academia 11 weighing and analysis in the laboratory news · 2020-01-24 · and developing...

Weighing and Analysis in the Laboratory

Ocean acidification has emerged as a major research focus in the study

of global biological changes in the world’s oceans. The METTLER TOLEDO

T50 Excellence Titrator helped a study at the University of California,

in Santa Barbara, to maintain the exact conditions necessary to provide

quality data on such a critical topic with possible serious ecological

consequences.

The uptake of anthropogenic carbon di-oxide from the atmosphere by the oceans has caused a decrease in oceanic pH. This process is known as ocean acidifi-cation. Changes in ocean chemistry can have extensive direct and indirect effects on organisms and their habitats. One of the most important repercussions of in-creasing ocean acidity relates to the dis-solution of shells, plates and coral reefs made of calcium carbonate. As the rate of change in the physical environment, as a result of anthropogenic influence, will likely occur faster than biologi-cal adaptation or microevolution can occur, ocean acidification has recently emerged as a major research theme in marine biology. One major research ac-tivity has been to explore the effects of elevated CO2, lowered pH, and/or altered

carbonate chemistry on the physiological performance of marine organisms in ma-nipulative laboratory experiments.

Total alkalinityTotal alkalinity is one fundamental analysis used to monitor the progress of acidification in seawater and is often de-termined together with pH, temperature and salinity. The Department of Ecol-ogy, Evolution and Marine Biology at the University of California in Santa Barbara monitored the total alkalinity with the METTLER TOLEDO T50 Excellence Titra-tor in a laboratory-based experimental study of ocean acidification effects on marine invertebrate larvae. The experi-mental system was designed to test the response of marine invertebrate embryos and larvae to different levels of CO2-acid-

Measuring Climate Change on Ocean LifeWith a T50 Titrator

11News

AcademiaAnalytical solutions in the laboratory

Edition 01/2012

2 METTLER TOLEDO Academia News 11

Titra

tion

Publisher Mettler-Toledo AG Laboratory Division Im Langacher CH-8606 Greifensee, Switzerland

Production Segment Marketing LABGlobal MarCom Switzerland

Subject to technical changes. © Mettler-Toledo AG 02/12 Printed in Switzerland.

ified seawater under tightly controlled water chemistry conditions.

Total alkalinity is defined as the amount of acid required in order to lower the sample pH to the point where all the bi-carbonate and carbonate could be con-verted to carbonic acid. This can be regard-ed as the buffering capacity of seawater. Analytically, total alkalinity in seawater is determined by a potentiometric titra-tion with hydrochloric acid to an equiva-lence point in the pH region of between 3.0 and 3.6.

Titration ExcellenceThanks to the intuitive One Click Titra-tion usability concept, the total alkalinity could be easily determined daily with the T50 Excellence Titrator. As the dissolu-tion of CO2 is affected by temperature, a thermostatable titration beaker was used together with the titrator during this study to set the temperature at a constant 25 °C. With LabX titration software, all data could be collected reliably and efficiently.

The Titration Excellence line offers many useful features, including the automatic recognition of plug & play sensors, in-telligent burettes and newly connected

components without any further con-figuration and a thorough method data-base that enables the easy adaptation of procedures to your current studies. The T50 Excellence Titrator helped in this lab-oratory experiment by maintaining the exact conditions necessary to efficiently study the current physiological plasticity possessed by marine organisms.

Read the full study, Fangue, Nann A. (2010) "A Laboratory-Based, Experimental System for the Study of Ocean Acidification Effects on Marine Invertebrate Larvae" Limnology and Oceanography Methods, 8.

Text: Claudia Keller, Product Management Titration

www.mt.com/one-click-titration

Photo 1: Acropora digitifera. Photo 2: Chromis viridis. Photo 3: Unidentified Gorgonian fan. (personal photos by Dipl.- Biol. (technically oriented) Markus Keller )

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Flash DSC Technology Revolutionizes Polymer Physics

The Flash DSC 1 is a completely new type of DSC instrument. It has

been developed to obtain not previously available information about

the formation of structure and reorganization of metastable materials

through the use of extremely high heating and cooling rates.

Flash DSC 1 is a completely new type of commercial DSC with a signal time con-stant of less than 1 millisecond. This allows very high heating and cooling rates to be achieved. Although the time constant is so short, the sensitivity of the DSC is still excellent so that measure-ments can also be performed at rela-tively low heating rates. The heating rate range is 1 K/s to 40 000 K/s (60 K/min to 2 400 000 K/min). The maximum cool-ing rate achieved is 4 000 K/s (240 000 K/min).

Isothermal crystallization of isotactic polypropylene (iPP)High cooling rates and rapid switching from cooling to isothermal conditions

(Figure 1) allow fast crystallization pro-cesses to be measured.

The crystallization of isotactic polypro-pylene (iPP) was measured at different crystallization temperatures after cool-ing from the melt at 2000 K/s. Some of the curves are displayed in Figure 2. The time to the crystallization peak charac-terizes the crystallization rate. At 100 °C, the material crystallizes relatively slowly with a peak time of about 2.5 seconds. The curves show that the crystallization rate first increases with decreasing crys-tallization temperature. The peak time at 80 °C reaches a minimum of 0.4 seconds. At lower crystallization temperatures, the crystallization rate then decreases due to

Figure 1: Behavior of the sample temperature after cooling to 50 °C at 1000 K/s.

reduced molecular mobility. At 48 °C, the peak time is about 0.5 seconds.

At still lower temperatures, the crystalli-zation process becomes faster again. The reason for this is the change from hetero-geneous to homogeneous nucleation.

This new technology will undoubtedly expand and enhance the knowledge of complex melting, crystallization and reorganization processes and will be an important tool for polymer and material scientists.

Text: Matthias Wagner, Product Manager Materials Characterization

www.mt.com/ta-flashdsc

Figure 2: DSC curves of the isothermal crystallization of iPP at tem-peratures between 100 and 46 °C, measured by the Flash DSC 1.

Flash DSC


Pore

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n Clever Solutions For Delicate Sample Preparation

Nanostructured materials have a wide range of potential applications

including catalysis, gas storage, opto-electronic components and fuel

cell technology. Pore size and surface area are hugely important prop-

erties of these materials and the XS205DU Analytical Balance plays a

key role in the determination process.

The structure and properties of functional materials are chosen specifically for one particular application. The functional materials working group at the Technical University of Berlin, Germany, is working on the synthesis and application of nano-structured materials. Their work is fo-cused on the production of highly porous functional materials. Inorganic, organic and inorganic/organic hybrid materials

are being used. In highly porous mate-rials, the large number of small pores constitutes a very large surface area. This enhances, or in some cases actually pro-duces, the property desired for the mate-rial. Highly porous materials also have a lower density and weight which reduces costs. Highly porous functional materi-als are used in catalysis (biocatalysis and photocatalysis), during the storage and

purification of gas, as a column material in chromatography, as an ion exchanger, in opto-electronic components and in fuel cell technology.

Pore size determinationDetermination of pore size is of crucial importance to the development of these functional materials. This directly de-termines the specific surface area of a

The XS205DU with external draft shield to accommodate reaction vessel.

Mrs. Christina Eichenauer and Dr. Jens Paraknowitsch from the functional materials working group.


material and, therefore, also takes into account its micro-structural surface properties. Determining pore size is an important process for making statements concerning the properties of materials, e.g. in terms of their catalytic proper-ties. The BET (Brunauer-Emmett-Teller) method involves determining the propor-tional adsorption of inert gases, such as nitrogen, on the solid matter’s surface. Appropriate measuring devices must be used in accordance with ISO 9277.

Preparing samplesIn order to determine the surface area using the BET method, small volumes (10 - 100 mg) of the substance must be accurately measured into a special glass reaction vessel. Weighing accuracy is by far the greatest influence on the mea-

surement uncertainty of the overall re-sult. Small initial weights of 10 - 100 mg are determined precisely by differ-ential weighing on an XS205 DualRange Analytical Balance with a readability of 0.01mg.

The reaction vessels, due to their size, (length 27 cm and weight of around 18g) cannot be weighed with the XS Balance draft shield closed. To ensure precise weighing results, an external draft shield was fitted around the complete balance. For easier operation, the balance terminal is located outside the draft shield via an extension cable.

The SmartGrid® grid weighing pan on the XS Analytical Balance also ensures that air turbulence and buoyancy have

minimal impact on the weighing result. A small ErgoClip basket with a specially designed bracket holds the round bot-tomed reaction vessel securely upright on the grid weighing pan, eliminating cor-ner load errors.

The functional materials working group have found that this particular set-up, using the XS205 Dual Range Analytical Balance, achieves the level of accuracy required for the BET method and ensures that weighing errors are avoided.

Text: Stefan Christian, Group Leader Product Management

Excellence Balances

www.mt.com/XS-analytical

The ErgoClip basket allows sample containers such as test tubes to be held securely on the grid weighing pan for ergonomic weighing.


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n Advanced Instruments forComplex Material Characterization

The C2P2 (Chemical, Catalysis, Polymer and Process research) re-

search lab is an authority in the fields of synthesis and material char-

acterization. Olivier Boyron is striving to meet the requirements of the

lab’s various areas of research. He called upon METTLER TOLEDO to

initiate a partnership including several Thermal Analysis techniques.

Based in Lyons, France, C2P2 is affiliated to the CNRS, the Claude Bernard Lyon 1 University and CPE. Its staff includes Dr. Yves Chauvin, a 2005 Nobel Prize laureate, and Dr. Emile Kuntz, winner of the grand prize awarded by the National Academy of Technologies in 2005. Olivier Boyron, a CNRS engineer, is at the heart of this operation and focuses on applying and developing techniques specifically re-lating to polymer analysis.

Increasing material performancePolymer characterization represents a vi-

tal stage in the work carried out by the C2P2. Olivier Boyron explains, "The lab aims to study polymers from a chemical perspective and in terms of chemical en-gineering and polymerization processes. Our role is to develop new synthesis tech-niques or to come up with ways of making the existing ones more effective or cleaner (eliminating solvents or toxic compo-nents). It also involves devising new and better-performing polymers."

Given that the structures and chemical composition of the synthetic polymers

that the C2P2 was focusing on were be-coming increasingly complex, Olivier Boyron set about researching innovative technologies and methods within the field of materials characterization.

A partnership agreement with METTLER TOLEDO has been signed. It authorizes the C2P2 to use various techniques that are absolutely unique within the ther-mal analysis market. In particular, the researchers are working with a multi-frequency temperature-modulated DSC 1 and a high-resolution TGA/DSC 1 con-

Olivier Boyron is at the core of the partnership agreement conclud-ed by C2P2 and METTLER TOLEDO.

The TGA/DSC 1 can be used to measure the impact of the inorganic compound on the polymer's decomposition temperature


nected to an FTIR equipped with a DSC high-temperature sensor.

Responding to laboratory challenges C2P2’s work includes the synthesis of hybrid organic/inorganic materials. The basic principle involves grafting an inor-ganic compound onto the polymer with a view to making it more resistant to tem-perature, abrasion or UV radiation. Olivier Boyron explains, "The TGA/DSC 1 allows us to control the tiny quantity of inorganic compounds that we graft onto the poly-mer. In order to do this, we just need to

measure the degradation temperature and the enthalpy variations of the polymer.”

The characterization of new polymers also entails studying the distribution of mono-mer and comonomer units in the chains. Within this context, the glass transition and melting temperatures measured pro-vide crucial information.

The C2P2's work has led to it undertaking a study into the branching of polyethylen, a polymer that is widely used in numerous applications. "The branches can be short, long and so on. This means that they af-

fect crystallinity and, in turn, the ther-momechanical properties of the materials and the associated applications. Because the DSC 1 is capable of measuring the melting temperature and enthalpy of ole-fin copolymers so precisely, we can inter-pret exactly what these branches mean".

Text: Joël Goursot, Communication Manager, METTLER TOLEDO France

www.mt.com/DSC www.mt.com/TGA


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New Electronic PipetteExtends Application Range

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www.mt.com/academiaFor more information

Mettler-Toledo AGLaboratory DivisionIm LangacherCH-8606 Greifensee, Switzerland

Stay Up to Date With METTLER TOLEDO

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Novel photovoltaic module technologies made it possible to construct an emission-free airplane and the successful 24-hour flight of a solar powered airplane is no longer just a vision! Solar cells offer a clean and sustainable source of power that demands high standards. Material studies are key features used in the constant improvement of module efficiency and lifetime where water analysis plays a major role.

Solar technology pioneerThe world of solar cells is a broad field with an immense potential for exploration and innovation. The world famous project ‘SOLAR Impulse’, which aims to pilot an airplane around the world solely powered by sunlight, is a challenging task waiting for realization. The official

EPFL (École polytechnique fédéral de Lausanne)Pioneering work in solar technology

Karl Fischer C30

Enhance Solar Cell LifetimeWith Automated Titration Analysis

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academia 11 weighing and analysis in the laboratory news · 2020-01-24 · and developing...

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