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   -Before using any instruments,    make sure the lab instructor (TA    or professor) has instructed you    on its use.   DO NOT use any of    the instrument unless you are    supervised by a lab instructor,    graduate instrument assistant,    or by a professor.   All of these    instruments are very expensive,    and printing out and reading    the directions alone is not    enough information to be able    to properly use any of the    instruments.

Atomic Absorption Spectroscopy

Perkin-Elmer AAnalyst 100

Operating Instructions for Perkin-Elmer AAnalyst 100:
Flame Atomic Absorption Photometry

1. Turn on atomic absorption unit (switch is on right hand side of instrument).

2. Turn on HGA 850 Graphite Furnace (the switch is on the left hand side of      instrument).

3. Turn on acetylene tank by twisting the main valve ½ to one full turn (left      regulator should read around 15).

4. Turn on computer.
     -When the window Enter Network Password appears - click on Cancel .
     -Double click on AA WinLab Analyst icon.
     -Checking Connections window will appear then close if all is OK.
     -When the window AA WinLab appears check that the Technique
     is Flame .
     -Click on button displaying green Erlenmeyer flask (Use basic system      procedure for performing analyses with manual sampling).
     -When the window Open Method appears:
     Fill in Method name ("Ca in water" for example).
     -Click on New Elem. (right side of window).
     -When the window Create New Method appears, click on down arrow 6      and scroll through to find element that is going to be analyzed then click on      it. The element should appear in the box next to the heading Element to be      determined. Click on OK . The window Manual Analysis will appear.

A. To align the lamp:
     1. Check to see that the proper hollow cathode lamp is installed (right side          of instrument under black door). If the wrong lamp is installed, carefully          remove lamp and place it back into its box, then carefully place the          correct lamp into the instrument. (Make certain that the lamp is properly          seated into its holder.)

     2. Click on the button in the AA WinLab window labeled Lamps.

     3. When the window Align Lamps appears check that Elements box and          the Lamp Type boxes contain the correct information then click on the          gray button under Set Up.

     4. Close window Align Lamps.

B. To turn on the flame:
     1. Make sure that the aspirating tube is in distilled water.

     2. Click on the button in the AA WinLab window labeled Flame .

     3. When the window Flame Control appears make sure the Safety          Interlock box is green with a check.

     4. Click the switch that appears in the Flame Control window form Off to          On.

     5. Adjust the flame manually using fuel and oxidant valves on the front of          theinstrument (the gauges should read about 3 for fuel and 8 for          oxidant).

C. To adjust and optimize burner:
     1. Prepare a blank solution (usually distilled water) and a sample          containing an ion to be analyzed (for Ca tap water is fine).

     2. Click on Tools a menu will appear, select and click on Continuous          Graphics.

     3. Aspirate blank when signal is steady click on Auto-zero.

     4. Aspirate the sample containing the analyte.

     5. Then use the three adjusting knobs on the burner to maximize the          signal, be sure that when you adjust the height of the burner that you          don't block the optical path with the burner. To determine if the path is          blocked, check to see if the signal goes back to zero when you place          the aspirating tube into distilled water.

D. To create a standard curve:
     1. Prepare standards of know concentration.

     2. Click on the button in the AA WinLab window labeled MethEd.

     3. Type in Method Desc. (Calcium in tap water) Check that the other          instrument settings are OK.

     4. Click on the tab (lower left corner) Calib.. Also, make sure you are on          the Equation, Units & Replicates tab/sheet. Enter the appropriate          information:
             Calibration Equation
             Equation ………… Zero Intercept: Linear
             Max. Decimal Places: 3 Max. Significant Figures: 4
             Units
             Calibration ………. choose appropriate units
             Sample……………. choose appropriate units
             Replicates
             Number Fixed 3

     5. Click on the tab Standard Concentrations (upper right side). Enter           information for each of your standards - standard ID and concentration.           Note: Do NOT enter zero as a standard concentration. The blank is           designed to be used in the place of the zero concentration standard.
          Go to Manual Analysis - Aspirate distilled water or appropriate blank           and click on Analyze Blank Click on Results icon

     6. To analyze standards, use the pull-down menu to choose the correct          standard and click on Analyze Standard.
         -Click on calibration button to show calibration curve - After each          standard is run, rinse sample capillary with distilled water.
         -Go to Sample Editor
         Enter data about samples
         -Go to Manual Analysis
         -Click on analyze sample

     7. Print sample information
         -Select the windows you would like to print - like your calibration curve          and then choose print - graphics

E. Shutting down the instrument:
     1. When analysis is complete
         -Click on flame icon and shut off flame
         -Go to file - exit - OK to lose method

     2. Shut off computer
         -Next, turn of the instrument using the switch
         -Finally, turn off the Acetylene tank

Operating Instructions for Perkin-Elmer AAnalyst 100:
Graphite Furnace (HGA 850) Usage

Getting Started:

1. Turn on atomic absorption unit (switch is on right hand side of          instrument).

2. Turn on HGA 850 Graphite Furnace (the switch is on the left hand side     of instrument).

3. Verify that the fume vent is operational and turned on.

4. Turn on argon gas (and special gas) to the specified pressures (see     pressure guides Table 1 and Table 2).

5. Turn on the cooling system by pressing the power switch at the rear     panel of the device. The cooling system is the device that looks like a     CPU, located below the lab bench.
        -Normally, it should be full to the maximum amount of coolant. The          coolant is a special mix of a 1:10 solution of glycerol to water (1 part          glycerol and 9 parts water).

6. Turn on the computer.
     -When the window Enter Network Password appears, click on Cancel .
     -Double click on the AA WinLab Analyst icon.
     -The Checking Connections window will appear, and then close it if       everything is OK. 
          - In the File menu, click on Technique. In the Select Technique dialog,             click on Furnace and then on OK.
          -When the window Open Method appears:
          -Fill in Method name ("Ca in water" for example).
          -Click on New Elem. (right side of window).
          -When the window Create New Method appears, click on down arrow             6 and scroll through to find element that is going to be analyzed then             click on it. The element should appear in the box next to the heading             Element to be determined. Click on OK.
           -The window Manual Analysis will appear.

7. To align the lamp:
     1) Check to see that the proper hollow cathode lamp is installed (right           side of instrument under black door). If the wrong lamp is installed,           carefully remove lamp and place it back into its box, then carefully           place the correct lamp into the instrument. (Make certain that the           lamp is properly seated into its holder.)

     2) Click on the button in the AA WinLab window labeled Lamps .

     3) When the window Align Lamps appears check that Elements box           and the Lamp Type boxes contain the correct information then click           on the gray button under Set Up.

     4) Close window Align Lamps.

8. Optimize the position of the furnace:
     1) Make sure that the lamp for the element of study is already installed and          aligned properly.

     2) Switch off the deuterium lamp of the background corrector if it is on.

     3) Move the furnace out of the atomizer compartment.

     4) Verify that the graphite tube intended for use is installed in the furnace,          after removing the window assemblies.

     5) Autozero the spectrometer:
         - In the Tools menu, click on Continuous Graphics.
         - Click on Autozero.

     6) Move the furnace back into the atomizer compartment. The absorbance          reading should be less than 0.002. If it isn't, then align the furnace          according to the steps below:
            - Move the locking lever to the left in order release lateral (left to right)
              movement of the furnace.
            - Rotate the vertical (up and down) and horizontal (forward and               backward) alignment controls alternately and in very small               increments to find the position giving minimum (less than 0.002)               absorbance reading on the display.
            - Holding the furnace assembly at the base, carefully move the furnace               laterally to the left and to the right to find the position that gives               minimum absorbance reading (less than 0.002) on the display.
            - Repeat the horizontal, vertical, and lateral adjustments until you have               achieved the minimum (less than 0.002) absorbance reading.

     7) After aligning the furnace:
         - In the Tools menu, click on Continuous Graphics.
         - Click on Autozero.

9. Reset the window assemblies. The absorbance, after replacing the     windows, should be between 0.06 to 0.09 measured at the Cu line at     324.8 nm (for example).

10. Conditioning the graphite furnace:
     1) Make sure that the graphite tube is properly installed and already          aligned.

     2) Click on Furnace on the Toolbar to open the Furnace Control Window.

     3) Within the Furnace Control window, click on Condition Tube. The          system uses a special furnace program for heating the tube to          successively higher temperatures.