Agilent Technologies Cary 630 FTIR User Manual
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Agilent Technologies Cary 630 FTIR User Manual

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Agilent Cary 630 FTIR
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User's Guide

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  • Page 1 Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 2 DFAR 252.227-7014 (June 1995), or as a “commercial item” as defined in FAR 2.101(a) or as “Restricted computer software” as defined in FAR 52.227-19 (June 1987) or any equivalent agency regulation or Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 3: Table Of Contents

    Turning On the Instrument Power switch LED status Turning Off Performance Verification Diagnostic values Validation 3. Analyzing Samples Interchanging Sampling Accessories Diamond ATR Sampling Accessory Cleaning Collecting a background spectrum Collecting a sample spectrum Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 4 Cleaning Collecting a background spectrum Collecting a sample spectrum TumblIR Sampling Accessory Cleaning Collecting a background spectrum Collecting a sample spectrum DialPath Sampling Accessory Cleaning Collecting a background spectrum Collecting a sample spectrum Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 5 Collecting a background spectrum Collecting a sample spectrum 4. Maintenance Cleaning Replacing the Desiccant Replacing Windows Replacing the Source 5. Spare Parts Sampling Accessories 6. Specifications Technical Safety Information ICES/NMB-001 Electromagnetic Compatibility EN55011/CISPR11 Environmental Conditions Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 6 Introduction This page is intentionally left blank. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 7: Introduction

    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.
  • Page 8 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.

  • Page 9: Information Symbols

    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.
  • Page 10 Introduction This page is intentionally left blank. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 11: Getting Started

    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.

  • Page 12: Packing List

    Keep all original packing material for storing, shipping and transporting the NOTE system in the future. Shipping the Cary 630 FTIR in packaging other than the original shipping NOTE container will void the warranty. Remove the Cary 630 FTIR system from its shipping case and place it on its side on a flat, stable surface.

  • Page 13: Installation

    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: Press the release lever outward The accessory is meant to slide into the recessed or dovetailed area.

  • Page 14: Connecting Power

    To connect power to the spectrometer system: Insert 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). Power Figure 2. Attaching the power cord Thread the blue cap onto the power connector by rotating it clockwise until finger-tight.
  • Page 15 Position the equipment for easy access to the disconnecting switch. Power cord selection If necessary, replace the power cord only with a cord equivalent to the one CAUTION specified below. The following power cords can be used: Figure 3. Suitable power cords Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 16: Environment

    Getting Started Environment Your Cary 630 FTIR must be kept away from hot surfaces and sources of CAUTION 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.

  • Page 17: 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. To help keep moisture out of the Cary 630 FTIR, it is recommended to leave the NOTE spectrometer on, even when not in use.

  • Page 18: 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.
  • Page 19 <43 or <42 or Indicates a problem with the cooling circuitry or an ambient temperature >44 >45 temperature over the specified range. 10–75 >75 >80 Indicates the ambient temperature over the temperature specified range. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 20: Validation

    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.
  • Page 21 Neither the multi-bounce ATR, nor the diffuse reflectance accessory measurements should be used for the laser frequency calibration test. Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 22 Getting Started This page is intentionally left blank. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 23: Analyzing Samples

    TumblIR Sampling Accessory DialPath Sampling Accessory Diffuse Reflectance Sampling Accessory The Agilent Cary 630 FTIR spectrometer requires a sampling accessory in order to present the sample to the infrared beam. You will have selected one or more sampling accessories when you ordered your Cary 630 FTIR.

  • Page 24: Interchanging Sampling Accessories

    To switch between different sampling accessories: Before attempting to change the sampling accessory, ensure that the Cary 630 FTIR system is on a solid surface with the accessory facing towards you. To remove an installed sampling accessory, push the retaining lever located on the right side of the instrument to the side.
  • Page 25 The lever will click back into place when the accessory is properly seated. Notice the two stainless steel dowel pins protruding out of the Cary 630 FTIR unit. This is to ensure proper placement and alignment of the accessories. Store the removed sampling accessory in a clean, protected area, such as in a plastic bag inside foam-lined shipping container.

  • Page 26: Diamond Atr Sampling Accessory

    (see Figure 5). It is in this position that the sample mounting area can be easily accessed for loading the sample into place and for cleaning the sampling surfaces before the next sample is analyzed. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 27: Cleaning

    Cleaning To clean the Diamond ATR accessory in preparation for analysis: Open the sample press by rotating the top knob counterclockwise until the top of the press travel is reached (see Figure 5). Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 28: Collecting A Background Spectrum

    In the case of a volatile sample, larger amounts of sample can be applied without concern of leakage or damage to the instrument. However, using the smallest amount of sample possible will ease in the cleaning process. Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 29 For instructions on reviewing results and handling sample data, refer to the Agilent MicroLab PC Software User’s Guide. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 30: Znse Atr Sampling Accessory

    (see Figure 5). It is in this position that the sample mounting area can be easily accessed for loading the sample into place and for cleaning the sampling surfaces before the next sample is analyzed. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 31: Cleaning

    Cleaning To clean the ZnSe ATR accessory in preparation for analysis: Open the sample press by rotating the top knob counterclockwise until the top of the press travel is reached (see Figure 5). Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 32: Collecting A Background Spectrum

    In the case of a volatile sample, larger amounts of sample can be applied without concern of leakage or damage to the instrument. However, using the smallest amount of sample possible will ease in the cleaning process. Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 33 For instructions on reviewing results and handling sample data, refer to the Agilent MicroLab PC Software User’s Guide. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 34: Germanium Atr Sampling Accessory

    Germanium ATR Sampling Accessory The Agilent Germanium attenuated total reflectance (Ge ATR) sampling accessory for the Cary 630 FTIR takes advantage of the physical properties of light when encountering two materials with differences in index of refraction. When coming in contact with a...
  • Page 35 When in the sample analysis mode, the ATR sample pathlength is fixed, based on the number of reflections in the ATR. The alignment of the accessory is also pre-set at the factory, so there is no optical or mechanical adjustment required. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 36: Cleaning

    Place a small amount of the material to be measured on the Ge crystal. The crystal is the clear, circular shaped material held in place by the surrounding metal disk. Ensure that the sample covers the entire surface area of the germanium crystal. Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 37 For instructions on reviewing results and handling sample data, refer to the Agilent MicroLab PC Software User’s Guide. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 38: Bounce Zinc Selenide Atr Sampling Accessory

    Clean the 5 bounce ZnSe sampling window area using an extra-low lint, non-abrasive wipe or cotton swab and a suitable solvent, such as acetone, methanol, ethanol or isopropyl alcohol. Figure 8. Cleaning the 5 bounce ZnSe ATR sampling window Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 39: Collecting A Background Spectrum

    However, it is still possible the crystal or metal mounting plate can be damaged by extreme samples. Only measure samples with a pH between 4 and 9. Do not measure samples or use cleaners that fall outside this pH range. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 40: Transmission Sampling Accessory

    Transmission analysis can also be used for quantitative analysis using sealed cells or demountable cells with constant pathlengths. The Transmission accessory for the Cary 630 FTIR is specifically designed to accept industry standard sized cells. These can be obtained directly from Agilent or from your preferred accessory vendor.

  • Page 41: Cleaning

    Collect a background spectrum. For instructions on collecting a background using the software, refer to the Agilent MicroLab PC Software User’s Guide. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 42: Collecting A Sample Spectrum

    10 and 45 Degree Specular Reflectance Sampling Accessories The Agilent 10 and 45 degree specular reflectance accessories (SRA) for the Cary 630 FTIR allow for near-normal (<10 degrees) or at-angle (>10 degrees) specular reflectance measurements. Specular reflectance measurements are made on samples that, in general, are designed to reflect light from a flat surface.
  • Page 43 Analyzing Samples The 10 degree SRA slides in and out of the Cary 630 FTIR in seconds with no alignment required. See Page 24 for installation instructions. The 45 degree SRA easily slides into the transmission accessory. To install the 45 degree SRA into the Cary 630 FTIR:...

  • Page 44: Cleaning

    45 degree SRA accessory sampling window. This is commonly the gold coated mirror supplied with the accessory. Collect a background spectrum. For instructions on collecting a background using the software, refer to the Agilent MicroLab PC Software User’s Guide. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 45: Collecting A Sample Spectrum

    In this position, the sample mounting area can be easily accessed for loading the sample into place and for cleaning the sampling surfaces before the next sample is analyzed. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 46: Cleaning

    9, but there are some materials, such as strong acids or heavily basic materials, that can harm ZnSe. Avoid having materials in contact with the ZnSe window that are outside of this recommended pH range. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 47: Collecting A Background Spectrum

    TumblIR is not to be used with any solid or powder samples, such as tablets. Using the TumblIR with solid samples will damage the ZnSe windows or modify the pre-set transmission pathlength. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 48: Dialpath Sampling Accessory

    DialPath makes it much easier to prepare, load, analyze and clean the sample, while providing the flexibility of choosing from three factory-set pathlengths. The DialPath operates in two modes: sample loading/cleaning and sample analysis. Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 49 The DialPath arm must be completely rotated around until it reaches the detent and clicks into position. This detent keeps the accessory stationary during sample measurement. Figure 14. Rotating the DialPath Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 50: Cleaning

    Figure 15. Cleaning the DialPath Position 3 window (left) and cleaning the sample mounting area Use only soft cotton cloth, such as cotton swabs or a suitable substitute to clean NOTE the optical windows and sample mounting area. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 51: Collecting A Background Spectrum

    Page 50 until the window surfaces are clear of any residue. Collecting a sample spectrum To load a liquid sample and collect a spectrum using the DialPath accessory: Open the DialPath by rotating the arm (see Figure 14). Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 52 4 and 9. Close the DialPath by rotating the arm clockwise until it clicks into place. For instructions on collecting a sample spectrum using the software, refer to the Agilent MicroLab PC Software User’s Guide. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 53: Diffuse Reflectance Sampling Accessory

    3 to 5%. However, the loading of the sample in KBr can be adjusted to obtain the required sensitivity. The Diffuse Reflectance accessory is optimized for use with the Cary 630 FTIR optical system, providing the greatest sensitivity available for quick, accurate measurements.

  • Page 54: Cleaning

    Analyzing Samples Figure 18. Diffuse Reflectance accessory attached to Cary 630 FTIR. The sample holder pushes into the slot on the lower right of the accessory. Cleaning To clean the Diffuse Reflectance accessory sample holder in preparation for analysis: Remove the sample holder from the accessory and dispose of the KBr/sample mixture accordingly.

  • Page 55: Collecting A Background Spectrum

    Transfer the samples to the appropriate holder position. Do not contaminate other positions. Completely fill the position and then use a spatula or flat sided tool to create a flat surface and remove any overfill. Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 56 For instructions on reviewing results and handling sample data, refer to the Agilent MicroLab PC Software User’s Guide. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 57: Maintenance

    Do not completely immerse the Cary 630 FTIR in water. Replacing the Desiccant The desiccant in the Cary 630 FTIR is a disposable cartridge (see Figure 19), which can be replaced by the user when required. Figure 19. Desiccant cartridge...
  • Page 58 (rather than pink or blue) color. Changing the desiccant is recommended once the humidity level has reached 30%. Figure 20. Humidity indicator on rear of Cary 630 FTIR (left), and close-up (right) Desiccant cartridge Figure 21. Desiccant cartridge location on bottom of Cary 630 FTIR To replace the desiccant: Remove the desiccant from the sealed bag.

  • Page 59: Replacing Windows

    Maintenance Replacing Windows Each Cary 630 FTIR spectrometer and sampling accessory has a window that seals the system shut (except for the Transmission sampling accessory). The exit window of the main unit is dependent on the version of the system (KBr or ZnSe), as well as the type of ATR sampling accessory.

  • Page 60: Replacing The Source

    • Phillips screw driver • Before starting this procedure, turn off your Cary 630 FTIR. Unplug the system from the main power source and from the USB connection to the computer. Also, remove any sampling accessory from the Cary 630 FTIR so you are left with just the main unit.
  • Page 61 Using the 3/32 ball driver, remove all four screws. Desiccant cartridge Figure 24. Bottom of Cary 630 FTIR, showing screws to remove (circled) All four screws are captive and will not completely disengage. Be careful not to NOTE mistake the screws that hold the foot placements as correct screws for removing the base plate.
  • Page 62 Identify the source assembly. The source is located on the top of the interferometer frame. It is secured by three Philips head screws (see Figure 28). Using the appropriate Philips head screwdriver, remove all three screws. Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 63 For alignment purposes, the opening on the source assembly goes towards the NOTE front of the instrument (where the sampling accessory is normally located). Attach with the three Philips head screws that were removed previously. Figure 29. Removing the source assembly Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 64 Perform only those procedures described in this manual. For all other technical problems, contact your authorized Agilent representative. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 65: Spare Parts

    Desiccant with purge fitting G8043-67402 KBr window with removal tool and purge fitting G8043-67403 ZnSe window with removal tool and purge fitting G8043-67003 Cary FTIR Swivel Diamond ATR Press G8043-67004 Cary FTIR Swivel Ge-ZnSe Press Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 66: Sampling Accessories

    10 Degree SRA G8043-68314 45 Degree SRA (for the Transmission accessory) G8043-68320 1B Diamond ATR G8043-68321 1B ZnSe ATR G8043-68322 1B Ge ATR For extra sampling accessories, service contracts, repairs and refurbishment services, contact Agilent. Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 67: Specifications

    Width: 21 cm (8.25 in)  Depth: 10.2 cm (4.00 in)  Height: 17.1 cm (6.75 in)  Weight: 2.9 kg (6.5 lb)  Power supply: 100–240 V AC, 0.93 A, 50–60 Hz  Agilent Cary 630 FTIR Spectrometer User’s Guide...

  • Page 68: Safety Information

    Specifications Safety Information The Cary 630 FTIR system contains a low-powered solid state laser required for operation but in no operation or maintenance mode will the operator be exposed to radiation levels that exceed those that define a Class 1 laser product Class 1 Laser Complies with 21 CFR 1040.10 and 1040.11 except for deviations...

  • Page 69: Environmental Conditions

    Make sure that all peripheral devices are also certified. Make sure that appropriate cables are used to connect the device to peripheral equipment. Consult your equipment dealer, Agilent Technologies, or an experienced technician for assistance. Changes or modifications not expressly approved by Agilent Technologies could void the user’s authority to operate the equipment.
  • Page 70 Specifications This page is intentionally left blank. Agilent Cary 630 FTIR Spectrometer User’s Guide...
  • Page 72 In This Guide The guide describes the following: Introduction  Getting Started  Analyzing Samples  Maintenance  Spare Parts  Specifications  © Agilent Technologies 2012, 2013, 2016, 2018 1/18 *G8043-90001* *G8043-90001* G8043-90001 Issue 5...

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