moisture and other volatile components plus investigating the thermal stability of a material.

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1 Machinery, Plastics, Electronics Analytical solutions in the laboratory 11 News The Key to Improving Electronic Packaging The packaging material used for integrated circuits in electronic equipment is generally an epoxy based compound. It is important that the epoxy has excellent thermal and dimensional stability as well as good weatherproofing properties. The characterization and selection of raw materials is paramount for a high quality end product. In the semiconductor packaging industry, process engineers are often faced with many questions when selecting suitable raw materials. Questions likely to arise include: What are the outgassing properties of the material? Is the material thermally stable at a given temperature? Thermogravimetric analysis (TGA) is an excellent technique suitable for raw material selection as it presents engineers with the answers to these questions. The METTLER TOLEDO TGA/DSC 1 provides engineers with great insight into material selection. The TGA/DSC 1 has the advantage of being able to detect very small weight changes. This is a useful tool when characterizing important material properties, such as outgassing of moisture and other volatile components plus investigating the thermal stability of a material. Determining temperature limits using TGA The results in Figure 1 (page 2) illustrate how easily the TGA/DSC 1 can determine the temperature limits of an uncured epoxy resin sample by investigating decomposition behavior. Two mass loss steps are easily identified on the TGA evaluation in Figure 1. The first, between 30 and 100 C, displays moisture loss. The second, beginning at 140 C, shows the start of the epoxy sample decomposition through pyrolysis. This results in the release of volatile reaction products. The SDTA curve

2 Materials Characterization provides a better visual separation of the individual mass loss steps. It also yields additional information that helps in the interpretation of the curve and displays effects that are not accompanied by mass loss. Thermogravimetric analysis is an excellent technique for the determination of an epoxy based compound s temperature limits where the compound is commonly used as an encapsulation material in the semiconductor packaging industry. The METTLER TOLEDO TGA/DSC 1 is a valuable tool for the characterization and selection of materials. With its wide measurement and temperature range, the TGA/DSC 1 has the ability to measure both small and large samples from ambient temperature to 1600 C. Thanks to its modular design, the TGA/DSC 1 is the ideal instrument for manual or automated operation in production, quality assurance or research and development. Figure 1. TGA curve of an uncured epoxy resin sample. (Source: Collected Applications Thermosets) Text: Dr. Matthias Wagner, Product Manager, Materials Characterization 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 08/13 Printed in Switzerland. 2 METTLER TOLEDO Machinery, Plastics, Electronics News 11

3 Seeing is Believing Melting of Polymers It is often difficult to conclude what happened to a heated sample from a thermal analysis experiment alone. Additional information, derived from the visual appearance, can help with this interpretation or support already drawn hypotheses. Thermal analysis results, combined with optical analysis (thermo-optical analysis), can be achieved with microscopy in transmission or reflective mode. Hot-stage microscopy is used in transmission mode and DSC microscopy is applied in reflection mode. In both cases, the sample is illuminated by a light source and observed through a microscope optic with the naked eye or a digital or analogue camera. The camera is connected to a computer with installed software that records and evaluates the images produced. Suitable software overlays temperature (for dynamic-) or time (for isothermal experiments). Modern software is also capable of evaluating light intensity in regions of interest. Hot-stage microscopy (HSM) measures samples in a temperature range between -50 C up to around 400 C. The HS84, DSC Microscopy Cell simultaneously measures a heat flow curve. Microscope design and focal length need to be adapted to the operation for hot-stage. A microscope polarization option facilitates the distinction of different crystal morphologies. Typical effects observed with hot-stage microscopy in polymers include: Melting Crystallization Crystal growth The analysis of crystal growth can also be used for the determination of crystallization kinetics. The analysis of melting is part of the EN ISO 3146 [1] standard. The ASTM F706 [2] standard concerns the characterization of polymers with HSM. The following example illustrates a multilayer polymer film melting investigation. A cross section of a polymer film was placed on a microscopy slide, which was inserted into a microscope hot-stage. The microscope was operated in polarization mode which displays solid compounds of the sample bright and molten dark. After preparation, the sample was heated at a constant rate. The original multi-layer structure of the sample (A, B, C from left to right) is clearly visible at 102 C. At 110 C, the second layer from the right (B) is molten. All layers to the left (A) have then melted by 125 C. The last layer (C) finally melts with the analysis finishing at 129 C. Conclusion The melting of different layers of polymer films could can be measured with DSC but recognizing which layer melts when is impossible. This can only be achieved with the additional, visual information achieved by hot-stage microscopy. Text: Dr. Matthias Wagner, Product Manager Materials Characterization Microscopic images of a multi-layer polymer film cross section in polarization mode while heated on the microscope stage. Bright areas of sample indicate solid matter and dark areas indicate molten. References: [1] ISO 3146: 2000: Plastics - Determination of melting behavior (melting temperature or melting range) of semi-crystalline polymers by capillary tube and polarizing-microscope methods. [2] ASTM F706: Determination of Fusion Temperature of Dry Electrostatic Heat-Fixing Toners. METTLER TOLEDO Machinery, Plastics, Electronics News 11 3

4 Sample Weighing Weighing Polymer Contamination Ensures Your Computer Works Correctly Electronic components in computer hard disks may not function correctly if the level of non-volatile residues (NVRs) present on the polymer parts is too high. A leading global producer of specialty polymers uses METTLER TOLEDO balances to ensure their polymers meet the computer industry s strict requirements. This Asian-based manufacturer produces specialty polymers for a broad range of consumer and industrial applications, including a range of different polymers, such as acrylic, polyester and urethane, for computer hard-disk manufacturers. The company performs NVR tests as part of their quality control procedures to ensure that the level of organic contamination remains within the required limits. Determining contamination ASTM E1235 is one such standard test method for the gravimetric determination of NVRs on surfaces in environmentally controlled areas, including electronics manufacture: The polymer sample is rinsed with 30 ml of pure hexane which is collected and allowed to evaporate. A control sample of 30 ml hexane is tested in parallel. The residues remaining are weighed. Other relevant testing standards include IDEMA M7-98 and MIL-STD-1246C. Gravimetric solution With a readability of 0.01 mg, METTLER TOLEDO s Excellence XP205 Analytical Balance has the level of accuracy required for weighing the small samples generated in this process. The built-in MinWeigh function provides a warning if the sample weight falls below the acceptable limit to ensure an accurately determined result. SmartSens sensors allow hands-free operation to improve operational efficiency. Furthermore, METTLER TOLEDO s Good Weighing Practice (GWP ) quality assurance assistance helped the company to select the most appropriate balance and to define and establish a balance testing regime. Choosing the XP205 has ensured that the company can prove the quality of their products to even the most demanding of customers. Text: Walter Krebs, Product Manager The XP205 was used to test the amount of NVR contamination. Electronic parts are sensitive to particles on plastic components. 4 METTLER TOLEDO Machinery, Plastics, Electronics News 11

5 Know-How Intelligent Functionality Means a Balance You Can Count On A thorough piececounting solution The accuracy of piece counting can greatly influence profits. Mistakes can be costly and translate as overfilling costs, unstable production processes, waste and reputational damage. METTLER TOLEDO s NewClassic MS16001L eliminates all these problems directly on the factory floor. Accuracy is key when counting thousands of parts every day. Piece counting with balances or scales is a simple and fast way to determine quantities of parts for a variety of purposes, including goods receiving, warehousing, production or shipping. Manufactured parts and sub-assemblies are produced in their millions. Weighing them individually isn t always feasible but weighing a larger, known quantity is a quick way of spotting a production quality problem. Piece counting is also a fast solution for determining the number of items in a container. These quality control checks typically take place directly on the factory floor requiring a balance that can provide fast yes/no answers under relatively harsh conditions. NewClassic MS16001L NewClassic fits the bill Thanks to the combination of durability, intelligence and fast settling times, the NewClassic MS16001L copes easily with both of these requirements. The robust aluminum housing offers IP54 In-Use to protect the interior of the balance against dust and splashing liquids. The MonoBloc weighing cell is highly durable and safeguards the balance from accidental overload. The balance will continue to work perfectly even if a heavy box of parts is accidentally dropped onto the weighing pan. Any interruption to the production process is, therefore, avoided. The display is clear and easy-to-read and an extra auxiliary display can be simply plugged in and mounted wherever is most convenient for even greater improved visibility. The SmartKeys simplify balance operation and contribute to increased productivity. Just one press of a button and operators can immediately see if a container of parts falls within the expected weight range tolerance. Another button quickly counts the number of pieces in a container of known parts. This is the difference an intelligent balance makes. Text: Isabelle Senn, Product Manager Our new White Paper, Best Practices in Counting, contains useful information to help you achieve accurate and reliable counting processes, whatever your application. Counting Best Practices in Counting How to Achieve Accurate Counting Results When counting thousands of parts every day, accuracy is key. Mistakes can be costly and translate in overfilling costs, unstable production processes, waste and a damaged reputation. Piece counting with scales is a simple and fast way to determine numbers of parts in receiving, warehousing, production or shipping. However, counting accurately requires a thorough counting solution. This includes: An efficient counting process for your operators Adequate counting scales Operator training and A plan to maintain the operational reliability and accuracy of the scales. What influences counting accuracy? Parts counting can be influenced by a multitude of factors. However, among the main impacts are the: Parts weights and its deviation The accuracy of the counting scales (counting resolution) The environment Let s take a closer look on each of those factors. Contents 1 Parts weights and deviation 2 The right counting scale system 3 Counting resolution vs. internal resolution 4 Benefits of scale calibration 5 The environment 6 What does accuracy mean for you? 7 Good Weighing Practice for Counting Request your free copy: counting METTLER TOLEDO Machinery, Plastics, Electronics News 11 5

6 Titration Automating Iodine Adsorption of Carbon Black Carbon black is used as a pigment and reinforcement in rubber, plastic, inks and as an electrostatic discharging element. Being one of the smallest particles used in manufacturing, carbon black is difficult to analyse and handle. It has multiple uses in industry and strict quality control specifications. One of the quality control tests, iodine adsorption, just became easier and more accurate with a fully automated titration system. tion. The most common technique is defined by ASTM D1510. Although proven and reliable, this method requires multiple, exact volume aliquots and filtration making it a difficult process to automate until now. Installation diagram of T70 Excellence Titrator and Rondo20 for automated carbon black analysis. With over 8 million metric tons of carbon black produced per year for manufacturing additives, keeping up with testing demands can be laborious. Over 90% of the carbon black produced and used has a particle size ranging from nanometers making it difficult to handle and filter during analysis. In addition to particle size; conductivity, structure, color and surface area are also key characteristics of carbon black, determining in which application it is suitable. A number of techniques are available for the determination of surface area, including iodine adsorp- Simple chemistry The surface area of carbon black can be directly related to the amount of iodine adsorbed. The surface area can be deduced by adding an exact volume of a known concentration of iodine and reacting this with a sample of carbon black. Once added and allowed to react, the solution must settle and an exact volume taken. This is filtered and the remaining iodine in this aliquot is titrated with sodium thiosulfate. In addition to the exact volumes required for accurate iodine adsorption, exact stir speeds and reaction times must also be observed as an accurate titration end point and this may vary from operator to operator. 6 METTLER TOLEDO Machinery, Plastics, Electronics News 11

7 Volume Calibration Temperature Temperature Repeatability d(table vinegar) Repeatability Repeatability Calibration EQPdetermination Bias VEQ Calibration Repeatability Temperature Displacement TITER (NaOH) V(Table vinegar) M(CH 3COOH) R Know-How Measurement uncertainty determination made easy Do you want to know the confidence interval of your titration results? Would you like to optimize your application? Do you need to meet ISO17025 accreditation? Our new MuPac service simplifies the calculation and documentation of your titrator s measurement uncertainty. Find out more information. Automation benefits The T70 Excellence Titrator can completely automate this error prone and tedious analysis. An accurate dosing drive and burette automatically add 50 ml of 0.1 M iodine to ensure repeatable dosing for both blanks and samples. After this iodine addition, the solution is stirred for a set time with an overhead, compact propeller stirrer. Once mixed, the solution settles and the TV6 sampling valve is used to draw an exact and repeatable volume for every sample and blank into the sample loop tube. The sample solution is filtered through a 5 µm filter on its way to the TV6. Pumped with deionized water, the sample is transferred to the titration beaker. The sample solution is then titrated with 0.1 M sodium thiosulfate detected by the DMi140-SC platinum ring redox electrode. The analysis can be further automated with the addition of a Rondo sam- ple changer allowing automated analyses of up to 30 samples with just One Click. After each analysis, the filter is backwashed into the sample reservoir by a powerful diaphragm pump and another TV6 is used to change line paths. Each filter has a lifespan of approximately 100 samples. The titration beaker and sampling valve are thoroughly flushed and rinsed to ensure that all components and lines are clean and ready for the next sample. Utilizing burettes for iodine and titrant addition, available inline filters and accurate sample aliquots with the TV6; a proven and simple analysis for carbon black iodine adsorption can be completely automated for accurate, repeatable, and efficient analysis. Text: Matthew Eby, Production Manager Titration Good Titration Practice MuPac Assess your Titration Application with Measurement Uncertainty Calculation Prove result reliability Many important decisions are based on the results of chemical analyses. It is therefore crucial to document the quality of the analytical results by providing a quantitative value for their trustworthiness and reliability. GTP MuPac is based on a widely accepted tool for this purpose: the measurement uncertainty. Ensure comparable results Based on a method that is ideally validated, GTP MuPac yields a confidence interval of the respective titration result. This ensures and enables comparsion of results that are achieved elsewhere with the same method and therefore ensure quality in different production or testing locations. Comply to regulations Laboratories that want to become or already are accredited according to ISO/ IEC/EN (2005) must know how to calculate the measurement uncertainty. They must also have documented proof. GTP MuPac supports all relevant aspects to comply to these requirements. Optimize your SOP Measurement uncertainty calculations performed with GTP MuPac yields a comprehensive quantitative assessment of all factors that influence your titration results. Based on the results, individual parameters can be precisely fine tuned and your standard operating procedure optimized. GTP MuPac: Measurement Uncertainty for daily Good Titration Practice Strictly speaking, the result of a chemical analysis is meaningless without an indication of the uncertainty involved in its measurement. In order to achieve analytical quality in the laboratory it is crucial to quantify the uncertainty. The Measurement Uncertainty Pac (MuPac), a Good Titration Practice (GTP) service of METTLER TOLEDO, delivers the measurement uncertainty of your titration application efficiently and securely. The calculation uses your application data and is performed remotely with a validated software. The results are included in a comprehensive report that you receive within one week. GTP MuPac can be applied to all known volumetric titration applications independent of the instrument used. With the GTP MuPac service you gain confidence to correctly assess and rely on your titration results. The provided documentation takes the worry out of future quality audits. METTLER TOLEDO Machinery, Plastics, Electronics News 11 7

8 LabX Laboratory Software LabX Software Power the Bench LabX software brings power to your laboratory bench by providing full user guidance on the instrument touchscreen, handling all data auto matically, and ensuring a high level of process security. LabX is installed on a PC inside or outside your laboratory and can be connected to a variety of instruments, such as density meters, refractometers, melting point instruments, and Excellence Balances. LabX allows you to centrally manage your application methods, instruments, products and user rights. Individual process applications are implemented in LabX and provide full SOP workflow coverage directly on the instrument. With a variety of licensing options, LabX adapts to your needs. LabX Services support you and your LabX system and are completely flexible to meet individual system and user needs, including full integration with your existing information systems. In the Office In the Lab On the Instrument All data and process information is centrally managed in LabX. At any time, LabX can provide a complete overview of the activities in the lab. Manage your SOPs, users and instruments, and even view results as they are generated. Operators work at their instruments as usual. Tasks are started directly on the instrument touchscreen. All data and calculations are taken care of by LabX. The operator just has to perform the task. Reports can be generated automatically and sent to a printer inside the lab or in the office. LabX provides full step-by-step SOP user guidance directly on the instrument touchscreen. All data is handled automatically so manual transcription of results is no longer necessary. Results and instrument data are available directly on the touchscreen. 8 METTLER TOLEDO Machinery, Plastics, Electronics News 11

9 On the PC Use the design tools to create application methods and reports in accordance with your SOPs. Instrument tasks can be generated from the PC, ELN, LIMS or ERP. Secure results and electronic signatures assist in compliance with regulations, including 21 CFR Part 11. Precision Balance Analytical Balance Quantos Dosing System Refractometer Melting Point Instrument Titrator Density Meter To order our LabX brochure or for more information: METTLER TOLEDO Machinery, Plastics, Electronics News 11 9

10 Product HIghlight Simple and Flexible Solution for Dynamic Mechanical Analysis Dynamic Mechanical Analysis (DMA) is the method used to measure the mechanical and viscoelastic properties of materials as a function of temperature, time and frequency when subjected to periodic stress under a defined environment. The analyzed materials encompass thermoplasts, thermosets, composites, elastomers, ceramics and metals. In addition to operation in DMA mode, the DMA 1 permits measurements in TMA mode and under various environments. Controlled humidity experiments The humidity generator and humidity chamber allow samples to be analyzed under varying relative humidity conditions at a given temperature. Immersion measurements The fluid bath option permits the user to perform immersion studies on a sample. All DMA modes are supported by the immersion option. TMA experiments In addition to the established DMA modes, the DMA 1 permits operations to be performed under constant force (TMA or creep), in stress-strain or stress relaxation mode METTLER TOLEDO Machinery, Plastics, Electronics News 11

11 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 Machinery, Plastics, Electronics News 11 11

12 Info Spot 20 Thermal Analysis of Polymers Selected Applications This handbook shows how thermal analysis techniques can be used to analyze polymers and in particular to study the behavior of thermoplastics, thermosets and elastomers. Explanations and descriptions are based on samples from daily practices using the four important thermal analysis techniques: DSC, TGA, TMA and DMA. Register to get access to the Thermal Analysis of Polymers guide. Mettler-Toledo AG Laboratory Division Im Langacher CH-8606 Greifensee, Switzerland For more information