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

T HE NEW MIL E STO NE

MILESTONE

Soxhlet Extraction

1879

Soxhlet

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

Ganzler
Microwave Extraction

The 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.

Benefits
of the
Microwave-Assisted
Solvent

2006

ETHOS EX

Extraction

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.

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.

Microwave
Extraction System

Speed Economy
Simplicity
Effectiveness and
Consistency

Speed
Milestone'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 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.

Simplicity
An 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 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 ETHOS EX 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.

Advanced Microwave Hardware

Higher microwave power provides fast vessel heating

The 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 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 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 the
cavity coating against corrosion for 5 years!

Convenient, user-centric design

The ETHOS EX 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 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 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 ETHOS EX 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.

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 control
of the microwave sample preparation process.
EasyCONTROL software

(1) Microwave
program editing

Milestones new EasyCONTROL

software is the most advanced
and powerful operating system
in the field of microwave 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 automatically follow the drawn
temperature or pressure profile, utilizing a sophisticated PID algorithm.

(2) Actual temperature

profile. The microwave
power is automatically
adjusted, based on
continuous feedback from
the process sensors, to allow
the reaction to follow the
desired temperature profile.

Industrial grade touch-screen controller. 6,5 screen with 65.000 colours

VGA resolution 640x480 for sharp process graphics
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-card

Advanced Reaction Sensors

The ETHOS EX 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.

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 vessels
specifications.

Contact-less temperature
control in all vessels
The ETHOS EX features a focused, highsensitivity infrared sensor for contact-less
temperature monitor and control of all
vessels.

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.

Advanced Vessel Technology

High temperature and pressure

Highest safety standards

Easy of use

Fast air cooling

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.

Vent-and-reseal vessels are the

foundation of Milestones
microwave digestion technology.
Continuously enhanced, this
patented (US Patent 5,270,010)
technology provides analysts with
unsurpassed performance

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.

capabilities.

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

SK-6LV

Nr.
of vessels
6
12
16
24
42

Vessel
material
TFM
TFM
TFM
TFM
PFA

SK-12

Vessel
volume (ml)
270
100
75
75
65

Max.
temperature (C)
200
260
200
200
180

PRO-16/PRO-24

Max.
pressure (bar)
10
35
30
30
15

MULTIPREP

ETHOS EX Major Applications

Polymers

Pharmaceuticals

Environment

Oils

Less Solvent, Shorter Time

EPA 3540 (Soxhlet)
Time required
Solvent consumed
13.167 hours
450 L

PAHs and
Pesticides
in Soil
samples

Time required
257 hours

ETHOS EX
Solvent consumed
16 L

Comparison study for processing 1.000 samples.

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

Time required Soxhlet

3 to 16 hours
16 hours
20 hours

Additives from Polymers

Fat from Meat
Impurities in Food Dye

Time required ETHOS EX

20 minutes 140 C
25 minutes 100 C
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
ETHOS EX
Soxhlet

Phenol Resin
31.000
28.000

ABS Resin
2.200
2.200

PET
480
460

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 ETHOS EX Labstation

Post-Extraction Solvent Evaporation
With Milestones patented vacuum evaporation technology, the ETHOS EX
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
Milestones VAC-2000 vacuum module.

ETHOS EX

Technical
Specifications
Microwave hardware

Control terminal

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.

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.

U.S. EPA Methods:

3546, 3052, 3051a, 3015a.
ASTM (American Society of Testing and Materials) Methods:
D-5765, D-6010, D4309-96.

Reaction sensors

Standard Methods Compliance

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.

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 INC.
25 Controls Drive - Shelton, CT 06484 - USA
Tel: (203) 925-4240 - Toll-free: (866) 995-100
Fax: (203) 925-4241
E-mail: mwave@milestonesci.com
www.milestonesci.com
UNI EN ISO 9001: 2000 CERT I F I E D

MILESTONE srl
Via Fatebenefratelli, 1/5
24010 Sorisole (BG) - Italy
Tel: +39 035 573857 - Fax: +39 035 575498
E-mail: analytical@milestonesrl.com
www.milestonesrl.com