Simplified pH Values of Agrochemicals Surfactants€¦ · Rhodia relies on METTLER TOLEDO’s SevenExcellence S400 and InLabRoutine Pro Sensor for accurate and secure analyses. Rhodia

1News

Chemicals & PetrochemicalsAnalytical solutions in the laboratory

February 2014

An accurate pH value is a fundamental parameter in ensuring the high-est quality and performance of the surfactants used as emulsifiers in agrochemicals. Standard pH regulation UNI 24003 (AS™ - E70) toler-ates almost no margin of error. Rhodia relies on METTLER TOLEDO’s SevenExcellence S400 and InLabRoutine Pro Sensor for accurate and secure analyses.

Rhodia is a specialty chemical com-pany and member of the larger chemi-cal group ‘Solvay’. Rhodia is located in Italy and began commercial operations in the 1950s. Today, Rhodia holds a lead-ing position in supplying a large range of surfactants used as emulsifiers in agro-chemicals.

Stability and turbidity under controlThe right pH value is essential for en-suring the quality and efficiency of sur-factant solutions. In particular, pH has important effects upon the stability of the emulsion formed by the surfactants, as well as the color and turbidity of the final products.

An incorrect pH value can cause the sep-aration of the phases in the emulsion, color changes (degradation) or turbidity (separation of the inorganic salts) of the final products, which all have a negative effect on quality.

When surfactant solutions arrive at the Rhodia laboratory, the operators im-mediately check the pH and eventually correct it before verifying the emulsify-ing power of the solutions. Rhodia per-forms these pH measurements according to standard UNI 24003 (AS™ - E70) and must assure an accuracy of ± 0.2 pH. The range of measurements is normally between 5 to 7 pH so they perform a two point calibration with buffer solutions 4.00 and 10.00 pH.

Simplified pH Valuesof Agrochemicals Surfactants

2 METTLER TOLEDO Chemicals & Petrochemicals News 1

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

Production LAB Division MarketingGlobal MarCom Switzerlandwww.mt.com/lab-segmentnews

Subject to technical changes. © Mettler-Toledo AG 02/14 Printed in Switzerland.

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Proven instrument interfaceRhodia has been using a SevenMulti with InLab Routine and an external NTC30K Temperature Sensor for several years. Being satisfied with its performance, they decided to update their lab with the new SevenExcellence generation.

Lab technicians particularly appreciate the new One Click® user interface, “We already use a Titrator Excellence T50

in our lab and the possibility of having the same interface allowed us to install and start using new SevenExcellence in a very short time’’.

Traceability: The full pictureSevenExcellence makes it possible to di-rectly save calibrations and measure-ment protocols in PDF format on a USB flash drive. “In this way, we have fully traceable data and can easily create a database of our results,’’ Explains Rho-dia’s QC Manager.

Rhodia has always chosen the latest state-of-the-art in pH measurement solu-tions from METTLER TOLEDO in order to deliver the highest quality surfactants solutions – making the transition now from SevenMulti to SevenExcellence.

Text: Konrad SägesserMarketing Manager pH Lab

www.mt.com/sevenexcellence

Surfactants’ pH measurement wit SevenExcellence at Rhodia’s lab.

All you need to know about pH

Our pH guide provides clear and useful descriptions of how pH is measured, offers a com-prehensive pH applications overview and provides for tips and tricks on proper pH mea-surement

Get your copy now

www.mt.com/lab-ph-guide

Tips & Tricks

An emulsifier (also known as an ‘emulgent’’) is a substance that stabilizes an emulsion by increasing its kinetic stability. An emulsion is a mixture of two or more liquids that are nor-mally immiscible. ‘Surface ac-tive substances’, or surfactants, is one class of emulsifier.

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Natural science laws experience “live” – learn easily

pH T

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A Guide to pH Measurement Theory & Practice of Laboratory pH Applications

Laboratory environment

Practical description of

how to measure pH

Our pH guide provides clear

3METTLER TOLEDO Chemicals & Petrochemicals News 1

Testing petrochemical samples has its challenges. Whether dealing

with volatile samples and solvents, odoriferous fumes or hard to

dissolve matrixes; InMotion Autosamplers make for simple, safe

and controlled titrations.

Solvents used for the titration of petro-chemicals are not very pleasant. Tolu-ene, chloroform, acetic acid, dichloro-benzene, etc., are not only unpleasant smelling, but potentially hazardous to the health of personnel. InMotion Auto-sampler CoverUp™ Lid Handling Kits protect operators simply and effectively from hazardous solvents and fumes. Sim-ply place the lids onto titration beakers, remove them just prior to analysis and replace them promptly after a titration.

Total sample controlProtecting samples is an important step in any titration safety checklist, espe-cially when handling volatile samples. Not only does the CoverUp System help

to protect operators, but it also pro-tects volatile samples. Further protect volatile samples from evaporation by combining the CoverUp System with a water-bath rack and an external water- bath chiller. Use the water bath rack to automate methods requiring tempera-tures of around 4 ºC (e.g. methyl mercap-tan content or bromine index) according to standard AS™ and DIN procedures.

Raise the temperature on the water-bath rack to help dissolve difficult sam-ples, such as crude or used engine oils. Normally requiring the addition of chlo-roform, these samples are easily dissolved in standard TAN AS™ D664 solvent at higher temperatures.

The InMotion Autosampler not only au-tomates processes, but also handles very different and difficult situations when combined with the necessary accessories. Keep operators safe and samples secure with InMotion Autosamplers for optimal productivity.

Text: Matthew EbyProduct Manager Titration

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Protect Samples and Operators with InMotion™ Autosamplers

Titrator T70 with InMotion Autosampler.

Protect Samples and Operators

Titrator T70 with InMotion Autosampler.


Parti

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Crystallization and precipitation are two of the most important separa-

tion and purification processes in the chemical industry. Crystallization

throughput and product quality are improved by optimizing the particle

size distribution. Today, established technologies measure particle

size, shape and count inline in order to make real-time, informed deci-

sions and, therefore, ensuring quality and replicability.

Chemical companies are under increas-ing pressure to understand and develop scalable crystallization processes faster, at lower costs and with higher quality. Companies must control crystallization conditions if they want to improve cycle times and optimize product quality and yields. The need to produce products with a specific particle size distribution con-tinues to drive crystallization research.

Challenges with crystallizationIf misunderstood, the thermodynamics and kinetics of crystallization can some-times result in unexpected behavior, such as rapid precipitation or agglomer-

ation, which leads to variability in yield, centrifugation times and other quality attributes. It has been established that the root cause of this variability is often inconsistency in the particle size distri-bution. Fine particles or agglomerates can form in the crystallizer. These cause slow centrifuge throughput caking, dust, or bulk density problems in transport and consequently particle size leading to quality variability in the final product. These problems can be controlled in the crystallizer by measuring crystal growth rates while optimizing solvent addition rates, mixing conditions, seeding and cooling rates.

Understanding crystallization with in situ analysisA well-designed crystallization or precip-itation process can be scaled-up to man-ufacturing giving the desired crystal size distribution, yield, form and purity. In-line particle size and shape analysis al-low scientists and engineers to measure and observe crystal behavior in situ with-out sampling or dilution. Crystal nu-cleation and growth are tracked at full concentration and operating tempera-ture and this information is then used to troubleshoot the root cause of variabil-ity and optimize processes. By applying real-time measurements, scientists and

Optimize Industrial Crystallization Track Particle Size Inline


engineers understand when and why in-consistencies occur and can then make informed decisions on how to produce repeatable, high quality products.

Tracking real-time particle size distributions ParticleTrack inline particle measure-ments ensure a clear understanding of how changes in fundamental process variables directly impact upon the final product. Inline technologies track criti-cal parameters, such as the crystal size and shape, crystal form and even the level of supersaturation, all at full pro-cess concentration and in translucent or opaque slurries. ParticleTrack provides process knowledge that enables real-time

improvements in yield, throughput and profitability of laboratory- or process-scale crystallization. It accelerates the characterization of critical operating pa-rameters for increased productivity and identifies undesired events in real-time to fully ensure final product quality.

Text: Ben SmithMarket Manager Particle System

Characterization

www.mt.com/particle_track

Read our white paper to better understand how in-line particle technology is used to comprehend, op-timize and control crystallization in order to improve product quality and yield.

Optimize Industrial Crystallization by Tracking Particle Size InlineA Review of Modern Technologies

Benjamin Smith, Brian O’Sullivan, Mettler-Toledo AutoChem, Inc.

Industrial crystallization is an important separation and purification step in the chemical, food ingredient, and mining industries, yet it is often treated as an art rather than a science. If misunderstood, the thermodynamics and kinetics of crystallization can sometimes result in unexpected behavior such as rapid precipitation or agglomeration which leads to variability in yield, centrifugation times, and other critical quality attributes. It has been established that the root cause of this variability is often inconsistency in the particle size distribution1,2,3,4. Fines or agglomerates can form in the crystallizer which cause slow throughput in the centrifuge,

caking, dust, or bulk density problems in transport and consequently particle size and quality variability in the final product. Particle size is also directly correlated with yield. Many of these process inconsistencies can be solved by understanding, optimizing, and controlling the crystallization unit operation.

In the crystallizer, solvent addition rates, impurities, mixing conditions, seeding, and cooling rates, all impact process performance. By tracking the rate and degree of change to particles and particle structures as they naturally exist in process, scientists and engineers proactively measure, understand, and

optimize process conditions in real time to consistently achieve targeted particle size, yield and quality specifications, in the lab or manufacturing.

Today, inline particle characterization technologies are used to provide inline particle size, shape and count measure-ments at full process concentrations and in translucent or opaque slurries. Companies including the American Crystal Sugar Company3, Dow5, Archer Daniels Midland (ADM)6, and Nestle7 have successfully applied best practices with inline particle size characteriza-tion to collect real time data and ensure true statistical understanding of their process.

Case Studies from the Chemical, Food Ingredient, Mining and Minerals Industries

www.mt.com/wp-industrial-crystallization

ParticleTrack E25


Worry-Free Weighing Follow the Green Light

“Laboratories are facing increased pres-sure to comply with industry regulations, such as United States Pharmacopeia (USP) Chapter 41 and Good Manufactur-ing Practice, to improve overall equip-ment effectiveness, reduce total cost of ownership and increase profit margins. METTLER TOLEDO has designed a new line of analytical balances, in conjunc-tion with customer to ensure end-re-sult accuracy and compliance. Through streamlining processes, these balanc-es will enhance laboratory efficiency and reduce operational overheads, such as operator time,” Says Simon Taylor,

Product Manager of analytical balances at METTLER TOLEDO.

Giving weighing the green lightWhen balance calibration and routine tests are up to date, the StatusLight™ built into the edge of the balance termi-nal provides confirmation at a glance. A green light means that it’s safe to start weighing. Warnings are shown in yellow and errors in red. The user has the secu-rity of knowing that all acquired weigh-ing results meet pre-defined process re-quirements and, hence, also the relevant regulations.

Electrostatic solutionsInfluences from electrostatic charge are one of the biggest challenges in analyti-cal weighing. Through normal handling, samples and weighing containers can easily accumulate static, leading to dif-ficulties in dosing and errors in weigh-ing results. With high electrostatic in-fluence, it may not even be possible to achieve a stable reading on the balance. When a container or sample is placed on the balance, StaticDetect™ measures the weighing error attributable to electro-static charge and gives a warning if the process tolerance limit is exceeded. An-

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METTLER TOLEDO’s new XPE and XSE balances introduce a new dimension in analytical weighing with a combination of features that make daily weighing tasks easy and error-free. Benefit from solid weighing performance and ensure full regulatory compliance and high process security.


The enhanced XPE terminal with StatusLight™ pro-vides at-a-glance information of the balance readiness for weighing.

RFID technology in our SmartTags sim-plifies workflows and avoid transcrip-tion errors and mix-ups.

StaticDetect™ warns you when electro-static charges might affect the weighing results.

tistatic measures can then be employed. The new compact point electrode acces-sory attaches to the side of the balance for convenient deionization of charged samples and containers. For the highest process security, users can elect to block the release of the weighing result.

Processes under controlBy fixing SmartSample™ RFID tags to titration beakers, sample information en-tered at the balance can be securely trans-ferred to METTLER TOLEDO’s titration autosampler. RFID tagged pipettes can also be scanned at the balance via

Easy Scan™ in order to check calibration and test dates, guaranteeing that pipettes are valid for use. Test dates on the tag can be updated when the pipette check is carried out using the built-in balance application. The new RFID capabilities not only eliminate transcription error but also offer users a higher level of process security.

Go paperlessAll the new balances are fully compati-ble with METTLER TOLEDO’s LabX lab-oratory software, which guarantees pro-cess security and manages measurement

uncertainty. Full traceability is assured thanks to flexible Standard Operating Procedure (SOP) user guidance on the balance touchscreen, automatic calcula-tions and comprehensive data handling. LabX fulfills the highest process securi-ty requirements and, with all data stored securely in a central database, fully supports the move towards establishing a paperless lab.

Text: Simon TaylorProduct Manager

Excellence analytical balances

www.mt.com/green-light

8 METTLER TOLEDO Chemicals & Petrochemicals News 18 METTLER TOLEDO Chemicals & Petrochemicals News 1

Met

hod

Libr

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Always at hand

Search, download and store your meth-ods in a convenient and easy way. The digital method library is always acces-sible from any digital device. No more leafing through endless book pages.

+60 years of knowledge

It is been long since in 1945 Dr. Erhard Mettler, a Swiss engineer, invented the substitution principle with a single-pan balance. Since then we have developed and tested many precision instruments. Benefit from this wealth of knowledge for free.

+2000 methods

More than 2000 methods for our titra-tors, thermal analysis instruments and moisture analyzers are available to you. Find the right method in the shortest time thanks to the filtering options.

Setting up a new Method in Your Instrument?Let us Give You a Hand

Setting up a new measuring method in your instrument for the first time is not straightforward if lacking the right instructions. METTLER TOLEDO has attained over the years a wealth of know-how about instruments’ methods for a broad range of industry applications. This compendium of knowledge is just one click away from you.

Four Steps to Your Desired Instrument Method.

Methods pages available for:Thermal Analysis www.mt.com/ta-applicationsTitration Analysis www.mt.com/titration_applicationsMoisture Analysis www.mt.com/moisture-methods

1. Go to www.mt.com/ta-applications

2. Define the search criteria either with filters or keywords

3. Get your search results

4. Download your application method

www.mt.com/ta-applicationswww.mt.com/titration_applicationswww.mt.com/moisture-methods

Methods pages available for:Methods pages available for:Thermal Analysis www.mt.com/ta-applicationsTitration Analysis www.mt.com/titration_applicationsMoisture Analysis www.mt.com/moisture-methods

Methods pages available for:

Thermal Analysis Application No. UC 293Application published in METTLER TOLEDO Thermal Analysis UserCom 29

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Measurement of thin films in shear by DMA

IntroductionIn the DMA, a sample undergoes periodic deformation. However, the force neces-sary to deform the sample acts not only on the sample but also on the sample holder. This means that the measured displacement amplitude is the sum of the deformation of the sample and the defor-mation of the sample holder. Ideally, the deformation of the sample holder should be negligible compared with the defor-mation of the sample.

When thin samples (thickness < 0.2 mm) are loaded in the shear sample holder, the danger is that the shear clamping plates tilt slightly and touch each other.

The results from a DMA measurement performed under these conditions are then completely wrong. To make sure the plates do not touch each other, one intuitively tends to measure thin sam-ples with large diameters. The stiffness

of such samples might then be greater than the stiffness of the sample holder. In such cases, the deformation of the sample holder contributes more to the to-tal deformation than the deformation of

the actual sample. When the modulus is calculated, the measured total deforma-tion or stiffness must be corrected. This is done using the so-called stiffness cor-rection.

Thin films with a thickness of 50 to 200 µm are usually measured in tension in the DMA. They can, however, also be measured in shear if proper attention is paid to sample prepara-tion and other factors. In this article, we present two examples to show how this is done.

Figure 1. Determination of the sample holder stiffness from a “displacement scan” for the shear sample holder. The alignment insert for the small clamping assembly was used as a sample.



www.mt.com/easysampler

Representative samplingA unique probe operation enables auto-matic sample quenching at the point of sampling. This eliminates the variabil-ity caused by the delay between sample point and quench, providing more ac-curate, precise and consistent sampling data.

Understanding Reaction DynamicsAcross a Wide Range of Conditions

Taking samples from reactions and analyzing them using offline methods is an established technique to better understand reaction progress, product conversion and determine impurity profiles. How ever, taking samples is not always a precise operation due to difficulties in handling reaction matrices, temperature, pressure and delays in quenching the sample. These processes can all lead to inaccuracies. With the new EasySampler, instrument sampling is carried out automatically and inline.

Unattended operationSamples are taken at the touch of a button. If unattended sampling is re-quired, a sample sequence can be pro-grammed to provide sampling opera-tions, day or night.

Difficult matricesOvercome the difficulties of sampling homogeneous, heterogeneous, slurries and viscous reaction mixtures using the same probe. Samples can be taken un-der a wide range of temperatures and pressures enabling the sampling of 95% of liquid systems found in a R&D lab.

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www.mt.com/LabXTitration

WorkbenchEach instrument connected to LabX has its own workbench. It offers all the components needed to run your dai-ly tasks and the tools to monitor your sample series and results.

LabX® TitrationPower Your Titration Bench

Single SoftwareLabX connects your titrators, balanc-es, density meters and refractometers, melting point instruments and Quan-tos systems. This means less training and also helps increase your efficiency.

Software ArchitectureLabX can be installed as single software or as a distributed system. Build up the system that suits your need and have ac-cess from any PC to LabX and your in-struments in the laboratory.

Titration joins the LabX family. Connect your METTLER TOLEDO instruments to LabX software and benefit from simplified op-eration, efficient method editing with the graphical layout, fast sample series modifications and tailored reports. LabX uniform software and interface means less training and also helps to increase your efficiency.

www.mt.com/lab-chemicals

Info Spot

For more information

From crude to gasoline, diesel, liquid gas, lubricants, plastics and many other end products, petrochemicals are ever present in our lives. The number of standards available for analysis further reflects the importance and variety of petrochemical raw materials and products.

Our Petrochemical Industry guide advises you on the right analytical solution to achieve accurate and compliant results.

• Density measurements of crude oils and refined products

• Water content test in crude oils by Karl Fischer• Dropping and softening point of polymers

or waxes. • OneClick operation for simplicity

www.mt.com/lab-petrosolutions

Analytical Solutions for the Petrochemical Industry

Mettler-Toledo AGLaboratory DivisionIm LangacherCH-8606 Greifensee, Switzerland

Analytical InstrumenAnalytical Instrumenfor the Petrochemical Indu

Petro

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Analytical InstrumentsAnalytical Instrumentsfor the Petrochemical Industry

The METTLER TOLEDO DP Excellence instruments enable automatic and video-recorded dropping and softening point testing of pitch, asphalt/bitu-men, polymers and waxes. Standard compliant cups and test methods, secure sample preparation and the innovative visual camera observation with digital image analysis ensure comparable and reliable results.

Automated Drop and Softening PointStandard-Compliant and Video-Recorded

A

B

Automated Lubricant Grease Drop Point TestingTime consuming manual lubri-cant drop point tests according to ASTM and IP standards can be securely automated with the DP70 Excellence system. The video-based image analysis reli-ably detects the drop point event. Operator-dependent result inter-pretation becomes a thing of the past.

Standard-Compliant Soften-ing Point Tests of Bituminous SamplesMETTLER TOLEDO instrument specified ASTM D3104/D3461 standards are widely accepted for quality control of bituminous materials. The video-recorded process may be played back for verification. The test efficiency is notably improved by simultane-ous analysis of two samples.

Sample Carrier Increases Safety and EfficiencyA cup lid with vent hole prevents spilling and furnace contamina-tion in case of expanding sample B Standard compliant cup for dropping or softening point deter-minations C disposable glass collector The sample carrier keeps all parts together and can be placed into the stand D.

Comparable Drop Point Tests of Polyolefines and WaxesPolymers and waxes can be eas-ily prepared with the smart sam-ple preparation tool. It enables repeatable sample preparation by controlled filling of the drop point cup with the pre-melted sample. The ASTM D3954 based drop point test ensures excellent result comparability.

One Click® ResultsThe color touch screen enables intuitive operation and provides clear information. Just one click is all that is needed to start the measurement – the instrument does the rest for you. The end of the measurement is signaled with an acoustic tone and measured results are displayed.

Watch the one click-dropping point video

CD

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Simplified pH Values of Agrochemicals Surfactants€¦ · Rhodia relies on METTLER TOLEDO’s SevenExcellence S400 and InLabRoutine Pro Sensor for accurate and secure analyses. Rhodia