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MILESTONE

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

Thank you for selecting our microwave system.


We are sure that you will be completely satisfied with the performance of
this new unit entering your laboratory. We invite you to read carefully this
user manual and to keep it in reach for convenient and fast consulting. The
person who will be using this unit should have received an appropriate
training from a Milestone trained technician. For any possible clarification or
any request for assistance please contact either our Representative in your
country:

or Milestone at the following address:

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

Pubblication date (gg/mm/aaaa) 06/02/2019

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Milestone Srl MA174-003 – ETHOS EASY – User Manual

Index

1 MILESTONE ETHOS EASY ............................................ 6


1.1 SETUP YOUR ETHOS EASY ........................................................................ 6
1.2 START USING YOUR ETHOS EASY ............................................................. 7

2 SAFETY RULES .......................................................... 11


2.1 General Information ............................................................................... 11
2.2 Safety rules for Start-up .......................................................................... 11
2.3 Safety in operations ................................................................................ 11
2.4 Safety in service operations ..................................................................... 12
2.5 No manipulation of the unit allowed......................................................... 12
2.6 Parts replacement................................................................................... 12
2.7 Customer support ................................................................................... 12
2.8 Other hints ............................................................................................. 12
2.9 Instructions for safety operations ............................................................ 13
Handling of unknown samples .......................................................................... 13
Vessels number, weigh, acid quantity, program run, material .............................. 14
Samples type – spontaneous reactions .............................................................. 14
Chemical reactions .......................................................................................... 14
High microwave power for long time ................................................................. 15
High boiling point solvents ............................................................................... 15
Care of accessories .......................................................................................... 15
Control of accessories ...................................................................................... 15
2.10 Maintenance and care ............................................................................. 16

3 DESCRIPTION OF THE SYSTEM ................................. 17


3.1 General overview .................................................................................... 17
3.2 Technical description .............................................................................. 17
Pulsed microwave irradiation ............................................................................ 17
Not pulsed microwave irradiation ...................................................................... 17
3.3 Technical data ........................................................................................ 18
Microwave cavity ............................................................................................. 18
Sensors 19
Exhaust 19
3.4 Delivery ................................................................................................. 19
Unit unpacking ................................................................................................ 19
Included parts ................................................................................................. 20

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Milestone Srl MA174-003 – ETHOS EASY – User Manual

Installation of the unit...................................................................................... 20


Exhaust 21
3.5 Connections ........................................................................................... 21
Back panel ports.............................................................................................. 21
TERMINAL T480 ports...................................................................................... 22
3.6 Microwave door ...................................................................................... 23
Emergency opening of the door ........................................................................ 23
3.7 Upper flange .......................................................................................... 24
3.8 Milestone logo with backlighting .............................................................. 25

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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Milestone Srl MA174-003 – ETHOS EASY – User Manual

Sensitivity, software setting .............................................................................. 39


P2 (or QP-A) sensor for digestion ...................................................................... 40
P2-S (or QP-S) for organic solvents ................................................................... 40
Operation and safety instructions ...................................................................... 40

5 ADDITIONAL DEVICES .............................................. 41


5.1 Magnetic stirring (Optional) ..................................................................... 41
Function description......................................................................................... 41
Stirring in several vessels ................................................................................. 41
Stirring in only one vessel ................................................................................ 41
Applications 41
Stirring bars choice .......................................................................................... 41

6 CHEMISTRY OF DIGESTION TECHNIQUE .................. 43


6.1 Digestion chemicals ................................................................................ 43
6.2 Digestion reaction ................................................................................... 44
6.3 Digestion methods and tips ..................................................................... 44
Digestion quality not satisfactory – simply operations for the user: ...................... 45
Q/P sensor regulates too early– simply operations for the user:........................... 45
T1 desired curve is not achieved – simply operations by the user: ....................... 45
6.4 Digestions with high boiling acids or mixtures........................................... 45
Direct use of high boiling acids and mixture ....................................................... 45
Method development using high boiling chemicals .............................................. 45

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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Milestone Srl MA174-003 – ETHOS EASY – User Manual

Method selection from Milestone database ......................................................... 53


Create new methods ........................................................................................ 55
8.4 Program sequence .................................................................................. 57
Graphical representation .................................................................................. 58
Load control function ....................................................................................... 59
8.5 Setup ..................................................................................................... 59
Access window ................................................................................................ 60
Settings window .............................................................................................. 60
Setup window ................................................................................................. 62
8.6 Create, Edit, Delete a User profile ............................................................ 62
First Steps 62
Overview of user profiles and access levels ........................................................ 63
Create a new ID user profile ............................................................................. 65
Edit or Delete an existing ID user profile ........................................................... 66

9 MILESTONE CONNECT .............................................. 68


10 MESSAGES AND INQUIRIES...................................... 71
10.1 List of queries and (error) messages ........................................................ 71
Login 71
Sensors, Settings and Twist .............................................................................. 71
Program 72

11 APPENDIX 1 – ANALYTICAL INDEX OF SOFTWARE


SCREENS ................................................................... 74

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Milestone Srl MA174-003 – ETHOS EASY – User Manual

1 Milestone ethos easy


Setting up your Milestone ETHOS EASY is simple. Just read the following instructions. Once completed
the setup, take some time to explore the features of your system. The user manual provides tips and
instructions to help you learn the basics of your ETHOS EASY.

1.1 SETUP YOUR ETHOS EASY

DESCRIPTION PICTURE

Plug the terminal cable in the “TERMINAL” port


on the back side of the unit and then the other
side in the “DEVICE” port of the terminal

When connecting the terminal to the


unit, the instrument must be switched
off.

Connect the power cord to the back side of the


unit

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Milestone Srl MA174-003 – ETHOS EASY – User Manual

Connect the exhaust tube to the unit and place


the opposite side into the fume-hood (or any
connection to it)

Switch “ON” the unit

1.2 START USING YOUR ETHOS EASY


Milestone ETHOS EASY can be used with a wide range of rotors, inserts and accessories. In the following
instructions we will quickly show the way to use a Milestone closed vessel digestion system. The
description of Your configuration is fully reported into the 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

Remove the vessel from the rotor

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Milestone Srl MA174-003 – ETHOS EASY – User Manual

Place the vessel on the balance and weigh the


sample*

Add the reagents*

Introduce the vessel into the protection shield.

Place the cover and the safety spring on the


vessel and place it into the segment.

Close the vessel into the segment using the


torque wrench.

Place the segment into the rotor plate.

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Milestone Srl MA174-003 – ETHOS EASY – User Manual

The main page will be visualized on the screen

Press “LIBRARY” icon

Press “DIGESTION” icon

Select your Application Field (i.e. Agriculture)

Select your Method (i.e.Dried plant material


method)
and press ✓ icon

Close the door and press Start icon

After the cooling remove and open the vessels

After the end of program, you have to


wait to reach 80°C temperature
(internal temperature) before to open
the microwave door, remove the rotor
and open the vessels.
Slowly unscrew the segments to allow
the residual pressure to be gently
released from the vessels.

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Milestone Srl MA174-003 – ETHOS EASY – User Manual

Transfer the solution into a marked flask. Dilute


it and rinse the vessels with distilled water

*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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Milestone Srl MA174-003 – ETHOS EASY – User Manual

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.

Information = indicates important information/recommendations for the user.

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.

2.2 Safety rules for Start-up


The first start-up of the system must exclusively be carried out by authorized and trained service
engineers appointed by Milestone.

2.3 Safety in operations


• The unit must exclusively be operated for its intended use, otherwise the protection can be
compromised.
• The unit must only be operated within the power limits set forth by the technical specifications.
• The unit must be operated exclusively by specially trained people.
• All electrical parts must always be protected from wet and humidity.
• The unit must be kept clean.
• Disconnection from the power cord.

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Milestone Srl MA174-003 – ETHOS EASY – User Manual

• 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.)

2.4 Safety in service operations


• In case of failure or damage of the unit, the intervention of an authorized and trained service
operator must be requested. The unit shall not be used until successful repair is completed. The
unit includes components in which lethal high voltage of 4kV can be reached. Improper repairs
by unauthorized people may cause microwave leakage and consequent injuries to personnel.
• Do not operate the unit, if a minimum doubt exists about its trouble-free operation and good
functioning.
• Service can only be carried out by authorized and trained service engineers of the company
Milestone. Works on the electrical and electronic components of the system must be carried out
exclusively by specialized electrical/electronic engineers.
• Before every repair – service – installation, always make sure that the unit is disconnected from
the power supply line and cannot involuntarily be switched on.

2.5 No manipulation of the unit allowed


Constructive changes/modifications of the unit and its accessories are forbidden, in particular any
openings in the sample chamber must be carried out, because microwaves can be released there.

2.6 Parts replacement


In order to guarantee the good functioning of the unit and user’s safety, all replacement parts must be
exclusively original supplied by Milestone. Original spare parts are granted by high quality control on the
material and during the production.

2.7 Customer support


• The Warranty and the Service Report are included in the documentation delivered together with
the unit.
• After the installation, you are kindly requested to send us the filled in warranty card via fax or e-
mail (form on the website).
• In case of required unit reparation, you should send us the filled in Service Report including
precise description of the errors.
• For any request or order, please contact your local area representative or directly Milestone.

2.8 Other hints


• The microwave unit can be provided with several sensors and built-in devices, which are in part
described in this user manual. This does not mean that all the options are installed in your unit,
but the supply depends on your order.
• The unit must be connected to a socket with protective grounding.
• Be careful that voltage and frequency of the power supply match with the values indicated on the
shield on the unit back.
• The system must be operated with the original power supply cable supplied together with the
unit.
• The power supply cable must be in perfect conditions and must not show any damage.
• The unit must be operated only in upright position.
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Milestone Srl MA174-003 – ETHOS EASY – User Manual

• 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.

2.9 Instructions for safety operations


• All samples and chemicals can be used only in the tested and released vessels by MILESTONE.
• The use of flammable liquids and substances developing toxic and harmful gases depends on the
user’s requirement, who is responsible for his own care.
• The user is responsible for the correct and safe use of chemicals.
• When following Milestone application notes, all parameters, settings and equipment shall be
noted and followed. The proposed application notes by Milestone are only to be considered as
general guidelines and must be adapted to each single sample or used material.
• The pursuing of different application must be discussed with Milestone Application Specialist.
• Application requirements must be met.
• If damages occur to the microwave unit, in particular to the door, door frame, welded joints and
ventilation openings, the microwave unit may no longer correctly work. The microwave unit must
be shipped back to Milestone for a safety check.

Handling of unknown samples

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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Milestone Srl MA174-003 – ETHOS EASY – User Manual

Vessels number, weigh, acid quantity, program run, material

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.

Samples type – spontaneous reactions

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.

Basic principles for digestion, extraction or synthesis with the unit


• Check the vessels before and after a program run (or automatically by Q/P sensor).
• In case of method development, start firstly with little sample quantity.
• In case of digestion with unknown samples, start with basic program for reactive samples.
• Consider physical and chemical features of samples and chemicals. For example ignition
temperature of a solvent (i.e. diethyl ether 170°C), or undesired dangerous by-products; when
performing synthesis, clarify if the inert gas is necessary, in order to avoid accident reactions with
oxygen, etc.

Digestion of fine ground organic powders


Finely ground powders often react violently. In order to prevent damages, the below guidelines must be
exactly followed.
• Weight < 0,5 g.
• Except for plastic samples, the reagents must be diluted with 2 up to 3 ml distillated water, in
order to postpone the reaction. In case of plastic powders or foils, possibly employ only pure
HNO3 65% (see the applications for more details).

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Milestone Srl MA174-003 – ETHOS EASY – User Manual

• 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.

Mix the samples with digestion reagents


The sample must be well-mixed with the acid before starting a digestion. Reactive wet samples floating in
the sample or located on the vessel bottom, tend to originate violent reactions which could have
explosion features or could originate burns in the PTFE vessel. There are several possibilities to carry out
the mix: basic movement, ultrasonic bath, magnetic stirring, magnetic bars.

Gas and vapor pressure in digestion vessel


According to each sample, large quantities of reaction gases can develop. Then you should consider also
the vapor pressure of the reagents. Reaction vessels should never be opened without cooling down
below the boiling point. After the digestion, there still can be a big pressure of CO2 and NOx-gas. Thus
always open slowly the vessels, otherwise may develop excessive foaming, as a consequence of the too
fast release of gases present in the solution.

Very strong oxidation media


HClO4 – organic and inorganic perchlorate – etc., can violently react with organic samples. Thus is
recommended a first digestion with HNO3 and then, as second step, a digestion with very strong
oxidation media. If you want to perform only one step, don’t use no more than 20% HClO4 of the total
volume. Never use perchloric acid in compounds with sulfuric acid. Never evaporate perchloric acid
together with the organics still present.

High microwave power for long time

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).

High boiling point solvents

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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Milestone Srl MA174-003 – ETHOS EASY – User Manual

2.10 Maintenance and care


• Please, be sure that the sample chamber is always clean. Contamination in the door area can
obstruct the correct door sealing, letting out microwave irradiation.
• Before each run, check and remove eventual contamination in the sample chamber, in particular
the area near the door and its wall.
• Sediments in sample chamber such as contamination and solvent residues etc. can cause burns
and damages.
• Before starting a working step, test the protection cover for the camera in the inner chamber. In
case it’s dirty, clean it with a soft cloth wetted only with water.
• Contamination on the bottom can stop the rotor movement.
• Normally a gentle cleaning with a soft cloth or paper towel, dried or moistened with water,
should be carried out.
• To remove strong contamination, you can use mild detergents.
• Don’t use any abrasive cleaner on the sample chamber walls and on the door, because they
could damage the PTFE coating.
• If the microwave unit is equipped with a QP sensor for digestion, don’t use cleaning agents
containing alcohol or solvents, because such substances are responsible for the sensor output
signal for several days, and the sensor cannot be used.
• In case of extreme vent or vessel rupture after a spontaneous reaction, perform absolutely the
following control: behind the barred opening of the sample chamber light, there is a disk. Check
if the disk is not lose or splintered, by gently pressing with a blunt pointed object through the
grids on the disk. If the disk is damaged, have absolutely it repaired.
• Contamination on the external side of the housing can be removed with a damp cloth and mild
detergents.
• The unit life, in particular of the electrical and electronic parts, is mainly depending on the
environmental conditions. The unit should not be installed under a hood, but in a well-ventilated
room, free from acid vapors and corrosive atmosphere. Although the housing is stainless steel
made and the critical parts are coated, components like plugs, electronic boards, etc. can be
damaged by corrosion. These parts cannot be manufactured in more resistant materials. Thus,
the most common problems are due to corrosion and chemical attack to these components.
• All components in direct contact with samples, sample vessels, etc. must be handled with the
utmost care, i.e. the parts must be free from chemical residues/traces and dried before use. This
principle is of course well-unknown in the trace analysis, but not always properly taken into
account.
• Dust in the laboratory atmosphere is very frequently responsible for deposits in the ventilation
area (air inlet and exhaust, etc.) and must be removed, to prevent overheating and/or damages.
• Check that the exhaust tube is regularly introduced into its opening. If the pipe is disconnected,
reintroduce it until it’s firmly fixed.

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Milestone Srl MA174-003 – ETHOS EASY – User Manual

3 Description of the system


3.1 General overview
The ETHOS is a microwave system destined exclusively to laboratory applications.
By contactless microwave irradiation it’s possible to heat several kinds of material. The heating is
different for all substances and depends on their dipole.
The irradiation of microwave occurs from the ceiling of the sample chamber.
The terminal is used to control and represent the parameters during the reaction. All parameters can be
simultaneously pursued and actively optimized during the run.
The unit is equipped with a built-in suction and cooling fan with tube connection to an external exhaust.

3.2 Technical description


The microwaves irradiation is performed through two industrial magnetrons, connected to a power supply
with 4 kV high tension and filament current. Both a pulsed and not pulsed (continued) microwaves
irradiation are possible.
The high microwave power permits fast heating rates and in addition offers a homogeneous microwaves
impact and temperature distribution.
The microwaves are reflected in the sample chamber through a turntable field distributor. Thanks to it, a
regular distributed microwaves field develops.
The microwave power can be set in steps of 10 Watt in the terminal.
The unit is designed, so that the power density near the irradiating microwave surrounding area is
inferior to 1 mW/cm² in a distance of 50 mm.

Pulsed microwave irradiation

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

Not pulsed microwave irradiation

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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Milestone Srl MA174-003 – ETHOS EASY – User Manual

3.3 Technical data

Microwave cavity

230 (±10%) V; 50 Hz
Power supply
230 (±10%) V; 60 Hz

2 x 16A reversible
Fuses
500 mA, 250V Heating trafo

Built-in fuses Cutout 16A with circuit breaker C or D

Power consumption at max. heating power 3500 VA

Microwave power 2 x 950 W

Microwave in heating room Frequency: 2,45 GHz Wave length: 12,25 cm

Dimensions without terminal

C
B
A. Height: 66,5 cm
B. Width: 54 cm
C. Depth: 68 cm

Weight without terminal ca. 85 kg

Required space with terminal Width: 1,0 m Depth: 0,75 m

Temperature range 5 – 40°C

Max. altitude above sea 2000 m

Volume 75dB (A)

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Milestone Srl MA174-003 – ETHOS EASY – User Manual

Height: 40 cm
Dimensions of microwave cavity Width: 43 cm
Depth: 41 cm

Cavity material Stainless steel, PTFE-plasma coated

Door Left opening door

Lighting 6x LED

Sensors

Sensor name Model

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.

Suction capacity 180 m3/h / or variable adjustable at 24 V suction


Operation temperature Continuous use 60°C / up to max. 120 °C short time
Deviation of suction Flexible tube to the exhaust port on the unit side

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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Milestone Srl MA174-003 – ETHOS EASY – User Manual

1. Carefully cut the protective belts and open


the box from above.
2. Remove the packed parts.
3. Lift the box up and away.
4. Remove any eventual additional
packaging.
5. Slightly tilt the unit forward, until you can
reach the instrument’s back side.
6. Take the microwave unit with one hand
on the front handle and with the other one on the
unit back bottom. Lift it in twos from the box.

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.

Installation of the unit

• The device must be operated only in an upright position on its foot


• The operation must be carried out only under the following ambient conditions:
• Indoor
• Max. altitude 2000 mt.
• Temperature range 5°C-40°C
• Relative humidity: 25 % up to 80 %
• Voltage fluctuation in the main power supply should be inferior to ±10% of the nominal value.
• On the device housing there are several ventilation openings serving for internal components
cooling. The ventilation openings must not be obstructed.
• The back side of the ETHOS EASY must be at least 10 cm away from a wall, because there are
connected cables there. Please be careful that there is free air access through the ventilation
openings on the unit back.

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.

Installation of the angular item

3.5 Connections

Back panel ports

Microwave back side connections

MAIN Power Supply

COM port Control connection 24 V for external devices operation via relay box

Fuse 0.5AT Fuse (500 mA, carry) heating trafo 250V

16A 2 pieces reversible main fuses

TERMINAL RJ45 port for the connection with the control terminal (RJ45 cable)

VIDEO 1 Output video signal for camera

VIDEO 2 Output video signal for camera (optional)

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TERMINAL T480 ports

Connections front side terminal 480

Terminal Model T480, 4.3’’ – Color – Touch Screen

USB 1 USB port for Service updates

Connection to Ethos EASY unit


Cable required: RJ45 with following scheme

PIN SIGNAL
Device port (RJ45) 2 RxT (In)
5 GND
6 TxD (Out)

Connecting the unit to the T480 terminal


1. Connect the microwave unit to the power supply via the power cable. Check that the main
switcher on the front side is set to OFF position.

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

Device connection Terminal connection

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3.6 Microwave door

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.

Emergency opening of 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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To open the door after a black-out, there is a


hole with blind stopper in the housing on the
right unit side.

For emergency release, remove firstly the blind


stopper.

Introduce the touch-pen ca. 3,5 cm in the hole


and press it down. Thereby a lever is activated
inside the unit and the door is unlocked. Keep the
touch-pen pressed and at the same time open
the microwave door.

3.7 Upper flange

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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3.8 Milestone logo with backlighting


The frontal Milestone logo change color giving information about the status of the system.
Below is a list of color codes:

White: The device is ready to start

Yellow: Software/system is not ready to start

Red: Microwave program is running


Red - flashing: Device in error state, or software
in setup

Blue: Cooling after the digestion program

Green - flashing: Microwave program is


completed

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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.

Temperature measuring in microwave with solvents

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.

4.2 Rotor setup/Sensor configurations

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)

4.3 easyTEMP sensor (T2)


The easyTEMP sensor is an infrared sensor that reads the vessel's internal temperature. This is possible
thanks to the special infrared frequency emitted by the sensor which is completely transparent to PTFE.
ETHOS system is equipped with two easyTEMP sensors placed on the bottom of the microwave cavity in
order to read the temperature from the bottom of vessels:

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According to the rotor configuration, ETHOS EASY microwave platform can be equipped with one or two
eT sensors:

With SK-15 (eT) rotor one easyTEMP sensor


is required (back position).

With MAXI-44 (eT) rotor two easyTEMP


sensors are required (back and left position),
one for the inner ring and one for the outer
ring.

The easyTEMP sensor read the internal temperature of all vessels, and control the microwave emission
according with the vessel at the highest temperature.

In order to have a good homogeneity of Temperature and Pressure conditions in all


vessels, it’s necessary to load the same sample type, sample amount, acids type and
acids volume.

The easyTEMP sensor start to read the temperature from 30°C. The system will not monitor the
temperature below the 30°C.

START LOAD function

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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Care and maintenance of IR (easyTEMP) sensor

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.

Cleaning of IR (easyTEMP) sensors


The recommended cleaning procedure of easyTEMP sensor housing and lenses is the following:
1. The eT sensor for SK eT rotor is located on the back side of the cavity bottom. For MAXI eT rotor
two easyTEMP sensor must be used (one on the left and one on the back side of the cavity
bottom).

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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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.

EasyTEMP Calibration Test instructions

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.

eT Calibration Test procedure (SK-15 eT rotor configuration)

For the calibration test, a single SK-15 vessel


is used.

Fill the vessel with 30 mL of DI water.

Insert the vessel into the safety shield and


place it into the segment.
The vessel must be used without cover.

Place the rotor body into microwave cavity.

Place the segment into the rotor (Pos.1).

Close microwave door.

Enter the software library and select “eT-


Test” method from “Cleaning” application
folder.

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eT-Test method.

Start the MW program.

When the temperature stops increasing,


despite continuous microwave emission, the
boiling point of the solution is reached.

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.

eT Calibration Test procedure (MAXI-44 eT or multiple rotor configuration)

For the calibration test, a single MAXI vessel is


used.

Fill the vessel with 30 mL of DI water.

Place the threaded cover on the vessel, without


the TFM valve (open vessel conditions).

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Left-positioned eT sensor (MAXI external ring)

Place the vessel into the external ring of the


rotor (i.e. Pos.1).

Place the rotor into microwave cavity.

Close microwave door.

Enter the software library and select “eT-Test”


method from “Cleaning” application folder.

eT-Test method.

Start the MW program.

When the temperature stops increasing,


despite continuous microwave emission, the
boiling point of the solution is reached.

Back-positioned eT sensor (MAXI internal ring)

Place the vessel into the internal ring of the


rotor (i.e. Pos.23).

Place the rotor into microwave cavity.

Close microwave door.

Repeat the test above.

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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.

eT protection cover (SL0239C)

If used, eT protection cover conditions must be


periodically checked and, in case, it must be
replaced.
To check the conditions of eT protection cover,
repeat the eT calibration test (explained
above), placing the cover on eT sensor.
If both tests, with and without cover, are
passed, the cover is in good conditions and it
can be re-used.
In case the test with cover fails, the protection
cover must be replaced with a new one.

4.4 ATC-CE-400 Thermocouple sensor (T1)


ATC-CE-400 sensor can be used to control the temperature with high pressure rotor such as SK-15 rotor.
The sensor is coated with PTFE and it’s additionally protected by a coated ceramic thermowell.
The sensor tip is pulled in the thermowell by the cover and then fixed. The sensor tip can rotate in the
thermowell and therefore is subjected to very low mechanical stress during the rotor movement.

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.

• The limit values of the ATC sensor must be absolutely observed.

Technical data and limit values of the ATC-CE

Linearized measuring range according to DIN IEC 584-1 from 0 up to


Measuring range:
1100°C

Short term (< 3 minutes) 310°C (PTFE boundary specs)


Limit values:
Routine load (lower rate) up to 50 bar at up to 270°C

Temperature accuracy: ± 1 K over the measuring range by multi-points linearization

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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.

1. Fix very well the adapter into the segment


screw.
Introduce the temperature sensor in the
thermowell through the hole in the screw
of the reference segment.
The temperature sensor must be
fixed in the central hole of reference
vessels.
If the sensor slips out of the
reference vessel during microwave
operations, the microwave program
must be absolutely interrupted. If
the sensor tip is no longer inside the
thermowell, it is no possible to
guarantee a correct measurement of
the internal temperature.

2. Fix the sensor, by slightly pushing the


fixation adapter into the screw of the
segment.

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3. Remove the protection cover and unplug,


if present, the jumper of the ATC-400
from the sensor connection in sample
chamber.

4. Place the rotor on the drive coupling in


sample chamber.
See more details on the rotor user
manual.

5. Connect the sensor to the plug of sample


chamber. Bend the temperature sensor as
shown by the previous picture.

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.

Operation and safety instructions

▪ 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.

4.5 IR-TC (infrared sensor)

The IR-TC contact-less temperature control measures


the infrared heating radiation from vessels or
protection shields.
When measuring the infrared warm radiation from a
body, the measuring depends on the following factors:
▪ Emission factor of the material
▪ Surface nature
▪ Body distance and dimensions
▪ Body geometry

IR-TC-Sensor

IR-TC rotor configuration Temperature control mode


Maxi 44 Direct temperature control (T2)
SK15 Safety temperature monitoring (T2)

Optimal use of IR control as addition to ATC temperature of the reference


vessel (SK-15 rotor).

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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4. Set only the limit value for the outside temperature.


5. Save the optimized method and use it in the routine.

On the right, you can find a typical ratio indoor-outdoor temperature.


In case the outside temperature reaches the limit value, you should not
set a major limit value. Possible reasons are:

▪ Vessels absorb different microwave (see vessel maintenance in


the rotor manual)
▪ Defective reference vessel
▪ Different samples

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.

Operation and safety instructions with IR-TC

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.

Care Instructions of IR-TC

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.

4.6 Pressure sensors


Pressure sensors allow automatic monitoring of vessel internal pressure during program execution.
The pressure is influenced by the temperature and the amount of sample. Therefore it is not
possible to set up a digestion program by setting a pressure profile.

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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.

4.7 APC-100 Automatic Pressure Control (P1, Optional for SK-15


and SK-15 eT)
The pressure sensor enables the control of a microwave program by measuring the reaction
pressure in the reference vessel. The pressure sensor installed outside the sample chamber is
connected by a pressure tube to the pressure vessel.
In MILESTONE rotors the pressure development can be measured, represented and controlled
during a run by help of the pressure cover. In the terminal is set the desired max pressure value,
which should be respected by the used vessels.
The pressure tube is designed for routine operation up to 50 bar during 30 minutes. At higher
pressure it has shown an increased stress. When program above 50bar are used, an accurate
monitoring of the program run is necessary. This can occur also with the help of a Q/P-Sensor. In
addition you should choose such a power that, even in case of pressure control failure, it enables
to discard a strong pressure increase.

Technical data and limit values of the APC

Measuring range: 1 bar up to 200 bar

Accuracy: ± 1bar above the measuring range by multi-points linearization

Max. temperature load: Up to 20 minutes 280°C (indoor temperature) at pressure up to 50 bar

APC Connection

APC-Sensor for SK-15 rotor (with ATC)

APC-Sensor for SK-15 eT rotor

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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.

4. Place the pressure vessel in the rotor. After the pressure


sealing of the reference vessel, the reference segment is
positioned as the last segment on the rotation plate. Right
therefrom a position must remain free. Monoblock rotors
have a connecting passage for the pressure tube to the
rotor middle.

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.

Operation and safety instructions

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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First use of APC-100

For the first use, a test run with water should be performed as here below:
- Water volume: 10 ml
- Microwave program:

Step Time Power T2 / T1 P

1 00:20:00 1800 W 180 °C 50 bar

2 00:10:00 1800 W 180 °C 50 bar

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.

Aeration and slope of the reference vessel

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.

4.8 P2 sensor (QP, Optional)


P2 (or QP) sensor for digestion detect toxic gases in the air sucked from the sample chamber and
contribute to the working safety conditions.
The respective gas sensor is installed between the exhaust opening in sample chamber and the fan. The
gas detection is performed directly in the air flow.
When the detected gas overpasses a set concentration value, the microwave heating is stopped until the
gas concentration returns below the set limit value. In connection with the reversible overpressure valve
of the vessel, the P2 sensors enables a contact-less automatic overpressure control in all reaction vessels.
The measuring with the P2 sensors has a relative power and does not permit any measuring of gas
concentration.

Sensitivity, software setting

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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P2 (or QP-A) sensor for digestion

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).

P2-S (or QP-S) for organic solvents

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.

Operation and safety instructions

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 automatic magnetic stirring is not visible under the


sample chamber bottom plate. It’s composed by a
turntable disk, where two permanent magnets are
secured one opposite to the other. The disk can be
moved with variable speed. The magnetic poles in the
vessel placed in the sample chamber receive the rotation
impulse of both permanent magnets.
The magnetic stirring is controlled in the terminal.

Principle of magnetic stirring

People with pace-maker


Inside the sample chamber there is a value of magnetic field multiple than the max.
limit (0,5 mT in frequency range 0 up to 1 Hz) for people with pace-maker.

The magnetic field inside the sample chamber can cause damages for example to wristwatch on
wrist.

Stirring in several vessels

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).

Stirring in only one vessel

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.

Suggested stirring speed to set is between 60% - 90%

Stirring bars choice

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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6 Chemistry of digestion technique


6.1 Digestion chemicals
Wet digestion is the most common sample preparation strategy for elemental determination. Acids are
normally used once the sample must be converted into appropriate form for further instrumental analysis.
When working with samples containing a large quantity of organic compounds (e.g. food, API, raw
materials, biological tissues, etc.), wet digestion based or organic matter oxidation is the conventional
approach. For samples, whose constitution is inorganic (e.g. geological and metallurgical samples), a
dissolution step is generally used.
Both procedures are based on the use of oxidizing and non-oxidizing reagents as described in the table
below.
Table: Characteristics of common reagents used for wet digestion.

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.

6.2 Digestion reaction


Wet digestion with oxidizing acids is the most common sample preparation strategy for further elemental
determination of organic matrices. It is based on the oxidation reaction of compounds in the organic matrix
due to the action of an oxidant agent (normally HNO 3, H2O2, or their mixtures), of which HNO3 is the most
common. When the oxidant agent comes in contact with organic matter, a spontaneous and exothermic
reaction begins. Under ideal conditions, organic matter is fully oxidized to CO 2 and water, as presented in
Equation (1). The aim of this reaction is that inorganic analytes ideally shall be present in final solutions
free of any organic compound, ready to be determined by analytical techniques.

(CH2)n + 2HNO3 (aq) → CO2 (g) + 2NO (g) + 2H2O (l) (1)

Where “(CH2)n” is a general representation of organic material.


Although the oxidation of organic matter is thermodynamically spontaneous, depending on the organic
matrix and operational conditions, this reaction normally takes a long time to complete. Nevertheless, it
can be sped up by increasing the sample surface area (e.g. sample milling), applying high temperatures,
and/or increasing the acid concentration.

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.

6.3 Digestion methods and tips


A large database of methods divided by application field is included in the control software. With these
tested programs a large variety of samples can be succesfully digested.

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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Digestion quality not satisfactory:

• Optimize digestion chemicals.


• Reduce the weight.
• Increase T1 in the final two program passages in step of 10°C (when possible).
• Increase time of the last steps (when possible).
• If available, use the stirring.
• With good digestion quality, the last program step can be shortened.

P2 (QP) sensor regulates too early:

• Reduce the weight, in order to have lower gas production.


• Replace eventual defective vessel/cover etc.
• Increase heating step 1 and 2 (Temperature rising/gradient becomes lower)
• Last heating step – re-set a bit the max. temperature. There are i.e. to expect no losses for
heavy metals, if the temperature remains over 200°C for more than 10 minutes.
• Reduce the reaction speed (organic samples except for plastic!). Increase water addition.
• Reduce the HCl proportion in digestions with HNO3 / HCl.
• In case of good digestion quality, the last program step can be shortened.
• Reaching very high temperatures, add high boiling acids.
• Reasons of spontaneous reactions: recognizable, when the Q/P signal response during the first
both program steps (at low T1, i.e. below 160 °C ).
• Use correct basic program for reactive biomass.

Desired temperature curve is not achieved:

• Possible defect in the reference vessel. Please check it.


• Possible different microwave absorption due to the age (see maintenance)
• Possible digestion of too much different samples
• Extend the appropriate heating steps
• Increase the power (microwave power was not enough for your sample quantity)
• Too little total solvent amount – caution in increasing the power
• Use vessels for small volume (i.e. HPV-40)

6.4 Digestions with high boiling acids or mixtures

Direct use of high boiling acids and mixture

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.

Method development using high boiling chemicals

• 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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• Slow heating of samples with low weight and at least 10 ml liquid.


• Application requirement must be matched.
• Replace vessels with damages, i.e. if the inner surface in range of liquid level is corroded.
• Always check the vessels and develop the optimal conditions for the routine operations.
• Contact Milestone specialist for more details on your application with high boiling chemicals.

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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.

Terminal T480 ports

Terminal 480 connections – back side -

Control terminal touch-screen 4,3” TFT display, 480x272 VGA resolution with 16M
Terminal model
colors

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One USB port Connection for Milestone service tech.

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

Connecting the unit to the T480 terminal

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

Device connection Terminal connection

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Transfer of Settings between Terminal and Interface

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.

Display during start procedure

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.

8.2 General operations tip


The software operations are carried out by a touch-screen. By touching the screen, the icons or the input
field are activated.
Activated field are ready for input via a keyboard. By touching again the activated field, a numeric or
standard keyboard appears on the screen.

Numeric input via touch-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

Text input via touch-screen

For steps requiring a designation/description, a standard keyboard will appear by double-touching the
touch-screen.

Standard keyboard

Generally used icons

General Menu

Methods menu

Select - OK

Delete - Cancel

Save

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New

Back to previous page

START button

Editable fields with numeric values and defined range

• P2 limit: %
• Door locking: °C

• t (time): hh:mm:ss
• MW (power): W
• T2 (temperature 2): °C
• P1 (pressure optional): bar
• Cooling:min

• Number of vessels loaded on the rotor


plate: Number of vessels

• Background
o Red
o Green
o Blue

• Number of positions on the rotor plate:


Samp.

• 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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• Exhaust fan speed: %

8.3 Methods

Method selection from Milestone database

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).

Log-in with your administration password.


At time of the unit shipment, the password
represented here is assigned.

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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Modified method selected and/or modified by the


administrator.
This method is located as well in the category
“Recent”.

Method designed for a specific rotor not included


in your configuration.

Select a method and click the upper right icon


(check mark).

In the following registers, there are all method information and settings.

General information Setting Parameter


By clicking again the check mark, you can open and run the method.

If a method is opened by the Administrator, this


is automatically saved in the respective category
with a star and in the category „Recent“.
The methods in the category „Recent“ can be
opened and run by all operators.
By the Administrator right, the methods in the
category „Recent“ can be modified or deleted
from „Recent”.

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.

If you open a method already included in the


category „Recent“, a warning message is
displayed.

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If you confirm this window, the method is


overwritten and therefore it replaces the original
one in „Recent“.
If you don’t want to modify the original method,
quit this interface window. Open „Recent“ and
assign a different name to the method. In this way
you can open the original one without rewriting
the original data in „Recent“.

Create new methods

Press the upper left check mark and select the


icon method.

Log in as Administrator, in order to create a new


method.

If you are already logged as Administrator


(21CFR-11 password) you will be directly
addressed to the method page

Log in with your Administrator password.

To create a new method, click on the showed


icon in the upper right side of the screen.

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General information

Select the type of application and the application


field. The method will be saved in the
corresponding folder of the library.

Enter the name for the new method.

In the Note box you can specify further info


concerning the method (i.e. sample amount,
acids, etc…).

Double-click in the editable fields to access


the keyboard.

Parameters

Edit the setting for the new method.


Unlock (turn to green colour) the parameters that
have to be monitored. The shaded parameters
cannot be changed.

• T1: Internal temperature, thermocouple


sensor
• T2: External temperature, Infrared
temperature sensor
• P1: Pressure sensor
• P2: Contactless pressure sensor.
Electronic sensor sensible to the presence
of NOx and Cl2 in the cavity.
• Twist: Rotor movement (changes
direction after 360 ° or continuous in the
same direction)
• Rotor ctrl: Shows the highest temperature
(leave this function always on)
• MW continuous: activate the continuous
or pulsed microwave emission.
• P2 limit: Limit of acid fume percentage
(Milestone suggests to set 80 – 90%)
• Rotor: Select the your rotor configuration
from the scroll menu.
• Vessel: number of rotor positions
• Control for: Sensor selected to control
and drives the reaction.
• Door locking: Temperature limit that
allows you to open the door.

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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

Depending on the rotor configuration, T1 and P1


may not be visible because both are optional.
Save the new method by clicking on the icon on
upper right side of the screen.

8.4 Program sequence


During the MW-cycle, the software records all data of control parameters. The gradients of temperature,
pressure and power are displayed graphically in real time on graph.
The recorded curves of temperature (and pressure) appear in darker of the given curves.
After the program, the graph can be printed or saved on the USB pen.

Program sequence

PAUSE
While the program is running, the pause icon
appears to the right.

With the pause button the process can be


interrupted (the timer is stopped and the
microwave irradiation is stopped).

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During the pause, the button changes to a split


view. Now you can continue or stop the program.

In the graph, a marker appears from the point of


interruption (at the top of the graph at the
position where it was interrupted).

The opening of the chamber door has the same


effect as pressing the pause button.

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.

It’s possible to follow the digestion run selecting


the window.
Here there are all details about the actual internal
temperature (set point and readed temperature),
external temperature, pressure, microwave
energy.

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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P2, LIGHT BLU


Curve of P2 (QP sensor) that detect venting of
the vessels by detecting the amount of NOx or Cl2
in the cavity.

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.

Load control function

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.

According to the rotor configuration, when you start


the digestion program, the software asks to indicate
the number of vessels that you are using.

With a MAXI-44 rotor, a minimum of


10 vessels must be indicated to have a
better functionality of the system.

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.

To enter the Setup menu, click on the upper left


icon of the screen and then on the settings icon
in the menu.
Here you have to log with the administrator
password.

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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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Maximum working conditions


These limits can only be set by Service.

Sensor settings
These settings can only be edited by Service

Control settings
These settings can only be edited by Service

Cavity control system (CCS)


The settings of the cavity control system (CCS)
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.

The administrator can at any time reset the


countdown.

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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

The below parameters can be modified only by a Milestone service engineer.

8.6 Create, Edit, Delete a User profile

First Steps

When the unit is turned on, the system will ask


for the first access.
The first login MUST be done by the administrator
of the lab and the default password is 123456.

The default password MUST be


changed after the first login. It’s
responsibility of administrator to
change the default password with a
new one. See the next chapters for
more details on how to change the
password.

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Select the arrow at the top left of the screen and


open the settings page.

Select the Terminal > Users window in order to


get access to the Users list. From this page it is
possible to Create, Edit or Delete a user profile.

Overview of user profiles and access levels

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.

Login type General Description Access level

Can only open files selected by


the administrator. The user
User Low
cannot modify any parameter of
the method.

Can create User and Manager


Manager profiles. Can open and modify the Medium
methods.

Can create User, Manager and


Administrator profiles. Can open
and modify the methods.
Administrator High
It have access to the time and
data of the software and other
technical options.

Here below a table with more details concerning the privileges according with the login type

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Open and Modify existing


Open and run
Run a methods (not Create a new
a method from Create a new
method from the one from Administrator
thedigestion Method
the Recent the Milestone account
Library
folder library)

User     

Manager     

Administrator     

Accessories Create a new


Power test Sensor check Create a new
Setup (Rotor Manager
window settings User account
configurations) account

User     

Manager     

Administrator     

There are two additional login levels that cannot be modified by the Administrator.

Login Type General Description Access level

This access is only for the Milestone


Service Engineer.
Service High
It gives access to the sensor calibration
and others technical feature of the unit.

This access is for Milestone Producer for


Supervisor software optimization (engineering, High
updates, etc.).

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Create a new ID user profile

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.

For the above reasons, Milestone suggests to:


• Mandatorily use name and surname of each users as ID Username.

User name and


surname

• 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.

Open the scroll menu on the upper left side of the


display and select “Settings”.

Select “Access” page and “Users” tab.

Create a new user changing the password.

Press to add new User

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Insert Username, privileges and password.

The password must be at least 6


characters long

Go back to the Main page and log out

Edit or Delete an existing ID user profile

Open the scroll menu on the upper left side of the


display and select “Settings”.

Select “Access” page and “Users” tab.

Select the user to edit or delete from the list.

1. Press to edit existing User

2. Press to delete existing User


Pressing the edit function you can change the
privileges and the login password

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Pressing the delete function a message will appear


for confirmation. Press YES to remove the account.

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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.

Following are all the steps to access the Milestone Connect.

Open the internet browser of your PC and type


the following address:
www.milestoneconnect.com

Choose the section concerning your instrument


configuration.

As first login, use the Username and password


that you have on the Milestone connect ID card
attached to the “Getting start guidelines” of the
system.

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Fill the form with all information and change the


username and password with a new one.

After the login you have the access to the


Milestone connect where you can find important
information about your system, accessories and
applications.

Scrolling down the page of the site you will find


different categories:

Here you can find personal


information, warranty and
configuration of your unit.
Here you can find news about
info and products connected to
the ETHOS UP unit.
Here you can find application
notes and scientific papers
divided by application field.

A collection of easy video


tutorials that describe the use of
the system.

This button will automatically


connect the browser to the main
page of the terminal, so you can
monitor your run and, if
necessary, stop it.
This function is only available for
Ethos UP configurations and not
for Ethos EASY
You will find the contact details
of Milestone local representative
and Milestone Team.

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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10 Messages and inquiries

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.

Messages are acknowledged by pressing the OK


button.

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

10.1 List of queries and (error) messages


In this chapter, most queries and (error) messages and their meanings are listed. They are sorted by the
following keywords:

• Login

• Sensors, Settings and Twist

• 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.

Sensors, Settings and Twist

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?

Twist error No change of direction of rotation is detected by the system.


A twist error occurred. Check the twist mode Check the twist function or contact service.
of your
system.

Program

Text Meaning / Comment


You have already executed a microwave application You have not saved the program file. During a restart, all
without storing these data. unsaved data of the last run will be lost.
Do you want to ignore the recordings and load a new The program file can be stored in the sequence register.
method file?
No program is selected. You have not yet defined a program. In the register
method \ program allows you to create a program or load
Please enter a valid program or select a from disk (see Chapter program).
predefined method.
Your microwave program is longer than 2 hours. In all applications, an examination of the length of the
Is it correct? program takes place. With a length of more than 2 hours,
this prompt appears. The program is not limited to 2
hours.
You have already executed a microwave application The method and sample table are stored with the
without storing these data. Do you want to ignore the program file. When loading a sequence, the current
recordings and load a new method file?

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Text Meaning / Comment


method, sample table and chart the course will be
overwritten.

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11 APPENDIX 1 – Analytical index of software


screens

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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

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