Reagent Step in ProcedureObservations Data collected Mass: 3.0437 Pinacol Measured on balance Sulfuric acid added Heat Distillation (start) Distillation (finish) Volume: 5.0 750 EPM 150°C 750 RPM 250°C Pinacolone Purification Mass:\.4644 IR NMR 2,4-DNP Test Solid yellow color

Reagent Step in ProcedureObservations Data collected Mass: 3.0437 Pinacol Measured on balance Sulfuric acid added Heat Distillation (start) Distillation (finish) Volume: 5.0 750 EPM 150°C 750 RPM 250°C Pinacolone Purification Mass:\.4644 IR NMR 2,4-DNP Test Solid yellow color

Principles of Instrumental Analysis

7th Edition

ISBN:9781305577213

Author:Douglas A. Skoog, F. James Holler, Stanley R. Crouch

Publisher:Douglas A. Skoog, F. James Holler, Stanley R. Crouch

Chapter33: Automated Methods Of Analysis

Section: Chapter Questions

Problem 33.4QAP

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Question

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Can you answer all parts to this question

Theoretical yield of pinacolone in grams and moles
- show your calculations
Final yield of pinacolone (grams and % yield)
- show your calculations

Reagent Step in Procedure Observations Data collected
Mass: 3.0437
Pinacol
Measured on balance
Sulfuric acid added| Heat
Volume: 5.0
750 EpM
Distillation (start)| iš0°c
150°C
Pinacolone
Distillation (finish)| 250°c
750 RPM
Purification
Mass:\.4644
IR
NMR
2,4-DNP Test
Solid yellow color

Part 1: Formation of pinacolone
Add 3.0 g of pinacol and 30 mL of deionized water to a 100 mL round-bottom flask.
Add a stir bar and clamp the flask to a ring stand, with the flask hovering 2-3 in above the
hot plate. Turn on the stirring function on the plate until the mixture is evenly moving.
Then slowly, carefully, add 5.0 mL of concentrated sulfuric acid. This is an exothermic
reaction. Allow the mixture to stir for 10 minutes.

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