M I C R O W A V E E X T R A C T I O N S Y S T E M THE NEW MILESTONE MILESTONE

Transcription

1 M I C R O W A V E E X T R A C T I O N S Y S T E M THE NEW MILESTONE MILESTONE

2 Soxhlet Extraction Soxhlet 1879 Samples submitted for organic analysis can rarely be used in their raw state; they require pretreatment. The principal step in sample pre-treatment is extraction of the analytes of interest from the sample matrix. This is the least evolved (many people still use the Soxhlet method invented in 1879), most error-prone step in the analytical procedure. Dr. Soxhlet 1984 The use of microwave energy to accelerate solvent extraction procedures was first described by Ganzler et al. in These Microwave Extraction Ganzler reserchers used polar, microwave absorbing solvents or mixtures to extract crude fat from food and pesticides from soil matrices. Microwave extraction rates were found to be significantly faster, with recoveries comparable or superior to traditional Soxhlet extraction, and with a substantial reduction of the amount of solvent required. Benefits of the Microwave-Assisted Solvent Extraction 2009 START E The use of laboratory microwave ovens for organic extraction elevates sample preparation to the same level of sophistication as sample analysis. Milestone's START E extraction labstation is a high-performance microwave-accelerated system with some of the most advanced process control and safety features currently available. The START E system was created to give analysts an extraction platform just as technologically advanced as GC, GC-MS, HPLC, and other analytical techniques. Speed Microwave extractions can be completed within minutes; a fraction of the time, compared to older methods. Economy Lower solvent usage reduces the costs of solvent purchase and disposal. Effectiveness Microwave extraction produces higher analyte recoveries than older methods. Consistency Precise, software-based control of all reaction parameters ensures method reproducibility. Simplicity Use polar or non-polar solvents; no need to modify your existing chemistry.

3 Microwave Extraction System Speed Economy Effectiveness and Consistency Simplicity Speed Milestone's START E labstation can simultaneously process multiple samples in a matter of minutes. Microwave assisted extraction uses closed vessels to heat the extraction solvent above its atmospheric boiling point. The elevated temperature increases the solubility of the analyte of interest and lowers the viscosity of the solvent, allowing it to better penetrate the matrix. Higher temperatures help overcome matrix effects and accelerate the desorption and diffusion of the analyte molecules. This all leads to dramatically reduced extraction times. Economy Microwave extractions are carried out in closed, sealed vessels. The matrix is constantly bathed with hot solvent in a self-promoting reflux action with no loss of volatile analytes or solvent. The use of closed vessels, with the speed and efficiency of microwave heating, allows extractions to be performed with significantly less solvent, without sacrificing accuracy or precision. The simplicity of the microwave technique, along with the ability to process multiple samples simultaneously, reduces the attended labor time and increases overall productivity. Effectiveness and Consistency Thanks to a combination of higher extraction temperatures, closed vessels, magnetic stirring, and precisely controllable temperature conditions, users of microwave extraction can expect a better quality of data. The homogeneity of the microwave field and the precision of the temperature control are key elements in microwave extraction. The START E labstation contains a unique microwave diffusion system to ensure uniform heating of all samples. The heating is controlled using a PID algorithm and a graphical interface that allows heating profiles to be set similar to GC or GC/MS instrumentation. Simplicity An important feature of the START E system is that it easily adapts to existing extraction chemistry. This is accomplished through the use of a unique, patented material, called Weflon. Without Weflon, extractions could only be performed with polar solvents (Acetone, Methanol, etc.) or mixtures of polar and non-polar solvents, because non-polar solvents are not heated by microwaves. Weflon eliminates this problem by acting as a coupling agent. Weflon stir bars are heated by microwaves and they subsequently transfer this heat to the non-polar solvent. Each Weflon piece is precisely manufactured to contain the same amount of high-purity microwave absorbing material, ensuring reproducible heating conditions from vessel to vessel and run to run.

4 Advanced Microwave Hardware Higher microwave power provides fast vessel heating The START E is equipped with an industrial magnetron. Delivered power is watts, allowing rapid heating of high-throughput rotors. Homogeneous microwave distribution throughout the cavity A microwave diffuser located above the microwave cavity evenly distributes microwaves throughout the cavity, preventing localized hot and cold spots. All stainless-steel construction The chassis of the START E is made of corrosion-resistant stainless steel, not molded plastic. The cavity and the door are plasma-coated with PTFE to protect the unit. Milestone s warranty covers the cavity coating against corrosion for 5 years! Convenient, user-centric design The START E door includes a shock resistant double-glass window, for easy viewing of the pressure vessels. The door opens downward and it can be used by the chemist as working platform to facilitate the loading of vessels into the microwave cavity. Fast air cooling of vessels for higher throughput The START E is equipped with a heavy duty air flow system, placed above the microwave cavity. The air flow rapidly cools the external surfaces of the vessels. An acid-resistant flexible hose connects the exhaust fan to a fume hood, ensuring a safe working environment. Alternatively, the Milestone vessels can be cooled in a water bath, further reducing the cooling time to less than 10 minutes. Magnetic stirring in all vessels The START E can be equipped with a powerful magnetic stirrer with variable speed, allowing the simultaneous stirring of the solutions in all vessels. Efficient stirring guarantees that the sample continuously remains in contact with fresh solvent and further enhances the microwave extraction process.

5 State of the Art User Interface Monochrome industrial grade touch-screen controller with 5 screen Resolution 240 x 128 dots for sharp process graphic 1 PS2 port for mouse, 1 RS 485 port for microwave unit, and 1RS 232 port for external devices Methods and process reporting data saved on internal memory EasyCONTROL software Milestone s new EasyCONTROL software is the most advanced and powerful operating system in the field of microwave sample preparation. Automatic, realtime monitoring and feedbackbased control of multiple parameters offers unsurpassed process control. Simply recall a factory stored program or create a new one. Press Start, and the system will automatically follow the defined temperature or pressure profile, utilizing a sophisticated PID algorithm. Microwave program editing. Actual temperature profile. The microwave power is automatically adjusted based on continuous feedback, allowing the reaction to follow the desired temperature profile. Advanced Reaction Sensors The START E is equipped with the most advanced reaction sensors, including contact-less temperature and pressure control in all vessels, and direct temperature and pressure control in a single reference vessel. Direct temperature control The ATC-FO Fiber-Optic Automatic Temperature Control system allows for direct continuous monitoring and control of a reference vessel. The temperature sensor is housed in a thermowell and protected from chemical attack by a multiple layer of inert PTFE and ceramic, ensuring trouble-free operation. Contact-less temperature control in all vessels The START E features a focused, highsensitivity infrared sensor for contact-less temperature monitor and control of all vessels. Direct pressure control The APC Automatic Pressure Control system allows for direct monitoring and control of a reference vessel. Pressure monitoring and control is ideal to maintain pressure limits within the vessel s specifications. Contact-less pressure control in all vessels Unlike contact-less temperature control devices, which focus on one vessel at a time, this sensor monitors vapor concentration in the entire microware chamber, and effectively controls all vessels simultaneously, preventing any leakage of organic solvents.

6 Advanced Vessel Technology High temperature and pressure Highest safety standards Easy of use Fast air cooling Vent-and-reseal vessels are the foundation of Milestone s microwave digestion technology. Continuously enhanced, this patented (US Patent 5,270,010) technology provides analysts with unsurpassed performance capabilities The dome-shaped spring is temporarily flattened in case of overpressure, allowing the cap to lift up slightly and release the pressure. Once the pressure has been released, the cap closes again, and the microwave program can continue. Burst disk venting. When a specific pressure is achieved, the disk bursts, and the pressure dramatically drops to zero. Sample is lost, and the program must be manually stopped. Milestone unique vent-and-reseal technology. Only the excess pressure is released from the vessel, and the digestion process can be completed in full safety. Widest Choice of Vessels A wide choice of vessels are available from Milestone, to accommodate all sample preparation requirements. Rotor Nr. Vessel Vessel Max. Max. type of vessels material volume (ml) temperature ( C) pressure (bar) SK-6LV 6 TFM SK TFM PRO TFM PRO TFM MULTIPREP 42 PFA SK-6LV SK-12 PRO-16/PRO-24 MULTIPREP

7 Start E Major Applications Polymers Environment Pharmaceuticals Oils PAHs and Pesticides in Soil samples Less Solvent, Shorter Time EPA 3540 (Soxhlet) START E Time required Solvent consumed Time required Solvent consumed hours 450 L 257 hours 16 L Comparison study for processing samples. H. M. Kingston et al., Microwave Assisted Organic Extraction and Evaporation: an Integrated Approach. LCGC, Vol. 20, Time required Soxhlet Time required START E Additives from Polymers 3 to 16 hours 20 minutes 140 C Fat from Meat 16 hours 25 minutes 100 C Impurities in Food Dye 20 hours 1 hours 85 C Milestone application notes. Effectiveness and Consistency Polybrominated Diphenyl Ethers (PBDEs) from various polymer samples. RoHS (Restriction of the use of certain Hazardous Substances in electrical and electronic equipment) and WEEE (Waste Electrical and Electronic Equipment) directives. Method/Sample Phenol Resin ABS Resin PET Start E Soxhlet Total results. All concentrations in ppm. Microwave extraction time: 30 minutes. Solvent: toluene. Milestone application notes. Dioxins and Furans from Fly Ash Microwave extraction time: 15 minutes. Solvent: toluene. The Start E Labstation Post-Extraction Solvent Evaporation With Milestone s patented vacuum evaporation technology, the START E turns into a true microwave evaporator, allowing the user to carry out safe and complete evaporation of organic solvents. No sample transfer needed, as the evaporation takes place in the same vessels previously used for digestion/extraction. A complete solvent recovery is ensured by the Milestone s VAC-2000 vacuum module.

8 Start E Technical Specifications Microwave hardware Single magnetron system with rotating diffuser for homogeneous microwave distribution in the cavity. Magnetron protected from reflected microwave power. Installed power watts. Output power up to watts, controlled via microprocessor. Large microwave cavity 37 x 34,5 x 33,5 (h) cm. Cavity illumination. Microwave cavity entirely made of 18/8 stainless steel housing with innovative multi-layer PTFE plasma coating applied at over 350 C. All hardware protected against acids/organic solvents with polymer coating both on inside and outside surfaces. Total of safety interlocks 4 micro-switches to prevent microwave emission with door open. Exhaust located in the side of the cavity, separate from electronics to prevent corrosion. Reaction sensors Direct temperature monitoring and control in a reference vessel. Contact-less temperature monitoring and control in all vessels. Direct pressure monitoring and control in a reference vessel. Contact-less pressure monitor and control up to the vessels highest working pressure. Control terminal Monochrome touch-screen industrial grade controller 5 screen. Resolution 240 x 128 dots for sharp process graphic. 1 PS2 port for mouse, 1 RS 484 port for microwave unit, and 1 RS 232 port for external devices. Methods and process reporting data saved on internal memory. Weight ~ 75 kg. External dimensions 57 x 51 x 61 (h) cm. Power 220V/50-60Hz, 2,4 kw. Standard Methods Compliance U.S. EPA Methods: 3546, 3052, 3051a, 3015a. ASTM (American Society of Testing and Materials) Methods: D-5765, D-6010, D International Regulations Compliance Suitable for RoHS (Restriction of the use of certain Hazardous Substances in electrical and electronic equipment), WEEE (Waste Electrical and Electronic Equipment) and ELV (End-of-Life vehicles) sample preparation. Specifications are subject to change without notice. MILESTONE srl Via Fatebenefratelli, 1/ Sorisole (BG) - Italy Tel: Fax: analytical@milestonesrl.com MILESTONE INC. 25 Controls Drive - Shelton, CT USA Tel: (203) Toll-free: (866) Fax: (203) mwave@milestonesci.com Start E/01/2009 UNI EN ISO 9001: 2000 CERTIFIED MLS GmbH Auenweg 37 - D Leutkirch im Allgau - Germany Tel: +49 (0) Fax: +49 (0) mws@mls-mikrowellen.de MILESTONE GENERAL K.K. KSP, 3-2-1, Sakado - Takatsu-Ku, Kawasaki Japan Tel: +81 (0) Fax: +81 (0) info@milestone-general.com