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Experiment 23 Determination of the iron content with Spectrophotometry

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1 Experiment 23 Determination of the iron content with Spectrophotometry
Purposes 1. Learn to operate 722 Spectrophotometer. 2. Master to determine the iron content by use of sulfosalicylic acid method.

2 Principles In this experiment, we use Fe3+ ions to react with sulfosalicylic acid and produce brown [Fe (Ssal) 2]- ions under a condition of HAc-NaAc buffer solution (pH=5). Determine the absorbance with λ=460nm. The Lambert-Beer law provides the mathematical correlation between absorbance and concentration. It is usually stated as

3 The relationship between A and c serves as the basis for the quantitative analysis of a great many substances.

4 Standard Curve A0 A1 A2 A3 A4 A5 ········· ··········· · cx · · · Ax ·
λ=460nm c0 c1 c2 c3 c4 c5 A0 A1 A2 A3 A4 A5 The graph should be a straight line

5 Prepare standard solutions and a sample solution
Procedure Prepare standard solutions and a sample solution Prepare a series of standard solutions of different accurately known concentration. Get 6 volumetric flasks (10mL) and use the measuring pipets to transfer solutions into the volumetric flasks (according to the table). Prepare a sample solution of unknown concentration.

6 Preparation of Fe3+ standard solutions and a sample solution
solution/mL unknown 0.2mol/LHNO3 /mL sulfosalicylic acid solution /mL Buffer (pH=4.7)/mL Add distilled water to mark /mL Final c(Fe3+) cx Absorbances (A)

7 2. Determine of absorbances (A)
According to the usage of 722-type spectrophotometer, use λ=460nm and use blank solution (1#) as reference solution to determine absorbance of each standard solution and a sample solution. Record the results.

8 3. Draw a calibration curve
Draw a working curve. The abscissa is the concentration of Fe3+ of standard solutions, the ordinate is the absorbance of the standard solution.

9 4. Determine the [Fe3+] of sample solution
According to the determined absorbance of the sample solution, We can look up the concentration of Fe3+ in sample from the working curve drew by yourself. Calculate the concentration of Fe3+ in original undiluted sample. [Fe3+] (original undiluted sample) =[Fe3+] (diluted sample) ×10


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