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Chem3472lab Aa F2014
Chem3472lab Aa F2014
To obtain determine the concentration of one or more common metal ions in commercial
vitamin tablets by developing an analytical method based on atomic absorption
spectrophotometry.
Apparatus:
Instructions:
Chemicals:
Vitamin sample: Each tablet contains 2 mg manganese (as manganese sulfate), 162 mg of
calcium (as calcium phosphate and calcium carbonate), 20 g of selenium (as sodium
selenate), 75 g molybdenum (as sodium molybdate), 150 g boron (as sodium borate)
Procedure:
1. You will need to construct a calibration curve for Mn. Then develop dilutions of the
solution prepared from the tablet which allow you to work in the linear range of the
calibration curve
2. Calibration curve
1
Manganese
Pipet 5 mL of the manganese standard into a 50 mL flask and dilute to the mark.
Pipet 0, 1, 5, 10, and 20 mL of this Mn stock (100 g/mL) into 50 mL volumetric
flasks. Add 25 mL 8 M HCl to each and dilute with deionized water to the mark.
Aspirate each of the calibration standards and record the absorbances. Rezero the
instrument with the blank and repeat your readings at least 5 times.
3. Unknown
Carefully weight a tablet and place it in a 250 mL Erlenmyer flask with 25 mL 8 M
HCl. Boil slowly on a hot plate for 5 min. Cool and add 10 mL deionized water.
Filter through a Whatman No. 1 filter paper. Transfer the filtrate to a 100 mL
volumetric flask and dilute to the mark with deionized water. This is the vitamin
stock solution.
Before aspiration of the samples, filter through a 0.2 m syringe filter. Aspirate the
sample and read the absorbance. Rezero with distilled water and remeasure. Each
student should have at least 5 independent measurements. [Remember more
independent measurements reduce the error in the mean as an estimate of the
concentration.
Be sure to neutralize all your solutions and dispose of them properly. The TA;s will
guide you in this.
Data Analysis
1. Construct a calibration curve. Be sure to include y error bars. Note any non-
linearities. Try to work in the linear portion of the curve. Fit the linear portion of the
curve using linear regression.
2. Determine (1) the amount [report it as mg (or g, as appropriate) per gram of crude
sample] and (2) the 95% confidence interval.
Lab Report
In addition to the data analysis and results, you will need to address the following:
1. Does a 1000 ppm standard have to be exactly 1000 ppm?
2. Must one always work in the linear portion of a calibration curve?
2
Brief Operating Procedure for
Varian SpectrAA-5 Flame Atomic Absorption Spectrophotometer
2. Turn on Mn lamp
Press Lamp 1 mA
Press3
Press Abs
3. Ignite Flame
3
5. Set Zero
6. Measurements