FT IR Operating procedure by using SPECTRUM v. 1.22 1- Press On button to start the FT-IR spectroscopy instrument (lower left side).2- Press Proceed ( soft key on instrument – top right) to make machine ready for scanning samples.3- Click (left mouse button) on SPECTRUM v.2.0 icon to start software.4- Go to menu under Instrument and click on Scan background option.5- Verify Scan background form which specifies spectrum details ( 1. file name =scanbkg.sp, 2. Description = Air) and Scan Parameters ( 1. Range: 4000- 600 cm-1, 2.Number of scans = 16,3. Resolution = 4.0 cm-1, 4. Interval = 2.0 cm-1, 5. Apodization =weak) then click Ok to start the scanning of background.6- Type in file- name.sp in the Instrument -Auto save form, and save the backgroundspectrum generated by instrument by clicking on New name option in the bottom of the form.7- Click on Print under File opt~n menu to print the background spectrum. 8-Click on New to start a new spectrum field.9- Insert the sample in the instrument's Sample Holder.10- Go to menu under Instrument and click on Scan sample option.11- Enter sample Spectrum details and Scan Parameters in Scan Sample form, as described in# 5 above, then click Ok to start scanning.12- Enter samplename.sp and click on New Name in the Instrument - Auto Save form, to savethe spectrum of your sample.13- To add text or comments to spectra, click on Add / Edjt Text option under View, then typethe comments ( sample name.sp, date, # of scans and resolution) in the Add/ Edit Text formand click on Ok.14- To move the text around the spectrum field, left click mouse button and drag text.15- To copy or delete text click on text to be edited, then select Cut! Copy under Edit menu.16- To label the peaks click on Label Peaks option under View.17- To move peaks labels around click on label and drag around.18- To remove peaks labels click on Clear All peak- Labels option under View.19- Go to Print under File menu to print the produced sample and background specta.FT-IR Manual Operation :1- To Reset: Shift Restore (Red Key), Set Up (Soft Key) and Factory.2- To get a spectrum: Select Storage area (X, Y, Z, Background), Scan, # of Scans, Executeand View spectra.3- To plot a spectrum: Ready plotter with pens 1 and 2, Place vertical cursor on peak ,and pressPlot (green key).4- To save to disk: Copy, Source (X,Y,i, Background), Disk, File Name, Enter (Blue Key)and comments.5- White Keys: Cursor and peaks are Onl OfT. Rearrange & RescaJe return spectra to original.Appendix:When scan background or sample. If the computer gives the message: (Instrument maybe busy,disconnected or wrongly configured) , then do the following:Press Setup, Others, Devices, Remote, (IBM PC – RS 232) Custom, Baud, 9600, Exit, Exit. This sequence should help solve the problem for the time being. .IR/FTIR Diamond A TR Instrument Operating ProceduresUpdated on: (10/13/04) Prepared by: D.L.L. and K.J.H.Installation of Diamond A TR1. Remove cover, lower plate,and black sample holderlocated on the left hand sideand place in the drawerlabeled 'ATR/FTIRAttachments'2. Find SensIR DuraScopediamond A TR attachment(located on the gray shelves near the blackboard) and slide it into the slotwhere the previously removed bottom plate was located. (Be sure to firmlyplace the ATR all the way to the back of the instrument).3. Extend adjustable purge tubes all the way and tighten the screws to secure.4. Plug in the DuraScope power supply.5. Attach the nitrogen purge line.6. Turn on the nitrogen gas at the cylinder (regulator should be set to 40-50ml/min)7. Turn on power to DuraScope ATR and LCD integrated video monitor.Obtaining a Background Spectrum1. Turn On the computer and FTIR.2. Press Proceed (soft key on instrument)3. Start SPECTRUM v.2.0 software.4. Obtain a background scan of nitrogen before running sample by:5. Go to Instrument menu. Select Scan Background. (until Energy%Transmittance is between 4-4.5.) The nitrogen should run for 30 min prior torunning background IR spectrum. The lab instructors will have it turned on beforeclass starts.6. Verify Spectrum Details (file name = scanbkg.sp, Description = Air) and ScanParameters (Rang~ = 4000-600 cm-I, Number of scans = 4, Resolution = 4.0cm-I, Interval = 2.0 cm-I, Apodization = weak). Click OK to scan thebackground. Specify a filename to save the spectrum.7. Go to File, Print to print the spectrum.Sample PreparationLiquids:1. Swing sample press to the back.2. Place O-ring centered on diamond sampling area3. Place desired amount of liquid in O-ring.4. For volatile liquids such as Acetone, cover sample with the glass cupto inhibit evaporation. (For best results, place volatile liquids inrefrigerator for at least 3Ominutes)Solids:1. Swing sample press to the back22. Grind solid with mortar and pestle until a fine powder. (Be careful tonot inhale dust)3. Place crushed sample over center ring making sure that it is coveredand verify by looking at the LCD to make sure sample is completelycovering the area.4. Swing sample press over center position.5. Obtain a stainless steel or polycarbonate pin, and fasten it in the swingarm. (Tile stainless steel pin is recommended.)6. Twist the large black knob on the sample press to apply pressure onthe sample. The":Load' gauge on the DuraScope will display greenlights. Continue twisting the knob until the first yellow light appears at8. Stop. Do not twist the knob further.Spectrum Collection1. Click New to start a new spectrum field.2. Insert the sample into the Sample Holder.3. Go to Instrument, Scan Sample.4. Enter the Spectrum Details and Scan Parameters as in Step 5. Click OK toscan. Specify a filename to save the spectrum.Editing SpectrumAdd text or comments: Go to View, Add/Edit Text. Click and drag to move text.3Shutdown the computer.Label Peaks: Go to View, Label Peaks. Click and drag to move a peak label. Go toView, Clear All Peak Labels to clear labels. To change sensitivity in labelingpeaks, go to Setup, Options, Peak. Change Threshold values.Print: Go to File, Print.Cleaning and Shutdown ProceduresClean the sample staging area with acetone and a kimwipe.Switch the FTIR off.Shut off nitrogen gas flowReference Spectrawww.aist.go.ip/RIODB/SDBSwebbook.nist.govGreen binder labeled 'FTIR Spectra, Plastics' on shelf above