chemical 6 news

Weighing and Analysis in the Laboratory

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Chemical

Testing the materials used to insulate sub-sea structures and pipelines is

a top priority for Trelleborg Offshore. With METTLER TOLEDO's innovative

solutions, the company can now determine and confirm the density of

Glass Syntactic Polyurethane insulation materials quickly and easily.

In Search of Suitable SolutionsHistorically, Trelleborg used traditional gas purged pycnometers to measure den-sity at its testing facility in Skelmersdale, Lancashire in the UK. When the company was asked to provide additional client sup-port by building a mobile laboratory for its remote operations in Angola, West Africa, it decided to upgrade the equipment.

A particular criterion in the set-up stage was to identify apparatus suitable for trans-portation by sea. Additionally, they needed equipment that required minimal assem-bly, was simple to operate and reliable in technologically demanding environments.

Density Determination Made Easy To meet these demands we suggested XS64 Analytical Balance with optional density

kit enabling the company to determine mass in air and water. The instruments have dramatically reduced analysis time, allowing 5 tests to be completed in 5 min-utes rather than 30. As well as providing accurate results, they are also compliant with density specifications, another im-portant criterion for the company.

Mr. Lee Butler, senior quality control ma-terials testing inspector, says, “We chose METTLER TOLEDO products because we always found them easy to use, reliable and comply with our testing specifica-tions. METTLER TOLEDO also has an ex-cellent customer service department andtechnical team dedicated to solving prob-lems and offering advice when needed.”

www.mt.com/xs-analytical

Analytical solutions in the laboratory

Engineering Solutions in Technologically Demanding Environments

2 METTLER TOLEDO ChemicalNews 6

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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 08/09 Printed in Switzerland.

Reliable Determination of Polymerisation of Acrylic ResinsA major component in composite sinks is liquid acrylic resin which is polymerised to form the solid sinks. Additives, such as mineral fillers and pigments, provide the desired colour and wear resistant proper-ties. The polymerization of acrylic resins is a critical step in the process and its un-derstanding is vital to maintaining quality

and improving productivity by optimizing the polymerization cycle times.

Mr. Ian Hunter, production chemist, is in charge of the laboratory and also has re-sponsibility for many new product devel-opments. He is a long standing contented METTLER TOLEDO thermal analysis in-strumentation user and has recently up-graded his DSC System with a new DSC 1 measuring module, STARe software (ver-sion 9.01) and the new TOPEM® multi frequency temperature modulated DSC technology. The DSC 1 is also fitted with a 34 place sample changer allowing unat-tended instrument operation.

Upgrading Benefits Mr. Hunter explains that, “Faced with problems of time consuming sample prep-

Upgrading for a Better Future

Carron Phoenix, part of the Swiss Franke group, is one of the largest

manufacturers of stainless steel and composite sinks in Europe. An up-

grade of their DSC system was required to optimize testing procedures

at their UK manufacturing site in Falkirk. Mr. Ian Hunter explains how

the efficiency and workflow in his laboratory has been greatly improved

by the upgrade.

aration, slow returns to start temperatures and difficulty in determining reproduc-ible glass transition temperatures, this up-grade was necessary.” The DSC 1 replaced their older DSC25 system which has been in use at Carron since its purchase in 1996. DSC is an excellent tool for analyz-ing and optimizing the resin polymeriza-tion process. Information about the rate of reaction, heat generation and time to completion can be obtained quickly and easily, which all benefited their produc-tion process. In addition, the glass transi-tion temperature of the ‘cured’ resin can be determined by DSC and also by the new TOPEM® measurements.

Our solution significantly saved time through sampling robot functions, pro-vided accurate Tg determinations and saved the company money as they no lon-ger needed to outsource activities.

Mr. Hunter explains, “We have always found METTLER TOLEDO to be respon-sive to the needs of their customers and to offer a competitively priced package. Excellent technical support from special-ists meant the steps from initial selection of techniques, through to specification of equipment was quick and easy.” he con-cludes.

www.mt.com/ta

DSC 1

3METTLER TOLEDO ChemicalNews 6

HR83

Gypsum Purity Control with the HR83Before being released into the atmosphere, flue gas from coal burning power stations undergoes a cleaning process known as flue gas desulphurisation. The final prod-uct of this chemical reaction between sul-phur dioxide and limestone is synthetic gypsum, which has a higher purity than its natural counterpart and is increasingly used in plasterboard manufacture. Crystal size and quality are indicators of purity in synthetic gypsum and are derived from the content of free water and crystalline bound water. The HR83 Halogen Mois-ture Analyzer provides the quick and easy availability of the two moisture values crucial for in-process control.

Drying Step by Step The HR83’s step drying program offers the advantage of determining gypsum surface

water and crystallization water separately within the same measurement. During both of the temperature stages required – 80°C for surface water and 200°C for crystallization water respectively – the halogen technology provides precise tem-perature control and fast, homogeneous drying. If preferred, the two moisture fractions can be determined separately within 20 minutes of each other. Chang-ing between the two methods is as easy as a simple keystroke. The time required for analysis and manual weighing is signifi-cantly reduced with the HR83 compared to drying in a muffle oven. Accurate and precise results, combined with its robust construction, make the HR83 the per-fect choice for routine operation during gypsum production.

www.mt.com/HR83

Two Values with one KeystrokeFree and Crystallization Water in Gypsum

The cleaning technologies used to reduce SO2 emissions from power

stations produce high purity gypsum as a by-product. The prompt avail-

ability of free and crystallisation water values are needed for in-process

control and are provided within one test sequence by the HR83 Halogen

Moisture Analyzer from METTLER TOLEDO.

Tips & Tricks

Correct Moisture Measurement, Thanks to Online Moisture Guide

The moisture guide explains how to perform a correct moisture measurement in short and sim-ple steps and provides key points about working with a METTLER TOLEDO moisture analyzer.

The guide also illustrates how to find the optimal parameters for your sample or the correct method for duplicating a refer-ence procedure, e.g. drying oven. You will find useful tips on how to obtain outstanding results with special samples, such as liquids or substances which form a skin.

For more info, visit:

www.moisture-guide.com

Gypsum mountain


Quality Assurance Made Easy With METTLER TOLEDO Titrators

Titra

tion

A US based innovative chemical company brings chemical, plastic and

agricultural products and services to many essential consumer markets.

Reaching customers in more than 175 countries, they invest significant

amount of time testing to ensure the quality of every product.

Upgrade for Optimum ResultOne of the quality assurance labs of the customer focuses on general acid/base titrations to safeguard every batch of prod-ucts they dispatch. Using old competitor models to perform their daily titrations, our customer was ready to upgrade. Not only were they dissatisfied with the effi-ciency of their products, but they also re-quired a quality provider who could meet all their service needs.

A METTLER TOLEDO sales representative took the time to show the customer prod-ucts that would fit their needs and dem-onstrated step-by-step equipment use. In addition, the company was impressed by the extensive METTLER TOLEDO service plans. Not having to worry about losing production time because a product is down was very important. They were relieved to know that a factory-trained METTLER TOLEDO service rep was only a phone call away. The exhaustive preventative main-

tenance available would help to signifi-cantly reduce product breakdowns.

Right Instruments Guarantees QualityOur customer purchased both a T90 and a T70 titrator, from the Titration Excel-lence line featuring One Click Titra-tion™. The titrators offered the automa-tion that they were looking for. The One Click Titration™ feature allowed them to perform titrations with just one press of a button. In addition, the parallel titration conditions in method functions and series sequence features offered unlimited lab flexibility. Our customer also purchased several SP250 peristaltic pumps for adding solvents and reagents and was very pleased with how easily the pumps could be added and used.

Customer also purchased a DL38 Karl Fischer titrator which comes with 10 pre-programmed methods to perform every-

thing from routine Karl Fischer titrations to more demanding tasks such as external extraction, high speed homogenizing and Bromine Index determination. Complete with LabX software, they are now able to control all of their titrators from anywhere in the lab or office via the network.

Our customer is very pleased with the systems they have purchased. The level of automation, ease-of-use and the security of a solid service network have been para-mount in their satisfaction with METTLER TOLEDO.

Discover more about the successor of the DL38, the V30 Volumetric Karl Fischer at:

www.mt.com/titration www.mt.com/one-click-titration

T90 Excellnce Titrator (left) and V30 Volumetric Karl Fischer (right)


In-Lab Viscous Electrodea Sharp Weapon for Viscous Samples

pH MattersWhile visiting clients, our salesman was told that the company is researching and developing a new type of aqueous acrylic acid adhesive, which promises to reduce the use of organic solvents, acquire higher shearing-resistant strength and improve performance. A pH value of 7–10 must be maintained in order to avoid any instabil-ity and therefore, pH has become one of their most important test parameters.

However, an analysts pointed out that, “One month after measuring pH values, the electrode response was found to be becoming slower with the measurement process often lasting up to 3 min, had poor repeatability with errors surpassing 0.1 pH and needing a new electrode every month.”

With careful analysis, it is known that the viscosity of client’s sample lies around 500 CPS which is the main cause of the above-mentioned phenomenon. Samples with high viscosity result in the ceramic junction blockage of regular pH elec-trodes, therefore, hindering smooth liquid sample flow.

InLabTM for Viscous Sample METTLER TOLEDO’s InLabTM Viscous Electrode is the answer for such samples. It features the latest ‘steady force tech-nique’ which means that the electrode is

previously pressurized in order to ensure that the electrolyte liquid flows out past the junction at a constant speed to avoid clogging and guaranteeing the accuracy and repetition of a measuring result. The electrode, with its 6mm tip avoids adhe-sion and is very easy to clean.

The InLabTM Viscous Electrode is suitable for measuring highly viscous and adhesive samples. After installation and training, our professional service team continues to offer support. “Since applying the elec-trode”, one analyst says, “The effects on measurements is obvious. Measurements now take only 1 min with excellent rep-etition, errors not exceeding 0.02 pH and ensured product quality. Measurement and cleaning time has been greatly saved allowing greater efforts to be spent on the test itself.”

www.mt.electrode.com

Tips & Tricks

www.mt.electrode.com

Electrode DiagnosisCockpit – Get help tofix problems quickly

An operative electrode is key for successful analysis in the labora-tory since an electrode is always in direct contact with the sample. Selection and maintenance of this instrument has a great influence on precise and accurate measure-ments. Nevertheless even a proper-ly selected electrode can suddenlystart to perform badly. Our pHElectrode Troubleshooting Guidewill help you to restore its original performance quickly.

Visit our diagnosis cockpit on:InLabTM Viscous Electrode 40

An international precision chemicals manufacturing company has

occupied the leading market position globally in the innovation of special

materials and suggestion of solution scheme along with industry devel-

opment. Measuring pH values of viscous samples was a challenging and

time-consuming tasks until they found METTLER TOLEDO.


iC Safety™ Software for Safe and Economical Processes

WeylChem Corporation, a global fine chemical company specializing in

custom synthesis, performed a series of reactions to develop a synthesis

of 2.4-diformylmesitylene (DFM) which would be scalable to produc-

tion. Understanding the energy involved, including the accumulation and

reaction of this salt, was necessary to ensure plant conditions would not

permit a runaway reaction.

Experiments at a Laboratory Scale:A synthetic protocol1 was previously pub-lished although it was felt that improve-ments could reduce material costs and improve reaction safety. The synthesis in-volves the use of potassium 2-nitropropane as a key reactant. This molecule has been known to self detonate upon standing,2

which required WeylChem to produce and use the salt in-situ.Experiments were carried out in a METTLER TOLEDO RC1e™ reaction cal-orimeter, automated with iControl™ soft-ware. An initial set of three experiments was carried out using different addition rates to assess the impact of feed rate on the reaction heat, thermal accumulation and maximum temperature rise with cooling failure.iC Safety™ software was used to con-solidate data from the RC1e™ with data from GC and DSC analysis. iC Safety™ is a novel software package that is designed to greatly speed up the data analysis and preparation of Thermal Hazard Analysis. Charts are easily generated from the experiments to show (a) KOH solution addition, (b) heat of reaction, (c) ther-mal conversion and (d) thermal accumu-lation.

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iC Safety™ Software for Safe and Economical Processes

Conclusions from WeylChem’s Report:From only three experimental runs we were able to get very useful data from the new iC Safety™ software. This data has provided us with a superb insight into the heat of the reaction as well as the amount of heat generated during different portions of the reaction. Without the use of the soft-ware in conjunction with the RC1e™ we would not have discovered how exother-mic this reaction was until we scaled up

The RC1e™ Reaction Calorimeter with iC Safety™

the reaction in the plant. (Lab runs did not show any heat kick or substantial exo-therm.) We found that the amount of heat generated will prevent us from doing the fast feed that we had envisioned. With the three different feed rates and subsequent heat ups, we were able to ob-tain enough data to allow us to extrapo-late cycle times, run-away scenarios and cooling failure issues. From this study, in conjunction with additional DSC data, we now feel confident that we have developed

1 Lieberman, S.V., JACS, 77, 1114-6 (1955); Parker, Dane Kenton, US 6355826 B1, Goodyear Tire and Rubber Company.2 Stoessel, Francis; Thermal Safety of Chemical Processes: Risk Assessment and Process Design, Wiley-VCH, 2008, ISBN 3527317120, 9783527317127, pg257-265.

a protocol that will allow for the scale up of this reaction to a plant production scale in the future. In addition, this added in-formation allowed us to calculate a more accurate costing on this desired interme-diate molecule. Another impressive aspect of the iC Safety™ is the speed in which data is obtained (i.e conversion of raw data into usable data). Before the release of the new iControl™ / iC Safety™, the turnaround time from running a reaction to issuing data was commonly days and often longer. With the new software and little manipula-tion, data is available immediately. Some of the data obtained from iC Safety™ was almost impossible to obtain previously (TCF curves, accumulation and conver-sion curve) without substantial amounts of time, effort and mathematical abil-ity. Now, with this new software, a tool is available that will make it easier to obtain useful data on laboratory reactions that will make rapid scale-up to plant models safer and more reliable.

www.mt.com/icsafety


Use www.mt.com as aWork Efficiency Resource

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METTLER TOLEDOApplication Data Sheet for Moisture Determination Using the Halogen Moisture Analyzer

This data sheet contains details of Halogen Moisture Analyzer settings for drying coffee cream. These settings enable you to develop your own drying method. The settings must be checked individually and adapted to the relevant sample. The reference method data enables you to make comparisons with the Halogen Moisture Analyzer method.

Moisture Determination Method for Coffee Cream Description/material properties Valflora coffee cream UHT, 0.25 l TetraPak, Migros

Reference Method: Oven Accessories METTLER TOLEDO AX205 DR balance, oven, aluminum pans, pipette, desiccator with silica gel, sea sand, small glass stirrer, spoon

Sample preparation/procedure Pre-dry the aluminum pans with 20 g of sea sand and a small glass stirrer in the oven (1 hour at 110°C) and then leave to cool in the desiccator. Using the pipette, place the cream in the pre-weighed aluminum pans and stir well. Leave the samples to thicken in the oven for 30 mins at 90°C, then start drying them at 103°C in the oven. Remove the contents after the preset drying time has elapsed, leave to cool in the desiccator and weigh. Repeat the process until mass constancy is achieved.

Sample weight: 4 [g]

Drying temperature: 103 [°C]

Drying times: 3/1/1 [hour(s)]

Moisture content (average of 6 measurements): 77.67 [%]

Standard deviation: 0.30 [%]

Important notes/bibliography Literature: Schweizerisches Lebensmittelbuch (Swiss Food Book) (Issue 5), 3A / 03

We offer comprehensive application support for weighing, moisture analysis, titration and many other analytical methods. Our titration application database alone holds over 300 applications for each relevant industry segment.

e.g. Titration Applications: www.mt.com/titration_applications

e.g. Moisture Applications: www.mt.com/moisture-methods

Quick results with application notes

www.mt.com offers a great deal of background information on techniques, such as weighing processes, in addition to tips and tricks on how to improve your results. Our UserCom magazines offer many examples of how to carry out better and more efficient working practice.

e.g. Good Weighing Practice: www.mt.com/GWP

e.g. Thermal Analysis UserCom: www.mt.com/ta-usercoms

Tips & tricks for daily work improvements


You can join a wide array of webinars to gain know-ledge about various topics from process optimization and applications to advanced techniques.

e.g. Automated Chemistry Webinars: www.mt.com/ac-webinars

e.g. Thermal Analysis Webinars: www.mt.com/ta-webinars

Download comprehensive documentation

We offer manuals and other documents related to our products and your business including various information supporting your equipment qualification needs.

e.g. Balance Instruction Manuals: Find corresponding manuals on our product page

e.g. Conformity Documents: Find corresponding manuals on our product page

Get the right help to fix problematic issues quickly

We offer tools which interactively troubleshoot common issues with lab equipment, such as electrodes for example.

Electrode Diagnosis Cockpit: www.mt-electrode.com

Learn new techniques with little time or effort in our webinars


A broad range of instruments is used within research and development to create and explore new chemical compounds. Therefore, scientists are looking for instruments that are versatile, can be easily upgraded and provide very best instru-ment performance.

Combined Weighing and Mixing Thanks to a Magnetic Protection ShieldPreparation of a chemical solution is a common task that often involves a beaker and a magnetic stirrer. Thanks to the special MPS (Magnet Protection Shield) weighing pan of the Excellence Precision Balances line, the substance to be weighed-in can be directly added to the solu-tion whilst mixing. Additionally, Excellence Precision Balances have an easy-to-use menu structure, a built in software application and easy to clean housing.

www.mt.com/xp-precision

Innovative Solutions Improve Chemicals

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Thermal Analysis Excellence for Process OptimizationThe Differential Scanning Calorimeter (DSC) provides important information in order to identify chemical substances, make safety investigations and study reaction behaviour. Thanks to its modu-lar design, the Differential Scanning Calorimeter DSC 1 is the best choice for manual or automatic operations within research and development.

www.mt.com/dsc

Research & Development

Water Determination Made Easy with ‘One Click™’The water content of reagents plays a crucial role within chemical reactions. Water determination is simply effi-cient and secure with our compact C30 Karl Fischer Coulometric Titrator. One Click™ KF titration provides intuitive yet easy operation, maximizes daily task efficiency and eliminates potential operator errors.

www.mt.com/karl-fischer


Whether inspecting incoming raw materials or outgoing finished products, quality control labs are under great pressure to produce reliable results of the highest quality in a very short time period.

Performing Titrimetric Analyses with just ‘One Click™’To release a final chemical product or reagent, a variety of quality parameters need to be determined - some of them by titrimetric analysis. Results are obtained rapidly and reliably with the robust and easy to use Titration Excellence line. Simply define a shortcut operation key and start an analysis with just one click directly from the large and clearly laid out touch screen.

www.mt.com/one-click-titration

Fast Density Measurement for Ultra-Pure SolventsDensity measurement is a convenient method to ascertain the purity of organ-ic solvents used in particular for liquid chromatography. The DE45 DeltaRange Density Meter with its 5 place accuracy is ideally suited for such applications. The DE45 Delta Range can even be expanded to a complete measuring system with LiQC software and SC1/SC30 sample changers in order to improve sample throughput and productivity.

www.mt.com/de-re

In-Process Monitoring and Control of Particles and DropletsParticles and droplets are pervasive in all chemical industries. Particles grow, agglomerate, break, dissolve and change shape – all of which can have an impact on process performance and product quality. FBRM® and PVM® immediately optimize and control the particle dis-tribution in a manufacturing process, ensuring consistent product quality and maximum productivity.

www.mt.com/particles

Quality Control

In order to achieve high product yields and guarantee produc-tion process safety, chemical reactions constantly need to be monitored with online measurement systems.

Production and In-Process Control

The New SevenEasy™ pH Meter S20 and Conductivity Meter S30 Version 2 Offer:

•Optimal documentation: The printer RS-P26 has an integrated date and time function – in order to create the perfect printout with date and time recorded.

•Perfect protection: A protective cover is included with each instrument in order to protect the instru-ment against splashes and spills.

•Greater precision: The new S20 has a resolution of 0.001 pH and an accuracy of 0.004 pH.

www.mt.com/SevenEasy-GLP

Complete GLP Documentation, Easy WorkflowUse your pH meter more efficiently

Spotlight on PromotionSpecial

offering

on pH meter/

printer!

Buy a SevenEasy™ pH or Conductivity Meter and get a discount on an RS-P26 Printer.

www.mt.comFor more information

Mettler-Toledo AGLaboratory DivisionIm LangacherCH-8606 Greifensee, Switzerland

Contact your local representatives for detailed information.