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«Analyze This»: 2020 in review

«Analyze This»: 2020 in review

I wanted to end 2020 by thanking all of you for making «Analyze This» – the Metrohm blog for chemists such a success! For our 60th blog post, I’d like to look back and focus on the wealth of interesting topics we have published this year. There is truly something for everyone: it doesn’t matter whether your lab focuses on titration or spectroscopic techniques, or analyzes water samples or illicit substances – we’ve got you covered! If you’re looking to answer your most burning chemical analysis questions, we have FAQs and other series full of advice from the experts. Or if you’re just in the mood to learn something new in a few minutes, there are several posts about the chemical world to discover.

We love to hear back from you as well. Leaving comments on your favorite blog posts or contacting us through social media are great ways to voice your opinion—we at Metrohm are here for you!

Finally, I wish you and your families a safe, restful holiday season. «Analyze This» will return on January 11, 2021, so subscribe if you haven’t already done so, and bookmark this page for an overview of all of our articles grouped by topic!

Stay healthy, and stay curious.

Best wishes,

Dr. Alyson Lanciki, Scientific Editor, Metrohm AG

Quickly jump directly to any section by clicking a topic:

Customer Stories

We are curious by nature, and enjoy hearing about the variety of projects where our products are being used! For some examples of interesting situations where Metrohm analytical equipment is utilized, read on.

From underwater archaeological research to orbiting Earth on the International Space Station, Metrohm is there! We assist on all types of projects, like brewing top quality beers and even growing antibiotic-free shrimp – right here in Switzerland.

Interested in being featured? Contact your local Metrohm dealer for details!

Titration

Metrohm is the global market leader in analytical instruments for titration. Who else is better then to advise you in this area? Our experts are eager to share their knowledge with you, and show this with the abundance of topics they have contributed this year to our blog.

For more in-depth information about obtaining the most accurate pH measurements, take a look at our FAQ about pH calibration or read about avoiding the most common mistakes in pH measurement. You may pick up a few tips!

Choose the best electrode for your needs and keep it in top condition with our best practices, and then learn how to standardize titrant properly. Better understand what to consider during back-titration, check out thermometric titration and its advantages and applications, or read about the most common challenges and how to overcome them when carrying out complexometric titrations

If you are interested in improving your conductivity measurements, measuring dissolved oxygen, or the determination of oxidation in edible fats and oils, check out these blog posts and download our free Application Notes and White Papers!

Finally, this article about comprehensive water analysis with a combination of titration and ion chromatography explains the many benefits for laboratories with large sample loads. The history behind the TitrIC analysis system used for these studies can be found in a separate blog post.

Karl Fischer Titration

Metrohm and Karl Fischer titration: a long history of success. Looking back on more than half a century of experience in KFT, Metrohm has shaped what coulometric and volumetric water analysis are today.

Aside from the other titration blog posts, our experts have also written a 2-part series including 20 of the most frequently asked questions for KFT arranged into three categories: instrument preparation and handling, titration troubleshooting, and the oven technique. Our article about how to properly standardize Karl Fischer titrant will take you step by step through the process to obtain correct results.

For more specific questions, read about the oven method for sample preparation, or which is the best technique to choose when measuring moisture in certain situations: Karl Fischer titration, near-infrared spectroscopy, or both?

Ion Chromatography (IC)

Ion chromatography has been a part of the Metrohm portfolio since the late 1980s. From routine IC analysis to research and development, and from stand-alone analyzers to fully automated systems, Metrohm has provided IC solutions for all situations. If you’re curious about the backstory of R&D, check out the ongoing series about the history of IC at Metrohm.

Metrohm IC user sitting at a laboratory bench.

Common questions for users are answered in blog posts about IC column tips and tricks and Metrohm inline ultrafiltration. Clear calculations showing how to increase productivity and profitability in environmental analysis with IC perfectly complement our article about comprehensive water analysis using IC and titration together for faster sample throughput.

On the topic of foods and beverages, you can find out how to determine total sulfite faster and easier than ever, measure herbicides in drinking water, or even learn how Metrohm IC is used in Switzerland to grow shrimp!

Near-Infrared Spectroscopy (NIRS)

Metrohm NIRS analyzers for the lab and for process analysis enable you to perform routine analysis quickly and with confidence – without requiring sample preparation or additional reagents and yielding results in less than a minute. Combining visible (Vis) and near-infrared (NIR) spectroscopy, these analyzers are capable of performing qualitative analysis of various materials and quantitative analysis of a number of physical and chemical parameters in one run.

Our experts have written all about the benefits of NIR spectroscopy in a 4-part series, which includes an explanation of the advantages of NIRS over conventional wet chemical analysis methods, differences between NIR and IR spectroscopy, how to implement NIRS in your laboratory workflow, and examples of how pre-calibrations make implementation even quicker.

A comparison between NIRS and the Karl Fischer titration method for moisture analysis is made in a dedicated article.

A 2-part FAQ about NIRS has also been written in a collaboration between our laboratory and process analysis colleagues, covering all kinds of questions related to both worlds.

Raman Spectroscopy

This latest addition to the Metrohm family expands the Metrohm portfolio to include novel, portable instruments for materials identification and verification. We offer both Metrohm Raman as well as B&W Tek products to cover a variety of needs and requirements.

Here you can find out some of the history of Raman spectroscopy including the origin story behind Mira, the handheld Raman instrument from Metrohm Raman. For a real-world situation involving methamphetamine identification by law enforcement and first responders, read about Mira DS in action – detecting drugs safely in the field.

Mira - handheld Raman keeping you safe in hazardous situations.

Are you looking for an easier way to detect food fraud? Our article about Misa describes its detection capabilities and provides several free Application Notes for download.

Process Analytics

We cater to both: the laboratory and the production floor. The techniques and methods for laboratory analysis are also available for automated in-process analysis with the Metrohm Process Analytics brand of industrial process analyzers.

Learn about how Metrohm became pioneers in the process world—developing the world’s first online wet chemistry process analyzer, and find out how Metrohm’s modular IC expertise has been used to push the limits in the industrial process optimization.

Additionally, a 2-part FAQ has been written about near-infrared spectroscopy by both laboratory and process analysis experts, which is helpful when starting out or even if you’re an advanced user.

Finally, we offer a 3-part series about the advantages of process analytical technology (PAT) covering the topics of process automation advantages, digital networking of production plants, and error and risk minimization in process analysis.

Voltammetry (VA)

Voltammetry is an electrochemical method for the determination of trace and ultratrace concentrations of heavy metals and other electrochemically active substances. Both benchtop and portable options are available with a variety of electrodes to choose from, allowing analysis in any situation.

A 5-part series about solid-state electrodes covers a range of new sensors suitable for the determination of «heavy metals» using voltammetric methods. This series offers information and example applications for the Bi drop electrode, scTrace Gold electrode (as well as a modified version), screen-printed electrodes, and the glassy carbon rotating disc electrode.

Come underwater with Metrohm and Hublot in our blog post as they try to find the missing pieces of the ancient Antikythera Mechanism in Greece with voltammetry.

If you’d like to learn about the combination of voltammetry with ion chromatography and the expanded application capabilities, take a look at our article about combined analysis techniques.

Electrochemistry (EC)

Electrochemistry plays an important role in groundbreaking technologies such as battery research, fuel cells, and photovoltaics. Metrohm’s electrochemistry portfolio covers everything from potentiostats/galvanostats to accessories and software.

Our two subsidiaries specializing in electrochemistry, Metrohm Autolab (Utrecht, Netherlands) and Metrohm DropSens (Asturias, Spain) develop and produce a comprehensive portfolio of electrochemistry equipment.

This year, the COVID-19 pandemic has been at the top of the news, and with it came the discussion of testing – how reliable or accurate was the data? In our blog post about virus detection with screen-printed electrodes, we explain the differences between different testing methods and their drawbacks, the many benefits of electrochemical testing methods, and provide a free informative White Paper for interested laboratories involved in this research.

Our electrochemistry instruments have also gone to the International Space Station as part of a research project to more efficiently recycle water on board spacecraft for long-term missions.

The History of…

Stories inspire people, illuminating the origins of theories, concepts, and technologies that we may have become to take for granted. Metrohm aims to inspire chemists—young and old—to be the best and never stop learning. Here, you can find our blog posts that tell the stories behind the scenes, including the Metrohm founder Bertold Suhner.

Bertold Suhner, founder of Metrohm.

For more history behind the research and development behind Metrohm products, take a look at our series about the history of IC at Metrohm, or read about how Mira became mobile. If you are more interested in process analysis, then check out the story about the world’s first process analyzer, built by Metrohm Process Analytics.

Need something lighter? Then the 4-part history of chemistry series may be just what you’re looking for.

Specialty Topics

Some articles do not fit neatly into the same groups as the rest, but are nonetheless filled with informative content! Here you can find an overview of Metrohm’s free webinars, grouped by measurement technique.

If you work in a regulated industry such as pharmaceutical manufacturing or food and beverage production, don’t miss our introduction to Analytical Instrument Qualification and what it can mean for consumer safety!

Industry-focused

Finally, if you are more interested in reading articles related to the industry you work in, here are some compilations of our blog posts in various areas including pharmaceutical, illicit substances, food and beverages, and of course water analysis. More applications and information can be found on our website.

Food and beverages
All of these products can be measured for total sulfite content.

Oxidation stability is an estimate of how quickly a fat or oil will become rancid. It is a standard parameter of quality control in the production of oils and fats in the food industry or for the incoming goods inspection in processing facilities. To learn more about how to determine if your edible oils are rancid, read our blog post.

Determining total sulfite in foods and beverages has never been faster or easier than with our IC method. Read on about how to perform this notoriously frustrating analysis and get more details in our free LC/GC The Column article available for download within.

Measuring the true sodium content in foodstuff directly and inexpensively is possible using thermometric titration, which is discussed in more detail here. To find out the best way to determine moisture content in foods, our experts have written a blog post about the differences between Karl Fischer titration and near-infrared spectroscopy methods.

To determine if foods, beverages, spices, and more are adulterated, you no longer have to wait for the lab. With Misa, it is possible to measure a variety of illicit substances in complex matrices within minutes, even on the go.

All of these products can be measured for total sulfite content.

Making high quality products is a subject we are passionate about. This article discusses improving beer brewing practices and focuses on the tailor-made system built for Feldschlösschen, Switzerland’s largest brewer.

Pharmaceutical / healthcare

Like the food sector, pharmaceutical manufacturing is a very tightly regulated industry. Consumer health is on the line if quality drops.

Ensuring that the analytical instruments used in the production processes are professionally qualified is a must, especially when auditors come knocking. Find out more about this step in our blog post about Analytical Instrument Qualification (AIQ).

Moisture content in the excipients, active ingredients, and in the final product is imperative to measure. This can be accomplished with different analytical methods, which we compare and contrast for you here.

The topic of virus detection has been on the minds of everyone this year. In this blog post, we discuss virus detection based on screen-printed electrodes, which are a more cost-effective and customizable option compared to other conventional techniques.

Water analysis

Water is our business. From trace analysis up to high concentration determinations, Metrohm has you covered with a variety of analytical measurement techniques and methods developed by the experts.

Learn how to increase productivity and profitability in environmental analysis laboratories with IC with a real life example and cost calculations, or read about how one of our customers in Switzerland uses automated Metrohm IC to monitor the water quality in shrimp breeding pools.

If heavy metal analysis is what you are interested in, then you may find our 5-part series about trace analysis with solid-state electrodes very handy.

Unwanted substances may find their way into our water supply through agricultural practices. Find out an easier way to determine herbicides in drinking water here!

Water is arguably one of the most important ingredients in the brewing process. Determination of major anions and cations along with other parameters such as alkalinity are described in our blog post celebrating International Beer Day.

All of these products can be measured for total sulfite content.
Illicit / harmful substances

When you are unsure if your expensive spices are real or just a colored powder, if your dairy products have been adulterated with melamine, or fruits and vegetables were sprayed with illegal pesticides, it’s time to test for food fraud. Read our blog post about simple, fast determination of illicit substances in foods and beverages for more information.

Detection of drugs, explosives, and other illegal substances can be performed safely by law enforcement officers and first responders without the need for a lab or chemicals with Mira DS. Here you can read about a real life training to identify a methamphetamine laboratory.

Drinking water regulations are put in place by authorities out of concern for our health. Herbicides are important to measure in our drinking water as they have been found to be carcinogenic in many instances.

Post written by Dr. Alyson Lanciki, Scientific Editor at Metrohm International Headquarters, Herisau, Switzerland.

Real World Raman: Mira DS in Action – Detecting drugs safely in the field

Real World Raman: Mira DS in Action – Detecting drugs safely in the field

Methamphetamine (meth, Figure 1) abuse is one of the top drug problems impacting the social, economic, and health welfare of many developed and developing countries. Short-term use of meth, a powerful stimulant, provides a euphoric sense of alertness and enhanced capability for work-related activities. Chronic use inevitably leads to addiction, antisocial and sometimes violent criminal behavior, and a pronounced decline in the overall health and well-being of the user.

The proliferation and use of meth across the US, Asia, and Europe is aided by underground «kitchen» laboratories, which are the primary source of clandestine meth production and distribution.

Figure 1. Methamphetamine crystals.

Meth can be easily synthesized from pseudoephedrine extracted from over-the-counter cold medications (Figure 2) and easily purchased commercial products enriched in required reagents.

Figure 2. Pseudoephedrine tablets.

A number of different procedures have been adopted for the clandestine synthesis of meth. However, the widespread one-pot «Shake and Bake» method is uniquely adapted for covert small-scale cooking operations due to the inherent simplicity of the chemical reaction and laboratory setup.

Increasingly, methamphetamine production has moved from large-scale laboratory operations to small-scale syntheses using one-pot methods. To address this challenge, police must identify the contents of potential reaction vessels and establish a pattern of production within a discrete geographical area in order to apprehend and convict methamphetamine producers.

The target in these cases can be a discarded glass jar or plastic drink bottle containing reaction residue (Figure 3).

Figure 3. Plastic waste that appears to be the remains of a clandestine meth laboratory.

Effective suppression of meth production requires rapid confirmation of meth, or its related precursors and byproducts. Ideally, such tests are performed at the scene of suspected primitive «cooking» facilities by drug enforcement officers and first responders. On-site detection must utilize instrumentation that is compact, cost-effective, fast, and incorporates user-friendly operation procedures. 

However, rapid and portable detection capabilities for front-line law enforcement officers are lacking. These include pH strips, direct observation of odors, lab-related trash and chemical containers, and notoriously unreliable colorimetric tests. The alternative is laboratory analysis, which is complicated due to costs, time, transport, and availability.

Handheld Raman is a relatively new method that streamlines field identification of potentially flammable and explosive residues in one-pot vessels (Figure 4). Sampling and identification occurs through plastic and glass surfaces, ensuring police safety by reducing exposure to potentially hazardous materials.

Figure 4. Metrohm Raman Mira DS identifying meth in the field through a glass jar.
Did you read our last blog about handheld Raman at Metrohm? If not, read it here!

In this article, the advantage of using handheld Raman to obtain forensic evidence linking a suspected «cook» site with meth production is demonstrated. Mira DS is Metrohm’s premier handheld Raman system designed to meet the needs of first responders (Figure 5). 

Figure 5. Metrohm Raman Mira DS and optional measurement attachments for the simple identification of illicit and hazardous materials.
Want to find out more about Mira DS? Visit our website!

Unlike trained analytical scientists, defense and security professionals need a solution that gives them instant results without complicated routines. With Smart Acquire, Mira DS is a point-and-shoot solution. Simply power up the instrument, touch the screen once to activate the laser and again to take a sample, then Mira DS automatically optimizes acquisition parameters, processes data, identifies the target through library matching, and delivers the results with relevant chemical warnings – all in less than a minute. When Mira DS is used with MiraCal M mobile software, these results can be shared instantly to alert others of potential danger.

 

Response Team Training with Mira DS

Simulated testing of a small-scale meth production facility was conducted in the US Midwest by the Security and Defense directorate of Metrohm USA to support Civil Support Team (CST) Training. During the Civil Support Skills CBRNE Course training, first responders are taught to recognize laboratories in which Chemical, Biological, Radiological, Nuclear or high-yield Explosive materials are being manufactured or manipulated.

Equipped with a detailed education in weapons of mass destruction and drug chemistry, attendees are required to recreate and evaluate realistic clandestine laboratories using innovative methods (Figure 6). Upon the successful completion of training, CST graduates possess unique capabilities, expertise, and an in-depth command of the technologies required for responding to CBRNE defense scenarios.

Figure 6. Images of CST test site for illicit chemical synthesis using Mira DS with Standoff Attachment for safe measurement.

During CST training, meth was synthesized using the one pot «Shake and Bake» method. This is the preferred route for making meth in low resource labs, despite relatively low product purity. The key ingredients for synthesis are easily sourced from hardware and drug stores. Preparatory procedures, the chemical reaction steps, and drug recovery can be performed in a few hours using emptied glass jars or plastic beverage bottles, tape, and tubing. Plastic is preferred to glass, as the risk of explosion during the course of the reaction is very high.

For more information about our Standoff Attachment, visit our website and watch the video below!

Testing for illicit substances is simple with Mira DS

Trainees used Mira DS (Figure 5), a handheld Raman device, to directly interrogate liquid waste in glass jars at a simulated cook site directly through the container material. Attachments for Mira DS snap on with a simple magnetic interface. Figure 7 shows the analysis of the actual one-pot meth reaction waste, seen as a bi-phasic liquid layer that remained following the removal of product. 

First, the Intelligent Universal Attachment (iUA) was used in its «bottle» setting to test each liquid waste layer directly through the glass. This attachment has three settings, including «surface» for direct contact with a material, and «bag» and «bottle» for sampling through thin and thick barriers.

Figure 7. Mira DS with Intelligent Universal Attachment in use at CST training, testing bi-phasic one-pot meth reaction waste. Left: measuring the bottom (yellow) layer – identified as calcium nitrate. Right: measuring the top (orange) layer – identified as acetone.

Next, the Contact Ball Probe Attachment (CBP) was used to confirm the identity of the waste. CBP is a chemically resistant quick dip solution for direct sampling, and can be used with both liquids and powdered solids.

In short, Mira DS was outfitted with an attachment, powered up, the laser activated, and testing initiated using the touch screen. On-board Smart Acquire algorithms automatically optimize acquisition parameters (Laser Power, Integration Time, Averaging, etc.), process spectral data, perform library searches and matching for the user, and report results in under a minute with color-coded chemical warnings and alerts.

Results of the CST training

The library spectral stack in Figure 8 includes the product, methamphetamine, and reagents used in its synthesis during the training course. Actual data acquired during both training and real-world testing scenarios can be expected to be «messy» due to substandard reaction conditions and resulting complex chemical mixtures. Mira DS addresses this challenge by automatically correlating acquired spectra with library spectra of illicit substances, performing Mixture Matching routines, and rapidly reporting the top matches.

Figure 8. Raman Illicit Library reference spectra for the major reagents used in one-pot meth production (click to enlarge).

To learn more about identifying narcotics in complex samples using handheld Raman, download our free white paper!

To summarize, Mira DS is capable of rapidly identifying key components of a popular method for clandestine meth synthesis. Two notable aspects of these results:

  • additional peaks in experimental spectra correlate with unidentified reaction byproducts, but
  • the excellent spectral resolution here, reinforced by very high correlation (HQI) scores, is a reflection of the suitability of handheld Raman as an on-site analytical tool.

In real world situations, first responders must maintain their training and stay current regarding the diverse materials and methods they are likely to encounter to ensure that Raman library entries are up to date.

Conclusion

In most situations, the product has already been removed from the cook site. Therefore one-pot meth site inspection does not realistically result in a methamphetamine identification, but the discarded waste chemicals can provide forensic evidence of meth production. These results illustrate the unique capabilities of handheld Raman in the hands of law enforcement in real world scenarios. This technique is powerful in several ways:

  • Data can be collected on-site and shared electronically for increased technical support
  • No-contact sampling of container contents reduces danger during investigation
  • Results are given in a few seconds
  • Mixture Matching provides results for real world scenarios
  • Results provide forensic evidence to link a suspected cook site with methamphetamine production

Mira DS is a promising and robust analytical tool for obtaining corroborative forensic evidence and successfully prosecuting drug crime.

Learn more about Mira DS in action in our next installment of the Real World Raman series!

Download our free white paper

Safety in Any Situation – Addressing the needs of first responders

Post written by Dr. Mark Harpster (Research Scientist, University of Wyoming/Applications Chemist, Metrohm Raman, Laramie, Wyoming, USA), Dr. Melissa J. Gelwicks (Applications Chemist, Metrohm Raman, Laramie, Wyoming, USA), and Dr. Bryan H. Ray (WMD Clandestine Production Laboratory Site Safety Officer Course/Civil Support Skills CBRNE Course Instructor, Metrohm USA, Tampa, Florida).