Milestone ultraWAVE 3 User manual

ultraWAVE 3
Operator Manual
MA245
MILESTONE
HELPING
CHEMISTS

Milestone Srl MA245-003 –ultraWAVE 3 –User Manual
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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 carefully read 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 [phone]
Fax [phone]
Website www.milestonesrl.com
E-mail [email protected]
The instruments commercialized by Milestone are intended for the use in strict compliance with
all applicable laws and in a manner that promotes public safety and/or linked to approved
scientific or medical research purposes.
Milestone does not endorse, encourage or promote the use of its instruments for any illegal
activities.
No liability for any consequences, direct or indirect, is accepted if the ultraWAVE 3 is used in
any way in which the instrument is not intended to be used.
Pubblication date (dd/mm/yyyy) 27/09/2023

Milestone Srl MA245-003 –ultraWAVE 3 –User Manual
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1QUICK START - START USING YOUR
ULTRAWAVE 3.........................................................9
Switch on and login............................................................9
Closing and starting of the system ......................................9
Set a Program ................................................................. 10
Pressure load................................................................... 11
Open the system ............................................................. 12
Maintenance after each run .............................................. 13
2WARNING FOR SAFE OPERATION OF
MILESTONE MICROWAVE UNITS..........................14
Symbols used in this manual ............................................ 14
Do not use the system unattended ................................... 14
High temperature - long reaction times ............................. 14
Type of materials............................................................. 14
Type of reagents ............................................................. 14
Metal parts ...................................................................... 14
Cleaning.......................................................................... 15
Service............................................................................ 15
Safety ............................................................................. 15
Basic rules of microwave chemistry................................... 16
ultraWAVE 3 –chemistry guidelines .................................. 17
3SAFETY RULES...............................................18
General Information......................................................... 18
Safety Rules for Start-up .................................................. 18
Safety in operation........................................................... 18
Safety in Service Operation .............................................. 18
No Manipulations of the unit allowed................................. 19

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Replacement of Parts ....................................................... 19
Other Hints...................................................................... 19
Safety of operation.................................................................................. 19
Pressure Parts ........................................................................................ 20
Observance of safety regulations.............................................................. 21
Placement and movement of the unit........................................................ 21
Definition of personnel skills and capabilities ............................................. 21
How to operate with the unit ............................................ 21
Operate according to Milestone Applications.............................................. 21
Synthesis of liquids.................................................................................. 21
Digestions with aggressive Chemicals e.g. acids, caustic solutions, etc......... 21
Do not use gas phase digestion applications.............................................. 22
Base load and gas loading pressure.......................................................... 22
Aggressive Media .................................................................................... 22
Pre-loading Pressure ............................................................................... 22
Spontaneous reactions ............................................................................ 22
Pressure line........................................................................................... 22
Care and Maintenance............................................................................. 23
4DESCRIPTION OF THE SYSTEM .....................24
Unpacking/Check-list........................................................ 24
Installation site ................................................................ 24
Technical Specifications.................................................... 24
Unit ....................................................................................................... 24
Pressure Vessel....................................................................................... 25
Cooling water ......................................................................................... 26
Instrument Sensors................................................................................. 26
Proximity sensors for lifting system........................................................... 26
General Information ................................................................................ 27
Microwave Heating.................................................................................. 27
Description of the ultraWAVE 3 ports and connections ....... 28
Front view .............................................................................................. 28
Operating elements and connections on the back panel ............................. 29
Exhaust system....................................................................................... 30
Emergency vent valve ............................................................................. 30
UltraWAVE 3 built in touch screen terminal........................ 31
Description ............................................................................................. 31
easyCONTROL ........................................................................................ 31

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Transfer of Settings between Terminal and Interface ................................. 32
5SENSORS AND ACCESSORIES .......................34
Temperature Sensors ....................................................... 34
Pressure sensor ............................................................... 34
Overpressure protection .......................................................................... 34
Position Sensors .............................................................. 34
Recirculation water chiller................................................. 34
Recirculation water chiller installation ....................................................... 35
Gas filter ......................................................................... 36
6PRESSURE LINE INSTALLATION ...................38
Connection of ultraWAVE 3 to the Nitrogen or Argon gas line
38
Direct connection to the gas cylinder................................. 38
Pneumatic Booster (Optional) ........................................... 41
Installation of the Pneumatic booster (optional)......................................... 42
Setup of the pneumatic booster ............................................................... 44
High pressure compressor (Optional) ................................ 45
Installation of the High-pressure compressor............................................. 46
Setup of the High-pressure compressor .................................................... 49
Employment of a longer supply line .................................. 49
7FIRST USE AFTER INSTALLATION.................50
Check-up before first start................................................ 50
Switch-on the ultraWAVE 3............................................... 50
Opening of the cover ....................................................... 50
Pre-conditioning of ultraWAVE 3 before the use................. 52
8ULTRAWAVE 3 OPERATION...........................53
Sample handling and weighing ......................................... 53
Samples tray ................................................................... 55

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Acid mixtures................................................................... 55
Addition of Reagents........................................................ 57
Addition of base load in the main PTFE vessel ................... 57
Handling of sample rack................................................... 59
Locking of clamps ............................................................ 60
Pressure load before the microwave run............................ 61
Microwave run................................................................. 62
Pressure release after microwave run................................ 62
Opening of reactor after digestion run............................... 63
System status indicator .................................................... 64
Emergency Stop of UltraWAVE 3....................................... 65
9MAINTENANCE AND CLEANING PROCEDURES
67
Cleaning after each run .................................................... 67
Cleaning of reactor and checking of the main PTFE vessel .......................... 67
Cleaning of reactor and cover with protective oil and grease
69
How to apply the PFPE grease with anticorrosion additive........................... 70
NOx decontamination of the main PTFE vessel .................. 71
Cleaning before long operational Breaks............................ 71
Cleaning of the metal cover.............................................. 72
Cleaning instructions in case of spilt acids ......................... 73
Vessel Covering ............................................................... 75
Leak Test of the main reactor ........................................... 75
Measures in case of fast pressure release.......................... 76
Maintenance of High-pressure compressor (optional) ......... 76
Check Oil Level ....................................................................................... 76
Condensate draining................................................................................ 77
10 EASYCONTROL SOFTWARE............................78

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Program start .................................................................. 78
General Operation tip....................................................... 79
Graphic color .......................................................................................... 79
Numeric input via touch-screen ................................................................ 80
Text input via touch-screen .............................................. 80
Editable fields with numeric values and defined range........ 81
Generally used icons ........................................................ 83
Methods .......................................................................... 86
Method selection from Milestone library .................................................... 86
Create new methods ............................................................................... 88
How to start a microwave program ................................... 90
Opening of the reactor when the microwave program has
finished ..................................................................................... 93
Open the front cover........................................................ 94
Program sequence ........................................................ 94
Run file opening / saving / deleting .......................................................... 96
Graphical representation.......................................................................... 97
Sample table................................................................. 98
Open new sample table ........................................................................... 98
Adding lines.......................................................................................... 100
Delete record........................................................................................ 100
Direct connection with balance............................................................... 101
Automatic tare...................................................................................... 101
Enter Chemicals .................................................................................... 101
Sample Table open / save / delete ......................................................... 102
System PAGE .............................................................. 103
SETTINGS................................................................... 105
Terminal page ...................................................................................... 105
Settings page ....................................................................................... 107
Other setup windows............................................................................. 110
11 21CFR –PART 11 SOFTWARE......................112
Activation of the 21CFR –part 11 ................................... 112
Create, Edit, Delete the User Profiles............................... 113

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First Steps ............................................................................................ 113
Overview of user profiles and access levels ............................................. 114
Create a new ID user profile .................................................................. 115
Edit or Delete an existing ID user profile ................................................. 119
Switch on the unit and create new microwave method..... 120
Save and export the final digestion temperature profiles .......................... 123
How to save a temperature digestion profile............................................ 124
Files format and auto-save option (Administrator, Service)124
Continuous recording ............................................................................ 125
Save of the run file................................................................................ 125
The Audit Trail............................................................... 126
12 MILESTONE CONNECT .................................128
13 LIST OF QUERIES AND (ERROR) MESSAGES
130
Login ............................................................................ 130
Sensors, Settings and Twist............................................ 130
File and Data ................................................................. 131
Program ........................................................................ 132
Sample table ................................................................. 132
Internal memory, disks and signature ............................. 132
14 ULTRAWAVE 3 CLEANING PROCEDURE ......134
15 APPENDIX 1 –ANALYTICAL INDEX OF
SOFTWARE SCREENS ..........................................137
16 APPENDIX 2 - DECLARATION OF COMPLIANCE
"EASYCONTROL SOFTWARE" WITH FDA-
21CFRPART11 .....................................................144
17 APPENDIX 3 - TIPS & TECHNIQUES ............151
Applications................................................................... 151

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Standard base load ............................................................................... 151
Microwave program guidelines ............................................................... 151
Cleaning/ Maintenance ................................................... 152
Maintenance of the PTFE vessel ............................................................. 152
Protective oil or grease.......................................................................... 152
Cleaning before long operational breaks.................................................. 153

Milestone Srl MA245-003 –ultraWAVE 3 –User Manual
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1QUICK START - START USING YOUR
ULTRAWAVE 3
Milestone UltraWAVE 3 can operate with a wide range of racks and vials type; here a fast description of
the most important operation steps. The complete description of the procedure is fully described into the
ultraWAVE 3 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).
Switch on and login
Turn the main switch of the UltraWAVE 3 on „I“. Wait few seconds until the touch screen terminal turns
on and the software is ready to operate.
The UltraWAVE 3 is ready to work and it shows the last method used
Closing and starting of the system
Fill- the big PTFE-vessel with the base load of 150 ml H2O + 5 ml HNO3 (base load could be different
according the application note) and place it inside the ultraWAVE 3 stainless steel cavity.

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Weight the sample, add the reagents according to the application note and close the vials with PTFE
covers.
Warning!
Keep your hands away from the reactor when the steel cover is closing
Set a Program
Select a recent method or choose one from the application library.

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Only the administrator has access to the Milestone library. After selecting the method, you have to be
logged in (as administrator) to load and run it.
Press start on software and follow the instructions on the terminal screen to close the reactor.
To close the clamps simply tight the locking screw until the “clamps ears” overlaps
Pressure load
Check that the pressure regulator is open and adjusted to the correct pressure.

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The system will automatically start the gas loading into the reactor to reach the initial set pressure
(usually 40 bar).
Open the system
After the run, the system automatically cool down the solutions, releases the pressure from the reactor
and run the flushing of the pressure line.
A message on the terminal and the green light indicate that the unit can be opened.
Follow the instructions on the terminal to complete the opening of the reactor.
Remove the rack and place it on the rack-holder to recognize positions and easily remove the vials.
Transfer the solutions to volumetric flask for final dilution.

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Maintenance after each run
•The base load must be replaced every run and the PTFE vessels must be removed from the
cavity.
•Dry very well the steel cavity (inside and outside) and the clamps. Clean them using Ethanol.
•Before turning off the unit, it is recommended to grease all the steel part of the reactor using a
small amount of oil or grease provided with the unit.
More detailed information concerning the operating steps and the maintenance can be found into the
next chapters of ultraWAVE 3 user manual.

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2WARNING FOR SAFE OPERATION OF
MILESTONE MICROWAVE UNITS
Symbols used in this manual
An instruction accompanied by this symbol provides a cautionary statement:
WARNING. Failure to follow the instruction may endanger the user or cause damage
to the instrument.
Information = indicates important information/recommendations for the user.
Warning means that the non-observance of the warning may cause injuries, even
severe, to people.
Do not use the system unattended
Never leave the microwave labstation unattended during operation. Microwave labstation must always be
closely monitored during the process, especially during high temperature processes (above the boiling
temperature of the solution).
High temperature - long reaction times
High temperature processes during prolonged times can cause damage to the vials as well as to the reaction
vessel and its components. There are accessories suitable for working at high temperatures and for long
periods of time. Always consult the application book and if in doubt, contact your dealer for advice.
Type of materials
Matrices with a low flash point must be treated with special attention to avoid the auto ignition and eventual
damages of the vials. Always consult the application book and if in doubt, contact your dealer for advice.
Type of reagents
Always consult the safety data sheet of the reagents to take the necessary precautions according to their
specific properties. Some reagents have explosive properties and their use is not recommended.
Metal parts
Never insert metal objects into the reaction chamber (except those that are samples to digest). High
voltage discharges can occur causing uncontrolled temperature increase that may damage the
equipment.

Milestone Srl MA245-003 –ultraWAVE 3 –User Manual
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Cleaning
To ensure safe use of the equipment and to extend its service life, always follow the cleaning and
maintenance instructions described in this manual. The cleaning and care of the parts are indicated with
the recommended periods (i.e. every cycle, every week, every month) are necessary to keep the
equipment in perfect conditions of use and safety.
Service
To operate under safe conditions and to avoid any danger or risk of accidents, the following rules must
be strictly followed:
1. Always disconnect the unit from power supply before any repairs
2. Before switching the unit on after every repair, it is necessary to make sure that:
•all internal connections are correctly soldered
•all cables are insulated and do not come into contact sharp edges of the unit
•both the electrical and mechanical connections are virtually faultless
•no modifications have been made to the built-in service devices
•the spare parts are those required by the manufacturer
Warning!
Do not operate the unit if the slightest doubt exists that it may not working properly
In case of damage to the unit, call for a trained Service Engineer immediately and do not operate the unit
until repaired. The unit can be serviced and opened exclusively by a properly trained service engineer.
Warning!
High voltage present when opening the cabinet.
Safety
Your personal safety is of the utmost importance for us, therefore, the precautions necessary to perform
chemistry under these conditions must be strictly followed. All persons involved in the use of this equipment
must read the following precautions.
•External fire protection should be installed according to local regulations for equipment operating
unattended.
•If materials inside the equipment should ignite, keep the cavity closed, switch off the equipment
and disconnect the power cord or turn off the power at the fuse or circuit breaker.
•Do not insert metal objects of any kind into the cavity (except of samples), as arc welding and
uncontrolled temperature increases may occur.
•It is inadvisable to use some reagents (i.e. triethyl orthoformate) in high temperature microwave
chemistry because of the risk of explosion associated with their chemical properties. Please consult
MSDS data sheets for the specific properties of each chemical before use.
•Reactions in which there may be a risk of explosion or that are extremely exothermic should not
be performed with the system.

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•The system is a closed vessel system; specific precautions have to be applied to reactions or
reagents that release gases, e.g. decarboxylations or ammonium hydroxide, respectively. Low
concentrations and temperatures are recommended for this type of reaction.
•Chemicals whose behaviours are unknown when exposed to microwave heating must be treated
with caution e.g. test the reaction at lower temperatures and lower concentrations, use shorter
reaction times and perform the reaction in a fume hood with the window closed.
•Chemicals that absorb microwave energy well and that are not mixed properly in the reaction
mixture may cause damage to the process vial. Examples are palladium on carbon or
polyphosphoric acid. These chemicals can melt the vial if present on dry pieces adhering to the vial
wall outside of the reaction mixture.
•The equipment shall not be used for heating and ventilation of laboratories. The equipment shall
not be used as a sterilizing equipment.
•The equipment shall not be used as a medical electrical equipment. The equipment shall not be
used for heating food and beverages. The equipment shall not be used for mass production. The
equipment shall not be used in an explosive atmosphere.
•The equipment shall only be operated indoors, where the altitude does not exceed 2,000 meters
(1,242 feet), at temperatures between +5°C and +40°C +(41°F and +104°F). The maximum
relative humidity is 80% for temperatures up to 31°C (87.8°F) decreasing linearly to 50% relative
humidity at 40°C (104°C).
•The equipment shall be operated in places where fluctuations of the main supply voltage are not
exceeding values of 1.10 times the nominal voltage and are not below 0.90 times the nominal
voltage. The equipment shall only be operated in places where transient overvoltage on the main
supply are not exceeding values of overvoltage category II specified in IEC 60364-4-443.
•The equipment shall only be operated in places where normally only non-conductive pollution
occurs and occasionally, however, a temporary conductivity caused by condensation may occur.
•The equipment shall not be stored or operated in places where special conditions prevail, such as
the presence of a corrosive or explosive atmosphere (dust, vapour or gas).
Basic rules of microwave chemistry
The basic rules of chemistry also apply in a microwave field. The conditions outlined in the Milestone
applications books describe optimized microwave processes for particular materials. The procedures in
Milestone applications books are only guidelines. Please refer to your local Milestone Application Specialist
for any modifications or suggestions.
Basic rules are described below:
•The maximum acid volume should always be 50% -60% of the total volume of the vial.
•The minimum volume is one that keeps the sample soaked and submerged.
•Be sure to use the appropriate volume according to the type of vial and / or sample.
•Use the appropriate vial depending on the type of reagent.
•To prevent hot spots, the samples must be completely wet by the acids.
•If, during the addition of the acids an exothermic reaction occurs or foams are formed, add these
drop by drop, use dilute acid or add a little amount of water and mix using a Vortex system.
•Periodically check the condition of the reaction vessel, cover, vials and o-rings.
•When adding water to the digested samples, do it carefully and consider the reagents used.

Milestone Srl MA245-003 –ultraWAVE 3 –User Manual
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Read the operator manual before using the instrument!
ultraWAVE 3 –chemistry guidelines
UltraWAVE 3 is suitable for the digestion of any kind of samples with any kind of acid mixture.
The most common acid mixtures used in the ultraWAVE 3 are reported below:
•HNO3
•parts of HNO3, 1 part of HCl, 1 part of H2O
•HCl, Aqua regia
•Mixture of HNO3and HF
•Mixture of HNO3, H3PO4, HF
•Mixture of HCl, HF, H3PO4, H2O2
A wide variety of samples can be digested in the ultraWAVE 3, below are reported some guidelines:
Sample type
Suggested acid mixture
Organic samples.
Only HNO3
4 ml of HNO3and 0,5/1 ml of HCl
General inorganic samples
Reversed Aqua Regia (3 ml of HNO3, 1 ml of HCl,
1 ml of H2O)
Samples with high concentration of Fe, Al,
Sb, Sn and noble metals
Reversed Aqua Regia (3 ml of HNO3, 1 ml of HCl,
1 ml of H2O)
Alloy, Steel and Ores
Reversed Aqua Regia (3 ml of HNO3, 1 ml of HCl,
1 ml of H2O) only HCl
Mixture of HNO3and HF
Rocks, cement, ash
Mixtures of HNO3/ H3PO4/ HF
The UltraWAVE 3 can be used only with methods/ procedures agreed with
Milestone Application Specialist.

Milestone Srl MA245-003 –ultraWAVE 3 –User Manual
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3SAFETY RULES
General Information
•Carefully read 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, also carefully read the
instruction manuals of such accessories.
•Follow particularly the recommended instructions for Service and Maintenance.
•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 ruling national 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.
Safety Rules for Start-up
First start-up of the system must exclusively be carried out by authorized and trained service / application
engineers appointed by Milestone.
Safety in operation
•Pressure vessel may only be opened once the user has made sure –by looking at the operating
pressure display in front of the unit –that there is no more pressure inside. The pressure sensor
alone has not to be considered as a sufficient safety device.
•The ultraWAVE 3 must exclusively be operated for its intended use.
•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.
•The unit must be operated only for applications released and recommended by MLS-Milestone.
•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 takes all those safety measures that are
usually required (e.g. lab coat, protective gloves, protective glasses mask, exhausts hood, etc.)
Safety in Service Operation
•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 pressures up to 200 bars can be reached.
•The unit includes components in which lethal high voltage of 4kV can be reached.