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© Siemens AG 2007

Process
Gas Chromatographs

2/2 Introduction

2/3 MAXUM edition II


2/3 General
2/14 Documentation

2/15 MicroSAM
2/15 General
2/22 Documentation

2/23 SITRANS CV
2/23 General

Siemens PA 01 · 2008
© Siemens AG 2007

Process Gas Chromatographs


Introduction

■ Overview
Process gas chromatography is one of the most powerful mea-
suring and analysis methods for process engineering. It is a pro-
cedure which is both discrete and extractive. This procedure is
frequently used for online monitoring of processes since the se-
quences are easy to automate and a large number of compo-
nents can be measured simultaneously.
Process gas chromatography can be used to separate and
quantify the components of almost all homogenous gaseous or
liquid mixtures. It must be possible to vaporize the liquid compo-
nents without decomposition. The individual components of a
discrete sample pass through the column system at different ve-
locities, and are recorded in succession by a detector.
The time between sample introduction and registering of a sub-
stance at the detector (the retention time) is a characteristic of
the substance and is used to identify it. The magnitude of the de-
tector signal is a measure of the volume concentration of the
component in the gas.

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© Siemens AG 2007

Process Gas Chromatographs


MAXUM edition II
General

■ Overview ■ Benefits
MAXUM edition II with its combination of different analytical
components offers a wide range of analytical possibilities. It is
therefore possible to solve highly different measuring tasks with
just one product. This reduces the costs for investment, training
and stocking of spare parts.
The MAXUM edition II platform offers:
• Numerous oven configurations
permit an optimum solution for almost every application
• Numerous types of detector and valve
for the optimum analytical solution
• Smart electronics, local operation and central workstation
for fast and simple operation, monitoring and maintenance
• Powerful software for improved results
• Comprehensive I/Os and serial interfaces
for internal and central interfacing
• Versatile networking possibilities
for central maintenance and secure data transfer
• Many analytical possibilities
as result of large application database
• Large and experienced support team provides global sup-
port.
Hardware and software features:
Densification: Use one MAXUM edition II to provide the func-
tionality of several GCs 4
Parallel chromatography: Separate complex analytical tasks
into simple parallel tasks
Cost of ownership: Flexible oven concept results in low con-
sumption of air and energy.

MAXUM edition II
The MAXUM edition II is a universal process gas chromatograph
for flexible process applications with a wide variety of analytical
possibilities. The MAXUM edition II combines various functional
modules with a flexible oven concept and can therefore also op-
timally solve complex applications.
The MAXUM edition II is used in all sectors of the chemical in-
dustry, petrochemicals and refineries. It analyzes the chemical
composition of gases and liquids in all production phases. The
MAXUM edition II is suitable for installation in an analysis cabinet
close to the process or in a close laboratory. Thanks to the flexi-
ble application possibilities, it can be used to analyze the initial
material, the end product and also secondary products. The
MAXUM can also be used for many applications with environ-
mental measurements.
The MAXUM edition II has extremely rugged and specially de-
signed hardware and software. It automatically takes a sample
from the process, and injects it into the chromatographic col-
umns.
With its powerful software and hardware, it satisfies the highest
demands for measurement repeatability, and can be operated
for a long time without manual interventions. Using powerful
communications tools, the MAXUM edition II can send its results
to process control systems and recording devices. The compre-
hensive networking facilities can be applied to use several
MAXUM edition II chromatographs together in large networks.

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Process Gas Chromatographs


MAXUM edition II
General

■ Application Extension of functionality


Network Access Unit (NAU):
Chemical industry
• A MAXUM edition II without analytical section
• Monitoring of benzene in styrene in the ppb range
• Available with or without HMI
• Traces of residual gases in ultra-pure gases
• Has 7 slots for optional I/O plug-in cards
• Determination of traces of hydrocarbons in air separation
plants • Offers central Modbus interfacing of several chromatographs
to the control system
• Fast analysis of CS2 and H2S in seconds
CAN expansion unit:
• Fast measurement of C6 to C8 aromatic compounds including
the measurement of C9+ aromatics For 10 additional I/O plug-in cards which can be controlled over
• Monitoring of hydrogen in chlor-alkali plants the CAN bus.
Can be connected to the NAU or directly to any MAXUM
• Measurement of sulfurous components edition II or MicroSAM chromatograph.
• Measurement of C9 to C18 paraffins
DataNET Hub:
• Determination of vinyl chloride in room air in a 60-second cy-
cle Converts standard Ethernet into a completely redundant Data-
NET. Uses twisted standard pairs or class-fiber technology. Cov-
• Gas analysis during manufacture of vinyl chloride monomer
ers large distances.
(VCM).
Oil & gas ■ Function
• Crack gas analysis
Supply with carrier gas, combustion gas and auxiliary gases
• Natural gas: chromatographic determination of hydrocarbon
dew point and calorific value A gas chromatograph must be supplied with carrier gas and, if
• Fast determination of benzene in naphtha applicable, combustion gas and other auxiliary gases. The car-
rier gas is used to transport the sample through the analytical
• Determination of high boiling aromatics in a distillation fraction system. Auxiliary gases are used to operate valves, as combus-
4 • Fast measurement of acetylene in ethylene
• Total sulfur in petrol and diesel.
tion gases for flame ionization detectors, and to purge the oven.
Injection system
Water/waste water The injection system is the link between the continuous process
• Determination of halogenated hydrocarbons stream and the discrete analytical process. It is responsible for
injecting an exactly defined portion of the sample in a reproduc-
• Simultaneous determination of chlorinated hydrocarbons, aro- ible and pulsed manner (as far as possible) into the carrier gas
matics and alcohols in water stream.
• Wastewater monitoring with PGC and stripper.
The injection can be carried out in the conventional manner us-
Power engineering ing valves or by means of a live injection:
• Power generation in coal-fired power plant. • Gaseous samples (0.1 to 5 ml)
Automotive industry • Vaporizable liquid samples (0.1 to 10 µl)
• Fast analytical measurement of methane in car exhausts Gas injection valves
• High-speed chromatography for small molecules in propel- Model 50 10-port valve:
lants.
• Combined gas injection and backflushing valve
■ Design • Activation by pressure on the diaphragm without moving
parts.
Chromatographic measuring equipment consists of a sampling
Model 11 6-port valve:
system matched to the application, sample conditioning with
switchover to various sample streams, and the gas chromato- • Can be used as gas injection valve, liquid injection valve or for
graph with the analytical and electronic hardware as well as data column switching
processing, operation and communications software. • Diaphragm controlled by tappet
The MAXUM edition II gas chromatograph is divided into three • One million switching cycles without maintenance
sections:
Liquid injection valve FDV
• The upper section contains the electronics with the power
supply, controllers and analog electronics. A constant quantity of a liquid sample can be automatically in-
jected using the liquid injection valve, and subsequently vapor-
• The center section contains the pneumatics and some of the ized rapidly and completely. The valve can also be used to inject
detectors. small volumes of gas.
• The bottom section contains the oven and the complete ana-
lytical components responsible for the separation. The liquid injection valve consists of three sections:
• Thermostatically-controlled vaporization system
The MAXUM edition II is available prepared for wall mounting or
for free mounting on a rack. • Sample passage section with seal
• Pneumatic drive

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© Siemens AG 2007

Process Gas Chromatographs


MAXUM edition II
General

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• Ambient temperature -20 to +150 °C Live injection
• Material of parts wetted by sample: Stainless steel, mat. Oven
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A further important factor for the separating performance is the
• Control pressure 400 to 600 kPa temperature. This has a very high influence on the vapor pres-
• Max. sample pressure 5000 hPa, recommended 0.5 to sure of the individual components, and thus on the diffusion be-
1000 hPa tween the mobile and stationary phases of the column. This in-
• Connections for pipe: 3 mm outer diameter. fluences the retention times, and thus the identification of
components. Therefore very high demands are placed on the
• Live injection temperature stability of the oven and also on the injection equip-
• Flexible selection of the injection volume which is exactly ment and the detectors.
matched to the requirements of the columns is possible with a
live injection. Two different types of oven are available:
Airless oven for extremely stable isothermal oven temperatures
(0.02 °C control accuracy) up to 280 °C.
Airbath oven for
• isothermal (5 to 225 °C) or
• temperature-programmed mode.
Both types of oven are available as
• single ovens or
• dual ovens.
With the dual ovens, two separate heating circuits provide inde-
pendent oven temperatures. It is then possible to carry out two
different applications in one chromatograph.
In order to measure sample components with highly different vol-
atilities, a temperature program is frequently used for the chro-
matographic separation. In this case the column temperature is
continuously increased according to a selectable heating-up
rate. This method (PTGC) is available with the MAXUM edition II.

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Process Gas Chromatographs


MAXUM edition II
General
The internal oven consists of a chamber with low thermal capac- Columns
ity located within the standard oven. It contains the capillary col-
umn used for the separation. The columns are the central component of the chromatograph.
They resolve the gas mixture into its individual components. The
The ovens have separate, independent temperature control. The following distinction is made:
temperature of the internal oven is freely programmable. The • Packed/micropacked columns with internal diameter of 2 to
temperature changes according to the time-dependent profile 5 mm
assigned to the respective analysis. Up to three linear ramps
and four constant periods can be configured. • Capillary columns with internal diameter of 0.15 to 0.53 mm
internal diameter
It is then possible to determine components with low and high
boiling points in one analysis. Laboratory applications can be Packed columns are mechanically stable and simple to handle.
opened up by PTGC for use in the process industry. Capillary columns have a significantly higher separating perfor-
mance, often with a shorter analysis period and lower analysis
"Simulated distillation" is an important application of PTGC in re- temperature.
fineries. The distillation range - a quality criterion for fuels - is
chromatographically traced "online".

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Types of column

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© Siemens AG 2007

Process Gas Chromatographs


MAXUM edition II
General
Column switching systems Model 11 6-port valve:
Process chromatographs are almost always equipped with col- • Can be used as gas injection valve, liquid injection valve or for
umn switching functions. Column switching is understood to be column switching
the combination of several columns in the carrier gas path which • Diaphragm controlled by tappet
are arranged in succession or parallel. These columns usually • One million switching cycles without maintenance
have different separating performances, and are interconnected
by valves for switching over the gas path. A distinction is made Valveless switching technique
between backflushing, cut and distribution.
The valveless live column switching is exactly controlled by elec-
A wide range of techniques is available for column switching. tronic pressure regulators, and prevents falsification of results
since the sample does not come into contact with valves. A spe-
The techniques comprise highly stable diaphragm gas valves, cial pressure-controlled coupling element connects the capillary
diaphragm piston valves, sliding vane rotary valves and also columns.
valveless switching techniques.
This technique is optimally suitable for capillary columns, and of-
Valves fers the best long-term stability and reliability. Live column
Model 50 10-port valve: switching is a technique where backflushing, cut or distribution
• Combined gas injection and backflushing valve is carried out on two different columns without any switching of
valves or other moving components in the separation path.
• Activation by pressure on the diaphragm without moving parts
This is achieved using a unique coupling unit, the live T-piece.
• Switches gas samples at an overpressure of 0 to 5000 hPa Its function is based on a pressure difference controlled by the
electronic precision pressure controllers of the MAXUM edition
II. Because there is no dead volume whatsoever, it is ideally suit-
able for the low flow rates used with capillary columns. Mainte-
nance of the column switching configuration is then superfluous,
the separating performance is improved, and complicated sep-
arating procedures are simplified.

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Column switching systems (examples)

Siemens PA 01 · 2008 4/7


© Siemens AG 2007

Process Gas Chromatographs


MAXUM edition II
General

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Live switching Detectors


Solenoid valve control module Thermal conductivity detectors (TCD) and flame ionization de-
• Contains all control elements in one module in order to reduce tectors (FID) are mainly used in process chromatography. Spe-
downtimes during repairs to a minimum cific detectors such as flame photometer detector (FPD), elec-
tron capture detector (ECD), helium ionization detector (HID) or
• Has 3-way and 4-way distributors for control of many different
4
electrolytic conductivity detector (ELCD) are used to a lesser ex-
types of valve tent.
• Uses separate, plug-on pipe connectors to permit implemen-
tation of variable gas supplies The detector modules described above can be combined to-
gether in many different manners in the MAXUM edition II:
Electronic pressure controller module (EPC) • A maximum of three detector modules can be used in the air-
• Permits exact control of pressure without needle valves. Short- bath oven
ens the setup time since the pressure is set by an operator in- • Up to two modules can be used in the airless oven, the dual
put. airless oven and the ovens with temperature programming
• Permits programmable pressure changes for fast chromatog- • Multiple modules can be operated in parallel at offset times in
raphy and modern applications order to increase the number of analyses within a specific time
• Controls the supply of carrier gas and combustion gas. Avoids • Parallel modules can each be used for one sample stream.
drift and deviations which can occur with mechanical pres- This shortens the total cycle time with multi-stream applica-
sure control. tions
• Parallel use of two identical modules provides redundant mea-
surements which can be compared together, thus reducing
the necessity for calibration

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Process Gas Chromatographs


MAXUM edition II
General

Detector Measured value Selectivity Typical detection limit Application example


dependent on:
Concentration Universal 10 ppm Main and subsidiary
components

Mass stream Hydrocarbons 0.1 ppm Hydrocarbons

Mass stream Substances contai- 0.1 ppm Traces of sulfur in HC


ning S or P matrices

Universal 25 ppb Analysis of ultra-pure


(except He) gases

Mass stream Molecules with elec- 0.1 ppb Traces of halogenated


tro-negative groups substances

Suitable detectors for process gas chromatography

Siemens PA 01 · 2008 4/9


© Siemens AG 2007

Process Gas Chromatographs


MAXUM edition II
General
Thermal conductivity detectors (TCD) Ionization detectors
The measuring principle of the TCD is based on the difference Ionization detectors (e.g. ECD) can be used to determine traces
between the thermal conductivity of a pure carrier gas stream of halogens and also of inert gases down to the ppb range.
and that of a gas mixture containing carrier gas and a compo-
nent eluted from the column. Therefore all components whose Accessories: Catalytic air purifier
thermal conductivity differs from that of the pure carrier gas can Instrument air is usually contaminated by traces of hydrocar-
be detected by a TCD. bons. If this air is used as the combustion gas for a flame ioniza-
TCDs mainly comprise two measuring cells and two reference tion detector (FID), the impurities are evident as disturbing back-
cells which are electrically heated and contain wire resistors ground noise.
connected in the circuit of a Wheatstone bridge. The catalytic air purifier eliminates interfering impurities of hydro-
The bridge resistors are balanced as long as pure carrier gas carbons in the combustion gas for the FID detector. The prod-
flows through the measuring and reference cells. If a mixture of ucts of the catalytic oxidation (H2O, CO2) have no influence on
carrier gas and sample component flows through the measuring the detector. Use of the catalytic air purifier significantly reduces
chamber, the change in thermal conductivity of the gas mixture the background noise. It has a flameproof enclosure and is
also changes the temperature and thus the resistance of the therefore explosion-proof.
heating wires. The air within the purifier is passed through a spiral lined with
The resulting offset in the bridge circuit is directly proportional to palladium. This metal spiral is heated up to approx. 600 °C. Pal-
the current concentration of the sample component in the carrier ladium has a high activity at this temperature, and almost com-
gas stream. plete catalytic oxidization is achieved despite the short dwell
time. The air subsequently passes through a cooling loop, and
Versions of TCDs: is output purified and cooled.
• Thermistor detector Parallel chromatography
• Filament detector
This function divides a complex application into several simple
Both detectors are available for universal use, except that the fil- sub-applications which are analyzed in parallel. This reduces
ament detector is more sensitive than the thermistor detector the cycle times.

4
and can also be used at higher temperatures. The thermistor de-
tector is available as a block with 6 measuring detectors and two The hardware and software of the MAXUM edition II permit a
reference detectors. The filament detector is available as a 4- complex chromatographic analysis to be divided into several
fold block. simple analyses. Each of these simple analyses (referred to as
"Applets") can then be simultaneously executed in parallel. This
Flame ionization detector (FID) not only simplifies the complete analysis, it can also be carried
out faster and with greater reliability.
With the flame ionization detector (FID), the gas mixture leaving
the column is burnt in a hydrogen flame. If this gas mixture con- The ability for dividing the chromatographic measurements into
tains flammable organic compounds, ions are generated during simple, parallel Applets also makes it possible to define stan-
the combustion which are collected on an electrode. dard configurations for frequently encountered applications.
This significantly reduces the requirements for stocking spare
An acceleration voltage is applied between the nozzle from parts, and shortens the cycle times. These standard applets can
which the flame burns and the ion collector electrode positioned be configured on their own or combined depending on the mea-
above it. suring requirements.
The resulting current is amplified, and is the measured signal.
In contrast to the TCD (concentration-dependent signal), the sig-
nal with the FID is proportional to the mass flow of the compo-
nents.
The FID features a linear range of 6-7 powers of ten, and permits
detection limits of less than 0.1 ppm (referred to the concentra-
tion of the hydrocarbon in the sample). Non-flammable compo-
nents (e.g. inert gases and water) cannot be measured with the
FID.
In addition to the carrier gas, hydrogen and air are required as
the flame gases to operate this detector.
Flame photometer detector (FPD)
Further detector principles are used for determination of trace
concentrations of specific components. For example, the flame
photometer detector is used to determine traces of compounds
containing sulfur or phosphor. The emission of light of character-
istic wavelengths is measured when burning the substances in
a hydrogen flame.

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Process Gas Chromatographs


MAXUM edition II
General
State-of-the-art communication Compatibility
TCP/IP communication and standard Ethernet hardware mean MAXUM edition II is compatible with all older types of chromato-
that MAXUM edition II is compatible with many networks. graphs from Siemens: PGC 302, RGC 202, Advance Maxum,
Optichrom Advance.
Software
For simple operation and maintenance, MAXUM edition II offers Application
an online software system with local operation over an HMI and Certain parameters must be observed during application and
a flexible GUI accessible using a computer workstation. subsequent operation of the MAXUM edition II. It can then be
The online software system is installed in every MAXUM edition II determined qualitatively whether the task is fulfilled. The basic
or NAU and contains: prerequisite for this is that all components can be detected
clearly isolated from the interfering components. Important pa-
• pSOS operating system rameters are: Analysis time, measuring ranges, detection limits
• Polyhedra database machine and reproducibility of the results.
• Embedded EZChrom evaluation
• Embedded MaxBasic in the runtime version
• Communications software, network software I/O driver in order
to operate the GC
The workstation software consists of:
• MAXUM edition II workstation tools:
• System manager for network overview
• EZChrom method builder
• MMI maintenance panel emulator
• Data logger
• MODBUS download utility
• Backup and restore utilities
• Online system download utilities
4
• Optichrom Advance APC version 8.1 (emulation of old
Optichrom operation)
• Online help and documentation
and optional packages for individual ordering, e.g.:
• MaxBasic editor
• Simulated distillation method
• Air monitor reporter
• OPC communications server.

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Process Gas Chromatographs


MAXUM edition II
General

■ Technical specifications
General Number of detector modules 1, 2 or 3 in any combination of
detector module types for airbath
Measuring ranges (depending on Thermal conductivity: ovens
application) 0 ... 500 ppm
Sampling and column valves 1 or 2 in any combination of
Flame ionization: 0 ... 1 ppm detector module types for fan-free
Temperature range in oven 5 ... 225 °C ovens
Temperature control ± 0.02 °C Valveless option Diaphragm valves, diaphragm
piston valves, sliding vane rotary
EMI/RFI design CE-compatible; certified accor- valves or slider valves
ding to 89/336/ECC (EMC direc-
tive) Columns "Live" switching
CE-compatible; certified accor- Regulation of gas supply Packed, micropacked or capillary
ding to 73/23/EEC (low-voltage columns
directive)
Electrical characteristics
Tested according to
EN 61010-1/IEC 1010-1 Power supply Single-phase AC,
Calibration 100 ... 130 V or 195 ... 260 V
(selectable), 47 … 63 Hz
• Type Manual or automatic
Single oven: max. 14 A
• Zero value Automatic baseline correction
Dual oven: 2 circuits, max. 14 A
• Span Standard sample cylinder each
Design, enclosure Gas inlet conditions
Mounting Spacing on left: 460 mm from Sample flow 5 ... 20 ml/min (depending on
walls and other devices application)
Spacing on right: 460 mm in all Sample filter size 5 µm

4 cases
Spacing at front: 654 mm in all
cases
Minimum sample pressure
Maximum sample pressure
35 kPa, standard
2070 kPa standard; higher pres-
Wall-mounted units sure as option
Center-to-center: 1120 mm in all Maximum sample temperature 121 °C standard; higher tempera-
cases ture as option
Weight 77 kg Materials wetted by sample SS and Teflon; other materials as
option
Degree of protection IP54, NEMA 3
Liquid injection (valve)
Danger class Standard configurations:
Vaporization temperature 60 ... 400 °C
Certified according to CSA C/US
for use in Class I, Zone 2, Groups Injection volume 0.3 ... 9.5 ml
B,C,D
Ambient temperature -20 ... +150 °C
Suitable for use in Zone 2, Groups
IIB and H2 with local approval Material of parts wetted by sample SS, mat. no. 1.4571, Hastelloy,
Monel or special materials
Suitable for use in non-hazardous
areas and with non-dangerous Control pressure 400 ... 600 kPa
conditions.
Sample pressure Max. 5000 kPa, recommended
Optional configurations: 0,5 ... 1000 kPa
Certified according to CSA C/US Connections for pipe 3 mm outer diameter
for use in Class I, Zone 1, Groups
B,C,D with air or nitrogen purging Measuring response
Certified by CENELEC as EEx Sensitivity (depending on applica- ± 0.5% of span
pedmib IIB + H2 with air or nitro- tion)
gen purging and purging control
for Zone 1 or 2. Linearity (depending on applica- ± 2% of span
tion)
Configuration
Effects of vibrations Negligible
Oven options Single isothermal oven or divided
oven with two independent iso- Repeatability in % of full span bet- 2 and 100%: ± 0,5%;
thermal zones ween 0.05 and 2%: ± 1%;
Single oven or two independent, 50 and 500 ppm: ± 2%;
fan-free ovens. The dual version
5 and 50 ppm: ± 3%;
has two separate oven areas
which operate completely inde- 0.5 and 5 ppm: ± 5%
pendently.
Detection limits See detectors
Detector modules for thermal conductivity, flame ioniza-
Influencing variables
tion, flame photometry, helium
ionization, electrolytic conducti- Effects of ambient temperature None with electronic pressure
vity and electron capture control
Different effects with mechanical
pressure control (depending on
application)

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Process Gas Chromatographs


MAXUM edition II
General
Electrical inputs and outputs Gas supply
Standard input and output 2 analog outputs; Instrument air At least 350 kPa for units with val-
4 digital outputs (1 for output of ves Model 11 or Valco
system faults, 3 are user-configu- At least 825 kPa for units with val-
rable); ves Model 50
4 digital inputs; At least 175 kPa for airbath
1 serial output ovens; 85 l/min per oven
No instrument air for fan-free
Card slots for optional inputs and 2 ovens
outputs
Carrier gas Nitrogen or helium in compressed
Input and output cards AO 8: 8 electrically isolated ana- gas cylinder, purity 99.998%, or
log output channels hydrogen with a purity of 99.999%
D IO: 4 digital inputs and 4 digital (depending on application).
outputs Typical consumption quantity:
A I/O: 2 digital inputs and 2 digital 5100 l/month per detector module
outputs, 2 analog inputs and 2
analog outputs Combustion gas Hydrogen with a purity of
99.999%
Digital inputs Optocoupler with internal power Typical consumption quantity:
supply (12 … 24 V DC); 2000 l/month per detector module
switchable by floating contacts.
Alternative: switchable by exter- Combustion air Reference air (< 1 ppm THC, O2
nal power supply 12 … 24 V DC concentration 20 … 21%). Supply
(only floating relay contacts), through instrument air with cata-
external power supply, negative lytic purification (optional).
connection linked to ground, for a Typical consumption quantity:
specific digital input. 26000 l/month
Digital outputs Floating changeover contacts, Corrosion protection Purging with dry air to protect the

4
max. contact rating: electronics
1 A with 30 V DC. Oven with stainless steel lining
Diode bypass suppression Steel lining painted on outside
should be used for inductive (epoxy powder coating)
loads.
Communication
Analog inputs -20 ... +20 mA in 50 Ω or
Serial output RS 232, RS 485
-10 ... +10 V Rin = 1 MΩ, alternate
insulation up to 10 V Ethernet Standard 10BaseT Ethernet with
RJ45 connectors
Analog outputs 0/4 ... 20 mA in max. 750 Ω, com-
mon negative pole, electrically DataNET Special high-speed TCP/IP net-
isolated from ground; freely-con- work (redundant pair of cables)
nectable to ground Data highway Special serial communication net-
Termination Screw terminal for shielded or work (redundant pair of cables)
solid cable with a maximum area
of 16 AWG or 1.5 mm2
Climatic conditions
Ambient temperature -18 ... 50 °C

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© Siemens AG 2007

Process Gas Chromatographs


MAXUM edition II
General

■ Dimensional drawings




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Notes: Only for airbath oven:


Left outlet for applications with one single oven
Left and right outlets for applications with divided oven
MAXUM edition II, dimensions in mm

Documentation

■ More information
Order No.
Compact Manual
• German C79000-G5300-C568
• English C79000-G5376-C568
• French C79000-G5377-C568
• Spanish C79000-G5378-C568

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© Siemens AG 2007

Process Gas Chromatographs


MicroSAM
General

■ Overview • 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 chloralkali
plant
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 re-
former/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 con-
trol 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
MicroSAM • Analysis of low-boiling hydrocarbons in an ethylene plant/vis-
breaker
The MicroSAM is a miniaturized process gas chromatograph
(GC) in an Ex-d enclosure. Through consistent use of microsys- • Analysis of exhaust gas in flares
tem technology (silicon wafer technology), all analytical compo- • Analysis of gas loop in a propylene oxide plant
nents are concentrated in the smallest possible area. The design • Analysis of CO in crack gas in an LDPE plant
particularly enables a distributed installation close to the pro-
• Analysis of refinery gas in a pilot plant
4
cess.
• Calorific value analysis in natural gas preparation plants
■ Benefits Iron & steel
• The distributed field installation reduces investment costs, • Analysis of exhaust gas in blast furnaces
and opens up new fields of application, e.g.:
- Installation in plant areas where mounting within an analyzer Pharmaceutical industry
shed is not possible • Analysis of O2, N2, CO2 and water in fermenting processes
- Installation at remote locations without extended infrastruc-
ture • Analysis of alcohols in nitrogen for vacuum drying plants
• Reduction in laboratory analyses through online measure- Metals, aggregates, cement
ments • Analysis of mine gas for inert gases and hydrocarbons
• Low space requirements in analysis cabinets reduce invest-
ment costs ■ Design
• Low maintenance requirements and gas/energy consumption
reduce operating costs Enclosure
• High-resolution capillary columns permit fast analyses • EEx-d version standard (according to ATEX II 2G)
• Live injection permits representative sample injections • Heating adjustable from 60 to 165 °C (isothermal)
• Maintenance-free, valveless column switching with electronic • Remote installation close to sampling point
pressure controllers Analytical module
• The use of several micro thermal conductivity detectors (mul-
tidetection) provides exact results and also validation possibil- The compact analytical module contains all functional compo-
ities nents of a chromatograph. The MicroSAM works with:
• Versatile networking possibilities for central maintenance and • Live injection
secure data transfer • Valveless live switching on microchip basis
• Remote monitoring with Windows-based software and Ether- • Standardized analytical modules
net communication • Multidetection through use of up to 8 micro-thermal conductiv-
• Simplified maintenance through replacement of modules ity detectors in smallest possible area (e.g. on all column/
purging outputs and injection)
■ 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

Siemens PA 01 · 2008 4/15


© Siemens AG 2007

Process Gas Chromatographs


MicroSAM
General

■ Function
Live injection Electronic pressure regulators
The MicroSAM has a two-stage injection system. Using a micro A high pressure stability together with rapid changing rates in
injection valve, a defined quantity of sample is first brought up to the hPa range are required for precise and fast switching. This is
the carrier gas pressure. This eliminates the pressure-depen- achieved in the electronic pressure regulators by means of a
dent error in the dosing quantity present with conventional sys- piezo actuator.
tems. In the second stage, the sample is transferred to the col-
umn by a valveless micro injection system (live injection). The Detector
result is an "active" injection. The principle of the micro TCDs (silicon wafer technology) is
The injection volume can be varied time-controlled, and exactly based on the continuous measurement of the different thermal
matched to the column requirements. conductivities of the carrier gas and the components to be mea-
sured.
Valveless live column switching
The measurement can be carried out without falsification by
Because of the high dead volume of conventional valves, only avoiding catalytic effects on the heating wires and maintaining a
the valveless version can be considered for a miniaturized sys- constant flow velocity. This permits consistent in-line detection,
tem. In this case, the generation of differences in flow using sev- i.e. without qualitative or quantitative losses of substances.
eral electronic pressure regulators at appropriate positions of
the column setup causes a change in the flow directions. (The Application modules
system operates according to the Wheatstone principle, but The standardized application modules all contain live injection
pneumatically.) The functions "Cut" and "Backflushing" can then and live switching. Modules A01 to A03 and A09 have four de-
be implemented free of dead volume. tectors and three columns, while A04 to A08, A10 and A11 have
The column system three detectors and two columns.

The column system consists of two or three capillary columns The application modules are suitable for separation of the com-
connected in sequence. Micro TCDs or micro live circuits are in- ponents described below.

4
stalled in sequence ("inline") upstream and downstream of the in-
dividual columns. Three electronic pressure regulators supply
the columns with carrier gas and carry out the switching func-
tions (injection, backflushing and cut).
By using narrow-bore capillary columns, the separation at high
resolution is carried out within a much shorter time, approx. fac-
tor 2 to 3 compared to standard capillary columns.
Detector Column 1 Detector Column 2 Detector Circuit Column 3 Detector
A01
Injection Molecular filter
Sil5 PoraPLOT/Porabond Q
TCD TCD TCD Live H2, (Ar+O2), N2, C1, TCD
C3, C4, C5, C6+ CO2, C2, H2S, H2O
CO
A02
Injection SilicaPLOT
Sil5 Molecular filter
TCD TCD C2, C3, C4 (saturated, TCD Live TCD
C5+ H2, (Ar+O2), N2, C1, C
unsaturated), C5+
A03
Injection Wax ALOX
Sil5 Volatile pole compon- C1, C2, C3, C4
TCD TCD ents such as alcohol, TCD Live TCD
C5+ (saturated,
ether, ketones, aldehy-
des, C7+ unsaturated)

A09
Injection Sil5 Sil5 Porabond Q
TCD Non-polar aromatic TCD Non-polar aromatic TCD Live All components TCD
and aliphatic hydro- and aliphatic hydrocar- except molecular fil-
carbons bons ter components

Application modules A01 to A03 and A09

4/16 Siemens PA 01 · 2008


© Siemens AG 2007

Process Gas Chromatographs


MicroSAM
General

Detector Column 1 Detector Circuit Column 2 Detector


A04
Injection Wax
SilicaPLOT
TCD Volatile pole components such as TCD Live TCD
C2, C3, C4, C5, C6 (saturated,
alcohol, ether, ketones, aldehydes,
unsaturated)
C7+
A05
Injection Wax Wax
TCD Polar aromatic and aliphatic hydro- TCD Live Polar aromatic and aliphatic TCD
carbons hydrocarbons
A06
Injection Sil5 Sil5
TCD Non-polar aromatic and aliphatic TCD Live Non-polar aromatic and aliphatic TCD
hydrocarbons hydrocarbons
A07
Injection Wax Sil5
TCD Polar aromatic and aliphatic hydro- TCD Live Non-polar aromatic and aliphatic TCD
carbons hydrocarbons
A08
Injection Porabond Q
Molecular filter
TCD All components except molecular TCD Live TCD
H2, (Ar+O2), N2, C1, CO
filter components
A10
Injection
TCD
Sil5
Non-polar aromatic and aliphatic TCD Live
Wax
Polar aromatic and aliphatic TCD
4
hydrocarbons hydrocarbons
A11
Injection RTX-5+
RTX-200 SilicaPLOT
TCD Non-polar aromatic and aliphatic TCD Live C2, C3, C4, C5, C6 TCD
hydrocarbons and medium-pole (saturated, unsaturated)
components such as chlorosilane

Application modules A04 to A08 and A10


Application
Various solution concepts are available:
• Adjustment without development of method
- 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 test gas. The measured com-
ponents and switching functions (live injection, backflush-
ing, 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 development of method
Non-standardized applications require specific development
of the method:
An optimum solution is elaborated on the basis of an existing
specification and a selected calibration gas or with applica-
tion of a customer sample.

Siemens PA 01 · 2008 4/17


© Siemens AG 2007

Process Gas Chromatographs


MicroSAM
General

■ Technical specifications
Design, enclosure Sample and injection
Weight 15 kg Sample streams 1
Degree of protection IP65 (NEMA 4X) Calibration sample streams Max. 2
Mounting Phase Gaseous
Installation on Post, pipe or wall Required filtration Degree of separation 99.99% for
< 2 µm particles
Distance from wall or next chroma- 300 mm (12")
tograph Material wetted by the sample Stainless steel, fused silica, polyi-
mide
Distance from ceiling or floor 200 mm (8")
Injection "Valveless" live injection
Explosion protection ATEX II 2 G Ex d IIC T4
Certificate DMT 03 ATEX 069 X • Controller With multifunction diaphragm
valve
FM Class I, Div 1, Groups A, B, C,
D T4, Certificate 3017424, CSA • Injection volume adjustable using 2 ... 50 ml
Class I, Div 1; Groups B, C, D switching times
Support bracket • Max. operating temperature 165 °C
• Mounting part, dimensions (D x H) 380 x 110 mm Oven
• Gas connections 8 Number/type 1/isothermal
• Bracket for gas connection, di- 146 x 110 mm Purging with N2 Possible
mensions (D x H), bracket on right Dimensions (DxH) 160 mm x 10 mm
side, mounted at right angle
Max. heating power 35 VA
Electrical characteristics
Temperature range 60 … 165 °C
Auxiliary power 24 V DC +10/-15%

4
Temperature stability ± 0.1 K (60 ... 165 °C)
Power consumption
Temperature accuracy ± 3 K (60 ... 165 °C)
• Typical 18 VA
Retention time variations per 10 °C Approx. 0.3%
• Maximum 60 VA change in ambient temperature
• Electrical safety IEC 61010/DIN VDE 0411 Heating-up period from 30 ... 10 minutes
EMC immunity According to 100 °C
IEC 60801/DIN VDE 0843 Columns and gases
• Conducted interferences on AC Column type Capillary columns 0.15 ...
supply lines 0.25 mm/internal
- According to Part 4 (burst) 2 kV Column switching Multidimensional chromatography
- According to Part 5 (ms pulses), 1 kV with backflushing and cut in live
line against line system
- According to Part 5 (ms pulses), 2 kV Multifunctional diaphragm valve for injection and backflushing
line against ground Gas connections Pipe 1.5 x 0.25 (approx. 1/16")
• Conducted interferences on signal Pressure regulators Max. 4 single-channel electronic
lines pressure regulators
- According to Part 4 (burst) 1 kV Solenoid valves for control of dia- 2 NC contacts, 2 NO contacts
• Immunity to static discharge phragm valve
- According to Part 2 (ESD) 8 kV Carrier gas H2, N2, He, Ar
• Immunity to fields • Gas purity (minimum requirement) > 99,999%
- According to Part 3 and Part 6 10 V/m • Solid components < 2 µm
• Noise suppression According to CISPR 11/ • Required filtration Degree of separation 99.99% for
EN 55011/DIN VDE 0875 Limit 0.1 mm particles
class B • Consumption 10 ... 60 ml/min
• Fuse 12.5 A • Input pressure 500 … 700 kPa
Gas inlet conditions Instrument air Not required
Permissible sample pressure 10 … 50 kPa Detectors, calibration and perfor-
Sample flow 20 … 100 ml/min mance data
Max. sample temperature 120 °C Detector type TCD, max. 8 sensors
Solid components < 0.1 mm Ambient temperature Negligible
Climatic conditions Vibrations Negligible
Permissible ambient temperature -20 ... 55 °C Cell volume 0.02 ml
Permissible storage/transport tem- - 30 ... 70 °C Calibration Manual or automatic, single-level
perature or multi-level
Permissible relative humidity Max. 90% Smallest measuring range 300 ppm
Linear range > 104
Cycle time Typically 30 … 120 s

4/18 Siemens PA 01 · 2008


© Siemens AG 2007

Process Gas Chromatographs


MicroSAM
General
Electrical inputs and outputs
Basic equipment
• Digital outputs (relay contact 2, freely-usable (expandable by
0.4 A/24 V DC) NAU, see communication)
• Digital inputs (24 V to optocoupler) 2, freely usable (expandable by
NAU, see communication)
Interfaces
• Communication 1 x Ethernet 10BaseT/TCP/IP
• Control system coupling 1 x RS 485 or RS 232/
MODBUS RTU, OPC (ODPC) over
Ethernet
Electronics
Communication and analytical cont-
roller (CAC)
• Microprocessor Intel 586 architecture
• Flash EPROM 128 MB
• Dynamic RAM 64 MB
• Operating system Windows CE 3.0
• Software Preinstalled. Modifications or
upgrades for operation PC down-
loadable via network or locally
Realtime signal processor (RSP)
• Microprocessor Motorola 68376, 20 MHz
• Flash EPROM
• Static RAM
1 MB
1 MB
4
• Operating system Forth
• Software Preinstalled. Modifications or
upgrades downloadable via inter-
nal service interface
Controller
• Sample streams 3
• Calibration sample streams 1
• Status LEDs for Supply voltage, software, heart-
beat, ready, maintenance
request, fault, sample flow
Recommended operating unit
• Personal computer Desktop or laptop
• Processor At least Pentium III
• Clock 800 MHz
• Interfaces 1 x Ethernet
• Operating system Windows 98, NT, 2000 or XP
• Software Advance System Tools,
version 4.0 or later

Siemens PA 01 · 2008 4/19


© Siemens AG 2007

Process Gas Chromatographs


MicroSAM
General

Selection and ordering data Order No. Cannot be combined


MicroSAM process gas chromatograph F) 7KQ3101- 7 7 7 0
Basic unit, mounted on holding bracket
Explosion-proof, for Zone 1
24 V DC auxiliary power
For post, pipe or wall mounting
For gaseous sample 0
Workstation operator software
(1 operator software workstation required per GC network)
Without operator software A
With workstation operator software B
Version
Separately supplied basic unit and application module. Parameter set A
(on CD-ROM)
Fully mounted unit with basic parameterization, ready for user-specific settings, incl.. B
system checkout
Further versions Order code
Add "-Z" to Order No. and specify order code
Application modules A01 to A11
See description at function of application modules
Standard applications with predefined hardware
User-specific setting
During commissioning B01
During RUN-OUT ex factory, incl.. adjustment of oven temperature, carrier gas pres- B02 B01, C0x
sures and switching functions
Method development and application
4 (specified by application laboratory)
Very simple application C01
Simple application C02
Medium application C03
Special application (incl. production of a special application module) C04
Acceptance and customer information
(in agreement with application laboratory)
Remote acceptance D01 B01
Factory acceptance, 1 day D02 B01
Factory acceptance, 2 days D03 B01
Factory acceptance, 3 days D04 B01
Repeatability test
Standard E01 B01
Up to 8 hours E02 B01
Up to 24 hours E03 B01
Up to 72 hours E04 B01
Data transmission
Modbus mapping (during commissioning) F01
Data transmission analog and operator panel (MMI)
Analog values via external unit; 2 analog values (standard package); 230 V G01
Analog values via external unit; 2 analog values (standard package); 115 V G02
Expansion: Ethernet 10Base FO (glass fiber) G03
Expansion: MODBUS Map in the NAU G04
Expansion: Module with 8 analog outputs G05
Expansion: Module with 4 digital outputs/4 digital inputs G06
Expansion: Module with 2 DO/2 DI/2 AO/2 AI G07
Expansion: Operator panel (MMI) G08
Customized parameterization G09
Diverse calculations and functions
by means of BASIC interpreter integrated in 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 GPA 8 H04
Application setup: Natural gas - customer-specific calculations H05
F) Subject to AL export regulations: 9I999, ECCN: 5D002ENC3

4/20 Siemens PA 01 · 2008


© Siemens AG 2007

Process Gas Chromatographs


MicroSAM
General

Calibration Calibration Calibration


gas I in Vol% gas II in Vol% gas III in Vol%
1,2-butadiene – – 0.1
1,3-butadiene – – 0.1
1-butene – – 0.1
2,2 dimethylpropane 0.3 0.3 –
cis-2-butene – – 0.1
Cyclopropane – – 0.1
Ethane 4 4 0.1
Ethene – – 0.1
Ethine – – 0.1
Ethyl acetylene – – 0.1
Helium – – Residual
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
Methyl acetylene – – 0.1
n-butane 0.5 0.5 0.1
n-heptane
n-hexane
0.05
0.05
0.05
0.05

0.1
4
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 –
trans-2-butene – – 0.1
Vinyl acetylene – – 0.1
Hydrogen – 0.5 –
Standard calibration gases for system test and run-out

Siemens PA 01 · 2008 4/21


© Siemens AG 2007

Process Gas Chromatographs


MicroSAM
General

■ Dimensional drawings

  






 
  
/ PP

4
1 5





4 8

'  [

MicroSAM, dimensions in mm

Documentation

■ More information
Order No.
Manual C79000-D5300-C564
Compact Manual
• German C79000-G5300-C568
• English C79000-G5376-C568
• French C79000-G5377-C568
• Spanish C79000-G5378-C568
• Italian C79000-G5372-C568

4/22 Siemens PA 01 · 2008


© Siemens AG 2007

Process Gas Chromatographs


SITRANS CV
General

■ Overview ■ Design
Enclosure
• EEx-d version standard (acc. to ATEX II 2G)
• Heating adjustable from 60 to 165 °C (isothermal)
• Remote installation close to sampling point
Analytical module
The compact analytical module contains all the functional com-
ponents of a chromatograph. The SITRANS CV operates with:
• Live injection
• Valveless live switching on microchip basis
• Standardized analytical modules
• Multidetection through use of up to 8 micro thermal conductiv-
ity detectors in smallest possible areas (e.g. on all column/
purging outputs and injection)

■ Function
SITRANS CV
Live injection
The new SITRANS CV gas chromatograph (GC), which is based
on the innovative analytical technology of the MicroSAM, is an The SITRANS CV has a two-stage injection system. Using a mi-
analyzer that has been specially developed for natural gas anal- cro injection valve, a defined quantity of sample is first brought
ysis. The device concept enables the higher and lower calorific up to the carrier gas pressure. This eliminates the pressure-de-
value, standard density and Wobbe index (according to ISO pendent error in the injection quantity that prevails on conven-
tional systems. In the second stage, the sample is transferred to
4
6976) to be determined in a way that is not only cost-effective,
but also quick, precise and reliable. the column by a valveless micro injection system (live injection).
The result is an "active" injection.
■ Benefits The injection volume can be varied time-controlled, and exactly
matched to the column requirements.
Flexible installation: The rugged and compact design enables
installation in even extreme areas of application, such as off- Valveless live column switching
shore exploration, or directly at the pipeline. The SITRANS CV
Because of the high dead volume of conventional valves, only
has the certification required (such as explosion protection or
the valveless version can be considered for a miniaturized sys-
splashwater protection) to meet the requirements of these appli-
tem. In this case, the generation of differences in flow using sev-
cations.
eral electronic pressure regulators at appropriate positions of
Like the MicroSAM, the SITRANS CV consists of a basic unit and the column setup causes a change in the flow directions. (The
an analysis module, which, if necessary, can be replaced in as system operates according to the Wheatstone principle, but
short a time as possible. Combined with low power and gas con- pneumatically.) The functions "Cut" and "Backflushing" can then
sumption, this keeps operating costs down. be implemented free of dead volume.
Notable features of the CV Control software, which has been The column system
specially developed for calibration-related applications, in-
cludes its ease of operation and transparency. The column system consists of three capillary columns con-
nected in sequence. Micro TCDs or micro live circuits are in-
The automatic method optimization integrated in the software in- stalled in sequence ("inline") upstream and downstream of the in-
creases the repeatability of the calorific value measurement and dividual columns. Three electronic pressure regulators supply
reduces the cost of ownership. the columns with carrier gas and carry out the switching func-
tions (injection, backflushing and cut).
The serial RS 485 and Ethernet interfaces enable communica-
tion with both the control system and a flow computer. By using narrow-bore capillary columns, the separation at high
resolution is carried out within a much shorter time, approx. fac-
Like the MicroSAM, the unit’s high analytical capability can be at-
tor 2 to 3 compared to standard capillary columns.
tributed to narrow-bore capillary columns, live injection, live
switching and in-line detection. Electronic pressure regulators

■ Application A high pressure stability together with rapid changing rates in


the hPa range are required for precise and fast switching. This is
• Analysis of natural gas in power plants: achieved in the electronic pressure regulators by means of a pi-
- For quality control ezo actuator.
- For turbine optimization
Detector
- Pipeline monitoring
• Analysis of natural gas when opening up sea beds (off-shore The principle of the micro TCDs (silicon wafer technology) is
facilities) based on the continuous measurement of the different thermal
conductivities of the carrier gas and the components to be mea-
• Analysis of bio-natural gas in preprocessing plants sured.
• Analysis of natural gas in liquefaction and regasification plants
(LNG Regasification & Storage) The measurement can be carried out without falsification by
avoiding catalytic effects on the heating wires and maintaining a
• Analysis of calorific value in natural gas for power plants, in constant flow velocity. This permits consistent in-line detection,
gas transfer stations, or during turbine optimization i.e. without qualitative or quantitative losses of substances.
• Calorific value analysis in natural gas preparation plants

Siemens PA 01 · 2008 4/23


© Siemens AG 2007

Process Gas Chromatographs


SITRANS CV
General
Module
The standardized application module contains live injection and
live switching, and has four detectors and three columns.
Detector Column 1 Detector Column 2 Detector Circuit Column 3 Detector
C09 Sil5 Sil5 Porabond Q
Injection TCD Non-polar aromatic TCD Non-polar aromatic TCD Live All components except TCD
and aliphatic hydro- and aliphatic hydro- molecular filter compo-
carbons carbons nents

Application tion, the ambient temperatures of the calibration gas cylinders


during transportation and operation, potential condensation of,
The SITRANS CV is a storage product. Precalibration is carried for instance, higher hydrocarbons in a calibration gas cylinder,
out at the factory, using helium (as the carrier gas) and a test and the functionality of the sample preparation device.
gas. The measured components and switching functions (live in-
jection, backflushing, cut) are saved in the GC. The calibration Under optimum conditions, the SITRANS CV achieves an MPE of
process itself should be performed during commissioning on- < 0.1% for the calorific value and standard density.
site.
SITRANS CV is designed for measuring different types of natural
Table 1: Measurements can be made within the following work- gas. The table below lists the typical specifications of natural
ing ranges: gases (measured and residual components):
Component Smallest working Largest working Table 3:
range (in %) range (in %)
Dutch natu- Russian Algerian LNG
Methane 90 ... 100 55 ... 100 ral gas natural gas natural gas
Nitrogen1) 0 ... 0.1 0 ... 25 Helium 0.035 0.007 0.150 0.045
Carbon dioxide 0 ... 0.1 0 ... 20 Nitrogen 2.072 0.873 5.493 0.948
Ethane 0 ... 1 0 ... 20 CO2 1.131 0.102 0.210 0.000

4 Propane
i-butane
0 ... 1
0 ... 0.5
0 ... 10
0 ... 5
Hydrogen
CO
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
n-butane 0 ... 0.5 0 ... 5 Methane 90.179 98.022 83.774 89.373
Neopentane 0 ... 0.1 0 ... 1 Ethane 4.976 0.701 7.660 7.793
i-pentane 0 ... 0.15 0 ... 1 Propane 1.161 0.204 1.892 1.421
n-pentane 0 ... 0.15 0 ... 1 i-butane 0.144 0.035 0.256 0.178
Hexane+2) 0 ... 0.1 0 ... 3 n-butane 0.186 0.035 0.345 0.238
Helium No measured compo- Concentration can be Neopentane 0.005 0.0005
nent entered as a fixed
value in the compon- i-pentane 0.038 0.007 0.070 0.001
ents list n-pentane 0.031 0.005 0.079 0.001
H2 S No measured compo- < 500 ppm Hexane+ 0.047 0.009 0.071 0.002
nent
O2+Ar 0.000 0.000 0.000 0.000
Standard measuring ranges of natural gas components
1) H2S < 10 mg/m3 < 50 mg/m3 < 10 mg/m3 < 10 mg/m3
Any oxygen or carbon present in the sample will be detected along with
the nitrogen and, therefore, taken into account when the nitrogen concen- Mercaptan < 20 mg/m3 < 20 mg/m3 < 20 mg/m3 < 20 mg/m3
tration is determined. sulfur
2)
Hexane+ = iso/n-hexane to iso/n-nonane H2O Dew point Dew point Dew point Dew point
Table 2: < ground < ground < ground < ground
temp. for line temp. for line temp. for line temp. for line
Concentration range (mol.%) Repeatability according to pressure in pressure in pressure in pressure in
ISO 6974-3 (2000); rel. standard dev. each case each case each case each case
(in %)
Total 100.000 100.000 100.000 100.000
50 < xi < 100 ± 0.1
Calorific 39061.265 37811.062 39604.232 40797.089
1 < xi < 50 ±1 value
(KJ/m3)
0.1 < xi < 1 ±3
Heating 35250.449 34055.754 35789.664 36842.640
xi < 0.1 ± 0.003% absolute value
The repeatability of the measured components satisfies the criteria of ISO (KJ/m3)
6974-3 (2000) Density 0.75617 0.69388 0.79422 0.75555
(kg/m3)
The repeatability of the calorific value and standard density
achieve a relative standard deviation of < 0.015%. Z factor 0.99764 0.99796 0.99752 0.99750

Maximum permissible error (MPE) of the gas chromatograph: Composition of Dutch, Russian and Algerian natural gas, as well as LNG
The calibration gas is an extremely important factor for consid-
eration in terms of the MPE, and has a significant effect on the
accuracy of the overall measuring system. For this reason, SI-
TRANS CV - based on a comparative measuring procedure -
can never be more accurate than the calibration gas used. Other
parameters besides the accuracy data on the calibration gas
certificate have a part to play when considering the accuracy of
a system. Examples of these include the optimum gas composi-

4/24 Siemens PA 01 · 2008


© Siemens AG 2007

Process Gas Chromatographs


SITRANS CV
General

■ Technical specifications
Climatic conditions Oven
Permissible ambient temperature -20 ... 55 °C (depending on oven Number/type 1/isothermal
temperature)
Purging with N2 Possible
Permissible storage/transport tem- -30 ... 70 °C
perature Dimensions (D x H) 160 x 10 mm

Permissible relative humidity Max. 90% Max. heating power 35 VA

Protection against dust and humi- Temperature range 60 ... 165 °C


dity Temperature stability ± 0.1 K (60 ... 165 °C)
• According to EN 60529/IEC 60529 IP65 Temperature accuracy ± 3 K (60 ... 165 °C)
• According to NEMA 250 NEMA 4X Retention time variations per 10 °C Approx. 0.3%
Power supply change in ambient temperature

Auxiliary power 24 V DC +10/-15% Warm-up period from 30 ... 100 °C 10 minutes

External fuse T 2.5 A Columns and gases

Power consumption, typical 18 VA Column type Capillary columns


0.15 ... 0.25 mm ∅internal
Power consumption, maximum 60 VA
Column switching Multidimensional chromatography
Dimensions and weights with backflushing and cut in live
system
Width x depth x height 360 x 300 x 220 mm (approxima-
tely 14" x 12" x 9") Multifunctional diaphragm valve For injection and backflushing
Weight 15 kg (35 lb) Gas connections Swagelok 1/8"
Mounting Pressure regulator Max. 4 single-channel electronic
pressure regulators

4
Installation on Post, pipe or wall
Solenoid valves for control of dia- 2 NC contacts, 2 NO contacts
Distance from wall or next chroma- 300 mm (12") phragm valve
tograph
Carrier gas He
Distance from ceiling or floor 200 mm (8")
• Gas purity (minimum requirement) ≥ 99.999% (5.0)
Electromagnetic compatibility
• Solid components < 2 µm
Noise suppression According to
CISPR 11/EN 55011/ • Required filtration Degree of separation 99.99% for
DIN VDE 0875 Limit class B < 0.1 µm particles
EMC immunity According to • Consumption 10 ... 60 ml/min
IEC 60801/DIN VDE 0843
• Input pressure 500 ... 700 kPa
Conducted interferences on AC
supply lines Instrument air Not required

• According to Part 4 (burst) 2 kV Sample and injection

• According to Part 5 (ms pulses), 1 kV Sample streams 3


line against line Calibration sample streams 1
• According to Part 5 (ms pulses), 2 kV Phase Gaseous
line against ground
Permissible sample pressure 10 ... 500 kPa, but at least 200
Conducted interferences on signal kPa under carrier gas pressure.
lines NOTICE: Sample must not con-
• According to Part 4 (burst) 1 kV tain acetylene!

Immunity to static discharge Sample flow 20 ... 100 ml/min

• According to Part 2 (ESD) 8 kV Max. sample temperature 120 °C

Immunity to fields Solid components < 2 µm

• According to Part 3 and Part 6 10 V/m Required filtration Degree of separation 99.99% for
< 0.1 µm particles
Safety
Material with which the sample Stainless steel, fused silica, polyi-
Electrical safety IEC 61010/DIN VDE 0411 comes into contact mide
Explosion protection ATEX II 2 G EEx d IIC T4 Injection "Valveless" live injection
FM Class I, Div 1, Groups B, C, D T4 Controller With multifunctional diaphragm
FM Class I, Zone 1, Group IIB+H2 T4 valve
CSA Class I, Div 1, Groups B, C, Injection volume adjustable using From 2 ... 50 µl
D T4; Enclosure Type 4X switching times

Siemens PA 01 · 2008 4/25


© Siemens AG 2007

Process Gas Chromatographs


SITRANS CV
General
Detectors, calibration and perfor-
mance data
Detector type TCD, max. 8 sensors
Cell volume 0.02 ml
Calibration Manual or automatic, single level
Repeatability for calorific value and ≤ 0.01%
density
Accuracy for calorific value and ≤ 0.1%
density
Linear range Typically ≥ 104
Cycle time 180 s
Ambient temperature influence Negligible
Influence of vibrations Negligible
Mean Time to Repair/MTBF < 1 hour/3 years (without con-
sumables)
Electronics: Communication and
analytical controller (CAC)
Microprocessor Intel 586 architecture
Flash EPROM 128 MB
Dynamic RAM 64 MB
Operating system Windows CE 3.0
Software Preinstalled. Modifications or

4
upgrades for operation PC down-
loadable via network or locally
Electronics: Realtime signal pro-
cessor (RSP)
Microprocessor Motorola 68376, 20 MHz
Flash EPROM 1 MB
Static RAM 1 MB
Operating system Forth
Software Preinstalled. Modifications or
upgrades downloadable via inter-
nal service interface
Interfaces
Communication 1 x Ethernet 10BaseT/TCP/IP
Control system coupling 1 x RS 485 DSfG to DVGW G 485
Inputs/outputs: Basic equipment
Digital outputs (relay contact 0.4 4, 3 x samples, 1 x calibration
A/24 V DC)
Digital inputs (24 V to optocoupler) 4, for 1 = sample flow; 2 = time
synchronization; 3 = revision
(results have no effect on average
values); 4 = calibration
Status indicator
LEDs for Supply voltage
Software Heartbeat
Ready
Maintenance request alert
Fault
Sample flow
Recommended operating unit
Personal computer Desktop or laptop
Processor At least Pentium III
Clock ≥ 800 MHz
Interfaces 1 x Ethernet
Operating system Windows XP
Software CV Control as of version 1.16.0.0

4/26 Siemens PA 01 · 2008


© Siemens AG 2007

Process Gas Chromatographs


SITRANS CV
General

Selection and ordering data Order No. Ambient temperatures


SITRANS CV process gas chromatograph F) 7KQ3105- 7 The chromatograph is designed for ambient temperatures from
Basic unit, mounted on holding bracket -20 °C to +55 °C as standard.
Explosion-proof, for Zone 1
24 V DC auxiliary power A solution (in tempered casing) is also available as an option for
For 3 sample flows + 1 calibration flow temperatures outside the limits specified above.
For ambient temperatures of -20 to +55 °C
Stand-alone communication via 1 RS 485 interface Communication
(MODBUS RTU)
For post, pipe or wall mounting SITRANS CV has 1 serial interface (RS 485, MODBUS RTU).
Includes CV Control operator software (English) A standard Modbus mapping (see manual) is included. It is op-
erated using an internal Ethernet interface (TCP/IP).
Applications
For standard calorific value analysis (N2, CO2, C1-C5,
Other serial and analog (4 to 20 mA) interfaces are available as
C6+) according to ISO 6976 an option; these can be ordered as a supplementary solution
package.
- Not certified - 0
For standard calorific value analysis (N2, CO2, C1-C5, Documentation
C6+) for CIS countries 8 The documentation contains a CD-ROM version of the
Further versions Order code SITRANS CV Manual in English and German.
Add "-Z" to Order No. and specify order code The manual contains chromatograms of the test gas and typical
Acceptance and customer information natural gases.
(in agreement with application laboratory)
CV Control operator software
Remote acceptance D01
The operator software (language: English) is included in the
Factory acceptance, 1 day D02
scope of supply.
Factory acceptance, 2 days (only in conjunction with D03
D02 or D03) Order No. Pos. 8: Applications

4
Repeatability test These positions contain a general system check of the basic unit
Up to 8 hours (only in conjunction with D02) E02 and C09 integrated application module. The module and basic
unit are described in the manual. Currently, only the original
Up to 24 hours (only in conjunction with D02) E03
master setup is available as he standard method. Other country
Up to 72 hours (only in conjunction with D02) E04 or user-specific method setups can be supplied on request. The
F) Subject to AL export regulations: 9I999, ECCN: 5D002ENC3 performance record ex works contains the analysis check, in-
cluding a repeatability record (4h test).

Test gas 1 in vol.% Order No. Pos. 8_0: Applications - Standard calorific value
analysis - Not certified
Nitrogen 5
This application comprises the standard calorific value analysis
Oxygen 0.1
for the non-certified range. The chromatograph’s measurement
Carbon dioxide 2 method is set at the factory, using a synthetic natural gas mixture
Carbon monoxide 0.5 (test gas 1). The performance parameters for the individual com-
ponents, specified in Tables 1 and 2 and the physical dimen-
Methane 85 sions, apply here.
Ethane 4 The calorimetric values are calculated on the basis of ISO stan-
Propane 2 dard 6976-95 as standard. The reference states for the combus-
Isobutane 0.5
tion/gas volume that must be specified for calculation purposes
are preset to the default state (Tb = 25 °C, Tn = 0 °C) and can be
n-butane 0.5 easily changed to other reference states during commissioning,
2.2 dimethylpropane 0.3 using the operator software.
Isopentane 0.3 The standard method (original master setup) is installed in the
chromatograph, and two CD-ROMs are supplied with the follow-
n-pentane 0.3
ing:
n-hexane 0.05
• SITRANS CV Software Upgrade (including the Manual and
Standard test gases for standard calorific value analysis original master setup A09, as well as country-specific master
setups)
Support bracket
• Analytical module documentation (including documentation
For easy mounting, incl. support for 8 gas connections consist- for the individual module with TCD bridge voltages and EPC
ing of: pressures, as well as module-specific hardware setups)
Mounting part: Dimensions 380 x 110 mm (W x H) Order No. Pos. 8_8: Application - Standard calorific value
analysis - For CIS countries
Bracket for gas connection: Dimensions 146 x 110 (D x H),
bracket on right side, mounted at right angle Required for final determination of analyzer for CIS countries
(former Soviet Union); the product name in these countries, such
Sample flow switchover as Russia or the Ukraine, is MicroSAM. The country-specific
The chromatograph enables automatic selection and switchover master setup "CIS" (containing the calculation in accordance
of 3 sample flows and 1 calibration flow. The DO signal from the with GOST 22667) must be loaded during startup.
GC requires an external relay for the solenoid valve. A sample
flow selector/sample preparation device can be ordered sepa-
rately.

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© Siemens AG 2007

Process Gas Chromatographs


SITRANS CV
General
D01 - Acceptance and customer information - Factory accep- The test gases have the following uncertainties:
tance, visual check, 1 day
Proportions of component Uncertainty (or smaller)
The scope of supply is checked and the documentation and op- materials (Mol.%)
eration of the unit explained as part of the factory acceptance 0.1 to 0.25 ± 5.00%
process. The factory acceptance does not include another unit
performance record. 0.25 to 1 ± 1.00%
1 to 10 ± 0.50%
D02 - Acceptance and customer information - Factory accep-
tance with performance record, 1 day 10 to 100 ± 0.20%

Any performance records required in addition to the original The test gases specified in Table 4 are set at the factory, as part
record supplied have considerably higher demands in terms of of the acceptance for the linearity test, and are available free of
production/application and logistics. When it comes to demon- charge.
strating a fully functional unit as part of the factory acceptance
If the customer specifies other test gases with different compo-
process, this is no exception.
sitions or higher uncertainty requirements, they must provide
If requested by the customer, a country-specific method (master these gases for acceptance purposes. As an option, Siemens
setup methods, available soon) that has not been preinstalled can procure these special test gases (subject to a charge).
can be set at the factory as part of the factory acceptance pro-
cedure.
The performance range of the tests to be performed is listed in
Tables 4 and 5 below.
D03 - Acceptance and customer information - Factory accep-
tance, from 2nd day
Only in conjunction with D01 or D02.
E0x - Repeatability test

4 A tested repeatability record for 4 h is included as standard.


Longer repeatability records for the unit can be ordered by
means of the supplementary item E0x.
E01 to E03 - Repeatability test, 8 h - 24 h - 48 h
Only in conjunction with D02.
Table 4: Recommended test gases for linearity test during ac-
ceptance
Component Gas #1 (Mol.%) Gas #2 (Mol.%) Gas #3 (Mol.%)
Methane Residual (appro- Residual (appro- Residual (appro-
ximately 75) ximately 85) ximately 96.5)
Nitrogen 15.5 5 2.5
Carbon dioxide 0.5 2 0.1
Ethane 8 4 0.5
Propane 0.5 2 0.15
i-butane 0.15 0.5 0.03
n-butane 0.15 0.5 0.03
Neopentane 0.08 0.3 0.03
i-pentane 0.08 0.3 0.03
n-pentane 0.08 0.3 0.03
Hexane 0.05 0.1 0.015

Table 5: Test performance range, acceptance and customer in-


formation
Record of component isolation According to current chromato-
gram display, 5 analyses
Stability test (repeatability) Acc. to order E01 to E03
Performance criteria acc. to table
Linearity test With 3 different calibration gases
(N2, CO2, C1-C5);
10 analyses per calibration gas
Calculation test Comparison of the values calcula-
ted by CV Control with a customer
comparison procedure (optional)
Auto-calibration function
Alarm and event messages Simulation of alarm situations; as
per customer requirement

4/28 Siemens PA 01 · 2008


© Siemens AG 2007

Process Gas Chromatographs


SITRANS CV
General

■ Dimensional drawings

  






 
  
/ PP

4
1 5





4 8

'  [

SITRANS CV, dimensions in mm

Siemens PA 01 · 2008 4/29


© Siemens AG 2007

Process Gas Chromatographs


SITRANS CV

7
4/30 Siemens PA 01 · 2008

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