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Agilent Technologies 5500a, Operation Manual

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Agilent Technologies 5500a Operation Manual Download Page 35

Analyzing Samples 

Agilent 5500 Series FTIR Operation Manual 

35 

                                            

 

Figure 7.

 Sample press in highest position providing easy access for sample loading and cleaning 

In the sample analysis mode, the ATR sample press is lowered such 
that the sample press tip is in contact with the sample. In this 
position, contact is made between the sample and the IR energy 
emitting from the diamond ATR window (see Figure 8).  

NOTE 

If the sample is a liquid or paste, the sample press does not need to be used at 
all. In this case, you are now ready to proceed with the analysis. Only liquid or 
paste samples should be used with the triple and nine reflection ATR accessory. 

 

 

Figure 8.

 Sample press lowered for analysis 

Diamond ATR crystal

Sample press tip 

Sample press  

Summary of Contents for 5500a

Page 1: ...Agilent 5500 Series FTIR Operation Manual ...

Page 2: ...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...

Page 3: ...Turning on the instrument 15 Power switch LED 15 Starting the software 16 Logging on to MicroLab PC for the first time 16 Performance verification 17 Diagnostic values 18 Performance validation 20 3 Analyzing Samples 23 Lube samples with the Agilent 5500t FTIR 23 Cleaning the TumblIR accessory 25 Collecting a background spectrum 26 Measuring a sample 26 Agilent 5500t FTIR with a TumblIR 28 Cleanin...

Page 4: ...he accessory 36 Collecting a background spectrum 36 Collecting a sample spectrum 37 Agilent 5500 DialPath FTIR 39 Cleaning the DialPath accessory 41 Collecting a background spectrum 43 Measuring a liquid sample 43 4 Spare Parts 47 5 Specifications 49 Environmental conditions 50 Electromagnetic compatibility 50 ICES NMB 001 51 ...

Page 5: ...gilent 5500t FTIR system is designed specifically for onsite oil analysis and the Agilent 5500a FTIR system is designed for sample analysis in challenging multi user environments Both platforms provide versatility for use in a traditional analytical chemistry laboratory a temporary field laboratory or even in the field However it is primarily intended for indoor use and is not designed for water r...

Page 6: ... external computer running a Microsoft Windows XP 32 or 64 bit or Windows 7 32 or 64 bit operating system The computer must have at least a Pentium IV 3 GHz processor with 1 GB of memory and at least 40 GB hard disk capacity The laptop computer is offered as an option which provides the flexibility of supplying it yourself or purchasing from Agilent The 5500 FTIR system is available in a number of...

Page 7: ...is an ideal tool for oil analysis of diesel generators wind farms off shore applications or marine applications Both systems are equipped with a software user interface that is intuitive simple to use and requires no specialized technical training With the touch of a button the system provides valuable information about the identity and amount of chemical substances present in a material ...

Page 8: ...Introduction 8 Agilent 5500 Series FTIR Operation Manual This page is intentionally left blank ...

Page 9: ...s 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 2 The shipping enclosure should contain the items listed below 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 b...

Page 10: ...umblIR sampling accessory One Agilent 5500 Series FTIR Operation Manual One power cord One USB cable One installation disk One shipping container Options Although the spectrometer system comes standard as shown above there are a number of options available including Laptop computer Surfactant kit Extra cords Agilent 5500a FTIR packing list One Agilent 5500a FTIR mid IR spectrometer system includin...

Page 11: ...s To convert your 5500a FTIR system to a different accessory contact Agilent Connecting power To connect power to the spectrometer system 1 Insert the provided power cord into the power connector located on the lower left side at the rear of the 5500 Series FTIR system see Figure 1 Figure 1 Attaching the power cord 2 Thread the blue cap onto the power connector by rotating it clockwise until finge...

Page 12: ...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 CAUTION All cords must be kept away from high traffic areas The system could sustain damage to the apparatus or adapters...

Page 13: ...Getting Started Agilent 5500 Series FTIR Operation Manual 13 Power cord selection The following power cords can be used Figure 2 Suitable power cords ...

Page 14: ...5500 Series FTIR system see Figure 3 Figure 3 Attaching the USB cable 2 Thread the blue cap onto the USB connector by rotating it clockwise until finger tight To avoid damage to the plastic connector be careful not to over tighten 3 Connect the opposite end of the USB cable to the computer that will run MicroLab PC software NOTE The 5500t FTIR must be directly connected to the computer USB slot an...

Page 15: ...ff In order to turn the system on or off hold the button down for two 2 seconds Power switch LED The power button contains a two colored LED The color displayed on the LED can indicate the state of the system Table 1 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 S...

Page 16: ...MicroLab PC software application splash screen briefly appears showing the version copyright and trademark information The software will launch and display a logon screen When the logon screen appears the user name will be Admin when logging onto the system for the first time the software automatically initiates in an Administrator mode The default password for initial logon to MicroLab PC softwar...

Page 17: ...Features software page 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 5500 Series FTIR instrument is performing properly before using the system to make critical measurements The instrument provides both diagnostic values and performance validation tests to demonst...

Page 18: ...sts are within specification the instrument should provide data that works well with methods developed for the 5500 Series FTIR spectrometer 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 from the Diagnostics page in the MicroLab PC software These values can be used to...

Page 19: ...2 5 or 1 0 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 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 35 44 35 or 44 30 or 48 Indicates a problem with the cool...

Page 20: ...blank background Both the background and sample are measured at 4 cm 1 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 usin...

Page 21: ...libration Laser calibrations should only be set after consultation with an Agilent technical support engineer For this test a background is measured first 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 r...

Page 22: ...Getting Started 22 Agilent 5500 Series FTIR Operation Manual This page is intentionally left blank ...

Page 23: ...accessory designed and manufactured exclusively by Agilent to optimize the analysis of lubrication samples When comparing the TumblIR to traditional liquid cells for general analytical laboratories the TumblIR makes it much easier to prepare load analyze and clean the sample The TumblIR operates in two modes sample loading cleaning and sample analysis In the sample loading and cleaning mode the Tu...

Page 24: ...ards the 5500t FTIR sample mounting area In this position infrared IR energy passes through the sample making measurement possible Be sure to rotate the TumblIR arm completely around until it reaches the detent and snaps into position This detent keeps the accessory stationary during sample measurement see Figure 5 Figure 5 TumblIR with accessory window facing down Bottom window 2 mm diameter yell...

Page 25: ...n clean the bottom mounting window indicated in Figure 4 NOTE Only use soft cotton cloth such as found on cotton swabs or a suitable substitute to clean the optical sensor and sampling area CAUTION The windows are made of an IR transmitting material called zinc selenide ZnSe ZnSe is a relatively durable material but can be easily scratched or damaged if too much pressure is applied during cleaning...

Page 26: ... collecting a background refer to the MicroLab Software Operation Manual CAUTION To ensure an accurate background spectrum is collected perform a visual inspection of the ZnSe window surfaces looking for any haze or film present on the windows from measuring the previous sample If a film is observed repeat the cleaning procedures above until the window surfaces are clear of any residue Measuring a...

Page 27: ...aqueous solutions or even thick pastes such as grease the TumblIR is not to be used with any solid samples such as hard graphite lubricant Use of the TumblIR with solid samples will damage the ZnSe windows CAUTION The sample mounting window and accessory window are made from ZnSe ZnSe can be damaged by samples with a pH below 4 and above 9 Only measure samples with a pH between 4 and 9 CAUTION ZnS...

Page 28: ...ethods and reviewing data using MicroLab PC software refer to the MicroLab Software Operation Manual Agilent 5500t FTIR with a TumblIR The Agilent 5500t FTIR instrument can be provided with a dedicated sampling interface called the TumblIR accessory The TumblIR is a proprietary liquid transmission sampling accessory designed and manufactured exclusively by Agilent to optimize the analysis of many ...

Page 29: ...tory and so there is no adjustment required The steps involved with analyzing a sample on the 5500t FTIR system with a TumblIR are 1 Clean the sample windows 2 Collect a background spectrum 3 Collect a sample spectrum Cleaning the accessory To clean the TumblIR accessory 1 Rotate the TumblIR arm so the optical sensor is pointing upward 2 Clean the top window first then clean the bottom window indi...

Page 30: ...hat 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 For detailed software instructions for collecting a backgr...

Page 31: ... of leakage or damage to the instrument however using the smallest amount of sample possible will ease in the cleaning process Although it is safe to run a variety of liquid samples including aqueous solutions or even thick pastes such as grease the TumblIR is not to be used with any solid or powder samples such as tablets Use of the TumblIR with solid samples will damage the ZnSe windows or modif...

Page 32: ...oftware screen to proceed with the analysis 6 For detailed software instructions for measuring a sample refer to the MicroLab Software Operation Manual 7 After completing the sample measurement immediately clean the sample from the accessory using the instructions provided above It is important to make sure both the top and bottom windows are free of any residue from the previous sample 8 For deta...

Page 33: ...s the interface between the sample and the IR energy The diamond provides the advantage 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 Agilent offers three choices of ATR sampling accessories a single reflection triple reflection and nine reflection DuraDis...

Page 34: ...cm 1 The nine reflection ATR is slightly recessed into the mounting plate and does not operate with a sample press device It is however designed to accommodate an optional flow cell attachment CAUTION Although diamond is a very hard material the ATR window is relatively thin 0 5 mm or less and can crack under extreme pressure conditions Ensure that the sample makes contact with the entire surface ...

Page 35: ...h the sample In this position contact is made between the sample and the IR energy emitting from the diamond ATR window see Figure 8 NOTE If the sample is a liquid or paste the sample press does not need to be used at all In this case you are now ready to proceed with the analysis Only liquid or paste samples should be used with the triple and nine reflection ATR accessory Figure 8 Sample press lo...

Page 36: ...ss tip first then clean the sample mounting window indicated in Figure 7 NOTE Kimwipes or a suitable substitute such as cotton swabs should be used to clean the sensor and sampling area Clean the sample interface and press with a suitable solvent such as acetone methanol ethanol or isopropyl alcohol CAUTION Do not break the spectrometer seal and attempt to clean interior surfaces Breaking the seal...

Page 37: ...f a film is observed repeat the cleaning procedure above until the diamond surface is clear of any residue Collecting a sample spectrum To load an ATR sample into the system 1 Open the sample press by moving the arm back as far as it can go so that the sample press tip is elevated slightly from the diamond ATR surface see Figure 9 Figure 9 Opening the sample press 2 The diamond sampling window sho...

Page 38: ... samples with a pH between 1 and 14 Do not leave extremely acidic samples on the metal mounting plate for an extended time CAUTION 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 the use of the samp...

Page 39: ...e from the previous sample 8 For detailed software instructions on reviewing results and handling sample data refer to the MicroLab Software Operation Manual For additional instructions on editing methods and reviewing data using MicroLab PC software refer to the MicroLab Software Operation Manual Agilent 5500 DialPath FTIR The Agilent 5500 DialPath FTIR instrument is provided with a dedicated sam...

Page 40: ...ple analysis mode the DialPath is rotated such that the accessory optical window is facing down towards the 5500 DialPath FTIR sample mounting area In this position infrared IR energy passes through the sample making measurement possible Make sure that you rotate the DialPath arm completely around until it reaches the detent and snaps or clicks into position This detent keeps the accessory station...

Page 41: ... there is no adjustment required The steps involved with analyzing a sample with the 5500 DialPath FTIR are 1 Clean the sample window 2 Collect a background spectrum 3 Collect a sample spectrum Cleaning the DialPath accessory Rotate the DialPath so that optical sensor 2 is pointing upward Clean the window of the position used first then clean the bottom window indicated in Figure 10 If using Posit...

Page 42: ... or if an abrasive material such as Kimwipes is used Materials such as cotton swabs dipped in acetone are recommended for cleaning see Figure 12 Figure 12 Cleaning the Position 3 window and sample substrate CAUTION ZnSe is relatively chemically resistant to materials with a pH range between 4 and 9 but there are some materials such as strong acids or heavily basic materials that can harm ZnSe Avoi...

Page 43: ...ZnSe window surfaces looking for any haze or film present on the windows from measuring the previous sample If a film is observed repeat the cleaning procedure above until the window surfaces are clear of any residue Measuring a liquid sample To apply a liquid sample to the system 1 Open the sampling device DialPath by rotating the arm see Figure 10 2 The bottom window should be visible Place a sm...

Page 44: ...the DialPath with solid samples will damage the ZnSe windows or modify the pre set transmission pathlength CAUTION The top and bottom windows are made from ZnSe ZnSe can be damaged by samples with a pH below 4 and above 9 Only measure samples with a pH between 4 and 9 CAUTION ZnSe windows can be easily scratched by hard or abrasive samples Avoid use of samples that may scratch the surface of the w...

Page 45: ...is 6 For detailed software instructions for measuring a sample refer to the MicroLab Software Operation Manual 7 After completing the sample measurement immediately clean the sample from the accessory using the instructions provided above It is important to make sure both the top and bottom windows are free of any residue from the previous sample as well as adjacent windows to minimize any cross c...

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Page 47: ...ual 47 4 Spare Parts Part number Description 430 0001 Agilent 5500 Series FTIR power supply 430 0018 Agilent 5500 Series FTIR USB cable 0020 900 Surfactant kit For sampling accessories service contracts repair and refurbishment services contact Agilent ...

Page 48: ...Spare Parts 48 Agilent 5500 Series FTIR Operation Manual This page is intentionally left blank ...

Page 49: ...e Wire wound element Spectral range 4000 to 650 cm 1 Detector 1 3 mm diameter thermoelectrically cooled dTGS Power supply 100 120 240 V AC 3 A 50 to 60 Hz Computer External laptop Pentium IV 3 GHz processor or greater Microsoft Windows XP 32 or 64 bit or Windows 7 32 or 64 bit operating system Operating temperature range 0 to 50 C 32 to 122 F WARNING Laser Hazard Agilent 5500 Series FTIR systems c...

Page 50: ...he equipment itself Class A equipment is equipment suitable for use in all establishments other than domestic and those directly connected to a low voltage power supply network which supplies buildings used for domestic purposes This device complies with the requirements of CISPR11 Group 1 Class A as radiation professional equipment Therefore there may be potential difficulties in ensuring electro...

Page 51: ...ectrical outlet so that the device and the radio or television are on separate electrical circuits 4 Make sure that all peripheral devices are also certified 5 Make sure that appropriate cables are used to connect the device to peripheral equipment 6 Consult your equipment dealer Agilent Technologies or an experienced technician for assistance Changes or modifications not expressly approved by Agi...

Page 52: ...Specifications 52 Agilent 5500 Series FTIR Operation Manual This page is intentionally left blank ...

Page 53: ......

Page 54: ...m In This Guide The guide describes the following Introduction Getting Started Analyzing Samples Spare Parts Specifications Agilent Technologies 2008 2013 Printed in Malaysia 09 13 0020 401 0020 401 0020 401 Issue 5 ...

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