Agilent 4200 FlexScan FTIR Operation Manual
Contents
1. e e 00 e e 1 Introduction a 8 6 The Agilent 4200 FlexScan FTIR instrument is a portable handheld battery operated analyzer designed to measure a variety of solid and liquid samples in locations difficult or impossible to analyze ina laboratory It can be used for quantitative or qualitative analysis of materials The system is small lightweight and packaged ina weather resistant enclosure suitable for outdoor use It comes standard with internal battery power for operation of up to 4 hours The 4200 FlexScan FTIR can be safely used in operating temperatures ranging from 0 to 50 degrees Celsius 82 to 122 degrees Fahrenheit and in humidity environments as high as 95 for extended periods of time WARNING Fire Hazard 4200 FlexScan 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 manual the protection provided by the equipment may be impaired Agilent 4200 FlexScan FTIR Operation Manual 5 Introduction CAUTION Although the 4200 FlexScan FTIR system is designed to withstand significant shock and vibration found in a field environment use caution when handling and avoid dropping the system when it is out of the shipping case Dropping the system may result in equipment failure The 4200 FlexScan FTIR uses technology known as Fourier transform infrared FTIR spectrosco2. Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met A WARNING notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly performed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indicated conditions are fully understood and met Agilent 4200 FlexScan FTIR Operation Manual Contents Contents 1 Introduction 5 2 Getting Started 9 Unpacking 9 Packing list 10 Components 11 Installing the battery 12 Power switch LED status 13 Starting the software 14 Charging the handheld PC 15 Logging on to MicroLab Mobile for the first time 15 Performance verification 16 Diagnostic values 17 Performance validation 19 3 Analyzing Samples 23 External reflectance grazing angle and diffuse reflectance 23 Reflectance standards and gain settings 24 Steps 25 Collecting a background spectrum 25 Collecting a sample spectrum 26 Internal reflectance ATR 27 Steps 28 Cleaning the sample probe 28 Collecting a background spectrum 29 Agilent 4200 FlexScan FTIR Operation Manual 3 Contents Collecting a sample spectrum 30 Using the solid sample ATR press 31 4 Maintenance 35 5 Spare Parts 37 6 Specifications 39 Technical 39 Environmental conditions 40 Handheld PC data station 40 4 Agilent 4200 FlexScan FTIR Operation Manual Introduction amp E
3. For additional instructions on adding a user to the system and other initial software setup procedures refer to the MicroLab Software Operation Manual CAUTION If a 2 4 GHz cordless phone or a cellular telephone is used near the 4200 FlexScan FTIR you may experience problems with the wireless communication and spectroscopic performance Try turning off the phone or moving further away from the instrument and attempt the application again Performance verification The 4200 FlexScan FTIR spectrometer systems have 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 instrument is running properly To run and interpret the performance test refer to the MicroLab Software Operation Manual The performance test measures the energy level of the instrument 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 now ready to analyze a sample A yellow or red circle indicates the instrument is operating outside of the factory defined parameters These parameters are listed below as well as on the Advanced Features software page If the circle at the top of the software screen is yellow or red contact Agilent technical support for assistance 16 Agilent 4200 FlexScan FTIR Operation Manual Getting Started Like any measurement device it is important to veri
4. 301 304 305 307 520 2002 2003 2004 2005 0018 300 Spare Parts e 5 Spare Parts Description Agilent 4200 FlexScan FTIR system with external reflectance Agilent 4200 FlexScan FTIR system with diffuse reflectance Agilent 4200 FlexScan FTIR system with grazing angle Agilent 4200 FlexScan FTIR system with diamond ATR Diffuse gold reflectance reference cap for diffuse reflectance Polystyrene frequency reference cap for diffuse reflectance Diffuse gold reflectance reference cap for external reflectance Polystyrene frequency reference cap for external reflectance Mirrored stainless steel reflectance reference cap for external reflectance ATR sample press Handheld PC PDA Handheld PC docking station includes USB and power cables Replacement handheld PC battery Replacement lithium ion battery USB cable For sampling accessories upgrades service contracts repair and refurbishment services contact Agilent Agilent 4200 FlexScan FTIR Operation Manual 37 Spare Parts This page ts intentionally left blank 38 Agilent 4200 FlexScan FTIR Operation Manual Specifications amp E e e 0 e 6 Specifications 09 Technical 39 ae e A Environmental conditions 40 ia Handheld PC data station 40 Technical Interferometer geometry High throughput Michelson interferometer with fixed and moving flat mirrors Standard beamsplitter Zinc selenide Maximum spectral
5. FlexScan FTIR Operation Manual Getting Started WARNING Electrical Shock Hazard Avoid shock hazard Never allow liquid to run into the 4200 FlexScan FTIR battery compartment 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 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 Low battery Green 50 0 5 s on 0 5 s off Critically low battery Red 50 0 5 s on 0 5 s off Dead battery No LED illumination N A Firmware update Red green Green blinks rapidly twice then red blinks rapidly twice CAUTION The power button is a momentary switch to avoid accidental power off In order to turn the system on or off hold the button down for two 2 seconds The 4200 FlexScan FTIR contains a lithium ion rechargeable battery pack Agilent has fully charged the 4200 FlexScan system prior to shipment The 4200 FlexScan battery life under continuous use is approximately 4 hours Agilent 4200 FlexScan FTIR Operation Manual 13 Getting Started Starting the software 14 The 4200 FlexScan FTIR systems are supplied with the Agilent MicroLab Mobile software which has already been installed on your handheld PC To s
6. 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 45 degree external reflectance and grazing angle reflectance measurements the appropriate reflectance reference cap should be in place for the entire test No reference cap is needed when using the ATR sample interface The test results are expressed as Transmittance difference versus 100 of maximum deviation during the Stability test The table below gives the minimum performance for this test Table 4 Minimum performance for the Stability test Time Specification 3000 cm Specification 1000 cm 30 min 2 1 20 Agilent 4200 FlexScan FTIR Operation Manual Getting Started Laser Frequency Calibration test The Laser Frequency Calibration test measures the frequency X axis accuracy The test is conducted by measuring a spectrum of a polystyrene film Absorbance frequencies from this spectrum are compared to frequencies set by NIST SRM 1921 polystyrene film The software enables administrative level users to use the test results to set the laser calibration Laser calibrations should only be set after consultation with an Agilent technical support engineer For this test a background is measured first For 45 degree external reflectance and grazing angle reflectance sample
7. grazing angle sample probe Table 2 Diagnostic values Value Optimal green Energy 29 000 21 000 centerburst Battery life AC or gt 30 min Source 1 9A Laser signal 12 000 4 000 Detector 35 44 temperature CPU 10 75 temperature 18 Marginal yellow gt 29 000 or lt 21 000 30 5 min gt 2 2 or lt 1 6 gt 12 000 or lt 4 000 lt 35 or gt 44 gt 75 Critical red gt 31 000 or lt 18 000 lt 5 min gt 2 5 or lt 1 0 gt 15 000 or lt 3 000 lt 30 or gt 48 gt 80 Comment Indicates the overall alignment and proper gain adjustment for the system Indicates a problem with the source control voltage or that the source has burnt out Both voltage and amperage are displayed however amperage provides a sufficient diagnostic Can verity gross alignment errors even if the reflectance cap is not in place Indicates a problem with the cooling circuitry or an ambient temperature over the specified range Indicates the ambient temperature over the specified range Agilent 4200 FlexScan FTIR Operation Manual Getting Started Performance validation The MicroLab PC and MicroLab Mobile software have three tests appropriate for performance validation of the 4200 FlexScan FTIR All of these tests can be accessed from the Advanced Features System Check page of the MicroLab PC and MicroLab Mobile software The 4200 FlexScan system should be warmed up for at least 30
8. minutes before conducting any of these tests These tests can be run on a quarterly bi annual or annual basis to determine that the instrument is performing within its specification Performance signal to noise test This test measures the signal to noise level at two regions of the IR spectrum 2500 cm and 1000 cm The signal to noise is defined as the reciprocal of the root mean squared RMS noise in the defined region for a blank sample measured with a blank background Both the background and sample are measured at 4 cm resolution with a one minute collection time This test takes 2 minutes per test The user can specify a number of tests to be conducted For 45 degree external reflectance and grazing angle reflectance measurements the appropriate reflective reference cap should be in place for the entire test No reference cap is needed when using the ATR sample interface At least 10 tests should be collected in order to obtain an accurate picture of the performance The table below gives the minimum performance for each sample interface Table 3 Minimum performance for the Signal to Noise test Sample interface Specification 2500 cm 1 Specification 1000 cm 1 ATR 2500 6000 External reflectance 1500 2800 Grazing angle 1500 2800 Agilent 4200 FlexScan FTIR Operation Manual 19 Getting Started Stability test This test measures the short term stability at two regions of the spectrum 3000 cm and 1000 cm Stability is
9. near the sample interface Overlap the strap around the loop and secure using the Velcro at the end of the strap 3 For detailed software instructions for collecting a background refer to the MicroLab Software Operation Manual Collecting a sample spectrum To collect a sample spectrum 1 Once the background is finished collecting the software will instruct you to put the probe in contact with the sample It is recommended to use the provided strap to secure the 4200 FlexScan FTIR to the user and avoid damage due to dropping the system To install the strap hook both ends 2 spring clips of strap to the rod on the lower back panel of 4200 FlexScan just above the handle Place the strap around the shoulder or neck 2 The software will now display a graph showing the intensity absorbance of the sample measurement This screen is used to ensure that the sample has been correctly placed at the sampling interface For 4200 FlexScan FTIR applications using reflectance the value should be between 0 01 and 2 AU Use the real time data viewer in the software to ensure good contact between the sample and the probe and then choose to collect the data using the 4200 FlexScan FTIR software 26 Agilent 4200 FlexScan FTIR Operation Manual Analyzing Samples 3 Click the Next button on the software screen to proceed with the analysis Clicking the Home button will stop the measurement and return you to the Home screen 4 For detailed soft
10. resolution 4 cm Laser Low powered solid state Source Wire wound element Spectral range 4000 to 650 cm Sample interface External reflectance 45 grazing angle 82 diffuse reflectance normal incidence or single reflection diamond internal reflectance Detector 1 3 mm diameter thermoelectrically cooled dTGS Optical compartment 5 5 x 4 75 x 3 9 in 14 x 12 1 x 9 9 cm 3 2 lb 1 45 kg Electrical compartment 7 5 x 4 x 2 5 in 19 x 10 2 x 6 4 cm 2 5 lb 1 16 kg Cord 6 5 ft 1 98 m extended 20 in 7 8 cm coiled 2 1 lb 0 95 kg Battery Li ion 10 8 V 4400 mAh Agilent 4200 FlexScan FTIR Operation Manual 39 Specifications Environmental conditions Temperature 0 to 50 C 32 to 122 F during use Temperature Minus 30 to 60 C 22 to 140 F storage Humidity Up to 90 non condensing Handheld PC data station Processor 520 MHz Intel PXA270 Memory 64 MB low power RAM Hard drive 128 MB NAND flash 40 Agilent 4200 FlexScan FTIR Operation Manual www agilent com In This Guide The manual describes the following e Introduction e Getting Started e Analyzing Samples e Maintenance e Spare Parts e Specifications Agilent Technologies 2010 2011 2013 Printed in Malaysia 05 13 0024 401 Issue 3 Ete Agilent Technologies
11. the sample press on samples that may be sharp or pointed Steps The steps involved in performing an ATR analysis are 1 Clean the ATR sample mounting window 2 Collect a background spectrum 3 Collect a sample spectrum Cleaning the sample probe Before using the 4200 FlexScan FTIR ATR system on a new sample it is important as a first step to ensure the sampling surface is clean Kimwipes or a suitable substitute such as cotton swabs should be used to clean the sensor and sampling area Clean the sample interface with a suitable solvent such as acetone methanol ethanol or isopropyl alcohol Visually inspect the probe tip after cleaning to make sure there is no film haze or other residue present Agilent 4200 FlexScan FTIR Operation Manual Analyzing Samples Do not break the spectrometer seal and attempt to clean interior surfaces Breaking the seal will void the warranty Collecting a background spectrum To ensure accuracy of the measurement it is recommended that the system is configured in the software to collect a background spectrum before every sample is analyzed This provides a baseline profile of the system conditions with no sample loaded on the instrument By collecting a background automatically before each sample measurement negative effects of changes in the environment can be avoided To collect a background spectrum 1 From the software choose a method and click Start to begin the measurement T
12. 00 FlexScan FTIR Operation Manual 33 Analyzing Samples This page ts intentionally left blank 34 Agilent 4200 FlexScan FTIR Operation Manual Maintenance amp o e e c e 4 Maintenance o9 amp S When the outside of the Agilent 4200 FlexScan FTIR system needs cleaning disconnect the USB cable and ensure that the battery compartment is closed Use a damp soft cloth and a mild detergent to wipe down the outside of the unit Do not completely immerse the 4200 FlexScan in water Although the main optical housing is sealed water can penetrate the electrical compartment Hazard User servicing of parts and components beyond the procedures outlined in this manual may pose a safety risk to you damage your instrument and invalidate the instrument warranty Perform only those procedures described in this manual For all other technical problems contact your authorized Agilent representative Hazard The 4200 FlexScan FTIR was designed to operate in remote locations However analyzing certain materials and some maintenance procedures may be hazardous if the following guidelines are not practiced Agilent 4200 FlexScan FTIR Operation Manual 35 Maintenance 36 This page ts intentionally left blank Agilent 4200 FlexScan FTIR Operation Manual Part number 0024 0024 0024 0024 0023 0023 0023 0023 0023 0023 800 800 800 800 430 001 002 003 004
13. Agilent 4200 FlexScan FTIR Operation Manual Agg Agilent Technologies Notices Agilent Technologies Inc 2010 2011 2013 No part of this manual may be reproduced in any form or by any means including electronic storage and retrieval or translation into a foreign language without prior agreement and written consent from Agilent Technologies Inc as governed by United States and international copyright laws Manual Part Number 0024 401 Edition Third edition May 2013 Printed in Malaysia Agilent Technologies Inc Errata Statement NOTICE This document contains references to A2 Technologies Please note that A2 Technologies is now part of Agilent Technologies For more information go to www agilent com chem Warranty The material contained in this document is provided as is and is subject to being changed without notice in future editions Further to the maximum extent permitted by applicable law Agilent disclaims all warranties either express or implied with regard to this manual and any information contained herein including but not limited to the implied warranties of merchantability and fitness for a particular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing use or performance of this document or of any information contained herein Should Agilent and the user have a separate written agreement with warrant
14. antage of extreme hardness as well as chemical resistivity Diamond can accept samples with a pH range from 1 to 14 which means hard or abrasive samples and even strong acids can be safely analyzed The Agilent 4200 FlexScan FTIR ATR sampling probe is a single reflection system The diamond is the world s most durable substance and the ZnSe monolithic substrate is used as a focusing lens to provide the maximum IR signal Agilent 4200 FlexScan FTIR Operation Manual 27 Analyzing Samples 28 The single reflection ATR is most suitable for higher absorbing samples such as rubber polymers paints and fibers Powder and solid samples are best measured on the single reflection ATR as well due to the optional sample press device that can apply high pressure to powder and solid samples to ensure good contact with the diamond sampling surface The single reflection ATR is also a good choice when the amount of available sample is limited The single reflection diamond is 2 mm in diameter with a 200 um active area and provides an approximate 2 micron depth of penetration for IR energy at 1700 cm The single reflection ATR element protrudes slightly above the probe s metal mounting plate Although diamond is a very hard material the ATR window is relatively thin and can crack under extreme pressure conditions Make sure the sample makes contact with the entire surface area of the diamond and not just a point within the diamond Avoid the use of
15. battery gives approximately 4 hours of run time A battery charger is also included refer to the battery charger manual for information on its operation There is an LCD display on the front of the battery indicating the level of charge Five 5 bars indicate a full charge The 4200 FlexScan FTIR has a door on the front of the handle The door on the front gives access to the system battery The door must remain closed and locked while the system is in use The 4200 FlexScan should arrive with one battery in the shipping case To install the battery 1 Release the battery door tab on the top of the electrical housing see Figure 1 2 Slide the battery into the compartment with the tab of the battery facing downward and towards the front side of the 4200 FlexScan FTIR The V grove on the top of the battery interfaces with the tab on the top of the battery compartment 3 Slide the battery towards the back of the compartment until you feel the battery engage 4 Continue to slide another eighth of an inch until completely engaged If the battery is not fully engaged the system will not operate properly 5 Close the battery compartment door Depending on temperature and age of the battery the system should generally operate for a period of four hours on battery power To remove the battery from the compartment open the door and pull on the black plastic tab to slide the battery out of the 4200 FlexScan FTIR housing Agilent 4200
16. be for the 4200 FlexScan FTIR is a single reflection ATR The single reflection ATR sampling technique is ideal for identification of thick or highly absorbing samples where small IR pathlengths are required typically 2 micron depth of penetration Agilent 4200 FlexScan FTIR Operation Manual 7 Introduction The 4200 FlexScan FTIR is equipped with a handheld PC Socket PDA as standard and can be interfaced to the optional laptop computer for development of new methods and for detailed viewing and manipulating the spectra The 4200 FlexScan software user interface is intuitive simple to use and requires no specialized technical training The spectral display is represented with easy to read status bars and report formats which increase ease of use on the smaller handheld PC display With the touch of a button the system provides valuable information about the identity and amount of chemical substances present in a material 8 Agilent 4200 FlexScan FTIR Operation Manual Getting Started 2 ee 2 Getting Started D Unpacking 9 i m Components 11 i Installing the battery 12 Power switch LED status 13 Starting the software 14 Performance verification 16 Unpacking To unpack your spectrometer system 1 After receiving the Agilent 4200 FlexScan 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 th
17. d by extreme samples Only measure samples with a pH between 1 and 14 Do not leave extremely acidic samples on the metal mounting plate for an extended time Although diamond is a very hard material the ATR window is relatively thin and can crack under extreme pressure conditions Ensure that the sample makes contact with the entire surface area of the diamond and not just a point within the diamond Avoid using the sample press on samples that may be sharp or pointed Using the solid sample ATR press The 4200 FlexScan FTIR ATR system is offered with an optional sample press attachment that is removable when not required The sample press enables improved measurement of solid or powder samples The press ensures that the sample is in good contact with the diamond ATR sample interface which ensures the best possible results for these sample types The press is designed to deliver 15 pounds of force to the sample or over 2500 pounds per square inch of pressure It is not for use with liquids gels or pastes as the press may come directly in contact with the IR energy and alter the results These types of samples make good contact without the use of a press Agilent 4200 FlexScan FTIR Operation Manual 31 Analyzing Samples 32 Installing For initial installation of the ATR sample press 1 Clean any remaining sample residue off the diamond sample interface and the stainless steel sampling tube 2 Hold the 4200 FlexScan FTIR with t
18. e 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 4200 FlexScan FTIR has been packed to ensure that it arrives at your facility ready to go to work Custom foam inserts protect the instrument from damage during travel Whenever your instrument is shipped via common carrier it needs to be re packed in the shipping case Using this case your 4200 FlexScan can be removed and re packed in the case in a matter of seconds while maintaining instrument security Agilent 4200 FlexScan FTIR Operation Manual 9 Getting Started 10 2 The shipping enclosure 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 Keep all original packing material for storing shipping and transporting the system in the future 3 Remove the 4200 FlexScan 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 Plastic shipping case One Agilent 4200 FlexScan FTIR spectrom
19. ectra it is important to use the correct reflectance standard and to appropriately set the detector gain Detector gain is an electronic setting that maximizes the detector response from the available light The detector gain must be set such that both the reference material and the sample are within the linear range of the detector Agilent 4200 FlexScan FTIR Operation Manual Analyzing Samples The response of the detector is reported on the MicroLab PC and MicroLab Mobile software on the Diagnostics page available from the Advanced Features page it is labeled Energy The energy value has a range from 1000 to 30 000 First select the reference standard that is most similar to the sample the diffuse standard should be used for samples that scatter light while the mirror standard should be used for samples that reflect light With the appropriate reference in place observe the energy value The value should be close to 26 000 with the reference standard in place If the energy value is below 23 000 or above 29 000 counts click the Gain Adjust button The Gain Adjustment screen shows the Energy value at the top and has up down arrows to adjust the gain With the reference in place adjust the gain to bring the energy to 26 000 counts Once the appropriate gain is set it can either be saved as the System Default or Method gain The System Default gain is used for all methods while the Method gain is used only for the currently selected
20. eter system One Agilent 4200 FlexScan FTIR mirrored reference cap One Agilent 4200 FlexScan FTIR diffuse reference cap One Agilent 4200 FlexScan FTIR polystyrene frequency check standard Two Agilent 4200 FlexScan FTIR Li ion batteries One Agilent 4200 FlexScan FTIR Operation Manual One Agilent MicroLab Software Operation Manual One Socket handheld PC system PDA One Agilent 4200 FlexScan FTIR wrist strap One shipping container Agilent 4200 FlexScan FTIR Operation Manual Getting Started Cardboard box One handheld PC USB cable with power connector One battery charger One power supply for battery charger One AC line cord One installation disk needed as backup copy only One Agilent 4200 FlexScan FTIR USB cable Components The 4200 FlexScan FTIR is designed to measure samples in a handheld configuration Sample measurement can be started using the handle mounted trigger or the handheld PC touch screen Reference cap Handheld PC PDA Sample interface Battery door latch Battery compartment yE Agilent Technologies hee 4200 FloxSean FTIR PERENS Electrical housing Trigger RETURN Belt clip USB connection Power on off button Figure 1 Agilent 4200 FlexScan FTIR Agilent 4200 FlexScan FTIR Operation Manual 11 Getting Started Installing the battery 12 The 4200 FlexScan FTIR comes with two lithium ion batteries which are fully charged Each
21. fy that the 4200 FlexScan FTIR is performing properly before using the system to make critical measurements The 4200 FlexScan 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 instrument s function If the instrument is not functioning properly one of the diagnostic values will be out of specification Typically the instrument will not allow data collection if the diagnostic values are out of specification Performance validation tests are longer more involved tests that measure how well the instrument is working The tests listed under Performance validation check the instrument 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 The instrument will not collect data if the diagnostic values are grossly out of specification but it is good practice to verify that the instrument is working properly Performance validation should be run on a quarterly or bi annual basis Highly regulated industries may require the performance validation to be run monthly depending on the use of the instrument The performance validation verifies the key aspects to the instrument s ability to measure good data If the performance validation tes
22. he diamond sample interface pointing up Open the press arm Slide the ring of the press onto the stainless steel sampling tube Rotate the press in the clockwise direction while pressing down until the ring locks in place The press arm will be located at 12 00 4 00 or 8 00 There should be an audible click when the ring locks into place Installation of the solid sample press with the press arm in the downward position can damage the diamond sample interface Always install the press in the open position Removing To remove the ATR sample press 1 Hold the 4200 FlexScan FTIR with the diamond sample interface pointing up 2 Open the sample press arm so that the press tip is not in contact with the diamond sample surface 3 Twist the press ring in a counterclockwise direction approximately one quarter of a full rotation turn 4 Slide the press off the stainless steel sampling tube Measuring a sample To collect a sample spectrum using the ATR press 1 From the software choose a method and click Start to begin the measurement 2 Once the background is finished collecting the software will instruct you to put the diamond in contact with the sample Agilent 4200 FlexScan FTIR Operation Manual Analyzing Samples Place a small amount of material to be measured against the diamond ATR crystal The crystal is the clear circular shaped material held in place by the surrounding metal disk at the end of the probe For li
23. he software will collect a background automatically if the method selected was set up as recommended in the paragraph above The diamond should not be in contact with the sample or any substance other than the air in the atmosphere during the background measurement 2 For detailed software instructions for collecting a background refer to the MicroLab Software Operation Manual To ensure an accurate background spectrum is collected perform a visual inspection of the diamond ATR sample mounting surface looking for any haze or film present on the diamond from measuring the previous sample If a film is observed repeat the cleaning procedure above until the diamond surface is clear of any residue Agilent 4200 FlexScan FTIR Operation Manual 29 Analyzing Samples Collecting a sample spectrum To collect a sample spectrum using the ATR probe 1 Place a small amount of material to be measured against the diamond ATR crystal The crystal is the clear circular shaped material held in place by the surrounding metal disk at the end of the probe For liquid samples simply immerse the tip of the sample interface in the sample Small samples can be measured by placing a drop of sample on the center of the diamond interface Solid samples require establishing good contact between the diamond sampling interface and the sample Press the diamond firmly into the sample Tilt the instrument to ensure that the diamond surface is flat to the samp
24. interfaces the reflective reference cap is required for background measurements After the background collection a spectrum of polystyrene film is measured as instructed by the software When using the 45 degree external reflectance and grazing angle reflectance interfaces the polystyrene sample should be placed between the reference cap and the sample interface For the ATR sample interface the reference cap is not required for a background but the polystyrene test sample must be pressed firmly against the diamond sample interface during the sample collection The specification is listed below for each sample interface The difference between any of the listed frequencies and the standard value should be no greater than the specification Table 5 Minimum performance for the Laser Frequency Calibration test Sample interface Specification ATR lt cm External reflectance lt 1 cm Grazing angle lt 1 cm Agilent 4200 FlexScan FTIR Operation Manual 21 Getting Started 22 This page ts intentionally left blank Agilent 4200 FlexScan FTIR Operation Manual Analyzing Samples o oe 0 0 e 3 Analyzing Samples External reflectance grazing angle and diffuse 23 m Internal reflectance ATR 27 The Agilent 4200 FlexScan FTIR instrument is provided with a sample probe interface as specified on your order This section covers instructions for how to analyze a sample with all sampling probes offe
25. ion The grazing angle probe should be used when very low level contamination needs to be analyzed nanometer thickness levels Each reflectance sample interface requires the use of a reference sample for taking the background measurement prior to analyzing the sample The reference sample is incorporated into the 4200 FlexScan FTIR by means of a metal disk mounted into a cap that snaps onto the tip of the reflectance probe The 4200 FlexScan system offers two reference caps designed for this purpose a diffuse gold reference cap with a rough surface finish and a stainless steel mirror reference cap with a very smooth surface finish The diffuse gold reference cap should be used with the 45 degree reflectance probe when measuring low reflectance samples The mirror reference cap should be used with the 45 degree reflectance probe when measuring thin films or highly reflecting samples The mirror reference cap should always be used with the grazing angle sample probe The diffuse cap should always be used with the diffuse reflectance sample interface Ensure that the sample makes solid contact with the entire surface area of the external reflectance probe tip and is not held at an angle against the sample and that no movement occurs between the sample and the probe during the measurement Reflectance standards and gain settings The 4200 FlexScan FTIR is designed to measure a variety of sample types In order to measure the best quality sp
26. le 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 In all cases please be sure that the sample covers the entire surface area of the diamond crystal If the sample is a powder or solid the optional sample press may be needed to ensure good contact with the sample 2 Use the real time data viewer in the software to ensure good contact between the sample and the diamond and then choose to collect the data using the 4200 FlexScan FTIR software 3 Click the NEXT button on the software screen to proceed with the analysis 4 For detailed software instructions for measuring a sample refer to the MicroLab Software Operation Manual 5 After completing the sample measurement immediately clean the sample from the accessory using the instructions provided above It is important to make sure the sample mounting window is free of any residue from the previous sample 30 Agilent 4200 FlexScan FTIR Operation Manual Analyzing Samples 6 For detailed software instructions on reviewing results and handling sample data refer to the MicroLab Software Operation Manual The sample mounting window and accessory window are made from type lla synthetic diamond which is extremely chemically resistant However it is still possible the diamond or metal mounting plate can be damage
27. method Once the gain has been set it is useful to check the energy from a sample The sample must have energy greater than 1000 Also the sample should have energy less than that of the reference Steps The steps involved in performing an external reflectance analysis are 1 Collect a background spectrum using the reflectance cap 2 Collect a sample spectrum Collecting a background spectrum To ensure accuracy of the measurement it is recommended that the system is configured in the software to collect a background spectrum before every sample is analyzed This provides a baseline profile of the system conditions using the gold reference cap By collecting a background automatically before each sample measurement negative effects of changes in the environment can be avoided Agilent 4200 FlexScan FTIR Operation Manual 25 Analyzing Samples To collect a background spectrum 1 From the software choose a method and click Start to begin the measurement 2 The software will collect a background automatically if the method selected was set up as recommended in the paragraph above The software may prompt you to install the reference cap Install the appropriate gold reflectance reference cap tightly against the tip of the sample probe The reference cap has a black nylon strap with Velcro that can be used for convenience and security To install slide the nylon strap into the loop located on the front of the 4200 FlexScan FTIR
28. of solid or hard surface samples especially thickness measurement of thin coatings and films on reflective surfaces Typical applications include thickness measurement analysis of anodization of metals and measurement of surface cleanliness The External Reflectance System uses a 45 degree specular reflectance probe or a grazing angle specular reflectance probe The 45 degree probe is optimal for analysis of thin films greater than 1 micron in thickness Specular reflectance is an ideal method for the analysis of surface contamination Agilent 4200 FlexScan FTIR Grazing Angle System The grazing angle sample interface works in a similar manner to the external reflectance sample interface however the angle of incidence is 82 degrees The increased angle of incidence increases The grazing angle probe is optimal for analysis of ultra thin films less than 1 micron in thickness The grazing angle probe should be used when very low level contamination needs to be analyzed nanometer thickness levels Agilent 4200 FlexScan FTIR Internal Reflectance System For the chemical analysis of liquids powders pastes and gels The Internal Reflectance System uses a diamond optical sampling probe that incorporates the attenuated total reflectance ATR technique This method is optimal for the identification of a variety of samples and has the advantage that no sample preparation is required to obtain the proper IR absorbance levels The diamond ATR pro
29. py which is the current state of the art technique for molecular compound identification and quantification FTIR uses an infrared IR 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 In addition to the capability to measure samples onsite that in the past were typically measured in the lab this system is a non destructive tool NDT that allows the analysis to be performed without damaging the sample The heart of the Agilent FTIR spectrometer system is a patented Michelson interferometer design mounted on shock dampening mechanisms to protect the components from shock and vibration in the field This proprietary design is the key to successfully making FTIR technology compact lightweight rugged and field portable The 4200 FlexScan FTIR system can be configured for a number of different sampling configurations to accommodate the analysis of a range of liquids solids powders pastes and gels Information on the optimal use of the different sampling configurations of the 4200 FlexScan system is listed in the following categories 6 Agilent 4200 FlexScan FTIR Operation Manual Introduction Agilent 4200 FlexScan FTIR External Reflectance System For the chemical analysis
30. quid samples simply immerse the tip of the sample interface in the sample Small samples can be measured by placing a drop of sample on the center of the diamond interface Solid samples require establishing good contact between the diamond sampling interface and the sample Firmly press the diamond into the sample Tilt the instrument to ensure that the diamond surface is flat to the sample 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 In all cases ensure that the sample covers the entire surface area of the diamond crystal 3 Use the real time data viewer in the software to ensure good contact between the sample and the diamond and then choose to collect the data using the 4200 FlexScan FTIR software 4 Click the NEXT button on the software screen to proceed with the analysis 5 For detailed software instructions for measuring a sample refer to the MicroLab Software Operation Manual 6 After completing the sample measurement immediately clean the sample from the accessory using the instructions provided above It is important to make sure the sample mounting window is free of any residue from the previous sample 7 For detailed software instructions on reviewing results and handling sample data refer to the MicroLab Software Operation Manual Agilent 42
31. red on the 4200 FlexScan External reflectance grazing angle and diffuse reflectance The 4200 FlexScan FTIR instrument can be provided with three different reflectance interfaces external or specular reflectance grazing angle reflectance or diffuse reflectance Each of these sample interfaces relies on light reflecting from the sample surface When coming in contact with a sample the infrared IR light passes through the top surface of the sample before being reflected back out of the sample and into the detector of the 4200 FlexScan system This small and consistent pathlength provides the advantage of no sample preparation required to get good measurement results on a variety of samples The key to obtaining good results with external reflectance is making sure the tip of the probe makes stable contact with the sample surface and does not move during the measurement process The front of the sample interface defines the IR light focus or each of the reflectance sample interfaces Agilent 4200 FlexScan FTIR Operation Manual 23 Analyzing Samples 24 The 45 degree probe is optimal for analysis of thin films greater than 1 micron in thickness The grazing angle probe is optimal for analysis of ultra thin films less than 1 micron in thickness Diffuse reflectance is specifically designed for measurement of rough surfaces that scatter rather than reflect light Specular reflectance is an ideal method for the analysis of surface contaminat
32. tart the software once the 4200 FlexScan FTIR has been powered up 1 Turn on the handheld PC data station by depressing the power button on the top right corner of the data station see Figure 2 Power button socket f Figure 2 Data station showing power button location 2 The system is provided with a shortcut to the MicroLab Mobile software in the Start menu Upon initial power up of the handheld PC look in the computer display window and tap Start Then tap the MicroLab Mobile icon This will launch the MicroLab Mobile software application If the you see this message upon loading your software Instrument failed to initialize Instrument returned error code 2 The application will exit then power cycle the instrument and restart the application the spectrometer is not connected to the computer When using the handheld PC with MicroLab Mobile verify that the instrument displays a green light on the power button and verify that the Bluetooth communications of the handheld PC are turned On The instrument must be connected via Bluetooth for the MicroLab Mobile software to launch Agilent 4200 FlexScan FTIR Operation Manual Getting Started Charging the handheld PC To connect the handheld PC to an AC power source for charging the battery 1 Connect the USB cable to the handheld PC 2 Connect the computer AC power cable to the Y connector of the USB cable 3 Connect the handheld PC power cable
33. to the AC power source Alternatively if purchased place the PC in the optional handheld charging cradle For more information on the operation of the handheld PC see the supplied Socket User Manual Logging on to MicroLab Mobile for the first time As mentioned above the 4200 FlexScan FTIR systems are supplied with the Agilent MicroLab Mobile software already installed on your system A software disk for the Agilent MicroLab PC software is also included This allows use of the 4200 FlexScan with a desktop or notebook computer In addition the handheld PC is provided with a shortcut to the MicroLab Mobile software already installed in the Start menu To start the software 1 Tap Start then tap the MicroLab Mobile icon Upon initial launch of the system the MicroLab Mobile software automatically loads and a MicroLab application splash screen appears briefly showing software version copyright and trademark information The software will launch and display a logon screen If the 4200 FlexScan FTIR instrument has not been turned on first you will receive an Instrument Failed to Initialize warning message on the handheld PC If this happens tap OK power cycle the 4100 ExoScan instrument and restart the MicroLab Mobile application Agilent 4200 FlexScan FTIR Operation Manual 15 Getting Started 2 For detailed instructions on initial software logon and user management refer to the MicroLab Software Operation Manual
34. ts are within specification the instrument should provide data that works well with methods developed for the 4200 FlexScan As with any instrument however results can always be verified by running a known sample with the sample specific method Diagnostic values The following values can also be viewed on the Diagnostics page in the MicroLab Mobile or MicroLab PC software These values can be used to determine if the instrument is working properly They can be used on a daily basis to determine that the instrument is operating as intended In each case the Optimal value indicates that the system is running at its intended performance level The Marginal value indicates that the instrument is still functioning but at a lower performance level The Critical value indicates that the system is not working correctly Contact Agilent technical support for assistance if there is a problem with your instrument Agilent 4200 FlexScan FTIR Operation Manual 17 Getting Started When using the external reflectance or grazing angle sample interface the appropriate reflectance cap must be in place to make these measurements The diffuse gold reference cap should be used with the 45 reflectance probe when measuring carbon black or other low reflectance samples The gold mirror reference cap should be used with the 45 reflectance probe when measuring thin films or highly reflecting samples The gold mirror reference cap should always be used with the
35. ware instructions for measuring a sample refer to the MicroLab Software Operation Manual 5 After completing the sample measurement immediately clean the sample from the accessory using the instructions provided above 6 For detailed software instructions on reviewing results and handling sample data refer to the MicroLab Software Operation Manual Internal reflectance ATR The 4200 FlexScan FTIR instrument can be provided with a dedicated sampling probe interface called the attenuated total reflectance ATR probe The ATR takes advantage of the physical properties of light when encountering two materials with differences in index of refraction When coming in contact with a sample having a different index of refraction the infrared IR light creates an evanescent wave that provides a very small and specific depth of penetration into the sample before reflecting back into the detector of the 4200 FlexScan FTIR system This small and consistent pathlength provides the advantage of no sample preparation required to get good measurement results on a variety of samples The key to obtaining good results with an ATR is making good contact between the sample and ATR crystal of the sampling device The ATR technique can be used for analysis of liquids pastes powders and even some solid samples The Agilent ATR uses a type Ila synthetic diamond crystal as the interface between the sample and the infrared energy The diamond provides the adv
36. y terms covering the material in this document that conflict with these terms the warranty terms in the separate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accordance with the terms of such license Restricted Rights Legend If software is for use in the performance of a U S Government prime contract or subcontract Software is delivered and licensed as Commercial computer software as defined in 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 contract clause Use duplication or disclosure of Software is subject to Agilent Technologies standard commercial license terms and non DOD Departments and Agencies of the U S Government will receive no greater than Restricted Rights as defined in FAR 52 227 19 c 1 2 June 1987 U S Government users will receive no greater than Limited Rights as defined in FAR 52 227 14 June 1987 or DFAR 252 227 7015 b 2 November 1995 as applicable in any technical data Safety Notices A CAUTION notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly performed or adhered to could result in damage to the product or loss of important data
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