Agilent Technologies Cary 630 FTIR User manual

Agilent Cary 630 FTIR
Spectrometer
User’s Guide

2 Agilent Cary 630 FTIR Spectrometer User’s Guide
Notices
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Manual Part Number
G8043-90001
Edition
Fifth edition, January 2018
Agilent Technologies Australia [M] Pty
Ltd
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Mulgrave, Victoria 3170, Australia
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Contents
Agilent Cary 630 FTIR Spectrometer User’s Guide 3
Contents
1. Introduction 7
Information Symbols 9
2. Getting Started 11
Unpacking 11
Packing list 12
Options 12
Installation 13
Components 13
Connecting Power 14
Environment 16
MicroLab PC software 16
Turning On the Instrument 16
Power switch LED status 16
Turning Off 17
Performance Verification 17
Diagnostic values 18
Validation 20
3. Analyzing Samples 23
Interchanging Sampling Accessories 24
Diamond ATR Sampling Accessory 26
Cleaning 27
Collecting a background spectrum 28
Collecting a sample spectrum 28

Contents
4 Agilent Cary 630 FTIR Spectrometer User’s Guide
ZnSe ATR Sampling Accessory 30
Cleaning 31
Collecting a background spectrum 32
Collecting a sample spectrum 32
Germanium ATR Sampling Accessory 34
Cleaning 36
Collecting a background spectrum 36
Collecting a sample spectrum 36
5 Bounce Zinc Selenide ATR Sampling Accessory 38
Cleaning 38
Collecting a background spectrum 39
Collecting a sample spectrum 39
Transmission Sampling Accessory 40
Cleaning 41
Collecting a background spectrum 41
Collecting a sample spectrum 42
10 and 45 Degree Specular Reflectance Sampling Accessories 42
Cleaning 44
Collecting a background spectrum 44
Collecting a sample spectrum 45
TumblIR Sampling Accessory 45
Cleaning 46
Collecting a background spectrum 47
Collecting a sample spectrum 47
DialPath Sampling Accessory 48
Cleaning 50
Collecting a background spectrum 51
Collecting a sample spectrum 51

Contents
Agilent Cary 630 FTIR Spectrometer User’s Guide 5
Diffuse Reflectance Sampling Accessory 53
Cleaning 54
Collecting a background spectrum 55
Collecting a sample spectrum 55
4. Maintenance 57
Cleaning 57
Replacing the Desiccant 57
Replacing Windows 59
Replacing the Source 60
5. Spare Parts 65
Sampling Accessories 66
6. Specifications 67
Technical 67
Safety Information 68
ICES/NMB-001 68
Electromagnetic Compatibility 68
EN55011/CISPR11 68
Environmental Conditions 69

Introduction
6 Agilent Cary 630 FTIR Spectrometer User’s Guide
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Introduction
Agilent Cary 630 FTIR Spectrometer User’s Guide 7
1. Introduction
Information Symbols 9
The Agilent Cary 630 FTIR is a small, mid-infrared spectrometer
designed to provide the capabilities of much larger, traditional FTIR
spectrometers, but without the complexity, maintenance requirements
or cost. The main optical unit dimensions are only 16 x 22 x
13 centimeters (6.3 x 8.7 x 5.1 in) and it weighs only 2.9 kilograms
(6.3 lb). The Cary 630 FTIR provides versatility for use in a traditional
analytical chemistry laboratory. The system is intended for indoor use
and is not designed for water-resistance or other extreme outdoor
conditions
WARNING
Fire Hazard
The Cary 630 FTIR systems are NOT intrinsically safe. Use the system only in
atmospheres that have been tested for flammable materials. If the equipment
is used in a manner not specified in this guide, the protection provided by the
equipment may be impaired.

Introduction
8 Agilent Cary 630 FTIR Spectrometer User’s Guide
The Cary 630 FTIR uses technology known as Fourier transform
infrared (FTIR) spectroscopy, which is the current state-of-the-art
technique for molecular compound identification and quantification.
FTIR uses an infrared light source to pass through the sample and
onto a detector, which precisely measures the amount of light
absorbed by the sample. This absorbance creates a unique spectral
fingerprint that is used to identify the molecular structure of the
sample and determine the exact quantity of a particular compound in
a mixture. At the heart of the Cary 630 FTIR spectrometer is a unique
Michelson interferometer. This proprietary design is the key to making
FTIR technology compact, lightweight and rugged.
The Cary 630 FTIR is available in two configurations depending on the
frequency range necessary for your application. Please see the Cary
630 FTIR specifications for details.
In addition, a number of different sampling accessories are available
to suit various sample types and sensitivities. The accessories
accommodate the analysis of a range of liquids, powders, gases, pastes
and gels. They include:
Diamond ATR: For the chemical analysis of liquids, powders,
pastes and gels. The attenuated total reflectance (ATR) system is
available as a single-reflection (most common) ATR.
ZnSe ATR: For the chemical analysis of liquids, gels and soft
solids within a pH range of 5-9. The attenuated total reflectance
(ATR) system is available as a single-reflection ATR (most
common) and a multi-bounce ATR (Liquids only)
Transmission: A classic infrared sampling interface, allowing
measurement of solids, liquids and gases. A 50 mm slide-mount
gas cell is also available from Agilent.
TumblIR: Single pathlength transmission for rapid chemical
analysis of liquids under ambient conditions.
DialPath: For rapid chemical analysis of liquids under ambient
conditions, with three set pathlengths that allow you to choose the
sensitivity necessary for your analysis.
Diffuse Reflectance: For quantitative and qualitative
measurement of powdered and solid samples. Provides more
sensitive quantitative analysis than ATR, while still being easy to
use.

Introduction
Agilent Cary 630 FTIR Spectrometer User’s Guide 9
Germanium ATR: For measuring samples that are too highly
absorbing for diamond ATRs or for samples with high amounts of
carbon black.
10 degree Specular Reflectance: For measuring specular
reflectance of solid samples at near normal.
45 degree Specular Reflectance: For measuring specular
reflectance of solid samples at angle. This accessory is placed into
the transmission compartment.
The Cary 630 FTIR is computer-controlled using Agilent MicroLab PC
software. MicroLab PC is intuitive, simple to use and requires no
specialized technical training. With a click of the mouse, the system
provides valuable information about the identity and amount of
chemical substances present in a material.
Information Symbols
The following symbols appear on the instrument for your information.
I On (Power)
0 Off (Power)
Direct current

Introduction
10 Agilent Cary 630 FTIR Spectrometer User’s Guide
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Getting Started
Agilent Cary 630 FTIR Spectrometer User’s Guide 11
2. Getting Started
Unpacking 11
Installation 13
Components 13
Connecting Power 14
Environment 16
MicroLab PC software 16
Turning On the Instrument 16
Turning Off 17
Performance Verification 17
Unpacking
To unpack your spectrometer system:
1After receiving the Agilent Cary 630 FTIR delivery, do not
immediately open the shipping container. Instead, place the
shipping case in a room-temperature environment and allow
several hours for the contents of the container to reach the room
ambient temperature. This is to avoid unnecessary condensation
on the components prior to the initial setup and installation
process.
Your Cary 630 FTIR has been packed to ensure that it arrives at
your facility ready to go to work. Custom foam-in-place inserts
protect the instrument from damage during travel. Whenever your
instrument is shipped via common carrier, it needs to be re-
packed in the original shipping container. Using the original
shipping container, your Cary 630 can be removed and re-packed
in its container in a matter of seconds, while maintaining
instrument security. Shipping the Cary 630 FTIR in packaging
other than the original shipping container will void the warranty.

Getting Started
12 Agilent Cary 630 FTIR Spectrometer User’s Guide
2The shipping container should contain the standard items listed
below as well as any optional items ordered. Inspect the enclosure
closely to make sure all items have been removed from the
shipment packaging. Also ensure that all the items in the packing
list below have arrived undamaged and are in good working
condition. Contact Agilent immediately if any items are found to
be missing or damaged in shipment.
NOTE Keep all original packing material for storing, shipping and transporting the
system in the future.
NOTE Shipping the Cary 630 FTIR in packaging other than the original shipping
container will void the warranty.
3Remove the Cary 630 FTIR system from its shipping case and
place it on its side on a flat, stable surface. The instrument must
be kept away from hot surfaces and any sources of
electromagnetic interference.
Packing list
One Agilent Cary 630 FTIR spectrometer system
One Agilent Cary 630 FTIR Operation Manual
One Agilent MicroLab Software CD
One Agilent Cary 630 FTIR AC power cable
One Agilent Cary 630 FTIR external power supply
One Agilent Cary 630 FTIR USB cable
One shipping container
Options
Although the Cary 630 FTIR system comes standard as shown above,
there are a number of options available, including:
Laptop/Desktop computer
Interchangeable Accessories as ordered
Spare USB cable
Spare Power Cable/Supply

Getting Started
Agilent Cary 630 FTIR Spectrometer User’s Guide 13
Installation
The Cary 630 FTIR is designed to be completely customer-installable.
Install your Cary 630 according to the guide lines below. For a quick
reference guide refer to the installation card.
Components
Attaching the sampling accessory or interface is necessary in order to
ensure proper working order of the Cary 630 FTIR. To install any of
your accessories:
1Press the release lever outward
2The accessory is meant to slide into the recessed or dovetailed
area. This is done by matching the dovetail to the front plate and
sliding in a downward fashion. (Figure 1)
3The accessory is in place when the release lever snaps back into
place.
Figure 1. Press the release lever of the Cary 630 Engine outwards before sliding
the accessory into place.

Getting Started
14 Agilent Cary 630 FTIR Spectrometer User’s Guide
Connecting Power
To connect power to the spectrometer system:
1Insert the provided power connection from power supply into the
power connector located on the lower left side at the rear of the
Cary 630 FTIR system (see Figure 2).
Figure 2. Attaching the power cord
2Thread the blue cap onto the power connector by rotating it
clockwise until finger-tight. To avoid damage to the plastic
connector, be careful not to over-tighten.
3The appropriate power supply cabling will be provided with the
system. Connect the opposite end of the power cable to the AC
power outlet.
4Connect the Mini USB communication cable to the USB connector
on the back right of the instrument.
Thread the blue cap onto the power connector by rotating it
clockwise until finger-tight. To avoid damage to the plastic
connector, be careful not to over-tighten.
CAUTION To prevent any power startup damage or problems, connect the power cord to
the spectrometer system first and then to the power outlet.
CAUTION To avoid damage to the system due to power surges or a faulty power source,
always use a UL approved power surge protection strip between the power
outlet source and the system power cord.
Power USB

Getting Started
Agilent Cary 630 FTIR Spectrometer User’s Guide 15
CAUTION All cords must be kept away from high traffic areas. The system could sustain
damage to the apparatus or adapters if excessive strain to the power cord
connections occurs.
Position the equipment for easy access to the disconnecting switch.
Power cord selection
CAUTION If necessary, replace the power cord only with a cord equivalent to the one
specified below.
The following power cords can be used:
Figure 3. Suitable power cords

Getting Started
16 Agilent Cary 630 FTIR Spectrometer User’s Guide
Environment
CAUTION Your Cary 630 FTIR must be kept away from hot surfaces and sources of
electromagnetic interference.
MicroLab PC software
Your Cary 630 FTIR is supplied with Agilent MicroLab PC software.
For instructions on installing the software, see the Agilent MicroLab
PC Software User’s Guide. The software manual is located on the
Software installation CD. It provides more in depth information about
logging on, managing users, editing methods and reviewing data.
Turning On the Instrument
To turn on the instrument:
1Press the power button of the Cary 630 FTIR system and hold for
two (2) seconds. Initially, the light will flash between red and
green while the firmware is being loaded. This process should take
less than 15 seconds. When the LED light illuminates solid green,
the instrument is now ready to use.
2The spectrometer must have a warmup period of 5 minutes before
reliable analysis may begin.
When finished using the instrument, press the green power button
again to turn off the system. The LED light will turn red.
Power switch LED status
The power button contains a two-colored LED. The color displayed on
the LED can indicate the state of the system. The table below lists the
colors of the LED and the status of the instrument.

Getting Started
Agilent Cary 630 FTIR Spectrometer User’s Guide 17
Table 1. Power switch LED status
Status LED color Action (% duty cycle)
System OFF No LED illumination N/A
System OFF Red 100%
System startup Red / green Green 0.5 s on / red 0.5 s on
System ON Green 100%
Firmware update Red / green Green blinks rapidly twice then red blinks
rapidly twice
Turning Off
When you have finished using the spectrometer, press the green
power button to turn off the system. The LED light will turn red.
NOTE To help keep moisture out of the Cary 630 FTIR, it is recommended to leave the
spectrometer on, even when not in use.
CAUTION The power button is a momentary switch, to avoid accidental power off. In order
to turn the system on or off, hold down the button for two (2) seconds.
Performance Verification
Your Cary 630 FTIR has been thoroughly tested at the factory, so no
alignment steps are required. However, it is recommended to run the
performance test initially to ensure the spectrometer is running
properly. To run and interpret the performance test, refer to the
Agilent MicroLab PC Software User’s Guide. The performance test
measures the energy level of the spectrometer (based on the
interferogram voltage or height). A successful test will be indicated by
a green circle at the top of the software screen. You are then ready to
analyze a sample. A yellow or red circle indicates the spectrometer is
operating outside of the factory-defined parameters. These parameters
are listed in Table 1 as well as on the Advanced Features software
page.

Getting Started
18 Agilent Cary 630 FTIR Spectrometer User’s Guide
NOTE If the circle at the top of the software screen is yellow or red, contact Agilent
technical support for assistance.
Like any measurement device, it is important to verify that the Cary
630 FTIR is performing properly before using the system to make
critical measurements. The Cary 630 provides both diagnostic values
and performance validation tests to demonstrate the system’s
performance.
The diagnostic values provide an easy to understand, quick
assessment of the spectrometer’s function. If the spectrometer is not
functioning properly, one of the diagnostic values will be out of
specification.
Performance validation tests are longer, more involved tests that
measure how well the spectrometer is working. Validation tests check
the spectrometer’s sensitivity (performance), stability and frequency
precision (laser calibration).
Each industry has different requirements for instrument verification.
In general, the diagnostic values should be checked on a daily or
weekly basis. Typically, the spectrometer will not collect data if the
diagnostic values are grossly out of specification, but it is good
practice to verify that the spectrometer is working properly.
Performance validation should be run on a quarterly, bi-annual or
annual basis. Highly-regulated industries may require the
performance validation to be run monthly, depending on the use of
the instrument.
Diagnostic values
The following values can be viewed on the Diagnostics page in the
MicroLab PC software. In each case, the Optimal value indicates that
the Cary 630 FTIR system is running at its intended performance
level. The Marginal value indicates that the spectrometer is
functioning, but at a lower performance level. The Critical value
indicates that the system is not working correctly, in which case you
should contact Agilent technical support for assistance.

Getting Started
Agilent Cary 630 FTIR Spectrometer User’s Guide 19
NOTE When using the Diffuse Reflectance sampling accessory, the appropriate
reflectance disk must be in place to make these measurements. The diffuse gold
reference disk should be used with the Diffuse Reflectance sampling accessory.
This disk is permanently mounted into Position 1 of the sampling tray.
Table 2. Diagnostic values
Value Optimal (green) Marginal (yellow) Critical (red) Comment
Energy
(center-burst)
28,000-15,000 >28,000 or
<10000
> 30,000 or
< 3000
Indicates the overall
alignment and proper gain
adjustment for the system.
Source 1.9 A >2.2 A or
<1.6 A
>2.4 A or
<1.4 A
Indicates a problem with the
infrared source control
voltage, or that the source
has burnt out. Both voltage
and amperage are displayed;
however, amperage provides
a sufficient diagnostic.
Laser signal 15,000-3,000 >15,000 or
<3,000
>17,000 or
< 2,000
Can verify gross alignment
errors even if the reflectance
cap is not in place.
Detector
temperature
43–44 <43 or
>44
<42 or
>45
Indicates a problem with the
cooling circuitry or an ambient
temperature over the
specified range.
CPU
temperature
10–75 >75 >80 Indicates the ambient
temperature over the
specified range.

Getting Started
20 Agilent Cary 630 FTIR Spectrometer User’s Guide
Validation
The MicroLab PC software has three tests appropriate for
performance validation of the Cary 630 FTIR. Performance validation
verifies the key aspects of the instrument’s ability to measure good
data. If the performance validation tests are within specification, the
spectrometer should provide data that works well with methods
developed for the Cary 630. As with any instrument, however, results
can always be verified by running a known sample with the sample-
specific method.
The validation tests are accessed from the Advanced Features, System
Check page of the MicroLab PC software. The Cary 630 FTIR system
should be warmed up for at least 120 minutes before conducting any
of these tests.
Performance (signal-to-noise) test
This test measures the signal-to-noise level at two regions of the
infrared spectrum: 2,500 cm-1 and 1,000 cm-1. Both the background
and sample are measured at 4 cm-1 resolution with a one minute
collection time. This test takes two minutes per test. You can specify a
number of tests to be conducted. For diffuse reflectance
measurements, the appropriate sample position must be in place with
the diffuse gold mirror. No sample is needed when using the Diamond
ATR sampling accessory. At least 10 tests should be collected in order
to obtain an accurate picture of the performance.
Stability test
This test measures the short-term stability at two regions of the
spectrum: 3,000 cm-1 and 1,000 cm-1. Stability is a measurement of the
baseline differences observed over the selected time period. The test
measures a background at the beginning, then one sample every
minute for the duration of the test as specified in the ‘Number of
minutes’ field in the software. For diffuse reflectance measurements,
the appropriate sample position must be in place with the diffuse gold
mirror. No sample is needed when using the Diamond ATR sampling
accessory. The test results are expressed as %Transmittance
(difference versus 100%) of maximum deviation during the Stability
test.