For Indirect Iodometric Analysis of Copper... ~0.0896g KIO3 necessary to consume 350mL of 0.1 M Na2S2O3, Na2S2O3 is stored in an amber glass bottle until ready for use. Primary Standard KIO3 has 2g of KI, 50mL of DI water, and 10 mL of 1.0M HCl is added then immediately titrated with Na2S2O3 until medium yellow or straw... then 5mL of starch indicator is added and titrated again until blue black color turns clear. Unknown CuO use 1.2G of Unknown, 20mL of HNO3 heated until sample dissolved, 25 mL of DI water added and boiled until clear light blue color, after cooling 1:1 NH3 added (~34.47 mL of NH4OH reagent) until permanent deep blue color amine complex, 2g of NH4HF2 added and swirled until dissolved, 3 g of KI is added then titrated immediately with Na2S2O3 until brown color of iodide is nearly gone (brown milk color), 2 g of KSCN and 3 mL of starch indicator is then added with titration continuing until disappearance of new blue black color. 1. Na2CO3 is often added to thiosulfate solutions - what purpose does this serve? 2. What is the purpose of adding the KSCN (or NaSCN) near the end of the unknown analysis? Be specific and give the reaction. 3. Why do you not need to accurately weigh out the KI used in standard and unknown analyses?

Fundamentals Of Analytical Chemistry
9th Edition
ISBN:9781285640686
Author:Skoog
Publisher:Skoog
Chapter27: Molecular Fluorescence Spectroscopy
Section: Chapter Questions
Problem 27.11QAP
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For Indirect Iodometric Analysis of Copper...

~0.0896g KIO3 necessary to consume 350mL of 0.1 M Na2S2O3, Na2S2O3 is stored in an amber glass bottle until ready for use.

Primary Standard KIO3 has 2g of KI, 50mL of DI water, and 10 mL of 1.0M HCl is added then immediately titrated with Na2S2O3 until medium yellow or straw... then 5mL of starch indicator is added and titrated again until blue black color turns clear.

Unknown CuO use 1.2G of Unknown, 20mL of HNO3 heated until sample dissolved, 25 mL of DI water added and boiled until clear light blue color, after cooling 1:1 NH3 added (~34.47 mL of NH4OH reagent) until permanent deep blue color amine complex, 2g of NH4HF2 added and swirled until dissolved, 3 g of KI is added then titrated immediately with Na2S2O3 until brown color of iodide is nearly gone (brown milk color), 2 g of KSCN and 3 mL of starch indicator is then added with titration continuing until disappearance of new blue black color.

1. Na2CO3 is often added to thiosulfate solutions - what purpose does this serve?

2. What is the purpose of adding the KSCN (or NaSCN) near the end of the unknown analysis? Be specific and give the reaction.

3. Why do you not need to accurately weigh out the KI used in standard and unknown analyses?

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