Sairem

tel : +33 (0) 4 72 01 81 60

82 rue Élisée Reclus
http://www.sairem.com
69150, Décines-Charpieu, FRANCE

User Manual

MODEL MicroChem System & OPTIONS

MODEL DESCRIPTION 2.45 GHz MICROWAVE GENERATOR + CAVITIES

INDEX 2

THIS MANUAL PROVIDES INSTRUCTIONS AND RECOMMENDATIONS

FOR USE. TO BE STORED FOR FUTURE USE

© Sairem 2024. All rights reserved

 MicroChem System & OPTIONS

Product Specifications

TECHNOLOGY MicroWave (solid-state)

100-260 V
SUPPLY VOLTAGE Single phase AC
50-60 Hz

POWER SUPPLY 690 VA

OPERATING
adjustable: 2 400 to 2 500 MHz (100 kHz step)
FREQUENCY
MICROWAVE POWER 0 to 200 W (1 W step)
4% stability at start up
POWER STABILITY
2% stability after 40 min
RIPPLE RATE <0.2% RMS at nominal power

POWER RISE TIME <1 ms (Rise time & fall time)

Adjustable maximum value up to 100 W
REFLECTED POWER
Limited to 70 W after 2 min
Fiber optic probe: -40 to 200°C (standard)
wider range available on request
TEMPERATURE
MEASUREMENT
Compatible with pyrometer (external sensor input)
range of pyrometers available on request
Generator 400 × 220 × 342 mm
DIMENSIONS
S-Cavity 220 × 200 × 272 mm
(L X W X H)
M-Cavity 287 × 210 × 289 mm
Generator 15.5 kg
WEIGHT S-Cavity 7.5 kg
M-Cavity 5 kg
COOLING METHOD Air cooled

PROTECTION INDEX IP20

OVERVOLTAGE
II
CATEGORY
ELECTRICAL CLASS Class 1

POLLUTION DEGREE 2
STORAGE
0 to 60°C (32°F to 140°F)
TEMPERATURE
OPERATING
8 to 32°C (46°F to 90°F), no condensation
CONDITIONS

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 MicroChem System & OPTIONS

Revision Index
Issue date
Index Author Checker Revision comments
(dd/mm/yy)
1 HMO/TGAR ADO 04/10/2022 Creation of the document
Overall update & adding the
2 TGAR/HMO ADO 28/07/2023 installation guide for the continuous
flow and the pressure options

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DANGER WARNING

ELECTROMAGNETIC MICROWAVE GENERATOR

TAKE PARTICULAR ATTENTION TO SAFETY WARNINGS

REGARDING RADIATION RISKS
CAUTION RISK OF ELECTRIC SHOCK IF NO LOAD IS
CONNECTED IN CASE OF CONTACT WITH CONNECTOR
"MW OUTPUT"

TO AVOID SHORT CIRCUIT AND RISK OF ELECTRIC

SHOCK, DO NOT USE THE GENERATOR IN A WET
ENVIRONNEMENT WHICH CAN CAUSE
CONDENSATION.

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WARRANTY
Generators are guaranteed against any manufacturing fault for one year. Where generators
include components such as tubes, triodes, tetrodes or magnetrons, guarantee of these
components is limited to the manufacturer’s warranty.

Warranty remains valid on condition that the system is operated under normal conditions and
any repairs are done either by SAIREM, on site or at the SAIREM factory, or by our local
distributors.

Warranty is limited to the cost of repair, spare parts and labour. No indemnity is given against
loss incurred due to any malfunction. Travel expenses incurred during repair are not covered
by this guarantee.

Warranty is void if seal indicator is broken without SAIREM agreement.

The user is responsible for the installation of this equipment with due regard for the risks
stemming from electromagnetic radiation.

In case of difficulties, the list of maintenance centers authorized to intervene is available from:

SAIREM SAS
82 rue Elisée Reclus
69153 Décines Cedex, France
Tel. + 33 4 72 01 81 60 (Reception)
Web: www.sairem.com
Email: [email protected]

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 MicroChem System & OPTIONS

Pictograms used in this manual

Pictogram Meaning

Electrical hazard

General risk – non-specific

Risk of non-ionizing radiation

Caution hot surface

Precaution, read the manual carefully

Reading the manual is recommended

Wear protective gloves

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Glossaries of acronyms and abbreviations used in

the manual
The abbreviations and acronyms appearing in this manual are presented in the following table

Acronym Meaning Definition

MW Microwave

P Power

FP Forward power Power output of the generator

RP Reflected power Power returned to the generator

TP Transmitted power Difference between FP and RP

Estimation of the power absorbed by the product from the

AP Absorbed power
TP and the system losses (entered by the user)
Programmable Logic
PLC
Controller
Human Machine
HMI
Interface
Personal Protective
PPE
Equipment

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 MicroChem System & OPTIONS

TABLE OF CONTENTS

Product Specifications ...................................................................................................................... 3

Revision Index .................................................................................................................................. 5

DANGER WARNING .......................................................................................................................... 7

WARRANTY ....................................................................................................................................... 8

Pictograms used in this manual ....................................................................................................... 9

Glossaries of acronyms and abbreviations used in the manual ..................................................... 10

TABLE OF CONTENTS ...................................................................................................................... 11

1. SAFETY RULES ........................................................................................................................ 13

General precautions ...................................................................................................... 13
Qualification of personnel ............................................................................................. 14
Electromagnetic precautions ........................................................................................ 15
Approved operating conditions for cavities .................................................................. 16

2. PRESENTATION ...................................................................................................................... 17
MicroChem line ............................................................................................................. 17
MicroChem connectivity overview ............................................................................... 18
Useful definitions .......................................................................................................... 19
Cavity tuning.................................................................................................................. 19
Forward, reflected and absorbed powers..................................................................... 20

3. INSTALLATION & OPERATION..................................................................................................... 21

Installation ..................................................................................................................... 21
Positioning of the generator ......................................................................................... 21
Connections ................................................................................................................... 21
Remote control.............................................................................................................. 27
Connecting..................................................................................................................... 27
Main controls ................................................................................................................ 28
Program Tab .................................................................................................................. 29
Cycle configuration........................................................................................................ 31
AutoPID ......................................................................................................................... 32
Faults Tab ...................................................................................................................... 33
Scan tab ......................................................................................................................... 34
Configuration Tab .......................................................................................................... 34
Starting and operating .................................................................................................. 36

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 MicroChem System & OPTIONS

Cavity installation........................................................................................................... 36
Power operation and taking out of the sample ............................................................. 47
Status indicator .............................................................................................................. 48
Stop Button .................................................................................................................... 48
Cavities tuning................................................................................................................ 49
MicroChem S-Cavity....................................................................................................... 50
MicroChem M-Cavity ..................................................................................................... 52

4. TROUBLESHOOTING & MAINTENANCE...................................................................................... 53

Faults .............................................................................................................................. 53
Issues with operating conditions ................................................................................... 54
Preventive maintenance ................................................................................................ 55
Maintenance .................................................................................................................. 55
Preventive maintenance actions ................................................................................... 55

APPENDIX ....................................................................................................................................... 57
Mechanical drawings ..................................................................................................... 57
Generator ....................................................................................................................... 57
25 mL cavity ................................................................................................................... 58
100 mL cavity ................................................................................................................. 59
Electrical drawings ......................................................................................................... 60
Modbus data mapping ................................................................................................... 61

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 MicroChem System & OPTIONS

1. SAFETY RULES
General precautions

Read the manual before handling the equipment

SAIREM is not responsible for any damage caused by inappropriate use of the equipment.

EQUIPMENT TRANSPORT

Please pack carefully. Take all necessary precautions to avoid

shocks during transport. If possible, use the original package.

GENERATOR ENVIRONMENT

Never operate the generator in an environment containing

inflammable vapours or corrosive materials.

The generator should be installed in a clean, dry place, protected

against water or moisture. In case water is spilled on the generator,
first unplug, dry and then restart the system.

Ensure that there is sufficient circulation of cooling air. The

ventilation grids must be free from any obstructions in order to
avoid overheating of the system.

Never operate the generator in a dusty environment.

Do not hesitate to consult SAIREM or local SAIREM representatives if there is the slightest
doubt about the operating environment.

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HOT SURFACE

Avoid contact without proper equipment (PPE) with hot surfaces.

Some parts of the S and M-Cavities may heat up during operation.

The heating of the cavities can be the result of heat transfer

between the product, the vial and the cavity.

Under inappropriate conditions of use, the adapter stub may

become abnormally hot.

With the high-pressure option, the metallic parts of the high-

pressure reactor can be hot. Be sure to wait for the high-pressure
reactor to cool down before handling it.

Qualification of personnel

Only competent personnel are permitted to start-up and operate

SAIREM generators and cavities. The user must know and
understand both i) how to handle microwave cavities and ii) how to
handle his/her own processes. The user must be able to react
properly in an emergency.

The user is responsible for chemical interactions and the

consequences of his/her experiment. The user must be familiar with
the effects of chemical and thermal reactions. It is the responsibility
of the user to take all measures possible to prevent injuries to
personnel, damage to the equipment and building as well as avoid
environmental pollution.

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Electromagnetic precautions
MICROWAVE RADIATIONS

Never operate the generator without connecting the MW output to

the loaded cavity, or another appropriate load.

Do not apply MW power when the cavity is not properly closed and
not properly loaded.

Check that the MW connectors are tightly screwed, the MW cable

is not damaged and the shielding is operational. Use the cable
supplied by SAIREM or one with equivalent ratings. The cable must
not be bent too tightly.

On commissioning, start the generator at low power and check for

possible leakage. Then, progressively increase the power whilst
ensuring that there is no leakage.

Ensure that leakage is such that P<5 mW/cm2 at 5 cm from system.

It is recommended to check periodically if there is no microwave
leakages.

ARCING HAZARD

Do not insert items that could cause arcs into the cavity (metallic
probe or other object that could act as antenna).

Always ensure electrical contact of the stub with the cavity.

- When adjusting the stub, always apply pressure to the stub
along its screw axis.
- Once the stub has been adjusted, lock it in position with the
locknut.

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Approved operating conditions for cavities

The maximum allowable working pressure and the maximum allowable temperature for the
MicroChem cavities are:
• Standards design : 1 bar and 200°C at the Viton seal of the gland or the optical fiber, and 525°C
for the borosilicate glass
• Continuous flow option : 2 bar and 200°C
• High pressure option : 10 bar and 200°C

The provided vials are made of borosilicate glass. Do not work with solvents that can damage
the integrity of the glass such as hydrofluoric acid, phosphoric acid or alkaline solutions (non-
exhaustive list).

If the user uses a self-made quartz vial, then the achieved temperatures can be higher than
525°C. The maximum allowable working pressure is determined by the provider of the quartz
vials.

Rapid and fluctuating changes in temperature (rise and cooling) or pressure can cause high
levels of stress in the glass. Avoid glass vials under pressure being heated or cooled too
quickly.

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2. PRESENTATION
MicroChem line
The MicroChem line includes a microwave generator, cavities and various accessories to suit
your application. This line of product has been specially designed for research purposes.

- Figure 1: Synthesis of the MicroChem line -

The basic element of the line, the MicroChem system includes the generator and the S-Cavity,
and their accessories.

The generator solid-state technology allows for accurate power delivery, frequency tuning,
and reflected power measurement.

The S-Cavity is supplied together with vials of different diameters (10 mm, 18 mm and 24 mm)
to accommodate different volumes (from 1 to 25 mL). The S-Cavity can be titled to change the
orientation of the field to the volume of the treated product. This adds an extra degree for
the cavity adaptation and thus increases the range of products for efficient MW heating.

The following options are available to expand the experimental opportunities of the
MicroChem system:
• A specially designed cavity, M-Cavity, to handle larger volumes of product (40 to 100 mL)
• A kit for working in continuous flow with the S-Cavity
• A kit allowing to work under pressure up to 10 bar with the S-Cavity

Both cavities (S-Cavity and M-Cavity) are compatible with magnetic stirring.

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MicroChem connectivity overview

MicroChem generator is connected to the cavity by the MW coaxial cable. The temperature
monitoring device can be fiber optic or pyrometry, that is connected to the generator. The full
control of the process proceeds via PC, using GeneLink software

- Figure 2: MicroChem diagram, global connectivity overview -

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Useful definitions

The aim of this section is to define some of the terms used in this manual, for
a better understanding of the following sections.

Cavity tuning

Cavity tuning indicates an adjustment of the microwave system in order to ensure a transfer
of MW power from the generator to the product for heating:
• A bad-tuned cavity will send a large portion of the MO power back to the generator without
heating the product
• A well-tuned cavity ensures that the majority of the MO power from the generator is
transferred to the product.

It is possible to tune the cavity for the product by different ways:

• In the case of the S-cavity, adapt the configuration of the cavity (orientation and vial diameter)
to the product and the volume to be treated.
• Adjust the Microwave frequency of the generator (from 2400 to 2500 MHz)
• Use the screw, called "stub" (or MW tuner on mechanical drawings), located near the coaxial
cable connection

- Figure 3: Identification of the “stub” on the cavities -

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Forward, reflected and absorbed powers

The balance of microwave power is given by the following equations :

𝑃𝑡𝑟𝑎𝑛𝑠𝑚𝑖𝑡𝑡𝑒𝑑 = 𝑃𝑓𝑜𝑟𝑤𝑎𝑟𝑑 − 𝑃𝑟𝑒𝑓𝑙𝑒𝑐𝑡𝑒𝑑 (1)

𝑃𝑎𝑏𝑠𝑜𝑟𝑏𝑒𝑑 = 𝑃𝑡𝑟𝑎𝑛𝑠𝑚𝑖𝑡𝑡𝑒𝑑 − 𝑃𝑙𝑜𝑠𝑠 (2)

The forward power is defined as the microwave power generated by the magnetron or solid-
state generator.

The definition of the reflected power is the portion of the generated microwave power that
was not absorbed during the process and that returns back to the magnetron or solid-state
microwave generator. The generator dissipates this power using an isolator. The maximum
reflected power value is 100W, reduced to 70W after 2 minutes. The generator automatically
limits the forward power to respect this limitation.

The transmitted power is the amount of power dissipated outside of the generator. It is
obtained by subtracting the reflected power from the forward power (equation (1)).

The power loss is defined as the fraction of transmitted power that is dissipated in parts of
the system other than the sample (cable, connectors, tuning stub, body of the cavity).

The absorbed power by the sample is equal to the transmitted power, minus the power loss
(equation (2)).

The value of the reflected power is an important parameter, indicating the efficiency of the
interaction between microwaves and the material. Lower reflected power means stronger
interaction and efficient transfer of the microwave energy to the material.

Note that the absorbed power estimation, available on the interface, is an estimation of the
power absorbed by the sample, based on transmitted power and known losses (cable,
connectors). The accuracy is decreased when reflected power is high (due to reflected power
estimation accuracy), and/or the tuning stub is inserted deeply (due to additional losses in the
stub and the cavity).

At high temperatures, the heat radiation from the sample should be taken into account when
performing energy analysis.

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3. INSTALLATION & OPERATION

Installation

Positioning of the generator

The system must be located in a dry and clean place, away from flammable
vapours, or corrosive materials. Avoid introduction of water, conductive or
corrosive material into the generator. Protect from risks of condensation.

Ensure that the system is properly ventilated. Make sure that the heat
exhaust can escape through the back of the generator. Ensure the air inlet
and exhausts are not obstructed and air can circulate properly.

- Figure 4 : Air flow directions

Inlets in blue, outlets in orange -

Connections

Safety interlock

Safety is ensured by a “safety interlock” switch input which prevents the microwave
emissions, suitable for interlock devices. The safety input has two actions: hardware and
software. If the circuit is opened, MW emission is stopped and a fault is triggered.

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 MicroChem System & OPTIONS

- Figure 5: Location of the safety interlock connector on the back panel -

Connect any external security device (interlocks) on the external security connector.
If not used, tie the pins together. Connector type is M12 5 pins. Connectors are provided with
the connection above already in place.

- Figure 6: Safety interlock connector wiring -

Power supply

Use the supplied power cable to connect the socket on the back of the generator (below the
power switch) and a compatible power outlet.

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 MicroChem System & OPTIONS

- Figure 7: Localization of the power supply socket -

PC connection

The MicroChem system is designed to be controlled remotely using SAIREM GeneLink

software (cf. Remote Control section below). The communication protocol used is MODBUS®
RS485, which allows to connect additional devices on the same data line.

Connect the computer to the RS485 IN port, using the provided USB-to-RS485
adapter.

- Figure 8: Localization of the MODBUS sockets -

If an external device is used, connect it to the RS485 OUT port, taking into account the RS485
parameters and pinout below (external devices may use a different pinout).

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 MicroChem System & OPTIONS

RS485 Parameters
Baud rate Data bits Parity Stop Bits Handshaking
19200 8 None 1 None

Available RS485 pinouts:

RS485 Pinout
PIN 3 PIN 5 PIN 7
Common /
A+ B-
GND

- Figure 9: DB-9 male (RS485 IN) and female (RS485 OUT) pinout -

The following Modbus IDs are reserved for the MicroChem system: 3, 4, 5, and 247. Make
sure the external device ID is not in conflict with one of these.

Finally, use the interface to configure the IN and OUT terminations.

On a RS485 data line, there must be a termination on the first and last
devices of the line, and no termination in-between.
These 120 Ω terminations allow transmission line impedance matching.

Termination IN should be activated if the MicroChem generator is the first device on the line.
The MicroChem is the first device on the line if the USB adapter connects it to the laptop.

Termination OUT should be activated if no device is connected to the RS485 OUT port.
Otherwise it should not be activated, it is the last device on the line that should provide the
termination.

If an external device is connected on the OUT port, and the terminations are not set up
properly, it can cause a stop of the communication. In this case, unplug the device from the
OUT port, and set up the terminations before connecting the device back.

The interface also allows to disconnect the data out line. This is for maintenance purpose only,
as it cuts the internal communication with the temperature regulator.

The data mapping is given on appendix.

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Temperature measurement / External sensor

The standard temperature measurement of the MicroChem system is an optical fiber, which
is connected to the generator via the associated ST socket.

S S

- Figure 10: Localization of the optical fiber and external sensor sockets -

An external sensor can be used in a complement of the optical fiber temperature probe. This
sensor can be an infrared pyrometer, a pressure sensor, or any other sensor. The connector
is compatible with both 0-10 V input and 4-20 mA input.

- Figure 11: M12 5 pins connector for the external sensor and associated terminations (user view) –

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 MicroChem System & OPTIONS

MW cable

Before connecting or disconnecting the MW coaxial cable or opening the

cavity, microwaves must be stopped and the generator turned off, to avoid
electric shock or burns by microwaves.

Make sure that the connectors are correctly tightened to avoid microwaves
leakage.

Make a connection between the 7/16 N coaxial transition and the cavity.
Make a connection between the generator and the cavity using the MW coaxial cable. The 90°
coaxial transition can facilitate this connection depending to the relative positions of the
generator and the cavity. The 90° coaxial transition can be used either on the side of the
generator, either on the side of the cavity, either not being used.

- Figure 12: Localization of the microwave output socket and illustration of connection between the
generator and the cavity with the MW coaxial cable -

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 MicroChem System & OPTIONS

The presence or absence of the 90° coaxial transition will have an effect on
the energy efficiency of the process. The insertion losses of each connector
are estimated at 0.1 dB (i.e. 2.3%).

Remote control

The system is controlled by GeneLink software developed by SAIREM. General

operations of this software are provided in its user manual. The following
section provides details about the control of the MicroChem system
specifically.

Connecting

Launch the GENELINK software available in the USB key supplied with the equipment.

- Figure 13: GENELINK home –

1) In the "Chemistry" tab select "MicroChem"

2) Select the COM port associated with the connection from your PC to the MicroChem generator
3) Click on "+Add"

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Main controls

The MicroChem dashboard features main controls and indicators on the left side (number 2-
11), plus additional control and indicators located in tabs on the right side.

- Figure 14: MicroChem interface (main controls) -

1) Status (left panel icon). This reflects the status of the generator: Offline (black), Fault (red),
Ready (green), or On (orange).
2) Forward Power Set Point. In Manual mode, the power can be set using the grey slider or
directly typing the desired power. In other modes (thermal cycle, for instance), the set
point is disabled.
3) Ticking the Transmitted Power box forces the generator to interpret the previous command
as a transmitted power set point (cf. Useful definitions section). This also applies in Power
Cycle mode.
4) Forward Power Set Point Readout. This is the readout that comes from the generator.

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5) Forward Power Measure, in green.

6) Reflected Power Measure, in red. Alternatively, this indicator can display the transmitted
power or an estimation of the absorbed power (cf. Useful definitions section). Use the
Power Displayed slider located below to choose the indicator. Note that the reflected
power measurement is used for protection of the generator against excessive power, so it
is calibrated to never under-estimate the actual value.
7) Microwave Frequency is displayed in blue.

8) Microwave Frequency Set Point. It can be set using the associated slider or a typing tab.

9) Enable Autotune. When enabled, the generator dynamically finds the best frequency
(lowest reflected power). The manual choice of the frequency is disactivated when the
autotune function is on.

10) Temperature/Process Value Measurement. It displays the temperature of the sample.

Alternatively, if the power regulation is based on another physical parameter (e.g. pressure
by the means of external pressure sensor), then the value of this parameter is displayed.

11) Start/Stop Process button. Enables/disables Microwave power (Manual mode), or

starts/stops the configured cycle.

Program Tab

The Program tab contains the necessary options for programming the regulation. These
values are needed to set up prior of clicking Start Process.

- Figure 15: Program tab (thermal cycle mode) -

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 MicroChem System & OPTIONS

• (1) Power Set Point Mode is used to select between:

o Manual mode. In this mode, the forwarded power is controlled directly by the
user.
o Simple Set Point mode. In this mode, the system will reach the temperature set
point and then maintain it (for infinite time)
o Thermal Cycle mode. In this mode, the process will consist of a series of steps
(ramp – ramping, plateau* – holding) based on temperature.
o Power Cycle mode. In this mode, the process will consist of a series of steps
(ramp – ramping, plateau* – holding) based on microwave power.
*Previously called “dwell”

• (2) Stop Threshold is the maximal temperature of the sample. If the temperature
exceeds this threshold, the microwave power is automatically stopped.

• (3) Reflected Power. The maximum value of the reflected power can be adjusted on
the right-hand side. There are two different options in the case of exceeding the
adjusted reflected power: Limitation and Stop on fault. If Limitation is selected, then
the forwarded power will be automatically decreased to keep the reflected power
within the chosen limits. If Stop on fault is selected, then the forwarded microwave
power will be automatically stopped.
Depending on the selected Power Set Point Mode, some other functions will be displayed:

• Set Point (displayed in Simple Set Point mode). Temperature to be reached and
maintained.

• Max Power (displayed in Simple Set Point and Thermal Cycle modes). The maximum
forwarded microwave power of the generator.

• Launch AutoPID and Max Power (AutoPID) (displayed in Simple Set Point and Thermal
Cycle modes). These are to Launch AutoPID cycle (details can be found below).

• Time Unit (displayed in Thermal Cycle and Power cycle modes). A choice of the time
unit of the cycle steps: seconds, or minutes.

• Configure Cycle (displayed in Thermal Cycle and Power cycle modes). It opens the cycle
configuration window for easier operations (details can be found below).

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Cycle configuration

- Figure 16: Cycle configuration window -

This window is used to set up both thermal cycles and power cycles.
Choose the type of cycle and the time unit in the Cycle Parameters panel.

The cycles can be saved on disk and loaded, using the SAVE CYCLE and LOAD CYCLE buttons.

In the Cycle panel, the segments are displayed for the manipulations. If the cycle contains
more than 5 segments, use the slider or arrows to navigate. For easier use, it is also possible
to insert, append, or remove a segment using the buttons on the left-hand side. Each segment
is either a ramp (ramping) or a plateau (maintain), except for the last one (end).

The behavior is slightly different depending on the cycle type. In a thermal cycle, the dwell
will maintain the set point previously ramped (for example, the temperature was ramped to
50°C and it can be maintained only at 50°C ). In a power cycle, there is no such restriction (for
example, the power was ramped 50 W and then it can be maintained at 100 W if required).
Finishing with an end type segment is mandatory for a thermal cycle mode, but not for a
power cycle. In case of illogical thermal cycle parameters, an error message will appear
when starting process, and it might be necessary to reboot MicroChem.

The segments can be edited directly.

Clicking the APPLY button closes the window of Cycle Configuration. All the data about the
configured cycles are imported into the MicroChem dashboard.

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AutoPID

- Figure 17: AutoPID behavior sequence

The purpose of the AutoPID is a calculation of the regulation coefficients. These coefficients
are needed for a correct temperature regulation of the sample. These coefficients can vary
greatly depending on the sample, so it is necessary to estimate them before starting a process
on a new sample.
Before starting uto D, choose “Simple Set oint” mode and set up an adequate value of the
temperature. The adequate value of the temperature means i) this value has to be above the
ambient/initial temperature (high enough for ambient cooling to be significant); ii) but this
value has to be low enough to be reached in a reasonable time.
The behaviour of AutoPID, relative to this set point, is explained in the - Figure 17. The PV
refers to the Process Variable (i.e. temperature), SP is the Set Point and Working Output
indicates the Forward Power. The various stages of the autoPID sequence are explained
below:

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A : Start of AutoPID
A to B : Initial delay. Output is set to 0% for precisely one minute.
B : Tuning temperature calculation. The tuning temperature is equal to the
temperature at time B plus 3/4 of the difference between the set temperature
(referred as the “adequate temperature” above) and the temperature at time B.
Example: if sample T°B is 25°C, and set temperature (referred as the “adequate
temperature” above) is 85°C, then tuning T°TUNING will be 25+(3/4)×(85-25)=70°C
B to C : On/Off power cycles. The output is set to the allowed maximum (Max Power –
AutoPID) until the sample temperature reaches the tuning temperature. Then,
output power is set to 0 W until the sample temperature decreases below the
tuning temperature. Finally, this cycle is repeated for a second time.
Note, this phase can take a long time if Max Power – AutoPID and the
Temperature Set Point are not adjusted to adequate values. If necessary, stop the
process, change these values, and restart the operation.
C/D : Analysis and completion. Once the second on/off cycle is over, the regulator
analyses the data and computes the optimal regulation (PID) parameters. The
time between C (end of cycle) and D (end of autoPID process) is a few seconds.

Faults Tab
Faults tab displays the list of current faults and warnings. If a fault occurs, this tab is displayed
automatically.

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Scan tab
This tab controls the microwave frequency scan feature. When activated, the generator
sweeps through the entire frequency band, while monitoring reflected power.

- Figure 18: Scan tab –

Press the Run Scan button and wait a few seconds. The results will appear on the right-hand
side (Scan Results MicroChem). Two frequencies which give the lowest values of reflected
power, and the corresponding reflection coefficients, will be displayed.

Configuration Tab
This tab contains the configuration options of the MicroChem system.

- Figure 19: Configuration tab (user level) -

Press the READ ALL button to visualize the current parameters.

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 MicroChem System & OPTIONS

• Regulation Mode. Select type of the input signal needed for process regulation: fiber
optic temperature measurement (TEMPERATURE) or external sensor input (EXTERNAL
4-20 mA or 0-10V)

• External Min & External Max, or Temperature Min & Temperature Max (depending on
the selected regulation mode). If an external sensor was used, then insert the
measurement range External Min & External Max (based on the specification of the
external sensor). If fiber optic (provided by SAIREM) was used, then the values installed
by SAIREM should not be modified.

• Apply. IMPORTANT: If the regulation mode or the range of measurement have been
modified, then it is necessary to click “Apply” for implementing the changes.

• Modbus address. The Modbus ID of the MicroChem can be changed here.

• RS Termination. Select the appropriate termination setup, if additional devices are

connected with the RS485 bus. Cf. Modbus data mapping (in appendix) for
interpretation of the number.

• Cable Loss. The estimated attenuation factor (in dB) of the cable and connectors. It is
used for absorbed power estimation. This value can be modified for adjusting the
measurements.

IMPORTANT: Once the modifications have been applied, press SAVE ALL to store the
parameters into the generator memory.
The other configuration options (cooling fan parameters, etc) are password-restricted, and
meant to be set up by Sairem during production of the MicroChem unit.

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 MicroChem System & OPTIONS

Starting and operating

Before starting the generator, check all microwave connections: cable,

connectors, and cavity.

Cavities installation

Standard versions

Place the cavity on a flat, uncluttered surface so that

it can be easily handled.

Two orientations are possible in the case of the S-

cavity. Choose the working orientation (E or H).

The “Cavities tuning” paragraph provides the recommendations about choice

of the orientation (E or H) according to the product properties and the loading
volume.

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 MicroChem System & OPTIONS

The S-Cavity is supplied with three vial diameters and

their associated glands.
Depending on the working vial, screw the compatible
gland onto the thread on the top surface of the cavity
(depending on its orientation).

All other openings must be closed with the supplied

lat cap for
caps. magne c s rring

Three types of caps are available. The flat cap, which

allows a magnetic stirring system to be placed as close Standard
cap
as possible, a cap with a threaded hole to screw in a
pyrometer, and a standard cap. ap with
threaded hole
for pyrometer
The M- avity doesn’t have standard cap.

In order to facilitate the screwing/unscrewing of the

S-Cavity flat cap, a tool is available.
It is located on the edge of the base of the cavity.

For the M-Cavity, there is no need for the tool.

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 MicroChem System & OPTIONS

A ground-to-thread adapter is provided to connect a

cap to the vial. This cap allows to keep the optical fiber
in place.
Fill the vial with an appropriate volume of product.
Screw the cap with its different parts on the adapter.
Insert the adapter into the vial.
Insert the fiber optic through the cap and position it
in the middle of the product height.

It is recommended to grease the adapter's ground joint, with silicone grease,

to facilitate its disassembly.

Use the upper ring of the sample holder and turn it in

an anti-clockwise direction to allow soft penetration
of the sample inside the cavity.
Adjust the height of to make the sample in the middle
of the cavity. Hold the sample.
Use the upper ring of the sample holder and turn it in
a clockwise direction to fix the sample inside the
cavity.

Ensure that the sample is completely inside the cavity and does not rise
partially into the gland.

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Continuous flow option

The following section describes how to

assemble the continuous flow option
with the MicroChem S-Cavity.

Orient the S-Cavity in H orientation (long sides

vertically).
Screw the glands supplied onto the top and bottom of
the cavity.
An 18x3 mm O-ring should be positioned in the lower
gland.
A 24x3 mm O-ring should be inserted into the
shoulder of the upper gland.

Insert the continuous vial into the cavity through the

glands from the top surface to the bottom surface.
Close the upper gland with the associated metallic
part.

All other openings must be closed with the supplied

caps.

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 MicroChem System & OPTIONS

hermowell

Screw the cap with its seal on the Y glassware.

ap
Insert the thermowell through the cap and position it Seal
at the desired height.

glassware

Connect the remaining glassware, elbows and Y with

thermowell, to the continuous vial.

Maintain the different elements of glassware with the

help of clamp clips for taper glass ground.

You can now connect your circuit to the S-cavity.

It is recommended to grease the adapter's ground joint, with silicone grease,

to facilitate its disassembly.

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 MicroChem System & OPTIONS

Pressure option

The documentation for the Büchiglasuster reactor, supplied with the

MicroChem pressure option, must be consulted before any operation.

The following section

describes how to assemble the
pressure option with the
MicroChem S-Cavity.

The pressure option consists of:

• a reactor manufactured by Büchiglasuster
• a connecting piece to make the reactor
compatible with the MicroChem S-cavity
• a glassware reactor for high-pressure
operations
• a cable connection between the MicroChem
generator, a pressure sensor and a pyrometer
(the pressure cord set, see below).

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 MicroChem System & OPTIONS

The pressure cord set connects both power supply of the pressure sensor and pyrometer to
the generator. In this way, the temperature can be monitored via GENELINK during high-
pressure operations.

- Figure 20: MicroChem diagram, global connectivity overview of the pressure option -

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 MicroChem System & OPTIONS

Take the PTFE ring from the mesh guard and fit it into
the shoulder of the cavity to reactor connecting part.

Orient the S-Cavity in H orientation (long sides

vertically).
Screw by hand the cavity to reactor connecting part.
Check that the PTFE ring is properly seated in the
shoulder of the connection piece.

All other openings must be closed with the supplied

caps.

Fill the glass reactor of product without exceed 10 mL.

Insert the glass reactor into the cavity through the
reactor connecting part.
Check that the reactor glass is correctly positioned
onto the PTFE ring.

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 MicroChem System & OPTIONS

Screw the reactor cover to the connecting part.

Screw the pyrometer to the cap with a threaded hole.

In order to facilitate the unscrewing of the cavity

reactor connection part, a tool is available.
It is located on the edge of the base of the cavity.

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 MicroChem System & OPTIONS

Connect the pyrometer and the pressure reactor to the generator as it follow:
• The 9-PIN SUB D FEMALE PLUG to the MODBUS OUT plug on the generator
• The M12 MALE 5 PINS B-CODED PLUG to the SENSOR plug on the generator
• The unsheathed wires to the pyrometer's electronic box
o WHITE to GND
o BROWN to +VDC
o GREEN to OUT
• The M12 FEMALE 5-PIN A-CODED PLUG to the pressure sensor on the reactor

- Figure 21: Photograph of the pressure cord set and connection indication between
generator, pressure sensor and pyrometer -

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 MicroChem System & OPTIONS

When selecting the MicroChem in the GENELINK software, check the "High Pressure option"
box to access the pressure monitoring and threshold function.

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 MicroChem System & OPTIONS

Power operation and taking out of the sample

• To check for MW leakage, it is recommended to use MANUAL mode with 0 W set point.
Increase the power set point progressively. Ensure there is no microwave leakage. If leakage
exceeds 5 mW/cm2 at 5 cm, turn off the generator, then check that the cavity is properly
closed and the microwave connections are correctly tightened.

• When working with a new sample, it is also recommended to use MANUAL mode with 0 W
set point. Increase the power set point progressively, up to 20 W. Once this level is reached,
check that the reflected power remains low (<20%). If it is not the case, adjust the tuning stub
on the cavity to minimize reflected power. Then, use the frequency scan to find the best
matching frequency. Once reflected power is minimized, the MW power can be increased
progressively, up to the adequate value for the sample. If the properties of the product change
as it warms up, an increase in reflected power may be observed. It may be appropriate to
readjust the stub setting or activate the autotune function (which automatically adjusts the
output frequency to minimise the reflected power).

It is necessary to ensure that the tuning stub always makes electrical

contact with the cavity. To do this, the locknut of the tuning stub has to be
screwed to secure the stub in its position.

If it is necessary to adjust the position of the tuning stub during power

operation, be sure to manipulate the tuning stub while applying pressure
to the locknut to maintain the electrical contact between the tuning stub
and the cavity

• If the reflected power level is unstable, bring the power level back to 0 W, switch off the
power supply and check that the cavity is properly enclosed, is not empty, and the cable is
connected.
• To unload the sample, use the upper ring of the sample holder and turn it in an anti-
clockwise direction to allow soft taking out of the sample.

After the MW run, please make sure that the temperature of the sample
is lower than 60°C before taking the sample out.

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 MicroChem System & OPTIONS

Status indicator

- Figure 22: Localization of the LED indicator -

The status of the generator is indicated visually using a LED strip.

Color Meaning Description

Blue Starting up Generator did not receive any communication since power-up

Green Ready Generator is ready to be turned on

Yellow Microwaves ON Generator is ON, microwave output is active

At least one fault has been detected, microwave output is

Red Fault
disabled until the fault has been reset

Stop Button
The toggle button located below the status indicator acts as a hardware safety feature,
allowing the user to shut off the power supply of the microwave module inside the generator.

Switching the button to the OFF position stops the microwave module almost instantly
(<100 ms), and puts the generator into Fault state. Switch the button back to ON and reset
the fault to make the generator ready again.

In regular use, it is recommended to stop the microwave output using the

GeneLink interface, rather than the toggle button. The microwave module is
intended to stay on, except in cases of emergency stop.

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 MicroChem System & OPTIONS

Cavities tuning

The cavities can be adapted to the product via different ways. A tuned cavity
ensures the efficient transfer of microwave power from the generator to the
product, i.e. has a low reflected power value.

To reduce the reflected power ratio for a product it is possible to operate with:
• The product (volume, shape etc.)
• The orientation of the product in relation to the microwave field (E- and H- orientations)
• The position of the tuning stub
• The frequency of the microwaves

To adapt the cavity to a given product and in a given configuration (volume and orientation),
it is recommended to proceed as follows:
1) Raise the stub so that it does not penetrate the cavity
2) Start the microwave at 2450 MHz and at low power
3) Screw the stub in such a way as to minimize the reflected power
4) Lock the stub in its position with its lock nut
5) Start a frequency scan

If after these steps the reflected power remains high:

1) Check your installation (connections, cavity installation etc.)
2) Review your configuration (change orientation and/or product volume)

Low reflected power alone does not guarantee an efficient power transfer.
The power can be consumed by other elements such as connectors,
microwave cable or even the stub if it is too deep.

Under poor matched conditions some surfaces may become hot,

especially the connectors and the microwave cable as well as the stub and
its locknut.

If you have difficulties with an efficient heating of the product, then it is recommended to
increase volume of product and repeat the tuning procedure.

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MicroChem S-Cavity

Available volume is between 1.5 mL and 25 mL.

On the S-Cavity, a mechanical system allows to change the orientation of the applicator to
irradiate the product either in parallel (E orientation, figure below) or perpendicularly (H
orientation, figure below) to the electric field. This system provides a good cavity matching
for a wide range of products with various dielectric permittivities.

- Figure 23: Parallel orientation (E orientation) of the MicroChem S-Cavity and perpendicular
orientation (H orientation) of the MicroChem S cavity. The figure displayed all available diameters of
the vials: 10 mm, 18 mm, 24 mm for MicroChem S-Cavity -

The recommendations on the optimal cavity orientation of some compounds are displayed
below:

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 MicroChem System & OPTIONS

- Figure 24: Recommended configurations for experimental chemistry depending on the volume and
dielectric properties (2 orientations: E & H; 3 vials: 10 mm, 18 mm and 24 mm) -

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 MicroChem System & OPTIONS

The recommended configuration does not ensure full efficiency of product

heating.
To increase chances of a good coupling with the product, it is recommended
to use the volume of 25 mL with the H24 configuration

MicroChem M-Cavity

Available volume is between 40 and 100 mL

The MicroChem M-Cavity is designed for reactions at the volumes larger than 40 mL.
The M-Cavity orients the product perpendicular to the electric field, which is the most suitable
configuration for large volumes.

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4. TROUBLESHOOTING & MAINTENANCE

Faults
Fault code Corrective action
Check external safety connector. Pin 1 & 5 must be
connected. This input can be used to connect an
EXTERNAL SAFETY
external device providing a normally closed dry
contact to prevent microwave when opened.
If fault happens only at startup, it can be ignored.
Otherwise, for EXTERNAL COMMUNICATION fault,
check RS485 connections and check the state of RS485
EXTERNAL COMMUNICATION
IN and OUT terminations (i.e. OUT termination is off if
INTERNAL COMMUNICATION a device is connected on the OUT port).
INTERNAL COMMUNICATION happens when shutting
off the MW module with the emergency button

Check the ambient temperature is in accordance with

TEMPERATURE specifications. Ensure the cooling fans are functioning
properly and the air flow is not obstructed.

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Issues with operating conditions

Condition Corrective action
Check MW cable and connectors.
Reflected power is fluctuating Check microwave leakage level.
Also happens when water sample reaches boiling point
Use frequency autotuning.
Adjust tuning stub.
Reflected power is too high
Put a sufficient load inside the cavity.
Check MW cable and connectors.

Turn microwaves OFF.

Forward power does not Check the ambient temperature is in accordance with
reach set point specifications. Ensure the cooling fans are functioning
properly and the air flow is not obstructed.
Go into the Configuration tab of the MicroChem
dashboard in GeneLink.
Click READ ALL, check the selected Regulation Mode is
Temperature measurement is correct (select External when using a pyrometer), as well
incorrect as the measurement range.
Click Apply and wait a few seconds.
Click SAVE ALL
If issue persists, cycle power of generator

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 MicroChem System & OPTIONS

Preventive maintenance
Maintenance
• Only fuse replacement is allowed (in the main socket of the rear panel).
• All other maintenance operations must be done by SAIREM or S M’s
representatives.

Opening of the generator is not allowed without SAIREM's authorisation.

Warranty will be void if you do this and it will be at your own risks.

Preventive maintenance actions

• Every month :
o Check MW connectors tightening
o Check the MW connectors temperature (Maximum 50°C)
o Check the MW cable temperature (Maximum 45°C)

• Every 6 months :
o Check the air temperature at the outlet of the radiator
o Check the air flow out of the radiator (Minimum 4.0 m/s at full power)

• Every 12 months :
o Removal of the MW connectors to check the connection quality. There
shouldn’t be any burn marks.

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 MicroChem System & OPTIONS

APPENDIX
Mechanical drawings
Generator

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S-Cavity

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M-Cavity

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Electrical drawings

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 MicroChem System & OPTIONS

Modbus data mapping

The MicroChem system is controlled in Modbus RS485. Two Modbus IDs are used to address
the equipment. Modbus ID n is configurable (3 by default), the second ID is always n+1.

Read-only values (ID n)

Registers from 100 to 119 are supported, those that do not appear in this table are either not
used or reserved.

Register
Register Name Description
Address
100 FP_SP_Volts Value read for forward power set point in mV

101 FP_SP_Watts Value read for forward power set point in W

102 FP_Meas_Volts Value read for forward power measure in mV

103 FP_Meas_Watts Value read for forward power set point in W

104 Temperature_Volts Value read by temperature sensor in mV

105 Temperature_Celsius Value read by temperature sensor in °C

Value read from external input in mV or mA,
106 External_measure_V_mA
depending on the regulation mode
Value read from external input in natural unit (°C,
107 External_measure
mbars)
Estimation of power absorbed by the sample in W,
108 Absorbed_power
taking losses into account
115 Current_Level Current access level (based on password input)

118 SW_Version Software Version

Read-only values (ID n+1)

Registers from 100 to 119 are supported, those that do not appear in this table are either not
used or reserved.

Register
Bit Name Description
Address
100 FP Set Point Readout Readback of forward power set point
Readback of maximum reflected
101 RP Set Point Readout
power value set by the user
102 FP Measure Forward Power measurement, in W

103 RP Measure Reflected Power measurement, in W

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0 External Safety Fault

1 RP Limit (in RP Limitation Mode)

104 3 Overcurrent Fault

1 = Active
4 Humidity Fault

5 External communication Fault

6 Temperature Fault

7 Relay Fault

1 Status FAULT

2 TP Not Reached

3
105 1 = Active
4

5 End Of Scan

6 Status ON

7 Status READY
In scan mode, returns scan
106 Scan Reflection Coeff Register
coefficients (every 100ms)
Minimal reflection coefficient #1
107 Scan Reflection Coeff Minimum 1 (corresponds to frequency indicated
in register 114)
1=Scan data is being sent on register
0 Sending Data In Progress
106
1

2 Max RP Fault (RP disjunction mode) 1 = Fault

3 External Communication Fault 1 = Fault

109
4

7 Set Point - Measure Disparity 1 = Fault

110 Module Sofware Version MW module software version

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Minimal reflection coefficient #2

111 Scan Reflexion Coeff Minimum 2 (corresponds to frequency indicated
in register 115)
112 MW Frequency Current microwave frequency
In scan mode, returns scan frequency
113 Scan Frequency Register
(every 100ms)
114 Scan Frequency Minimum 1 Minimal reflection frequency #1

115 Scan Frequency Minimum 2 Minimal reflection frequency #2

Read-Write parameters (ID n)

Registers from 0 to 31 are supported, those that do not appear in this table are either not
used or reserved.
Register Access
Register Name Description
Address Level
Regulation Mode
0 – Fiber optic probe
0 Regul_Mode User
1 – External 0-10V
3 – External 4-20mA
Minimum value of external input, in natural
1 External_min User
unit (°C, mbars)
Maximum value of external input, in natural
2 External_max User
unit (°C, mbars)
3 Attenuation Attenuation value (losses), in dB*100 Advanced
Register used to save parameters.
5 Save_Param BIT15 (rising edge) : Save order User
BIT7-BIT0: register to save (255: save all)
6 Password Password. Sets user level User

7 Temperature_min Minimum value of fiber optic measure, in °C Advanced

8 Temperature_max Maximum value of fiber optic measure, in °C Advanced

Resistor terminations state :
Bit 0 : 1 → Termination IN Enabled
9 RS485_Terminations User
Bit 1 : 1 → Termination OUT Enabled
Bit 2 : 1 → Disconnect out line
Modbus ID of the equipment
10 Microchem_ID Applied when restarting, if the parameter has User
been saved
20 Generator_Power Nominal power of generator Restricted

21 Nb_Leds Number of LEDs on the status indicator Restricted

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22 PWM_Min Minimal PWM value for fans control (%) Restricted

23 PWM_Max Maximal PWM value for fans control (%) Restricted

24 PWM_Lo_Thresh Corresponding Power for PWM_Min (W) Restricted

25 PWM_Hi_Thresh Corresponding Power for PWM_Max (W) Restricted

Access level at start-up. Applies at next
28 Startup_Level User
startup, only if this parameter has been saved

Read-Write commands (ID n+1)

Registers from 0 to 19 are supported, those that do not appear in this table are reserved.
Register
Bit Name Description
Address
Forward/Transmitted Power Set
0 Readback of forward power set point
Point
Reflected Power (RP) Set Point Readback of maximum reflected
1
power value set by the user
0
1 Enable autotuning 1 = Enable

2
3 Pulse Mode 1 = Enable
2 4 Reflected Power Limitation Mode 0 = Max RP Fault Mode
1 = RP Limitation Mode
5
6 ON/OFF Microwaves 1 = Start Microwaves
0 = Stop Microwaves
7 Reset Faults Pulse to 1 = Reset Faults

3 Start Mode 0 = Normal; 1 = Overshoot; 2 = Ramp

4 Start Time 1 → 60s in amp

5 Low Power Pulse Set Point
6 High Power Pulse Set Point
7 Pulse Frequency Set Point
8 Pulse Duty Cycle Set Point
9 Frequency Set Point
11 Scan Low Frequency
12 Scan High Frequency
16 Scan Frequency Step
0 Scan Mode
17 1 Transmitted Power Regulation Mode
2 Send Scan Data

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