MILESTONE

T HE NEW MIL E STO NE

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

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.

1879Soxhlet ExtractionSamples submitted for organic analysis can rarely be used in their raw state; they require pre-

treatment. 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.

19 8 4

2 0 0 6

Microwave ExtractionThe use of microwave energy to accelerate solvent extraction procedures was first described by Ganzler et al. in 1984. These

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.

Dr. Soxhlet

Soxhlet

Ganzler

ETHOS EX

Extraction

Benefitsof the

Microwave-Assisted Solvent

The use of laboratory microwave ovens for organic extraction elevates sample preparation to the same level of sophistication

as sample analysis. Milestone's ETHOS EX extraction labstation is a high-performance microwave-accelerated system with some

of the most advanced process control and safety features currently available. The ETHOS EX system was created to give analysts

an extraction platform just as technologically advanced as GC, GC-MS, HPLC, and other analytical techniques.

SpeedMilestone's ETHOS EX labstation can simultaneously process multiple samples in a matter of minutes.Microwave assisted extraction uses closed vessels to heat the extraction solvent above its atmosphericboiling point. The elevated temperature increases the solubility of the analyte of interest and lowers theviscosity of the solvent, allowing it to better penetrate the matrix. Higher temperatures help overcome matrixeffects and accelerate the desorption and diffusion of the analyte molecules. This all leads to dramaticallyreduced extraction times.

EconomyMicrowave extractions are carried out in closed, sealed vessels. The matrix is constantly bathed with hotsolvent 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 lesssolvent, without sacrificing accuracy or precision. The simplicity of the microwave technique, along with theability to process multiple samples simultaneously, reduces the attended labor time and increases overallproductivity.

SimplicityAn important feature of the ETHOS EX 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.

Effectiveness and ConsistencyThanks to a combination of higher extraction temperatures, closed vessels, magnetic stirring, and preciselycontrollable temperature conditions, users of microwave extraction can expect a better quality of data. Thehomogeneity of the microwave field and the precision of the temperature control are key elements inmicrowave extraction. The ETHOS EX labstation contains a unique microwave diffusion system to ensureuniform heating of all samples. The heating is controlled using a PID algorithm and a graphical interface thatallows heating profiles to be set similar to GC or GC/MS instrumentation.

MicrowaveExtraction System

SimplicitySpeed Economy

Effectiveness and Consistency

Advanced Microwave Hardware

Higher microwave power provides fast vessel heatingThe ETHOS EX is equipped with an industrial magnetron. Delivered power is 1.200 watts, allowing rapid heating of high-throughput rotors.

Homogeneous microwave distribution throughout the cavityA microwave diffuser located above the microwave cavity evenly distributes microwaves throughout thecavity, preventing localized hot and cold spots.

All stainless-steel constructionThe chassis of the ETHOS EX is made of corrosion-resistant stainless steel, not molded plastic. The cavity and the door are plasma-coated with PTFE to protect the unit. Milestones warranty covers thecavity coating against corrosion for 5 years!

Convenient, user-centric designThe ETHOS EX door includes a shock resistant double-glass window, for easy viewing of the pressurevessels. The door opens downward and it can be used by the chemist as working platform to facilitate theloading of vessels into the microwave cavity.

Fast air cooling of vessels for higher throughputThe ETHOS EX 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 theexhaust fan to a fume hood, ensuring a safe working environment. Alternatively, the Milestone vessels canbe cooled in a water bath, further reducing the cooling time to less than 10 minutes.

Magnetic stirring in all vesselsThe ETHOS EX can be equipped with a pow e rful magnetic stirrer with variable speed, allowing thesimultaneous stirring of the solutions in all vessels. Efficient stirring guarantees that the sa m p l econtinuously remains in contact with fresh solvent and further enhances the microwave extraction process.

Industrial grade touch-screen controller. 6,5 screen with 65.000 colours VGA resolution 640x480 for sharp process gra p h i c s 1 USB port for printer, 2 PS2 ports for mouse and keyboard, 3 RS 232 ports for external devices Methods and runs are saved on a removable flash-ca r d

EasyCONTROL softwareMilestones new EasyCONTROLsoftware is the most advancedand powerful operating systemin the field of microwave samplepreparation. Automatic, real-timemonitoring and feedback-basedcontrol of multiple parametersoffer unsurpassed process

c o n t r o l . Simply recall a factory stored program or create a new one.Press Start, and the system will automatically follow the drawntemperature or pressure profile, utilizing a sophisticated PID algorithm.

Direct temperature controlThe ATC-FO Fiber-Optic AutomaticTemperature Control system allows fordirect continuous monitoring and controlof a reference vessel. The temperature sensor is housed in athermowell and protected from chemicalattack by a multiple layer of inert PTFE andceramic, ensuring trouble-free operation.

Contact-less temperaturecontrol in all vesselsThe ETHOS EX features a focused, high-sensitivity infrared sensor for contact-lesstemperature monitor and control of allvessels.

Direct pressure controlThe APC Automatic Pressure Controlsystem allows for direct monitoring andcontrol of a reference vessel. Pressure monitoring and control is ideal tomaintain pressure limits within the vesselsspecifications.

Contact-less pressure controlin all vesselsUnlike contact-less temperature controldevices, which focus on one vessel at atime, this sensor monitors vaporconcentration in the entire microw a r echamber, and effectively controls allvessels simultaneously, preventing anyleakage of organic solvents.

The ETHOS EX is equipped with the most advanced reaction sensors, including contact-less temperature and pressure control inall vessels, and direct temperature and pressure control in a single reference vessel.

Advanced Reaction Sensors

(1) Microwave program editing

(2) Actual temperatureprofile. The microwavepower is automaticallyadjusted, based oncontinuous feedback fromthe process sensors, to allowthe reaction to follow thedesired temperature profile.

Advanced User Interface

The ETHOS EX is operated via a compact terminal with bright, full-color, touch-screen display.The terminal runs the Milestones unique EasyCONTROL software, to provide simple, user-friendly controlof the microwave sample preparation process.

High temperature and pressure

Highest safety standards

Easy of use

Fast air coolingThe dome-shaped spring is temporarily flattened incase of overpressure, allowing the cap to lift upslightly and release the pressure. Once the pressurehas been released, the cap closes again, and themicrowave program can continue.

Burst disk venting.When a specific pressure is achieved, the diskbursts, and the pressure dramatically drops to zero. Sample is lost, and the program must be manuallystopped.

Milestone unique vent-and-reseal technology.Only the excess pressure is released from thevessel, and the digestion process can becompleted in full safety.

1 2 3

Vent-and-reseal vessels are thefoundation of Milestonesmicrowave digestion technology.Continuously enhanced, thispatented (US Patent 5,270,010)technology provides analysts withunsurpassed performancecapabilities.

Advanced Vessel Technology

Widest Choice of VesselsA 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 270 200 10SK-12 12 TFM 100 260 35PRO-16 16 TFM 75 200 30PRO-24 24 TFM 75 200 30MULTIPREP 42 PFA 65 180 15

SK-12SK-6LV PRO-16/PRO-24 MULTIPREP

Polymers Environment Pharmaceuticals Oils

ETHOS EX Major Applications

Effectiveness and Consistency

Post-Extraction Solvent EvaporationWith Milestones patented vacuum evaporation technology, the ETHOS EXturns into a true microwave evaporator, allowing the user to carry out safeand complete evaporation of organic solvents. No sample transfer needed,as the evaporation takes place in the same vessels previously used ford i g e s t i o n / extraction. A complete solvent recovery is ensured by theMilestones VAC-2000 vacuum module.

The ETHOS EX Labstation

Dioxins and Furans from Fly AshMicrowave extraction time: 15 minutes. Solvent: toluene.

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 ElectronicEquipment) directives.

Time required Soxhlet Time required ETHOS EXAdditives from Polymers 3 to 16 hours 20 minutes 140 CFat from Meat 16 hours 25 minutes 100 CImpurities in Food Dye 20 hours 1 hours 85 C

EPA 3540 (Soxhlet) ETHOS EXTime required Solvent consumed Time required Solvent consumed13.167 hours 450 L 257 hours 16 L

Comparison study for processing 1.000 samples.

Less Solvent, Shorter TimePAHs andPesticides in Soil samples

Method/Sample Phenol Resin ABS Resin PETETHOS EX 31.000 2.200 480Soxhlet 28.000 2.200 460

Total results. All concentrations in ppm. Microwave extraction time: 30 minutes. Solvent: toluene.

H. M. Kingston et al., Microwave Assisted Organic Extraction and Evaporation: an Integrated Approach. LCGC, Vol. 20, 2002.

Milestone application notes.

Milestone application notes.

ETHOS EXTechnical

SpecificationsMicrowave hardware

Single magnetron system with rotating diffuser for homogeneous microwave distribution in the cavity.

Magnetron protected from reflected microwave power. Installed power 1.200 watts. Output power up to 1.200 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 350C.

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.

MILESTONE srlVia Fatebenefratelli, 1/524010 Sorisole (BG) - ItalyTel: +39 035 573857 - Fax: +39 035 575498E-mail: analytical@milestonesrl.comwww.milestonesrl.com

UNI EN ISO 9001: 2000 CERT I F I E D

Control terminal

Touch-screen industrial grade controller 6,5 screen with 65.000 colours.

VGA resolution 640x480 for sharp process graphic. 1 USB port for 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 (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, D4309-96.

International Regulations ComplianceSuitable for RoHS (Restriction of the use of certain HazardousSubstances in electrical and electronic equipment), WEEE (WasteElectrical and Electronic Equipment) and ELV (End-of-Life vehicles)sample preparation.

Specifications are subject to change without notice.

MILESTONE INC.25 Controls Drive - Shelton, CT 06484 - USATel: (203) 925-4240 - Toll-free: (866) 995-100Fax: (203) 925-4241E-mail: mwave@milestonesci.comwww.milestonesci.com