Bring colour to your workplace: Excellence Plus XP precision balances – for higher productivity, full complianceand amazing solutions

A sparkling solution – making champagne last

METTLER TOLEDO helps to solve a monster mystery

We igh ing and Ana lys is

in the Labora to ry

1/ 2004

LABmagazine

L A B magazine

A matter fo timeAccelerating product and process

development

Compliance, productivity and solutionsThe new Excellence Plus XP precisionbalance

How low can you go?MX5 and WinWeigh for precise

and reproducable results

The Doctor recommendsMETTLER TOLEDO

Speed it upUltra microbalance dramatically increases

throughput at environmental laboratory

Bring safety on the roadFast & easy moisture content

determination

MonoBlocThe heart of the “space balance”

AutoChem 4

Balances 6

8

10

12

Moisture 13determination

Mass calibration 14

6 The smart way of weigh

L A B magazine

Density 16

pH meters 18

Thermal Analysis 20

Titration 22

24

A sparkling solutionRefractometer and density meter maintain

the lasting quality of Champagne

The Big Monster DigMETTLER TOLEDO helps solve

a monster mystery

Under control Analysis of thermoplastic materials

ensures product quality

A trio of titration solutionsEnsure accurate oil analysis for leading

Spanish company

Precise and reliable –Titrators save time and improve quality

for household detergent manufacturer

Excellent addition to precision balancerange

MonoBloc takes weighing out of this world

The LabMagazine is published twice a year for laboratory customers of METTLER TOLEDO.

Publisher: Mettler-Toledo GmbH, CH-8606 Greifensee, Switzerland

Editorial Team: Julia McHugh, Philippe Burki, Jörg Burmester, Urs Groth, Rolf Rohner,

Hans Tinazzi, Sascha v. Wangenheim

Layout, Graphic and Production: MarCom Greifensee

Specifications of all products mentioned are subject to change without notice.

C o n t e n t s

14

A sparkling solution !16

preHistoric task for laboratory meter18

6

The story of Avantium reads like a businessman’s dream. It all starts by spotting just theniche that an industry needs.Next, influential parties from a range of disciplines are convinced to invest in the idea.The plans are put into actionand, in just three years, it isnow a company with more than 100 employees and aworldwide reputation.

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Rapid researchAvantium has three market-oriented businessunits of approximately the same size: Chemicals,Pharma and Crystallics.

Crystallics focuses on quickly finding the best pos-sible crystalline form of a substance for a certainapplication. In the case of many medicines, forexample, the effectiveness of an active reagentdepends heavily on the form in which it occurs.Crystallics is able to conduct a thorough investi-gation into the development of a substance’s var-ious crystalline forms within six weeks. To com-plete this work, fewer than five grams of materialis needed to conduct tests under more than athousand different experimental conditions.

A similar system of rapid research is used in theother two business units. For example, findingjust the right catalyst to accelerate a chemicalprocess, to make it more specific, or to increasethe yield of a reaction, is often a very prolongedand costly process. Also, the question is not limit-ed to finding the most suitable catalyst, but also tofinding the conditions under which it will func-tion most effectively. Avantium can also provideanswers to these questions within six weeks. Thistime it makes use of its Quick Catalyst Screeningplatform. This is a system that carries out themany experiments automatically and with a min-imum of material. Avantium stocks more thanfive thousand catalysts for use during thesescreening procedures. Finding combinations ofprocess parameters for optimising specific steps inproduct synthesis can be done even faster. TheQuick Process Screening service developed byAvantium can provide this information within anincredible three weeks.

A u t o C h e m

Avantium is an advanced R&D company that hasbecome internationally renowned in the fields ofcatalysis, high throughput experimentation, nan-otechnology and the study of chemical processes.The company delivers these services in response toa definite market requirement. In order to remainahead of the game, companies in the chemicaland pharmaceutical industries have to speed upthe development of new products, optimise theirproduction processes and shorten the time neededto get these products to the market. But to con-stantly develop the technologies and competenciesrequired for accomplishing all this, each individ-ual company would have to invest substantialamounts of extra money in R&D. So the ideabehind Avantium was to create a research centreto provide everything required for acceleratedproduct and process development. This centrecould then support industry on a commercialbasis by means of contract research.

A matter of time –Accelerating productand process development

P r o c e s s d e v e l o p m e n t

Investments in people and softwareTo make such high-speed research projects possi-ble, Avantium had to invest heavily in people, soft-ware and hardware. Tom van Aken, Vice Presidentof Business Development for the company’s LifeSciences Division is clearly proud of what he calls “the gigantic amount of brainpower” withinAvantium Technologies. “The vast majority of ourpeople”, he explains, “are university-educatedmathematicians, chemists, pharmacologists,engineers and IT graduates specialised in softwarefrom all over the world.” The fact that the com-pany has already invested heavily in software canalso be seen in the wide range of special packagesthat Avantium uses for its projects. For its researchin catalysts, it has accumulated an extensivelibrary of information about heterogeneous,homogeneous and biocatalysts from many differ-ent manufacturers which is used for quick accessto existing information. Avantium also developsits own software. A good example is its DAP pack-age, a piece of software that helps the chemist dealmore efficiently with the vast amounts of datagenerated by High Throughput Experimentation.In addition, statistical packages help in analysingthis data and in planning experiments – bothuseful for attaining a high degree of efficiency.

Obtaining results and conclusions is made fasterby utilising software for modelling and simulat-ing processes and reactions. For this, Avantiumdoes not only utilise commercially available soft-ware but also VirtualLab™, a package developedin cooperation with METTLER TOLEDO. This soft-ware solution offers the chemist an intuitive plat-form to design, conduct and analyse experiments.These experiments are then fully compliant withthe traceability requirements stated in 21 CFRpart 11.

Investments in hardwareAvantium has invested in the FlexiWeigh instru-ment developed by METTLER TOLEDO. It weighssolid substances from a dispensing vial and then dispenses them into destination tubes. Theamounts being weighed are mere milligrams ofmaterial. The FlexiWeigh instrument is part of theworkflow of Avantium’s High Throughput Experi-mentation platform. The other part, developed byAvantium itself consists of a block in which 96reactions can be conducted simultaneously, andunder pressure if desired. In fact, finding opti-mum commercially feasible reaction conditionsby means of this parallel processing technique isthe first experimental step toward scaling up theseprocesses.

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However, scientists are not limited just to findingthese optimum conditions – they can also con-duct a study into the robustness of a process. Themore robust a process is, the less its yield will varyas fluctuations occur in the reaction conditions.This is particularly valuable information for amanufacturing plant.

The further scaling up of reactions can be done inthree successive steps. Here again, the companyuses METTLER TOLEDO equipment. The secondof these steps involves the use of the MultiMaxmultiple reactor system. This technology canutilise up to four reactor blocks, each containingeither 16, four, or two reactors, with a volumerange of 10 ml to 250 ml. Step three involves theuse of the LabMax, an automatic single vesselsystem that can contain up to 1000 ml. An RC1 isalso used, with a volume in this case up to sixlitres.

Avantium has also invested in in-situ technologiesto further study what goes on in the vessel duringa reaction. Using the Lasentec FBRM systemallows scientists to see if and when particles form(crystallise) or dissolve in the reaction vessel. TheRaman and the complementary Mid-IR technologymake it possible to study how the concentration of chemical substances change during the reaction.

Next to the RC1, we see more thermal analysisequipment. This time, it’s a DSC unit and a TGAunit. The reason for this high amount of METTLER TOLEDO equippment: METTLERTOLEDO had been in contact with Avantium’sfounders since 1998 and that the two companiesshared many similar ideas in the field of parallelprocess development. This led to a close coopera-tion that resulted recently in Avantium’s writing asupplement to the software package for the MultiMax.

FutureAvantium Technologies’ customer base has grownto more than 30 customers and its number ofpartnerships has increased as well. In addition toits initial investors and METTLER TOLEDO, Avan-tium now works with such organisations asDegussa and Engelhard in the field of catalysis,with Amcis, a subsidiary of Solutia PSD, in thefield of scaling up pharmaceutical processes andmodelling production, and with the University ofMalaysia in the field of developing high-gradeproducts from palm oil. Avantium’s customers arevery satisfied with the results the company hasachieved in such a short space of time. And itlooks very much as if they will continue to do soin the future as well.

Full regulatory complianceThe new Excellence Plus XP precision balance actively supports you by ensuringregulatory compliance. A key part in this isplayed by SmartScreen, the unique colordisplay with touchscreen operation. High-resolution graphics and brilliant colorsprovide groundbreakingly clear user guid-ance, while innovative QM tools supportyou with efficiently enforcing your qualityguidelines in everyday routine. Forinstance, individual access rights for up toeight users can be defined by the adminis-trator and protected with passwords. Allchanges to protected settings and adjust-ments are registered in the HistoryFile, andall measurement results can be document-ed to conform to G x P – for seamless trace-ability. In addition to proFACT, the auto-matic internal adjustment mechanism,BalanceCheck reliably enforces validationof the measurement certainty, for examplewith an external test weight specified byyou, at the times you define. In short: theExcellence Plus XP opens up a new, color-ful world of weighing in which you decidehow much certainty you need.

Maximum productivityThanks to inovative weighing technology,the results of the Excellence Plus XP stabi-

lize rapidly, even in harsh environments.Color graphics and full-text instructionsguide you safely through applications andhelp avoid errors. If the repeatability ofyour processes is crucial, the correctness ofsmall weighings is highly important.Ifdesired, visual signals warn if the definedminimum weight is not achieved. Thanksto the MinWeigh function, even the small-est samples are always weighed in withhighest accuracy. The Excellence Plus XPactively contributes to your process securi-ty and thereby helps increase your produc-tivity.

Pure ergonomicsYou don’t always have a hand free to oper-ate the balance. So sometimes hands-freeoperation of the balance would be ideal, forexample when you weigh toxic substancesin a laminar flow. Thanks to SmartSensand ErgoSens, the intelligent infrared sen-sors of the Excellence Plus XP, this is possi-ble without difficulty. At the wave of a handyou tare the balance or send your results tothe printer – depending on which of thefreely selectable functions you haveassigned to the sensors. With both handsalways free for weighing, you can completeyour work quickly and safely.

As the world’s leading manufac-turer of laboratory balances,METTLER TOLEDO pursues onegoal: to make weighing easierwith innovative solutions. With the Excellence Plus XP, thelatest generation of precisionbalances at the ProfessionalLevel, this success story contin-ues. Created for a wide spec-trum of applications in highlydiverse industries, the Excel-lence Plus XP offers maximumsecurity in regulated environ-ments, utmost productivity, andunique flexibility when tailoredsolutions are called for.

B a l a n c e s N e w p r o d u c t

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Compliance, Productivity and amazing SolutionsThe new Excellence Plus XP precision balance

Data exchange – fluent in alllanguagesThe new Excellence Plus XP was developedto fit into a networked world with total con-fidence. Whether with stare-of-the-art wire-less connections based on the Bluetoothstandard, USB, PS/2, or network solutionsvia Ethernet: the flexible interface conceptguarantees connection and compatibility,forwards as well as backwards. For clearcommunication in the information age.

No matter where it is used: the new Excel-lence Plus XP precision balance sets newstandards for weighing in the laboratory.

SmartScreen brings color intothe lab – greater certainty

thanks to clear user guidance.

Bluetooth, a wireless connection between balanceand printer. You place theprinter just where you want it – with no cable to worryabout.

ErgoSens. These freely placeable IR sensors enable hands-freeoperation of the bal-ance.

For more information visit :

www.mt.com/XP

M i n W e i g h i n s t a l l a t i o n

Founded in 1880 in the Bour-gogne region of France, FournierPharma is one of the leadingmanufacturers of lipid reducingagents (for treating cholesteroland triglycerides) and hormonaltreatment patches. The 4th

largest independent laboratoryin France, with exports account-ing for 70% of its turnover, it invests heavily in R&D in thefields of pathologies of themetabolism and nuclear recep-tors.

We met Mrs Céline Peter, thePhysical/Chemical Laboratorymanager, on the dry form (cap-sules and tablets) productionsite in Fontaine-lès-Dijon inFrance, following the installa-tion of a MX5 microbalanceequipped with MinWeigh.

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B a l a n c e s

How low can you go – MX5 and MinWeigh for preciseand reproducible results

Example of a MinWeigh certificate issued by the Technical Department when the balance is installed.

Mrs Céline Peter: “Unlike balances accurate to 1/100th of a milligram, the MX5 fully meets our requirements.”

A group with a strong presence onthe American market Fournier Pharma has several establish-ments in France: production, chemicalsynthesis (manufacture of active ingredi-ents), R&D and galenic and analyticaldevelopment. However, its second largestmarket, after France, is the United States.The company therefore has to operate inaccordance with American standards (eachprocess modification requiring an audit)whereby everything can be traced andeverything can be validated, notably inaccordance with Food and Drug Adminis-tration standards – its three productionsites in Chenôve and Fontaine-lès-Dijon inFrance and Cork in Ireland are all FDAapproved.

We have to weigh out 50 mgmaximum“Why did we decide to upgrade to this typeof balance? When preparing chromatogra-phy standards, we weigh out between 5 and50 milligrams in micro-cups. We neededmore sensitivity and precision for our stan-dards, which are used for the differentdosages: the MX5 gives us a display preci-sion to three decimal points, i.e. to one µg,and the MinWeigh provides us with thesecurity we required as regards minimumweighing operations,” explains Mrs Peter.

The MinWeigh is a facility that wasinstalled by the METTLER TOLEDO techni-cian and is memorised in the balance forcarrying out minimum weight operations.

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Galenic formulation is named aftera 3rd Century AD Greek physician,Claudius Galen, who recordedimportant discoveries on anatomyand paved the way in the Westernworld to research into how a bodyabsorbs different medicines. Hisname is associated with principlesof preparing and compoundingmedicines that still have theircounterparts in today’s laboratories.

Minimum weight =Expansion factor x Repeatability (s)

Uncertainty (U)

Minimum weight =3 x 0.001 mg x 100

= 3 mg0.1

It integrates the tare so that the operatorcan work on the net weight, in other wordsthe actual quantity of sample. In otherwords, the lower the tare weight, the betterthe repeatability of the balance and themore one can reduce the minimum weight.As Article 41 of the US Pharmacopoeia stip-ulates, “the measurement uncertainty ismet if three times the standard deviation ofat least 10 successive weighings, divided bythe quantity to be weighed, does not exceed0.001 (0.1%)”: if the minimum value hasnot been validated, it cannot be exported tothe United States. Thanks to the MX5equipped with the MinWeigh, FournierPharma can now perform minimumweight operations of 5 mg with a repeata-bility of 1µg! If the operator does not reachthe defined limit memorised in the bal-ance, a message appears in the form of acontrast on the display unit and the weigh-ing cannot be validated.

Céline Peter has decided to dedicate theMX5 balance uniquely to these smallweighing operations and told us that herAmerican customer was very impressed bythis METTLER TOLEDO technology.

The minimum weight of a balance isaffected by the balance’s repeatability, thetare weight, the relative error given in %and the expansion factor (usually 2 or 3).To calculate the permissible minimumweight of a balance according to USP thefollowing formula can be used:

USP requires an expansion factor of 3 anda relative uncertainty of 0.1%. For an MX5balance with a repeatability of 1mg theminimum weight results in:

For more information also visit:

www.mt.com/MinWeigh

E n e r g y w e i g h i n g B a l a n c e s

1 1L A B magazine

Balance meets ’UKAS’ criteriaAs well as needing to upgrade existing balances,which were growing tired, the Torquay-basedcompany was seeking UKAS accreditation andnew equipment was essential to reflect thisprestigious certification. In order to meet theUKAS criteria, Pipette Doctor® set its ownrequirements for the new balances. It specified0.01 mg readability, a reliable and robustdesign and instruments that were easily trans-portable. The company also wanted to buy awell-known and respected brand.

When searching for suitable equipment, PipetteDoctor®, approached all the leading manufac-turers before finally deciding on the SAG105weighing module. One of the decisive factorswas the efficient manner in which the METTLER TOLEDO team treated them, as Ian Hemmings, Managing Director, explains.“Other companies we approached failed toreturn our calls, did not turn up to demonstratethe product or were unable to show us the spe-cific product we had requested to see. As a pur-chaser all these factors influence the buyingprocess and METTLER TOLEDO provided uswith the confidence we needed.”

The flexible choice for fast weighingThe SAG105 is a flexible solution for unusualweighing tasks and is ideal for use in time-critical processes where a quick balance makesa major contribution to higher productivity.Under optimal environmental conditions, theSAG105 shows the weighing result accurate to0.01 mg and is four times faster than conven-tional semi-micro balances. The speed andaccuracy of this model is enhanced by the useof separate weighing and control modules. Theflexible draught shield provided with theSAG105 helps achieve the rapid stabilisationthat is a feature of the entire SAG range, whichin this model is one second.

For pipette calibration software installation ona PC is essential. The volume of liquid is calcu-lated from its weight and density and comparedwith the nominal volume of the pipette. Theevaporation trap prevents liquid being lost andthe balance transfers the weight values to thePC for automatic calculation by the software.

The Doctor recommends METTLER TOLEDO

When seeking balances suitablefor UKAS accreditation, UK com-pany Pipette Doctor® turned toMETTLER TOLEDO to meet itsrequirements.

Pipette Doctor®, established in2000, has rapidly grown tobecome the established expertsin the field of liquid handlingservice and calibration. Inresponse to customer demands,it developed a programme toservice and calibrate all makes,models and volumes of pipettesin line with individual require-ments and industry regulations.

Ian Hemmings continues “the SAG105 met allthe technical criteria we had stated. The carrycases make them easily transportable andsecure and they have proved to be very reliableand robust over the past 17 months. Even whenwe had a fault on one of the balances, due to itbeing dropped, the Service Department com-pleted a quick and efficient repair.”

Engineer’s efficiency improvedThe SAG105’s have been issued to seven fieldengineers as an essential part of their kitenabling them to increase efficiency. They arequick to stabilise when set up at a new locationand work well in a variety of conditions, whichis critical for the engineers as they are notalways presented with the ideal balance envi-ronment. The specialist pipette calibrationglassware are expertly designed allowing all-round access, which is key for calibratingmulti-channel pipettes.

Expanding operationPipette Doctor® offers a pan-European serviceand has advised companies in Europe andSouth America on how to establish a “PipetteDoctor” operation. Ian Hemmings explains,“We have now established a full Pipette Doctorfranchise in Ireland and Northern Irelandwhich is running well. We have not completedthe set-up for South America although they arestill looking to do something with regard toservice. In all cases, the Mettler SAG 105 was thebalance supplied and the only balance we recommend for field calibrations.”

Following a successful audit in April 2003,Pipette Doctor® secured UKAS accreditation.Ian Hemmings adds, “I am pleased toannounce that we became UKAS accredited in2003. We have also expanded our Torquay Calibration Lab and are adding another 6 placebalance – needless to say a Mettler AX26 comparator!”

B a l a n c e s

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The introduction of a new analyticalbalance has improved the speed of analysis, stability and accuracyof weighing results for a leadingenvironmental consultancy.

Established in 1970, RPS Labora-tories is now part of the Health,Safety and Environment Division of the RPS Group PLC – the largestindependent environmental consul-tancy in Europe.

The site in Salford Quays, Manchester is one of theUK’s leading environmental and occupationalhealth laboratories. It provides private and publicsector clients with UKAS accredited analyticalservices for workplace and ambient atmosphericpollutants, stack emissions and biological moni-toring. The expert staff – chemists, biologists andenvironmental scientists – provide analyticalsolutions to a wide range of industries fromaround the world. Wendy Martindale, Operationaland Sales Manager, explains “People are exposedto hazardous products and substances throughouttheir working day – it is imperative that these aremonitored to prevent ill health and disease andcomply with strict Health and Safety legislation.RPS Laboratories specialise in helping our cus-tomers to identify and measure these hazardoussubstances accurately and with confidence.”

Stability and accuracy are vitalIn order to provide the service its customers’demand, RPS Laboratories needed to upgrade oneof its existing balances. The replacement balance

Speed it up –Ultra microbalance dramaticallyincrease sample throughput atenvironmental laboratory

E n v i r o n m e n t

had to be sufficiently accurate to comply with theexacting standards of UKAS accreditation. Typical-ly, the equipment is used to weigh filters andmembranes used to assess nuisance dust levels. Asthe samples are very small, the new instrumentshad to have excellent stability as well as provideaccurate and reliable results. Following a productdemonstration and consultation, the companydecided that the MX5 microbalance with a Hauganti-static 20cm de-ionising bar was ideal for itsrequirements.

Automatic operation ideal for delicatesamplesThe balance features SmartSens which allowshands-free operation of the draught shield. Thesystem comprises two sensors, at each side of theuser display, which activate the automatic doorfunction. SmartSens ensures fast and accurateweighing by eliminating environmental effects.This was one of the main reasons the MX5 waschosen as Joanne Dewhurst, Laboratory Manager,explains “the automatic doors enable both leftand right handed users to effectively use the bal-ance and with the delicate samples we analyse, itis essential that we have the best equipment.”As well as the MX5 balance, a Haug anti-staticunit was required as the filters can be prone tostatic, which results in unstable readings. Whenpowdery samples are electrostatically charged, adraught is often enough to blow the substance into the air. With minute changes in the overallweight of a sample being critical, incidences suchas this can be problematic. The Haug ioniser discharges even the smallest objects. Its probe,with a diameter of approximately 25mm, can alsobe installed into the inside of containers and theflexible cable allows it to be used in any positionsimply and easily.

With the installation of the new equipment, stability has increased – readings now only takeseconds to stabilise and not minutes. “Our abilityto process urgent samples on a daily basis hasincreased by 50%” concludes Joanne Dewhurst.

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Other features including the user-friendly menuand RS232 interface for recording data on aprinter or PC to meet GLP and GMP requirementshave also been beneficial according to Gail. “Wealso have confidence in our results as the printerticket can be attached to reports confirming thelevels of moisture content in the raw materials. Itis also simple to use and the robust design is idealfor our laboratory environment.”

The HB43, which is suitable for both laboratoryand production environments, offers the companyultra-rapid halogen drying as the heat is distrib-uted evenly across the sample in seconds. The drying temperature can be precisely controlledensuring better reproducibility and reduced meas-urement times. In Prismo’s case the drying timewas reduced to just one and a half minutes.

Halogen dryer saves timeThe back-lit display is easy to reach and two dif-ferent drying programmes allow the Quality Con-trol laboratory to test various samples – helping toincrease productivity, improve results and savetime. The flat surface of the instrument provideseasy access to the sample chamber ensuring it iseasy to clean. This was one of the reasons theHB43 was selected as Gail outlines: “One of theproducts we test is aggregate which is quite messy.By having easy access to the drying pan the equip-ment is kept clean. For the dry powders we test, there-usable trays are ideal and cost-efficient.” Thenew instrument has improved processes at the site.“It saves us time as our processes are now quick-er,” explains Gail.

M o i s t u r e d e t e r m i n a t i o nPrismo Products Services hasmastered moisture control withhelp from METTLER TOLEDO.Thanks to the introduction of a halogen dryer, analysis timehas been cut from one and a half hours to just one and ahalf minutes.

The Chorley-based companyspecialises in the design,development and manufactureof road markings, surfacedressings and bituminous prod-ucts – including traffic safetyproducts, thermoplastic anti-skids and coloured imprints. It supplies a wide range ofinnovative product technology to customers worldwide.

’Wet’ your appetite with new moisture solutions

Increase productivity, save time and improveresults with our enhanced halogen moistureanalysers.

The top-of-the-range HR83 now has 40methods, three level password and sample identification with bar code reader. In addition itoffers AutoMet – automatic method development– which can cut development time by 50%. Our HB43 halogen dryer can now run methodsdeveloped on the HR83, while the HG63 has 10 methods and sample ID – ideal when morethan one product is tested with different dryingcriteria.

The site has two laboratories – Quality Controland Research and Development – but it was theQuality Control laboratory that was experiencingproblems, including extended analysis times,when testing and checking deliveries of raw mate-rials. The company uses a pneumatic transfer system to move raw materials from the deliveryvehicle to its silos and mixers. If moisture ispresent in any of these areas the system becomesclogged and production halts – costing time andmoney.

Fast, accurate results neededGail Stephenson, QA Manager, explains: “The sys-tem we use is very sensitive to moisture and it isessential that the raw materials delivered do notcontain excess moisture. We must obtain fast andaccurate results but our existing moistureanalyser took one and a half hours to dry the sam-ple and the delivery driver was not happy to waitfor that length of time!” Following a consultationand product demonstration by the local METTLERTOLEDO Account Manager, Prismo decided thatthe HB43 halogen moisture balance was ideal forits requirements.

Road safety matters –Fast and easy moisture content determination

R o a d m a r k i n g s

M a s s c a l i b r a t i o n M a s s c o m p a r a t o r s

1 4 L A B magazine

The mass measurement of small bodies ina space laboratory cannot be made usingtraditional balances since they give thevalue of the mass of a body by measuringthe gravitational force acting on it. In theabsence of gravity or when gravity is exactlycounter-balanced by a centrifugal force (asin stable orbital conditions), a traditionalbalance does not work. In these environ-ments the mass of a substance can only bedetermined by evaluating its inertial prop-erties.

NASA and the Soviet Space Agency havedeveloped inertial scales for their spacelaboratories to study the weight changes ofastronauts during space missions. Thesescales were based on the evaluation of thenatural frequency of an oscillating systemconsisting of two elements: a preloadedspring and an astronaut (fastened to oneend of the spring). This system allowedmass determination up to 10 kg with anuncertainty of about 0.1%.

MonoBloc – the heart of the ’space balance’

Although the oscillating technique is agood way to measure the inertial mass ofrigid bodies, it cannot be used for estimat-ing the mass of substances in liquids, powders or gels. For these materials thecentrifugal method should be used – anobject rotating at constant angular speedaround a vertical axis is subjected to asteady force radially directed. The mass of arotating object is achieved by accuratelymeasuring the centrifugal force, angularspeed and distance between the axis andcentre of gravity. The most critical meas-urement is the last one. While it is difficultto precisely locate the centre of gravity thatis geometrically regular, it is almost impos-sible to do so with an irregular body orpowder.

A simple artifice may be adopted to over-come this difficulty. Instead of a singlemeasurement, take two of the same objectat different radial positions – provided thatthe radial distance between these two posi-tions is accurately known.

IMGC (Istituto di MetrologiaGustavo Colonnetti), theItalian metrology instituteresponsible for mass meas-urement, has developed aninertial balance to accuratelymeasure the mass of smallbodies in zero-gravity condi-tions. Three ground proto-types have been built at IMGC(CNR) in co-operation withAlenia Spazio and the ItalianSpace Agency (ASI). Theground prototype has to becompatible (weight anddimension) with the shuttleflight.

The IMGC inertial centrifugalbalanceThere are several possible ways to build aninertial scale by application of the centrifu-gal method. In conventional precision bal-ances, the gravitational force acting on themass is not measured directly but is coun-terbalanced by another force. The sameapproach was adopted – the centrifugalforce acting on the mass opposes the centripetal force exerted by a pre-loadedhelical spring. Through closed-loop con-trol, the motor angular speed is adjusted sothat the centrifugal force exactly counter-balances the elastic force of the spring. Alinear position sensor, which also operatesas the sensing element of the control loop,indicates whether such a condition is satis-fied. Three study prototypes were assembledat IMGC to demonstrate the suitability ofthis method. One of the key components ofthe prototype was a MonoBloc weighingcell manufactured by METTLER TOLEDO.

New prototype developedTo cover the lower range required by bio-logical application (50 g full scale) and toimprove the performance of the secondprototype, a new design was developed.

Although based on the same centrifugalmethod, the new balance (BIC 3) adopts adifferent functional approach from previ-ous prototypes. Instead of a known con-stant centripetal force (the spring) to beequalised by a centrifugal force through a controlled angular speed, a known con-stant angular speed (then a constant cen-trifugal field) is produced. An integralbeam measures the centrifugal forcewhich is directly derived from a METTLER TOLEDO electronic balance. The newprototype is not affected by dynamicunbalancing due to the radial displace-ment of the platform housing the beam.

Better results than expectedThe ground model of the inertial balance,from the mechanical point of view, is finished. The testing phase provided betterresults than those forecast, so a flight pro-totype could be designed in the future withenhanced performance. The co-operationbetween METTLER TOLEDO and the Italian Research Council is setting a newmilestone in weighing. After the analyticalbalances installed in the research lab on K2 (5500 m) the next step will hopefully bethe International Space Station

D e n s i t y P r o c e s s c o n t r o l

1 6 L A B magazine

A sparkling solution –Refractometer and density meter maintain the lasting quality of Champagne

The Comité Interprofessionneldes Vins de Champagne(CIVC) is a semi-public inter-professional organisationwhich groups together winegrowers (grape producers)and traders (Champagnefirms) in order to protect theinterest of the Champagne“Appellation” (guaranteed vintage). Its Technical Depart-ment carries out researchwork and provides wine growing, oenological and environmental advice to producers.

The Technical Department laboratory has 3 principal missions As Dominique Tusseau, the laboratorymanager, explains: “Our missions are toprovide experimental support, to carry outanalyses for exports and to help defend theChampagne Appellation both in Franceand abroad.” Champagne is a very highquality product and it should remain so!The laboratory has ISO 17025 Standardaccreditation and is fully geared to adapt-ing or adopting new analysis methods.

METTLER TOLEDO instruments are usedto measure parameters that are critical inmonitoring experimental fermentations.These include total acidity, sulphur dioxideconcentration, pH, density and refractiveindex of musts and wines and the volatileacidity and the alcoholic strength of winesusing the officially approved assayingmethod.

Measurements carried out with a high degree of reliability andexcellent precision The key words for Dominique Tusseau aretherefore exactness (accuracy and preci-sion), equipment reliability and the speedof measurement: “We needed high technol-ogy, autonomous equipment, with a print

The rule is simple: there is onlyone champagne and that is realChampagne The CIVC acts as a management, regulato-ry and advisory body for the whole Cham-pagne production chain. It is responsiblefor registering and licensing all of the pro-fessional organisations situated in theAppellation d’Origine Contrôlée region,organising the grape harvest (for example,by setting the date for the start of the grapeharvesting season each year), pressing andproduction. The production of champagne,as we know it today, began in the early 18thCentury and now stands at 300 million bot-tles per year and covers a wine growingarea of 34,000 hectares. In 1950, the CIVCset up a Technical Department to carry outresearch and experimentation to improvewine making and oenological techniques:combating frost or pest damage, selectingyeasts and bacteria in order to guaranteethe quality of the alcoholic and malolacticfermentations that determine the efferves-cent quality of the wine, approving winepresses and press houses (a requirementthat is specific to the region). The Techni-cal Department also carries out research onmonitoring production quality, from thegrape pressing stage up to the final bottlingstage.

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out of the results so that they could bechecked through cross referencing. Wehave been clients of METTLER TOLEDO formany years for our weighing and titrationequipment, and that’s why we turned toyou for a densitometer, refractometer andauto-sampler. Equipment reliability is veryimportant to us, particularly at grape har-vesting time, when a very large number ofmusts have to be analysed in a very shortperiod. We use a RE50 refractometer tomeasure the refractive index of musts anda DE45 electronic densitometer (accurateto five decimals) to measure their densityand thus estimate their potential alcoholicstrength by volume. With the DE45, wemeasure the alcohol strength of the winesusing the officially approved method. Weare only a small team – 7 persons in all –but we carry out 10,000 measurement peryear for export and 45,000 for research anddevelopment purposes!

Obviously, all of the analyses carried out in the laboratory are backed up by tastingtests in order to control aroma, taste andcolour.”

p H m e t e r s S c i e n c e

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The Big Monster Dig –METTLER TOLEDO helps solvemonster mystery

Each of the seven programmes focused on a particular geographical area andexplored the life that once roamed it bypiecing together clues from a current exca-vation, previous historical fossil finds andtoday’s geology. The fossil-hunting seriesdiscovered new relics from the age ofdinosaurs and every week the crack team ofpalaeontologists solved a mystery datingfrom the deepest recesses of our geologicalpast. During the series the team investi-gated sabre-tooth tigers in Spain, iceagemammoths in Wiltshire and a pterosaur onthe Isle of Wight. Integral to investigationsfor the Spanish adventure was the analyti-cal instrumentation used to determine scientific facts and METTLER TOLEDO washappy to help.

Sabre-tooth tigers under the spotlightA high concentration of predators includ-ing the extinct sabre-tooth tiger were foundin a group of mysterious, large earthmounds left over from the mine in a lime-stone quarry near Banyoles, Catalonia,North Eastern Spain. Carnivore fossils nor-mally make up to 10% of the fossil recordfrom any given location - but the level herewas much higher. An important part of theinvestigation into sabre-tooth tigers was toestablish why these earth mounds were sorich in fossils of vertebrate creatures butcontained none of the associated matternormally found with these types of animal– for example plant material and mol-luscs. Perhaps the answer to this wouldlead to the mysterious cause of their death.This hugely significant find suggested thatthis area may have been some kind of pre-historic death trap which is very excit-ing in the world of palaeontology. To aidthe investigations RDF Media needed afully functional portable pH meter andapproached METTLER TOLEDO who hadbeen recommended as the “best in thebusiness.”

METTLER TOLEDO has helpedunearth important clues relating to the extinction of the sabre-tooth tiger. In theautumn UK broadcasting company Channel 4 screenedThe Big Monster Dig – a factual programme from lead-ing independent productioncompany RDF Media. And aMETTLER TOLEDO instrumentenjoyed a leading role in oneof the episodes.

pH readings provide important data The MP125 instrument was used to deter-mine the pH level of the water in a newlyformed natural lake near to the fossil sitewhich the scientists believe would havebeen similar to the million year old lakethat formed the earth mounds. The ancientearth mounds were formed by the build upof sediments in pre-historic lakes. Theunderlying bedrock in this area means thatsimilar lakes are geologically formed in theregion today. Professor John Howellanalysed the sample from the lake toobtain the pH level. Certain levels of acidi-ty/alkalinity can stop plant matter, shellsor shelly organisms from either living orbeing preserved in the fossil record. Thesample was pH 6.2 and at that low aciditythings like bones which are made of phos-phates will be preserved. But anything elsewould have little chance of being found inthe fossil record. The pH meter is easy touse as Professor Howell explains “theequipment was great for its portability andease of use and the level of pin-point accu-racy it provided in field experimentationwas impressive. I actually refer to it in theprogramme as my «little James Bondcase».”

The ’pHortable’ choiceThe portable pH meter has been designedwith hard-working routine measurementin mind. The RS232 output enables themeter to be directly linked to a printer orcomputer allowing results to be stored,analysed or simply printed out. An inte-grated analogue output can link to a chartrecorder for the monitoring of process andreactions. The wider measuring range ofthe meter caters for the most unusual sam-ples while the three point calibration givesthe flexibility to measure samples withwidely varying pH values accurately. Theselectable resolution allows the choicebetween accuracy and speed in samplemeasurement depending upon the applica-tion. The InLab®413 electrode used by theBig Monster Dig team is a versatile combi-nation pH electrode with integrated tem-perature sensor – ideal for a wide range ofapplications. It has a polymeric electrolyteand requires no junction at all. As a resultthese sensors are particularly insensitive tocontamination – making it ideal for theSpanish adventure.

T h e r m a l a n a l y s i s R e s e a r c h

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IPL was established in 1975 and, thanks tocontinuous technology innovation, hasbeen able to develop products and processesto achieve impressive results, regarding bothproducts and commercial performances.Today it is based in Besozzo and employs110 people with an annual turnover ofapproximately 20,000,000 Euros.

Application and needsRaw materials are one of IPL’s most impor-tant resources. Adopting the right qualitycontrol policy and prudent management of suppliers has helped improve productquality. More than 200 raw materials aremanaged daily – therefore the Quality

Control and R&D Laboratory wanted tomonitor and investigate raw materials andfinished products more thoroughly.

The usual characterisation previously car-ried out on materials – density, hardness,traction characteristics, etc – no longerguaranteed consistent tube quality. Inaddition the company also wanted toanalyse the products’ composition as wellas verify the qualitative and quantitativenature of the formulations used to repro-duce and optimise product performance. Asa result, Paolo Negri, Head of the QC/R&DLaboratory, selected a METTLER TOLEDOTGA/SDTA851e instrument for thermalanalysis, to complement the other equip-ment used in the laboratory.

BenefitsDespite being a sophisticated instrument,the TGA/SDTA851e is not difficult to oper-ate. It allows precise qualitative and quan-titative analysis on materials and finishedproducts and provides fast and accurateresults.

Thermal analysis is playing a key role in the control andresearch of new thermoplasticproducts and materials for aleading Italian company.Industrie Plastiche LombardeS.p.A.(IPL) monitors and studiesraw materials and products toguarantee high quality standardsand constant innovation.IPL produces flexible thermo-plastic tubes for different appli-cations such as agriculture,industry, gardening and hobbies.The range of products includesspiralled tubes and flat hoses aswell as screened and metallicreinforced spiral tubes manufac-tured from materials such asPVC-P, PVC-U, polymeric alloy,polyurethane TPU, TPV thermo-plastic rubber, EVA and polyole-fines.

Under control – Analysis of thermoplasticmaterials ensures product quality

The instrument is princially used to char-acterise:• polymeric alloys• contents of possible plasticisers• content of inorganic fillers• efficacy of PVC thermal stabilisers

(dehydrochlorination)

The TGA/SDTA851e also produces a DTAsignal (comparable to DSC) which isextremely useful for identifying polymersin the compounds – particularly semi-crys-talline polymers.

Thermal analysis has proved to be very use-ful when there have been complaints aboutraw materials. It allows the identificationof unsuitable materials from the point ofview of composition as well as the investi-gation of production problems.

Mr Negri explains: “It is also good to knowthat we can expand the instruments in thefuture especially with the possibility ofcoupling the TGA with an evolved gasanalyser (EGA). Regarding the quantitativeanalysis of volatile compounds such asplasticisers we already obtained goodresults by using the TGA under vacuum.”

IPL found METTLER TOLEDO to be a qualified and reliable partner. “I knew METTLER TOLEDO thermal analysisinstruments from previous working experi-ences,” Mr Negri explains “and I was sureof its usefulness, reliability, ease of use andof the support from, and availability of, METTLER TOLEDO technicians.”

“The TGA/SDTA851e works every time,meets our expectations and has allowed usto solve some previously unsolved prob-lems,” Mr Negri continues, “our choice hasbeen justified by the results achieved.”

T i t r a t i o n Q u a l i t y c o n t r o l

AGIP España is a subsidiary of the ENI Group’s Refining & Marketing Division. ENI(Ente Nacionale di Idrocar-buri) is one of the largestenergy companies in theworld, specialising in theoil, natural gas, electricity generation and petrochemi-cals sectors.

METTLER TOLEDO visited AGIP España’soil and lubricant production plant in Gavá(Barcelona). Plant Manager Mr AntonioTorres explained the factory’s main activityis producing, marketing and selling oilsand lubricants for industry and the auto-motive sector – for both the Spanish mar-ket and export to Europe and overseas. Thefacility also produces fuel for its own chainof service stations and for sale direct to endclients; in the latter field, it is Spain’s lead-ing operator.

The Gavá plant produces 47,500 tons of oilsand lubricants per year and employs 38people, working in two shifts. In terms ofcapacity, it is ENI R&M’s second largestlubricant producer in Europe.

Laboratory Head Mr Joan Pallí showed usthe plant’s Quality Control Laboratorywhere monitoring of raw materials for pro-duction takes place. The department alsoanalyses finished products and packagingand provides technical assistance for usedoils.

Variety of tests for quality purposesTo carry out these controls and thus fulfilquality regulations, the four-strong QualityControl laboratory team undertake a num-ber of analyses. Total Acid Number analysis(TAN) ascertains the durability of the oil,as well as the acidity and alkaline reserve,while Total Base Number analysis (TBN)counteracts any acidity created and exam-ines viscosity, point of ignition, corrosivemetals and density.

Mr Pallí commented that to carry out thesemandatory analyses, where the priority is toachieve the most accurate results, the com-pany uses METTLER TOLEDO equipmentto ensure optimum precision.

Automation speeds up analysesThe Quality Control Laboratory uses aDL53 titrator with a Rondo sample chang-er to determine the state of the used oilssubmitted by carrying out TAN and TBNanalyses. Based on the findings it subsequently advises clients on the oil’sdurability. Now that the laboratory isundertaking more and more technical sup-port services, including examining oils forbuses and machinery oils, the automationwhich the Rondo equipment provides savestime and increases efficiency as staff cancarry out analyses faster.

To determine water levels, analysis is madevia electrochemical reactions using a KarlFischer DL39 coulometer and Strombolisample changer/oven. The equipment isused extensively for analysing base oils as

A trio of titration solutions ensure accurate oil analysis for leadingSpanish company

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well as oils for industry because the ovenallows additives in the oils (which cancause interference) to be tested directly. Mr Pallí explained that the titrator is opti-mised for straightforward routine analysesand is therefore ideal for the type of diag-nosis they need. Again, thanks to theautomation offered by the sample changer,the laboratory staff, who work in shifts, areable to undertake other tasks. As a resultthe DL39 and Stromboli has helpedimprove the testing process for the plant’sQuality Control Laboratory.

In order to determine the water level in cer-tain used oils, where the ignition point istoo low due to contamination from exter-nal agents, such as petrol, the companyuses a Karl Fischer volumetric titrator.

It is through the implementation of theseprocesses that AGIP España manages tomaintain and assure its quality standards.

T i t r a t i o n Q u a l i t y c o n t r o l

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The company is particularly focused on improv-ing products, to ensure that it is safeguarding theenvironment and saving energy. One of its leadingbrands is PULIRAPID, a liquid lime scale remover,which enjoys a market share of 10%. This hasdoubled in the last two years after distributionchannels were strenghtened.

Need to optimise productivityThe R&D and QC team, which is constantly com-mitted to researching new formulations, plays afundamental role in the process of keeping pacein this highly competitive market. Dr Cavalli,head of the team, explains how they have beenimproving processes. “A decision was made tooptimise productivity and we needed accurate andreproducible results. So we decided to buy anoth-er automatic titrator to be used with the one webought two years ago.

“Now we are running two DL5X titrators equippedwith phototrodes that are used to analyse tensides,in particular cationic tenside employed in softenermanufacturing. After quick preparation, samplesare tested and the instrument supplies accurateand reliable results rapidly avoiding the use ofsolvents such as chloroform normally employedin the classic two-phase titration. The whole sys-tem is supervised by a PC using LabX software.

“Considering the necessity to fully consider allrequirements related to the ISO9001 certification,METTLER TOLEDO instruments were chosen fortheir precision and repeatability. We also wantedto reduce operator interpretation and errors. Ourcustomers benefit from us using the latest tech-nology because it ensures them improved andconsistent final product quality.

“As METTLER TOLEDO titrators are easy to oper-ate, we started to analyse not only tensides butalso other active principles which we previouslyinvestigated using other analytical techniques. Wehave now developed and validated specific meth-ods for these as well. As a result the laboratoryoperators are relieved from routine tests and arefree to carry out other analysis to ensure a higherstandard of quality of our products.”

Recently the need to upgrade and automate theanalytical process has meant that Madel has pur-chased a Rondolino sampler changer. “With theintroduction of this the productivity of our labo-ratory has considerably improved, as we can runthe instrument also overnight,” adds Dr Cavalli.

Precise and reliable –Titrators save time and improvequality for household detergentmanufacturer

The Madel S.p.a. company wasestablished 20 years ago by theDella Cuna family. Initially itproduced and distributed itsrange of homecare detergentslocally, before moving into per-sonal care products which weresold throughout Italy.

Today Madel is establishedworldwide, is ISO9001 certifiedand is a member of severalassociations including AISE(International association forsoaps, detergents and mainte-nance products), ASSOCASA(National association for house-hold detergents) and UNIPRO(Italian cosmetics produc. association).