One method for the analysis of Fe3+, which is used with a variety of sample matrices, is to form the highly colored Fe3+–thioglycolic acid complex. The complex absorbs strongly at 535 nm. Standardizing the method is accomplished using external standards. A 10.00-ppm Fe3+ working standard is prepared by transferring a 10-mL aliquot of a 100.0 ppm stock solution of Fe3+ to a 100-mL volumetric flask and diluting to volume. Calibration standards of 1.00, 2.00, 3.00, 4.00, and 5.00 ppm are prepared by transferring appropriate amounts of the 10.0 ppm working solution into separate 50-mL volumetric flasks, each of which contains 5 mL of thioglycolic acid, 2 mL of 20% w/v ammonium citrate, and 5 mL of 0.22 M NH3. After diluting to volume and mixing, the absorbances of the external standards are measured against an appropriate blank. Samples are prepared for analysis by taking a portion known to contain approximately 0.1 g of Fe3+, dissolving it in a minimum amount of HNO3, and diluting to volume in a 1-L volumetric flask. A 1.00-mL aliquot of this solution is transferred to a 50-mL volumetric flask, along with 5 mL of thioglycolic acid, 2 mL of 20% w/v ammonium citrate, and 5 mL of 0.22 M NH3 and diluted to volume. The absorbance of this solution is used to determine the concentration of Fe3+ in the sample. What is an appropriate blank for this procedure? Ammonium citrate is added to prevent the precipitation of Al3+. What is the effect on the reported concentration of iron in the sample if there is a trace impurity of Fe3+ in the ammonium citrate? Why does the procedure specify that the sample contain approximately 0.1 g of Fe3+? Unbeknownst to the analyst, the 100-mL volumetric flask used to prepare the 10.00 ppm working standard of Fe3+ has a volume that is significantly smaller than 100.0 mL. What effect will this have on the reported concentration of iron in the sample?

8th Edition

ISBN:9781305079113

Author:David W. Oxtoby, H. Pat Gillis, Laurie J. Butler

Publisher:David W. Oxtoby, H. Pat Gillis, Laurie J. Butler

Chapter8: Bonding In Transition Metal Compounds And Coordination Complexes

Section: Chapter Questions

Problem 36P

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One method for the analysis of Fe³⁺, which is used with a variety of sample matrices, is to form the highly colored Fe³⁺–thioglycolic acid complex. The complex absorbs strongly at 535 nm. Standardizing the method is accomplished using external standards. A 10.00-ppm Fe³⁺ working standard is prepared by transferring a 10-mL aliquot of a 100.0 ppm stock solution of Fe³⁺ to a 100-mL volumetric flask and diluting to volume. Calibration standards of 1.00, 2.00, 3.00, 4.00, and 5.00 ppm are prepared by transferring appropriate amounts of the 10.0 ppm working solution into separate 50-mL volumetric flasks, each of which contains 5 mL of thioglycolic acid, 2 mL of 20% w/v ammonium citrate, and 5 mL of 0.22 M NH₃. After diluting to volume and mixing, the absorbances of the external standards are measured against an appropriate blank. Samples are prepared for analysis by taking a portion known to contain approximately 0.1 g of Fe³⁺, dissolving it in a minimum amount of HNO₃, and diluting to volume in a 1-L volumetric flask. A 1.00-mL aliquot of this solution is transferred to a 50-mL volumetric flask, along with 5 mL of thioglycolic acid, 2 mL of 20% w/v ammonium citrate, and 5 mL of 0.22 M NH₃ and diluted to volume. The absorbance of this solution is used to determine the concentration of Fe³⁺ in the sample.

What is an appropriate blank for this procedure?
Ammonium citrate is added to prevent the precipitation of Al³⁺. What is the effect on the reported concentration of iron in the sample if there is a trace impurity of Fe³⁺ in the ammonium citrate?
Why does the procedure specify that the sample contain approximately 0.1 g of Fe³⁺?
Unbeknownst to the analyst, the 100-mL volumetric flask used to prepare the 10.00 ppm working standard of Fe³⁺ has a volume that is significantly smaller than 100.0 mL. What effect will this have on the reported concentration of iron in the sample?

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