STEP BY STEP AAS INSTRUCTIONS - Iron (Fe)

1. Turn on AAS, computer, and printer.

2. Double click on inst.exe icon.
3. The Lab Benchtop window will open - do not proceed until the 5100
icon underneath the AAS icon is highlighted.
4. While you're waiting for the icon to light up, open your acetylene tank
and air line. Acetylene pressure should be at 14 psi (this is marked on the
gauge in black) and air pressure should be about 45-50 psi (neither air
pressure nor acetylene pressure should vary much between sessions, but
it's important to always check it, especially after changing tanks). The
gauge that reads pressure in the tank is the gauge on the right. The gauge
on the left reads how much fuel is in the tank. NOTE: when first
opened, the acetylene tank, will usually read above 15 psi (red zone).
Don't adjust the pressure right away, because 93% of the time, after
about 10 minutes, it will have sunk to 14.1 psi always check the pressure
after you light the flame. NOTE: the acetylene tank should be
replaced when the fuel level drops below 75 psi (using the scale on
the inside of the circle on the left hand gauge). Since contaminants
sink to the bottom of the tank, it is not advisable to drain a tank to
absolute empty .
5. Under "Windows" at the top of the page, scroll down and open
the Element Parameter file. This file is your method file; you can't run
an element unless you have defined a method.
6. The Element Parameter file will ask you whether you want a
previously defined file, or a new one (so it is possible to use the same
method for different sample runs). In the Element Parameter file, you
have three pages to fill out - M ain, Calib, and Options.
7. Main - specify the element (standard wavelength and slit width will
automatically appear), select an appropriate sampling time (default is 5
sec), make sure the flame sensor is on, and confirm that the fuel is
acetylene and the oxidant is air. "Time average" and "AA" remain as is.
8. Calib (Calibration) - enter the concentration of your standards and how
you want to refer to them (i.e. Sl, or standard 1, or whatever). The most
important thing to do is to make sure that if, for example, you have a 10
ppm standard, the standa rd units are set at mg/L. To change standard
and sample units you just double click on the line. It is possible to have
standard units and sample units different. You decide the number of
significant digits (up to the machine's precision level of course) by
entering "5.0" as a standard, or "5.00", etc. Last, click on Nonlinear to
 change the type of standard curve that will be drawn; absorbance vs.
concentration for Fe is only linear up to about 10 mg/L.
9. Options - highlight the printing options you prefer and type in any
comments about your samples. This page prints out at the beginning of
your run automatically.
10. Save your Element Parameter file. The computer will always use
the Element Parameter file most recently opened when you begin
running samples. Close your newly named file.
11. You should be back at the Lab Benchtop. Now you will open four files
that you will need to manually run your samples. Under Windows, scroll
down and select "Flame Control", "Manual Control", "Display
Calibration", and "D isplay Data".
12.OK, but before you begin running samples, you need to adjust the lamp,
and then optimize the burner head position, the fuel, and the nebulizer.
13.NOTE: For fe, you must use the longer burner head with the BLACK
PIN. When running samples that use acetylene and air, you use the
longer burner head with the black pin, but for any elements that require
the hotter N20 flame, you use the shorter burne r head with the red pin. I
know from experience that the AAS will not light if you mix up the
burner heads!
14. Adjust the lamp by first opening "Adjust Lamp" under Windows (see,
there really is logic to all this; before you know it you won't need this
sheet!). If you have created your Element Parameter file (as you should
have by now) the AAS has already selected the Fe lamp. Your lamp
current should read 25 or 30, and your lamp energy should be in the 60's
or 70's [in the past lamp energy has fluctuated, and Perkin Elmer
maintains that even at a low lamp energy precise sample measurements
are possible, but if lamp energy drops dramatically it is probably a sign
something is wrong - call Perkin Elmer!]. Now, open the lid covering the
lamps, and maximize the absorbance bar by 1) moving the whole lamp
forward and backward and 2) turning the two knobs you will see near the
15.back end of the lamp, which adjust the lamp's position.
16. Optimize the vertical position of the burner head by first lowering the
burner head with the large right hand knob next to the nebulizer. Then
open "Continuous Graphics" under Windows and Autozero by
clicking on "Autozero" under < B>Continuous. Raise the burner head
until you get a reading, that is, when your .000 goes up, to .004, then .
018, etc. Lower the burner head until you have .000 again, then lower it
one quarter of a turn more.
17. Now it's time to light the AAS. Don't close your Continuous Graphics
window, just click on the Flame Control window. After opening your
 air and acetylene lines (air comes through a line from a compressor next
door, acetylene is in a tank) click on the flame icon to light the
flame. By the way, the exhaust system should be turned ON now!!
18.Adjust the fuel and oxidant levels by using the Fuel Up/Down and
Oxidant Up/Down keys on the keyboard (towards the right on the top
line of F keys). For iron, I have found that a fuel of 2 and an oxidant of 8
- 10 works well. Basically, you wa nt a lean flame (meaning the blue line
on the burner head at the bottom of the flame is about 1/8" high). You
don't want a rich flame, which is the result of a high fuel level.
19. To adjust the burner head horizontally and diagonally, go back to
the Continuous Graphics window. While aspirating a standard (you'll
probably want to make more of the standard you choose to aspirate,
since a lot of liquid can be used up in thi s step) turn the large shiny left
hand knob (horizontal) in both directions until you reach maximum
absorbance. Repeat this process with the inside-the-compartment-to-the-
right-of-the-burner-head shiny knob (diagonal). Some people like to
readjust the ver tical knob at this point, to fine tune it. I don't, but try it
yourself and see what you prefer.
20. The nebulizer is also adjusted using the Continuous Graphics window.
Loosen the lock on the nebulzier by turning the "locking ring"
counterclockwise. This will allow you to adjust the sample flow rate by
twisting the "knob ring"; the knob ring being the ring which the
nebulizer tube directly connects into (the locking ring is immediately
behind the knob ring, touching the knob ring in fact when it is
completely tightened). When the nebulizer tube is no longer locked (i.e.
the locking ring has b een loosened) you can adjust the rate at which the
tube sucks samples by twisting the knob ring. Now, put the nebulizer
tube in a standard, and turn the circular knob ring until bubbles
come OUT of the tube in your standard; then turn the circular knob ring
in the other direction until you reach a maximum absorbance on
your Continuous Graphics window.
21. NOTE: it is my experience that the nebulizer sucking rate does not
change much at all in between running samples. When you have a good
rate, I recommend not messing with it unless you're having
problems. NOTE: it is also my experience that sucki ng rate doesn't
effect absorbance that much, so I usually fill a volumetric flask up to
the very top and visually watch the rate at which the level of solution
drops. Once you have adjusted the nebulizer using absorbance a few
times, you will get a fe el as to what is a good rate for the solution to
drop in the neck of the volumetric flask. NOTE. Remember to always
"relock" the locking ring after making an adjustment!!
22. Now you can close the Continuous Graphics window. Then, click on
the Manual Sampling window, where you will want to double click on
the line above the "save data on/off" icon, to name the file where your
sample data will b e stored. If you do not name a file and thereby cause
the "save data on/off" icon to be highlighted, your data will not be
saved!!!
23. Now you're ready to begin running your standards/samples. You will
always begin a sample run by running a standard curve. Simply put the
nebulizer tube in your first standard (your "zero" standard") and scroll
down under Calibration to autozero . When the READ icon stops being
highlighted, that means the AAS is finished reading that standard, so you
will remove the tube, wipe it with a ChemWipe, put it in your second
standard, and scroll down to your next standard . Repeat this process
until all your standards have been analyzed. NOTE: some people think
the neb tube should always be placed in distilled water in between
samples, to flush the tube. I have tried it with and without the de-
ionized water and found that if you let the nebulizer tub e sit in your
standard for one second before its analyzed, then you don't need to
do the distilled water wash every time. I tell the AAS to delay
analyzing the standard/sample after I hit READ by typing in 1.0
second Delay in the Elem ent Parameter file, Main section.
Experiment yourself!
24. You have to use the mouse to analyze standards (and the nebulizer tube
must be in the standard before you click on autozero, Sl, S2, etc.) but to
analyze samples you can either use the mouse to click on the
large READ icon on the Manual Cont rol screen or the keyboard (in
the middle, top row). After your first standard curve is run, rinse with de-
ionized water and then put the nebulizer tube in your first sample,
hit READ (mouse or keyboard), and then keep the tube in the sample un
til the READ icon is no longer lit up. Rinse with de-ionized water, then
put the tube in your next sample, hit READ, wait, etc. I recommend
running a standard curve after every 10 to 15 samples. In between every
sample, I always wipe the neb ulizer tube with a ChemWipe.
25. The Display Data window will show you the concentration of your most
recent sample/standard. The Manual Control window will keep track of
the total number of samples/standards you've run. To view your most
recent standard curve, click on the Display Calibration window. To edit
a standard curve, click on Edit Calibration.
26. When you've finished running all your samples/standards, you turn off
the flame (using keyboard or Flame Control window), close the
 acetylene/air lines, and bleed the gases remaining in the lines (click on
bleed gases in Flame Control window).
27. To save your data file in, for example, ASCII, so that you can transfer
the information into a spreadsheet, go to the Data Benchtop. Then scroll
down toReformat Data. A window will open that will allow you to call
up your data fi le (double click on the data line), and then choose various
options for what you want saved in your ASCII file. The options are too
numerous to list here; most are pretty straightforward, but for a detailed
listing consult the manual. Once you've made your choices, simply click
on Execute Reformat.
28. To view your ASCII file, exit the software. At the C prompt, type x.
Scroll up using the arrow keys until you find Data - AAS. Hit return
twice and you will see a listing of all the Data files. Then follow the
commands at t he bottom of the page: hit V to view the document, C to
copy it onto a disk, etc.

Link to the experiment

Last update: February 18, 1998.