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IA - Lab Report. Aim to prepare a sample of p-nitro acetanilide from the given acetanilide.

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Introduction

CHEMISTRY (HL) EXPERIMENT NO. : Date: To prepare a sample of p-nitro acetanilide from the given acetanilide. EXPERIMENTAL DESIGN Aspect 1 RESEARCH QUESTION: How to prepare a sample of p-nitro from the given acetanilide? SELECTING VARIABLES > Manipulated variables The amount of acetanilide Volume of Methylated spirit > Responding variables Reaction of the acetanilide with the nitrating mixture > Controlled variables Pressure and temperature of the solutions Mass of acetanilide - 5g Volume of glacial acetic acid - 5cm3 Volume of concentrated sulfuric acid - 10cm3 Volume of fuming nitric acid - 10cm3 Volume of Methylated spirit - 20cm3 HYPOTHESIS Since it is difficult to carry out the nitration of aniline with the nitrating mixture as the amino group gets oxidized which is not required, we first protect the amino group to form acetanilide which is then nitrated to give p-nitroacetanilide which is then re-crystallized with ethanol so that the soluble ortho-compound can be removed and the pure p-nitroacetanilide can be obtained. EXPERIMENTAL DESIGN Aspect 2 CONTROLL OF VARIABLES > The entire experiment should be carried out at a standard room temperature. ...read more.

Middle

o Place this conical flask into a freezing mixture of water and ice cubes. Stir the contents with a glass rod and keep checking the thermometer for when it reaches 5oC. o Once cooled, slowly add the contents to a conical flask and keep stirring. Make sure that the temperature doesn't rises above 25oC. o After letting the flask be in the ice bowl, take it out leave it for 30 minutes. o With the help of a funnel and a filter paper, scrape out the crude product and then thoroughly wash it with cold water to remove the acid. o Dissolve the crude product into about 20 cm3 Methylated spirit in another 100 cm3 conical flask and warm the mixture with the help of a burner. o Filter the solution while still hot and then put the filtrate in ice. o O-Nitroacetanilide comes out as the filtrate and p-nitroacetanilide is obtained as colorless crystals on the filter paper. o Wash the obtained solid on the filter paper with cold water, dry it and then weigh it. ...read more.

Conclusion

CONCLUSION AND EVALUATION Aspect 2 EVALUATING PROCEDURES Percentage errors (%) = uncertainty * 100 True value * Amount of acetanilide taken 0.005 * 100 = 0.1% (Weighing machine) 5 * Volume of glacial acetic acid = 0.05 * 100 = 1.0% (Measuring flask) 5 * Volume of HNO3 to test tube = 0.05 * 100 = 1.0% (Measuring flask) 5 * Volume of H2SO4 added to test tube = 0.05 * 100 = 2.5% (Measuring flask) 2 * Volume of H2SO4 added to conical flask = 0.05 * 100 = 0.625% (Measuring flask) 5 * Volume of Methylated spirit = 0.05 * 100 = 0.25% (Measuring flask) 20 * Mass of the watch glass used = 0.005 * 100 = 0.024 % (Weighing machine) 21.05 * Total mass of the watch glass and the product = 0.005 * 100 = 0.020% (Measuring flask) 25.025 Total uncertainty = 7.019 CONCLUSION AND EVALUATION Aspect 3 IMPROVING THE INVESTIGATION o Equipment with the least chance of causing uncertainties should be used o The experiment should be performed very meticulously, with the help of a fume cupboard and at the same room temperature and pressure. ?? ?? ?? ?? ...read more.

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