FT IR Operating Procedure by Using SPECTRUM V. 1.22

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 background

spectrum 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 save

the spectrum of your sample.

13- To add text or comments to spectra, click on Add / Edjt Text option under View, then type

the comments ( sample name.sp, date, # of scans and resolution) in the Add/ Edit Text form

and 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, Execute

and View spectra.

3- To plot a spectrum: Ready plotter with pens 1 and 2, Place vertical cursor on peak ,and press

Plot (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 Procedures Updated on: (10/13/04) Prepared by: D.L.L. and K.J.H.

Installation of Diamond A TR

1. Remove cover, lower plate,

and black sample holder

located on the left hand side

and place in the drawer

labeled 'ATR/FTIR

Attachments'

2. Find SensIR DuraScope

diamond A TR attachment

(located on the gray shelves near the blackboard) and slide it into the slot

where the previously removed bottom plate was located. (Be sure to firmly

place 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 40-50

ml/min)

7. Turn on power to DuraScope ATR and LCD integrated video monitor.

Obtaining a Background Spectrum

1. 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 to

running background IR spectrum. The lab instructors will have it turned on before

class starts.

6. Verify Spectrum Details (file name = scanbkg.sp, Description = Air) and Scan

Parameters (Rang~ = 4000-600 cm-I, Number of scans = 4, Resolution = 4.0 cm-I, Interval = 2.0 cm-I, Apodization = weak). Click OK to scan the

background. Specify a filename to save the spectrum.

7. Go to File, Print to print the spectrum.

Sample Preparation

Liquids:

1. Swing sample press to the back.

2. Place O-ring centered on diamond sampling area

3. Place desired amount of liquid in O-ring.

4. For volatile liquids such as Acetone, cover sample with the glass cup

to inhibit evaporation. (For best results, place volatile liquids in

refrigerator for at least 3 Ominutes)

Solids:

1. Swing sample press to the back

2. Grind solid with mortar and pestle until a fine powder. (Be careful to

not inhale dust)

3. Place crushed sample over center ring making sure that it is covered

and verify by looking at the LCD to make sure sample is completely

covering the area.

4. Swing sample press over center position.

5. Obtain a stainless steel or polycarbonate pin, and fasten it in the swing

arm. (Tile stainless steel pin is recommended.)

6. Twist the large black knob on the sample press to apply pressure on

the sample. The":Load' gauge on the DuraScope will display green

lights. Continue twisting the knob until the first yellow light appears at

8. Stop. Do not twist the knob further.

Spectrum Collection

1. 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 to

scan. Specify a filename to save the spectrum.

Editing Spectrum

Add text or comments: Go to View, Add/Edit Text. Click and drag to move text.

Shutdown the computer.

Label Peaks: Go to View, Label Peaks. Click and drag to move a peak label. Go to

View, Clear All Peak Labels to clear labels. To change sensitivity in labeling

peaks, go to Setup, Options, Peak. Change Threshold values.

Print: Go to File, Print.

Cleaning and Shutdown Procedures

Clean the sample staging area with acetone and a kimwipe.

Switch the FTIR off.

Shut off nitrogen gas flow

Reference Spectra

webbook.nist.gov

Green binder labeled 'FTIR Spectra, Plastics' on shelf above FTIR