friction. Due to this, the dropping point is determined for fresh- or used greases and is often carried out following the IP396 standard.

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1 Petrochemicals Weighing Analytical and solutions Analysis in the Laboratory laboratory 15 News Edition No. 1 / February 2013 Identification and Performance Limits of Lubrication Grease Dropping point is the temperature, in degrees Celsius ( C), at which a small amount of grease develops into a long drop under defined test conditions. This thermal value is used to indicate thickener type and the cohesiveness of the oil and thickener of grease. Together with results of other types of analyses, it also determines the suitability of greases for specific applications. Moving machinery parts have to be lubricated in order to protect them from premature wear and tear. If a continuous supply of lube points cannot be achieved, or only achieved with great technical efforts, lubrication grease is used. These lubricating greases consist of base oils, most commonly mineral or synthetic oils and additives, both of which are hindered from clear out by a sponge like thickener. So called metal soaps are composed of powdery raw materials, such as lithium, calcium, sodium and aluminum, or combinations of these, which are used as thickeners. When using lubrication greases, it is important that the grease does not drop away at elevated temperatures caused by friction. Due to this, the dropping point is determined for fresh- or used greases and is often carried out following the IP396 standard. Method A sample is placed into a cup with a defined orifice. This cup is then placed in a thermostatically controlled aluminum block furnace. The temperature is increased at a constant rate until a drop of grease falls to the bottom. When this happens, the temperature is recorded as the dropping point. The fully automated METTLER TOLEDO DP70 Excellence Dropping Point System determines the dropping point and delivers standard compliant results. A camera records the live image to video. The drop-

2 Dropping Point Determination Only One Click is needed to start a pre-programmed measurement. ping point is detected and evaluated as soon as the drop falls from the cup from the live image. The results can be documented via a connected roll printer, network printer or in a PDF protocol, which can then be directly transferred to a computer. Up to two dropping points can be determined simultaneously. Consequences for the material The maximum allowable usage temperature is often substantially below the determined dropping point, often more than 50 C below. The detection of a lower used Visual camera observation and digital image analysis guarantee that the determinations are reliable. grease dropping point, in comparison to that of fresh grease, can be the result of different factors: Mixing with grease that contains another thickener has taken place. Mixing different greases always results in a softer consistency. It can become partly lumped or soup-like but never more solid. The fat was stressed so much that the soap structure, i.e. the sponge container, was sheared into so many small particles that it is no longer capable of holding the oil. The grease present has to be removed in any case. This can be completed by wash out or increased greasing. Conclusion Using a DP70 Excellence Dropping Point System offers a simple and efficient way of determining the temperature limits of lubricating greases, which are result compliant to common international regulations. One Click shortcuts start entire measurement processes with the simple touch of a button. 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 02/13 Printed in Switzerland. 2 METTLER TOLEDO Petrochemicals News 15

3 Know how Efficient and Trouble Free Determination of Bitumen Density Density measurement of petroleum products which are solid at room temperature, such as low boiling bitumen, is cumbersome. METTLER TOLEDO offers a solution for the trouble-free and secure measurement of such samples. Watch how One Click Density and Refractive Index in the Petrochemical industry works Demanding process environment and high throughput operation, petrochemical workplaces require tough and reliable instruments. Operators may deal with dangerous chemicals and require protection. LiquiPhysics takes care of all of these demands and much more besides. Bitumen mainly consists of high molecular hydrocarbons making it highly viscous or solid at an ambient temperature and remaining extremely viscous even after heating. The density or related units, such as API gravity degrees or the specific gravity, need to be determined for quality control requirements. METTLER TOLEDO has the solution for greatly simplifying this measurement: The powerful and reliable SC1H and SC30H heated automation units are designed to keep samples at elevated temperatures of up to 80 C and completely automate the measurement of all required parameters. Convenient health protection and increased efficiency When taking measurements from petroleum products, hexane and toluene are effective cleaning agents, but prolonged exposure to them can be harmful. The automated measuring systems protect operators from direct contact with toxic solvents or vapors. Moreover, there is no need to remove protective gloves as the measurement can be started without touching anything. Moving a hand over the ErgoSens, an infrared sensor for hands-free operation, is all that s needed. After the density determination, the required measurement units are calculated while the entire system is cleaned thoroughly without any operator interaction. The toxic and smelly waste is collected in a separate container, which can be equipped with the optional LevelSens Level Sensor to eliminate the risk of overfilling. Automatic error detection securely excludes the presence of bubbles, which are impossible to see in such pitch-black samples, therefore ensuring that the results obtained are consistently reliable. Text: D. Buchmann, Product Manager Density & Refractometry liquiphysics-petrochem METTLER TOLEDO Petrochemicals News 15 3

4 Anti-Static Kit effectively removes electrostatic charge from filters. Filter Weighing Determining Fuel Contamination with Accurate Filter Weighing It takes good quality fuels and lubricants to keep the world in motion. The EN norm is one of many oil-refining standards and applies to contamination determination in middle distillates, such as kerosene, diesel and jet aviation fuel. The contaminants are collected via vacuum filtering and METTLER TOLEDO Balances are ideal for determining the level of particulate matter on the filters in accordance with the norm. The principle of the EN 12662:2008 standard states that, A sample portion of 800ml ± 25 ml is weighed and filtered under vacuum through a pre-weighed filter. The filter with the residue is washed, dried and weighed. Contamination is determined from the calculated difference in filter mass and expressed relative to the sample mass as mg/kg. The norm specifies two balances: a top load balance, capable of weighing 1,500 g to the nearest 0.1 g, and an analytical balance, capable of weighing to the nearest 0.1 mg. Precision balance for sample weighing The first weighing step in the process involves weighing an 800 ml fluid sample in a 1 liter beaker on a balance with a readability of 0.1 g and a weighing capacity of minimum 1,500 g. METTLER TOLEDO s NewClassic M32001S/01 Precision Balance is perfectly suited to this task. The balance has a full metal housing with an International Protection Rating of 54 (IP54 In-Use). This offers the highest level of protection against hazardous and 4 METTLER TOLEDO Petrochemicals News 15

5 Know how toxic samples. This robust and easy-to-use balance offers enough capacity (32 kg) to fulfil the demands of many other tasks in the laboratory. Analytical balance for filter weighing A glass fibre filter with a 0.7 µm pore size is weighed on an analytical balance before the sample is vacuum filtered. After washing, drying and cooling, the filter is weighed again by placing it directly on the analytical balance. METTLER TOLEDO s Excellence Plus XP105 DeltaRange Balance offers high accuracy for the best weighing results. The Swiss-made Delta Range Balance offers a fine measurement range of 0-81 g with a readability of 0.01mg and a maximum capacity of 120g. The filters can be positioned perfectly on the SmartGrid Hanging Weighing Pan. The grid design minimizes air turbulence in the weighing chamber guaranteeing fast results and easy filter handling with tweezers. Passing the filters through an Anti-Static Kit before weighing removes electrostatic charge and eliminates its influence from the weighing result. The glass draft-shield can be dismantled by hand in seconds and all parts are dishwasher safe for the perfect easy-cleaning solution. The built-in filter weighing application also offers a secure error-free process with full traceability. Contamination is determined from the difference in filter weight before and after filtering and is expressed as a fraction of the original sample in mg/kg. The builtin application on the XP105 Delta Range Balance performs this calculation automatically. Meeting quality demands The EN norm is just one of many standards used in quality control during the oil refining process. Products, including kerosene, diesel and jet aviation fuel must remain at a consistent quality and free from contaminants, such as soot and sulphur etc.. METTLER TOLEDO has a wide balance portfolio to completely support these demanding quality control procedures. Text: Daniel W. Fuchs, Head of campaigns & MarCom Learn the proper way to determine particulate matter on filters Our expert on filter weighing solutions explains in detail how to determine particulate matter on filters accurately and reliably using manual or automatic balances. He reveals best practice techniques, e.g. to minimize external influences on the weighing result, and provides valuable background information on how to successfully manage challenging weighing processes. Sign up and join the webinar: webinar-filterweighing Filters cooling in desiccators. The vacuum filtering apparatus. XP105 Delta Range Balance XP105 Delta Range Balance METTLER TOLEDO Petrochemicals News 15 5

6 Tips & Tricks Titration Increased Refinery Efficiency with One Click Excellence Titration The Valero Houston Refinery is moderately sized compared to most refineries. Being small demands excellent efficiency. Optimizing rich amine loading analysis with a T90 Excellence Titrator greatly improves efficiency. Simple Daily Laboratory Work with One Click See what One Click can do for your laboratory. Potentiometric and Karl Fischer titrators, density and refractive index meters as well as dropping point and melting point instruments all designed with operator safety and ease of use in mind from METTLER TOLEDO. Watch the video: one-click-titration T90 and T70 titrators at Valero Houston Refinery used for multiparameter testing of CO2 loading as well as mercaptan and TAN analysis of their finished products. Refineries use rich amine loading as an indicator of their scrubber s ability to effectively remove H2S (hydrogen sulfide) and reduce unit corrosion in order to ensure quality and meet regulations. This analysis typically involves testing for H2S content, amine strength and acidity on three different samples. This leaves room for operator errors, as well as transcription and calculation errors, in the complex formula integrating results. When the mixture indicates that the rich amine load is high, additional steam must be used to regenerate these amines to effectively remove the H2S and CO2 from products. Ultimately, a small error can result in a tremendous amount of unnecessary energy spent on steam generation. T90 Excellence pays off Consulting their local METTLER TOLEDO Titration Sales Representative was a smart investment for Valero. Utilizing the T90 s flexible and powerful methods, the three determinations to comprise the CO2 loading can be analyzed using just one sample, as opposed to three, with an accurately calculated final result. Using the T90 s One Click interface to combine all these tests has resulted in an initial investment return of less than 6 months on labor costs alone. With the increased throughput of analysis and accuracy, the frequency and amount of steam used for regeneration can be more tightly controlled resulting in major annual energy savings. By making a commitment to optimize their rich amine loading analysis with a T90 Excellence Titrator, the Valero Houston Refinery has increased its refinery efficiency saving time, energy and money. Text: Matthew Eby, Product manager, Titration 6 METTLER TOLEDO Petrochemicals News 15

7 Ensuring Asphalt and Pitch Quality with Softening Point Analysis Asphalt and pitch are frequently used in demanding environmental conditions. The suitable material characteristics are determined by the softening point of fine-tuned binder mixtures that require careful quality control. The DP70 Excellence Dropping Point System offers a time- and cost saving way of determining the softening point temperature of asphalt and pitch. DP70 Excellence Dropping Point System The softening point temperature of asphalt and pitch is usually measured according to ASTM D3104 and ASTM D3461 standards. These standards control the conditions of the temperature induced softening of brittle or pasty asphalt and pitch samples into less viscous liquids. These standards are recognized as the best methods for quality control. Automatic dropping point instrument The DP70 Excellence Dropping Point system fully automizes the determination based on standardized sample cups and well-approved test methods. The measurement methods are clearly structured to an exact replication of standard procedure. The unique video based detection algorithm yields operator independent endpoint detection with unsurpassed accuracy and repeatability. The analytical process can be recorded and stored for post visual inspection and documentation. Simple, fast and cost-efficient The DP70 features METTLER TOLEDO's One Click operation philosophy, meaning that all tasks can be started with one touch of the users touch-screen making instrument operation very simple and efficient. Samples are quickly and reliably prepared with the smart tools provided in the sample preparation box and mounted in the innovative sample holder. Two measurements can then be performed simultaneously to improve efficiency and result quality. Cumbersome cleaning with dangerous solvents and oven contamination are a thing of the past thanks to disposable aluminum sample cups and glass sample collectors. Results and video captions can be printed as PDF files or stored on a connected network drive. The DP70 reliably assists in the selection of binder mixtures for high quality asphalt and pitch products. Text: Hans-Joachim Muhr, Marketing Manager, Excellence Thermal Values METTLER TOLEDO Petrochemicals News 15 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 Petrochemicals News 15

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 Petrochemicals News 15 9

10 Product Highlight Boost Productivity with Efficient Moisture Control The HS153 is the instrument of choice where fast and accurate determination of moisture content is critical for productivity. The unique graphical user interface and personalized method shortcuts make it fast and intuitive to use even in fast-paced workplaces. The new design means the instrument can be thoroughly cleaned in just 30 seconds to save time and provide a further boost to productivity even in challenging petrochemical environments. 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 Petrochemicals News 15

11 Understand and Control Process Chemistry Better Challenged by space constraints and/or complex installation requirements? ReactIR 247 is a unique process-hardened FTIR spectrometer designed to fit into nearly any space without sacrificing the proven performance of ReactIR technology. The design of the ReactIR 247 yields an analyzer with high stability and sensitivity in a product format that delivers extreme space savings with plug-in and measure operation. Turn-Key Integrating the Sentinel probe technology to a flow cell permits easy integration into existing flow stream and immediate analysis of the reaction as it occurs. From Lab to Plant Specifically designed for the production environment, ic Process enables the transfer of critical control parameters determined in the lab. Flexibility Flexible sampling arrangements allow for the use of longer probes to reach the fill level for small volume starting conditions. METTLER TOLEDO Petrochemicals News 15 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