News. Lab. Measuring Polymer Melting for Healthy Sport Shoes. Edition No. 1 / February 2013

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1 Lab Weighing Analytical and solutions Analysis in the Laboratory laboratory 11 News Edition No. 1 / February 2013 Measuring Polymer Melting for Healthy Sport Shoes The quality of sports shoe soles rely on the characteristics of the polymer s raw material used for injection moulding. The moulding process for the production of sports shoes with defined mechanical properties requires an optimal melting temperature. This temperature is determined from the accurately measured melting range of the raw material in question. In order to achieve comparable results, the determination of a melting range should comply to regulations, such as EN ISO This standard is based on the capillary method and details sample preparation, method parameters and the report. The method provides easy and fast access to this important quality control task, which can be made even easier and faster through automization. Simple and efficient melting range determination The METTLER TOLEDO Excellence MeltingPoint Systems exactly fulfill all these analysis requirements. The detection principle is based on the evaluation of the transparency increase during the melting processof a small portion of the substance in a glass capillary. The endpoint is automatically detected and the process video recorded for documentation purposes and subsequent review when necessary. The Excellence Melting Point System comes with the well-proven One Click short cut function for simple, easy-to-learn measurement methods and routines. Up to six individual capillaries can be measured simultaneously for utmost efficiency. Accurate results The instrument records a transmission light and a reflected light video. The transmission light video is evaluated by digital image analysis, which delivers an intensity curve of the melting process (figure 1). The start- and end points of the material s melting process are extracted from the reflective light video and shown in the two images displayed in figure 2.

2 Tips & Tricks Melting Point Determination Figure 1: Typical intensity curve (light transmission intensity vs. temperature) achieved when melting a polyethylene homopolymer powder. The start of melting is evaluated at around 5% transmittance. The end of melting is evaluated at the steep slope change at around 98.5 C. Figure 2: Images taken at important melting events. Top: Start of melting at 89.3 C. Bottom: End of melting at 98.5 C. The measured material is a polyethylene homopolymer powder. Characteristic temperatures, such as the start and end of the melting process, can be evaluated on the intensity curve. A global supplier of sports equipment selected the METTLER TOLEDO MP90 Excellence Melting Point System for their quality control of polyurethane. This material is used in part for the soles of different types of sport shoes, among other things. After thorough testing and application development, several instruments now form the installed analytical instrument base for the reliable quality control of raw polymers. This ensures the high quality production of sport shoes and accessories in various factories around the world. Text: Hans-Joachim Muhr, Market Manager Thermal Values Excellence Watch how One Click melting point determiantion works The melting point is without doubt the thermal value most frequently used to characterize materials. With METTLER TOLEDO Melting Point Systems operators only need to press one button to run a melting point determination! Publisher Mettler-Toledo AG Laboratory Division Im Langacher CH-8606 Greifensee, Switzerland Production LAB Division Marketing Global MarCom Switzerland Subject to technical changes. Mettler-Toledo AG 02/13 Printed in Switzerland. 2 METTLER TOLEDO Lab News 11

3 Chemical Synthesis Beyond the Round Bottom Flask Researchers in synthetic organic chemistry are under increasing pressure to discover and develop new and improved chemical reactions and processes as quickly as possible. While analytical technologies have changed dramatically, chemical synthesis itself has remained largely unchanged for over fifty years. A new type of approach is now helping chemists to redefine the way that chemical syntheses are researched and performed. Know-how Learn more insight about chemical synthesis A white paper is now available that discusses how newly developed methodologies for chemical synthesis are eliminating key challenges and introduces the concept of chemical synthesis without the traditional round bottom flask. New experimental techniques for organic synthesis. Download here: organicsynthesis Historically, the round bottom flask has been the work-horse in the synthesis lab but it has its drawbacks. Heating and cooling of the reaction mass is difficult and imprecise and maintaining temperature over several hours is challenging. In many cases, synthesis steps are impossible to perform unless a scientist is present to supervise the reaction and repeating a synthesis is not always straightforward. A new technology has been developed that helps scientists develop a greater understanding of the reactions they study and has redefined the way organic syntheses are researched and performed while maintaining their current workflow. Replacing the round bottom flask EasyMax and OptiMax synthesis work stations eliminate the need to use heating mantles, oil and ice baths and cryostats. With no training requirement, EasyMax is fast and easy to set-up making users immediately productive. The touchscreen is used to change conditions and program a few steps ahead. Reactions can be run safely unattended day or night and the workstation captures experimental data to deliver an enhanced understanding of the reaction under investigation leading to faster reaction optimization. Every reaction event is captured and experiments are easily compared and repeated. Text: Urs Groth, Head of Communications Reaction Engineering EasyMax METTLER TOLEDO Lab News 11 3

4 Differential Weighing Simplify Ashing Process with Differential Weighing Application Determining sulfate ash content is an important parameter in the quality control of plastic raw materials used in the manufacture of contact lenses. The procedure is based on the differential weighing of a sample before and after ashing using a microbalance or a semi-microbalance. Bausch + Lomb GmbH, in Germany, are now using the built-in application on METTLER TOLEDO s XP56 Microbalance along with an ErgoClip basket for improved sample handling and accurate results. Sulfate ashing is the thermal decomposition of hydrocarbon products using sulfuric acid. The process is used to determine the proportion of inorganic components in a sample and is an important quality control parameter for the incoming inspection of raw materials, such as plastics for contact lenses, to ensure stable material properties. Bausch + Lomb in Berlin, Germany, is one-of the leading international manufacturers of technology-oriented ocular products, including contact lenses, surgical instruments and pharmaceuticals. Sulfate ashing is employed as a quality control tool for pharmaceutical products in line with Ph. Eur and USP <281>. A sample of approximately 5 g is weighed into a tared 30 g platinum crucible, mixed with sulfuric acid and then carefully ashed. After cooling, the sample is reweighed and the sulfate ash content is determined to be around 2 5 mg. Two series of around five different samples are processed in parallel for double determination. 4 METTLER TOLEDO Lab News 11

5 Know-how The METTLER TOLEDO solution for differential weighing The XP56 Microbalance offered Bausch + Lomb the ideal solution. With a readabil ity of 1 µg, the XP56 boasts an unusually high maximum capacity of 52 g perfect for determining the ash content of just a few mg with a relatively high weight tare container. The micro ErgoClip basket fits directly onto the SmartGrid weighing pan so that the crucible can be positioned securely on the balance. The ErgoClip also acts a Faraday cage, dissipating any electro static charges. The XP56 s integrated differential weigh ing application is perfect for Bausch + Lomb s ashing processes: Following entry of a sample ID on the balance terminal, users are guided through the weighing process of the respective sample series. This virtu ally eliminates any risk of confusion or mix-up between samples. The XP56 performs all calculations and eliminates the risk of errors associated with manual calculation and record ing, while saving considerable time. Up to three back-weighing steps are possible until a constant weight is achieved. The application software can manage up to 99 samples, which are broken down into a maximum of 10 series. Au tomatic results storage, including the standard-compliant evaluation of the ashing residue, guarantees traceable results. Learn more about Good Weighing Practice Good Weighing Practice (GWP ) is a universal approach to selecting and testing weighing instruments based on user require ments. GWP allows to reduce measurement errors and ensures reliable weighings in a straightforward and efficient way. Sign up for the White Paper: White Paper However, Bausch + Lomb has experienced difficulties with the process as heating the platinum crucible causes the base to per manently warp so that crucible no longer sits securely on the microbalance weigh ing pan. This leads to extremely long sta bilization times and poor reproducibility. A Risk Based Approach to Select and Test Weighing Instruments Good Weighing Practice (GWP ) is a universal approach to selecting and testing weighing instruments based on user requirements. GWP allows to reduce measurement errors and ensures reliable weighings in a straightforward and efficient way. The differential weighing application on the XP56 Microbalance, coupled with the ErgoClip basket, has guaranteed Bausch + Lomb accurate and error-free differ ential weighing with exceptional trace ability. Text: Stefan Christian, Head Market Support Group Contents 1 2 Summary Selection of a Weighing Instrument 2.1 Specifications & Uncertainty 2.2 Essentials to Select a Weighing Instrument 2.3 Example 2.4 Safety Factor 3 Testing Procedures and Frequencies 3.1 Regulatory Requirements 3.2 Test Procedures 3.3 Test Frequencies 3.4 Test Limits 3.5 Test Weights 3.6 User Tests 3.7 Instruments with Automatic Test and Adjustment Features 4 Appendix 5 Glossary 6 Literature References Laboratory Technicians at Bausch + Lomb praise METTLER TOLEDO s solution for their ashing application. The micro ErgoClip basket holds the platinum crucible securely on the balance. The XP56 microbalance with the micro ErgoClip basket help Bausch + Lomb to control their quality precisely. METTLER TOLEDO Lab News 11 5

6 Two Phase Titrations Made Easy with the DP Phototrode Two Phase Titration Quality control is of utmost necessity for surfactants due to their constant contact with the human body and even the mouth in some cases. Standard methods of two-phase titrations require long and tedious analyses steps. Surfactant quality control is made simple with One Click titration and the DP5 Phototrode. Most surfactants exist in a polar and nonpolar state where one end of the molecule is ideal for bonding with polar molecules and the other end of the molecule is ideal for bonding with water and other nonpolar solvents. These properties make surfactants ideal for removing oil, grease and dirt from our bodies or clothes, but not always ideal for quantitative analysis. Some surfactants and appropriate indicators, such as an anionic dye, are more soluble in polar solvents, like chloroform, yet the titrant is most soluble in water. Standard method Widely recognized by ASTM, DIN and BPI, two phase titrations involve a layer of water and chloroform where the sample and indicator are in the chloroform and the titrant is added to the water layer. After a small addition, the two-phase solution is vigorously mixed to allow the titrant to come into contact with the sample in the chloroform and then allowed to sit and separate for observation. Once all the sample has reacted with the counterionic titrant, the dye moves to the aqueous phase, leaving the chloroform clear with an observable end point. Two phase automation Adding a small amount of titrant, vigorously shaking or stirring the solution, letting it rest and separate for observation then repeating the process can lead to long and tedious analyses of up to 30 minutes in length. METTLER TOLEDO s Excellence Line Titrators and the DP5 s 2-phase titration method can completely automate titration freeing up valuable operator time. The method automatically incorporates the sequence of titrant addition, vigorous stirring for a set time and a settling period with a very slow stir rate before the DP5 optically measures the color of the chloroform. With the One Click titration concept, twophase titrations are as easy as a single button click. The titrator completely automates the solvent addition, titration and calculations unattended. A B C Text: Matthew Eby, Product manager, Titration. Stages of a two-phase titration using specialized two-phase titration beaker, the DP5 Phototrode on an Excellence Line Titrator. A) prior to equivalence point B) at equivalence point C) after equivalence point 6 METTLER TOLEDO Lab News 11

7 Know-how Gain Accuracy and Save Money in Balance Testing A world-famous food & beverage manufacturer with a US$100 million-plus annual turnover needed to confirm minimum weights for balances in their standard setting, Singapore based R&D facility. Quality assurance managers now insist on GWP Verification for bullet-proof documentation and enhanced accuracy during internal reviews. Learn more our risk based approach to select and test your weighing instruments Get insight into typical customer cases and configuration examples by downloading our complimentary white papers. The company s goal was to reduce the environmental impact for product and package manufacturing. However, the company s QA manager suspected that minimum weights on several balances at their Singapore based R&D facility, which helps set quality standards for plants worldwide, were giving inaccurate readings. Fearing skewed results - and the errors and waste that comes with them he sought a methodology that could help ensure accuracy and set the stage for subsequent improvements across multiple manufacturing operations. GWP and local regulations The GWP Verification solution is uniquely designed to help manufacturers set and confirm minimum weights for accurate results while meeting process requirements. Before Good Weighing Practice could be used in a comprehensive SOP review, METTLER TOLEDO Singapore needed to assure management that GWP works within, and not alongside, a wide range of QA schemes in use today. This included their national standard (SAC- SINGLAS). ISO accreditation was also mandatory for the company. Complementing internal procedures Ultimately, this food & beverage manufacturer ordered a complete GWP Verification. While SOPs were found to be solid, the GWP Verification assessment complemented the company s existing ISO calibration protocol. METTLER TOLEDO Singapore was also able to make several helpful suggestions for balance adjust ments and capital investments that would enhance accuracy and reduce waste. These improvements have paid for themselves many times over through savings in materials and fewer bad batches at plants around the world. Gaining compliance and peace of mind In addition to guaranteed accuracy and, therefore, product quality, the QA manager also gained peace of mind that his minimum weight values were safe. METTLER TOLEDO s GWP Verification output was able to validate the company s internal quality standards and issue ISO certificates for all new balances to further ensure bullet-proof weighing procedure compliance during audits. Based on the savings this global company is beginning to see as a result of more accurate weighing and recipe formulation, one executive noted that GWP Verification is a new must have standard for their internal quality evaluations. To learn more about how GWP Verification can help meet internal quality demands and external compliance requirements, visit: Text: Dimitri Burkhard, Product Manager GWP Download free GWP White Papers: White Paper A Risk Based Approach to Select and Test Weighing Instruments Good Weighing Practice (GWP ) is a universal approach to selecting and testing weighing instruments based on user requirements. GWP allows to reduce measurement errors and ensures reliable weighings in a straightforward and efficient way. Contents 1 Summary 2 Selection of a Weighing Instrument 2.1 Specifications & Uncertainty 2.2 Essentials to Select a Weighing Instrument 2.3 Example 2.4 Safety Factor 3 Testing Procedures and Frequencies 3.1 Regulatory Requirements 3.2 Test Procedures 3.3 Test Frequencies 3.4 Test Limits 3.5 Test Weights 3.6 User Tests 3.7 Instruments with Automatic Test and Adjustment Features 4 Appendix 5 Glossary 6 Literature References METTLER TOLEDO Lab News 11 7

8 Good Measuring Practices Good Measuring Practices Reliability Throughout the Lifecycle Good Measuring Practices by METTLER TOLEDO is a global program supporting you in laboratory and production environments with quality assurance recommendations for weighing, pipetting and chemical analysis. The five steps of every Good Measuring Practices guideline cover the entire lifecycle of your instruments. By focusing on your processes and its associated requirements and risks, we provide you with effective measures to maximize operational security and minimize testing efforts and process risk. GWP Good Weighing Practice GTP Good Titration Practice GPP Good Pipetting Practice Guaranteed better weighing results GWP helps ensuring consistent product quality and avoiding outof-spec results or bad production batches. With GWP you comply with all regulations relevant to your industry for a minimal time and financial investment. GWP provides documentation to verify the accuracy of your balances and recommends optimal testing procedures. Reliable results and dependable titration in practice GTP forms the basis of dependable and risk-free titration. The appropriate titration system is selected based on user requirements, and professionally commissioned and installed. GTP helps protecting your investment far into the future, supporting you with tailored training and equipment qualification. It also proposes schedules for regular inspection and preventive maintenance. Optimize workflows for more reliable and repeatable results Improve your data quality with GPP our comprehensive, systematic approach to maximizing pipetting accuracy and repeatability. GPP is grounded in 40+ years of expertise working side-by-side with researchers in order to achieve the highest level of accuracy and precision across all applications METTLER TOLEDO Lab News 11

9 GDRP Good Density and Refractometry Practice GEP Good Electrochemistry Practice Minimize risk and improve performance GDRP is based on our expertise in density and refractive index measurement. Understanding the reasons and sources of measurement errors helps improving quality while reducing risks and costs. Professional commissioning, training, qualification and seamless documentation guarantee compliance with your process requirements from the very first step. Optimized ph results from the beginning GEP assists with professional tools and documentation to get reliable results for your laboratory ph, conductivity, DO, ion and redox applications. Use GEP to select the correct calibration solutions to comply with regulations, perfectly maintain your sensors to optimize product lifespan and reduce costly measurement mistakes to a minimum. Check your risks in weighing, titration and chemical analysis Risk Check All of the Good Measuring Practices guidelines start with an evaluation of your measurement processes and an assessment of their associated risks. Based on this information, you are provided with straightforward recommendations for selecting, installing, calibrating and operating your devices. For more Information: Good Measuring Practices METTLER TOLEDO Lab News 11 9

10 Product Highlight Boost Productivity with Fast and Accurate Moisture Control For determining the correct moisture content in plastic granulates, the new generation HX204 Halogen Moisture Analyzer is perfect. With a resolution of 0.001% MC the high measurement performance of the HX204 ensures outstandingly accurate results. The easy-access weighing pan, real-time drying curves, integrated control charts and the unique graphical user interface combine to give you a moisture analyzer that is convenient and intuitive to use and requires only very little training. Clear Decisions With process control limits, a green or red results screen indicates the pass/ fail' of measurements at a glance. Control charts monitor any trend in results over time and provide increased process control. Easy Cleaning The measurement chamber is flat and fully sealed and can be cleaned in a matter of seconds. Furthermore, the weighing cell is fully protected and any spilled samples do not interfere with the weighing result. Ensure valid moisture results SmartCal is a granular test substance to check Moisture Analyzers and reliably verifies whether the instrument is working within specifications. Order your free SmartCal sample: METTLER TOLEDO Lab News 11

11 Precise and Secure ph Measurements with SevenExcellence The SevenExcellence easily deals with the demanding data input, measurement and archiving tasks that are so important during production and for the QC of raw materials and finished products. It has an ingenious method concept ensuring that each particular analysis is always performed with the identical, SOP compliant settings. Its professional user management system eliminates the risk of unintentional or unauthorized changes to settings and deletion of results. Start a method with OneClick The intuitive touch screen menu speeds up and simplifies the instrument s operation. Flexible peripherals Choose from a vast collection of peripherals to increase efficiency and optimize workflow even further. Modular expansion New measurement parameters can be added to the instrument at any time to make it flexible and expandable enough to cope with any measurement requirements. METTLER TOLEDO Lab News 11 11

12 Everything in Our Lab Works With Just One Click Joanne, laboratory assistant: "Thanks to my personalized Homescreen, I can perform all the different analyses very quickly and efficiently." Bob, production assistant: "All I have to do to analyze the intermediate product every hour is press a Shortcut." Clark, quality assurance: "The individual user rights feature means that I can make sure that users stick to our quality guidelines." The One Click operation provides unsurpassed user guidance, secure navigation and easily selectable and adaptable methods. Learn more and see One Click in action: Key benefits of One Click operation: Know one know all One Click is a common interface for all your lab instruments. This means, if you can program and run analyses on a balance, you can also do it on a titrator, without extra information required. See only what is relevant to you User screen individualization permits you to adapt your home screen to your requirements: You only see what you need and avoid confusion by unneeded functionalities. Play by the rules Adherence to SOPs is now a functionality of your instrument via the pre-programming of methods. Transcription and calculation errors a thing of the past. Mettler-Toledo AG Laboratory Division Im Langacher CH-8606 Greifensee, Switzerland For more information