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Gen Chem Lab

Collection edited by: Mary McHale

Content authors: Mary McHale, Alvin Orbaek, and Andrew Barron

Online: < http://cnx.org/content/col10452/1.51>

This selection and arrangement of content as a collection is copyrighted by Mary McHale.

It is licensed under the Creative Commons Attribution License: http://creativecommons.org/licenses/by/2.0/

Collection structure revised: 2009/10/12

For copyright and attribution information for the modules contained in this collection, see the " Attributions" section at the end of the collection.

Gen Chem Lab

Table of Contents

Chapter 1. Avogadro and All That

1.1.

Chapter 2. Stoichiometry: Laws to Moles to Molarity

2.1.

Experiment 3: Stoichiometry: Laws to Moles to Molarity

Objective

Grading

Before Coming to Lab...

Introduction

Titration Calculations:

Example:

Procedure

Materials List

Part 1

Materials List

Part 2

Chapter 3. Totally, Terrific Table

3.1.

Lab 4: Totally, Terrific Table!

Objective

Grading

Background Information

Introduction

Procedure

I. Activity Series

Part 1: Reactions of Metals with Water

Part 2: Reactions of Metals with HCl

CAUTION: This part of the procedure must be done in a fume hood!!

Part 3: Reactions of Metals with Other Metal Ions

Note: It would be helpful to draw a diagram to remember where the drops

are on the sheet of metal before you begin.

ABDC

Part 4: Flame Tests

This station will be located inside a fume hood

Chapter 4. Going Green With Al

4.1.

Chapter 5. VSEPR: Molecular Shapes and Isomerism

5.1.

Grading

Chapter 6. Nanotechnology: Ferrofluids and Liquid Crystals

6.1.

Nanotechnology: Ferrofluids and Liquid Crystals

Objective

Grading

Background Information

Experimental Synthesis

Part I. Synthesis of Gold Nanoparticles (DEMO)

Nanoparticle Synthesis

Part II. Synthesis of the Aqueous Ferrofluid (Procedure modified from J.

Chem. Edu. 1999, 76, 943-948.)

Chemicals

Magnetite Synthesis

Ferrrofluid Properties

Part III. Synthesis of Cholesteryl Ester Liquid Crystals

Chemicals

Liquid Crystal Synthesis

Chapter 7. Solid State and Superconductors

7.1.

Solid State Structures and Superconductors

Objectives

Grading

Before coming to lab:

Introduction

Stoichiometry

Binding forces in a crystal

Close-packing

Packing of more than one type of ion (binary compounds) in a crystal

lattice

Coordination number and interstitial sites

Synthesis of solid state materials

X-ray crystallography

Superconductors

Solid State Model Kits

Use of the Solid State Model Kit:

Working groups and teams

Experimental Procedure

2. Cubic Cells

Team A

Group 2. Extended Structure

4. Interstitial sites and coordination number (CN)

Team A

5. Ionic Compounds

Team C

Fluorite: Calcium fluoride

Team D

Lithium Nitride

· Use the L template and insert 6 rods in the parallelogram portion of the

dotted lines.

· Construct the pattern shown below. Be sure to include a z=1 layer. 1 is a

green sphere while 1 and 2 are blue spheres. The 0 indicates a 4.0 mm

spacer tube; the 2 is an 18.6 mm spacer.

Teams E and F

Zinc Blende and Wurtzite: Zinc Sulfide

Pre-Lab: Solid State and Superconductors

(Total 10 Points)

Report: Solid State and Superconductors

A. Simple Cubic Unit Cells or Primitive Cubic Unit Cells (P)

B. Body-Centered Cubic (BCC) Structure

C. The Face Centered Cubic (FCC) Unit Cell

a. Fill out the following table for a FCC unit cell.

IV.Ionic Solids

Chapter 8. Colorful Copper

8.1.

Experiment 3: Colorful Copper

Objective

Grading

Before Coming to Lab…

Introduction

Experimental Procedure

Chapter 9. Metathesis: To Exchange or Not?

9.1.

Lab 4: Metathesis: To Exchange or Not

Objectives

Grading

Before Coming to Lab…

Introduction

Formation of a Gas

Formation of a Weak Electrolyte

Table 1 Solubility Rules

Table 2 Strong Electrolytes

Experimental Procedure

Part 1: Metathesis Reactions

Part 2: Solubility, Temperature and Crystallization

Pre-Lab 4: Metathesis – To Exchange or Not

Report 4: Metathesis – To Exchange or Not

Part 1: Metathesis Reactions

Part 2: Solubility, Temperature and Crystallization

First Batch of Crystals

Second Batch of Crystals

Third Batch of Crystals

Chapter 10. Electrochemistry/Alchemy: Molar Mass of Cu and Turning Cu into Au

10.1.

Electrochemistry/Alchemy:

Molar Mass of Cu and Turning Cu into Au

Objectives

Grading

Before Coming to Lab …

Introduction

Background Information

Experimental Procedure

Alchemy: Copper into Gold

Example of the calculation of Molar Mass:

Electrochemistry Pre-lab Exercise

Report Form: Electrochemistry

Questions:

Alchemy - Copper into gold

Chapter 11. Bonding 07

11.1.

Lab 5: Bonding 07

Objective

Grading

Background Information

Experimental Procedure

Part I. Predicting bond type through electronegativity differences.

Part II. Weak and strong electrolytes

Chemicals

Instructions for MicroLab Conductivity Experiment

Part III. Electrolyte strength and reaction rate

Chemicals

Part IV. Chemical reactions

Chemicals

Pre-Lab 5: Bonding 07

(Total 10 Points)

Part I. Bonding of chemicals in solution

Report 5: Bonding 07

Part I. Predicting bond type through electronegativity differences.

Part II. Weak and strong electrolytes

Part III. Electrolyte strength and reaction rate

Part IV. Chemical reactions

Chapter 12. Silver Nanoparticles: A Case Study in Cutting Edge Research

12.1.

Objective

Background

What is nanotechnology?

Why care about nanotechnology?

What are nanoparticles and how are they made?

Why silver nanoparticles?

TA Demonstration on the Hydrophobicity of Silver

Experimental Procedure no1 - ripening of silver nanoparticle

Experimental procedure no2 - lasers and colloids

Additional Information

Chapter 13. Thermochemistry

13.1.

Thermochemistry

Objective

Grading

Background Information

Calorimetry

Experimental Procedure

Materials Required

Setup of the MicroLab Thermistor

Part I. Reaction of Strong Acid with Strong Base

Part II. Enthalpy of Reaction

Calculations

Part III. Chemistry of Life

TA Procedure

Index

Chapter 1. Avogadro and All That

Experiment 2: Avogadro and All That

Objective

To help you become familiar with the layout of the laboratory including safety aids and the

equipment that you will be using this year.

To make an order-of-magnitude estimate of the size of a carbon atom and of the number of

atoms in a mole of carbon, based on simple assumptions about the spreading of a thin film of

stearic acid on a water surface

Grading

Lab Report (90%)

TA points (10%)

Before coming to Lab

Read the following:

Lab instructions

Background Information

Concepts of the experiment

Print out the lab instructions and report form.

Read and sign the equipment responsibility form and the safety rules. Email Ms. Duval, at

nduval@rice.edu, to confirm completing this requirement by noon on September 14 th.

Introduction

Since chemistry is an empirical (experimental) quantitative science, most of the experiments you will do involve measurement. Over the two semesters, you will measure many different types of

quantities – temperature, pH, absorbance, etc. – but the most common quantity you will measure

will be the amount of a substance. The amount may be measured by (1) weight or mass (grams), (2) volume (milliliters or liters), or (3) determining the number of moles. In this experiment we will review the methods of measuring mass and volume and the calculations whereby number of

moles are determined.

Experimental Procedure

1. Identification of Apparatus

On the tray (in DBH 214) we have a number of different pieces of common equipment. We will,

identify and sketch each - I know this may sound a trivial exercise but it is necessary so that we are all on the same page.

1. beaker

2. Erlenmeyer flask (conical flask)

3. side-arm Erlenmeyer flask

4. graduated (measuring) cylinder

5. pipettes, both types graduated and bulb

6. burette

7. Bunsen burner

8. test tubes

9. watch glass

10. volumetric flask

2. Balance Use

In these general chemistry laboratories, we only use electronic balances – saving you a lot of time.

However, it is important that you become adept at using them.

Three aspects of a balance are important:

1. The on/off switch. This is either on the front of the balance or on the back.

2. The "Zero" or "Tare" button. This resets the reading to zero.

3. CLEANLINESS. Before and after using a balance, ensure that the entire assembly is spotless.

Dirt on the weighing pan can cause erroneous measurements, and chemicals inside the

machine can damage it.

Balance Measurements:

1. Turn the balance on.

2. After the display reads zero, place a piece of weighing paper on the pan.

3. Read and record the mass. (2)

4. With a spatula, weigh approximately 0.2 g of a solid, common salt NaCl. The excess salt is

discarded, since returning it may contaminate the rest of the salt.

5. Record the mass (1). To determine how much solid you actually have, simply subtract the

mass of the weighing paper (2) from the mass of the weighing paper and solid (1). Record this

mass (3). You have just determined the mass of an "unknown amount of solid."

6. Now place another piece of weighing paper on the balance and press the Zero or Tare button

then weigh out approximately 0.2 g of the salt (4). Thus, the zero/tare button eliminates the

need for subtraction.

3. Measuring the volume of liquids

When working with liquids, we usually describe the quantity of the liquid in terms of volume,

with the usual units being milliliters (mL). We use three types of glassware to measure volume –

(1) burette, (2) bulb pipette, and (3) graduated cylinder. A volumetric flask will also allow for a high degree of accuracy and precision in the measurements of any liquids, so a 100 mL volumetric flask will contain precisely 100.0 mL of solution when filled to the line marked on the neck of the flask.

Examine each piece of equipment. Note that the sides of each are graduated for the graduated

cylinder and the burette. The bulb pipette delivers a specific volume, 10.00 mL. The burette

will be used to deliver a variable volume of solution and will also be precise to two decimal

places.

Put some water into the graduated cylinder. Bend down and examine the side of the water level.

Note that it has a "curved shape." This is due to the water clinging to the glass sides and is called the meniscus. When reading any liquid level, use the center of the meniscus as your

reference point.

Graduated cylinder

Look at the graduations on the side of the cylinder. Note that they go from 0 on the bottom and

increase upwards. Since volumes in graduated cylinders are only precise to one decimal place, a graduated cylinder is generally only used when a high degree of precision is not required.

1. Using your 10mL graduated cylinder, add water up to the 10 mL line as accurately as possible.

2. Dry a small beaker and weigh it (2).

3. Pour the 10 mL of water from the cylinder into the beaker. Reweigh (1).

3. Pour the 10 mL of water from the cylinder into the beaker. Reweigh (1).

4. Subtract the appropriate values to get the weight of the water (3).

Bulb Pipette

1. Half-fill a beaker with water.

2. Squeeze the pipette bulb and attach to the top of the pipette. Put the spout of the pipette under water and release the bulb. It should expand, drawing the water into the pipette. Do not let the water be drawn into the bulb.

3. When the bottom of the meniscus is above the line on the pipette, remove the pipette from the water.

4. Squeeze the bulb to run the extra water into a waste container until the bottom of the meniscus is level with the line on the pipette.

5. Add 10 mL of water to a pre-weighed dry beaker (5).

6. Weigh (4).

7. Subtract to get the weight of the water (6).

Burette

1. Examine the graduations. Note that 0 is at the top. Note that the stopcock is horizontal to close the burette and vertical to open it.

2. First, lower the burette so that the top is easy to reach and make sure the burette is closed.

Using a funnel, add about 10 mL of water.

3. Open the burette and run a little water into a waste container. Then turn the burette upside down and allow the rest of the water to run into the container.

4. You have just rinsed your burette. This should be done every time before using a burette – first rinse with water, then repeat the process using whatever liquid is needed in the experiment.

5. Fill the burette to any convenient level (half-way is fine). It is a good technique to add more liquid than you need, and allow some liquid to run into a waste container until you reach the

appropriate level so that you fill the space from the top to the tip of the burette.

6. Dry a beaker and weigh (8).

7. Add 10 mL of water to a pre-weighed dry beaker (7).

8. Subtract to get the weight of the water (9).

4. Estimation of Avogadro's number

Briefly, as a group with your TA, you will make an approximate (order of magnitude) estimate of

Avogadro's number by determining the amount of stearic acid that it takes to form a single layer (called a monolayer) on the surface of water. By making simple assumptions about the way the

stearic acid molecules pack together to form the monolayer, we can determine its thickness, and

from that thickness we can estimate the size of a carbon atom. Knowing the size of a carbon atom, we can compute its volume; and if we know the volume occupied by a mole of carbon (in the form

of a diamond), we can divide the volume of a mole of carbon by the volume of an atom of carbon

to get an estimate of Avogadro's number.

Procedure

Special Supplies: 14 cm watch glass; cm ruler; polyethylene transfer pipets; 1-mL syringes; pure distilled water free of surface active materials; disposable rubber gloves (for cleaning own watch glasses in 0.1 M NaOH in 50:50 methanol/water): 13 100 mm test tubes with rubber stoppers to

fit.

Chemicals: pure hexane, 0.108 g/L stearic acid (purified grade) solution in hexane. 0.1 M NaOH

in 50:50 methanol/water used for washing the watch glasses, dye.

SAFETY PRECAUTIONS: Hexane is flammable! There must be no open flames in the

laboratory while hexane is being used.

WASTE COLLECTION: At the end of the experiment, unused hexane solvent and stearic acid in hexane solution should be placed in a waste container, marked "Waste hexane/stearic acid solution in hexane."

Measurement of the volume of stearic acid solution required to cover the water surface

Your TA will do this as a group demonstration:

1. Fill the clean watch glass to brim with deionized water. One recommended way to do this is to set up your 25 mL burette on a ring stand.

2. Using a transfer pipette, obtain about 3-4 mL 0.108 g/L stearic acid solution in hexane in a clean, dry 13 100 mm test tube. Keep the tube corked when not in use.

3. Obtain more distilled water and fill the burette. Place your watch glass directly under the

burette (about 1 inch or less from the tip) and dispense the water until the entire watch glass is full. You may have to refill the burette 4 or 5 times to do this. With careful dispensing, the

surface tension of the water should allow you to fill the entire watch glass with relative ease.

4. Carefully measure the diameter of the water surface with a centimeter ruler. It should be close to 14 cm, + or - a couple of millimeters. Next, rinse and fill your 1 mL syringe with stearic

acid solution, taking care to eliminate bubbles in the solution inside the syringe.

5. Read and record the initial volume of the syringe (1 mL is always a good place to start.)

6. Then add the stearic acid solution drop by drop to the water surface. Initially, the solution will spread across the entire surface, and it will continue to do so until a complete monolayer of

stearic acid has been formed. If your first few drops do not spread and evaporate quickly,

either your water or watch glass is still dirty. As this point is approached, the spreading will become slower and slower, until finally a drop will not spread out but will instead sit on the

surface of the water (looking like a little contact lens). If this "lens" persists for at least 30 s, you can safely conclude that you have added 1 drop more than is required to form a complete

monolayer.

7. Now, read and record the final volume reading of the syringe.

When you have completed all of your measurements, rinse your syringe with pure hexane, and

dispose of all the hexane-containing solutions in the waste collection bottle provided.

Calculation of Avogadro's Number

The calculation p