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Name: Christina Frost ID Number: 1029538

Section: AA Lab Partner:

Experiment 1: Calibration Curves and an Application of Beer's Law


By signing below, you certify that you have not falsified data, that you have not plagiarized any part of this lab report, and that all calculations and responses other than the reporting of raw data are your own independent work. Failure to sign this declaration will cost you 5 points. Signature:

Note: All sections of this report must be typed

Total Points = 60 pts (5 pts notebook, 55 pts template)

Purpose and Method


Clearly state the purpose of this part of the lab. Explain how this is accomplished in this experiment. What calculations do you need to perform? What measurements will be made? [Do not provide experimental details here]. How do you go from calculated/measured values to accomplishing stated purpose? (10 pts: roughly divided 1 for the goal and 3 each for addressing each of the three parts of the experiment.) The purpose of this lab was to determine experimentally the amount of iron that is present in an iron tablet. To do this, a calibration curve first needed to be generated. This was accomplished by taking ferroin stock solution and diluting it down to established concentrations. Five cuvettes were then filled with these samples and sprectroscopy was used to determine the absorbancy of each sample at the point lambda max, or the peak (optimum) wavelength for analyzing ferroin. This point was established by running the cuvette with the highest concentration of ferroin first and recording all data at the point of lambda max for this solution. Concentration and absorbance were graphed from the resulting data and a curve was generated. The resulting linear regression line allowed for a mathematical relationship between absorbancy and concentration to be determined.
To calculate how much iron is present in a tablet, 20 g of the powdered tablet was measured, filtered, reduced to an iron(II) state, neutralized, and diluted. With this solution, spectroscopy was again used to determine an absorbancy. With the calibration curve generated earlier, the absorbancy could be used to find the concentration of this sample. Then this concentration was converted from mol/L to mol/mL. This allowed the concentration to be multiplied by the amount of solution, 100 mL, so that the number of iron moles in the solution could be found. This value was then multiplied by 20 as this experiment began with 100 mL of iron solution and only 5 mL had been used to produce the current sample. This means moles of iron were left behind and need to be accounted for. Once this calculation was complete, the gram formula mass of iron was used to convert the moles of sample to mass of sample. Upon converting this value to mg, a set of ratios could be established to related the determined amount of mass of iron in the 20 mg sample to the amount of iron in a single tablet. Cross multiplication and division made it possible to calculate the amount of iron in one tablet.

DATA, GRAPHS AND CALCULATIONS lmax: 513.5 nm 1 pt

Creating the calibration curve: Ferroin: Concentration (M) Absorbance 1.25E-05 0.100 2.50E-05 0.200 3.75E-05 0.320 5.00E-05 0.440 6.25E-05 0.450

2 pts

Place your calibration plot here. Make your plot big enough to cover this instruction box so that it is large Concentration of Ferroin vs. Absorbance enought for someone else to read. This calibration plot is Abs vs. concentration of ferroin (M) (y vs. x)
0.500 Use the online resources if you need help figuring out how plot a in Excel. y to = 7520x + graph 0.02 0.400 Title the graph and label the X and Y axis, including the correct units (Absorbance data is unitless). Be sure to double check your units and formatting once you print the report. Absorbance 0.300
Series1 Linear (Series1)

0.600

4 pts

Add a Trendline to show the linear fit of your data. Choose a linear line and choose the options that will 0.200 "display the equation on the chart".
0.100 0.000 0.00E+00

1.00E-05

2.00E-05

3.00E-05

4.00E-05

5.00E-05

6.00E-05

7.00E-05

Concentration of Ferroin (M)

Slope of Absorbance versus concentration graph -1 7520 M y-intercept of Absorbance versus concentration graph 0.02 Detailed calibration equation: y = 7520x + .02 Determining theAmount of Iron in an Iron Tablet 1) 2) 3) Average mass of a tablet Mass of crushed tablet used in analysis Final volume after filtered crushed tablet solution is diluted in volumetric flask (lab manual Part II, Step 5) Volume of diluted crushed tablet solution transferred to the new volumetric flask Final volume of ferroin complex solution (end of lab manual Part II, Step 9) Absorbance of the ferroin complex solution (lab manual Part III, Step 3) 436 19 100

1 pt 1 pt 2pts

mg mg mL 1 pt

(provided in manual)

4)

mL

5)

100

mL

6)

0.130

1 pt

7)

Using the calibration equation and the absorbance you measured for the prepared sample, calculate the ferroin concentration. Show your work and don't forget to include units. .13 = 7520x + .02 x = 1.46E-5 M

3 pts

8)

Based on the procedural steps and the ferroin concentration you just calculated, calculate the moles of ferroin in the final ferroin complex solution prepared in Part II, Step 9. Show your work. 1.46E-5 M / 1000 mL/L x 100 mL = 1.46E-6 mol
2 pts

9)

Based on the moles of ferroin in the final ferroin complex solution, calculate the moles of iron in the crushed tablet solution prepared in Part II, Steps 2-5. Show your work. 1.46E-6 mol x (100/5) = 2.92E-5 mol
3 pts

10)

Using the "moles of iron in the crushed tablet solution" you just calculated, calculate the mass (in mg) of iron in the crushed sample that you weighed out. Show your work. 2.92E-5 mol x 55.85 g/mol x 1000 mg/g = 1.63 mg
2 pts

11)

From the mass of iron in the crushed tablet sample you weighed out, calculate the mass (in mg) of iron in a whole tablet. Show your work. 1.63 mg = x 20 mg 436 mg x = 35.5 mg
3 pts

12)

mg of iron per tablet as listed on the bottle

27

mg

Results and Discussion


1. Compare your mass of iron per tablet with the amount listed on the bottle label. Calculate the % error and discuss YOUR major sources of error. ( 3 pts) 35.5 mg - 27 mg x 100 = 31.6% 27 mg
- not filtering the solution sufficiently - misreading the meniscus causing innacuracy in the degree of dilution - failing to rinse the cuvettes with solution prior to capping them - leaving fingerprints on the faces of the cuvettes

2. If you did not wait for the complete formation of the ferroin complex in Part II, step 10, how would your data look different and how would this affect your determination of the mass of iron in the tablet? ( 5 pts) If the feroin complex had not fully formed, the absorbancy would have been affected and the resultant mass of iron found in the tablet would have been too little. 3. You use atomic emission spectroscopy, another spectroscopic technique, to measure the Li+ concentration in 5 standard solutions of varying concentrations of LiCl. The intensities for the standard solutions are plotted versus the concentrations and the resulting calibration equation is: Intensity = 84,250 M-1 * [Li+] + 1.75
If the intensity of your unknown sample is 90, what is the concentration of Li+ in the analyzed sample? (5 pts)

90 = 84,250 M-1 * [Li+] + 1.75

[Li+] = 1.05E-3 M

If 2 mL of the original unknown sample was diluted to 150 mL prior to analysis, what is the concentration of Li+ in the original solution? (5 pts) .001 M x .001 L/mL x 2 mL / 150 mL = 1.33E-8 M

Laboratory Waste Evaluation (1 pt) Laboratory waste is considered anything generated during an experiment that is disposed of down the sewer drain, thrown in the garbage, collected in a container for disposal by the UW Environmental Health & Safety department, or released into the environment. Based on the written lab procedure and your actions during the lab, list the identity and approximate amount (mass or volume) of waste that you generated while performing this experiment.

- 2 mL 1 M HCl - .019 g iron - 2 mL hydroxylamine hydrochloride .23 M - 1 mL 1 M Na acetate sol. - 3 mL 3.6E-3 phenanthroline - around 250 mL water - about 400 mg of miscellaneous contents of iron tablet - wrappers from new lab equiptment - a few tissues

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