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Piper Stevens
Unknown Sample #1
Purpose
Identify the presence of IA and IIA metal ions in a simulated water sample
from the Clark Fork of the Columbia River using emission spectroscopy.
Determine the concentration of copper and iron ions in the simulated water
sample using absorption spectroscopy, and report if those levels are too toxic
to support life. Use the collected data to determine a possible cause of the
major fish kill in 1984 in the Clark Fork of the Columbia River.
Introduction
land, the threat of water contamination has become a major concern in the
public eye. Runoff from fertilizers and highways tends to carry dangerous
animal life and ecosystems worldwide. When toxic metals reach reservoirs,
ponds, and rivers, they have a dramatic effect on the wildlife that inhabits
those water sources. A dangerous level of toxic metals in water has shown to
kill massive populations of wildlife in and around a natural water source. This
was the case in Clark Fork of the Columbia River where a major fish-kill
simulated water sample from the Clark Fork of the Columbia River. To do this,
This will allow a direct comparison of the emission spectrums of each IA and
IIA metals to the emission spectrum of the lake sample. This will ultimately
determine which metal ions are present in Clark Fork, and if the salinity of
the water was too high to support wildlife. The levels of copper and iron in
the water solution will also be tested with this experiment using data from an
the concentration of iron is above 0.3ppm, the water is considered toxic. The
toxicity of the water will help in determining the cause of the fish-kill. Using
concentration of copper and iron in the sample. The water sample is highly
concentrated in Cl- molecules, therefore the copper and iron ions are present
3+ + 2+
. Solutions ranging from 400ppm of
Fe [ CuSCN ] and [ FeSCN ]
to 50ppm
+ 2+
[ CuSCN ] and [ FeSCN ]
will be created and tested using the
metal ions are present in a simulated water sample from Clark Fork? As well
as, are the iron and copper concentrations in that sample at a toxic level?
This lab utilizes skills that I have obtained through doing both emission and
absorption labs in the past. In fact, I performed a lab that required me to test
the emission spectrums of various known IA and IIA salts. The skills I learned
testing emission spectrums in the infrared flares lab will help me test the
unknown water sample in this lab. Also, the emission spectrum data I
gathered on IA and IIA metals in that lab can be used in this lab so I will not
spectrum. In that lab, I learned how to use one standard solution to create
above will assist me in performing the complex lab presented to me with this
problem.
The possible outcomes of this lab vary hugely based on the simulated
and IIA metals in the water sample. However, I predict that there will be at
least two detectable metals that I will be able to find traces of in the sample.
Furthermore, the concentration of copper and iron in the sample could also
vary hugely. I imagine that, because there was a major fish-kill, the water has
some form of contamination and either has high levels of copper, iron, or
both. I do not have any solid idea of the results I will get from doing this lab;
water at Clark Fork of the Columbia River caused the fish-kill in 1984.
Experimental
Chemical Reagents:
Instead, I decided to use data that I had collected from a previous lab
SCN- solution.
-10 mL each of four diluted Fe/Cu solutions having copper
Equipment
P
-Transmittance =
P0
1
-Absorbance = log
Transmitance
-Moles to ppm:
- R2 = linear correlation
- absorbance concentration
Proved using Beer Lamberts law and the molar absorptivity coefficient
Setup
1. Label a watchglass and pour 1-2mL of the unknown solution into the
watchglass. Place a labeled nichrome wire into the watchglass with the
unknown solution.
2. Fill two cuvettes with the 0.1 M iron (III) sulfate solution and the 0.1 M
copper (II) sulfate solution. These will act as a control test to show the
shape of the absorption graph for each metal. Only perform the
3+
/20ppm solution.
F e
2+ 3+
4. Place 8 mL of the 400ppm /20ppm solution into the 10mL
Cu Fe
volumetric flask and fill the remainder of the volume with distilled
water until the meniscus of the solution lines up with the 10mL line on
2+ 3+
the volumetric flask. This will create the 320ppm 16ppm .
Cu F e
5. Turn the flask upside down a few times to combine the solution. Poor
the solution into a labeled test tube and wash the volumetric flask.
6. Repeat steps 4 and 5 with different amounts of standard Fe/Cu solution
standard Fe/Cu solution to add for each concentration are in the chart
below:
concentrations. Fill the cuvette full of solution, and then wipe each
glass sides.
8. Fill an additional cuvette with distilled water. This will serve as the
burner about 6inches away from the probe of the measuring cable.
enter the station number of the workstation the data will be sent to.
a Bunsen burner flame and adjust the position of the Bunsen burner
until the intensity reading is above 500. Press Intensity again and a
sample solution. Place the wire in the Bunsen burner flame- on the tip
workstation.
18. Return to the MeasureNet workstation and examine the emission
spectrum. Adjust the intensity if the data exceeds the original y values.
If this happens, press Setup, then F2 and enter new min and max
values for y. Press display and the MeasureNet will re-plot the data.
- This step is optional only if the data exceeds the original
parameters.
19. Press File Options, then press F3 to save the scan. Enter a 3-digit
onto the excel sheet and delete the data for Magnesium and
Cesium.
- Using a smoothed line scatter plot, convert all the data into a
graph.
- Determine the wavelength of the highest emission for each
sample including the unknown and record them in the data table
below.
- Compare the graphs of the known IA and IIA metals with the
unknown sample.
21. Turn on the workstation that the absorption Spectrophometer data will
Visible source power switch is ON. Press Station Number and enter
the station number of the workstation that the data will be sent to.
3+
solution and press sample. Make sure the absorption graph
Fe
spectrum. To save the data, press File Options then press F3 to save
the simulated river water sample for its absorption spectrum. Save
email. This includes all the Fe/Cu solution concentrations, the unknown
sample, the 0.1M iron nitrate solution, and the 0.1M copper nitrate
solutions (if there was time to test the last two solutions).
- Open the files in excel. Using the smooth line scatter plot option,
create individual graphs for the 0.1 M iron nitrate solution and the 0.1M
copper nitrate solution. Look at the overall shape of each graph to get
an idea of where each metal will peak for the solution containing both
metals.
- Create another smooth line scatter plot with the Fe/Cu solutions as well
identify the curve that represents the iron in the solution. Determine
for both iron and copper ( max . Then record the absorbance for each
unknown water sample and record the concentration in the Lab Report.
Results
Wavelength (nm)
0.8
400ppm
0.6
320ppm
240ppm
Absorption 0.4 160ppm
80ppm
Unknown #1
0.2
0
100 200 300 400 500 600 700 800 900 1000
-0.2
Wavelength
*Data series are labeled based on the concentration of copper in each
solution.
400ppm 0.776
320ppm 0.552
240ppm 0.312
160ppm 0.121
80ppm 0.002
Unknown #1 0.126
2 Trendline equation: y = 0.0025x -
R = 0.98592
0.2411
0.2
0.1 0.12
0 0
50 100 150 200 250 300 350 400 450
Concentration (ppm)
Absorption Spectrum: Iron
20ppm 0.667
16ppm 0.521
12ppm 0.286
8ppm 0.136
4ppm 0.018
Unknown #1 0.077
Trendline equation: y = 0.0421x -
R2 = 0.98738
0.1793
0.7
0.67
0.6 f(x) = 0.04x - 0.18
R = 0.99
0.5 0.52
0.4
Absorption
0.3 0.29
0.2
0.14
0.1
0 0.02
2 4 6 8 10 12 14 16 18 20 22
Concentration (ppm)
Calculations
Copper: Iron:
146.84ppm = x 6.09ppm = x
Final Solution
The metals present in the simulated water sample are sodium and
calcium. This can clearly be seen in the emission graphs of these metals
compared with the graph of the unknown sample. The wavelengths at which
each metal peaks line up with the two peaks of the unknown sample. The
2+ 3+
absorption tests on dilutions of a 400ppm /20ppm solutions.
Cu Fe
Then, a linear regressions was created for the copper and iron curves of the
Discussion
The results of this experiment are in many ways relevant to the major
fish-kill in the Clark Fork of the Columbia River. The results of the emission
test show that there were two metals present in the water. This suggests that
there was a high level of salinity in the water at Clark Fork, which could have
(146.8ppm) and the concentration of iron (6.09ppm) in the water are both
considered toxic by the EPA standards for drinking water. This experiment
has identified several toxicities in the water sample. This narrows the
reasons that the fish-kill took place in 1984 and may allow researchers and
In doing this lab, every measure was taken to ensure accuracy of the
experiment. To begin, there are many instances where mistakes could have
been made while analyzing the data. In particular, when determining which
curve on the absorption graph was caused by copper and which was caused
by iron. Furthermore, the dilutions were made from adding distilled water to
a solution with known concentration of copper and iron. There was a high
chance for error while creating these samples. In the future, standard
solutions of each concentration would allow for more precision. Lastly, the
water sample had IA and IIA metal ions bonded to chlorine, while, in the data
I used those metals were bonded to nitrates. This caused a slight shift in the
emission graph of the sample compared to the known metals. If time had
allowed, running new tests with each IA and IIA metal chlorate would have
provided more accurate data for analysis. If this experiment were continued,
more accuracy in the solutions and testing would produce data with higher
accuracy.
Conclusions
the sample solution in order to find the exact concentration. I used the
graphs from the 0.1M copper and 0.1M iron solutions to identify the max of
the Cu(II) and Fe(III) curves. Then I identified which curve on the absorption
graph was the copper absorption and which curve was the iron absorption.
After identifying the curves, I chose a wavelength for both the copper and
iron that had the most separation between each concentration. For copper
this was 335.68nm and for iron it was 458.53nm. Then, using the absorptions
trend line. I was then able to use the equation of the trend line to calculate
the exact concentration of copper and iron in the unknown sample. Both of
these concentrations are over the level of toxicity allowed in drinking water,
The emission spectrum of the unknown sample shows that there are
and then comparing the graph it created with the graphs of known IA and IIA
metals. The sample has peak intensities at two wavelengths which each line
up with one of the unknown metals. The peak at 588.69nm lines up with the
sodium peak and calcium peak, and the peak at 769.54nm lines up with
because the sample emission graph lines up with some of the smaller peaks
of the calcium graph. There is room for error in these results, however I am
Bibliography
regression on Excel.
- "Dangerous for the Environment Hazard Symbol." Dangerous For The
proposal.
- "Drinking Water Contaminants Standards and Regulations." EPA.
procedure proposal.