green), it is possible to identify cells in prophase (upper panel), metaphase (middle panel) and anaphase (lower panel)

14 Spectroscopy

Special Topic


location within the section captured using standard fluorescence microscopy. Fluorescent dye molecules are then removed before the next iteration of extension and labelling. Antibody identity is determined by the iteration number and colour.

There are also techniques where the sequential labelling of tissue sections with fluorescent tagged antibodies (3 to 5 different colors) is performed in a single iteration. Images are captured using standard fluorescence microscopy followed by the removal or deactivation by photobleaching of fluorescence tags before the next labelling iteration. Zellkraftwerk ChipCytometry mounts a sample in a special flow cell that allows the exchange of solutions and Miltenyi have recently launched the MACSima system.

Hyperion mass cytometry system (Fluidigm) can be used to analyse sections with a panel of up to 40 different antibodies each coupled with a unique metal tag that are not common in nature giving very low background. A scanning laser beam is used to ablate the sample causing the release of particles that are carried by a stream of inert gas into a mass spectrometer for identification. This technique is capable of subcellular resolution down to 1 µm.

With Nanostring technology, conceptually thousands of different proteins or RNA can be labelled simultaneously, but not with subcellular detail. Whereas both Codex and ChipCytometry approaches can yield subcellular information, their iterative approaches requires significantly longer processing time, limiting the total number of targets and are dependent on image analysis software to identify cells and their labelling signatures. Tissuebased mass cytometry (Hyperion) is less susceptible to background noise but requires specialized equipment and currently is limited in the total number of targets. In many tissuebased techniques there is a need to identify

individual cells using algorithms to separate cellular information from background allowing segmentation of single cells.

The Future

There is always a compromise – ideally, phenotype, function and positional information are wanted. No one technique does all of that to the same level of information/resolution, so prioritization may be necessary depending on the biological question being asked.

The challenges in the era of highdimensional techniques are in data analysis as directed analysis is no longer possible. More and more operational pipelines have been published in general involving preprocessing of samples to remove unwanted and/or spurious events, this will be differ

ent with each methodology. Data analysis of highly multiplexed samples is a challenge and there is an increasing involvement of clustering or dimensionality reduction algorithms used in flow, imaging and mass cytometry data, although this has been common in sequencing for some time.

However, it is clear that emerging technologies such as those described here will be the driver in addressing tissue heterogeneity in health and disease.

Affiliations1The Francis Crick Institute, London UK2Bioscience Technology Facility, Department of Biology, University of York, UK

ContactDr. Peter O’TooleDirector of the Bioscience Technology FacilityUniversity of YorkYork, [email protected]

More on Flow cytometry: https://bit.ly/WAS-Flow-Cyt

References: http://bit.ly/GLJ-Davis

Fig. 3: Dimensionality reduction of a 35-metal panel using tSNE within the Phenograph package.

Fig. 2: Data generated using the Hyperion Imaging mass cytometry system Human tonsil was stained with 35 differently labelled antibodies. False-color ima-ging of 4 of these is shown. Smooth muscle actin (red), CD31 (green), DNA (Blue) and CD45RA (Cyan). Left panel is slide overview, middle panel is zoomed in and right panel is after cell segmentation using Ilastik and Cell Profiler – this then allows quantitation of signal at the single cell level.

Spectroscopy 15

Special Topic


Understanding how epigenetic mechanisms drive cellular differentiation and disease requires a nuanced map of the epigenome. Various modifications can alter the epigenome, such as histone modification, methylation, nucleosome positioning, proximity to other coregulated genomic regions, higher order chromatin structure, and nuclear positioning. Until recently, the study of epigenomics relied heavily [1] on assays that focused on specific areas of the genome, as well as bulk assays, which capture an average of the total modifications in large groups of cells. However, because every cell in our body has a unique epigenome that changes over time, the narrow scope and resolution of these assays makes them unsuitable to make a detailed map of the epigenome.

Now, new developments in singlecell technology, namely singlecell assay for transposase accessible chromatin (scATACseq), have enabled scientists to map the epigenomes of entire tissues and organs at a single cell level. Their research is cataloging how different cell

types come together to form functioning organs and is uncovering new cell types along the way.

The Link Between Cell Function and Epigenetics

The presence or absence of a gene isn’t the only factor dictating whether or not a gene expressed. When DNA is tightly packed in the form of chromatin, the genes within are under or not expressed. Epigenetic modifications are what dictate the level of chromatin packing, rendering genes accessible or inaccessible to the cell’s transcription machinery. This, in turn, impacts cell behavior and function (phenotype).

At times, epigenetic modifications decrease how much a gene is expressed by blocking transcription machinery. They can also amplify expression so that a cell is producing much more of that given gene than neighboring cells. The unique mosaic of epigenetic modifications within a cell helps regulate how much of every gene gets transcribed into RNA. Once

transcribed, that RNA can either be translated into a protein or serve an enzymatic or structural function within the cell.

Mapping the Epigenome With scATAC-Seq

From cell to cell, there are enormous epigenetic differences that evolve over time. We need single cell tools to study this heterogeneity; to understand why populations of cells are different, and how they function in the context of an entire organism. Ideal for this task, scATACseq enables scientists to examine individual cells within large populations simultaneously. The goal: build a complete map of the epigenome. With such a map, scientists could chart the epigenetic features of specific cell types throughout development. They could create a catalog of pathogenic epigenetic markers associated with disease. But to understand how scATACseq works and how it could be used to generate such a “cell atlas,” we must first understand its parent method, ATACseq.

ATACseq was not designed to provide single cell information. Instead, it offers a snapshot of the average epigenetic landscape of hundreds to thousands of cells. Research published by Jason Buenrostro in 2013 in Nature Methods [2], describes the development of ATACseq. Compared to other common epigenetic methods – such as MNaseseq, DNaseseq, and ChIPseq – ATACseq requires fewer cells per

The Epigenome: Illuminated One Cell at a TimeUsing scATAC-Seq to Study the Impact of Epigenetic Variation

▪ Kristopher Simonyi

A human’s inherited DNA sequence remains relatively consistent across healthy cells throughout life. But over time, epigenetic modifications accrue and influence the way those genes are expressed and, in turn, how the cells function. The challenge with un-derstanding how these changes impact human development and disease is that there is no single epigenome to decode – it differs across individual cells. Below we discuss the technological advances that are now allowing scientists to piece together the im-pact of epigenomic modifications at a single-cell level and at scale.

© Ja

ck M

oreh

16 Spectroscopy

Special Topic


sample and can be completed in a single day. During ATACseq, a hyperactive transposase mutant known as Tn5 binds to open regions of genomic DNA, cutting the bound DNA and ligating NGS adapters. After end polishing and PCR, ATAC fragments are sequenced to discern regions of open chromatin. The information derived from ATACseq indicates where in the genome transcription factors generally bind and where nucleosomes are typically positioned. It gives a sense of the average epigenetic state of a population of cells.

While useful in the lab, ATACseq does not have the singlecell resolution necessary to map the epigenome. Working out of Harvard, Buenrostro developed a technique using microfluidic technology to segregate individual cells before conducting ATACseq [3]. This resulted in the scATACseq method, published in Nature [4] in 2015. The microfluidic technique isolates hundreds of individual cell nuclei, then the Tn5 transposase tags open chromatin regions with sequencing adapters. Next, the open chromatin library is amplified with cellidentifying barcoded primers. After amplification, discreet libraries – each representing a different cell – are pooled and sequenced to reveal open regions in the genomes of individual cells.

Profiles of the open chromatin regions of thousands of cells can be generated from a single scATACseq experiment. The results represent a range of epigenetic variations throughout the population, which can be used to compare individual cells and classify different cell types within the sample. The results can identify epigenomic markers distinct to a specific cell type and can indicate that cell type’s relative frequency within the sample tissue.

Through scATACseq experimentation, scientists from numerous disciplines have uncovered new insights into complex diseases, such as autoimmune disorders, various cancers, and neurological disorders like Alzheimer’s, Huntington’s, schizophrenia, and Parkinson’s. But for a deeper understanding of epigenetic phenomena, researchers needed a way to evaluate more cells per experiment. In collaboration with Buenrostro, Ron Lebofsky at BioRad Laboratories and Caleb Lareau at Harvard University achieved this by developing two techniques [5] that expand on the original scATACseq method. Driving both is a fundamental shift from the use of microfluidics to isolate

nuclei to a more scalable dropletbased technology (Fig. 1).

Their first new version of scATACseq (dscATACseq) was named for its use of dropletbased technology along with a single cell isolator to prepare a library of thousands of nuclei for sequencing. Each nucleus is held within an individual nanolitersized droplet. dscATACseq offers alterations in the workflow, such as a custom, hyperactive transposase, to improve signal resolution and enhance library complexity. The dropletbased workflow is also faster, simpler, and more scalable than the original microfluidic method. With these improvements, scientists get highquality results while spending less time conducting each experiment. Taking advantage of dscATACseq’s expanded capabilities to generate data for large numbers of cells, researchers performed an unbiased analysis that cataloged the different regulatory elements and cell types within an adult mouse brain.

Lebofsky and Lareau then went a step further by introducing combinatorial indexing to the dscATACseq workflow, creating a new dsciATACseq method. In this approach, hyperactive mutant transposases integrate a first set of barcodes, into accessible chromatin regions as they are cleaved. These barcodes make it possible to differentiate between cells, even when several are encapsulated in a single droplet. Because of this, a larger quantity

of cells can be processed in a given dsciATACseq experiment. During subsequent amplification, DNA fragments are tagged with a second set of barcodes. Using this combinatorial indexing approach, researchers can generate highresolution chromatin accessibility profiles of as many as 50,000 cells per sample. Thanks to the colossal scope of the dsciATACseq assay, researchers have been able to study changes in the chromatin accessibility landscape in immune cell clusters across cell types at singlecell resolution. In one application, this depth of insight into the epigenome helped reveal the overall effects of different stimulation conditions on human bone marrowderived cells.

Conclusion

With an estimated 37.2 trillion cells making up the human body [6], tools with massive scalability are needed to generate a high resolution cell atlas. Tools like scATACseq fulfill this need, equipping researchers to decipher the epigenome for a greater understanding of how biological systems work and how to best treat complex diseases.

ContactKristopher SimonyiGlobal Marketing Manager, Digital Biology GroupBio-Rad Laboratories Pleasanton, CA, USA [email protected]

Related Articles: http://bit.ly/WAS-Epigenetics

References: http://bit.ly/WAS-Simonyi

Fig. 1: For scATAC-seq, droplet-based technology is used to partition thousands of nuclei or whole cells into individual nanoliter-sized droplets to facilitate library preparation for ATAC sequencing.

Spectroscopy 17

Special Topic

mailto:[email protected]


Data Integrity Compliance for Spectroscopy Systems

Compliance with data integrity requirements is already a demanding issue for companies that require GxP compliance. In addition to LC and GC systems, regulatory authorities have turned their attention to spectroscopy systems such as UV and FTIR spectrophotometers. Just to mention a few: MHRA (Medicines and Healthcare products Regulatory Agency)[1], FDA (U.S. Food and Drug Administration)[2] and WHO (World Health Organization)[3].

This increased attention to data integrity is based on repeatedly detected irregularities – ranging from carelessness to deliberate manipulation with intent to deceive. Auditors expect active proof that no improper actions have been taken with regard to analysis results.

This approach corresponds to a policy that punishes any practice which even appears to be suspicious, and represents a break with previous approaches. When deficiencies are found during an FDA audit, they are not only reported to the company being audited, but also published on the FDA website in socalled “warning letters”. The number of warning letters has

increased almost tenfold in the last 56 years.

So the question arises: what level of compliance is required to ensure the integrity of data from spectroscopy systems?

Obstacles to Ensuring Data Integrity Compliance for Spectroscopy Systems

As illustrated in figure 1, compliance is based on Good Manufacturing Practice (GMP), which requires validation of systems and analytical methods. Furthermore, data, audit trail (metadata) and user operations must be timestamped correctly in a secure environment. When a laboratory has both chromatography and spectroscopy systems, the elements shown in figure 1 apply to both such that compliance with data integrity requirements results in the operations indicated in Table 1.

Typical systems retain audit trail data (metadata) within the spectroscopy data acquisition system as indicated in Table 1, but cannot manage spectroscopy and audit trail data in a unified manner. This means that data cannot be managed in a linked state. The same applies to the user management. Typical systems cannot manage both data management users and data acquisition users in a unified manner.

UV-Vis and FTIR Instruments In Regulated EnvironmentsAn Innovative Solution for Molecular Spectroscopy

▪ Johannes Hesper

A current issue of analytical data is often the lack of data integrity due to data modifica-tion and replacement. Regulatory authorities for analytical instruments are interested not only in chromatography systems such as liquid chromatographs (LC) and gas chromato-graphs (GC), but also spectroscopy systems such as UV-Vis and FTIR systems. Conse-quently, many analytical laboratories urgently consider how to ensure data integrity for spectroscopy systems in an efficient and economical way. Innovative software solutions combine different analytical instrument categories into one management system to sim-plify and to harmonize validation processes, GxP* data or even disaster recovery policies.*) GxP refers to all guidelines for “good working practice”, which are particularly impor-tant in medicine, pharmacy and the pharmaceutical chemistry.

© Jack Moreh, freerangestock.com

18 Spectroscopy

Special Topic


Due to the attention on data integrity, focus has shifted towards provision of evidence to reviewers that no improper operations were performed with respect to analytical results. However, this approach represents a policy of punishing any practice that appears suspicious, which is a major departure from the approach used in previous investigations[4]. This approach applies to both chromatography and spectroscopy systems, meaning the conventional approach cannot be used to ensure appropriate compliance.

Advantages of a Unified Software Platform

Considering that data integrity compliance for spectroscopy systems could present a major obstacle for operating analytical laboratories in a regulated environment, there is a need for an innova

tive approach to ensuring data integrity that solves such problems.Reasons for one software platform: ▪ One software to learn ▪ One software to manage ▪ One software to update

Summary

Management of different instrumentations like UVVis, FTIR, RF, ICPMS, chromatographic, or TOC equipment etc. with one common software platform enables addressing of compliance issues in a univocal way, by having a single log. Harmonized procedures and immediate traceability of the data as well as a simple and quick consultation of the event register are highly valuable during inspections or audits. Finally, one software solution is easier to administrate, maintain by ITdepartment and handle by operators.

ContactJohannes HesperShimadzu Europa [email protected]

References: https://bit.ly/WAS-Hesper

Fig. 1: GMP - data integrity requirements

Typical Innovation

Equipment Chromatography Spectroscopy Chromatography and Spectroscopy

Data Acquisition Yes - Yes Yes

Data Management Yes Yes - Yes

Audit Trail Yes - Yes Yes

User Yes - Yes Yes

Security Yes Yes Yes Yes

Time Stamp Yes Yes Yes Yes

Remarks 3x Systems to manage 1x System to manage

Tab. 1: Typical data integrity in laboratories having chromatography and spectroscopy equipment like FTIR, UV-Vis or RF next to LC or GC systems.

THIS IS NOT A CHILLER AD.

ThThThThThThThThThThThThTThThTTThTTThTThhhisisisisisisisisissisisisssiss iiiiiiiiiiiiiiiiiiiiiiiisssssssssssssssssssssssss anananananananannnnnnnannnnnaannnnnanananaananaan aaaaaaaaaaaaaaaaaaaaaaaaddddddddddddddddddd fofofofofofofofofofofofofofofofofffofofoff r.r.r.r.r.r.r.r..r.r.r.rr.r.r.r..rr.....................................SiSiSiSiSiSiSiSiSiSiSiSiiiSiSSimpmpmpmpmpmpmpmpmpmpmpmpmmpmpppmmpmmpmpllillilililililililiillililliiillililiicicicicicicicicicicicciciciccccccciccc tytytytytytytytyyyytytytyytytyytytyytyytyttttyyy,,,,,,,,,,, bebebebbebebebebebebebebebebeb cacacacacacacacacaccccaacacac usususususususususususususususussu e ee ee e e e e eeeeeeeee

yoyoyoyoyoyoyoyoyoyoyooyyoyoyoooyyoyoyyyy ururururururururururururururururuurururrru jjjjjjjjjjjjjjjjjjjjoboboooobobobobobbbboboboobobobobobbobboboboboboo iiiiiiiiiiiiiiissssssssssssssssssss cocococococcococooccococcccccoccooc mpmpmpmpmpmpmmpmpmpmpmmpmpmpmpmpmpmpmpppppppppplilililililllllliilliliil cacacacacacacacaacacacacaaaaac tetetetetetetettetetetteteteed d d ddddd dd enenenenenenenenenenneneenennennououououououououououououououououuoooooouo ghghghghghghghghghghghghhghghghhghhghghhghghggh.......

NoNoNoNoNoNoNoNoNoNoNoNoNoNoNoNNoNoNoNoNoNoNooNoNoNoNoNoNNoNNooooNooNNoN mmmmmmmmmmmmmmmmmmmmmmmmmmmmmororororororoororororororororooororrorrorrrorrororro e ee e e eeeee eeeeeee ee eeeeeee prprprprprprprprprprrprprpprprprpprprpprprpprprprprpprprpprprprprpprrppppppppp evevevevevevvevevevevevevevevevevevevevevvve enenenenenenenenenenneneenenneneenennennntatatatatatatatatatatatatatatatatattattaaaatititititititittititiittititittttittitititivevevevevevevevevevevevvvevevveveevvvvvvaiaiaiaiaiaiaiaiaiaiaiaiaiaaiaiaiaaiiiiiiiir r rr rrrrrrrrrrrrrrrr r r rrr fifilfilfilfififilfilfilfilfilfilfifilfilfilfifilfilfilfilfilfifififilfifilfilfifififififilfififififififififififi tetetetetetetetetetetetetetetetetetetttetettettttt r rr r r rr rrrrrrrrr rrrrrrrrrr mamamamamamamamamamamamammmamamamamamamammmammmmamaamamammmmmmmmmm inininininininininnninnninnnnininniinnnnninnnnnnnnnntetetetetetetetetetetteteetetetetteeteteteetteteteeteeettttenananananannanannnanannananananananaannaanan ncncncncncncncncncncncnccncnncncncncnnnnnnnnceeeeeeeeeeeeeeeee

OurOurOurOurOurOurOurOurOurOuOurOuOurOurOurOurOurOurOurOurOOurrrOurrrOOOuOO neneneneneneneeeneenenenenenenneneeeneeneeew Dw Dw Dw Dw Dw Dw Dw Dw Dw Dw Dw DDw Dww DDDw Dw Dw DDynaynaynaynaynaynaynaynaynaynaynynynaynayynynnaynaynayyyyyyyyyy micmicmicmicmicmiccmicmicmicimicmicmicmicmicmicmicicmicmicmicccmiccccFFFilFFFilFilFiFilFilFilFilFillFiFillFFFFF lFiFFiF terterterterterterterereretertertertertertertereeeeerrrtee ™ S™ S™ S™™ S™ ™ S™ S™ S™ S™ S™ ™ S™ S™ S™ S™ ™™™™ S™ SSS™ SS™ ™™ S™™ Systysttystyystystystystyststystystttyststtyyy tyststtem em ememem em em m em em ememm mmmemmmmmemmmmmmmmemmmmmemmmmmmme is is is is is sis s iss issisisepreprepreprepreprepreprereeepreprpreeprep erepppprerpp propropropropropropropprorororororooproprroroproprpropprroooproop gragragragraggragragrararagragraragraggraragg aagggg mmemmemmemmemmmmemmemmemmemmemmemmemmemmemmemmemmemmemmmmeemmemmemmmeemmemmmeeeeem d td td td td td td td td td td tdd td td ttd td ttd tttdddd tooo co co co co co co co co co coo co coo co coooooo hanhahhanhanhanhahananhanhanh nhaanhanhanhhanannnh nha gege ge gege ge eeege ge eegegeggeegegeeege ee thethethethetheththehethethethethethehethetheththehehethehet ethet e aiaiaaiaiaiaaaiaaaiaiaiiaiaiaaiiir fir fir fir fir fir fir fir fififir fir fir fifir fifir firr firr fififiltelteltltltlteltelteltelteltetltetetetttettt rr rrrrrr rrr

autautautautautautauauaautautauautautautauttautuauauauututomomomaomomaomaomamamaomaomaomaomamaaaaomaomaaomaomaamaaaaaoooooomaooooooo aticticticticticctictictictictictictictict cttttt callallallallallallallalalallalallallalaalllaalally oy oy oy oy oy oy oy oy oy oy oy oy ooyyyy oy y oy oyy oy oy ncencencencencencencencencencencencennncncen e pepepepepepeppepeppepepepppepepeppepepppppeepepp r mr mr mr mr mr mr mr mr mr mr mr mrr mr mr mrrr mr montontontontontontontontontontontontontontonontontontontontonontntontntttontnoontontth ohh oh oh oh oh oh oh oh ooh ooh oh oh ooh h oh oh oh h ooverververververveveververververerveerverververrverveverrrverveevevvev rreer aa a aa a aa aaatwotwotwotwotwotwotwotwotwowowotwotwowtwotwotwowowotwowwowowwtwowtwottt oott yeyeyeyeyeyeyeeyeyeyeyeyeyeyeyeyyyeyeeearar arar ar ar ar rar ar arrar perperperpereerperperrperperpperppepperperppereeerpp iodiodiodiodiodiododoodiododiodiodiododdoodii dddi d ananananananananananananaannaa d cd cd cd cddd cd cd c d cd d cd cd cdd cd cccd ananananananananananananannnanann bebebebebebebebebbbebbbbbebebebbbbebbebebebeebeeeeee adjadjadjadjadjdadjadjadjadjddadjadjadjadjadjadjadjadjadjadjadadjdaadjadjaada jjustustustustustusttustustustustusustttustustustttuustusustustuus ed ed ed ed ed eded ed edededdedededed ed eedeedededddeedededddetototototototototottottooto uisusuisuisuisuisuisuisuisuusuiussuisuiusuuisu t y yt yt yt yt yt yt yt t yt yt yt yt t yt yyyyourourourourourourourourourououourroururuurururururouou opopopoopooopopopopopopopopopoopopperaeraeraeraeeraeeraeraeraeraeerararaeeraerraeeee aereeree atintintintintintintintintintintintintttinnnttitini g eg eg eg eg eg eg egg eeg eg eg g eg eg eg eg eg eg eg egg nvnvinvinvinvinvinvvnvnvnvvnvinvinvnvinvivivnnvvvnvvnvvinvvviv ronronronroronronronrononronronronoronronronronronronrononnononrrronronronnronmenmenmenmenmenmenmenmenmenmenmenmenmenmemenmenmenememmenmenmeneenmenmmenm t.t.t.t.t.tt.ttttt.ttt.t..t...t.........ThiThiThiThiThiThihiThiThhihThiThihihhihThiThihThThhhh s ws ws ws ws ws ws ws ws ws ws wws wwwwss wwwws wwww lillillillillillilllillilillillillillillillllilliii l rerererererereeerererereerereerrelielielielielielielieliellielielielielieelielielieeilieelieeei ve ve ve veeve veve vevveveve ve vvevvevevvvvvvvve youyouyouyoyouyouyouyouyoyouyouyouyyouyouyouyouuyyououuyyouy uou ofofofofofoofofofofofooofoo thththththththththttththhtt e be be bbe be be e e e bbe be be be e bbe bbe urdurdurdururdurduurdurdurdurdurdurdurdrdrdurddduurdddr en en eeen enenenen en n en neneeneneneeeeeeeeenennenenn ofof of ofof of of of of of ffofof oofof ofoooofoof o prepreprepreprepreprepreprepreprepreprepreepppreprevenvenvenvenvenvenvevenvenvenvenvvenvvvvveenevennveev tattattattattattattattattattatattatatatattatatatt iveiveiveiveiveiveveveveveveivevevvevevvvvee aiaiaiaaiaiaiaiaiaiaaaaaaair fir fir fir fir fir fir fir fir fififififififirr filteltelteltelteteteltel eeltelteltetetet r mr mr mr mr mmr mmmmr mr mr mmmainainaiainainainaiainainainainaaiaaiaaa tentetentententetententtetetentettetetenteenteneeneneneneneeneeteeeeteeeeee ancancancancaanancancancancancananccancancncnnnnn e ae aee ae ae ae e ae ae ae aee ae e aeee e nd nd ndnddnd ndnd ndndnndndnelielielielielielielielelieleleeeeee minminminminminminminmimiminmmimminminiminmminm aateateateateateateteteateteteateeateteeeaaaaaaat dododododododododododdododododododdoddddodd wntwntwntwntwntwntwntwnntwntwntwnwntwntwntwntttttttntwntwnttntwntnwnnw imeimeimeimeimeemeimememeimeimeimiiimeimeiimeiimmeimeimemeem frfrfrfffffrffrfrfrfrfffffrfrfffffrrffrfrfrffrfrrfrfrrrff omomomomommomomommomomomomommmo unnunnunnunnunnunnunnunnnnunnnnnnnnnnunnunnunnun eceeceeceeceeceecececeececececeecececececcccccceeceececcceceececceceeceececccceeceeeeec ssassassassassasssssassassassassaassssas asss ry ry ry ryryry ry ryry ry ryry ryry ryy yyysersersersersesersersersersersesersesereserrserrses rrerrvicvicvicvvicvicvicvicvicvicvicvicvicivivicvvicvvicvv cvice ce ce ce ce ce e ce cee ce ce cee ce e e ce cce e ccccallallallallallallallalallallallallalllallalllalaalaallallaal s ds ds ds ds ds ds ds dss ds ds dds s s ue ueue ueuue ue ue ue e uueeeee tototototototototototototottttto impimpimpimpimpimpimpimpmpimpmpimimimppmimmpimmpmmmmmmmmmmmmmpropropropropropropropropropropoopppopropropoproppppppppppppoppppper er er er er er ererer reeerreereereremaimaimaimaimaimamaimaimaimamaimamamamamaimaammam ntentententententententntententntentententenntenttenten ennn enannannannannannannannnannannannannannannnnannnannanannnnce.ce.ce.ce.ce.ce.cecece.ce.e.cce.eeceeee.eee.eeee

DuraChill®

Changing the world of Chillers...again.

Visit us! Hall B2, Stand 217

Spectroscopy 19

Special Topic


Classical analysis is a straightforward twostep process: (1) calibration using pure analyte standards, which renders the calibration model (slope and intercept of a calibration line), followed by (2) analyte quantitation in unknown samples, interpolating its signal in the calibration line. This classical (univariate) approach requires that the analyte is the only substance producing signal, or that: (1) all interferences are removed prior to the analysis (extraction, masking, distillation), (2) the analyte reacts specifically so that only its product produces signal, (3) the analyte and interferences are physically separated (chromatography), etc.

What Is Multivariate Calibration?

In comparison with this approach, multivariate calibration may seem like a mythi

cal animal. When building calibration models with spectra, such as near infrared (NIR) or Raman, there is no need to separate analytes from interferences, and measurements can be done without dissolving or grinding the sample. Just pointing a handheld NIR spectrometer the size of a smartphone at a sample may provide useful analytical results in a matter of seconds. Examples that are today routine in most industrial laboratories or field activities may appear as chapters of a science fiction book: fat, protein, moisture and starch can be measured directly on intact oil seeds, simultaneously, instantaneously and without organic solvents, organoleptic properties of foodstuffs (wine, coffee, beer, meat, olive oil) and textile properties or plant species can be assessed without human intervention. Many other examples abound in various industrial fields.

NIR cameras have introduced a new dimension to this scenario: the spatial one. Today it is possible to measure NIR or Raman spectra in each pixel of a material surface, so that a data table is collected with spectrospatial structure. These data are called hyperspectral, and allow one, among other things, to monitor the spatial distribution of chemical species on a surface. Applications include the study of the homogeneity of pharmaceuticals in solid tablets or pellets, the distribution of chlorophyll and other plant components in crop fields, etc., all made in a remote, noninvasive and automatic manner.

Where Is It Used?

The approach is not restricted to the digital processing of spectra. Other instrumental signals are slowly entering the analytical scene, whether optical (fluorescence, mid/far infrared, laser induced breakdown, nuclear magnetic resonance) or electrical (sensor arrays, impedance spectroscopy, voltammetry). Other scientific fields make use of similar approaches, e.g. bird species can be automatically classified from their sound, musical emotions and moods can be predicted from audio records, business cycles can be forecasted in econometric studies. It is a world open to scientific exploration as never before.

Exciting as it may seem, however, multivariate spectral calibration is not the analytical panacea. Infrared spectral sensitivity is rather low, so that detecting traces of analytes is not an easy task, and some analyte signals are difficult to measure (e.g., metallic elements), meaning that chromatography and atomic spectroscopy are still needed. Moreover, to be able to cope with the presence of interferents, the mathematical multivariate models need to be properly trained. This means that a large and diverse reference sample set is required for model building, usually involving hundreds or thousands of samples, for which nominal analyte values or target properties should be previously measured by classical techniques. Furthermore, the model performance needs to be monitored over time, because there is nothing to prevent future samples containing new interferents, not present in the calibration set. Should this occur, recalibrating the

Multivariate and Multiway CalibrationsWhat Analytical Chemists Would Ask from Aladin’s Lamp

▪ Alejandro C. Olivieri1

The holy grail of chemical analysis is the monitoring of sample properties or concentra-tions of selected substances, remotely, non-invasively, automatically, and avoiding the use of solvents or specific reagents. This can be achieved by measuring certain optical signals, e.g., near infrared or Raman spectra, provided they are processed by multivari-ate calibration models, appropriately trained with a large and diverse basis set of refer-ence samples. More complex signals obtained by hyphenated chromatography or ma-trix fluorescence spectroscopy provide an even more revolutionary bonus: quantitating analytes in complex interfering samples by calibrating with a handful of pure standards.

© Ja

ckM

oreh

, fre

eran

gest

ock.

com

20 Spectroscopy

Special Topic


model is required, adding the new interferents to the data base. These undesirable features can be overcome, however, by going one step further in the number of mathematical dimensions of the measured data.

The Mathematical View

From a mathematical perspective, spectra can be viewed as vectors (lists of numbers one below each other). However, more complex data can be measured and processed, and this is when we move to the multiway calibration field. For example, a liquid chromatograph hyphenated to a diode array detector is able to measure a data table for a given sample, i.e., a data matrix. Its columns are UVvisible spectra, each of them collected at a different elution time. In an analogous fashion, a gas chromatograph with mass spectral detection can measure a data table whose columns are mass spectra. One could also employ a fluorescence spectrophotometer to measure an excitationemission fluorescence matrix for each sample. Its columns are emission spectra, each of them collected at a different excitation wavelength. Scanning emission spectra at various excitation wavelengths is today possible in a matter of seconds using modern fastscanning spectrofluorimeters. Less popular in industrial laboratories, fluorescence matrix spectroscopy has played a

major role in developing multiway calibration, and is highly appreciated in scientific research. In principle, the complexity and number of data modes (the independent directions of a data array) can be increased, and some developments have been described by processing three and even fourdimensional instrumental data per sample. However, this higher multiway protocols are still in their infancy regarding their mathematical understanding and potential analytical advantages.

Fig. 1: Hierarchy of data structures and nomen-clature. For a single sample, univariate data are scalars (zeroth-order), multivariate data are vec-tors (first-order) and beyond, and multiway data are matrices (second-order), three-dimensional arrays (third-order) and additional, not shown, higher-dimensional data. For a sample set, the corresponding data arrays are named as one-, two-, three- and four-way arrays respectively.

Fig. 2: Univariate chromatogram for a mixture of polycyclic aromatic hydrocarbons, carried out accor-ding to the official protocol, and involving fluorescence detection at a single wavelength and solvent gradient. FLT, fluoranthene, PYR, pyrene, CHR, chrysene, BaA, benzo[a]anthracene, BbF, benzo[b]fluo-ranthene, BeP, benzo[e]pyrene, BjF, benzo[j]fluoranthene, BkF, benzo[k]fluoranthene, BaP, benzo[a]py-rene, DBA, dibenz[a,h]anthracene, BgP, benzo[g,h,i]perylene, IcP, indeno[1,2,3-cd]pyrene. The blue trace corresponds to the analytes; BeP and BjF are interferents.


TTTTTTTTTTTTTTTTTTTTTTTTTTTTThhhhhhhhhhhhhhhhhhhhhhhhhhhiiiiiiiiiiiiiiiiiiiissssssssssssssssssss iiiiiiiiiiisssssssssssssssss aaaaaaaaaaaaaaaaaaaaaaaaaaaaaannnnnnnnnnnnnnnnnnnnnnnnnn aaaaaaaaaaaaaaaaaaaaaaaaaaaaaaddddddddddddddddddddddddddddddd aaaaaaaaaaaaaaaaaaaaaaaaabbbbbbbbbbbbbbbbbbbbbboooooooooooooooooooooooooooouuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuutttttttttttttttttt...............................................................................KKKKKKKKKKKKKKKKKKKnnnnnnnnnnnnnnnooooooooooooooooowwwwwwwwwwwwwwwwwwwwwwwwwiiiiiiiiiiiiiiiiiiiiiinnnnnnnnnnnnnnnnnngggggggggggggggggggggggggggggg ffffffffffffffffffffffaaaaaaaaaaaaaaaaaaiiiiiiiiiiiiiiiillllllllllllluuuuuuuuuuuuuurrrrrrrrrrrrrrreeeeeeeeeeeeeeeeee iiiiiiiiiiiissssssssssssssssssss

nnnnnnnnnnnnnnnnoooooooooooooooooooottttttttttttttttttttt aaaaaaaaaaaaaaaaaaannnnnnnnnnnnnnnnnnnnnnnnnnn ooooooooooooooooooooopppppppppppppppppppppppppptttttttttttttttiiiiiiiiiiiiiiiiiioooooooooooooooooooooooooonnnnnnnnnnnnnn..........

WoWoWoWoWWoWoWoWoWoWoWoWoWoWoWWoWoWoWWWoWoWoWWoWoWoWoWoWWWWWWoWWoWoWooWWoWooW rrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrry-y-y-y-y-y-y-y-y-y-y-y-y-y-y-yyy-yyy-yy-y-yyyyyyyyy frfrfrfrffrfrfrfrfrrfrfrfrfrfrfrfrffrfrfrfffrfrrrreeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeee ppppppppppppppppppppppppppppppppppppppppppppprererererereerererrerererererererererereeer veveveveveveveveveveveveevevveveveevevvevveeventntntntntntntntntntntntntntnntnntntnnnnnttttioioioioioioiooioioiooiooioiooooiooioooionnnnnnnnnnnnnnnnnnnnnnnn ofofofofofofofoffofofoffofoooofofffoffprprprprprprprprprprprprprprprpprprrprppppprpprprppppppp ememememememememememmemememmmmmmmememmememeeemememememmemmemmmemeeeeeemeeemememmmatatatatatatatatatatatatatatatatatatttatataatatataatattaa urururururururururururururrururururrrrure e e e e ee eeeeeeeeeeeeeeeeee pupupupupupupupupuupupupupupuppppuppupupupupupupuppppppp mpmmpmpmpmmpmpmpmpmpmpmpmpmpmpmpmpmpmpmpmmpppmpmpmpmppmpmmmmmmmmpmpmpmppmppmmmmpppppppppp fffffffffffffffffffffffaiaiaiaiaiaiaiaiaiaiaiiaiaaiaiaiiaaiiaiiiaiaiiia lululululululululuuulululululluuurerererrererereererererererrere

BecBecBecBecBecBecBecBecBecBecBecBeBecBecBecBeBecBecBecBBeccBeccBB cBee auausausausausausausausausausausausausausaussauausausaussaussausausausaausausaaausa e pe pe pe pe pe pe pe pe pe pe pe pe e pe pe ppe pe pe ppe ppe umpumpumpumpumpumumumpumpumpmpumummumpumpumpmumpmpmpmpmummmmumm sesesesesesesesesesseseseseseseseeeeeeeeeealsalsalsaaalalsalsalsalsalslsalsalsalaalaaaaaalssalsala s wwiwiwiwiwiwiwwwwiwwwiwiwwwiwiwwilllllllllllllll fafaiaifffffaifaifaifafaifafaiifafafaafaaf l il il il il il iil iil ii ii n an an an an an an aan an aaan an an an an an an aan nnnn nn nnnnnnnnnnn nnn an s s s s sss sss s ssslitlitlitlitlitlitlitittttlitllitttitlittiiiittltletltletletletletltletlelettlleetltletleeett eeee asasasasasaasassasasasassassasasasaasassaasas 3030303030303030030303030030303003000000300 seseseseseseseseseseseseesseseseeseeeeseeeeeconconconconconconononconconconconnconcononcocconncc nonnnnnnconconondsddds dsds ds ds ds ds dds dds dsddsdsdsdsdddsdd ofoffofof of of of of of fofofof fofofffof ofof beibeibeibeibeieieeebeibeeebebeiebeibeibeibeiebebebeiibe ng ng ng ngng ng ngngngng nggngnngnngnggnggn runrunrunrunrunrunrunrununrunrunrunnrrunrunrurrurunnuuuu drdrdrdrdrdrddrdrddrddrddddddrddrd y, y, y,yy, y, y, y, yyy,y,y,y, yyyDurDurDurDurDuDurDuDuDurDuDurDurDurDuDuDurDurDurDuruD rDurDD rDurraChaChaChaChaChaaCaChChaCCaCaChaChhChChChChaChaCChhhhhhhhaaa illilillillllillilllillillllilllilllilii ® C® C® C® C® C® C® C® CC® C® C® C® C® CC®® C®®® C®® CCCCCChilhilhihhilhilhilhilhilhhihilhhhhhh li lerlerlerlerlerlerlerlerlerleelelerlereerssssss s sssssss incincincincincncincincncincncincinciinncinncnnncnnincn ludludludludludluudlludludludludludludududdududl de ae ae ae ae a ae ae ae ae ae aee ae ae aee aeee aee ae aae aaaaaaaaae stststststststststsstsss ateateateateaateateateateaateatetaateateteateateateaateaaateaatettatattatte-of-o-of-of-ofof-of-oof-o-of-o-o-o--offo--o--offo--oof-----thethethethethethethethethehthethethethethethetheheetheeeh -ar-ar-araaar-ar-ar-ar-a-araaaaaaaa-ara-aa-aaaart ct ct ctt ct ct ct ct ct ct ct ct ct ctt ct capaapaapaapaapaapaapaapaapapapapapaapaapapapapaappaaapaapaapp citcitcitcitcitcitciticitcitttcitttttcicccccic ancancancancancancanancancancancnancncnancanancnncncnn e e le lee le lee le lee lee leeee e leee iquiquiquiqiquiquiquiquiquiquququiqiqiquiqqqi uiquiquququiququqqqq ididididididiiddddidiididddd levlevlevlevlevlevlevlevlevlevevvlevlevlevevlevlelevvlelevevleeeeveveeeevlevvlevvveleleleleleleleeeeeleleeellleleeeeeeellellee sensensesensenenensenenensensensensesenenseseeeeneenseeenesse sossosorsorsorsorsorsororsosssororrorrorsssosorororsossssorossosssoorsoooroooo ononon on on ononoon on noon ono thethethethethethehetheheheheeheththethethhthehethethhheht et rererererererererrereererererreserserserserserserserserersersserserreserserserererrseee voivoivoovoivovoivoivoivoivovovoivovvovoivovoivvooovooovovov ioooovv i tr tr tr tr tr tr tr tr ttr tr tr ttr ttttr tr ttrr ttto po po po po po po ppo po po po ppo o pppppo o ppprotrorotrotrotrototrotottttroroorototrotrooottrotorotototoo ecteectectectectectecectectectecectecttcectctcteccttcectecececttttttecceccce ththththththththhhthhhththththththhththththe eee e e e e ee e eeeee e eee pumpumpumpumpumpumumpumpumpumpummuupumumpumupumumumumpumpumppumuupumpumumump mp pp p p ppp p p ppp ppp p ppp p pppppppppppppppppppfrofrofrofrofrorofrofffrofroffffrooroooooroor m pm pm pm pm pm pm pm pm m pm pm pm m pmm pppm ppm ppppremremremremremremremremremmemremremmemememremremremmremmmmmreremre atuatuatuatuatuatuatuatuatuatuatutuatattuatatuatuatuttuatutuuttuut re re rererere re re erereerere eereeeeereeeerrerrr faifaifaifaifaifaifaifaiffafafaifafaifffffafffaaifaaaaf lurlluruulurululurlurlurllullurlurrurlururruruu e. e.e. e. eeee. eeeeee.eeeee. eeee. e If If If If IfIf If IfIfff If f thethethethhethethethehethethethhehehhthethehheththeheheeee fluflufluflufluflufluuuuflufluflufluflufluflflufl idididdidididididididdddddddd levlevlevlevlevevlevevlevlevlevleevleveveeleel vvelelel el el el el el el el el elellelelelleeeleeelrunrunrurunrunrunrunrurunrurunrunrunnruunruuruururu s tss ts ts ts tts ts ts ts s ts ts tts ttts tsss tsssss ooooooooooo ooooooooooooooooooooooooooooooooooooooo lowlowlowlowlowlowlowlowlowlowwlowlowlowolowwwlowww, tt, t, tt, t, t, tt, tt, t, ttttttttthehhehhe he he hehe hehehehhe e hheehhee DurDurDurDurDurDurDuDurDuDurDurDuDuruDuurDuDDD rD raChaChaChaChaChaChhaChaChChChChChaChaChaChChChaChCaChaCaCha illillililliliiliiliilliilll® C® C® C® ® ® C®® C® C® C® CC® CCCC® CCC® CCCC®®® Chilhilhilhilhilhilhilhilhillhilhhhilhhhh lerlerlerlererlereelerlererlererlerrlererlerlerlerlerrr wiwiwiwiwiiwiwwwwwwiwwill llll lllllllllllllllggivgivgivgivgivgivigivgivgivgivgivgivigivgivgggg e e ee e e e eee eeeee visvisvisvisvisvisvisisvisvisvisvissvisvv ualualuauauaualualualualuaauualuaualualu luaaaaaaa anananaanananananannanaanana d ad ad ad ad ad ad ad ad ad add ad aaad aadd audiudiudiudiudiudiddudiudididiudiudiuududiuu iu iid blebleblebleblebleblbleblebbleblbbbbbbbbbbbbbblblebbbl alalalalalalaalalalalalalalalaaaaalarmarmaaarmarmarmarmrmarmarmarmarmrmmarmaarmrmarmarmrmmmmma mmms as as as as as as as aas as s as ass s aaassssss ndndndndndndndndndndndndndndndnndnddnnddnd if if ifififfififififififthetthethethetheththetheethehetheehehethetthet eee fluflufluflufluflufluflufluflufluufluflufluflufl diddididididdididdididdiddddididdid levlevlevlevvlevlevevlevlevlevlevevlevevlevlevlevvevlevelevvvvvlel vvvvvelel el el el elel eleel eleeeeee reareareareareareaeareareareaeaereareeereaerr aeee chechechechchchechechechehchehchechehechechechechchehehehhhc s as as as as as ass as aas as aasss as ass a popopopopopopopopppopoopoopp intiniintintintintintintinttintintntnttttntninntnttn whwhwhwhwhwwwhwhwhwhwhwwhhwhwhhereereereereereerereereereeereereereerereereeeeereeeeerere thethethethethethethethehethehethethehhehetheeeeheeeheeheeeeeeeeeeeeere’re’rerrere’re’e’re’reee’re’’re’reee’rereeeeeee s rs rs rs rs rs rs rs rs rrs rrs rs rrrs rrrrisksiskiskiskiskiskiskkiskiskiskkskisksiskskskiskissk ofofofofofofofofofofooffoofofofoffffffff sussusussususususussssusssus ckickickickickickickikickikckckcckikingngngng gng ng ng nngngngggnngngg g airairairairaiairairairairairairairairri inininininnnnnnnnnnntotototototototootototottto ttthethethethethethethehehettthehthettthetttthehettthehethettththethtt pumpumpumpumpumpumpumpumumpumpumpumpummpummpumpummpumuupup mppp pp,p, p,p, p,p, pp,pppp, pp,p, p,pppppp DurDurDurDurDurDurDuDurDurDurDurDurDurDurDurDuruDurruruuDuDurDDD aChaChaChaChaChaChaChaChaChaChaChaCChaCChaChaChCCCCCCCCCChaCaCCChhaC illlillilillillillillillillllillillililiiillilll® w® w® w® ® w® ww® w® w® w® ww® w® w w®® w® w® www® illillllllilllililllllilllllillil shshshshshshshshshshshshshhsssssssshhut ut ut ut uutut ut uutut utututuuuut thththethethethethethethethhethethetheethethetthhh chchchchchchchchhchchchccchcchcc illilillllillillillillillliillli er er ererererer ereer rerer erer errerdowdowdowdowowowdowdowowowdowowowwowdowowdowwdodowdo n n n an an an an an an aan aaaaann an aan aandndndddndndndndndndndndndnddnddndddndn prepreprepreprepreprepreprepreprepreprpreeepreprepp epp sensensensensensensensensensenensenssenenesenenssenensennnsenennt at at at at at at at at at aat a a at t at aatt notnotnonnonononotononotototnnononotnonotherherherherherherheeherherherhererherheher alalalaalalalalalaalalaaaa armarmarmarmarmarmarmararmarmarmarmmrmararmrmrarmarmmmaa ... . . .

DuraChill®



Spectroscopy 21

Special Topic


Multiway calibration and its outstanding properties are even more fabulous than those of multivariate spectral calibration. Just to give a common example, by measuring chromatographicspectral matrices or data tables, you may be able to quantitate analytes in complex samples, without the need of a large training set. Simply prepare a few pure analyte standards, measure their data matrices, join these data with those for the unknown sample, and let a multiway calibration model to mathematically separate the analyte contribution from those of the interferences. In other words, you do not need to worry about sample pretreatment or cleanup, baseline resolution of every analyte peak or background corrections. Chromatographic protocols become simpler, isocratic, cheaper, faster and, perhaps more importantly, greener. The approach has been called chroMATHography, a nice game on words proposed by a famous chemometrician. A more technical name for this property is secondorder advantage.

A Successful Application

A case worth mentioning here is the determination of polycyclic aromatic hydrocarbons (PAH) in aqueous samples. PAHs are environmentally concerned substances, many of them suspected to be carcinogenic to humans. The official liquid chromatographic protocol involves fluorescence detection and a mobile phase with solvent gradient, taking ca. 40 min to achieve baseline resolution. However, it is not free from potential interferents, and some nonregulated PAHs may coelute with the analytes. If liquid chromatographic matrices are measured with spectral (instead of singlewavelength) fluorescence detection, the job can be done under isocratic conditions and in less than 5 min. In our lab, ten highly coeluting PAHs have been resolved and quantitated at subppb levels in aqueous samples using this methodology, even in the presence of uncalibrated interferents in unknown specimens. The resolution of the ten individual analytes, and their digital separation from the interferents, was possible by applying a powerful data processing algorithm known as multivariate curve resolutionalternating leastsquares (MCRALS), which is based on the socalled bilinear model for matrix chromatographic data. Without going into further details, bilin

ear means that the matrix data can be conceived as the product of two separate matrices, one of them containing pure component chromatograms and another one the associated spectra. After the decomposition phase, the ‘virtual’ pure chromatograms can be employed in a classical manner to produce a calibration line, where the test sample signal is interpolated to yield the concentration of a specific analyte.

Fluorescence spectroscopy itself is also able to yield data matrices, by collecting emission spectra at a number of excitation wavelengths. The technique has allowed researchers to develop protocols for many different analytes in really complex natural or industrial samples. In fact, the first report showing that the secondorder advantage was possible, published in 1975, described the determination of a polycyclic aromatic hydrocarbon in the presence of other fluorescent congeners, calibrating only with pure analyte solutions. No one suspected at that time that

multiway calibration would be so revolutionary to analytical chemistry. A nice sequel of this work was recently developed in our lab: the determination of four PAHs on a nylon membrane attached to a rotating disk, which was left in contact with aqueous test solutions for a few minutes. Fluorescence matrices were then read directly on the membrane. Thanks to the preconcentration properties of nylon, the protocol allowed the quantitation of individual analytes with detection limits in the range from 20 to 100 ng L−1, i.e., 20 to 100 partspertrillions!

Why Is There No Widespread Adoption?

Even with all these almost unbelievably useful properties, there are no crowds of analytical chemists knocking on the door of multiway calibration. This implies that considerable work needs to be done on the communication side between chemometricians and end analytical users. Regrettably, there are many valuable resources for the analytical community buried in highly specific journals devoted to pure chemometrics. The communication issue has been addressed in a recent meeting (Topics in Chemometrics, TIC, Szeged, Hungary, May 2019), where one researcher suggested that the chemometricians should be out there, offering the digital products to chemists, rather than trying to solve problems that do not exist, or waiting until chemists come to them. Chemometricians may have the answer to the Chemist’s problem – so talk to each other!

Affiliation1Departamento de Química Analítica, (IQUIRCONICET), Rosario, Argentina

ContactProfessor Alejandro C. OlivieriUniversidad Nacional de RosarioInstituto de Química de RosarioRosario, [email protected]

Related Articles https://bit.ly/WAS-Calibration

Literatur: https://bit.ly/WAS-Olivieri

Fig. 3: Top: three-dimensional landscape of an elu-tion time-fluorescence emission wavelength data matrix, recorded for a mixture of similar composi-tion to the sample of Figure 2, but under isocratic conditions and in a much shorter time. Bottom: pure analyte chromatograms obtained by multi-way calibration of elution time-fluorescence emis-sion wavelength matrices. Individual analyte de-termination proceeded even when interferents are present in test samples. Analyte acronyms as in Figure 2. Reprinted with permission from [1]. Copyright 2009 American Chemical Society.

22 Spectroscopy

Special Topic


The Digital LaboratoryA Short Introduction

J Martin Graf-Utzmann

We all have heard the phrase: digitisation is unstoppable. In a coming series of articles we would like to highlight what we believe to be the most important aspects of digitiza-tion and the associated automation in the laboratory.

Many people think of automation on an industrial scale. That means a deserted production hall in which robots on the assembly line assemble metal parts into cars with uncanny speed and precision. In this series of articles, automation starts on a small scale. For me, a script that performs a repetitive task „at the push of a button“ is already automation. The machine takes over a part of the work that is repetitive and ultimately boring for me and therefore errorprone. The computer doesn‘t care how often values have to be written down, added, averaged, or processed in whatever way. In microbiology, for example, counting colonies in a petri dish can be done by an app on a smartphone, in other words, automated. There are solutions already available on the market that make pipetting into microtitre plates visually trackable and with that less errorprone. The system also takes care of the documentation. These are the first steps in transferring a task that does not involve any added value to a machine. Employees can use the time for more interesting and value adding tasks.

One Size Never Fits All

Of course there is no general solution to satisfy all users in all laboratories. However, the market offers solutions that can be implemented in your laboratory right now. For special cases tailormade solutions can be created in cooperation with the suppliers. The first step is to find out where timeconsuming processes can be sensibly automated and digitalised. The interaction of automation and digitization is what makes this setup so powerful.

But keep in mind that digitization requires thorough preparation. The processes to be automated must be well understood. After all, who benefits if a bad analog process is replaced by a bad digital process? It is also essential to involve the people who work in the laboratory in the planning, as they will have to use the new processes. The acceptance of the employees is decisive for the success of a

digitisation project. Processes that are automated but cause more work elsewhere have little chance to be accepted. On the other hand, if the work becomes more interesting by leaving out the „boring“ activities, everyone wins.

So - What Can you Expect?

In this issue of G.I.T. Laboratory Journal you will find an article by Dr. Thorsten Teutenberg from IUTA e.V. in Duisburg. Dr. Teutenberg is setting up an automated laboratory with funds from the state of North RhineWestphalia. The name of the project, on which we have reported on several occasions in our magazine, is FutureLab NRW. The article offers an insight into the possibilities of collaborative robotics.

Prof. Dr. habil Kerstin Thurow from the Center for Life Science Automation (celisca) in Rostock takes a different approach in her article and presents her point of view on the topic of collaboration with robots in the laboratory.

The editorial team and I look forward to presenting further insights and points of view in the course of the year within the series of articles. If you would like us to cover a certain aspect of digitization, please feel free to send us an email with the subject line „Digitalisation“ to gitla[email protected].

ContactDr. Martin Graf-UtzmannEditor-in-Chief, G.I.T. Laboratory JournalWiley-VCHWeinheim, [email protected]

Related Articles http://bit.ly/WAS-Robotics


TTTTTTTTTTTTTTTTTTTTTTTTTThhhhhhhhhhhhhhhhhhhhhhiiiiiiiiiiiiiisssssssssssssssssss iiiiiiiiiiiisssssssssssssssssssssssssss aaaaaaaaaaaaaaaaaaaaaaaaannnnnnnnnnnnnnnnnnnnnnnnnnn aaaaaaaaaaaaaaaaaaaaaaaaaaaaddddddddddddddddddddddd ffffffffffffffffffffoooooooooooooooooooooooooooorrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrr................................AAAAAAAAAAAAAAAAAAAAAAAAAAAAAA ccccccccccccccccccclllllllllllllllleeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeaaaaaaaaaaaaaaaaaaaaaaaaaaannnnnnnnnnnnnnnnnnnneeeeeeeeeeeeeerrrrrrrrrrrrrr

eeeeeeeeeeeeeeeeeeennnnnnnnnnnnnnnnnnnnnnnnvvvvvvvvvvvvvvvvvviiiiiiiiiiiiiirrrrrrrrrrrrrrrrrrrrrrroooooooooooooooooooooooooonnnnnnnnnnnnnnnnnnnnnmmmmmmmmmmmmmmmmmmmmmmmmeeeeeeeeeeeeeeeeeeeennnnnnnnnnnnnnnnnnnnnnnnnnttttttttttttt........

YoYoYoYoYoYoYoYoYoYoYoYoYoYYoYYoYoYoYYoYYoYoYYYYoYoYoYoYYYoYYYooooYoYoooururuururururururuurururruurururuururuuruuuruuruuuuuur flflflflflflflflflflflflflflflflflflflflflflflflflflflfluiuiuiuiuiuiuiiuiuiiiiiuiuiuiuiuiuiiuuiuiuiiuiuuuiuuuuiuuuu ddddddddddddddddddddddddddddddddddddd papapapapapapaapapappapapapapapapapapapapaappappappapppppppppp ththththtththththththhhhththhhthhthttthh ssssssssssssssssssstatatatatatatatatatatatatatatatatataataattaaaaaysysysysysysysysysysyssysysyysysyysyyyyyyyysyyyyy clclclcllcllclclclclclclclccclclclcclcccccccccccccc eaeaeaeaeaeaeaeaeaeaeaaaeaeaeaaeaaaaaeeaaaaeeeeeeeeeeeaeann,n,nnn,n,n,nn,n,n,n,,nnnnn,n,,n,n,n,n,nnn,nnnnnnnnnnn,nnnn wwwwwwwwwwwwwwwwwwwwwwwwwwwititititititititititittitititititittitttitititiittitttti hohohohohohohohohhohohohohohohohohohhohohohohhohohooohohohhohooohohoututututututututututututututtututtututtutttttutttuttutututtttut cccccccccccccccccccccccccccccccheheheheheheheheheehehheheheheheheehehhehhehhhehehhhh mimimimimimimimmimimimmimimimmimiimmimmmimmmmm cacacacacacacacacacacacacacacacacac lllllllll

adadadadadadadadaadadadadadadaddadaaddaaddaadaaaa didididdididididdidddidididiiddddddddddid tititititittitiittitiitititiititttitittitiveveveveveveveveveveveveveveveveveveveveveeveeevevvevveveessssssssssssssssssssssssss

AsAAsAsAsAAsAsAsAsAsAAsAsAsAAssAsAAssssAA parparparparparparpapaparaarparparparpararrrarparpparparparp t ot ot ot ot ot ot ott ot ot ot ott ot ot ottttt ottt oo of of of off of of of of of of of oof oof of our ur ur uurur ur uuurrrrruururu comcomcomcomcomcomcocomcomomcomomoocomcomcomcomcomcomc mccomcommmmitmitmitmitmitmmitmitittmitmittmitmmimitmmmmmi menmenmemmenmenmenmenmenmenmenemenmemenmemememmmemenmeenmenmeneeenmenm nemenmenem t tt tt tt tt tt t tt tt t tttt tt ttt tt ttt t tto to to to to to to o to to tto to to tto to o to ooooooo tooooooooooooooo oooooooooooooooooooo he he hhehehe he hehe hehehehehhenvenvenvenvenvenvenvenenvnvenvenvvenenvvenvene venennen iroiroroiroiroiroiroiroiroiroiroiriroirriroirorirrrroiroiroorrrorrr nmenmenmenmenmenmenmennmnmnmemnmenmenmnmemnnmnmenmenmenmmnmmm ntntntntntntntntntntntntntntntttntnnnn wewewewewwwewewewewewewewwewewwewwwwweww devdevdevdevdevdevevvvevevddevevvdeevevddevddevdeveeeveevvevdeveloeloeloeloeloeloeeloeloeleloooeloooeloeloeleleleloeeeee opedpedpedpedpedpedpedpepedpedpedpedpedpepedpedppeededpedeeedededededpeddedpp dddd aaaaaaaaaaaaaaaaaaaaaaaaaaaaaa patpatpatppatpatpatpapatpatpatpatpatapatatpppatppatpatpppappataaattteeneneneeenentntntenntntnentteenennttennteeenentnttteeeentnnnnnnnnnnnnntttn -------pepenpenpenpenpenpenpenpenpenenpenpennpenennpenepenenp npep ddddddddindindindindindindindindindindindindddinnddind nnninnnnddind nd g Ug Ug Ug Ug Ug Ug Ug Ug Ugg Ug UUg UUg Ug UUg Ug g UUg V lV lV lV lV lV lV V lV V lV lV lV lV lVVVVV llV VV ighighighighighighghghghighighighigghghghighghghghhhghghg t stt st st st st sst sst sssst sstt st st ssystystystystystystystyststysttysttystyyysysyssysyssystysystsssstysssyststtem em em em em ememmm em em em eemeemmmm emmemmmememmmmmmmm m thaththathathatthathathahathathathaththahahthathahhhhhhthhthat wt wt wt wwwt wwwt wt wwt wwt wwt wt wtt wtt wt wtt illillilillilllllilllllillillllillillilliiilllllll conconconconcononcononconcccconcoo tintintintintinttinitinininitintintinttt nnuouuouuouuouuouuouuouuouuouuououououuuouuouuuuuu uouuuu uuuuslyslyslyslyslyslylyslyslyslyslyslyslyls yyylysslyslyslyyyyy prprprprprprprprrprprprrprprprrrrrprrrrpppp eveeveeveeveeveeveeveeveeveeveeveeveeveeveeveeveeeeveeeeeeeeeevveeeevveventnt nnt nt ntnttnttntnttnntnt nntntnntn biobiobiobibiobbbiobiobiobiobioioiobiobioobbbb oobbb ooobioooologloglogloglogogogogoggloggoglogloglogggoggogogggl iiicicicicaicaicaicaicaicaicaicaicaicaiccicaicicacccacacaciccicall gl gl gl gl gg gl gl gll gll gl gl gl gl ggl gl gggrowrowrowrowowrowrowrowowrorowwwrooworowowwowwroo th th th thth ththththth th thhhhththth thhhhhthhhhhh hhthth hthttinininininininininnninnnnnnn thethethethethethehethethethethehethehhehethethehehehhhhhe fluflufluflufluflufluflufluufluuflufluflflufluflfluflufluflflflflflflflflflflflflflflflfl id idid ididid idddid ididdid patpatpatpatpatpatpapatpatpapapatatpatatatattpapataapatpa h wh wh wh wh wh wh h wh wh wwhh whh whh wwh wwithitithitithithithithithithithhithititiithtithithithhhhhoutoutoutoutoutoutoutououtoututoutoutououtoututouto ttutoo tt thththththththhththtthththhththe ne ne ne ne ne ne ne ne ne ne ne ne ne ne nnne neeee needeedeedeedeedeedeedeedeeedeedededdeededdeeedeededeedeedeeeed fofofofofofofofofofoofofoffoffofoorr r rrrrrrrrrrrrr cchechechechechechechechechechechechchechchehcc micmicmicmmmicmiccmicmicmicmicmiccmmmiccmicmmicmmmm alalalaalalalalalalalaalaaala grogrogrogrgrogggrogrogrogrogrogrogrorogrgrogrogroror wthwththwthwthwthwthhwthwthwthwtwthwthwtthhhwwtwtwwthhhhhhh inininininininininnininninniniinnnhibhibhibhibhhibhibhibhihibhibhibhibibibibiibbibbbibbibbibbibitoitoitoitotoooitoitoitoitooitooitoors,rs,rs,rs,rs,rsrs,rs,s,rs,rsrsrs,rsrrsrs,rssr , prprprprprprprprprprprprprrprprrprrprrrpprrreveveeveeveeveeveeveeveeveeveeeeveeveeveeveeeveeveeeeeee ntintintintintintintintintintintntntntintintnntintntinnt nng ng ng ng ngng ng ngngng ng nngnnngnngng algaalgalgalgalgalalgalgalglglgalglga gaaaa gggaecaecaecaecaecaecaecaecaecaecaaeeeaeaecaecaeaaea ideideideideideideideiidedeideededeideideidedeidideddeidddd s fs fs fs fs fs ffs fs ffs fs fffs fs ffss fs fs ffs fs romromromromromromromromromromomromromromromr momromommr mmrrrromromro bebebebebebbeebebbeebebebebbbbbebebebb iningingingingingingiingggingingingngngngngngnggnggnggng rerererrererererrererreerrer lealealealealeeaealelealealealeaeeaeleleaael aaasedsedsedsedsedsededsededseddedseddseddseddsedee ininininininininninnninnnnnnto toto to to tooto tototo totoototooooo thethethethethethethethethethetthehet ethetheetheeetheheet etththe wowowoworworwoworworwoworworwowororororooworwooooworoooooooooooo ldlldld’d’ld’ldd’dld’ld’dddldldld’dldd s ws ws ws wws ws wws ws ws ws wwss wwwws wwwwwateateateateatatateateateateateateteateateteateaatttttttta rwarwarwarrwarwarwarwarwarwawarwaarwarwrwawawarrwawaaaaaaays.ys.ys.ys.ys.ysys.ys.ys.ys.ys.sys.ysys.sysssys.yyyyyyy

DuraChill®



Laboratory Automation 23

Articles


The First Steps

In order to come close to the ideal of a completely digital planning, control and documentation of an analytical process,

laboratory equipment as well as the persons involved are to be registered in a central management system. The greatest technical challenges here are the definition and establishment of suitable inter

faces between a conventional laboratory information and management system (LIMS), an electronic laboratory journal (ELN) and a laboratory execution system (LES). Furthermore, the connection and interfacing of all devices and the integration of existing data and upcoming data is of utmost importance. Many of the devices currently in use do not have suitable hardware or software interfaces. Therefore, they can only be regarded as standalone solutions. In order to guarantee an automated data transfer, integration solutions are necessary, which additionally enable the acquisition and exchange of metadata (e.g. information about the type of measurement and the person operating

The Bot on the BenchCooperative Robotics and the Routine Lab

▪ T. Teutenberg1, K. Kochale1, M. Jochums1, M. Dronov1, L. Gehrmann1, N. Abdulin1, and J. Tuerk1

In spring 2016, the North Rhine-Westphalian state government launched an initiative to promote research and innovation potential. The application and implementation orien-tation in science and industry is to be strengthened in a targeted manner through sus-tainable and intelligent further development of existing research structures. This is meant to align the competencies of all players with the social challenges of the future. One of the projects funded is “FutureLab NRW”, in the context of which the Institut für Energie- und Umwelttechnik e. V. (Institute for Energy and Environmental Technology, IUTA) will implement the infrastructure for a digitized model laboratory for the miniatur-ized instrumental and effect-based analysis of the future.

Figure 1: Experimental set-up for the implementation of central automation steps.

© IU

TA

24 Laboratory Automation

Articles

the device). In addition, the central management system should be designed with sufficient flexibility to be able to take over the administration of new types of laboratory components (e.g. intelligent, functionalized laboratory furniture) and different types of sensor systems (e.g. for monitoring the room temperature).

Besides the question of higherlevel standards, collaborative robotics will play an important role. Figure 1 shows a first experimental setup for the implementation of central automation solutions. The robot shown in the figure 1 is initially intended to perform simple “pick and place” tasks that are normally carried out by qualified laboratory personnel. For humans, these are generally simple activities, such as loading an autosampler for HPLC with the corresponding sample trays. The transfer of this process to a robot is highly complex, very susceptible to interference and may require indepth programming knowledge. In order to meet the problem of skilled worker shortage, especially in the area of highly specialized IT professionals, an intuitive software is used for the first time. This allows the configuration and parameterization of basic functions of the robot by “drag & drop” to complex process chains. In this way it is not necessary for the user to have profound programming knowledge. Instead, the software translates the individual motion sequences as well as the force control of the robot into native program code, so that subsequent editing of the source code by a programmer is always possible. This experimental setup is intended to provide information as to whether and to what extent a domain expert (laboratory technician or technical employee) can automate work processes in the laboratory, without having to rely on corresponding IT specialists.

What’s Next?

After successful establishment of first workflows and the integration of all devices, the transfer to a mobile platform is planned. Against this background, IUTA has been a member of the Selfdriving Lab Robots Interest Group since 2019. Members of this group are mainly the large leading pharmaceutical companies. The objective is, among other things, to create a software platform that enables the integration of laboratory devices under a uniform standard. In this context, the IUTA FutureLab NRW can establish itself as an important link between industry and science by working on scientifictechnical issues that cannot yet be implemented in real operation even in the

largest companies due to, for example, current technical risk.

Acknowledgement

The funding from the State of NRW will be provided using resources from the European Regional Development Fund (ERDF) 2014 2020 “Investments in growth and employment”.

Affiliation1IUTA, Duisburg, Germany

ContactDr. Thorsten TeutenbergIUTA e.V. Duisburg, [email protected]

Related Articles: http://bit.ly/WAS-Robotics


TTTTTTTTTTTTTTTTTTTTTTTTTTTTThhhhhhhhhhhhhhhhhhhhhhhhhhhiiiiiiiiiiiiiiiiiiiissssssssssssssssssss iiiiiiiiiiisssssssssssssssss aaaaaaaaaaaaaaaaaaaaaaaaaaaaaannnnnnnnnnnnnnnnnnnnnnnnnn aaaaaaaaaaaaaaaaaaaaaaaaaaaaaaddddddddddddddddddddddddddddddd aaaaaaaaaaaaaaaaaaaaaaaaabbbbbbbbbbbbbbbbbbbbbboooooooooooooooooooooooooooouuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuutttttttttttttttttt............................................................................... HHHHHHHHHHHHHHHHHHHHeeeeeeeeeeeeeeeaaaaaaaaaaaaaaaaarrrrrrrrrrrrrrrrrrrrrrriiiiiiiiiiiiiiiiiiiinnnnnnnnnnnnnnnnngggggggggggggggggggggggggggggg yyyyyyyyyyyyyyyyyyyyyyyyyyyyoooooooooooooooooooouuuuuuuuuuuuurrrrrrrrrrrrrrrssssssssssssssseeeeeeeeeeeeeeeeeeelllllllllllllllfffffffffffffffffffffff

tttttttttttttttttttttthhhhhhhhhhhhhhhhhhhhhhhhhhhhiiiiiiiiiiiiiinnnnnnnnnnnnnnnnnnnnnkkkkkkkkkkkkkkkkkkkkkkkkk...........

CrCrCrCrCrCrCCrCrCrCrCCrCrCrCrCCCrCrCCrCrCCCrCrCrCCrrCCCrCCCCCCC eaeaeaeaeaeaeaeaeaeaeaeaeaeaeeeaeaaaeaeaaaaeaeaaaeateteteteteteteteteeeteeteeteettetetetetetettettetetettetete aaaaaaaaaaaaaaaaaaaaaaaaaaaaaaa qqqqqqqqqqqqqqqqqqqqqqqqqqqqqqquiuiuiuiuiuiuiuiuiuiuuiuuuiuiuuuuuiuiettetetetetetteteteteteteeteeteteeteeeeetteeterererererererererererererereererrerrereerrreewowowowowowowowowowowowooowowwoowooooowwoooowwwwwwwwwwwoworkrkrkrkrkrrrkrkrkrkrkkrkrkrkrkrkrkrkrkrrrkkrkrkrkkkrkrrkrrrrrkrrrr ininininininininninnininininininininininninnninngggggggggggggggggggggggggggg eneneneneneneneneneneneneenenenenenenennneneeneneneeeneneneneneenviviviviviviviviviviviviviviiviviiviviviiviiiiviivivivvirorororororororororororororororoororororrrrroroorrrororrrrororoooooonmnmnmnmnmnmnmnmnmnmnmmmnmnmnmmmnmmnmnmnmnnnmnmnnnn eneneneneneneneneneneneneneneeneneneeeneeenee tttttttttttttttttt

TheTheTheTheTheTheTheTheTheheThTheTheTheTheTheTheTheheeTheTheTheeeThTTheh sesesesesesesesesesesesesesesesesessssssessse newnewnewnewnewnewnewnewnewnewnewnennewn wnewewnewwnewewwnewewwneww hihihihihhihihihhhhhihihihhhihhhhhhhhh gh-gh-gh-ghgh-gh-gh-hgh-gh-gh-gh-gh-gghh-ghgh perperperperperperperperperpeperperperperpepeperpereepepeeeeeererrrpeeeerep forfoforforforforforforrrforooorforforrrfororororof manmanmanmanmanmanmanmanmanmanmanmanmanmanmamanmanamannmanmaanmammanmam nncecececececececececeeeceeeecc chichichichichichichichhihichhchichichihichichcchichiichiiiihichihch llellellllellellellelleeellellelleeeellllellellellleersrs rrs rs rs rs rsrsrs rrrsrsrrs srrsfeafeafeafeafeafeafeafeafeafeaaaeafeafeaaaefffeefeee turturturtuturturturturturtururururturuututurrurtuurturturru e oe oee oe oe oe oe oe oe oe ooooe oe ooee oe oee ouuurururururrururruruuuurrrrrr eexcexcexcexcexcexcexcexcccexcexccexcee cxcce ccccexcexcceexcxclusluslususlusluslususluslusluslususlususlullll iveiiveiveveveveiveiiveeiveveiveiveiveviveeveeiv WhWhWhWhWhWhWhWhWhWhWhWWhWhWhWWWhWhWhWWhWWhWhWWWhW ispispispsispispispispspispispppispsisppisisispissppppperCerCerCerCerCerCerCerCerCerCerCerCerCereerCerCereee Ce ooloolooloolooloooooooolooooooloooooloolooooooooolooo ®®®®®®®®®®®®®®®®®

NoiNoiNoiNoiNoiNoiNoNoNNoNoiNoNoiNoNoiNoioiNoiNNoNoNNNoNoNNNN se se se sese seseeese se seseseseessssssesesssssss RedRedRedRedRedRedRedRedRedRedRedRRedRedRedReRRRRRedRedRRReReeRRReReee uctuctuctuctuctuctuctuctuctuctucuctuctuctuctuctuctuctctctuctcttioiononionionionionionionionionioniononoononniiiono SySySySySySySySySSySySySySyyyyyysstestestestesteststestetestesteteetestesteeettsteeeteeet mm.m.mm.m.m.mmmm.mm.mm.mm.mmmmmmm ThThThThThThThThThThThhThThhhhTTThThhhhhhhhThTT isis sis iis is s is issis isssisssssssssssis patpapatpatpatpatpatpatpattpatttpattpatpatpatatatpatpatppappattppaa ententenentententententnttentententntentententententntententenenntentttnteneeenenn ed edeeed ed ed ed ed eded edeeed ddetectectectectectectectectececectecteceteteccecctecccceteettttttect hnohnohnohnohnonnonohnohnohnohnohnohnohnohnhnonohnohnohnonohnononhhhhhhhhhhhnh ologlogloglogogloglogloglogloglogloglologglogggy ey ey ey ey ey eey eeey ey eeey ey ey y ey eey eey vavalvalvalvalvalvalvavalvavalvalllvavvalvaalalaalavaaa uatuatuatuatuauauauatatuatatuattuatuatatuatuatuuauaattes es es eseses eseses es esesesseseessss thethethethethehhthethethethethethethehthehethethethhheehhehehet dedededdededededededdededededededededededededdeemanmanmanmanmanmanmanmmanmamamamanmannnmamanmanmmannmmannnmanmm d d d d dddd d dd d dddd ddddddddddforforfoforforforforforfororforfforf rrofor cococococcococococococccocoocococ oliolioliolioliololioloolioliololiololioooliingnngngngngngngngngngngngggnggggngng frofrofrofrofrofrofrofrofrorofrofrofrofrofrofroroffroomm mm ym ym ym ymm ym ym ym ym ym ym m m m m y ym ymm ym yourourouroouroourouroururouououruoururoouo rouru pprprprprprprprprprprppprprprpprpprprpp oceoceoceoceococeoceoceceoceoceocceocococeoceoceococeocccoccoceceoceecccess,ss,ss,ss,ss,ssssssss,ss,ss,ssss,sss,ss,sss,sssssssss,ss,ss,ssssss,s, ththtthhththththththtththththtththhthththhthttthenenenen enen en en en enenenen enenenenenenenenennnnnnnnnnnnnnnnnnnnnnnnadaadaadaadaadaadadaadaadadadadaadadaddadadaadadadaaddaddaptiptiptiptiptptiptiptittiptiptitptiptptpttptitpttp velvelvelvelevelvevevelvelvelvelelvelvevelveleleleveeelvvvvelv lveee y sy sy sy syy sy sy sy sy sy sy sy sy sy sy sy sy syy syyy sy syy lowlowlowlowlowlowowlowowlowwowlowlowlowlowololowwllowowoowoooowwws ts ts ts ts ts s ts ts ts t s s ts ts ttttttsss ts ts hehehehhehehehehehehehheeeeeeheheheehee fanfanfanfanfanfanfanfannfanfanfanffanfannnnnfannnnf nn spspsspspspsppppssppsspsppeedeedeedeedeedeedeedeedeedeeededeedeedeedeedeeddedeedeee totototototototototototototoootototoooooooooototo ththththththththhththththtthththhhhththtt e ee e e e e e eeeeeee eeeeee minminminminminmminminmmmminminmininminmmmininimuimuimuimuimuimumumuimuimuimuimuimumimuimuimimuimmimummui m nm nm nm nm nm nm nm nm nm nnmm nmm nm nmm nm neceeceeceeceececeeeceeceeceeceeceeceeceeceeceeceececee ssassassassassassassassassaaasaaassasssass ryrryryryryryyyyryrryyryryryyyyyyy totototototoototototo maimaimaimamammaimamamaimaimamammaammmmma ntantantantntntantantanntntantantantantantantaantatatatantantttattntttnttntttttt inininiininininininninininnnn conconconconconconconconoconconconocononconconnconnnconno trotrotrotrotrotrotrotrotrorotrotrotr l llll llllllpoipoipoipoipoipoipoipoipoipoippoipoipppoipoioint,nt,nt,ntnt,nt,nt,nttnt,ntnntnt,nttnnnntn , mamamamamamamamamamaamammaaaamamaammamaaaaakinkinkinkinkinkinkinkinkinkikinkkininkikikkinkinkinkk nng tg tg tg tg tg t tg tg tg g tg tg tttttg tg tttg ttg g tg tg tg gg hehe he ehhehehe hehehe hheeheheheheeeh cchchichichchichichichichiccchichicchcchihcccch llellellellellellelleellellelleel elleeeeeeeeer er er er er er er eeer eeeeeeeer er er xtrxtrxtrxtrxtrxtrxtrxtrxtxtrxtxtrxtxtxtxtxtxtttxttxtrtttttxtrttxtrxtrtxtrtrrrxtrxxx rt emeemeemeemeemeemememmemeemeemmeemmemeeemeemeemmemem ly y ly ly lyylyly ly yy ly lyyy y yyyquiquiquiquququiquiquiquiquiquiquiquiquiququququiuqquqqu etetetetetetetetetetetetetteteteeeeeeet wiwitwitwitwitwiwitwitwiwitwitwitwwitwitwitwitwitwititwitwwwiti houhouhouhouhouhouhouhouhouhouhouououhouhououoouhouohouohohhoouuuuuuh t st st st st st st st st st stt tt st st stt s t st t acaacracracracracracracracracracracraaacaca ificificificificfifiificificifiificificficfiifififiificifificficcinginginginginginginginingngingingngngnngnngngingg anananananananananannnnnanaanananaa y cy cy cy cy cy cy cy ccyyy cy y cyy cy cyy ccooloolooloolooloolooooloolooolooooloooooollllllllllllingingingingingingingingingngginginngiiininggnginginggingiiiii gg perperperperperpeperererpeperperperrrrrrperpere forforfororforforforoforfororoforforforfooforforfooormanmanmanmanmanmanmannmanmanmanmanmmanmanm nm nnannmanmanannnnce.ce.ce.ce.ce.ce.cecece.ce.e.cce.eeeceeee.eee.eeee

DuraChill®



Laboratory Automation

Articles


The term “cobot” is an abbreviation of “collaborative robot” and basically refers to industrial robots that are not separated from humans in the production process, but rather work together with them. In the 1997 patent, J.E. Colgate and M.A. Peshkin defined cobots as follows [1]:

“an apparatus and method for direct physical interaction between a person

and a general purpose manipulator controlled by a computer”

The establishment of the cobots was a significant further development of the classic industrial robots, which usually work completely separate from people. By integrating numerous sensors that improve safety, e.g. switching off when touching an obstacle, collaborative robots

can work in close proximity to humans or work directly with humans. Expensive protective devices such as housings or light barriers / curtains can therefore be omitted. Current versions of the standards ISO 1028 part 1/2 as well as ISO / TS 15066 define the safety requirements also for collaborative robots [2], [3], [4].

Cobots combine the classic advantages of robots such as power, high precision and reproducibility and endurance with human characteristics such as experience, creativity or the general overview and open up completely new possibilities and applications.

Collaboration?

Even if the word “cobot” is derived from the term collaboration, real collaboration between humans and robots is only the closest form of collaboration. Coexistence, in which humans and robots work in close proximity without a shelter, is most common, but human and robot do not share the workspace. If humans and robots share a workspace, we speak of cooperation. This can be for example transfer stations where people transfer a part, workpiece or sample so that the robot can pick them up. Humans and robots work in a common space, but at different times. The closest mode of operation is collaboration, in which humans and robots work on a part / workpiece at the same time (although both perform different tasks).

Numerous cobots have entered the market in recent years, initially under the more general name of ‘lightweight robots’. Companies like Kuka, Universal Robots, ABB, Rethink, Kawasaki, Yaskawa, Franka Emika or Denso offer numerous systems today.

How important are cobots in laboratory automation? Due to their lightweight construction, they have numerous advantages. Laboratory applications usually do not have the load capacity requirements as they exist in classical industrial areas. Classical industrial robots are often overengineered in the laboratory. This also has a significant impact on the price of the robotic systems. The modern cobots are powerful systems that are also characterized by moderate prices. The possible omission of safety enclosures and light barriers is also an advantage. Cobotbased automation systems therefore take up less

Cobots in the Analytical Laboratory Useful Tool or Gadget?

▪ Kerstin Thurow

We are currently experiencing a real cobot hype. Search engines like google now deliver more than 861,000 results. Everyone is talking about cobots today and they are also gaining increasing interest in laboratory automation. But what are cobots? Are they re-ally useful tools in laboratory automation or just a nice toy?

© Ja

ck M

oreh

, fre

eran

gest

ock.

com

26 Laboratory Automation

Articles


space and also allow a more flexible use of integrated subcomponents such as optical readers, centrifuges or analytical measurement systems (GC, LC, MS) if these are not used in the robot process.

But can cobots really be used in a collaborative way in the laboratory? Hardly likely. The number of processes in which robots and humans work together on one specific task is likely to be very low. It is hardly conceivable that classical laboratory work such as pipetting, weighing, shaking, extracting or recording measured values will be processed together by humans and robots. Cooperation and coexistence remain as possible forms of cooperation. In the latter, the cobots are used in automated systems in which classical industrial robots were used in previous concepts. The overall concept of automation is not changing. Due to the lower costs, automation of sample preparation and measurement technology are now possible in new areas, which did not use automation previously due to cost reasons. This makes automation of laboratory processes increasingly interesting and affordable for small and mediumsized companies as well as for research institutions. Here, flexible fully automated systems (automation lines) will be the focus of interest in order to be able to process larger numbers of samples at better prices. However, it should be noted that not all robots are also equipped with suitable control software. Software components can be purchased from external companies or must be developed inhouse. Depending on the scope of the task, considerable costs may arise.

More Cobots - More Problems?

Due to the low cost of the cobots, it is in principle also conceivable to equip different laboratory devices with robots. These could, in particular in the case of measuring systems, liquid handling systems, shakers, heaters and other laboratory devices, function as a transfer unit and feed the samples placed by humans to the respective devices or remove them again after the corresponding process times have expired. This corresponds to the cooperative mode and would make the laboratory work considerably easier. The existing laboratory environment and structure could be largely preserved, extensive restructuring is not necessary. There are several things to consider with this approach. If many laboratory devices are to be equipped with robots, the number of

cobots required results in high investment and maintenance costs. Simple transfer processes usually do not require a large number of degrees of freedom, i.e. cobots would also be overengineered in this case and could be replaced by simpler systems with fewer degrees of freedom.

The biggest problem, however, is the control of the systems. Superordinate control systems are required, especially if samples have to be processed at several stations and several robots and laboratory devices have to be managed and controlled. Depending on the desired scope of options and flexibility, these workflow management systems can quickly become very extensive and therefore also expensive.

Summary

So is the current cobot hype really justified? Cobots are a sensible and logical further development of classical industrial robots. Their possible use and the type of use (coexistence, cooperation, collaboration) are very dependent on the respective application. In the field of laboratory automation, the first two possibilities will surely prevail in the coming years due to the tasks and requirements. In the cooperating sector, a special form of cobots makes sense for different laboratory stations and transport between the stations: mobile robots. These can either only realize transport tasks between different stations or they can also take over the supply of samples to individual laboratory devices. This can limit the total number of robots required. However, the requirements for the workflow management systems remain and are additionally increased by a mobility component. Mobile robots are currently being used in the automation area. Due to the high costs (comparable to classic industrial robots), they are not yet a real alternative.

ContactProf. Dr.-Ing. habil. Kerstin Thurowcelisca, University RostockRostock, [email protected]


TTTTTTTTTTTTTTTTTTTTTTTTTTTTThhhhhhhhhhhhhhhhhhhhhhhhhhhiiiiiiiiiiiiiiiiiiiissssssssssssssssssss iiiiiiiiiiisssssssssssssssss aaaaaaaaaaaaaaaaaaaaaaaaaaaaaannnnnnnnnnnnnnnnnnnnnnnnnn aaaaaaaaaaaaaaaaaaaaaaaaaaaaaaddddddddddddddddddddddddddddddd aaaaaaaaaaaaaaaaaaaaaaaaabbbbbbbbbbbbbbbbbbbbbboooooooooooooooooooooooooooouuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuutttttttttttttttttt...............................................................................SSSSSSSSSSSSSSSSSaaaaaaaaaaaaaaaaaaaavvvvvvvvvvvvvvvvvvvvvviiiiiiiiiiiiinnnnnnnnnnnnnnnnnnnnnnnnggggggggggggggggggggggggggggggggg ttttttttttttttttiiiiiiiiiiiiiiiiimmmmmmmmmmmmmmmmeeeeeeeeeeeeeee.........

SaSaSaSaSaSaSaSaSSSaSaSaSaSaSaSSaSSaSaSSSaSSaSaSSSSaSSaSaaaaSaaaaaaaavevevevevevevveveveveveevevevevevevvvevvveevvvvvvvve ttttttttttttttttttttttttimimimimmmmmimimmmmimmimmimmimimimimimimimimmiimimmiimimimi eeee ee eeeee eeeeeeeeee eeeeeeeeeeeeee anananananannananananaannanananananaananna ddddddddddddddddddddd efefefefefefefefefefefefefefeefefefeeeeeffffofofofofofofofoofofofofofoofofooofooofooof rtrtrtrtrtrtrtrtrtrtrtrtrttrrtrrtrrrt wiwiwiwiwiwiwiwiwiwiwiwwiwiwiwiwiwiwwiwwiwwwwwwwwwwwww thththththththhththhhththhththththhhthhhhhhhhthhhttttttttthttttt eeeeeeeeeeeeeeeeeeeeeeeeeeeeasasasasasasaasasasasasasasasaaasaaasasaasaa y y y y y yy yy yyyyyyyy yyyyyyyyyyyyyyyyyy acacacacacacacacacacacacaaacacacacacacacaccacaaacacaccacacaacaaaa cecececececececececececeeceececececeeeceeeeceeeececeeeeeeeeecec ssssssssssssssssssssssssssssssssssssssssssssssssssssssssss tototototototototototototototottototoottototoootoooo tttttttttttttttttthehehehehehehhehehehehhehhehhehehehh

rererererrererererererererererrrerereeererreeerereeererrrreeererr sesesesesesesesesesesesesessessesesseeeeeesessseeseservrvrvrvrvvrvrvvrvrvrvvrvrrvvrvrrvrrvrrrrr oiooioioiooioioioioioiooioiiooooooooooio rrrrrrrrrrrrrrrrrrrr filfilfilfifilfilfilfilfilfifilfififilfilfifififififififilfifififilfilfifififififi llllllllllllllllllllll popopopopopopopopopopoopopopopopopopopopoopoppoopoopopoppopp rtrtrtrtrttrtrtrtrtrtrtrtttrttrtrttrtrtrrttrttttttt

DurDurDurDurDurDurDurDurDurDurDuuDDuuDDuurDuDDurDuurD aChaCaChaChaCaChaChaChaChaCChChaChaChChhChChChaChCCha ilillillllillillillilliliiliiiliilill ®®®®®®®®®®®®®®® ChChChChChChChCChChChChChCChhhChhChCChCChillillillillilllilllllllllilllillililllilll ersersersersersersrersrserserseerserserseeersre ofofofofofofoffofoffofofofooffoffffoofoffferferferferferferferferferferferfferfeferferereferffeferf aaaaaaaaaaaaaaa conconconconconconconconconcooncoococcccononconconcocoooonnncooonconnccocc venvenvenvenvenvenvenvenenvenvenvevennnnnnnv nnnnv nnnvennnnnnv nnienienienienienienienienienienennniennnieenei nieneii ne tlytlytlytltlytlytlytlytlytlytlylytlytt yy locloclocloclocococloclocococloclocloccooccoooco ateateateateateateateateateateateateateaatttatttatetetttatettettttttt d fd fd fd fd fd fd fd fd fd fd fd d dd d fd fdd fd fddd fronronronronroonononronononnnronronrorononronooonnnt fit fit fit fit fit fifit fit fit fit fit fififit fit fit fifififilllllllllllllll resresresresresesesesresresesresresreseeesreresesrreeser ssre ererververververververvververvrvervrverververveerrvervvvvvrvrrre oiroiroiroiroiroiroirroiroiroiroirooiro roiroiroioirooirooiooioioiiiii . Y. Y. Y. Y. Y. Y. Y. Y. YY.. Y. YYYYYY. YYYY. Y. . . YYYYYYYYYououououououououououuouoouoooououoououuouuouuu no no nono no no nono nono nnno nnoonnoooonono nnonnonnlonlonlonlonlonlonlonolonlonlonlonoonolonl nlonnlononoloonoloo gergergergegegergergergerrrrerggererrgergergergergegeergergeeeg hahahhahhhahahahahahahahaaahavevevevvevevvveveveveevevve totototo to to toto to totootototototooooooooooo gogogogogogogogogogogogogogoogoogogogooogoggg totototototototototootootoooooooto ththththththththhhhthththttttthththttththttththhhhe be be be bee be be be be be be be be be be bbbe be bbe be be be be bbackackackackckackackckackackackacackckckackackcackkkka kkcackckkckaaa ofofofofffffofofofofoffofoooofoffofffoffo thththththththhhhththhththhhhthtthhhhhhht e e e ee eeeeee eeeeeeeechichichichicchihiichchichiicccchh ellellellellellellleeelleellelleleeleeer tr tr tr tr tr tr tr tr ttr ttoo oo oo oo oo oo o oo oo oo oo ooo oo o oo ooooo o penpenpenpenpenpenpenpenpenpenepenpennpepenppenenenenennnnnpenppepp anananananananananananannaannannaanaa d fid fid fid fid fid fid fid fid fid fid fififid fid fifidd fifid fid fid fififid d fid llllll ll llllllllll llllllll thethethethethetheheeheeethethetheet ehethethetheheethhtheheeee rererererereeerereeeeererereeesersersererserserserserserssersserseererserere voiivoivoivoivoivoivoivoiiiiivovovoioivvovoivvoiir. r. r. r. r. r.r.r. rrrr.r. r.r. r. DurDDurDuDurDurDurDurDuDurDurDurDurrDurDurDuDurDurDD aChaChaChaChaChaChaChaChaChaChaChaChChhChaChaCaCaaChaChaChCaChaaChaChaChillillillillillllilillilliiliiilliillillilliiiiiiiiii ® h® ® h® ® h® h® h® h® h® h®® h® h® hhh® h®® asas asasassas sas as asssas asaassasasasas thethethethethetheththehthttheetththeehet eeee fifififilfilfilfilfilfilfilfilfififilfififififilfifi l pl pl pl pl pl pl p pl pl pl pl pl ppllll portorooortortortortooortortortrtooooooroortort ininininininininininininininniin ththththththhhththhthtththhhtthe fe fe fe fe fe fe fe fffffe fe ffe fe fee fe fronronronrororonororonoronronronronronrroronooorronror nttt,t,t, t,t, t,tt,t,t,tt,tt ,makmakmakmakmakmakmakmakmakmakmamakmakmamakamakmakkm ingiiingingingingggnginginggingininggiingngiiini ititititititititititittittiit eaeaeaeaeaeeeaeaeaeaaeaeaeaeeaaaaee sy ssysysy sy sy yssy syyysyyssysys to toototo toto to oto totootttoooooo accaccaccaccaccacaccccacccacaccaccaccaacaacccaa essessessessessessesessessesseeseseeeeeesseeeeseeesssesseese , a, a, a, a, aa, a, a, a, a, a, a, aaa, aaaa, voivoivoivovoivoivovovovoovoivooivovvvooivoivov ivoivoiv dindindindinindindindindinindindindindindinnndindinidddddddd nng sg sg sg sg sg sg ssg ssssg sg sg sg ssssg sg g spilpilpilpipilpilpilpilpipipilpilpipipipipipipipp ls ls sls lssls lsls lssss andaandandandandanandanddandndanddndnddandaaaa dddd sasasasasasasasasassassassas vinvinvininvinvinvinvinvvinvinvinnvininvinvinvininvivvinvviviv g tg tg tg tgg tg tg ttg tttg tg tg tg tttg tg tg tttg g tttg timeimeimeimeimemememeimemeimemememeemeimemeeeeimeim .........

DuraChill®



Related Articles http://bit.ly/WAS-Robotics

Laboratory Automation 27

Articles


The idea of using molecules as electronic components is in line with a general tendency followed by modern electronics, the miniaturization of individual components. The great promise of organic molecules over existing semiconductor electronic elements are: 1) their size – most of the simple molecules are significantly smaller than existing individual transistors, 2) their uniformity – molecules of the same compound are identical to the last atom, and 3) the flexibility in design – chemistry provides various wellestablished routes to tune the properties of molecules. These prospects paved the road for further investigations in the field.

Creating Electrodes on the Atomic Scale

A very successful technique to characterize electrical transport at the nanoscale

are mechanically controlled break junctions (MCBJ). Historically, they were developed to study the properties of weak links in superconducting materials using freshly broken metallic surfaces. The technology was then adapted for the study of atomicallysharp metallic electrodes where the quantization of the electrical conductance can be observed, and further on for the measurements of molecules [2, 3]. Nowadays, the MCBJ approach is one of the most common experimental techniques in the field of molecular electronics. The technique relies on the breaking of a metallic wire by pulling it in a controlled way. This is achieved by bending a flexible substrate on which a metallic constriction has been fabricated. Using modern nanofabrication techniques, metallic nanobridges with an attenuation factor (the ratio between the wire elongation and the sub

strate bending) below 104 can be achieved. In other words, bending the substrate by 1 micrometer leads to a wire elongation of less than 0.1 nanometer, resulting in remarkable mechanical stability and tunability of the system. The breaking of the metallic wire is monitored by applying a potential difference between its two ends and measuring the resulting current in the circuit (Fig.1). The magnitude of the current decreases as the metal wire is stretched until it ultimately consists of a single atom. Upon bending the substrate even further, the nanobridge is broken, accompanied by a drastic change in current as the resulting tunneling gap between the two atomically sharp electrodes slowly increases. To perform the electrical characterization of molecules, the latter are functionalized with ‘anchor groups’ – chemical groups that provide covalent or van der Waals binding to the electrodes and allow molecules to bridge the gap between them. Typical anchor groups are, for instance, thiols (SH), amines (NH2), cyanides (CN) and pyridils (C5H5N), with gold being the predominantly used electrode material. The properties of molecular junctions formed in this way are defined

Molecular ElectronicsBuilding Organometallic Chains Molecule by Molecule

▪ Anton Vladyka1, Jan Overbeck1, Mickael Perrin1, Michel Calame1

The concept of single-molecule electronics – the use of individual organic molecules as active elements in electrical circuits – strongly roots in the inspirational theoretical con-tribution by Aviram and Ratner where a molecular diode was proposed [1]. We describe here recent experimental progress showing how an organometallic chain can be as-sembled molecule by molecule between metallic electrodes.

Fig.1: Illustration of a break junction for measurements in liquid environment. The typical length of free-standing gold bridge (u) is 300-500 nm, and the width of its constriction is 60-100 nm. Figure adapted from [4].

28 Chemical Syntheses

Articles


by: 1) their chemical backbone, 2) the anchor groups, 3) the nature of the electrodes, and 4) the environment (e.g. a solvent).

Molecular Signatures

During the measurement process the junction is repeatedly broken (opened) and then reformed (closed) in the presence of molecules in solution. For every cycle, the change in conductance with electrode separation (conductance trace) is recorded. One or few of the molecules from the surrounding medium can bridge the gap between the electrodes, and this event is reflected in the conductance trace. In this way, the binding and unbinding of a single molecule in a nanometersized gap can be detected in real time. To capture the large amount of possible conformations of the molecule(s) between the electrodes, this process is repeated hundreds of times, and then statistically analyzed.

The data are usually presented as either conductance histograms or conductancedisplacement histograms (Fig.2). In a conductance histogram, the probabilitydistribution of conductance values during the entire breaking process is presented. If the target molecule forms stable molecular junctions, a peak appears in the conductance histogram. For the conductancedisplacement histogram, a twodimensional distribution of conductance values as a function of electrode displacement (roughly the gap size) is presented. In this case, the signature of molecular junction formation is a con

ductance plateau (i.e. a relatively flat area of high counts).

Knitting with Molecules

Because future applications based on molecular junctions require their stable integration into electronic circuits, studying the interaction of molecules with electrodes is of particular interest. In a recent study, we used the MCBJ approach to characterize BdNC molecules [4]. These are benzene molecules that have highly polar isocyano (NC) chemical groups as anchors. The interaction of isocyanides with gold is known to be particularly strong, with calculations confirming their binding energy to surpass even that of covalent sulfurgold bonds. Moreover, the isocyanogold bond is highly directional allowing for dense molecular surface coverage which makes these molecules an ideal test system for reliable junction formation.

The measurements were performed on a 100 micromolar solution of BdNC molecules in a mixture of THF and mesitylene. Multiple conductance plateaus were observed in the conductance histograms of openingtraces with a very high yield of plateau formation (Fig.2). This can be explained by the formation of multiple stable molecular configurations during the measurements process. In notable contrast to break junction measurements on most other molecules, a similar behavior was also observed for the closing conductance traces, i.e. while the electrodes are approaching. This is a result of the polarity of the isocyano

Fig.2: Conductance-displacement histogram of BdNC-molecules in solution. Three areas of high counts as well as three peaks on the conductance histogram (right) are the signatures of three con-secutive plateaus in conductance traces which are referred to stepwise chain formation. The inset shows the si-tuation when the third plateau is not formed. Figure reproduced from [4].

THIS IS A CHILLER AD.

ThThThThThTThThTThThThTTTThhisisisiisisisisisissisiss iiiiiiiiiiis s s s ss s ssssss aaaaaaaaaaaaaa cocococccocococococooococommmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmm ititititttitititttiitittititititiittittttmemememememememememeemmmemmentnntntntntntntnntnntn tttttttttttttoooooo ininiinnnnnnononononoonoooonnooooooooonnovavavavavavavavvavavaavavaavvvvavvvavvvavvatitititttitittiittitittititititt veveveveveveveeveveveeveveveeeee ththththththththtthththhhtht ininininininininininininnninkikikikikikikikikikikikikiikiiikiingngngngngngngngngngngnggggngg,,, ,, ,,, ,,, aaaaaaaaaaaaa rererererererererereefleflefleflefleflefleflefleflefleeeeectctctctctctctctctctcttcctctctcctcttcccttctcctcctioioioiioooioiiooioioooiooiooiiiiioiiiiiiiiiioiiiiiiiiii n n n n nn n n nnnnnnnn ofofofofofoffofofofoofoofoff ttttttttttttododododdoddoooooodayayaayayaya ’s’s’s’sssssssss mmmmmmmmmmmmmmmmmmmmmmmmosoososososososososososososoossososossosossooo t ttt ttttt ttttpopopopopopopopopopopopoopooppppopppp wewewewewewewewewewewewewewewwwwww rfrfrfrfrfrffrfrfrrfrfrfrfrrrfrrrrr ulululuulullululululuul eeeeeeeeeeeeengngnngngngngngngngngngggngginininininnnnninininininininnnnninnnneeeeeeeeeeeeeeeeeeeeeeeeeeeeeeee ririrririririiriiirrrririirrriiirr ngngngngngngngngnngngngggggngngggggngnngg, ,,, , ,, , aaaaaaaaaaaaaaaaa dedededededeedeedeededidididdiddddddiiiid cacacacacaaaaaaaaacaaaatitititititttittititttitititittttittitititttttttt ononononononononnononononoonoonoononnnonononnnn tototototototototototoottotoototototottooottoo qqqqqqqqqqqqqqqqqqqqqquauauauauauauauauauauaauaaaauauauuu lilililiililililiiliiiliiitytytytytytytytytytytytytytyyty... .. ThThThThThThThThThTThThhhhTThheeee ee eeeee eeeeeeeeee jojojojojojojojojojojjjjjjojjjjjoooojjoj inininnnninininininninininiiniinnnininininininnnininnniiinnnniniinnnnnnngggggggggggggggggggggg ofofofofofofofofofofofofoffofoffoof tttttttttttttttttttecececececececececececeeceecccce hnhnhnhnhnhnhnhnhnhhnhhnhhhhhhh olololololololololloloololooooogoogogogogogoggggggogoggogoggggoggggooggoogooogogogoogoggogoggggggggggogggogggggggggggyyy y y y y yyy yyy yyyyyyy y yyy yyyyyyyyyaanananananananananannnananana dddddddddddd crcrccrcrcrcrcrcrcccrcrreaeaeaeeaeaeaeaeeaeeaeaaatititititititittttt vivivvivivivviivivviiviiiiiivv tytytytytytytytytytytyttytytytytttttttt ,,,,,,,,,, rererererereeererererereeeerer dedededededeededededdedeededddd finfinfinfinfififinfinfifinfinfinfinfinfinfinfififinfinfififinfinfifififififinfinnfinfifinininiiiiininininiinininniininniii g ggg gg g g gg g gg whwhwhwhwhwwwhwwhwhwhhwhhwhwhhwhwhwhwhhwhwhwhwhwwwwwwwhwhw atatatatatatatttaatatattttatta aaaaaaaaaaaaaaaaaaaaaaa chchchchchchchchchchchccchcchcchilililililillilililililili lelelelelelelelellleeerrrrrrrrrrrr isisissisisisisisiss.....

FoFoFFoooFoFFoFoFFFFFFoFoooFoFFF r rr r rrrrr rr thththththththtththhthhhhtt ososososososososososososososssosoooo eeeeeeeeeeeeeee whwhwhwhwhwhwhwhwhwhwhwhwhwhwhwhwhww oooooooooooooooo rrerererererrereeeereereererefufufufufufufuffufufufuufufufuff seseseseseseseseseseseseseeseseseesesesesess tttttttttooooooooooooo sesesesseseesesesesesesetttttttttttttttttttttttleleleeleelelelllllee ffffforororororro anananananananananannnnanaanaaa ytytyytytytytyytytyytytyyytyyy hihihihhihihhihihihihihhhhhiiiihiingngngngngngngngngngnggngngnngg ssssssssssssssssssssshohohohohohohoohohohohohohohohohohohoooortrtrtrtrtrtrtrtrttrtrrrtrtrtrrr oooooooooooooooof ff f f ffffffff f pepepepepepepepepepepepepeeeppeeeeeeeppp rfrfrfrfrfrfrfrrfrfrfrffrrrrrr ecececececececececcceceeeeccce ttittititititittitttittttt ononononononononnonononononnon.....

DuraChill®

Portable Recirculating Chillers

FulFulFulFulFulFulFulFFullullulFulFFuFFuFFululull-Cl-l--Cl-Cl-Cl-Cl-Cl-Cl-Cl-l-Cl-l-Cl-Cl-Cl-Cl-CC-CC-- oloolooloolooloolooloolooloololooolooloolololoololoor Tr Tr Tr Tr TTTTTr TTr TTr TTr TTTTTToucoucoucoucoucoucoucoucucoucoucoucouuoucuucucuuucoucuuuouou hschschschshschschschschschschschschscscscchhsshsss reereereereereereeeereereereereeereeeereereeeeer n Dn Dn Dn DDn DDDn Dn Dn Dn Dn Dn DDn Dn ispispispiispispispispispiispsispspsppplaylaylaylaylayayayayaylaylayayayayAllAlAllAllAllAlAllAllAllAllAllAlAAlAllAlAllAlA thththtthththhhhththhhhthhe ie ie ie ie ie ie iee ie ie ie ie ie eee nfonfonfonfonfonfonfnfonfonfofnfonfnnfonfonnfonfonfooormrmarmarmarmamamarmamamarmarmarmarmarmamarmrmr tiotiotiottiottiotiotitioiotioiotiotiottiotioioitti n yn yn yn yn yn yyyyn yn yyn yyn yn yn ynn yyn yn youoouoououououououooooooooouou neeneeneeneeneeneeneeeeeneeneeneeeneeeeeed add ad ad ad ad ad ad ad ad ad ad ad ad at tt ttttt tt tt ttta ga ga ga ga ga ga ga g ga ga a glanlanlanannnanlanlananannlannanlanlanannceccecececececeeeccecccecccc

FroFrFFroFroFroFroFrorororooFFFFroFFFroFroFroFFFrroFrooFroFroFroFroFrF oFrFFrFFroFrFr ntntnt ntnt ntntntntntnntnttntnttntnntnn FilFilFilFilFilFilFiFilFilFilFFFili l Rl Rl RRRRl Rl Rl R Rl RRl RRRRReseeseeseeseeseeseseseeseseseeseeseeseeeeeses rvorvorvovorvorrvorvorvorvor ooorrrv iririrrririririiriririiririSavSavSavSavaSavaSavSavSavvvSavSavSavSavSavSavvavvavavvavaavaavvavvavaavSavSa e e teeee te te teee tte tte e teee teeee imeimimeimeimemimemimeimeimeeimemmemmeemei anananananananananaana d ed ed edd ed ed eed ed ed ed ed ed d ed ed d ed eeffoffoffofffoffoffoffoffoffofoffofoffoffff rtrtrtrttrtttrtrtrttrttrtrtr wwitwitwitwitwitwitwitwitwwwitwitwitw h eh ehh eh eh ehh eh eh eh eeh eh eeh ehh eeeasyasyasyasyasyasyasyasyasyasasya yyy accaccaccccccccaccaccaccaacccacccccaccccccccceeeeseessssessesseesssesesseseeeseeseee s totototototototototoototo thththththththththtthtththhhthe reeee re re ree re r re re re rrre re e e re re e reseeseeseseeseeseeseeseeseeseeseseeseeseeesseeeeeseeesesssss rvorvorvorvorvorvooovorvorvorvorvoorvooiririiririrrriiriririrrriirrrirrirrri fillfillfillfillfillfillfilfillfilfillfillfillfifillfillfillfillfilllfil popopopopopopopopopoppppppppp rtrtrtrtrtrtrrtrttrtttt

DynDynDynDynDynDynDyDynDyDynDynDynDynDynDynDyDynDynDynDynDDDDynyy aamiamamiamiamiamiamamiimiamiammiamamimiamiammmmimammiim cFicFicFcFiFicFiFicFicFFcFiFcFicFFcFicFicFicFicFicFicFicFiFccFFFFccFccFcFcFicccF lteltelteltelteltelteltelteteteeetetlteltelteltel etetteeeetttl er™r™r™r™r™r™™r™r™™™™r™™r™r™™™r™NNNo No NoNo No NoNo NNoNooNoNNo No NooNooNNNNNoNoNN mormormormormmormormormormormorormorrmormormorrrrormmmmo e pe pee pe pe pe pe pe pe pe pe pe pe e peee e pe pppe ppprevrevrevrevrevevrevevevevvvreevvveverevevevevvevevvvvrevententeentententntenttntnententenententenenteenenteeeeeenenenteennnnee atiatiatiatiatitiatiatiatatiatiatittaatiaatiaaaaaa vevevveveveveveveeveevevvvevvve airairairairairairaiairairaairairairairairaairairaaaaaa filfilfilfifilfilfilfilfilfilfilfillteterterterterterteterertteete maimamaimamaimaaimamamaimaimamaimaimaaiiimamaimmaaiaimaamaaaaaaaam ntententententententententetnteententntenntententn eeeenteteen eenannannannannannaannannannaaannanaaanaannnnncecececeececececccecceeeccecece

LiqLiqLiqLiqLiqLiqLiqqLiqLiqLiqLiqLiqLiqLiqLLLiqqqqquiduiduiduiduiduiddiduiduididuiuiduididiuididiuiduu LeLeLeLLeLeLLeLeLeLeLLeLeLLeLeLeLLLeLLevelvelvvevelvelvevelvevelvelllvevelvelvelleveve MoMoMoMoMoMoMoMoMoMoMoMoMMMMoMoMoMonitnnitnitnittnitnitnnitnitnnnnitnnititnititn tnititorioriorioriioriioriorioriorioriorioriroriioriorirorororo iingngngngnngngngngggngngnnngnngngngggWorWorWoWWorWorWorWorWorWorWorWorWoWorWoroWorWoWoWorryry-ry-ry-ry-ry-ry-ry-ry-ryryyy-rryyyy frefrefrefrefrefrefrefrerrererrerrefreerer e pe pe pe pe pe pe pe pe pe ppe pe pe pe pe e peee e ee ee revrevrevrevrevrevrevevreevrevrrevevreevever ententenententententententenenttntentntenttenententnenntteneenenenntntnn ionionionionionionniononionononionioonnoioonioonnoooooniooo ofofofofofofofofoffffofffoffffooofpreprepreprerepreprprepreprprepreprepreeprep eepp matmatammatmatmatmatmatmatmatmamammatmamatmmmataata ureureureurerereureurerereurereuureurerreurrerrerrure pupupupupupupupupupuupupupupupuppupupuuppp mpmp mp mp mpmp mp mpmpmppmpmmmp mmmmp ppmppp mp mpmmmm faifaffaifaifaifaifaifaaifaif ifaifaifaifaiafaifafaifafaffafafaaaaaa lurlurlurlururlurulurlurluruurlurlururururuururuuurruruuuuruureeeeeeeeeeeeeeeeeeee

WhiWhiWhiWhiWhWhiWhihiWhiWhWhiWhihWhiWhiWWWWWhhWWhWWWW spespespespespspepspespespespespespespepspespspepeppsppppppespspsspssppssspeep rCorCorCorCorCorCorCoCrCorCoCorCorCorCorCoCCCCoCoCooCoCoorCorCoC ololololololllollololololoooloo ®®®®®®®®®®®®®®®®®®®®

CreCreCreCreCreCreCreCreCreCrereeCreeCrCreCreCreeeereateateateateateatteateateataatteaaaa eaata aaaaaaaaaaaaaaa quiquiquiquiquiquiquiquiquiquqqquqquqqququuuiuqu eteeteeteeteeteeteeteeteeteeteteeteeteeteeteeteeeteeeteee r wr wr wr r wwr wwwr wr wwr wwwwworkorkorkorororkorkorkrkorkoorrkrkrkorkkkrooo ingingingingingngingingingingingngngngningnni ggg envenvenveenvenvenenvenvenvnenvenvenvenenveen iroiroiroiroiroiroroorooirororrooronmenmenmenmenmnmenmemnmenmenmenmenmmeemmmmnm ntntntntntntntnttntnnnnnnntt

UV UV UV UV UV UVUUUVUVUUVVVUVUVUUUVVVUUUVUVU AntAntAntAntAnttAntAntAntAntAntAntAntAAntAntntnAntnnAnAntAnAA i-B-Bi-Bi-Bi-Bi-Bi-i-Bi-BBBi iolioliololiolioliolioioolioologiogiogiogiogiogogiogiogiogiogigioggiiogiigoggg calcalcalalcalcalcalalacalcallcc lcaa LiLiLiLiLiLiLiLiiLiiLiL ghtghtghtghtghtghtghtghthhhhhhghhhhhthhhttgghthghtghtghYouYouYouYouYouYouYouYouYouYouYouYouYoYouYYouYYYYYoYYYYouYYYYYouuYooo r flr flr r flr flr flr flr flflr flflr flr flflr flr uiduiduiduiduiduiduiduididuiduidiuidiuidiuu du papapappapapappapapaapaapaathththththhthhthhhthhthhtttttttt stastastatstastastastastastattas aaayysysysysysysysysyssysssysysys clecleclecleclecleclccleclleclec eeeeleclecc aan,an,an,an,an,anan,an,nan,an,anananannnnan, witwitwitwitwitwiwitwitwititwwwwwitwitw twitw tttttwwwithouhouhouhouhouhouuoouooohouhouhouhouhohohhohhhoooo t ct ct ct ct ctt cct ctt ct ct ct ct ccchemhemhememmemhemhemhemhemhemhehehhemhemhhheemicaicacaicacaicaicaicaicaicacaicaicacaicacacaal al al aall a al al a aaaaddiddiddiddiddiddiddiddddiddiddidddddiidididitivtivtittivtivtivtivtivtttivtivtivtt vtivtittttt esesesesesesesesessesesses


Chemical Syntheses 29

Articles


gold bond resulting in molecules sticking out from the surface, ready to form a contact.

To attribute the conductance signatures to specific molecular configurations we performed theoretical calculations using Density Functional Theory based Molecular Dynamics (DFTMD) simulations at room temperature.

These allow us to visualize the interaction of molecules while pulling apart the electrodes at a temporal resolution of 1 fs. Evaluating several sets of these computational experiments, we are able to link moleculeelectrode configurations to observed conductance features. The first conductance plateau with higher conductance was attributed to the singlemolecular junction and its conductance value is similar to that observed in other molecules of comparable structure. The second, lower conductance plateau, corresponds to the configuration of organometallic chains which include two molecules plus one or more additional gold atoms. These chains form during the opening process because the strong interaction between the isocyano anchorgroup and gold allows the BdNC molecule to pull a gold atom from the electrode. The resulting organometallic compound can then interact with another molecule which is present in close proximity to the junction as a consequence of the dense surface packing described above. Detailed analysis reveals that in 29 % of all breaking traces a third plateau is observed, which is attributed to the formation of trimer chains at even larger electrode displacement and with correspondingly lower conductance.

Even longer chains are expected to form, however, with conductance below the detection limit.

Tuning Knobs

As the onsurface concentration of molecules in the vicinity of the initial monomolecular junction is of prime importance for the chaining process, we employ two complementary approaches to exercise control over organometallic chain formation. First, the same measurements were performed in solutions with smaller concentrations of BdNC molecules to reduce the equilibrium density of molecules on the electrode surface. In the second approach, the central benzene ring of the molecule was extended by two bulky side groups, namely methyl and tertbutyl instead of the usual hydrogen termination. These side groups are expected to decrease the effective electrode surface coverage through steric hindrance, and hence suppress the formation of dimers and trimers. Indeed, experimentally both routes were tested and yielded a suppression of the oligomerization process. Instead, a single highconductance plateau with modified shape (width and slope) was observed and attributed to a slightly modified configuration statistics of the monomolecular junction.

Microscopic Understanding

The formation of molecular dimers and trimers through incorporation of gold atoms can be considered as a controlled stepbystep synthesis of such a conductive metalorganic 1Doligomer. Here, the

exceptional stability of the MCBJ technique allows for the realtime observation of the process of chain formation, molecule after molecule, as revealed by their conductance properties. In stark contrast to other synthetic schemes, the process does not rely on the stepwise addition of different constituents of the organometallic compound, but occurs via insitu extraction of atoms from the electrode by the isocyanomolecules. These findings pave the way for the controlled formation of onedimensional, single coordination chains, which may be used as promising building blocks for organometallic frameworks.

Affiliation1Transport at Nanoscale Interfaces, Empa, Dübendorf, Switzerland

ContactMichel Calame Head of LaboratoryTransport at Nanoscale InterfacesEmpaDübendorf, [email protected]

Related Articles http://bit.ly/WAS-MatSci

More Information on http://bit.ly/GLJ-ME

References: http://bit.ly/GLJ-Calame

Fig.3: DFT-MD calculations demonstrating the chaining of two BdNC molecules while the gold elec-trodes are withdrawing. Figure reproduced from [4].

30 Chemical Syntheses

Articles

Advanced Biotechnology SeriesTo reflect the substantial advances in all areas of biotechnology, Sang Yup Lee, Jens Nielsen, and Gregory Stephanopoulos have joined forces as the editors of Wiley-VCH book series, Advanced Biotechnology. This series covers all pertinent aspects of the field and each volume is prepared by eminent scientists who are experts on the topic in question.

Industrial Biotechnology:MicroorganismsChristoph Wittmann, James C. Liao

ISBN: 978-3-527-34179-5792 pages | January 2017

Systems BiologyJens Nielsen, Stefan Hohmann

ISBN: 978-3-527-33558-9440 pages | April 2017

Emerging Areas in BioengineeringHo Nam ChangISBN: 978-3-527-34088-0 904 pages | January 2018

Applied Bioengineering:Innovations and Future DirectionsToshiomi Yoshida

ISBN: 978-3-527-34075-0656 pages | February 2017

Advanced Biotechnology

Edited by Toshiomi Yoshida

Applied Bioengineering

Volume 5Series Editors: S. Y. Lee, J. Nielsen, G. Stephanopoulos

Innovations and Future Directions


Synthetic Biology: Parts, Devices and ApplicationsChristina SmolkeISBN: 978-3-527-33075-1432 pages | April 2018

Edited by Christina Smolke

Synthetic Biology



Parts, Devices and Applications


Edited by Gyun Min Lee and Helene F. Kildegaard

Cell CultureEngineering


Recombinant Protein Production


Cell Culture Engineering: Recombinant Protein ProductionGyun Min Lee, Helene Faustrup Kildegaard

ISBN: 978-3-527-34334-8400 pages | October 2019

Coming Soon:

Fundamental Bioengineering John Villadsen

ISBN: 978-3-527-33674-6574 pages | February 2016

Edited by John Villadsen

Fundamental Bioengineering



Micro- and Nanosystemsfor BiotechnologyJ. Christopher Love

ISBN: 978-3-527-332816296 pages | April 2016

Edited by J. Christopher Love

Micro- and Nanosystems for Biotechnology



Industrial Biotechnology: Products and ProcessesChristoph Wittmann, James C. Liao

ISBN: 978-3-527-34181-8 640 pages | January 2017

Edited by Christoph Wittmann and James Liao

Industrial Biotechnology



Products and Processes

Visit www.wiley.com/go/adbio for more details and to order 19

–576

401


The project is funded as part of the European Union’s Horizon 2020 work program and is coordinated by Professor Albert Heck, project coordinator and professor of biomolecular mass spectrometry and proteomics at Utrecht University.

Why Now?

The idea to form a platform where all scientists in the field of proteomics can fur

ther develop their skills, share their expertise, and provide access to top of the range mass spectrometry equipment is not a new one. The high cost of mass spectrometry equipment has long been a precluding factor for the widespread use of proteomics for many institutions and clinical laboratories engaged in life science research. Most proteomics technologies use complex instrumentation, critical computing power, and expensive consum

ables. Taken together with the need to acquire, train and retrain highly qualified research staff, longterm sustainability of mass spectrometry equipment can be a challenge. As a result, the major contributors to progressive advancements in the field of proteomics are largely made by a small group of pioneers in the field; many of whom are located in Europe.

It was realized from a previous European proteomics project, PrimeXS, which facilitated access for life science researchers to highend mass spec infrastructure and expertise from pioneers in the proteomics field, that it had been successful in achieving a more coordinated effort within the proteomics community throughout Europe. The initiative (which finished in 2015) resulted in the publication of more than 300 articles and paved

European Proteomics Infrastructure Consortium – Providing AccessA European Proteomics Initiative

▪ Martina O’Flaherty

The European Proteomics Infrastructure Consortium - Providing Access (EPIC-XS) part-nership is a project funded by the European Union to provide proteomics expertise and mass spectrometry technology to all researchers within the life science arena. It brings together eighteen proteomics institutes, spread across fourteen European countries, with the objective to provide over 2,400 days of access to high-end proteomics technol-ogies. This initiative will also provide access to various workshops and training courses.

European Proteomics Infrastructure Consortium – Providing Access (EPIC-XS) research community, representing countries spread across fourteen European member states.

32 Mass Spectrometry

Articles


the way for a new initiative – the European Proteomics Infrastructure Consortium Providing Access (EPICXS).The EPICXS community has now expanded its consortium to include seven new European partners and will again provide expertise and access to proteomics technology to European researchers.

Why Proteomics?

Protein analysis is essential for understanding the complexity of the communication process that takes place within every living organism. This is important because proteins essentially represent the actual function of a cell. In order to contribute to advancements within the life sciences it’s important that we understand how proteins work. If we can figure out how proteins express themselves, how they function, and interact with other proteins, metabolites and nucleic acids, then we can gain valuable insight into potential disease biomarkers that can ultimately be used for detection, treatment and in some cases, disease prevention. The study of the interactions between all proteins, the proteome, is called proteomics.

Unravelling the secrets of the proteome is a challenging task, some may say even daunting, considering that every individual is unique and has an entire set of proteins which are constantly changing and reorganizing themselves and because protein expression spans many more orders of dynamic range than DNA and RNA, they are more difficult to work with. As proteins cannot be amplified like DNA and RNA, less abundant species are more difficult to detect, hence improving sensitivity and the dynamic range of proteomics analysis is essential and quite challenging. To complicate matters even more, is the fact that there may be more than several million distinct protein molecules in a cell, each having their own potential properties and functions and all of which undergo a certain degree of posttranslational modifications. Thus, analysis of the entire proteome presents a surmountable challenge. The goal of getting rid of high abundance components in biological fluids, tissues, organisms and cells in order to identify those proteins which contribute to illnesses and disorders and identifying those which could be used as potential biomarkers, has been the focus of many proteomics laboratories around the world. In achieving this goal, mass spectrometry has become one of the most powerful tools in the field of proteomics. This technology measures a fundamental characteristic of a molecule, its molecular weight. The measurement of the masstocharge ratio of ions helps identify and quantify molecules in simple and complex mixtures. Valuable information with regard to the analysis of low molecular compounds and macromolecules present in protein samples can be gained by use of this technology. Modern instruments feature very powerful analytical capabilities – sensitivity, selectivity, resolution, throughput, mass range, mass accuracy – so much so that these days pretty much any protein in a cell is identifiable. In fact, over the last ten years due to advancements in mass spectrometry technology and its cost effectiveness, that proteomics has evolved from a very specialized discipline to becoming a much more standard fixture in the laboratory [1,2].

Proteomics has also played an important role in cancer research [3]. It allows for monitoring drug responses of tumors, understanding mechanisms that lead to cancer pathogenesis, designing novel therapeutics, and even makes it possible to identify cancer cells in biopsies [4]. Some of the most exciting breakthroughs in proteomics involve the discovery of new biomarkers. One of the pioneers in the proteomics field, Ruedi Abersold of the ETH Institute in Switzerland, has employed proteomic profiling techniques to do exactly that [5].

Making translational proteome profiling a more mainstream technology in a clinical environment is also a project which will be addressed within the EPICXS initiative. Matthias Mann from the University of Copenhagen in Denmark leads this project. The team of researchers aim to address some of the most recent bottlenecks in clinical proteomics, by developing robust, reproducible high throughput proteomics workflows to analyze large sample cohorts from patient samples. They will investigate sensitivity issues, tackling the dynamic range in the plasma proteome and address the use of PTM’s and epigenetics as biomarkers for disease states. These technologies will be made directly available to the scientific community through their implementation in the European Proteomics Infrastructure Consortium access sites.

There have also been significant developments in many other types of medical conditions such as Alzheimer’s disease, schizophrenia and depression that have been enabled by proteomics. Amongst others, John Yates of the Yates Laboratory at the Scripps Research Institute, USA, develop and apply proteomics to study these conditions.

While proteomics has helped researchers develop new drugs to fight diseases, this field of research is not limited to the medical arena. Valuable information in relation to developing food products that are safe and contribute to our good health and wellbeing can also be attributed to proteomics. Interestingly, proteomics studies reveal that nutritional factors can play both a beneficial and a detrimental role in complex inflammationrelated disorders such as allergies, asthma, obesity, type 2 diabetes, cardiovascular disease and rheumatoid arthritis [6, 7].

It is obvious that improving our understanding of how cells interact is crucial, and while researchers can now identify almost any protein in a cell, the growing demands of identifying highly specific protein biomarkers in precision medicine means

Socorex Isba SATel. +41 (0)21 651 [email protected]

A product line that offers more to you.Mastering precision volumetry, Socorex provides for reliable liquid dosing instruments. Choose among a wide selection of manual and electronic micropipettes, dispensers, repeaters, pipette fillers and syringes for all dosing applications.

P R E C I S I O N L I Q U I D V O L U M E T RY

Hall 1 - Booth 427

Mass Spectrometry 33

Articles


that many researchers are now turning their focus to the characterization of single cells.

The ability to monitor how the proteome differs from cell to cell presents quite a challenge. In an article in 2018 [8] Assistant Professor Jia Guo, of the School of Molecular Sciences, Arizona State University, Tempe, AZ, USA, explained that ‘single cell analysis makes it possible to discover mechanisms not seen when studying a bulk population of cells.’

EPICXS researchers are also leading scientific investigations into the field of single cell proteomics. A consorted team within EPICXS will investigate the development of groundbreaking novel proteomics technologies improving sample throughput, posttranslational modification analysis, sensitivity towards single cell analysis, reproducibility, dynamic range, multiplexing capabilities and proteome coverage. The aim of this project is to go beyond state of the art, to bring proteomics into the future, taking proteomics research onestep further.

Aside from the exciting future mass spectrometry holds within the field of proteomic and metabolomic analysis of single cells [911] this technology is by no means limited to the medical and diagnostic sectors. Focusing on the everincreasing world population and global climate change, it is clear that the generation of new nutrient rich and sustainable food crops has become a necessity. Many developments of novel designer crops can also be attributed to mass spectrometry technology [12, 13] as well as advancements, which have led to the discovery of proteins hidden away not only within plant and animal life but also within other life forms such as tiny microalgae. The research team led by professor Albert Heck, professor of biomolecular mass spectrometry and proteomics at Utrecht University in The Netherlands, together with the proteomics team at Birmingham Univer

sity have unraveled insights about the composition and structure of the lightharvesting system within this tiny microalgae life form, which can facilitate the development of new solar panels [14].

Why EPIC-XS, Why Now?

While this project will provide access to highend proteomics technology which otherwise would not be accessible to many researchers, it’s also quite ambitious in its aim to tackle logistical hurdles presented by the plethora of datasets generated by proteomics methodologies, a subject close to the heart of many proteomics researchers.

Many laboratories find the mass spectrometry data difficult to handle and are working hard to overcome this issue. John Yates of the Yates Laboratory at the Scripps Research Institute, USA has also addressed this topic [15].

EPICXS researchers also have a team dedicated to computational proteomics. The team will develop algorithms and software standards for data handling, providing support to all scientists across the consortium, for managing processes and data manipulation.

All the research activities within EPICXS are built on the strong innovative trackrecord of the consortium members involved and are focused on designing novel approaches for future developmental efforts not only in computational and translational approaches but also, in structural and spatial proteomics. This project team is led by Paula Picotti, at the Institute of Molecular Systems Biology, ETH, Zurich, Switzerland and will focus on characterization of the subcellular organization of the proteome, yielding important information regarding protein function. High

Advanced Sustainable Systems

The high-impact, peer-reviewed journal for breakthrough research on sustainability across all scientific disciplines, with a strong focus on more efficient, less energy consuming, and less waste-producing systems and cycles.

advsustainsys.com

Submit now


Articles

er order structure of proteins will also be investigated, a research area which is critical to our understanding of biological function because changes in higher order structure of proteins can have a detrimental effect regarding the quality, stability, safety and efficacy of many medicines and can also lead to loss of biological function.

By providing the broader proteomics community access to experts in the field, and by enabling them to avail of highend mass spectrometry technology, hardware and bioinformatics tools, EPICXS will help overcome many challenges facing researchers in this field of science. Transnational access will also provide handson training for researchers, helping to develop best practice workflows, and aid the dissemination of proteomics data into publicly available databases thereby broadening the expertise of experienced scientists and those new to the field of proteomics.

The Future

It’s an exciting time to be involved in the field of proteomics and while the sensitivity of MS has steadily increased over the years, further improvements are possible and necessary, especially if ever single cell analysis can be reached. Limited mass spectrometry sensitivity, low dynamic ranges, undesirable long analysis time needed for clinical biomarker verification and validation, the lack of established and routine mass spectrometry based analytical technologies, taken together with equipment costs are all precluding factors in the struggle to achieve and expand the sustainability of mass spectrometry within the proteomics arena. This is where EPICXS can help. This dedicated consortium of expert proteomic scientists is committed in their efforts to address these challenges and are positive about the outcome of securing a bright and sustainable future for all of life science research. That there’s a

high demand for such a European proteomics initiative can be seen by the number of applications already received. Over ninety users have requested access to this technology and we are only at the start of this fouryear project. Not only that, but this project has also realized a requirement for initiative’s like this one to stretch further than its European borders, as applications have also been requested from Canada and America. While funding may have run its course by the end of 2022, the sustainability of the proteomics community, through this initiative, will continue to strengthen and develop long into the future.

ContactDr. Martina O’FlahertyUniversity of UtrechtUtrecht, The [email protected]

More information on EPIC-XS http://bit.ly/epic-xs-eu

Interview with Ruedi Aebersold: http://bit.ly/Interview-Aebersold

Consortium members and references: http://bit.ly/GLJ-OFlaherty2

© K

zeno

n - s

tock

.ado

be.c

om

WileyAnalytical

ScienceAward

Contact: Isabel Brenneisen [email protected]+49 6201 606 716

was-award.com

APPLYNOW!CLOSING DATE

APRIL 30, 2020

Good Products deserve an Award –our Wiley Analytical Science Award.

Articles

Phenylurea pesticides, including diflubenzuron (DFB) and fenuron (FEN) are widely used in agriculture to improve productivity and, consequently, they can produce residues in crops, soils and surface waters. Due to the photochemical reactivity of these pesticides, photoinduced fluorescence (PIF) methods were developed, based either on UV irradiation (classical PIF) or on direct laser irradiation (DLPIF), for determining their residues [1,2]. Therefore, in order to validate the PIF methods, analytical applications were performed in Senegal natural waters. Moreover, gas chromatographymass spectrometry (GCMS) was combined

to PIF to separate and identify the fluorescent DFB and FEN photoproducts by comparing them to standard compounds, including phenol and phydroxyaniline [3].

Procedures

Fluorescence measurements were carried out at room temperature on a Kontron SFM25 spectrofluorimeter, interfaced with a microcomputer. Phototransformation of both pesticides into strongly fluorescent photoproducts was realized under UV or DL irradiation of the DFB and FEN working standard solutions (105 M). Liquid extraction of 3 mL of DFB and FEN irradiated solutions was carried out three times with 10 mL of ethyl acetate. Then, the organic phase was dried with anhydrous magnesium sulfate (MgSO4) in order to remove the traces of water, and afterwards was evaporated to dryness at 45 °C with a rotavapor. The dried residues were dissolved in 300 μL of ethyl acetate. A 200μL sample was supplemented to 1 mL, and a 1.5 μL volume sample was studied by GCMS. A Nist library X calibur software was utilized to interpret the mass spectra (m/z values ranging from 50 to 650). All experimental conditions were optimized in our previous work [1].

Identification of the Fluorescent PhotoproductsAnalysis of Two Phenylureas by Photo-Induced Fluorescence (PIF) and GC-MS

▪ P. A. Diaw1,2,3,4, O. M. A. Mbaye2,3,4, D. D. Thiaré2, N. Oturan3, M. D. Gaye-Seye2,3, A. Coly2, B. Le Jeune2, P. Giamarchi4, M. A. Oturan3, J.-J. Aaron3

Quantitative analysis of diflubenzuron (DFB) and fenuron (FEN) pesticides was successfully performed using photo-induced fluo-rescence (PIF) methods. The analytical conditions were optimized for the determination of traces of these pesticides in Senegalese natural water samples. Mean recoveries were satisfactory, rang-ing between 80 and 120%. Also, gas chromatography-mass spectrometry (GC-MS) was combined with the PIF methods, in order to identify the formed fluorescent photoproducts.


©Imaging L - stock.adobe.com


Articles

Analytical Performances and Applications

First, the analytical performances of both PIF methods were studied. For the classical PIF method, strongly fluorescent photoproducts were obtained at λex/λem = 331/405 nm for DFB in pH4 watermethanol (30:70, v/v) mixture and at 282/343 nm for FEN in pH4 aqueous solution, with low limit of detection (LOD) values of, respectively, 9 and 28 ng mL1. In the case of the DLPIF method, the excitation/emission fluorescence matrix also revealed very fluorescent photoproducts at λex/λem = 240/342 nm for DFB in pH4 water/methanol (30:70, v/v) mixture and at 240/308 nm for FEN in pH4 aqueous solution, with LOD values of 4.5 and 1.5 ng mL1, respectively. A LOD value of 5 ng mL1 in propanol2ol was also reported by Coly and Aaron [4] for the PIF determination of DFB in technical formulations. For analytical applications, a liquidliquid extraction was applied using dichloromethane as extracting solvent. Standard addition method and direct spiking procedure were applied to determine mean recoveries. Standard addition slopes were found to be very close to those measured for the calibration curves. For both methods, the mean recoveries of DFB and FEN in Senegal natural water samples (tap, river and sea water) ranged between about 80 and 120% with relative standard deviation values below 10 %, according to the procedure and type of water sample [1,2].

Interference Studies of Added Foreign Species

Since several commonly used pesticides, namely fluometuron, monolinuron, linuron, carbaryl, pendimethalin and propanil, as well as various inorganic ions (Ca2+, (PO4)2

3; K+, NO3, Na+,

CO3), were generally found in

the Senegal natural waters, their possible interference effects on the determination of DFB and FEN was investigated. The DFB and FEN concentrations were respectively fixed at 0.1 mg mL1 and at 0.015 mg mL1. The tolerance limit of the interfering foreign species was defined as the concentration limit of these interfering species for which the percentage of PIF signal variation did not exceed ± 5% in the determination of DFB and FEN. Addition of foreign species neither changed the shape of DFB and FEN PIF emission spectra, nor shifted the maximum emission wavelength. But, significant PIF intensity changes occurred with

increasing concentrations of foreign species. In the case of the DLPIF method, the addition of increasing concentrations of DFB (up to 2 µg mL1) to a FEN solution (1 µg mL1) did not affect the FEN PIF spectra, because the DFB photoproducts were only formed in a water/methanol mixture, but not in pure water. In contrast, FEN produced relatively high interference effects, since a FEN concentration as low as 0.04 μg mL1 increased the DFB PIF signal above the tolerance limit. It might be explained by the formation of the same PIF FEN photoproduct at λem = 342 nm. To overcome the interference, the PIF signal obtained in water/methanol mixture was corrected by the FEN fluorescence obtained from PIF measurements in pure water [2]. Therefore, a correction factor was applied to take into account the fact that the fluorescence quantum yield of the FEN photoproduct was higher in water/methanol mixture than

Discover more at www.ymc.de

• RP with wide pores & superior stability

• SEC for high resolved MAbs

• IEX for high recovery

• HIC with exceptional effi ciency

Reproducibility in BioLC... ...YMC !

Visit us in MunichHall A1, Booth 405

Mass Spectrometry

Articles


in pure water. This correction minimized the interference effects and improved the PIF selectivity.

Identification of the Fluorescence Photoproducts

Only one fluorescent photoproduct was detected using the classical PIF method at λex/λem = 331/405 nm for DFB and 282/343 nm for FEN. In contrast, the DLPIF method revealed the formation of three fluorescent photoproducts at λex/λem = 225/308 nm (PIF1), 280/342 nm (PIF2) and 295/420 nm (PIF3) for FEN (Fig. 1), and of two fluorescent photoproducts at λex/λem = 230/342 nm (PIF’1) and 220/422 nm (PIF’2) for DFB (Fig. 2) [1,2]. GCMS allowed the identification of these photoproducts by comparing their fluorescence spectral characteristics (Fig. 3) to those of standard compounds (phydroxyaniline and phenol). The two later compounds are known to contribute to the photodegradation pathways of benzoyl and phenylurea pesticides. Indeed, both pesticides presented the same PIF photoproduct at λem = 342 nm than phydroxyaniline. This fluorescence emission wavelength might also correspond to the formation of 3[4(4aminophenyl)] phenyl]1,1dimethylurea, taking place during the photorearrangement of benzoyl and phenylureas [5]. In the case of DLPIF, it was found that the FEN PIF1 presented the same fluorescence characteristics than phenol (λem = 308 nm).

Conclusion

In this work, a simple, inexpensive, sensitive and precise PIF method has been developed for the determination of two benzoyl and phenylurea pesticides, namely diflubenzuron and fenuron, in Senegal natural water samples. Classical PIF and DLPIF methods were found to be of great analytical interest for monitoring both pesticides in natural waters. Also, it can be concluded that the combination of the PIF and DLPIF methods and of GCMS should be suitable to confirm the presence of both pesticides DFB and FEN and their photoproducts in natural waters, and to monitor their evolution in the environment.

Affiliations1 Equipe des Matériaux, Electrochimie et Photochimie Analyt

iques, Université A. Diop, Bambey, Sénégal2 Laboratoire de Photochimie et d’Analyse, Univ. Cheikh. Anta

Diop, Dakar, Sénégal3 Laboratoire Géomatériaux et Environnement (LGE), Université ParisEst MarnelaVallée, Paris, France

4 Laboratoire Optimag, EA 938, Faculté des Sciences, Université de Brest, Brest Cedex, France

ContactProf. Dr. Jean-Jacques AaronLaboratoire Géomatériaux et Environnement (LGE)Université Paris-Est Marne-La-Vallée Paris, [email protected]

Further articles on chromatography: https://bit.ly/WAS-Chromatography

Literatur: http://bit.ly/GLJ-Aaron

Fig. 3: Comparison of the PIF emission spectra of FEN and DFB photopro-ducts (PIF 1, 2 and 3) with the fluorescence emission spectra of the stan-dard compounds (phenol and p-hydroxyaniline) – Figure reprinted with authorization from reference [3].

Fig. 1: Evolution of the photoproducts DL-PIF emission spectra of a FEN aqueous solution (initial concentration = 2.5 μg mL-1) vs. the irradiation time. Laser beam: 240 nm, 1 mJ,10Hz – Figure reprinted with authorization from reference [2].

Fig. 2: Evolution of the excitation/emission fluorescent matrix with laser ir-radiation (at 240 nm) for DFB after 1 min of irradiation – Figure reprinted with authorization from reference [2].


Articles


New, Robust Wide Pore Columns

The new YMCTriart Bio C18 and the recently introduced YMCTriart Bio C4 columns are innovative wide pore phases for RP(U)HPLC. They are based on the modern hybrid silica support from YMC. With a pore size of 300 Å and their specific selectivity, the YMCTriart Bio columns provide the perfect solution for peptide and protein analysis as well as the analysis of antibodies and oligonucleotides. High flexibility in method development is available due to high temperature (up to 90°C) and pH stability (Bio C18: pH 112; Bio C4: pH 110). The superior columntocolumn and lottolot reproducibility guarantees reliable results in quality control for BioLC.

Wide Pore C18 Biocolumns

YMCTriart Bio C18 columns are designed for the separation of proteins and pep

tides with a medium MW e.g. Somatropin (22 kDa) or oligonucleotides. Due to the reduced hydrophobicity compared to conventional C18 phases, it is possible to achieve shorter analysis times for strongly retained substances when using these columns. Also, they are suitable for highly sensitive analytical and structural analysis of proteins using LCMS, due to the excellent peak shapes achieved using LCMS compatible eluents.

Wide Pore C4 Biocolumns

As the YMCTriart Bio C4 columns feature shorter ligands with reduced hydrophobicity their ideal application is the analysis of large proteins. Specifically, intact antibodies can be analysed without restrictions through use of the high temperature column stability. Furthermore, the columns are suitable for the analysis of very hydrophobic proteins and peptides

such as Amyloid β peptides, due to the reduced hydrophobicity of the phase.

Product Options

Both YMCTriart Bio phases are available with 1.9 µm particles for UHPLC together with 3 and 5 µm for HPLC separations. Optional, bioinert columns are available for especially sensitive separations as well as (semi)preparative YMCActus columns for high demanding preparative separations. YMCActus columns can be used at up to 300 bar and allow high sample throughput with long column lifetimes. To analyse very low sample amounts or to achieve high sensitivity, a variety of microLC and nanoLC dimensions are also available.

Innovative UHPLC/HPLC Solutions for BioLCNew UHPLC/HPLC phases for biomolecules such as peptides, proteins, antibodies or oligonucleotides need to possess a variety of demanding criteria. In particular these criteria include high temperature and pH stability, high resolution and MS compatibility. Characteristics such as robustness of the phase and excellent lot-to-lot reproducibility are of the highest priority for the use in quality control. To satisfy these requirements of BioLC users, YMC’s main focus is the production and provision of lasting reliable prod-ucts as well as the development of new and innovative phases.

YMC-Triart Bio C18 and Bio C4 columns are dedicated for the analysis of different biom-olecules: peptides/proteins, antibodies and oli-gonucleotides.

ContactDr. Daniel EßerProduct Manager Analytical ChromatographyYMC Europe GmbHDinslaken, [email protected]

Advertorial 39

Marketplace


ParticleScout: Find, Classify and Identify MicroparticlesWITec’s ParticleScout is a software tool that accelerates and simplifies the workflow of comprehensive microparticle analysis. Confocal Raman microscopy is used for labelfree and nondestructive chemical characterization of the particles.

In a whitelight image of the sample, particles are au

tomatically located and categorized according to physical properties such as area or perimeter. A Raman spectrum is then automatically acquired from each particle and used for chemical identification. To this end, WITec’s TrueMatch Raman database software is seamlessly integrated with ParticleScout. Fi

nally, a comprehensive report on the sample composition is generated. Userselectable filters reveal correlations between the physical and chemical properties of particles.

Key Features of ParticleScout:

▪ accelerated workflow ▪ automated largearea par

ticle survey ▪ userspecified classifica

tion by physical properties

▪ targeted Raman spectral acquisition

▪ fullyintegrated TrueMatch Raman database software

▪ quantitative summaries

ParticleScout is the perfect tool for thorough and detailed microparticle analyses

in microplastics or pharmaceutical research, environmental or food science, and many other fields of application.

Analytica 2020: Hall A2 / booth 406

ContactWITec GmbHUlm, [email protected]

Support for Maintenance Processes Using RFID

RFID handhelds from Pepperl+Fuchs and ecom paired with custom software from Neoception allow for convenient and effi-cient maintenance, even in hazardous ar-eas. Safety is of the utmost importance during the transport of potentially danger-ous process media in chemical processing plants, and regular inspection and mainte-nance of hoses is required by law. RFID handhelds enable maintenance processes to be performed and documented effi-ciently. Each hose is clearly identifiable via a UHF RFID tag, which stores the equipment number, test date and time, the hose length and diameter, its conductivity, the test pressure, and the due date of the next inspection. The auditor is guided by the software through the maintenance procedure step-by-step and the results of the test can be seam-lessly transferred to a back-end system and serve as the documentation and proof of the tests having been carried out.

Pepperl+Fuchswww.pepperl-fuchs.com

Easily Mop Industrial Spills

Brady Corporation introduces the Handy-sorb, a new, practical tool to remove spills in many workplaces. The mop fea-tures an extendable handle and works with engineered pads to safely remove spills in a highly efficient and easy way. It uses inert meltblown polypropylene pads and pillows that do not react with any spilled substance. Its no-touch quick-re-lease system enables users to clean up a wide range of fluids without ever having to touch any of the removed substances. If necessary, the extendable handle can be used to keep a safe distance while re-moving a spill, when fully extended up to 1.83 metres, which also offers easier accessibility in difficult to reach areas. The pads used can absorb spills in sec-onds and absorbs up to 25 times its weight in spilled fluids to reduce waste disposal volume and cost.

Brady Corporationwww.bradycorp.com

Showcase Advertorial

40 Products

Marketplace


Digital Microscope Ensures Quality and Safety of ImplantsMedical aesthetics specialist GC Aesthetics turned to Keyence recently to acquire a new digital microscope. One particular cli-ent requirement was to inspect the sur-face finish on implants to assess vari-ous metrology parameters and surface topography features, patterns, consis-tency and uniformity. Techniques such as scanning electron microscopy-SEM and digital microscopy were previously out-sourced and time-consuming. The VHX-6000 series digital microscope was purchased to have the in-house capability to produce high resolution images of surface to-pographies along with the necessary metrology parameter specific data on sur-face profiles. High volumes of sample data on varied and multiple samples are now available in days, and in some cases hours, compared to before.

Keyencewww.keyence.co.uk

SWIR Camera

The Nirvana HS camera from Tele-dyne Princeton utilizes the advan-tages of the second near-infrared window (NIR-II) window to meet the increasingly diverse needs of today’s scientific, industrial, and medical communities. Building on the high-perfor-mance Nirvana LN (liquid nitro-gen cooled) and the Nirvana 640 (super-cooled), the Nirvana HS version combines speed, flexibility, perfor-mance and value. The HS runs at 250 frames per second in 16 bit mode and offers both integrate-then-read (ITR) and integrate-while-read (IWR) modes for low noise and high duty cycle. The advanced thermal design includes deep cooling to -55 °C and incorporates a vacuum sealed chamber. The man-ufacturer’s Lightfield software provides an intuitive interface and powerful analytical functions, eliminating the need for any third party hardware or software.

Teledyne Princeton Instrumentswww.princetoninstruments.com

Service to Facilitate Target Validation of Deubiquitylase (DUB) EnzymesUbiquigent has launched its DUB profiler-Cell service, which is part of its Drug Discovery Screening Platform. The service supports the development of novel deubiquitylase (DUB) enzyme inhibitors by revealing the active DUBome in a given cell-line or tissue (e.g. non-diseased and diseased), and by reporting the target engagement of test compounds to that active DUBome. By pre-incubat-ing lysates or live cells with test compounds, the assay can be used to evaluate target engagement by compounds. This is the company’s first assay service that incorporates the use of mass spectrometry (MS) to enable an unbiased readout of cellular compound-target engagement, with further new assays planned for launch later this year.

Ubiquigentwww.ubiquigent.com

Operator-Free GMP-Compliant Cell Sorting System

With its new MACS GMP Tyto Cartridge, Miltenyi Biotec opens new possibilities for flu-orescence-based, GMP-com-pliant cell sorting. Specifically developed for the MACS Quant Tyto Cell Sorter, the car-tridge offers GMP-compliant multiparametric, fluorescence-based cell sorting under safe and sterile conditions. The cartridge is already being put to use in the first hu-man iPS trial of Parkinson’s disease, currently taking place at CiRA, Kyoto, where iPS cells were first discovered just twelve years ago. The cell sorter provides high-speed, multiparameter cell sorting in a fully closed system. Cells remain inside the closed cartridge at all times during the sorting process, and no sheath fluid is present in the system, so cells only come in contact with GMP-compliant products.

Miltenyi Biotecwww.miltenyibiotec.com

Compressor-Free Plate Sealer

Thermo Fisher Scientific announces the launch of a next-generation, compressor-free plate sealer, designed to alleviate the mainte-nance burden on operators, while offering unparalleled process customization capabili-ties, intuitive operation and significant work efficiencies. Biotechnology, pharmaceutical and academic research laboratories can now benefit from a system capable of simplifying the plate sealing process and enabling im-proved reliability and productivity for both stand-alone, as well as, integrated robotic projects. As a fully electrically operated system, the Thermo Scientific ALPS 5000 has been developed to increase the efficiency of the heat plate sealing process and offers maximum flexibility to support high throughput applications. The system eliminates the need for te-dious and costly replacement of expensive vacuum cups, onboard compressors and compressed air lines, typically required when using conventional pneumati-cally driven equipment.

Thermo Fisher Scientificwww.thermofisher.com

Integrated Encoder for Flat Motors

The BXT motor family from Faulhaber, comprising brushless DC-motors with an especially short design, has been expanded with the diameter-complaint IEF3-4096 magnetic encoder. With just 6.2 mm of additional length, the motor/en-coder units also remain extremely short. The encoder is fully integrated in the robust motor housing. In this flat design, the IEF3-4096 offers three channels with index function and a high resolution of up to 4096 lines per revolution. A variant with line driver is also available with the IEF3-4096 L. The encoder can be combined with the 2214…BXT H, 3216…BXT H and 4221…BXT H housed BXT motors.

Faulhaberwww.faulhaber.com

Products 41

Marketplace


Extracellular Vesicles-Focused Analytical Services

Exosomics has implemented NanoFCM Nanoanalyzer instrument at its Siena, Italy, facility to offer sophisticated contract research and measurement services worldwide and has become an approved service supplier of nano-flow cytome-try measurements. These can be performed as stand-alone or coupled to solu-tions provided by Exosomics who will be able to supply a wide range of nano-flow cytometry measurements. The instrument will also allow the company to further develop its own liquid biopsy pipeline, which requires the highest level of accuracy and reproducibility. The Nanoanalyzer is designed For Research Use Only. It is not for use in diagnostic procedures.

Exosomicswww.exosomics.eu

Vacuum Pump with Long-Term Performance

In addition to the intelligent and easy control of vacuum in the laboratory, the PC 3001 Vario select from Vacuubrand has been spe-cially designed for reliability and long-term performance. The combination of variable-speed Vario chemistry diaphragm pump and the Vacuu Select vacuum controller give the pump long service intervals, high reliability and whisper-quiet operation. The combination of special fluoroplastics that are used in construction guarantees uncompromising chemical resistance while the extreme diaphragm life of the vacuum pump of typically 15,000 operating hours is significantly extended by the automatic speed adjustment of the motor. Diaphragm pumps require neither oil nor water and are therefore very environmentally friendly and particularly easy to clean. As a special campaign, Vacuubrand offer a warranty extension of three years for all PC 3001 Vario select pumping stations until 31st March 2020.

Vacuubrandwww.vacuubrand.com

Wells for Cost-Effective Cell Culture and High-Resolution MicroscopyWith its thin polymer cov-erslip bottom, the µ-Slide 18 Well from Ibidi enables excellent cell adhesion onto the tissue culture-treated surface. In addi-tion, it has a high optical quality and is ideally suit-ed for a variety of micro-scopic techniques such as widefield fluorescence, confocal microscopy and DIC. For scientists who perform special microscopic applications, such as TIRF and super-resolution microscopy, the company offers the µ-Slide 18 Well Glass Bottom with a #1.5H D 263 M Schott glass. It is also available as a sticky-Slide 18 Well without any bottom, which enables the researcher to mount any chosen substrate. The entire µ-Slide 18 Well family is ideal for experiments with small cell numbers and low reagent volumes. The spaces between the individual well walls minimize any well-to-well crosstalk and contamination. Scientists who would like to test one of the variations with their own experiments can request free samples.

Ibidiwww.ibidi.com

Solvent Removal Evaporators

SP Scientific has launched its HT Series 3i Evaporators, the updated replacements for the highly successful HT Series 3 evapora-tor range. They have been developed to be even more user and environment-friendly, while enabling enhanced evaporation and lyophilization results. Anti-bumping tech-nology prevents foaming and bumping to eliminate cross-contamination and sample loss. The high-performance dry vacuum pump, and F-Gas compliant -75 °C auto-defrost and draining condenser with R449A and R170 refrigerants, ensure fast, controlled evaporation of all sample types, yet with a low environmental im-pact and global warming potential. Simplified help screens, and improved pre-set routine and automatic programming, allow the most complex, multi-stage evapo-ration methods to be performed quickly and easily, even by occasional users.

SP Scientificwww.spscientific.com

Visible/SWIR Machine Vision and Microscopy Camera

Princeton Infrared Technologies recently launched its compact MV Cam series short-wave-infrared (SWIR) and visible camera that supports a high frame rate at mega-pixel resolution with no ITAR restrictions. The megapixel indium gallium arsenide (In-GaAs) camera provides 1280 x 1024 reso-lution SWIR imagery at up to 95 frames per second, with higher frame rates for user-selectable regions of interest. At 12 µm pixel pitch, the MV Cam InGaAs image sensor yields extremely low dark current and high quantum efficiency, providing sensitivity across the SWIR and visible wavelength bands from 0.4 to 1.7 µm. The standard camera configuration uses a single-stage thermoelectric cooler with no moving parts, integrated in a sealed package to stabilize the image sensor at 20 °C. MV Cam’s advanced digital array (PIRT1280A1-12) generates 14-bit digital image data with no image lag and read noise less than 45 e-.

Princeton Infrared Technologieswww.princetonirtech.com

Improved Image Analysis Method for Steel Quality ControlThe release of Olympus Stream image analysis software version 2.4.2 in-cludes an improved image analysis so-lution to measure and rate non-metal-lic inclusion content in high-purity steel. The mode detects and classifies individual fields on a large scan area, expanding on the software’s capabilities to detect and classify individual inclusions in worst field mode and providing statistical results of inclusion content on the entire scan area ac-cording to three international standards: ASTM E45-18 (method D), ISO 4967:2013 (method B) and EN 10247:2017 (method K). The new version also optimizes Olympus Stream software for the Schott Visiled controller MC 1500, enabling users to easily control LED ring light illumination on their stereo micro-scopes and remove halation caused by LED reflection on the sample surface.

Olympuswww.olympus-ims.com

42 Products

Marketplace

IMPRINT

Published byWiley-VCH Verlag GmbH & Co. KGaAA Company of John Wiley & Sons, IncGIT VERLAGBoschstr. 12, 69469 Weinheim, GermanyTel.: +49 6201 606 0

GeschäftsführerSabine HaagGuido F. Herrmann

DirectorRoy Opie

Publishing DirectorHeiko Baumgartner

Director Corporate Sales PSEDr. Katja Habermüller

Editor in ChiefDr. Martin Graf-Utzmann Tel.: +49 6201 606 [email protected]

Editorial TeamDr. Christina PoggelTel.: +49 6201 606 [email protected]

Dr. Birgit WashburnTel.: +49 6201 606 [email protected]

Isabel BrenneisenTel.: +49 6201 606 [email protected]

Corinna HerbstTel.: +49 6201 606 [email protected]

FreelancerDr. Martin FriedrichTel.: 0178/4596064 · 0178/[email protected]

Segment Sales Manager Laboratory & BiotechnologyVanessa WindeTel.: +49 6201 606 [email protected]

Media ConsultantsDr. Stefanie KrauthTel.: +49 6201 606 [email protected]

Bettina WillnowTel.: +49 6201 606 [email protected]

Sales RepresentativeDr. Michael LeisingTel.: +49 6131 88 39 22 · Fax: [email protected]

Sales AdministratorKerstin KunkelTel.: +49 6201 606 731 · Fax: [email protected]

Wiley GIT Customer Service65341 Eltville / Germany Phone: +49 6123 9238 246Fax: +49 6123 9238 244E-Mail: [email protected] service is available for you from Monday to Friday 8 am – 5 pm CET

ProductionWiley-VCH Verlag GmbH & Co. KGaAA Company of John Wiley & Sons, IncGIT VERLAG

Jörg StengerTel.: +49 6201 606 742 · Fax: [email protected]

ReprintsCorinna MatzTel.: +49 6201 606 [email protected]

Printed bypva, Druck und Medien, Landau, Germany

Circulation20,000 copies, 4 times per annumAdvertising price list from October 1st 2019

Subscription 2020Four issues € 55.00 (+VAT), single copy € 16.30 plus VAT and postage. Pupils and students receive a discount of 50% at sight of a valid certificate. Subscription orders can be revoked within one week in writing. Dispatch complaints are possible only within four weeks after publishing date. Subscription cancellations are accepted six weeks before end of year.

Bank accountJ.P. Morgan AG, FrankfurtKonto-Nr. 6161517443BLZ: 501 108 00BIC: CHAS DE FFXXXIBAN: DE55501108006161517443

Specially identified contributions are the responsibility of the author. Manuscripts should be addressed to the editorial office. We assume no liability for unsolicited, submitted manuscripts. Reproduction, including excerpts, is permitted only with the permission of the editorial office and with citation of the source.

The publishing house is granted the exclusive right, with regard to space, time and content to use the works/ editorial contributions in unchanged or edited form for any and all purposes any number of times itself, or to transfer the rights for the use of other organizations in which it holds partnership interests, as well as to third parties. This right of use relates to print as well as electronic media, including the Internet, as well as databases/ data carriers of any kind.

All names, designations or signs in this issue, whether referred to and/or shown, could be trade names of the respective owner.

Printed in GermanyISSN 1611-6038www.gitverlag.com

Bio-Rad Laboratories 16

Brady Corporation 40

Celisca Center for Life Science Automation 26

Dr. Fritz Faulhaber 41

Empa – Materials Science and Technology 28

Exosomics 42

Hahnemühle Fineart 3

Ibidi 42

Institut für Energie- und Umwelttechnik (IUTA) 24

Keyence UK 41

Metrohm Titelseite, 12

Miltenyi Biotec 41

Olympus 42

Paperless Lab Academy 6

Pepperl+Fuchs 40

Polyscience 19, 21, 23, 25, 27, 29

Princeton Instruments 42

Shimadzu Europa 18, 4. US

Socorex Isba 33

SP Scientific 42

The Francis Crick Institute 14

Thermo Fisher Scientific 41

Ubiquigent 41

Universidad Nacional de Rosario 20

Université Paris-Est Marne-La-Vallée 36

University of Michigan 9

University of Utrecht 32

Vacuubrand 42

Witec 40

YMC Europe 37, 39

Surfing different wavesApplying different wavelengths, the compact UV-2600/2700i series of research grade UV-VIS spectrophotometers enables high-precision spectral analysis. It is based on the Shimadzu LO-RAY-LIGH® diffraction gratings optical system and covers a wide range of applications such as organic and inorganic compounds, biological samples, optical materials and photovoltaics. User-friendly economic design with smallest footprint in its class, energy saving electronics, comprehensive system control soft-ware including validation, USB connection as well as the widest scope of accessories

Wide wavelength range of up to 1,400 nm enables expanded research of photovoltaics with UV-2600i High absorbance level of the UV-2700i double monochromator optics allows measurement of high density samples up to 8 Abs. Ultra low stray light Shimadzu gratings offering “best in class” performance

www.shimadzu.eu /uv-2600i-uv-2700i

UV-2700i – UV-VIS Spectrophotometer

Shimadzu_GIT_032020.qxp_A4 25.02.20 15:28 Seite 1

Date post:	20-May-2020
Category:	Documents
Upload:	others
View:	4 times
Download:	0 times

Eligible authors at German institutions may publish open ... · 3, 2020. A 4hour workshop in which...

Documents