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MA182-003 ETHOS UP User Manual
MA182-003 ETHOS UP User Manual
H E L P I N G
C H E M I S T S
ETHOS UP
User Manual
MA182
Milestone Srl MA174-003 – ETHOS EASY – User Manual
Milestone Srl
Via Fatebenefratelli, 1/5
24010 Sorisole (BG) Italy
Tel +39 035 573857
Fax +39 035 575498
Website www.milestonesrl.com
E-mail analytical@milestonesrl.com
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Milestone Srl MA174-003 – ETHOS EASY – User Manual
Index
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Milestone Srl MA174-003 – ETHOS EASY – User Manual
4 SENSORS ................................................................... 26
4.1 Temperature sensors .............................................................................. 26
Temperature measuring in microwave with solvents ........................................... 26
4.2 Rotor setup/Sensor configurations ........................................................... 26
4.3 easyTEMP sensor (T2) ............................................................................ 26
START LOAD function ...................................................................................... 27
Care and maintenance of IR (easyTEMP) sensor ................................................ 28
EasyTEMP Calibration Test instructions .............................................................. 29
4.4 ATC-CE-400 Thermocouple sensor (T1) ................................................... 32
Important tips ................................................................................................. 32
Technical data and limit values of the ATC-CE .................................................... 32
Connection of ATC-CE ...................................................................................... 33
TWIST function ............................................................................................... 34
Operation and safety instructions ...................................................................... 34
4.5 IR-TC (infrared sensor) ........................................................................... 35
Optimal use of IR control as addition to ATC temperature of the reference vessel
(SK-15 rotor). ......................................................................................... 35
Operation and safety instructions with IR-TC ..................................................... 36
Care Instructions of IR-TC ................................................................................ 36
4.6 Pressure sensors .................................................................................... 36
4.7 APC-100 Automatic Pressure Control (P1, Optional for SK-15 and SK-15 eT)
............................................................................................................. 37
Technical data and limit values of the APC ......................................................... 37
APC Connection ............................................................................................... 37
Operation and safety instructions ...................................................................... 38
First use of APC-100 ........................................................................................ 39
Aeration and slope of the reference vessel ......................................................... 39
4.8 P2 sensor (QP, Optional) ......................................................................... 39
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7 TERMINAL ................................................................. 47
7.1 Description ............................................................................................. 47
easyCONTROL ................................................................................................. 47
Terminal T480 ports ........................................................................................ 47
Connecting the unit to the T480 terminal........................................................... 48
Transfer of Settings between Terminal and Interface .......................................... 49
8 EASYCONTROL .......................................................... 50
8.1 Program start ......................................................................................... 50
8.2 General operations tip ............................................................................. 50
Numeric input via touch-screen......................................................................... 50
Text input via touch-screen .............................................................................. 51
Generally used icons ........................................................................................ 51
Editable fields with numeric values and defined range ........................................ 52
8.3 Methods ................................................................................................. 53
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DESCRIPTION PICTURE
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Milestone Srl MA174-003 – ETHOS EASY – User Manual
Milestone suggests to entirely read the User Manual before to run the unit.
The below information can be used as guidelines for the customer Standard Operating
Procedure (SOP).
DESCRIPTION PICTURE
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*The sample amount, the reagents and the microwave program must be chosen in
accordance with the Milestone guidelines (see Milestone application notes on the software
library, Milestone connect or included in your USB Key)
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2 Safety rules
2.1 General Information
• Please read carefully this operator manual before starting the system and follow its prescriptions
with the utmost care.
• In case the system has been delivered with additional accessories (i.e. the terminal is an
additional accessory), also read carefully the instruction manuals of such accessories.
• This Operator Manual is part of the delivery, hence must be always kept together with the
instrument on its working place.
• It is imperative that every person operating this system has read and fully understood this
manual.
• The non-observance of the instructions contained herein or improper use may involve
damages/injuries that are not covered by product liability!
• The national ruling and international safety norms in working environment shall in any case be
observed under user’s responsibility.
• It is also user’s responsibility to keep constantly updated all safety norms ruling in the country or
operation.
Attention = means that the non-observance of the warning may cause damages to unit or
properties.
Warning means that the non-observance of the warning may cause injuries, even severe, to
people.
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• Basic rules of chemistry will always apply. The basic rules of chemistry are valid also for handling
chemicals in this unit. Working with chemicals, always take all those safety measures that are
usually required (i.e. lab coat, protective gloves, protective glasses mask, exhausts hood, etc.)
• Ventilation ports in the housing - for cooling the inside components – must not be covered or
obstructed by any objects.
• The unit must not be installed or stored in an explosive, corrosive or conductive atmosphere
(dust, vapor, gases).
• During program runs, the unit must be carefully attended, to enable timely recognition of
operator’s improper use or error. The unit must under no circumstances (i.e. at night) run
unattended.
• Metal parts in sample chamber
No metal parts must be introduced in the sample chamber of the microwave unit (except for
components incorporated in the original construction). The resulting arc effect can cause
damages.
• Flanges in the sample chamber
Unused flanges must be sealed with the provided screw or plug caps. In any case fingers or
objects in operations should not be held during operations. Flanges should not be modified.
• The microwave unit is exclusively intended for heating materials destined to chemical and
analytical laboratory applications.
• Magnetic stirrer/People with pacemakers
If the unit is provided with the magnetic stirrer, then there is a strong magnetic field inside the
sample chamber. Pacemaker wearers are at risk when in the immediate vicinity of the device.
• PC control device
If the microwave unit is controlled from a terminal or a PC, no changes can be operated on the
control unit. The installation of electronic cards or of additional software can compromise the
function of microwave unit control software.
When working with unknown samples, remember that the samples should react 10-15 minutes after
reagent addition and before the pressure-tight closure of the vessel! After the reaction, samples should
be stirred or homogenized a few minutes in an ultrasonic bath.
It’s important to ensure that no explosive substance and compounds generate together with the
reagents. The pre-reaction should in some case reduce the damages. Milestone doesn’t guarantee and
don’t take any responsibility, if the user create explosive solvents and mixtures! Therefore mixtures made
of solvents (alcohol, ketone, hydrocarbon substance etc.) with concentrated acids such as HNO3, HClO4,
H2SO4, etc. and strong oxidizing agents should be avoided (except under the specific directive of the
Milestone specialist).
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When approved applications are used, all parameters stated in the selected application must be followed,
in order to achieve the same reaction conditions. If this is not possible, the parameters transgression
must be avoided by means of a suitable control, i.e. pressure control.
In practice you should try to generate the most similar conditions as possible in all samples. This means
the same acid quantity and mixture in a considered step. This is necessary, otherwise the single vessel
will reach different conditions by different microwave absorption.
For example, considering a wet sample and a dried sample. In all the vessels, the dried sample should be
weighed according to the organic content of the wet sample and then dilute the dried sample with water,
in order to obtain the same volume (and have the same absorption of microwaves).
Use always the same vessels type in the microwave run. Never use different type of vessels (different
shape) in the same run.
Low microwave absorbing samples can start burning by a partial overheating (i.e. oil, finely ground
plastic, solvents). The tendency to strong exothermic spontaneous reaction is considerably higher in case
of major sample quantity.
Organic substances always react with oxidizing chemicals (e.g. acids, etc.). In addition are
generated CO2 and H2O and, depending on the elements, the corresponding oxidation products
as well. If digestions or reactions are performed without oxidizing chemical agents, a graphite
formation occurs through hydrolysis. Large amounts of (dry) carbon in the microwave generate
flashovers between the particles ("light arcs"), resulting in hot points (up to over 1000 ° C). In
addition, there is very high pressure due to the extreme temperatures and gas expansion. This
in turn causes burns on all PTFE parts and can cause serious damage to the unit.
Therefore, always carry out digestions, according to Milestone Application guidelines. In case of
unknown samples, start using a limited sample weighing (50 mg – 100 mg) to develop the proper
method.
Chemical reactions
The chemical principles find applications also in the microwave field. The reaction conditions i.e. for
digestion of different samples are to be considered as guidelines in MILESTONE applications. The user
may be obliged to adapt the proposed guidelines in MILESTONE applications to his samples.
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• First of all start with 7 up to 10 minutes at lower power i.e. start with 300 Watt, in order to avoid
violent spontaneous reactions and, when possible, use the suitable control.
• If possible, first run the reaction in not sealed vessels.
• The stirring decreases the risk of vessel damages.
In case of high power and/or long reaction last (> 45 minutes) and low microwave absorption (i.e. non
polar solvents/substances), a heating of the plastic components, walls etc. occur, with the risk of burns
or melts of several parts. This concerns particularly quartz or plastic vessels with low MW absorption
features. In this or similar cases, you must absolutely work with weflon absorbers. Suitable control should
be used (i.e. IR control of the shield external temperature).
For high boiling point solvents, which don’t build any pressure up to the application temperature (see
solvents prospectus, physical-technical data), standard glass vessels must be absolutely used (no
pressure vessel). This is particularly true for solvents not showing any high dipole moment; in this case
too high microwave power is irradiated without weflon use. In case of pressure systems, this leads to
heating and damages. In case of solvent, a dielectricity loss occurs at high temperature, therefore this
can be compensated with weflon accessories.
Care of accessories
Accessories such as rotors, reactors etc. should be regularly checked and cleaned. Never use organic
solvents for plastic parts cleaning (except for PTFE) (i.e. acetone attacks the PSU). Water residues must
be thoroughly dried, because they heat in the microwave with the risk of damages. This is particularly
true for water and acid residues located between the PTFE liner and the protection shield. For any
requests, contact Milestone or the authorized distributor in your country.
Control of accessories
Accessories considered important for safety must be tested before every run, in particular the protection
shields. Strong yellow discolorations on the HTC protection shield mean increased diffusions during
digestion which considerably weaken the HTC protection shield. When the inner part of the shield is
rough or even part of the HTC protection cover keeps stuck on the vessel PTFE surface, the protection
shield must be urgently replaced. Milestone representative can help you in this evaluation.
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Through changes of the magnetron on/off working phases, the power is regulated (Pulse Wide
Modulation PWM). The power results in the moment of single pulse signals
Controlled microwave irradiation version without on/off phase. The power supply controls simultaneously
both magnetrons. This technique offers particular advantages in photosynthesis applications for
continuous stimulation of microwave plasma rays.
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Microwave cavity
230 (±10%) V; 50 Hz
Power supply
230 (±10%) V; 60 Hz
2 x 16A reversible
Fuses
500 mA, 250V Heating trafo
C
B
A. Height: 66,5 cm
B. Width: 54 cm
C. Depth: 68 cm
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Height: 40 cm
Dimensions of microwave cavity Width: 43 cm
Depth: 41 cm
Lighting 6x LED
Sensors
ATC-400CE Thermocouple
T1 (Temperature)
ATC-FO Optic-fiber
easyTEMP Infrared-sensor
T2 (Temperature)
IR-TC Infrared-sensor
P1
APC-100 direct pressure control
(pressure)
P2
QP Contactless pressure control
(Pressure)
Exhaust
The acid resistant exhaust unit in the upper housing of microwave unit sucks aggressive gases from the
sample chamber and cools down the vessel shield during the microwave heating.
3.4 Delivery
Unit unpacking
The unit weighs ca. 85 kg, therefore two people, who should stay on the unit’s left and right
side, are required to lift the box.
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Included parts
At least the following parts are included in the supply together with the microwave unit:
• Flexible exhaust tube (Ø65 mm, Spiral, PVC), angle and two adapters included
• Power cord (16A)
• Terminal 480 with connection cable
• User manual
Check within 24 hours that the delivery is complete and, in case some of the items previously
listed are missing, contact Milestone or Milestone authorized distributor in your country.
Check eventual transport damages of the unit. Damaged unit must not be operated. Any
damage should be reported immediately in writing.
Keep the packing safely. In case of unit return to the factory for repair purpose, use only the original
packing and secure it with protective belts. Inadequately packed unit could be considerably damaged
during transport.
The unit must not be placed in a fume-hood to avoid any risk of inner electronic parts
corrosion.
The air sucked from the sample chamber of the microwave unit must be driven to a well-
working hood.
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• The microwave unit must be installed in a well-ventilated and acid vapors-free room, where the
atmosphere must not be highly corrosive. In fact aggressive vapors could penetrate by the
ventilation openings located on the housing, considerably damaging the circuit boards,
connectors, plugs etc.
• Any damage to the electric and electronic parts caused by corrosive influences are not covered
by any warranty. Thus follow the previous indications concerning the installation.
Exhaust
Connect the back outlet opening to the flexible tube in a hood. Do not place the tube with a downward
arc. This creates a siphon effect and acids are accumulated in the lower part.
3.5 Connections
COM port Control connection 24 V for external devices operation via relay box
TERMINAL RJ45 port for the connection with the control terminal (RJ45 cable)
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PIN SIGNAL
Device port (RJ45) 2 RxT (In)
5 GND
6 TxD (Out)
Never connect the terminal when the microwave unit is switched on, otherwise this could
damage the unit interface board.
2. Introduce the interface cable RJ45 in the DEVICE connection on the terminal front side.
3. Introduce the other end of the cable in the terminal connection on the microwave unit back side.
TERMINAL MICROWAVE
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Milestone Srl MA174-003 – ETHOS EASY – User Manual
The microwave door is mechanically locked in the off status or when the temperature is
higher than 80°C..
Never connect the terminal when the microwave unit is switched on, otherwise this could
damage the unit interface board.
If the measured temperature inside vessels is lower than 80°C, the door is UNLOCKED.
If the temperature is higher than 80°C, the door is LOCKED (pausing the run, a message appears on the
top of the screen).
The system does not allow to unlock the microwave cavity door if it is running a digestion
program.
Stop the run or put the system on pause before to unlock the door.
To unlock the door, open the scroll menu on the upper left of the screen and press the “Unlock” button
(see the picture below). Now you have 5 seconds to open the door.
Carefully open the microwave door, in particular when you don’t know the rotor conditions.
High temperatures and high pressure could be still present inside the rotor.
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Upper flange
The upper flange of the sample chamber is secured by a screw locking and can be removed i.e. using the
Venturi system.
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4 Sensors
4.1 Temperature sensors
The temperature control sensors enable the automatic display and monitoring of the internal temperature
or external temperature of vessels during a program run. The desired max. temperature limit value is set
in the terminal. Thereby the limit values of each used vessel system should be respected.
Temperature control helps in:
• Tracking and recording the kinetic of reactions
• Acceleration and optimization of digestion methods development
• Monitoring of reactions
• Preventing vessel damages.
In case of non-polar solvents use, stirring with Weflon buttons and ATC-FO are required in order to
correctly monitor the temperature and control the microwave emissions.
Sensors
ATC
easyTEMP IR-TC APC QP-A
(thermocouple)
Secondary Secondary
SK-15 eT Primary
(optional) (optional)
Rotor Setup
MAXI-44 Secondary
Primary
eT (optional)
Secondary Secondary Secondary
SK-15 Primary
(optional) (optional) (optional)
Secondary
MAXI-44 Primary
(optional)
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According to the rotor configuration, ETHOS EASY microwave platform can be equipped with one or two
eT sensors:
The easyTEMP sensor read the internal temperature of all vessels, and control the microwave emission
according with the vessel at the highest temperature.
The easyTEMP sensor start to read the temperature from 30°C. The system will not monitor the
temperature below the 30°C.
At the beginning of the run, the system delivers a fixed power according to the number of vessels that are
being used. As soon as the internal temperature of the containers reaches 30 ° C, the power is delivered
on the basis of the internal temperature read by the easyTEMP sensor (PID control).
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The IR (easyTEMP) sensor calibration must be weekly tested following the instructions in
chapter “EasyTEMP Calibration Test instructions” (see the following chapter).
In case the test is not passed, the IR sensor must be cleaned. Then the calibration test must
be repeated.
To ensure a correct measuring by the IR sensor, the sensor lenses must be periodically cleaned from
impurities.
In case of contamination, accidental liquid spillage or unusual program, the IR sensor must be cleaned
after each run.
In case chemicals reach the sample chamber, the IR sensor must be properly cleaned and its
functionality must be tested in accordance with test prescription.
The IR sensor lens can be chemically attacked by HF vapours. The consequence of sensor lens corrosion
is lower measuring values.
2. If present, remove the eT sensor protection cover ( SL0239C). For this operation, a small flat-
head screwdriver can be used, paying attention not to scratch the cavity coating.
3. Remove dust or possible solid residues from the IR housing. It can be easily done gently using a
gas duster or compressed air, if available.
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Milestone Srl MA174-003 – ETHOS EASY – User Manual
4. Clean IR lenses with a cotton bud moistened with water. Cotton buds package (p/n 70484 – 100
pcs) is included in the microwave system.
SK eT rotor is monitored by an infrared (easyTEMP) sensor which is positioned on the cavity bottom in
accordance to the rotor ring.
eT sensor calibration test is based on the boiling point of water in an open vessel (atmospheric pressure).
At this working conditions, the boiling point of water is unique and it can be used as reference for sensor
calibration check.
The boiling point of water depends on the elevation above the sea level. At sea level the boiling
point of water is 100 °C; at 1200 m it lowers down to 96°C. For the calibration test, this
variable data must be considered.
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eT-Test method.
The acceptability range of eT-Test is ±10°C from the expected boiling point (generally, 100°C).
If test result is out of the acceptability range, please check the vessel conditions for contaminations or
repeat the test using a different vessel.
If test repeatedly fails, please, contact the Service department.
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eT-Test method.
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The acceptability range of eT-Test is ±10°C from the expected boiling point (generally, 100°C).
If test result is out of the acceptability range, please check the vessel conditions for contaminations and
repeat the test using a different vessel.
If test repeatedly fails, please, contact the Service department.
The ATC-CE-400 sensor is not suitable for non-polar solvents. In this case a fiber optic sensor
(ATC-FO) must be employed.
Important tips
• The measured temperature refers to the reference vessel. In order to have the same
Temperature and Pressure conditions in all other vessels, it’s necessary to load the same sample
type, sample amount, acids type and acids volume.
• The ATC-Sensor is used for detecting the liquid temperature in a vessel. For this reason, the
sensor tip must be introduced in the solution and cannot be free in the gas phase (temperature
distortion).
The minimum volume of acids to use with the ATC400 sensor (in SK-15 rotor) is 10 ml.
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Connection of ATC-CE-400
The ATC-CE-400 sensor can be used in several vessel systems and rotors. Please take into
account the special indications for each system (rotors, vessels).
A Plug
B Fixation stopper (with adapter D)
C Protection shield for PTFE-coated sensor tip
ATC-CE-400
The sensor must be firstly introduced in the vessel outside the microwave cavity.
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Warning: do not pull free the sensor by using the cable! Pull only on the metal connector.
Be sure that the line on the white protection is facing out of the microwave cavity to ensure
proper connection.
TWIST function
The ATC-CE can be employed through its rotating suspension also without TWIST.
The TWIST function of microwave unit must be activated when APC (pressure) sensor is used
together with ATC sensor. Otherwise both sensors will be damaged.
▪ A good electrical connection is important for the sensor in the MW cavity. A good ground
connection ensures that the microwaves do not overheat the sensor. When the sensor is
disconnected, always place the protective cover over the sensor connection in the cavity.
▪ After microwave heating, always test whether the sensor plug-in on the MW cavity has been
heated. Strong heating indicates that the sensor is damaged.
▪ If the instrument does not follow the heating ramp despite a high microwave power emitted by
the system, the ATC sensor is probably damaged or faulty. In this case, immediately stop the
heating program to avoid developing out of control reactions that could cause damage.
▪ If the spring of the ATC-CE on the reference cover has changed color from brown to yellow-brown,
as a consequence of the intensive use, it must be replaced, since on the springs it may originate
graphite, which may cause burns.
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▪ If the ceramic tube screw on the reference cover is strongly discolored, replace it.
▪ Defective ceramic tube with breaking points should not be used.
▪ When the PTFE vessel cover does no longer seal correctly, i.e. due to large gap or damages on the
cover fringe, this must be replaced.
▪ If the PTFE coating of the sensor tip is defective, it must no longer be used. In case of damages
to the PTFE isolation, the sensor should not be used any more, even if it still correctly measures
the temperature.
▪ In case of sensor break, a repair is no longer possible.
▪ For a reliable temperature measuring it’s necessary that the end part of the thermowell is deep
into acids. In 100 ml standard vessel a minimum volume of 10ml must be respected. We
recommend the inserts technique to reduce the reagent quantities down to 5 - 2 ml.
IR-TC-Sensor
Even if the current temperature run is controlled by the inner temperature (T1), the control of the
external temperature (T2) could be a benefit to reach an optimal lifetime of the vessel system.
Observe the following procedure for a correct use of the IR-TC.
1. Each application and each vessel type should be considered separately.
2. To determine the correct relationship between indoor (T1) and outdoor (T2) temperature, use
your rotor with only one vessel, which should include typical sample weight and acid mixture
for the application.
3. Start the desired program to control the inner temperature (T1). The external temperature
(T2) is then recorded. Having only one vessel loaded, the run shows the current ratio of indoor-
outdoor temperature.
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According to our experience Milestone suggest to set the following maximum values for T2 (IR-
TC):
Rotor type T2
HPR (SK-15) (T1/2+10)
Example of T2 limit:
SK-15 rotor T2 = (180°C / 2) + 10 = 100°C
Using SK-15 with ATC-400, the value of T2 is only an extra safety limit; T1 must follow the set
temperature profile of the internal sensor. T2 does not reach its set temperature.
The contact-less measuring of the vessel surfaces serves as safety measure, because it prevents the
overheating, too high continuous pressure and enable i.e. a safe work on the material load limits. If a
set limit value in the software is exceeded, microwave irradiation is stopped, until the temperature
returns below the pre-set limit value.
In the software there is the option ROTOR-CONTROL. If this function is activated, it prevents that
cold places such as the PP rotor wall are considered during the temperature analysis. Moreover,
when ROTOR-CONTROL is activated, the recorded temperature curve is more regular. When
activated, the hottest vessel is considered for the regulation.
Milestone suggests to work always with rotor control ON when infrared sensor is installed.
The heating of vessel surfaces is not immediate as for the internal temperature. A microwave
program can not normally be controlled by the external temperature (T2). The IR-TC has only a
safety feature for the SK-15 configured with the ATC sensor.
The IR sensor is calibrated by the manufacturer by means of the supplied accessory, while the
recalibration can be performed by a service contract.
To ensure a correct measuring of the IR sensor, the sensor must be weekly cleaned with a cotton
bud (i.e. the measuring port and the sensor window located there). In case of unusual/abnormal
program runs, the IR sensor must be cleaned after every run.
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Thanks to the Vent-and-Reseal technology of Milestone vessels it is not mandatory to check the
internal pressure during the run. Unlike temperature sensors, pressure sensors are all optional.
APC Connection
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1. Introduce the pressure tube tip in the cover hole. The tube
is correctly placed, if clamped in the hole.
2. Tighten the screw by hand or with the supplied PP key. Be
careful that the PTFE thread can be rotated in the cover.
3. Check the screw after the first use and periodically and
tighten it, if necessary. An optimal stability is achieved, when PP key
the pressure tube is permanently connected to the reference
cover.
The reference cover of the segment rotors must be set, so that the pressure tube is located in the
direction of the rotor central point, in order to prevent the bending and therefore an additional
abrasion of the tube.
5. Screw the pressure tube in the left flange on the left side
of sample chamber.
The pressure sensor can be used for method development or unknown samples; for all other
digestions, the internal temperature control is sufficient to guarantee a safe process and good
digestion quality.
The measured pressure serves just for the reference vessel. Use the same sample type, sample amount,
acid volume and mixture in all other vessels. Always put the sample into the reference vessel.
By various chemical reactions (i.e. hydrolysis of BF3, SiF4, etc.), the pressure hose can be blocked and
therefore the pressure sensor measures a too low pressure. The user must accurately observe the
reaction procedure. The pressure tube can be normally cleaned i.e. by compressed air. Avoid to run
applications with HF when working with the pressure sensor.
The TWIST function of microwave unit must be activated when APC (pressure) sensor is used
in order to prevent damages to the probe.
Before starting each run, check that the pressure tube can freely move, without getting stuck
and twisted.
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Milestone Srl MA174-003 – ETHOS EASY – User Manual
For the first use, a test run with water should be performed as here below:
- Water volume: 10 ml
- Microwave program:
Check that the temperature profile is correct without jumps / falls in temperature and that no water drop
appears on the reference cover (near the pressure tube connection) or on the pressure sensor connection
on the cavity.
To release the pressure tube after the program run, first of all the APC vessel must be pressure-released.
This can be carried out, the same as for all other pressure vessels, only after the cooling down below the
boiling point of the vessel content. Reaction gases up to 20 bar can be present in the cooled pressure
vessel. If the inner pressure is reduced by a careful opening of the pressing screw, the pressure tube can
be safely removed. As alternative, the inner pressure can be vented directly to the screw of the pressure
tube, by carefully turning it with the protective gear.
Switch on the ventilation of the Microwave cavity before to release the gases from the pressure
tube.
Wear the suitable protective clothes and glasses and wipe splashed acid with a cloth.
The sensitivity and thus the response can be set in the control software. Follow the respective software
user manual. A high sensitivity should be selected, so that the sensor can promptly responds to each
incident.
The P2 sensor is not ready for ca. two minutes after the microwave unit switching on, because it displays
the highest value (up to 100%). After ca. two minutes the sensor is ready for measuring (display 0%).
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When the system is on, the P2 value is 0% (at the beginning) and the unit is ready for use (this
concerns only #QPA00200 and #QPS00200).
In case of contaminated laboratory air (from NOx, acid vapours, solvents, etc.), the measuring
value is compensated and therefore the sensor response is not reliable. In extremely
contaminated environments, the sensor loses its sensitivity.
The P2 sensor for digestion detects the NOx gases produced by the digestion.
High concentration of NOx and acid vapors in the lab causes an increased basic value of the P2 sensor.
However, the general rule is that a high sensitivity value is selected.
For P2 sensors for digestion (or QP-A), it is recommended a limit value of 70 - 90%.
If the gas concentration is above the set limit value (activate QP-Check), the microwave
irradiation is stopped, but the program run continues. The MW heating will restart, as soon as
the gas concentration returns below the pre-set value.
The P2 (QP) sensor can be damaged after constant exposure to acid vapors (or NOx) for a long
time.
You can check the correct function of the P2 sensor running a function test.
In a glass or plastic vessel are placed ca. 100mg copper wire (1,5mm²). The 2ml HNO3 65% are dosed
and the vessel is immediately closed with a cover. The cover is then removed in the unit during running
ventilator (max. ventilation) and the vessel is directly hold in the suction. The signal should be after short
time ca. 20% (displayed in the upper menu) or more (depending on the type of copper sample).
At higher sensitivity, the P2-S sensor detects the most frequently used solvents, including alcohol and
non-polar solvents. Since organic solvent vapors are often explosive, the P2 sensor contributes in a
considerable way to the working safety conditions.
You can check the correct function of the P2-S sensor running a function test.
The sensor must be tested with alcohol (ethanol) and a non-polar solvent. For this reason the open flask
or open vessel with solvent is placed at the exhaust end. The exhaust must be running. A signal increase
must be visible in the P2 sensor display.
If digestion applications are carried out in the microwave system with the P2-S installed, the function and
lifetime of the this sensor can be compromised.
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5 Additional devices
5.1 Magnetic stirring (Optional)
Function description
The magnetic field inside the sample chamber can cause damages for example to wristwatch on
wrist.
When using Milestone rotor, it’s possible to introduce a stirring bar in each vessel. The optimum stirring
range is measured from the rotating axis at ca. 220mm. For an optimized stirring, the center of the
stirring bars in each position should be placed in this range and can be used on the unit bottom up to ca.
80mm (optimal 35mm).
A sole stirring bar can be operated in the middle of the microwave unit. In order to achieve a good
stirring, the stirring bar should be placed not higher than 50mm from the unit bottom. A stirring bar in
the center can have up to 100mm diameter, according to the reaction vessel.
For larger diameter, take care of the MW heating by the microwave coupling.
In order to prevent stirring bar contamination Milestone offers PTFE or WEFLON (heating of non-polar
solvents stirring bars). Choose the correct stirring bars based on your vessel configuration.
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Too high temperatures (above 250 - 260°C) can damage the stirring bars.
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Reagent Characteristics
HNO3 Nitric acid is the most common reagent for the oxidation of organic matrices. Its
oxidation potential is strongly dependent on the reaction temperature since the boiling
temperature of azeotropic mixture with water is 121 °C at atmospheric pressure, the use
of closed reactors are normally recommended to increase its oxidant power. An
important feature is related to the ability of HNO 3 to dissolve most metals to form soluble
nitrates. Such oxidant action can be further enhanced by the addition of other acids or
H2O2.
H2SO4 Concentrated sulfuric acid (98%) can carbonize organic substances, its boiling
temperature is 338 °C. It is a strong dehydrating agent and commonly used in
combination with HNO3 or H2O2.
HClO4 Perchloric acid presents an oxidant power directly related to its concentration and
reaction temperature. It presents a strongly trend to react violently with organic matter
under heating, but its mixture with HNO3 decreases the reaction rate. HClO4 is thermally
decomposed at 245 °C, which releases higher amounts of gaseous by-products, leading
to high excess of pressure.
H2O2 Hydrogen peroxide is normally used in concentrations ranging from 30 to 50%. Higher
concentration can react explosively with some organic compounds. It is frequently used
in combination with HNO3 and H2SO4 in wet digestions.
HCl Hydrochloric acid is a non-oxidizing agent that exhibits weak reducing properties. HCl
readily dissolves many metal carbonates, peroxides, and alkali hydroxides. Despite a
major part of metals form soluble chlorides, some elements can form insoluble
compounds as AgCl, TiCl and PbCl 2. While HCl reacts with most metals, it is normally
combined with HNO3 to form Aqua regia, which is able to dissolve even noble metals.
HF Hydrofluoric acid presents a strong complexing nature. It is most commonly used for
inorganic matrices because it is one of the few acids that can dissolve silicates. Glass or
quartz reactors can not be used for sample digestion. In some cases its removal before
analysis is mandatory in order to prevent equipment damages. In this case, usually, boric
acid is often added to neutralize active HF, being necessary to filter the sample solution
at the end of the digestion. Its use prevents the formation of sparingly soluble products
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of groups 4, 5, 13 and 14 of the periodic table, increasing the solubility and stability of
Si, Sn, Ti, Zr, Hf, Nb, Ta, Pa, etc.
Aqua
Regia A mixture of concentrated HCl and concentrated HNO3 (volumes 3:1) is commonly called
as “aqua regia”. This reagent has an additional oxidizing effect by formation of NOCl
with a subsequent formation of nascent chlorine. The main feature of this mixture is the
ability for dissolution of noble metals, such as gold, silver, palladium and so on.
(CH2)n + 2HNO3 (aq) → CO2 (g) + 2NO (g) + 2H2O (l) (1)
In different organic samples, the HNO 3 and H2O2 addition must be carried out carefully, since it
can lead to excessive foaming generation. This is particular true for samples with higher Fe2+-
or Cl—concentration or additional carbonate replacement.
However listed programs can be changed and therefore adjusted for special applications. The basic
principle is that by choosing the right chemicals, it’s possible to achieve better digestions. The following
indications should be of help for the adjustment and optimization of the basic program to particular
problematic.
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When using pure high boiling chemicals for method development, the pressure cannot be controlled,
because i.e. pure H2SO4 ca. 96 % (high boiling point 338 °C).
The use of concentrated sulfuric acid (ca. 96 %), mixture with phosphoric acid or ammonium salts and
other additives requires particular precaution. Milestone do not suggest to run tests with H2SO4 ca. 96%
over the 280°C because you risk to damage the thermowell and Teflon vessel.
• Control of internal temperature (T1). An additional T control of the vessel shield with IR sensor
(T2) is suggested (at the same heating rate/power).
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7 Terminal
7.1 Description
The terminal 480 has a high-resolution color screen with touch-screen function. It’s a working interface to
simultaneously create, run and save microwave programs.
Terminal 480
The operation is carried out by touching the icons on the screen (touch-screen). The software
easyCONTROL is permanently installed in the memory of the terminal.
All control parameters with the desired and actual curves are simultaneously displayed in different
colours. The measuring values are represented in real time on the pre-determined parameter curve.
easyCONTROL
The easyCONTROL Software is installed in the TERMINAL at the time of delivery. Software Updates are
carried out by the Service.
Control terminal touch-screen 4,3” TFT display, 480x272 VGA resolution with 16M
Terminal model
colors
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RJ45 interface for the unit. Interface cable RJ 45. Connection for
communication with the microwave unit.
Cable: RJ45 plug in the Terminal side
PIN SIGNAL
One RJ45 Ports
2 RxT (In)
5 GND
6 TxD (Out)
The terminal T480 can be connected to the right side of the microwave unit. The silicon disc is positioned
between the terminal and the unit.
Assembly parts:
• P/N SG0010A Silicon disc Ø40/6x4mm
• P/N SR0069 Cylinder-hexagonal screw
M6x16
• P/N SR0166 External teeth lock washer
M6
1. Connect the microwave unit to the power supply via the power cable. Check that the main switch
on the front side is set to OFF position.
2. Introduce the interface cable RJ45 in the DEVICE connection on the terminal back side.
3. Introduce the other end of the cable in the terminal connection on the microwave unit back side.
Never connect or disconnect the terminal if the microwave unit is switched on, otherwise you
could damage the interface board of the microwave unit.
TERMINAL MICROWAVE
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The system administration settings (see also Chapter on System Administration) are saved on the
terminal and into the interface board (microwave). The settings in the control panel are exclusively saved
on the terminal.
Once the terminal is connected to the unit, the settings are transferred as follows:
If there are no settings saved on the interface board, they are downloaded from the
terminal to the interface board.
If settings are already saved on the interface board, then they are transferred from the
interface board to the terminal.
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8 easyCONTROL
8.1 Program start
Switching on the unit also the terminal is turned on and the program is initialized. The system takes 30
seconds to turn on. During the boot process, a white screen with Milestone logo will appear. After that,
the "play" icon will flash for a few seconds before allowing the microwave to start.
Power and
Temperature
values in real
time
Start screen
The green button in the lower right part of the screen is to start the method. By clicking the right
thumbnails, they will be enlarged and displayed on the centre of the screen.
In several steps of the program it is necessary to enter numbers. Touching twice on the field or on the
number to be changed, a numeric keyboard will appear
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Numeric keyboard
For steps requiring a designation/description, a standard keyboard will appear by double-touching the
touch-screen.
Standard keyboard
General Menu
Methods menu
Select - OK
Delete - Cancel
Save
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New
START button
• P2 limit: %
• Door locking: °C
• t (time): hh:mm:ss
• MW (power): W
• T2 (temperature 2): °C
• P1 (pressure optional): bar
• Cooling:min
• Background
o Red
o Green
o Blue
• Max jump: °C
• Above 50°C:
o Time: s
o Delta T: °C
• Amount of water: ml
• Ambient temperature: °C
• Weight of vessel: g
• Thermal capacity: kJ/Kg/K
• Start temperature: °C
• End temperature: °C
• Test energy: W
• Test time
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8.3 Methods
By touching the upper right icon, you can enter into the select menu of applications. In each category, you
can find a series of pre-installed methods.
Applications
Categories
You require the Administrator access to open the categories (except for Recent).
Administrator: 123456
The password can be changed in the Control
Panel.
Here you can open and run several methods.
The methods are optimized for each
rotor type. Choose the right method
according to your rotor configuration.
easyTEMP methods are signed with an
“eT”:
• SK et
• MAXI eT
Milestone method ready to be started. This
method cannot be deleted or overwritten.
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In the following registers, there are all method information and settings.
Upon delivery, the rotor included in the supply are activated in the setup menu. If you already have a
rotor or if you order it in a second moment, this can be activated by the administrator.
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General information
Parameters
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Program
Set the heating program and the cooling time for
the new method.
• Nr: Number of steps. Digestion methods
are usually made by a minimum oft wo
steps and a maximum of 4 steps.
t: Time of this step
• MW [W]: Microwave energy
• T1 [°C] (optional): Temperature limit of
the thermocouple
• T2 [°C]: Temperature limit of Infrared
sensor
• P1 [bar] (optional): Pressure limit
Program sequence
PAUSE
While the program is running, the pause icon
appears to the right.
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ZOOM
Touch the screen from the top left corner to the
bottom right corner and you remain in the final
position for about half a second before releasing.
The section will be zoomed on screen
ZOOM-OUT
Below the graph the "Zoom Out" button appears.
Tap this button to zoom out.
Graphical representation
The individual graphs can be displayed or hidden from the screen by pressing the corresponding button.
T1, RED
The curves (setpoint curve and measured curve)
for the ATC (thermocouple) sensor, internal
temperature.
T2, ORANGE
The curves (setpoint curve and measured curve)
for the easyTEMP / Infrared temperature.
P, BLU
Curve of internal pressure
E, BLACK
Curve of the Microwave emission
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SELECTION OF P2
When this button is activated, marks appears on
graphic, if the P2-limit is exceeded. When
pressing the button again, the P2 signal is shown
as a line.
For rotors which are directly controlled by the easyTEMP, the load control function is activated.
This function regulates the supplied microwave power depending on the number of vessels in the rotor to
avoid temperature overshooting during the run.
8.5 Setup
This part of software is dedicated for the setup of the system and only the Service login profile can
change all parameters.
Administrator and Manager can change few parameters form this page.
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Access window
Settings
Here you can edit the general setting of the
terminal.
Users
In this section you can :
• Create new users or administrators or edit
existing ones;
Settings window
In the following sections you can edit the system settings. The shaded settings can only be changed by
the service. The Printer icon allows to print the setting.
Applications
Here you have the possibility to select the
application library according with your
configuration.
Rotor
In this section you can set the number of vessels
for each rotor type or add new rotor types.
Sensor Check
In this section, for each rotor type it is possible to
set a different temperature and time range of the
sensor check alarm.
Contact your service engineer for more details
about these values.
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Sensor settings
These settings can only be edited by Service
Control settings
These settings can only be edited by Service
Rotor lifetime
Here is an automatic countdown of the
number of digestion cycles. at the end of the
number of cycles, a message will appear to
remind you to replace the consumable parts
of the rotor.
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MW energy test
This window is for the microwave energy test.
Contact your service engineer for more details
about the test.
Setup window
First Steps
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From the Users window, you can create a new login name. There are three different types of users with
different levels of accessibility (privileges) that can be created.
Here below a table with more details concerning the privileges according with the login type
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User
Manager
Administrator
User
Manager
Administrator
There are two additional login levels that cannot be modified by the Administrator.
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New ID profiles can be created by the Manager, Administrator, Service and Supervisor accounts.
Each user must have one single ID profile and each ID profile has to be associated to no more than one
person.
It’s responsibility of the user (with a Manager, Administrator, Service or Supervisor account) to
guarantee the uniqueness of each account to every single person.
• Have a register (notebook or excel file) with list of all ID Username with the corresponding name
and surname of users.
Here below all steps to create a new ID profile with the “CFR password” configuration activated.
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9 MILESTONE CONNECT
Milestone Connect is a website (www.milestoneconnect.com) where you can find information about your
own unit, application notes, scientific paper, user manuals, tips and techniques and everything else you
may need to improve the operations with your microwave system.
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In addition, the Milestone connect site offers direct online support (Support > Application support or
Service visit) and the possibility to download the list of consumables with the corresponding Part numbers
(Library > Spares).
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Security query
To avoid accidental modifications to the method,
the system perform security queries.
If the user start a program which is not entitled or
is not possible a message appears.
Error messages
If an error is detected by the software, a window
appears with the error message.
Error messages are acknowledged by pressing the
Cancel button
• Login
• Program
Login
Text Meaning/Comment
The password you entered is incorrect. The password you entered is invalid for the selected
Please repeat your entry or cancel the login. user.
You have no permissions for this device. The device has the login mode "with disk". The signature
Please contact your administrator. of the disk is part of a user who has no access to this
device.
The registered name already exists. No name can be The name of the user must be different.
used twice. Choose a different name.
Text Meaning/Comment
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In your system are no sensor inputs There are no configured sensors. The configuration of the sensors
configured. can be made only by the service (see Chapter sensor data).
Please contact your local service partner.
Your system contains a sensor for pressure The curve of a sensor is not defined.
measurement. During the program the measuring of this parameter is not verified.
Therefore, the pressure curve was checked. This can lead to uncontrolled power output (see chapter description
This curve is not sufficiently defined. of the program parameters).
Do you really want to start the application?
Your system contains a sensor for T2 The curve of a sensor is not defined.
measurement. During the program the measuring of this parameter is not verified.
Therefore, the T2 curve was checked. This can lead to uncontrolled power output (see chapter description
This curve is not sufficiently defined. of the program parameters).
Do you really want to start the application?
The control of the temperature sensors The sensor check has detected an error in the temperature
checked an error. measurement (see chapter Sensor Check).
The value of T1 (T2) has changed in one This message depending on the actual and nominal values and can
second of 25.0 ° C to 100.0 ° C and thus vary according to the appearance.
exceeded the limit of 50.0 ° C. Check the temperature sensor and the placement of the sample
(infrared sensor).
You have not entered a value for the element You do not have defined the parameter according to which the
"Control for". power has to be controlled.
In the register Method \ Parameters you must specify which
Please select one of the available sensor parameters you want to control (see Section parameters).
inputs.
Twist function will be disabled. Security check when disabling the twist function (see also Chapter
Temperature and pressure sensors can be Twist)
damaged.
Are you sure to deactivate the twist function?
Program
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MILESTONE
Milestone Srl - via Fatebenefratelli 1/5 - 24010 Sorisole (BG) - Italy
Phone +39 035 573857 - Fax +39 035 575498
H E L P I N G
e-mail: analytical@milestonesrl.com - web: www.milestonesrl.com
C H E M I S T S