© Siemens AG 2015
Process Gas Chromatographs
MicroSAM
■ Overview
■ Application
Chemical industry
• Analysis of ethylene in 1.2-dichloroethane (EDC) for process
control
• Fast determination of nitrogen in acetylene for process control
• Hydrocarbon analysis of starting product (LPG) of a cracker
• Safety measurement of ethylene oxide during unloading of
tankers
• Multicomponent analysis in ethylene oxide
• Analysis of methanol, water and dimethylether in a pilot plant
• Monitoring of coolant: Trace monitoring in chloromethane
• Analysis of nitrogen and hydrogen in pure gas of a chlor-alkali
plant
3
The MicroSAM is a miniaturized process gas chromatograph
(GC) in an Ex d enclosure. Through consistent use of microsystem technology (silicon wafer technology), all analytical
components are concentrated in the smallest possible area.
The design particularly enables a distributed installation close to
the process.
■ Benefits
• The distributed field installation reduces investment costs,
and opens up new fields of application, e.g.:
- Installation in plant areas where mounting within an analyzer
shed is not possible
- Installation at remote locations without extended infrastructure
• Reduction in laboratory analyses through online measurements
• Low space requirements in analysis cabinets reduce
investment costs
• Low maintenance effort and gas/energy consumption reduce
operating costs
• High-resolution capillary columns permit fast analyses
• Live injection permits representative sample injections
• Maintenance-free, valveless separating column switching
with electronic pressure controllers
• The use of several micro thermal conductivity detectors
(multidetection) provides exact measuring results and also
validation possibilities
• Versatile networking possibilities for central maintenance and
secure data transfer
• Remote monitoring with Windows-based software and
Ethernet communication
• Simplified servicing through replacement of modules
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Siemens AP 01 · 2015
Oil & gas
• Hydrogen analysis in recycled gas and other process gases
• Analysis of inert gases and low-boiling paraffins/olefins in
combustion gas
• Analysis of hydrogen and low-boiling hydrocarbons in
reformer/platformer plant
• Trace analysis of impurities in acetylene from a cracker
• Analysis of ethane in ethylene from a cracker
• Measurement of calorific value in exhaust gas for quality
control in a power plant
• Analysis of ethylene in methane in an ethylene plant
• Analysis of propadiene and propine in the C2 splitter of a
steam cracker
• Analysis of low-boiling hydrocarbons in an ethylene plant/
visbreaker
• Analysis of exhaust gas in flares
• Analysis of gas loop in a propylene oxide plant
• Analysis of CO in crack gas in an LDPE
(low-density polyethylene) plant
• Analysis of refinery gas in a pilot plant
• Analysis of calorific value in natural gas preparation plants
Iron & steel
Analysis of exhaust gas in blast furnaces.
Pharmaceutical industry
• Analysis of O2, N2, CO2 and water in fermenting processes
• Analysis of alcohols in nitrogen for vacuum drying plants
Metals, aggregates, cement
Analysis of mine gas for inert gases and hydrocarbons.
© Siemens AG 2015
Process Gas Chromatographs
MicroSAM
The column system
■ Design
The column system consists of two or three capillary columns
connected in sequence. Micro TCDs or micro live circuits are
installed in sequence ("inline") upstream and downstream of the
individual columns. Three electronic pressure regulators supply
the columns with carrier gas and carry out the switching
functions (injection, backflushing and cut).
Enclosure
• EEx d version standard
• Heating adjustable from 60 to 165 °C (isothermal)
• Decentralized installation close to sampling point
Analytical module
The compact analytical module contains all the functional
components of a chromatograph. The MicroSAM works with:
• Live injection
• Valveless live switching on microchip basis
• Standardized analytical modules
• Multidetection through use of up to 8 micro thermal
conductivity detectors (TCDs) in the smallest possible area
(e.g. on all column/purging outputs and injection)
By using narrow-bore capillary columns, the separation at high
resolution is carried out within a much shorter time, approx.
factor 2 to 3 compared to standard capillary columns.
Electronic pressure regulators
A high pressure stability together with rapid changing rates in
the hPa range are required for precise and fast switching. This is
achieved in the electronic pressure regulators by means of a
piezo actuator.
Detector
The micro TCDs (based on silicon wafer technology) work on the
principle of continuous measurement of the different thermal
conductivities of the carrier gas and the components to be
measured.
■ Function
Live injection
The MicroSAM has a two-stage injection system. Using a micro
injection valve, a defined quantity of sample is first brought up to
the carrier gas pressure. This eliminates the pressuredependent error in the dosing quantity present with conventional
systems. In the second stage, the sample is transferred to the
column by a valveless micro injection system (live dosing). The
result is an "active" injection.
The injection volume can be varied time-controlled, and exactly
matched to the column requirements.
Valveless live column switching
Because of the high dead volume of conventional valves, only
the valveless version can be considered for a miniaturized
system. In this case, the generation of differences in flow using
several electronic pressure regulators at appropriate positions of
the column setup causes a change in the flow directions.
(The system operates according to the Wheatstone principle,
but pneumatically.) The functions "Cut" and "Backflushing" can
then be implemented free of dead volume.
The measurement can be carried out without falsification by
avoiding catalytic effects on the heating wires and maintaining a
constant flow velocity. This permits consistent in-line detection,
i.e. without qualitative or quantitative losses of substances.
Application modules
The application modules contain live injection and live switching.
The modules D06, D08 and D11 have one separating column
less than the modules D01, D02 and D09. The modules D06,
D08 and D11 have one detector less than the modules D01 and
D02. The application modules are suitable for separation of the
components described below. However, when defining the
suitable application module for an actual, customer-specific
measuring task, technical evaluation by our Support Team is
required.
D01, D02 and D08:
These modules contain separating columns that can be
impaired in their separating performance by humidity in the
carrier gas. For this reason, a carrier gas dry filter (filter set:
Article No. A5E00400116) is integrated for these modules on the
support bracket of the MicroSAM or supplied as a separate part
as standard.
The application modules are suitable for separation of the
components described below.
Detector
Column 1
Detector
Column 2
Detector
Circuit
Column 3
Detector
TCD
Sil5 C3, C4, C5,
C6+
TCD
PoraPLOT/Porabond Q
TCD
Live
Molecular filter
TCD
Sil5 C5+
TCD
D01
Injection
CO2, C2, H2S, H2O
H2, (Ar+O2), N2,
C1, CO
D02
Injection
TCD
SilicaPLOT
TCD
Live
Molecular filter
TCD
H2, (Ar+O2), N2,
C1, CO
C2, C3, C4 (saturated,
unsaturated), C5+
D09
Injection
-
Sil5
Non-polar aromatic
and aliphatic hydrocarbons
TCD
Sil5
Non-polar aromatic
and aliphatic
hydrocarbons
TCD
Live
Porabond Q
TCD
All components
except molecular
filter components
Application modules D01, D02 and D09
Siemens AP 01 · 2015
3/19
3
© Siemens AG 2015
Process Gas Chromatographs
MicroSAM
Detector
Column 1
Detector
Circuit
Column 2
Detector
TCD
Sil5
TCD
Live
Sil5
TCD
D06
Injection
Non-polar aromatic and
aliphatic hydrocarbons
Non-polar aromatic and
aliphatic hydrocarbons
D08
Injection
TCD
Porabond Q
TCD
Live
Molecular filter
TCD
H2, (Ar+O2), N2, C1, CO
All components except
molecular filter components
D11
Injection
TCD
RTX-5+
RTX-200
TCD
Non-polar aromatic and aliphatic hydrocarbons and
medium-pole components
such as chlorosilane
3
Application modules D06, D08, and D11
Application
Various solution concepts are available:
• Adjustment without method development (on request)
- Run-out ex factory
The application modules are standardized. The functionality
of the MicroSAM is proven with a specified carrier gas, exact
setting of the oven temperature and the carrier gas inlet
pressures, and with a standard calibration gas.
The measured components and switching functions
(live injection, backflushing, cut) are saved.
- Commissioning on site
All application modules are standardized, i.e. the analytical
hardware is defined and cannot be changed. The specific
settings are carried out on site during commissioning.
• Adjustment with method development
Non-standardized applications require specific method
development:
An optimum solution is elaborated on the basis of an existing
specification and a selected calibration gas or with application of a customer sample.
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Siemens AP 01 · 2015
Live
SilicaPLOT
C2, C3, C4, C5, C6
(saturated, unsaturated)
TCD
© Siemens AG 2015
Process Gas Chromatographs
MicroSAM
■ Technical specifications
Design, enclosure
Sample and injection
Weight
15 kg
Sample streams
3
Degree of protection
IP65 (NEMA 4X)
Calibration sample streams
1
Phase
Gaseous
Required filtration
Degree of separation 99.99 % for
< 0.1 μm particles
Material with which the sample comes
into contact
Stainless steel, fused silica,
polyimide
Injection
• Controller
"Valveless" live injection
With multifunctional diaphragm
valve
2 ... 50 µl
Mounting
Installation on
Post, pipe or wall
Distance from wall or next chromatograph
300 mm (12")
Distance from ceiling or floor
200 mm (8")
Explosion protection
ATEX and IEC Ex: II 2 G Ex d IIC T4
Gb
Class I, Zone 1, Group IIB + H2 T4
Class I, Div 1, Groups B, C, D T4
Factory Sealed
Support bracket
• Mounting part, dimensions (D x H)
• Gas connections
• Bracket for gas connection, dimensions (D x H), bracket on right side,
mounted at right angle
Power consumption
• Typical
• Maximum
• Electrical safety
EMC immunity
• Conducted interferences on AC
supply lines
- According to Part 4 (burst)
- According to Part 5 (ms pulses),
line against line
- According to Part 5 (ms pulses),
line against ground
• Conducted interferences on signal
lines
- According to Part 4 (burst)
• Immunity to static discharge
- According to Part 2 (ESD)
• Immunity to fields
- According to Part 3 and Part 6
• Noise suppression
165 °C
3
Oven
380 x 110 mm
8
146 x 110 mm
Electrical characteristics
Power supply
• Injection volume adjustable using
switching times
• Max. operating temperature
24 V DC (18.5 ... 30.2 V)
18 W
60 W
IEC 61010 / DIN VDE 0411
According to IEC 60801/
DIN VDE 0843
Number/type
1/isothermal
Purging with N2
Possible
Dimensions (DxH)
160 x 10 mm
Heating capacity
20 W
Temperature range
60 … 155 °C
Temperature stability
± 0.1 K (60 ... 155 °C)
Temperature accuracy
± 3 K (60 ... 155 °C)
Retention time variations per 10 °C
change in ambient temperature
Approx. 0.3 %
Heating-up period from 30 ... 100 °C
10 minutes
Columns and gases
Column type
Capillary columns 0.15 ... 0.25 mm/
internal
Separating column switching
Multidimensional chromatography
with backflushing and cut in live system
Multifunctional diaphragm valve
For injection and backflushing
Gas connections
Swagelok 1/8"
1 kV
Pressure regulators
Max. 4 single-channel electronic
pressure regulators
8 kV
Solenoid valves for control of diaphragm valve
2 NC contacts, 2 NO contacts
10 V/m
According to CISPR 11 / EN 55011 /
DIN VDE 0875 Limit class B
T2.5 A
Carrier gas
• Gas purity (minimum requirement)
• Solid components
• Required filtration
Permissible sample pressure
10 … 60 kPa above atmosphere
Sample flow
20 … 100 ml/min
• Consumption
• Inlet pressure
H2, N2, He, Ar
> 99.999 % (5.0)
< 0.1 μm
Degree of separation 99.99 % for
< 0.1 μm particles
10 ... 60 ml/min
500 …700 kPa (g)
600 kPa (g) recommended
Max. sample temperature
120°C
Solid components
< 0.1 mm
• Fuse
2 kV
1 kV
2 kV
Gas inlet conditions
Important:
A continuous carrier gas supply is
required for error-free operation (frequent carrier gas failure has a negative effect on the life cycle of the
detectors and the internal device
pressure regulator. In addition, an
external two-layer pressure regulator for the carrier gas pressure is
strongly recommended.
Climatic conditions
Permissible ambient temperature
- 20 ... 50 °C (depending on oven
temperature)
Permissible storage/transport temperature
- 30 ... 70 °C
Permissible relative humidity
Max. 90 %
Instrument air
Not required
Siemens AP 01 · 2015
3/21
© Siemens AG 2015
Process Gas Chromatographs
MicroSAM
Detectors, calibration and performance data
Detector type
TCD, max. 8 sensors
Ambient temperature
Negligible
Vibrations
Negligible
Cell volume
0.02 μl
Calibration
Manual or automatic, single-level or
multi-level
Smallest measuring range
1 000 ppm (application-dependent)
Linear range
Typically > 104
Cycle time
Typically 30 … 240 s
Electrical inputs and outputs
Basic equipment
• Digital outputs
(relay contact 0.4 A / 24 V DC)
3
• Digital inputs (24 V to optocoupler)
Interfaces
• Communication
• Control system coupling
4, freely usable (expandable by
NAU or I/O Extender, see Communication in "General information")
4, 3 freely usable (expandable by
NAU or I/O Extender, see Communication in "General information")
1 x Ethernet 10BaseT / TCP/IP
1 x RS 485 or RS 232 /
Modbus RTU, OPC (ODPC) over
Ethernet
Electronics
Communication and analytical
controller (CAC)
• Microprocessor
• Flash EPROM
• Dynamic RAM
• Operating system
• Software
Realtime signal processor (RSP)
• Microprocessor
• Flash EPROM
• Static RAM
• Operating system
• Software
Controller
• Sample streams
• Calibration sample streams
• Status LEDs for
• LCD display for
Recommended operator panel
• Personal computer
• Processor
• Clock
• Interfaces
• Operating system
• Software
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Siemens AP 01 · 2015
Intel 586 architecture
128 MB
64 MB
Windows CE 5.0
Preinstalled. Modifications or
upgrades for operation PC downloadable via network or locally
Motorola 68376, 20 MHz
1 MB
1 MB
Forth
Preinstalled. Modifications or
upgrades downloadable via internal service interface
3
1
• Supply voltage
• Software sign-of-life
• Operational readiness
• Maintenance request alert
• Fault
• Sample flow
• Sample stream: S1, S2, S3, S4
• Sample components: e.g. CO2,
propane, etc.
• Measured value of sample as numeric value
Desktop or laptop
At least Pentium III
≥ 800 MHz
1 x Ethernet
Windows XP or 7
Gas chromatograph portal,
from version 1.02
© Siemens AG 2015
Process Gas Chromatographs
MicroSAM
Selection and ordering data
Article No.
MicroSAM process gas chromatograph
Basic unit, mounted on holding bracket
For 3 sample streams + 1 calibration stream
For ambient temperatures from -20 to 50 °C
Explosion-proof, for Zone 1 and Class I Div.1
Power supply 24 V DC
For post, pipe or wall mounting
7KQ3101- 7 7 0
Click on the Article No. for the online configuration in the PIA Life Cycle Portal.
Sample
For gaseous sample
0
For gaseous sample (standard UKOG)
8
Workstation operating software
(1 workstation operating software required per GC network)
Without operating software
A
With workstation operating software
B
Additional versions
3
Order code
Add "-Z" to Article No. and specify Order codes.
Application modules
D01, D02, D06, D08, D09, D11
See description at function of application modules
Standard applications with defined hardware
Method development in the application
Standard
Special
application1)
C01
C04
Acceptance and customer information
(in agreement with application laboratory)
Remote acceptance
J01
Factory acceptance, 1 day
J02
Factory acceptance, 2 days
J03
Factory acceptance, 3 days
J04
Repeatability test
Standard (2 hours)
E01
Up to 8 hours
E02
Up to 24 hours
E03
Up to 72 hours
E04
Data transmission
Modbus mapping (during commissioning)
F01
Inputs/outputs via I/O-Extender
Separate supply of the I/O Extender module
(without protective casing, not for hazardous areas)
4 digital inputs, 4 digital outputs, 2 analog inputs, 4 analog outputs
K01
Analog values via external unit (standard package 1); Zones 1 and 2
4 digital inputs, 4 digital outputs, 2 analog inputs, 4 analog outputs
K02
Analog values via external unit (standard package 2); Zones 1 and 2
12 digital inputs, 12 digital outputs, 6 analog inputs, 12 analog outputs
K03
Analog values via external unit (standard package 3); Class I Div 2
4 digital inputs, 4 digital outputs, 2 analog inputs, 4 analog outputs
K04
Analog values via external unit (standard package 4); Class I Div 2
12 digital inputs, 12 digital outputs, 6 analog inputs, 12 analog outputs
K05
Miscellaneous calculations and functions
using BASIC interpreter integrated in the GC
MicroSAM Basic Editor
H01
Application setup: Calculations in accordance with ISO 6976-95
H02
Application setup: Natural gas - calculations in accordance with GPA 2172-96
H03
Application setup: Natural gas - calculations in accordance with GOST 22667-82
H04
Application setup: Natural gas - customer-specific calculations
H05
1)
On request
Siemens AP 01 · 2015
3/23
© Siemens AG 2015
Process Gas Chromatographs
MicroSAM
Support bracket
F01 – Data transmission over Modbus
For easy mounting, incl. support for 8 gas connections
consisting of:
• Mounting part: Dimensions: 380 mm x 110 mm (WxH)
• Bracket for gas connection;
dimensions 146 mm x 110 mm (DxH)
Bracket on right side, mounted at right angle
Implementation and testing of a Modbus table for Modbus
communication (RS 232 / RS 485 RTU).
The bracket is stipulated in the manual.
Exception
The bracket is not required if the MicroSAM is fitted in a
protective casing approved by Siemens. In this case, however,
shipping of the unit is only permissible in this protective casing.
Sample streams
3
For up to 4 sample streams (including calibration stream); e.g.
3 sample streams + 1 calibration stream; controlled by 4 internal
digital outputs (relay contact 0.4 A / 24 V DC)
K0X – Inputs/outputs via I/O Extender
The MicroSAM basic unit provides four digital inputs and
outputs. If more interfaces are required, these are provided by
the I/O Extender. It should be noted, however, that the I/O
Extender requires two device-internal digital inputs and outputs.
The I/O Extender solution can generate up to 12 additional
analog outputs for the chromatograph (further inputs and
outputs on request). The latest generation of NESSI components
for sample preparation can also be controlled. The max. cable
length between MicroSAM (including master cable) and I/OExtender must not exceed 20 m. A 24 V DC power supply is
required for the I/O Extender. This must be provided separately,
but can also be covered by the power supply of the MicroSAM.
Note:
This position contains a basic unit prepared for integration of the
analyzer modules.
If the delivery is to include a protective casing from the Set CV
range, please refer to this category in Catalog AP 01. There you
can find more information on the I/O Extender and its specification within this total solution.
Pos. 8_8: Standard UKOG
K02 or K04 standard packets 1/3
Individual customers standard.
This position includes:
• Mounting rail
• An I/O Extender module
• Protective casing, Ex e with standard cable glands and
terminal block; 170 x 227 x 131 mm (L x W x D)
Pos. 8_0: For gaseous sample
Pos. 9_B: Workstation operating software
The workstation operating software can only be ordered together
with MicroSAM. Workstation operating software is required for
each gas chromatograph network.
C01 – Method development and application
Comprehensive and specific development of the method is
required for the tasks.
The measured components and switching functions are entered
completely using a customer sample (or a specially selected
calibration gas). Proof of repeatability is carried out in accordance with the customer specification.
If a natural gas analyzer for calculation of the calorific value is
ordered, the evaluation parameters are specifically optimized for
the natural gas analysis.
The required BASIC programs (H0X) are installed in the gas
chromatograph.
The retention time window C6+ is set to the measured components n-C6 to C9.
J0X – Acceptance and customer information
The scope of delivery is checked and the documentation and
operation of the device explained in detail during the factory
acceptance.
This also comprises presentation of the analytical solution
including communication, chromatograms, piping plan and gas
path plan. If present, inspection of the sample preparation and
discussion of the documentation are carried out.
Please supplement the order for J02 to J04 by the desired option
from E0x.
Only experienced MicroSAM users should consider the option
for starting up the MicroSAM in the context of remote acceptance, e.g. using a telephone conference (on request).
E0x – Repeatability test
Proof of repeatability over a period of 2 h is included as
standard. Longer proof of repeatability for the unit can be
ordered using the supplements E02 to E04.
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Siemens AP 01 · 2015
The delivery package of the I/O Extender solution for Class I
Div 2 contains adapters (female thread 1", 3/4", 1/2" for fitting of
conduits) which are suitable for cable glands in accordance with
this hazardous area.
K03 or K05 standard packets 2/4
This position includes:
• Mounting rail
• Three I/O Extender modules
• Protective casing, Ex e with standard cable glands and
terminal block; 340 x 170 x 131 mm (L x W x D)
The delivery package of the I/O Extender solution for Class I
Div 2 contains adapters (female thread 1", 3/4", 1/2" for fitting of
conduits) which are suitable for cable glands in accordance with
this hazardous area.
H0X - Various calculations and functions using
BASIC interpreter integrated in the GC
The BASIC programs are either preset ex-works or can be
created and modified by the customer.
H01 – MicroSAM BASIC Editor
The MicroSAM BASIC Editor allows individual programming of
calculations and functions by the user.
© Siemens AG 2015
Process Gas Chromatographs
MicroSAM
H02 - Application setup: Natural gas - calculation in
accordance with ISO 6976-95
Calibration
gas I in
vol.%
Calibration
gas II in
vol.%
Calibration
gas III in
vol.%
1.2-butadiene
–
–
0.1
1.3-butadiene
–
–
0.1
The calorific value is calculated as standard in MJ/m on a molar
basis referred to the reference temperature 25 / 0 °C
(combustion/metering temperature). Calculation on the basis of
other reference variables or tables (in accordance with the
standard) requires unambiguous specification by the customer.
1-butene
–
–
0.1
2.2 dimethylpropane
0.3
0.3
–
cis-2-butene
–
–
0.1
Cyclopropane
–
–
0.1
The BASIC program is preset ex works; a customer modification
is only possible with the supplement H01.
Ethane
4
4
0.1
Ethene
–
–
0.1
H03 - Application setup: Natural gas - calculation in
accordance with GPA2172-96
Ethine
–
–
0.1
Ethyl acetylene
–
–
0.1
The following physical variables must be calculated in accordance with the standard: calorific value, relative density and
compressibility factor.
Helium
–
–
Remainder
Isobutane
0.5
0.5
0.1
Isopentane
0.3
0.3
–
Isopentane
–
–
0.1
Carbon dioxide
2
2
–
Methane
Approx. 85
Approx.
84.5
0.1
The BASIC program is preset ex works; a customer modification
is only possible with the supplement H01.
Methyl acetylene
–
–
0.1
n-butane
0.5
0.5
0.1
H04 - Application setup: Natural gas - calculation in
accordance with GOST22667-82
n-heptane
0.05
0.05
–
n-hexane
0.05
0.05
0.1
The following physical variables must be calculated in accordance with the standard: calorific value, heating value, Wobbe
index, relative density.
n-pentane
0.3
0.3
0.1
Propadiene
–
–
0.1
Propane
2
2
0.1
Propene
–
–
0.1
Oxygen
0.1
–
–
Nitrogen
5
5
–
The BASIC program is preset ex works; a customer modification
is only possible with the supplement H01.
trans-2-butene
–
–
0.1
Vinyl acetylene
–
–
0.1
H05 - Application setup: Customer-specific calculations and
functions
Hydrogen
–
0.5
–
The following physical variables must be calculated in accordance with the standard: calorific value, heating value, Wobbe
index, density, relative density.
3
The calorific value is calculated as standard in BTU/ft3 (S)
referred to the reference temperature 60 °F. Calculation on the
basis of other reference variables or tables (in accordance with
the standard) requires unambiguous specification by the
customer.
These parameters are calculated based on the physical
properties of the pure components. As a special feature, the
methane concentration is defined as the residual value in this
operating mode.
3
Standard calibration gases for system test and run-out
An unambiguous description of the task is required in order to
guarantee correct functioning of the program.
The BASIC program is preset ex works; a customer modification
is only possible with the supplement H01.
The supplement H03 is only possible together with C0X.
Box with I/O Extender
Siemens AP 01 · 2015
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© Siemens AG 2015
Process Gas Chromatographs
MicroSAM
■ Dimension drawings
200
70
12
300
156
20
3
40 34
85
306
20
1
5
4
8
40
220
40
L = 4 000 mm
D 10 (4x)
MicroSAM, dimensions in mm
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Siemens AP 01 · 2015