M I C R O W A V E O P E N V E S S E L D I G E S T I O N S Y S T E M T HE NEW MIL E STO NE MILESTONE
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1 M I C R O W A V E O P E N V E S S E L D I G E S T I O N S Y S T E M T HE NEW MIL E STO NE MILESTONE
2 WHY THE START MOD The need for larger sample sizes Acid digestion of organic samples produces gaseous by-products, such as CO 2 and NO X. As a result, larger sample sizes produce higher pressures inside a closed digestion vessel. Furthermore, a larger sample size may lead to more exothermic and uncontrollable reactions. Generally, in a 100 ml pressure vessel, no more than 1 gram of dry organic sample can be digested. Larger organic sample sizes produce higher pressure and more exothermic reactions inside a closed digestion vessel. Larger samples, on the order of several grams, are desirable in a variety of applications, to serve as a more representative portion of a larger sample bulk, or to compensate for limitations in the sensitivity of the analytical instrument. This is particularly true in applications such as plastics and polymers, waste products, food and feed, and a variety of other highly reactive compounds. Food, feed, electronic waste, polymers sand environmental samples typically require large mass to be digested The answer for larger sample size Milestone s innovative START MOD system allows rapid digestion of 8 organic samples with dry weight up to several grams each. The unique advantage of the START MOD is that it can also be utilized as a closed-vessel digestion system, by adding any Milestone closed-vessel rotor, giving chemists the greatest flexibility within a single sample preparation platform. The built-in software allows the user to perform both open and closed-vessel procedures.
3 HOW THE START MOD WORKS START MOD ADVAN The START MOD (Microwave Open Digestion) system consists of a microwave unit with an MOD-8 rotor, for processing up to eight samples simultaneously, a VAC acid scrubber module, and a fully automated acid dosing system. The microwave unit is equipped with contact-less infrared temperature control in all vessels for consistent and reproducible results. Operation is very simple: place the samples to be digested into the 250 ml glass or quartz vessels of the rotor. Then select the appropriate method for easy, medium, or difficult samples or customize the timeat-temperature profile and dosing parameters to create your own program, which can be stored for repeated use. Press Start, and the system will automatically carry out the program, monitoring and controlling the temperature in each vessel, and continuously adjusting the microwave power output to match the desired temperature profile. The fully automated dosing system will deliver precise amounts of as many as three different reagents at specified intervals. As the digestion proceeds, the VAC-4000 acid scrubber module safely and efficiently exhausts and neutralizes the acid vapours produced. The START MOD is operated via a compact terminal with bright, full-color, touch-screen display. The terminal runs Milestone s unique E a s y CON TROL software, to provide simple, user-friendly control of the microwave sample preparation process. EasyCONTROL software Milestone s new EasyCONTROL software is the most advanced and pow e rf u l operating system in the field of m i c r owave sample preparation. Automatic, real-time monitoring and feedback-based control of multiple parameters offer unsurpassed process control. Simply recall a factory stored program or create a new one. Press Start, and the system will follow the drawn temperature or pressure profile, utilizing a sophisticated PID algorithm. (1) Microwave program editing (2) Actual temperature profile The microwave power is automatically adjusted, allowing the solution to follow the desired temperature profile. Fresh acid from an external dosing system is added at preset intervals.
4 CED USER INTERFACE THE UNIQUE MOD-8 ROTOR Industrial grade touch-screen controller. 6,5 screen with colours VGA resolution 640x480 for sharp process graphics 1 USB port to connect printer, 2 PS2 ports for mouse and keyboard, 3 RS 232 ports for external devices Methods and runs are saved on a removable flash-card Simultaneous digestion of up to 8 samples The MOD-8 rotor allows for the simultaneous open-vessel digestion of up to eight sa m p l e s, in 250 ml glass or quartz vessels. The entire rotor is composed of ultra-pure, chemically inert PTFE and PP polymers, to minimize contamination. The individual vessels are isolated, each with its own separately connected vacuum exhaust line, so there is no risk of cross contamination. Fu rthermore, each vessel is also individually connected to the automated dosing system, to ensure precise control over the distribution of acid to each sa m p l e. THE VAC-4000 High-efficiency acid scrubber module The VAC-4000 performs exhaust and neutralization of acid vapours during the digestion run. A vacuum sensor built in to the START MOD unit ensures that proper exhaust of vapours is carried out Water-cooled PTFE condenser (recovers up to 90% of the acid vapors). 2. PFA/PTFE collecting bottle. 3. Neutralizing solution Acid-resistant, all-ptfe vacuum pump. The flash card is removed from the START MOD terminal and introduced into a standard PCMCIA laptop slot for methods and runs storage, viewing and data transfer. MAXIMUM FLEXIBILITY The benefit of the EasyCONTROL software On-line control of all parameters Temperature driven microwave power Reaction is controlled at any temperature and not only once a set temperature is reached Better control of exothermic reactions Same digestion quality for different sample sizes One method only for any number of samples Full control of external dosing system Open and closedvessel digestion in a single microwave unit! The START system is the most flexible sa m p l e preparation platform available. Just by adding in-vessel temperature control and one of the pressure-capable rotors available from Milestone, it allows the chemist to perform both open and closed-vessel digestions in a single microwave unit. Closed-vessel digestion allows chemists to work at higher temperatures and pressures, completing digestions faster and minimizing acid volume and sample contamination.
5 A METHOD FOR ANY SAMPLE A few standard methods will digest larger masses or organics, according to their level of difficulty. In addition, the EasyCONTROL software allows the chemist to create customized methods. Sample Organic Environmental Inorganic <1 gram >1 gram <1 gram >1 gram Closed Closed Open Closed Open Easy Moderate Difficult Waste Juices, plants, cereals... Paper, biological, light oil... Oils, plastics, waste... Time 30 minutes Maximum temperature 120 C Reagents HNO 3 and H 2 O 2 Time 40 minutes Maximum temperature 200 C Reagents H 2 SO 4, HNO 3 and H 2 O 2 Time 60 minutes Maximum temperature 240 C Reagents H 2 SO 4, HNO 3 and H 2 O 2 START MOD, THE MICROWAVE KJELDHAL The comparison below refers to various agriculture products. MET H O D S TA RT MOD KJEL D H A L SA MPLE WEIGH T 7-9 grams 7-9 grams CATA LYST Not needed 7 g of (2,37 g CuSO 4 x 5H 2 O g Na 2 SO 4 ) REA GEN TS 16 ml H 2 SO 4 96% and 30 ml H 2 O 2 20 ml H 2 SO 4 96% and 8 ml H 2 O 2 30 % TEMPERATURE 235 C 390 C TOTAL TIME 1 hour and 15 minutes 4-5 hours Results for apple samples (all data in mg/100 g). MET H O D S TA RT MOD KJEL D H A L N 43,1 ± 1, 6 43,9 ± 1, 5 Ca 6, 01 ± 0,34 6,65 ± 0,67 M g 6,62 ± 0,30 6, 58 ± 0,53 P 10,2 ± 0,3 10,6 ± 0,7
6 Start MOD 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 4 micro-switches safety interlocks to prevent microwave emission with door open. Exhaust located in the side of the cavity, separate from electronics to prevent corrosion. Reaction sensors Contact-less temperature monitoring and control up to 300 C in all vessels. Vacuum control. Control terminal Industrial grade touch-screen controller. 6,5 screen with colours. VGA resolution 640 x 480 for sharp process graphics. 1 USB port to connect printer, 2 PS2 ports for mouse and keyboard, 3 RS 232 ports for external devices. Methods and runs saved on Windows -compatible removable flash-card. Weight ~ 75 kg. External dimensions 57 x 51 x 61 cm (h). Power 220V/50-60Hz, 2,4 kw. 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 UNI EN ISO 9001: 2000 CERT I F I E D 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
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