Metrohm NIRS XDS User manual

NIRS XDS Process Analyzer
Hardware & Installation Manual
8.928.8001EN

Metrohm Applikon B.V.
Schiedam
The Netherlands
Phone [phone]
Fax [phone]
[email protected]
www.metrohm-applikon.com
NIRS XDS Process Analyzer
Hardware & Installation Manual
8.928.8001EN November 2016 JZa

Metrohm Applikon B.V.
Schiedam
© 2017, Metrohm Applikon B.V.
All rights reserved. This manual is protected by copyright law. Without the prior written approval of
Metrohm Applikon B.V., this manual and any contents thereof may not be reproduced, stored or
made public in any form by any means.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
NIRS XDS Process Analyzer ￭￭￭￭￭￭￭￭ III
Table of contents
1 General 1
1.1 Warranty ................................................................................ 1
1.1.1 Warranty (guarantee) ............................................................... 1
1.2 About the documentation ................................................... 1
1.3 Safety instructions ................................................................ 2
1.3.1 General notes on safety ........................................................... 2
1.3.2 Electrical safety ........................................................................ 2
1.3.3 Potentially hazardous solvents and chemicals ........................... 3
1.3.4 Recycling and disposal ............................................................. 3
1.4 List of abbreviations ............................................................. 4
2 Introduction 5
3 Overview of the instrument 8
3.1 Exterior view of the Analyzer .............................................. 8
3.1.1 Front view of the analyzer ........................................................ 8
3.1.2 Left side view of the analyzer ................................................... 9
3.1.3 Right side view of the analyzer ............................................... 11
3.1.4 Top view of the analyzer ........................................................ 14
3.2 Interior view of the analyzer ............................................. 15
4 Overview of the accessories 17
4.1 Optical fibers ....................................................................... 17
4.1.1 Single fibres ........................................................................... 17
4.1.2 Microbundle fibres ................................................................. 17
4.1.3 Fibres connectors ................................................................... 18
4.2 Probes .................................................................................. 19
4.2.1 Probe types ........................................................................... 19
4.2.2 Probe disassembly ................................................................. 20
4.2.3 Probe drawings ..................................................................... 24
4.3 XDS Process Options .......................................................... 26
4.3.1 Multiplexer ............................................................................ 26
4.3.2 Fiber optic communication modem ........................................ 26
4.3.3 Purged System for Hazardous Environments ........................... 27
4.4 Instrument with Accessories ............................................. 28
4.4.1 Single Point ........................................................................... 28
4.4.2 Multiplexer ............................................................................ 29
5 Technical specifications 31
5.1 Basic Unit with Heat sink and Fans dimensions .............. 31

Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
IV ￭￭￭￭￭￭￭￭ NIRS XDS Process Analyzer
5.2 Basic Unit with Vortex Cooling dimensions ..................... 32
5.3 Basic Unit with Air Conditioning dimensions ................... 33
5.4 Purged Unit with Vortex cooling ....................................... 34
5.5 Purged Unit with AC cooling ............................................. 35
5.6 Weight ................................................................................. 35
5.7 Operating Temperature Range .......................................... 36
5.8 Operating Humidity Range ................................................ 36
5.9 Mains connection ............................................................... 36
5.10 Air Consumption ................................................................. 37
5.11 Scan Range .......................................................................... 37
5.12 Data Interval ....................................................................... 37
5.13 Clock/ Oscillator Frequencies ............................................. 37
5.14 Lamp Source ...................................................................... 37
5.15 Communication ................................................................... 38
5.16 Process communication ..................................................... 38
6 Installation 39
6.1 Mounting of the XDS Process Analyzer Enclosure .......... 39
6.2 Removal of Shipping Restraints ........................................ 41
6.3 Fiber optics .......................................................................... 43
6.4 Cable Tray ............................................................................ 43
6.5 Multiplexer .......................................................................... 44
6.6 Electrical connection .......................................................... 44
6.6.1 Permanent mains cable .......................................................... 44
6.6.2 AC Power Switch Settings ...................................................... 45
6.7 RJ-45 Network Connection ............................................... 46
6.7.1 Basic Process Instrument RJ-45 Connection ............................ 46
6.7.2 Purged Unit Instrument RJ-45 Connection .............................. 47
6.8 Temperature Controller Set-up .......................................... 48
7 Vision Software Operation 49
7.1 Installation .......................................................................... 49
7.2 Configuring ........................................................................ 51
7.2.1 Setting up the network properties in Windows ...................... 51
7.2.2 Establishing the communication between Vision and your
XDS Process Analyzer ............................................................. 54
7.2.3 Parameters in Configure, Options ........................................... 61

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NIRS XDS Process Analyzer ￭￭￭￭￭￭￭￭ V
7.3 Interactance Reflectance Probe Tests ............................... 62
7.3.1 Wavelength Linearization, Interactance Reflectance ............... 62
7.3.2 Reference Standardization, Interactance Reflectance .............. 65
7.3.3 Instrument Calibration, Interactance Reflectance .................... 70
7.3.4 Performance Test, Interactance Reflectance ........................... 73
7.4 Interactance Immersion Probe Tests ................................. 75
7.4.1 Wavelength Linearization, Interactance Immersion ................. 75
7.4.2 Reference Standardization, Interactance Immersion ............... 77
7.4.3 Instrument Calibration, Interactance Immersion ..................... 83
7.4.4 Window Correction, Interactance Immersion ......................... 86
7.4.5 Performance Test, Interactance Immersion ............................. 90
7.5 Transmission Probe Tests ................................................... 92
7.5.1 Wavelength Linearization, Transmission Probes ...................... 92
7.5.2 Reference Standardization, Transmission Probes ..................... 94
7.5.3 Instrument Calibration, Transmission Probes ........................... 98
7.5.4 Window Correction, Transmission Probes ............................. 100
7.5.5 Performance Test, Transmission Probes ................................. 104
8 Maintenance of the Instrument 106
8.1 Lamp Replacement ........................................................... 106
8.2 Fuse Replacement ............................................................ 113
9 Troubleshooting 117

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 General
NIRS XDS Process Analyzer ￭￭￭￭￭￭￭￭ 1
1 General
1.1 Warranty
1.1.1 Warranty (guarantee)
Metrohm Applikon guarantees that the deliveries and services it provides
are free from material, design or manufacturing errors. The warranty
period is 12 months from the day of commissioning or 18 months from
delivery, whichever comes first. The warranty remains valid on condition
that the service is provided by an authorized Metrohm Applikon service
organization. The warranty for the accuracy corresponds to the technical
specifications given in this manual. For components from third parties that
make up a considerable part of our instrument, the manufacturer's war-
ranty provisions apply. Warranty claims cannot be pursued if the Customer
has not complied with the obligations to make payment on time.
During the warranty period Metrohm Applikon undertakes, at its own
choice, to either repair at its own premises, free of charge, any instru-
ments that can be shown to be faulty or to replace them. Transport costs
are to the Customer's account.
Faults arising from circumstances that are not the responsibility of Met-
rohm Applikon, such as improper storage or improper use, etc. are
expressly excluded from the warranty.
1.2 About the documentation
The following symbols and styles are used in this documentation:
Instruction step
Carry out these steps in the sequence shown.
Warning
This symbol indicates a hazard with a medium level
of risk which, if not avoided, could result in death or
serious injury.
Warning
This symbol indicates hazards arising from dangerous
voltages.

1.3 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
2￭￭￭￭￭￭￭￭ NIRS XDS Process Analyzer
Warning
This symbol draws attention to a possible hazard due
to heat or hot instrument parts.
Caution
This symbol indicates a hazard with a low level of risk
which, if not avoided, could result in minor or mod-
erate injury.
Note
This symbol marks additional information and tips.
1.3 Safety instructions
1.3.1 General notes on safety
WARNING
This instrument may only be operated in accordance with the specifica-
tions in this documentation.
This instrument has left the factory in a flawless state in terms of technical
safety. To maintain this state and ensure non-hazardous operation of the
instrument, the following instructions must be observed carefully.
1.3.2 Electrical safety
All relevant safety measures are to be observed when working with equip-
ment.
WARNING
Only personnel qualified by Metrohm Applikon are authorized to carry
out service work on the analyzer.
WARNING
Only connect the analyzer to other equipment that is in compliance
with the appropriate directives (i.e.: LVD, EMC etc.).

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 General
NIRS XDS Process Analyzer ￭￭￭￭￭￭￭￭ 3
WARNING
If the analyzer is connected to ICT equipment, this equipment should be
in compliance with the EN 60950-1 incl. all (recent) amendments.
Mains voltage
WARNING
Only operate the analyzer with a mains voltage specified for it (see the
analyzer identification plate).
Protection against electrostatic discharge
CAUTION
Always take ESD precautions.
The electronic components are sensitive to electrostatic charges and
can be destroyed by discharges.
1.3.3 Potentially hazardous solvents and chemicals
WARNING
Depending on the analysis procedure and/or local regulations, it can be
possibe that the analyzer should be placed in a ventilated environment
(e.g. (walk in) fume hood).
1.3.4 Recycling and disposal
This product is covered by European Directive 2002/96/EC, WEEE – Waste
from Electrical and Electronic Equipment.
The correct disposal of your old equipment will help to prevent negative
effects on the environment and public health.
More details about the disposal of your old equipment can be obtained
from your local authorities, from waste disposal companies or from your
local dealer.

1.4 List of abbreviations ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
4￭￭￭￭￭￭￭￭ NIRS XDS Process Analyzer
1.4 List of abbreviations
Table 1 List of abbreviations
°C Degrees celsius
°F Degrees fahrenheit
ATEX Atmosphères Explosibles
DCM Data Collection Method
EMC Electromagnetic compatibility
ESD Electrostatic discharge
ID Inner diameter
IP Ingress Protection
Kg Kilogram
L/min Liter per minute
LBS Pounds
LED Light Emitting Diodes
LVD Low Voltage Directive
mm millimeter
NIR Near InfraRed
NPT National Pipe Thread Tapered Thread
OD Outer diameter
PSI Pounds per square inch
SMA SubMiniature version A
USB Universal Serial Bus
VAC Voltage in Alternating Current

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NIRS XDS Process Analyzer ￭￭￭￭￭￭￭￭ 5
2 Introduction
Congratulations on your purchase of an NIRS XDS Process Analyzer from
Metrohm Process Analytics! We welcome you to our family of satisfied
customers who enjoy the benefits of the highest quality NIR.
The NIRS XDS Process Analyzer provides the next generation of process
analyzers for real-time analysis in the pharmaceutical, chemical and petro-
chemical industries. Non-destructive, accurate measurements are per-
formed directly in- or at- the process line, granulator, dryer or reactor.
The XDS Process Analyzer uses Near Infrared (NIR) energy to determine
chemical and physical characteristics of a sample. The sample is illumina-
ted with white light, and the returning signal is broken down into visible
and NIR wavelengths for spectroscopic analysis. The spectroscopic data is
then processed using a PC, and results are output in real time. This allows
on-the-fly adjustments of the process to maintain optimum characteristics.
Vision Software® is used for the analysis. Vision® has a complete suite of
analysis methods for both quantitative measurements, and for qualitative
analysis. The quantitative tools permit the measurements of specific con-
stituents (analytes) within a given product. The qualitative tools permit the
identification (ID) of products, as well as their “qualification” to determine

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6￭￭￭￭￭￭￭￭ NIRS XDS Process Analyzer
the suitability of that particular product, as compared to previously scan-
ned samples. The pharmaceutical version is fully validatable and is a 21
CFR Part 11 compliant software.
The XDS Process Analyzer is able to distinguish between very small absorb-
ance differences at each data interval (0.5 nm). By scanning samples of
known constituent values, or known qualitative characteristics, the user
may develop a very precise calibration set, as well as a library of known
products, to produce a model specific to his process.
The instrument has been designed to be adaptable for a wide variety of
processes and withstand the harshest environments.
The analyzer is available in several versions according to your needs:
￭XDS Microbundle Fiber– Single Point
￭XDS Microbundle Fiber – Multiplexer 4 Ch
￭XDS Microbundle Fiber – Multiplexer 9 Ch
￭XDS Single Fiber – Single Point
￭XDS Single Fiber – Multiplexer 4 Ch
￭XDS Single Fiber – Multiplexer 9Ch
All versions can optionally be equipped with the following options:
￭Probes.
￭AC or vertex cooling.
￭Purge and vent.
￭Fiber optic communication module.
While the user should never perform service on the process instrument, it
is helpful to understand the component functions and be familiar with the
terminology.
A schematic representation as well as a picture of the instrument are pre-
sented. On the scheme, two types of probes (transmission and reflec-
tance) are connected to the instrument allowing sequencial analysis.
Two optical fibres (single fiber or microbundle fiber) are necessary for the
transmission probe whereas only one is necessary (microbundle) for the
reflectance probe.
Note the main components of the instrument from the light source to the
detector: the lamp box, the optical fibers, the probes, the Multiplexer, the
monobox and the detector.

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NIRS XDS Process Analyzer ￭￭￭￭￭￭￭￭ 7
Figure 1 System overview
Figure 2 System corresponding to the schematic system overview

3.1 Exterior view of the Analyzer ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
8￭￭￭￭￭￭￭￭ NIRS XDS Process Analyzer
3 Overview of the instrument
3.1 Exterior view of the Analyzer
3.1.1 Front view of the analyzer
1Insulated door
This door protects and gives access to the
core components of the analyzer.
2Locks
Two locks allow the door to be closed
thanks to a key provided in the accessory kit.
3Led Panel
The LED panel indicates, from left to right,
the lamp status (ON/OFF), the communica-
tion status (operating or not) and whether
the instrument is scanning or not.
4Temperature Controller Panel
The analyzer contains a temperature control-
ler to maintain internal temperature of the
enclosure. This is normally set to 38.0 °C
5Mounting brackets
The mounting brackets are used to install
and suspend the analyzer.

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NIRS XDS Process Analyzer ￭￭￭￭￭￭￭￭ 9
3.1.2 Left side view of the analyzer
3.1.2.1 Left side view basic configuration
CAUTION
Do not remove the optional purge unit plugs.
1AC cable entrance
The XDS Process Analyzer is shipped with an
AC cable for testing and lab use only, since
many instruments are operated in a labora-
tory setting prior to their implementation on
the process line.
This AC cable may be removed when the
XDS Process Analyzer is installed into the
process location. Wiring must follow all local
codes and requirements.
2RJ-45 connection
The RJ-45 Cable Connection applies to the
non-purged instrument. For the purged
units, fiber optic modems are provided, to
meet hazardous location requirements.
3Plugs
The four plugs shown are for the optional
purge unit. On the Basic XDS Process Ana-
lyzer, these plugs remain in place as shown.

3.1 Exterior view of the Analyzer ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
10 ￭￭￭￭￭￭￭￭ NIRS XDS Process Analyzer
3.1.2.2 Left side view with purge system
1Purge unit
The purge unit is used to operate the system
in an ex proof environment.
2Vent
The vent is used to prevent overpressure
inside the instrument.
3Stainless Steel Tube
Connection from the purge to the enclosure
of the process Analyzer. Note that Type 4X
(IP66) fittings for enclosure flow are used.
4Vent Cable
Cable to the vent is I.S. wiring and must be
properly isolated from other wiring.
5Protective gas supply inlet
The protective gas supply to the enclosure
system must be a clean, instrument quality
compressed air or inert gas filtered to a mini-
mum of 40 microns.

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NIRS XDS Process Analyzer ￭￭￭￭￭￭￭￭ 11
3.1.3 Right side view of the analyzer
3.1.3.1 Right side view with heat sink and fans
1Heat Sink
Heat sinks are used as a mean to air-cool the
process analyzer (Operating temperature
range: 0 - 30 °C)
2Fan housing
Two fans allow air circulation through the
heat sink for controlling the temperature of
the process analyzer enclosure.

3.1 Exterior view of the Analyzer ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
12 ￭￭￭￭￭￭￭￭ NIRS XDS Process Analyzer
3.1.3.2 Right side view with vortex cooling
1Vortex cooler
A Vortex Cooler is designed to use filtered
compressed air to cool industrial enclosures
without the use of any refrigerants (Operat-
ing temperature range: 0 - 40 °C). An inter-
nal Vortex tube lowers the temperature and
pressure of the compressed air supplied to
the enclosure.
2Solenoid valve
A solenoid valve is an electromechanically
operated valve. The valve used is rated
NEMA 4x.
3Filter
The compressed air supply must be filtered
to remove water and dirt using a 5 micron
or smaller filter. Failure to use a filter may
cause clogging (and freezing) of the com-
pressed air paths inside the system.