Specific details about the installation and operating parameters are described in the manual as well as elsewhere on this web site. Specific menu options are also described. The following are general comments plus a step-by-step procedure for acquiring spectra, printing, and saving data.
A computer is required to operate the instrument with Nu Spec software. The computer has Microsoft office, Adobe Acrobat, Labworks, and a spectra viewer from Grams. Excel can be used to import Raman data. The attached printer may not be as useful unless the data is imported into ACD software. Grams or Delta Nu software do not allow printing wave numbers or intensity of peaks.
The instrument is a black box with a shiny chrome plated ball in the front, shown at the right. Do not turn (play) with the shiny knob it is used to fine focus the laser inside the sample tube. Directly behind the shiny know is a round hole used to insert the sample in a standard vial. The o-ring holding the sample vial may hold the sample very tightly, in a new instrument. Use a firm downward pressure to insert the sample vial.
The top of the instrument has a vent to prevent the instrument from overheating. Do not cover the top of the instrument with books or papers. The instrument uses a laser and all users must wear safety glasses when working with the instrument and never look directly at the bright light.
Samples may be liquid or powders and even flat surfaces when the instrument is coupled with an X, Y, Z-stage solid sample holder. Liquid and powdered samples are placed into a glass vial with an ID number on the top. The ID number is cross-referenced to the name or type of sample in the user's notebook. Each vial is 8 mm X 40 mm with a plastic cap. The single vertical hole behind the shiny knob is used to insert the vial with the sample for analysis. Do not disconnect the the front screws when the instrument is turn on.
Software to process data is by Delta Nu (Nu Spec), National Instruments Lab (LabView), and Thermal Galactic (Grams). None of these software packages allow the correct printing of the axes or the labeling of peak height or intensity. The user must EXIT Nu Spec to save data with LabView. Once the data is saved it can be printed with through the Grams Spectra Viewer. Data saved as a ASCII.txt file can be imported into Excel. It can also be imported into Advanced Chemical Development UV/VIS program which does produce the proper axes labels and allows peaks to be labeled and integrated for area.
Working Procedure and Suggestions
1. Complete the instrument logbook showing the date, user's name (printed no initials) with responsible professor, application, and note of any problems.
2. Everyone working with or around the instrument must wear safety glasses to avoid eye damage from the laser. Never look directly at the laser.
3. Turn on the computer with the the front switch and the instrument with the switch on the upper right rear.
4. Click on the DeltaNu icon in the center of the screen. As soon as the NuSpectra data acquisition program is initialized a red indicator in the upper right hand corner will be visible. The indicator remains red until the system reached the proper operating temperature. After 4-5 minutes the indicator will turn blue.
5. Select a standard which has the same physical properties as the samples, if the sample is a liquid use polymethylmethacrylate if it is a solid use benzoic acid or if is a surface use polystyrene. In labeled blocks near the instrument.
6. For liquid or powder sample place them into a sample vial and insert the standard into the vertical hole in the center of the instrument. Set the integration time to 1 second. Press the Reference button. A green indicator in the upper left hand corner of the acquisition screen shows that a spectrum is being acquired.
7. To focus the laser beam repeat step 6.
8. Once the spectrum has been acquired it is saved and can be processed with ADC software if it also saved as a *.TXT file
Caution: The glass sample containers for sample with plastic lids should not be labeled but each vial stored in a small labeled beaker. A reference number can be placed on the bottom of the vial if the beaker or notebook of the user as an index of the type of sample or standard. The vial have a diameter of 8.2 mm and are 39.9 mm long. They are available from Delta Nu; at $25 for 250 vials. The same product is also available from VWR under part number 66015-702 for about the same price. Adaptors are now available to run samples in either standard NMR or melting point tubes.
