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Procedure
for the Analysis of Metals with Perkin-Elmer 3030B
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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.