Brittany Hicks
ICP & AA Lab- Dr. Foy
Spring 2013
ICP and AA
Introduction
Inductively coupled plasma is primarily used to analyze samples by the use of an argon plasma.
The analysis is particularly looking for certain metals within the sample. The torch within the ICP consists
of three tubes made of quartz. This chemical instrument measures the electron emission as the
electrons return to their ground state. Samples usually analyzed by the ICP are metals, but non-metals
analytes can also be analyzed.
Atomic absorption is used mainly for the detection and determination of a single element within
a desired sample. The analysis is completed by radiation or light specifically looking at the free atom
characteristic of the element. Both liquid and solid samples can be analyzed by AA with the overall goal
od determining the concentration of a particular element within the sample.
The purpose of these two experiments were to learn how to operate both of the instruments
and familiarize ourselves with the techniques of analysis. Both known and unknown samples will be
tested. Unknown samples will be determined, and most likely will be taken from York College’s campus.
The overall goal is to look at the amounts of Zinc and Copper within the samples.
Procedure – ICP
1) Turning on the ICP
a. The cooling unit should be on for ten minutes; this is left of the ICP and is a box. To turn
it on the switch is on the back of the cooling unit run for 15 minutes.
i. Make sure the unit has cooling liquid in it.
b. Flip the levers on the bottom right of the ICP and make sure that the tubes attached to
them do not twist. Otherwise the flow will be changed.
c. Turn on the argon gas for around 5-10 minutes. This is accomplished by turning the dial
on the argon tank in the gas cylinder room. The dial is on top of the tank and is to be
turned counter clockwise. Also turn the valve so that it is perpendicular to the tubing
(located behind tank). On the left of the instrument table there is a valve labeled argon
gas turn that so it is also parallel with the tubing.
d. Finally turn on the ICP. You should have a blank in the probe so that the bulb does not
burn out. This should be done at all times you’re not running a sample.
2) Software startup
a. Turn on the computer and click on ICP expert.
b. Click on the button that resembles a lock with electricity in the middle of the top page,
this will turn on the plasma. If you can’t find it there are pictures of the icon in the ICP
log book in the drawer. This should be heated for 15 minutes.
3) Method
a. On the main index window select worksheet.
b. On the load dialog worksheet box select new. You will then have a choice for either
quantitative or time resolved scan, this experiment uses quantitative. Save the
worksheet
c. Open the method editor; this is done by clicking on the box with the hand that seems to
be writing on paper. This should open the elements page.
d. To select the elements you will be looking for (zinc and copper) hold control and click on
the elements. They will then be highlighted blue
e. Click on the standards tab and edit the number of calibration standards. In the
experiment 5 are being used. Select the units of measurement you will be using. Keep
the correlation coefficient the same. Save and exit from file menu
4) Analysis
a. Once the flame has been on for 10 -15 minutes click on the sequence tab under the
worksheet window and make sure the source is set to manual.
b. Click the icon that looks like a wand and a magic hat; this is the sequence editor icon.
Enter the number of samples in the sample field count, on the samples and calibration
page. Click on begin with calibrations and select include a blank, then click confirm.
c. On the sequence page, select the sequence parameters icon, and choose stop for the
calibration failure option. Click okay to exit and yes to confirm selections.
d. Click the analysis tab and confirm all samples are selected, if not click the tube cell in top
left corner.
e. Click on play icon and follow instructions. If an error message pops up that says
“maximum error exceeded”, just click okay and run your samples
f. After your data is collected place a blank into probe.
g. On data chart, click on the diagonal line to get calibration graph. Print if you want and
print the data.
5) Turning off ICP
a. To turn off the plasmid press the lock with the electricity button or the F4 key
b. Turn off computer program
c. Turn off argon gas at bench top and in the gas cylinder room. Turn clockwise and valve
on wall and bench top should perpendicular.
d. Turn off ICP
e. After 15 minutes turn off coolant and take out blank.
Procedure –AA
1. Turning of the AA
a. Make sure the exhaust fan is turned on (it should always be on)
b.
c.
d.
e.
f.
2.
3.
4.
5.
Then turn on the AA cooling system, which is to left of the AA
Then turn on the AA, the power button is on the front left of the machine
Then go to the gas room and turn on the air and the acetylene
Open the gas valves for air and the acetylene on the left of the AA
Make sure the lamps for the specific elements you are looking for are installed
(zinc and copper were already)
Open the WinLab 32 software on the desktop of the computer
a. System check will appear for the flame, spectrometer, and the auto sampler
b. Then click the Lamps button at the top left of the screen. A window will open and
turn on the element you are searching for clicking on the on/off button and then
highlight the row of the element. When the light is green, the lamp is turned on.
Wait ten minutes for the lamp to warm up fully and when it is finished close the
window.
Create a Method
a. Click the “Wrkspc” button in the menu bar at the top. When a window pops up,
click the “AUTO.flm” or “MAN.flm”. Four new windows will then appear on the
screen.
b. Then click the “File” menu button and click “New” and the “Method”. Then select
the element you are going to be running for this experiment and click the checkbox
for “Recommended Values”.
c. A “Method Editor Window” will then appear. Click the “Spectrometer” tab, and
make sure the appropriate element is chosen. Do not change any of the other
settings.
d. Click the “Calibration” tab. Click the “Equations and Units” tab on the side of the
window. Select the equation of the line you want to use for your experiment (We
used linear through zero). Enter the concentrations (ppm) for your samples and
standards. Click the “Standard Concentrations” tab on the side of the window.
Enter the names of your standards and samples and the concentrations of your
standards in the appropriate places (Do not fill in the A/S column; it will be filled
in by the computer with your results). Close the window
Turning on the flame
a. Check to make sure the flame is safe to light by looking at the “Safety Interlocks”
box. Green check means it is safe and a red x means it is not safe and will not light.
b. Once it is safe to light, click the ignite flame button and the top middle of the
screen. (If it does not light, try again and if it continues to not work, check the
gases being used)
Run Standards and Samples
a. Look at the “Manual Analysis Control” screen
b. Place the tube in your blank (distilled water) and click “Analyze Blank”. (When
the green light goes out the sample is done being analyzed)
c. After the blank then run your standards the same way but in the Standard part of
the “Manual Analysis Control” screen
d. After the standards then your samples the same way but in the Sample part of the
“Manual Analysis Control” screen
6. AA Shut-down
a. Flush the probe with deionized water
b. Turn off the flame
c. Turn off the lamp
d. Close the air and acetylene valves at the bench next to the AA
e. Turn off the air and the acetylene in the gas storage room
f. Bleed the gases by clicking on the “Bleed Gases” button in the “Flame Control
Panel”
g. Close the software entirely
h. Turn off the AA
i. Turn off the AA cooling system
Data and Analysis
ICP and AA Measurements
1000𝑝𝑝𝑚𝑉 = 5𝑝𝑝𝑚(100𝑚𝑙) 𝑉 = .5𝑚𝑙
1000𝑝𝑝𝑚𝑉 = 10𝑝𝑝𝑚(100𝑚𝐿) 𝑉 = 1𝑚𝐿
1000𝑝𝑝𝑚𝑉 = 20𝑝𝑝𝑚(100𝑚𝐿) 𝑉 = 2𝑚𝐿
1000𝑝𝑝𝑚𝑉 = 30𝑝𝑝𝑚(100𝑚𝐿) 𝑉 = 3𝑚𝐿
1000𝑝𝑝𝑚𝑉 = 40𝑝𝑝𝑚(100𝑚𝐿) 𝑉 = 4𝑚𝐿
1000𝑝𝑝𝑚𝑉 = 50𝑝𝑝𝑚(100𝑚𝐿) 𝑉 = 5𝑚𝐿
AA Results
All water analysis results are located in my lab notebook for zinc, copper, and water samples
collected from around Campbell Hall located on York College’s campus.
The three unknown samples collected from the college include:
1. Tap water from within the instrumental lab
2. Water from the women’s bathroom sink
3. Water from the water fountain outside the men’s bathroom
Water results from the unknown samples were relatively low through comparisons of the
known concentrations for both zinc and copper. Zinc concentrations for the known samples
were higher in concentrations than known sample concentrations of copper. However, copper
concentrations of the unknown samples were higher than those recorded of the zinc
measurements. Copper concentrations were similar among the water fountain and girl’s
bathroom water and zinc concentrations showed the same similarity. Both zinc and copper
concentrations were significantly lower than the lowest standard concentration (1ppm).
ICP Results
Due to independent study experiments being conducted within the lab, I learned how to use this
particular instrument from my lab assistant Chris. He was running water samples looking for the
presence of lead within the water. Concentrations and intensities of the water samples were obtained
and are posted within my lab notebook. As the concentration increased, the intensities of the samples
increased as well showing a direct correlation between the two.
Conclusion
Both of these instruments were pretty easy to use and had similar procedures and result
techniques for analysis. Having Chris show me how to use the ICP made it easier to understand due to
having a hands on learning experience. Both instruments gave me good results and allowed for an easy
analysis of concentrations and correlations. There were trace amounts of copper and zinc within the
unknown water samples. The water taken from the lab actually contained the lowest amounts of zinc
and copper. For all three unknown samples, the concentrations were lower than the smallest
concentration standard sample at 1ppm. This suggests that lower standard samples of concentrations
should have been made to show a better correlation. The relationships between intensity and
concentration for data recorded on the ICP showed as positive relationship. As concentrations
increased, intensity values increased.