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New Mexico State University
College of Arts and Sciences
Department of Chemistry and Biochemistry
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 Procedure for the Analysis of Metals with Perkin-Elmer 3030B

 

1. Use the instrument log book to record name, date, and application. Install the appropriate HCL and connect it to the socket at the back of the lamp compartment. Insert the Model 3030B System disk in either disk drive. Use caution when handling floppy disks. Never touch the magnetic surface and protect it from strong magnetic fields and dust. The disk drive system is not compatible with DOS, Windows, or Apple systems. The general instruction for this instrument are basic for the understanding of AAS protocol.

2. Turn power switch ON. The 3030 logo appears, the system initializes and the Element Select Mode page appears in under a minute. A listing of instrument controls and keys is given as well as the Wavelength and Burner Control Panels.

3. Enter the atomic number of the element to be determined and press ENTER. The recommended conditions appears.

4. Turn on the exhaust hood directly above the burner. Select safe and proper setup conditions.

Background for AAS Gases

5. Examine the methods displayed and select the appropriate one by pressing the soft key for the desired method. The programing screen appears next.

6. Press 2 followed by ADVANCE to advance to the LAMP CURRENT entry. Enter the recommended lamp current value for the lamp installed and press ENTER.

7. Press 12 followed by ADVANCE to advance to S1 (Standard 1) entry. Enter the concentration of the first standard e. g. 10 mg/L and press ENTER.

8. Press SETUP to enter the setup mode for lamp alignment and wavelength adjustments are performed.

9. Select the required slit width.

10. Peak the wavelength selected by first adjusting the coarse (inner) wavelength control and then the fine (outer) wavelength control to obtain maximum energy.

11. Press GAIN to bring the energy bar graph to a mid-range value.

12. Adjust the lamp orientation using the two black-adjustment screws on the lamp to achieve maximum energy. If necessary press GAIN to maintain a mid-range value on the ENERGY bar graph.

13. Press CONT to enter the Continuous mode where burner alignment, nebulizer, and flame gas flow adjustments are performed.

14. Install the flow spoiler or glass bead and the appropriate burner head.

15. Lower the burner assembly using the burner vertical adjustment knob and press AUTO ZERO.

16. Raise the burner head until the main display starts to indicate slight absorbance, then lower the burner head slightly. Details of the adjustment without a flame are given elsewhere.

17. General pressures and flow rates for the oxidant and fuel are given elsewhere.

18. Light the flame by pressing the FLAME ON or (digital readout gas control) or IGNITE (interlocked gas control).  NOTE: Clean burner head when flame fluctuates orange. Use deionized water to soak the burner head and its parts overnight.

19. Aspirate a standard that gives approximately 0.2 absorbance units and adjust the horizontal and rotational adjustments knobs on the burner assembly until a maximum absorbance is obtained.

20. Press RUN to enter the Run Mode.

21. Aspirate a blank and press AUTOZERO.

22. Aspirate the first standard and press STD 1, when the display changes from WAIT to READ, calibration is established.

23. Proceed to determine the concentration of the samples. Aspirate the sample and press READ. The concentration of the sample appears on the main display. Aspirate DI water between each standard and sample. Record results.

24. Turn the flame off, turn the main gas valves to the acetylene and air off, reduce the current to the HCL, turn off the exhaust hood, and turn off the instrument power. Report any problems observed during the analysis in the instrument log book.


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