Metrohm NIRS User manual

NIRS
XDS RapidLiquid Analyzer
Manual
8.921.8005EN

Metrohm AG
CH-9100 Herisau
Switzerland
Phone [phone]
Fax [phone]
[e-mail]
www.metrohm.com
NIRS
XDS RapidLiquid Analyzer
Manual
8.921.8005EN 03.2013 fpe

Teachware
Metrohm AG
CH-9100 Herisau
[email protected]
This documentation is protected by copyright. All rights reserved.
Although all the information given in this documentation has been checked with great care, errors
cannot be entirely excluded. Should you notice any mistakes please send us your comments using the
address given above.

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Change Control
Change Control (initiated with version 1.04):
Version Date Summary of Changes
1.04 September 28,
2004
Address changes to reflect move to 7703 Montpelier Road, Laurel,
MD 20723.
1.05 November 16,
2006
Added note about serialized XC-1300 Wavelength Calibration
Standard on pages 27, 32 and 34. WST3WCAL is now serialized, and
is labeled WST3W105, for example. This change permits better
wavelength accuracy with the instrument, which aids in transferability
between XDS Rapid Liquid Analyzers.
Added last page note about closing/opening sample drawer using
Vision software.
1.06 June 25,
2009
Reformatted Table of Contents.
Replaced web address for FOSS NIRSystems.
Inserted new information about network connection to instrument.
Inserted current Configure, Options screens to manual.
Moved section on opening/closing drawer to main body of manual.
Removed flow-through cuvettes from manual.
Added information of flow-through bulkhead fittings.
Moved Wavelength Linearization ahead of Instrument Calibration.
Made similar note in Lamp Replacement, that Wavelength
Linearization must be run before Instrument Calibration.
Clarified correct use of wavelength standards in Instrument
Calibration and Wavelength Certification. These changes are fairly
extensive, and are not detailed in Change Control. Please refer to the
manual for a full explanation. Changes were required due to software
updates over time that were designed to provide additional
information to the user.
Added note that Instrument Calibration is performed at room
temperature.
Added clarification that Blank Correction is loaded only for a given
session, and does not carry over to subsequent connection sessions.
Removed XC-1330 Standard Set. It is not offered at this time.
Replaced photo in Lamp Replacement to show arrow on lamp
reflector.

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Table of contents
1Introduction................................................................................................................... 6
2Site Readiness................................................................................................................ 8
2.1 Temperature and Humidity .......................................................................... 8
2.2 General Environment.................................................................................... 8
2.3 Electrical Power ........................................................................................... 8
2.4 Vibration ...................................................................................................... 8
2.5 Instrument Communication.......................................................................... 8
2.6 Instrument Dimensions and Weight ............................................................. 9
3XDS Instrument Connection......................................................................................... 10
3.1 Network Connection, connected to an active network port as shown ....... 10
3.2 Direct Connection, in a free-standing manner with no network connection
11
3.3 Overview of XDS Instrument Communication ............................................ 11
3.4 Flowchart Diagram of XDS Communication Protocol ................................. 12
3.4.1 Network Evolution Issues...................................................................................... 13
3.4.2 Quick Glossary of Terms: ...................................................................................... 13
3.5 Connection in Vision .................................................................................. 14
3.6 Troubleshooting Connection Problems....................................................... 15
3.6.1 Network Troubleshooting Overview...................................................................... 16
3.6.2 Direct Connection Troubleshooting Overview ....................................................... 20
4Assembly of the Instrument......................................................................................... 21
5Rapid Liquid Module.................................................................................................... 26
5.1 Wavelength Calibration of the Rapid Liquid Analyzer ................................ 26
5.2 Blank Correction ........................................................................................ 26
5.3 Cuvette Types............................................................................................. 27
5.4 Flow-Through Fittings................................................................................ 27
5.5 Cuvette Lifting Handle................................................................................ 28
5.6Cuvette Spacers.......................................................................................... 28
5.7 Temperature Control Information .............................................................. 28
5.8 Instructions for closing the sample drawer using Vision ............................ 29
5.9 Liquid Sampling Considerations ................................................................. 29
6Vision Software: Connection to the Instrument ........................................................... 31
7Instrument Diagnostics................................................................................................ 36
7.1 Setup Diagnostics....................................................................................... 36
7.1.1 Instrument Identification ...................................................................................... 37
7.1.2 Wavelength Linearization ..................................................................................... 37
7.1.3 Blank Correction................................................................................................... 39
7.1.4 Instrument Calibration .......................................................................................... 40
7.1.5 IPV Setup (Instrument Performance Verification) ................................................... 45
7.2 Evaluation Diagnostics ............................................................................... 47
7.2.1 Wavelength Certification ...................................................................................... 47

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7.2.2 Performance Test..................................................................................................50
7.2.3 Photometric Test ..................................................................................................52
7.2.4 Gain Test ..............................................................................................................56
7.2.5 Low Flux Test........................................................................................................57
7.3 Temperature Control Setup ........................................................................59
8Instrument Maintenance ..............................................................................................61
8.1 Overview ....................................................................................................61
8.2 Fan Filter Replacement ...............................................................................61
8.3 Lamp Replacement .....................................................................................63
8.4 Fuse Replacement.......................................................................................68
8.5 Maintenance Log ........................................................................................70
9Validation Tools ...........................................................................................................72
9.1 Hardware Validation Tools .........................................................................72
9.1.1 Factory Instrument Test Guide and Results ............................................................72
9.1.2 Installation and Operating Qualification Documents..............................................73
9.1.3 NIRStandards® for Instrument Performance Verification .......................................73
9.1.4 Instrument Performance Certification....................................................................73
9.1.5 Metrohm Master Instrument Program...................................................................74
9.2 Software Validation Tools ..........................................................................74
9.2.1 Installation and Operating Qualification Documents..............................................74
9.2.2 Vision Certificate of Validation ..............................................................................74
9.2.3 21 CFR Part 11 Compliance...................................................................................75
10 Safety and Electrical Certification ...............................................................77
11 Troubleshooting .........................................................................................78
12 Lifting and transporting the Metrohm instrument......................................82
13 Index ..........................................................................................................83

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1Introduction
Thank you for selecting the XDS™ Rapid Liquid
Analyzer, manufactured by FOSS. This instrument is
the third generation in a series of instruments
designed for precision NIR measurement,
characterization of organic materials, and
qualification of known materials to quality
parameters.
The XDS™ is designed for stable operation in harsh
environments, while still providing the precision and
accuracy users have come to expect of FOSS
instruments.
The Rapid Liquid Analyzer uses a proven monochromator design, employing a digitally-controlled
dispersive grating, along with sensitive detection devices and state-of-the-art circuitry to enhance
signal output and minimize any extraneous noise that might influence performance. The XDS™ uses
various patented algorithms to provide superior accuracy and transferability between like
instruments.
This instrument uses near-infrared (NIR) spectral energy to illuminate the sample. By measuring the
energy passing through the sample, chemical information and composition may be determined. This
information may be used for quantification of constituents, or for comparison to a library of known
materials, providing identification and qualification of materials.
The Metrohm NIRSystems 6500-Series Liquid Analyzer was a versatile, proven design for NIR
sampling for many years. The XDS™ Rapid Liquid Analyzer benefits from the improvements in
wavelength accuracy, precision, low noise, speed, and overall performance.
A panel of 6 LED indicators provides user feedback on these functions:
Icon
Status
Green when power is ON
Amber when connected to network or direct
connection
Green when instrument lamp is ON
Red when scanning reference or sample

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Green when stable operating temperature is reached
Green when module is properly attached
Vision Software™ offers an easy user interface, using the familiar interface provided with previous
generations of NIR instrumentation. All functions required to perform identification, qualification, and
quantitation are provided, with easy tools for interpretation of results. Vision offers full instrument
diagnostics, with built-in acceptance specification tables for all tests. Vision stores all results in a
diagnostic database for later lookup, with control chart views of results tracked over time.
The menu-driven, validated Vision Software package meets all requirements of CFR 21 Part 11,
covering Electronic Records and Signatures. Vision comes with a full manual for operation and theory
of operation, with complete instructions for analytical development.
The XDS Analyzer provides 0.5nm data points, and uses several innovative methods to assure
wavelength accuracy and repeatability. Wavelength positions are traceable to NIST SRM-2035. The
XDS Liquid Analyzer uses a three-layer calibration standard, measured against SRM-2035, to provide
stable, repeatable wavelength settings. Use of this standard for Instrument Calibration enhances
calibration transfer between instruments.
Instrument communication is through RJ-45 network connections, which eliminates issues involved
with long runs of RS-232 cable. An Internet Protocol (IP) address is dynamically requested upon
connection. This address may be permanently installed, if required for network purposes. The RJ-45
connection also permits remote interrogation and diagnostics checks of the instrument, if necessary
and authorized.
The instrument enclosure is completely sealed to prevent contamination by dust or other substances.
The cooling fans operate outside the main enclosure, and are thermally linked to internal fans that
maintain a constant temperature inside the instrument enclosure. There is no airflow drawn into the
optics chamber of the instrument. This avoids contamination of the instrument in dusty
environments. An air filter is built into the door of this chamber. For cool environments, heaters are
embedded in the thermal transfer block to raise temperature when required.
Lamp changes are performed through a single panel on the rear surface of the instrument. The lamp
is easy to remove and replace, and requires no special tools or expertise.
The Metrohm Rapid Liquid Analyzer is available with a
variety of quartz cuvettes to make analysis
straightforward and easy. A sealable cuvette, suitable
for volatile liquids is shown.
Capped cuvettes and other styles are available, in
various path lengths. Select path length based upon
absorbance of the analytes of interest.
See section 5.0 for full information.

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2Site Readiness
Like most precision instruments, the Rapid Liquid Analyzer is sensitive to environmental conditions
that can affect its performance and useful life. Observe the following guidelines when selecting a site
and installing the instrument:
2.1 Temperature and Humidity
The XDS Analyzer is designed to work in ambient air temperatures from 40-95°F (4.5-35°C).
Use the XDS Analyzer only in 10-90% relative humidity levels, non-condensing. Rapid changes in
humidity can cause interferences by adding trace moisture absorptions to the spectra. In general,
lower humidity levels are preferred.
The Performance Test (a comprehensive instrument diagnostic test in Vision software) is somewhat
sensitive to changes in ambient humidity, and the Performance Test may fail under conditions of
extreme humidity, or rapidly varying humidity.
2.2 General Environment
Minimize exposure of the monochromator to dust.
Inspect the fan filter at least monthly. If an accumulation of lint, dust, or other matter has
accumulated, pull open the right-hand panel from the instrument. Replace the filter. If dust has
accumulated on the fans, carefully wipe them clean with a moist soft cloth. Do not distort or damage
the fan blades or fins, as this will impede cooling.
Do not place the instrument directly near any HVAC duct. The direct flow of heating or cooling air
will cause the instrument to exhibit high noise during the Performance Test.
2.3 Electrical Power
Power should be a single, separate, stable, transient-free filtered AC circuit. The circuit should have
surge protection.
Operating voltage for the instrument is 100-240VAC, 50/60Hz. The power supply is self-switching
and will provide the correct operating voltage to the instrument.
Typical power consumption is 100W, 750W maximum.
2.4 Vibration
Install the XDS Analyzer where it will not be affected by bench vibration from grinders, blenders,
stirrers, or mixers.
Never permit hammering or other physical impact on the bench top supporting the XDS Analyzer or
its computer.
2.5 Instrument Communication
The XDS instrument may be accessed directly through a network connection. This uses a standard RJ-
45 type “patch” cable, such as CDW #074092, available from CDW Computer Centers, Inc. The
instrument detects network capability and optimizes communication speed.

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Alternatively, the XDS Rapid Liquid Analyzer can communicate directly with the computer by use of a
UTP Crossover Cable, such as CDW #243786, supplied with unit. (gray cable)
The computer that operates the instrument must have clear access through the network, and be
configured to communicate properly. This communication is the responsibility of your on-site
network personnel.
Full instructions are given in section 3.0.
2.6 Instrument Dimensions and Weight
XDS™ Rapid Liquid Analyzer dimensions are:
•Width: 18.0” (457 mm)
(Leave about 6” (152mm) on the right side for ease of sample loading)
•Height: 15.0” (381 mm)
•Depth: 22.5” (572 mm) front to back
Leave a minimum of 3” (76mm) around the back and left side for airflow and access space. Leave at
least 6” (152mm) on the right side and in front for sample handling space.
•Monochromator Weight: 46.2 pounds (21.0 kg)
•Module Weight: 29.3 pounds (13.3 kg)
Follow lifting instructions (on last page) when moving the instrument. Avoid injury.

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3XDS Instrument Connection
The XDS instrument may be connected to the host computer in one of two ways: If the XDS
Instrument will be used as part of a network, use the Network Connection method shown
immediately below. If there are not enough active network ports near the XDS instrument, a hub or
router may be used.
This section assumes use of Windows® 2000, XP, or later versions of Windows Operating Systems.
For computers using Windows 95, 98, or NT 4.0, we recommend upgrade of the computer and
operating system to current specifications.
CAUTION: Metrohm NIRSystems does not recommend the use of two network cards under any
circumstances. Do not use Direct Connection to the instrument along with a network connection to
the company network. The use of two network cards -- on one data bus in the computer – may
result in lost commands, lost data, and unsatisfactory software operation. Metrohm cannot be
responsible for software and instrument problems resulting from the use of two network cards in the
host computer.
This information is correct as of the time of original publication. Changes to computers, operating
systems, and network protocols may require revision of this information without notice.
3.1 Network Connection, connected to an active network port as
shown
This is the preferred method of instrument communication when a connection to the company Local
Area Network (LAN) is necessary. Specific information about this method follows:
•The XDS instrument should be connected -- with a “patch” cable – to the network port.
•Upon power-up, the XDS instrument will request a dynamic IP address from the network
server. This is normally assigned in 5 to 10 seconds.
•The XDS instrument uses a proprietary, encrypted command language. It cannot be activated
by any program except Vision, or FOSS programs designed to operate the instrument.
Therefore, the instrument maintains “Closed System” status under 21 CFR Part 11 rules. No
hacking or support of viruses is possible with XDS instruments.

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•The XDS instrument appears just like a network printer (or other peripheral device) on the
LAN system. It generates no signals, and only responds when commanded by an authorized
user, logged into Vision software.
•This is the easiest connection method for XDS instruments.
3.2 Direct Connection, in a free-standing manner with no
network connection
This method allows users to connect to the instrument when there is no network present. In such
cases, a “crossover cable” (provided) is used. The XDS instrument, upon power-up, requests a
dynamic IP address. When none is supplied within 45 seconds, the XDS instrument concludes that no
DHCP server is available. It then defaults to an internal IP address which the computer may use for
“direct communication”.
This method of hookup should not be used when the computer is also connected to a network. Such
connection may result in lost commands, lost data, and unsatisfactory software operation. Metrohm
cannot be responsible for software and instrument problems resulting from the use of two network
cards in the host computer.
For IT personnel, it may be helpful to understand the sequence of events used by the XDS instrument
and Vision software when establishing an electronic connection. These are explained.
3.3 Overview of XDS Instrument Communication
The XDS instrument may be connected to LAN systems in the same manner as any printer or other
peripheral Ethernet-enabled device. These key items will help understand the communication
methods. See the flowchart diagram on next page.
1. The XDS instrument maintains “Closed System Status” under 21 CFR Part 11 guidelines. It
uses a proprietary, encrypted command language. It is not susceptible to hacking or virus
attacks.
2. The XDS system may only be addressed using proprietary software (usually “Vision”) which
can only be entered by an authorized user, using the “two-token” method of entry. (Unique
User ID and password)

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3. Upon being powered up on a LAN, the XDS instrument requests a “dynamic” IP address from
the DHCP server which controls the LAN. This IP address is normally granted promptly
(typically in 5-10 seconds) so the instrument can function on the LAN. Most DHCP servers
track the XDS instrument by the “MAC” (Machine Access Code) to later re-assign that same IP
address whenever the XDS instrument is on the LAN.
4. If there is no DHCP server available to assign an IP address (a free-standing router may serve
the same DHCP function), the XDS instrument will “time out” in 45 seconds --and it will know
that it is not attached to an active LAN. It will then default to an internally-stored default IP
address. This address, 169.254.0.2, is used for local, free-standing communication only. In
such cases, a crossover cable, or a hub with two patch cables, should be used to connect the
computer and the XDS instrument.
5. Upon the next power-down and subsequent power-up of the XDS instrument, it will again
request an IP address of the DHCP server. It will go through the same cycle, eventually
reverting to the stored default IP address. This is intentional.
6. A dynamic IP address is the preferred method of XDS instrument connection. The default IP
address is only used when no DHCP server is available to assign a dynamic IP address.
A short glossary of terms follows. See the flowchart diagram for XDS instrument communication
which visually outlines the items explained above.
3.4 Flowchart Diagram of XDS Communication Protocol

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3.4.1 Network Evolution Issues
This document is as correct as possible at the time or writing. However, network management is an
evolving discipline, and conditions will change. Some of the drivers for change include network
security, authentication, and data integrity. Technology changes factor into all of these issues.
Because the network communication environment is complex and ever-changing, we have tried to
provide the basic information needed for connection of the XDS instrument. 95% of users will have
no connection problems, if these instructions are followed.
In the rest of the cases, there may be network issues, corporate restrictions, or other issues which
inhibit easy connection. The troubleshooting section covers some of the most common problems.
In all cases, we recommend minimal tampering with computer settings. This can cause instability, and
may be prohibited by company policies.
At this time, we recommend Microsoft Windows® XP as the easiest operating system by which to
establish network communication. We strongly recommend that Windows 95, 98, and NT 4.0 be
avoided, as they require considerable expertise in network configuration.
3.4.2 Quick Glossary of Terms:
DHCP:
The Dynamic Host Configuration Protocol (DHCP) is an Internet protocol for automating the
configuration of computers that use TCP/IP.
DNS Server:
A Domain Name Server. DNS Servers run special-purpose software, as part of the Domain Name
System, for managing enterprise networks.
IP:
An Internet Protocol (IP) address is a numerical identification and logical address that is assigned to
devices participating in a computer network utilizing the Internet Protocol for communication
between its nodes.
IPv4:
IPv4 refers to “Internet Protocol version 4” which is the fourth revision in the development of the
Internet Protocol (IP) and it is the first version of the protocol to be widely deployed. Together with
IPv6, it is at the core of standards-based internetworking methods of the Internet and is still by far
the most widely deployed Internet Layer protocol. XDS Instruments use IPv4.
LAN:
A local area network (LAN) is a computer network covering a small physical area, like a home, office,
or small group of buildings, such as a corporate site, a university, or an airport. These are often called
“enterprises”.
Subnet Mask:
“Subnetting” is used to break a large network into smaller sections. This can enhance efficiency, raise
speeds, and reduce “packet collisions” within the network. To accomplish subnetting, “Subnet
Masks” may be applied to separate one section of the network from another. A subnet mask typically

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takes the form “255.255.255.0” or something similar. This scheme is becoming obsolete, as new
network management methods are being implemented.
TCP/IP:
(Transmission Control Protocol/Internet Protocol) is the basic communication language or protocol of
the Internet.
3.5 Connection in Vision
1. Log into Vision with your User ID and Password.
Click on Configure, Input as shown.
2. Highlight “NIRSystems XDS-series
Instrument Driver” as shown, then
click on “Configure”.
Information:
At this point, Vision requests any
XDS instrument on the local area
network (LAN) to report
connection status. This may take a
few moments.
If the instrument is not on a LAN,
and instead is connected with a
crossover cable, this will take a
minute or more. Vision first
requests a dynamic IP address, If
no server or router is available to
assign an IP address, Vision waits
45 seconds, then searches for the
default instrument IP address, in
the event of Direct Connection
using a crossover cable.

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3. When Vision “finds” the
instrument on the LAN, it
will be shown. The dynamic
IP address (assigned by the
server) is shown, along with
the XDS Serial number. The
instrument is shown as
“Available” on port 2083.
Highlight the instrument
and click “OK”.
4. If the IP Address field is empty, the user should consult “Troubleshooting Connection
Problems”.
3.6 Troubleshooting Connection Problems
Many connection problems are easily solved, especially with Windows® XP operating systems.
Windows XP is currently the preferred operating system, and has enhanced connectivity over other
operating systems. Vista is good also, but may impose user security restrictions. Windows 2000 is
almost as simple, but may require an extra step or two, as discussed.
If your computer uses Windows 95, 98, or NT 4.0 for the operating system, we strongly recommend
upgrade to Windows XP for easiest connectivity. This may require a full computer upgrade, as older
computers may not have the processor speed, memory, or connectivity required to run Windows XP
with full Ethernet compatibility.
1. Vision cannot see any
instrument on the
connection path.
Click on the “down
arrow” at the right side
of the empty field to
see if instrument(s) are
shown.
Solution:
By expanding the field,
Vision can display the
instruments shown.
Note that only the top
instrument, Serial
#3010-0878, is
“Available”. Highlight it
and click “OK”.

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2. Vision still sees no
instrument(s) after
expanding the field.
This indicates
connection or network
issues.
Verify Cable Type:
Verify correct cable type for hookup. Most networks use “patch” cables. Free-standing systems use a
“crossover cable”. Power down the XDS instrument, then power it back up. Wait 120 seconds for the
XDS instrument to fully reset its communication. If an instrument is shown, proceed to “Acquire”,
“Connect” in Vision.
If this does not resolve the problem, continue to the next section.
3.6.1 Network Troubleshooting Overview
If no XDS instrument shows as “available”, there may be a setting which should be changed. It may
be necessary to contact your IT department for assistance with these issues.
First, verify that the network has a DHCP Server. If no DHCP server is available, the instrument must
be connected by Direct connection, using a crossover cable. If this is the case, proceed to the section
entitled “Direct Connection Troubleshooting Overview”.
Network Solution 1:
Check Internet Protocol (TCP/IP) Properties. (You may need to contact your IT department to follow
these steps.)
•Click on Start, then Control Panel
•Double-click on Network Connections
•Double-click on Local Area Connection
•Click on Local Area Connection Properties
•Click on Internet Protocol (TCP/IP)
•Click on Properties
The full path, from Network Properties forward to Internet Protocol (TCP/IP) Properties, is shown:

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Verify these settings:
•Obtain an IP address automatically
•Obtain DNS server address
automatically
When finished, click “OK”. Close all other
boxes opened for this verification.
If the settings were not set properly, it may
be necessary to exit Windows XP, then re-
enter XP, to have the correct settings take
effect. If in doubt, do this and try XDS
instrument communications again after this
takes effect.

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Network Solution 2:
Returning to the Local Area
Connection Status dialog box, note
these items for the computer:
•Address Type:
(should be “assigned by
DHCP”)
•IP Address:
Write this address down for
the next step
•Subnet Mask:
Write this down for the next
step
If connection cannot be achieved, it
may be necessary to verify that the
XDS instrument is installed “within
the IP address range” of the
computer.
Network Solution 3:
Verify network has full IPv4
compatibility.
Some networks have moved to Ipv6
(Internet Protocol version 6) which
uses different address formats.
The IT department at your company can verify if the
network offers full Ipv4 compatibility. If the network has
migrated to Ipv6 operation, a “compatibility pack” may
need to be loaded to support Ipv4-enabled devices.