Agilent Cary 630 FTIR Diamond ATR Accessory SOP

Transcription

1 Laboratory Standard Operating Procedure Agilent Cary 630 FTIR Diamond ATR Accessory SOP Ver. 0.5 Dept: MSE Building/Room: Hoover 3365A Supervisor: Michelle Grawe Written by Ryan Braga date 12/31/18 Approved by date Effective Date from 12/31/18 to 12/31/19 1 P age

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3 1. Procedure overview The Agilent Cary 630 FTIR spectrometer provides quantitative and qualitative information for routine analysis of solids, liquids, and gases. Specifications: Interferometer: 25 mm, permanently aligned, Michelson, 45, mechanical flexure; Enclosure: Sealed and desiccated; Spectral range: KBr cm-1, ZnSe cm-1; Spectral resolution: < 2 cm-1; Wavenumber accuracy 0.05 cm-1; Wavenumber reproducibility: cm-1. The Diamond ATR sample accessory allows for liquids, pastes, powders and some solid samples, 2. Health and Safety A. Health and safety information for materials used: This safety document does not cover any samples or chemical brought in by the investigator/user of the equipment. Familiarize yourself with the SDS and hazards of any chemicals or samples that you bring in to use with the Agilent Cary 630 FTIR. Acetone, methanol, ethanol and isopropyl alcohol are used to clean the surface of the sampling accessories. Acetone is extremely flammable. B. Hazard Control Measures: Lab coat, eye and hand protection, and closed toe/heel shoes must be selected as required by Section D of the ISU Laboratory Safety Manual. Latex gloves Insulated gloves Face Shield Respirator Nitrile gloves Safety glasses Lab Coat Fume hood Neoprene gloves Vented goggles Apron Biosafety cabinet Vinyl gloves Splash goggles Dust mask Glove box Closed Toe/Closed Heel Shoes Other Control Measures: Flame Resistant Lab coat C. Waste Disposal Procedures: Waste disposal procedures are determined by the nature of the samples that the user brings into the lab. Consult the waste disposal procedures for your chemicals and samples before beginning your investigations 3 P age

4 D. First Aid Procedures: First Aid procedures are determined by the nature of the samples that the user brings into the lab. Consult the First Aid procedures for your chemicals and samples before beginning your investigations E. Spill/Release Containment, Decontamination, and Clean Up Procedures: Spill/release procedures are determined by the nature of the samples that the user brings into the lab. Consult the Spill/release procedures for your chemicals and samples before beginning your investigations Acetone: to be added in later revision F. Hazard Assessment Hazard Engineering Control(s) Administrative Control(s) Required PPE Acetone Extremely flammable Methanol, ethanol and isopropyl alcohol - flammable Do not bring acetone into the lab area unless cleaning procedures are needed Do not bring alcohols into the lab area unless cleaning procedures are needed Cleaning other than routine sample run cleaning can be done by MSE staff members Cleaning other than routine sample run cleaning can be done by MSE staff members Eye protection, gloves, closed toe/closed heal shoes, lab coat Eye protection, gloves, closed toe/closed heal shoes, lab coat G. Training Record Safety Training tracking is done online. Complete your safety training before using MSE lab equipment. 4 P age

5 3. Procedure A. Usage Log Entries must be placed in the log book each time the equipment is used. Entries should include: Users Name, Supervisor / PI, Equipment used and the material being analyzed Log book must be kept with the equipment. Record equipment usage in ILab. B. Equipment Setup a. Turning on the FTIR i. Press the power button of the Cary 630 system and hold for 2 seconds ii. The light will flash green and red during startup. Within 15 to 20 seconds the light should turn solid green iii. Allow the system to warm up and stabilize for at least 5 minutes before conducting analysis. Scheduling Instructions b. Open Software i. Open MicroLab PC software in the Agilent folder 1. Username: admin 2. Password: admin C. Operation c. Record usage of the instrument in ILab d. Sample preparation is determined by the user s sample and test. e. Select method from method list f. Press the flashing Start button 5 P age

6 g. Open Sample press and wipe clean the sample window and select Next h. The instrument will collect a background reading i. Place the sample on the sample window (close the sample press if it is a solid sample) j. Select Next and enter Sample ID and Comments into fields if so desired. 6 P age

7 k. Select Next to run sampling cycle. At the end of the sampling cycle, pressing the Details button will open a graph, Data Handling will allow for modification of sample ID and Comments as well as Reporting and Exporting l. Close sample press when done. D. Cleanup/Shutdown a. Shutdown the Cary 630 FTIR pressing the power button for 2 seconds and make sure the light changes to red. b. Wipe down sample windows with a damp kimwipe or using acetone if the sample is adhering to the sample window. c. Close the sample press if using the Diamond ATR accessory d. Place dust cover on Cary 630 FTIR e. Close out of the MicroLab PC software and log off workstation f. Remember to Log Out of ILab. Remember to Log Out of ILab 4. Troubleshooting Common errors and problems experienced by users. If you find additional errors or troubleshooting tips and hints, drop a note to the Lab Coordinator so that this document can be updated. 7 P age FTIR power light trouble shooting Power light off system is off or unplugged Power light it red System has power but is switched off Power light is flashing red and green System is starting up

8 Power light is green system is ready to use Power light flashes green twice and red twice System requires firmware update consult lab coordinator. Button on top of the FTIR must be green, if red then restart computer Changing the Sampling accessory head i. Press the release lever on the 630 base unit outward ii. Remove the accessory or the protective shield from the base unit and the protective shield from the desired accessory. iii. The accessory is meant to slide into the recessed or dovetailed area. This is done by matching the dovetail to the front plate and sliding it downward. iv. The accessory is in place when the release level snaps back into place 5. Revisions: Record of changes to procedures Revision 0.5 initial draft 12/31/18 Initial version of SOP v1.0 date Revisions date 8 P age

9 6. Troubleshooting 9 P age