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Identifying Unknown Metals using Specific Heats

Ian Barber Stuart Coles Elisa Monteiro

Macomb Mathematics Science Technology Center

Honors Chemistry

Section 10B

Mrs. Christine Kincaid-Dewey/Mrs. Jamie Hilliard/Mr. Mark Supal

24th May 2016


Table of Contents

Introduction ...................................................................................................................... 1

Review of Literature......................................................................................................... 3

Problem Statement .......................................................................................................... 8

Experimental Design ..................................................................................................... 10

Data and Observations .................................................................................................. 12

Data Analysis and Interpretation.................................................................................... 20

Conclusion ..................................................................................................................... 28

Application ..................................................................................................................... 31

Acknowledgements ....................................................................................................... 33

Appendix A: Constructing the Calorimeters ................................................................... 34

Appendix B: Randomization with Excel ......................................................................... 35

Appendix C: LabQuest Setup ........................................................................................ 36

Appendix D: Formulas and Sample Calcuations ........................................................... 37

Works Cited ................................................................................................................... 40


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Introduction

Molybdenum is a rare but essential element. Too much of it can kill an

animal, but too little of it and digestion will not function properly. Due to its rarity,

it is expensive in its pure form. Its precious and dangerous nature makes

identifying a molybdenum sample very important.

This paper describes an experiment that used the property of specific heat

to determine whether a sample of metal is molybdenum. Specific heat is

measured using calorimeters, which are relatively simple devices that are used to

create isolated systems. Since every element on the periodic table has a unique

specific heat, it is a very convenient and easily tested method of determining the

identity of a sample.

To carry out this experiment, first calorimeters were built to create an

isolated system, allowing changes in heat to be accurately measured. Metal rods

were heated in boiling water until they reached equilibrium with the water and

then placed inside calorimeters. The temperature change within the calorimeters

was then used to calculate the specific heat of the metal samples.

Specific heat is a property that makes it easier for industries to know how

to most effectively use an element. For example, waters relatively high specific

heat makes it very good for insulators or air-conditioning fluid in automobiles.

Similarly, molybdenums middling specific heat means it is a good conductor of

heat and can be used for applications which require heat transfer. It is for this

reason, along with its strength-adding properties, that molybdenum is often used

in the formation of alloys that will later be used for applications such as airplane
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engine components and parts within nuclear power facilities. (Uses of New

Molybdenum)
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Review of Literature

Specific heat is the amount of heat per unit of mass required to raise the

temperature of an element by one degree Celsius or one Kelvin (Nave, Specific

Heat). Specific heat is an intensive property of an element meaning each

element has a unique specific heat. This allows specific heat to be used to

identify an element. This experiment will use J/G * C, or joules over grams times

degrees Celsius.

Specific heat is measured as a unit of energy over a unit of mass

multiplied by a temperature scale. This experiment will use J/g * C, or joules

over grams times degrees Celsius, as the unit for specific heat. This will be

measured by using calorimetry, which uses calorimeters to create isolated

systems. (Calorimeter and Calorimetry.) These isolated systems are used to

measure the change in temperature during interactions, which can be done

because they do not allow for heat or matter to the system. The First Law of

Thermodynamics states that energy cannot be created nor destroyed, only

transferred. (Lucas) This means that any observed change of energy within an

isolated system must come from within the system itself and be transferred to the

surroundings. Calorimeters are isolated, and thus it can be said with certainty

that any perceived changes in the temperature of the calorimeter are actually just

redistributions of energy within the system, meaning that energy must have

transferred from one place within the system to another.

When describing heat transfer, the variable q is generally used to

represent heat. If the value of q is positive, it is an exothermic reaction, meaning


Barber-Coles-Monteiro 4

that heat is released during the reaction. If q is negative, it represents heat being

absorbed in the reaction. This is called an endothermic reaction, in that the water

lost heat energy to the sample.

Figure 1. Calorimeter Example

Figure 1, above, shows an example to a calorimeter. This calorimeter is

slightly different than the one used in this experiment in that it is a different

shape, but the general concept of a sample placed in water within an insulated

box is identical.

= +

( ) = ( )

Shown above is the equation used to determine the specific heat of the

metal. As stated previously, the variable q represents the heat in the system. The

variable s represents specific heat in J/g * C and m represents the mass of the

sample in grams. The temperature in the calorimeter after the sample has been

allowed to reach equilibrium ( ) will be the same on both sides, as the system

has reached equilibrium. The initial temperature ( ) will also be measured. All

temperature measurements will be in degrees Celsius. When performing the

calculations, these variables will apply to the water in the calorimeter on one side
Barber-Coles-Monteiro 5

of the equation, and the sample within the calorimeter on the other. This is

clarified by the subscripts.

There are multiple possible methods to determine the specific heat of an

item. One way to do this is, using calorimetry, is to heat up a sample in boiling

water, and then transition it to water of a different temperature within a

calorimeter. The initial temperature of the water in the calorimeter is recorded,

and after the metal has been in the calorimeter for some amount of time the final

temperature of the water is recorded. (Jaskew, ChemLab #17 - Specific Heat of

a Metal) While this experiment aims to take an approach similar to the one

described in ChemLab #17, there are other variations on how this experiment

can be done. For example, a different experimental setup, as used by Barth,

uses little metal beads and starts with chilled water as opposed to room

temperature water, recording the temperature increase with the metal at room

temperature (Barth, Improved Method for Determining the Heat Capacity of

Metals). This allows for easier setup and easier transfer of heat due to the

increased surface area of the beads as opposed to a smaller metal. The Barth

experiment also used more precise measuring strategies that are adopted in the

experiment discussed here, as well as a method of transferring a sample from

one body of water to another more efficiently than that described in Chemlab

#17.

Another method for determining specific heat is called the laser flash

method. In this method, a sample of a material is placed inside of a furnace. A

powerful laser is flashed at the sample. This sample then absorbs the radiation
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from the laser, thereby increasing the temperature of the sample. An infrared

light detector placed behind a focusing lens at the back of the furnace then

detects this change in temperature of the sample (Parker). This change in

temperature, along with the mass of the sample, can used to calculate the

specific heat of a substance. This value can be compared to that of a previously

identified sample tested under the same conditions, allowing for identification of

elements (Thermal Diffusivity, Specific Heat, and Thermal Conductivity of

Aluminum Oxide and Pyroceram 9606). As in this experiment, the specific heat

of the material in the experiment is determined based on other factors, and these

values must be compared to a known sample to get a useful metric. Neither

Chemlab 17 nor the Barth experiment use comparative methods for determining

the identities of a sample. The comparison methodology used in this experiment

is based off of the methods put forth in Thermal Diffusivity.

Table 1
Properties of Molybdenum and Water
Specific Heat Density
(J/g * C) (g/cm3)
Molybdenum 0.25 10.2
Water 4.18 1.00

Table 1, above, shows the specific heats of molybdenum and water.

Molybdenum, the known material for this experiment, has a specific heat of 0.25

J/g * C, meaning that it would take 0.25 joules of energy to raise the

temperature of one gram of molybdenum by one degree Celsius. The density of

molybdenum is 10.2 g/cm3 (Nave, Molybdenum). Water has a specific heat of

4.184 J/g * C, which is abnormally high (Kuo and Brewster), and a density of 1

g/cm3 (General Water Information). This means that molybdenum heats faster
Barber-Coles-Monteiro 7

than water, making water the better insulator. It also means that molybdenum is

great for any uses that require transfer of heat.

All of the methods outlined in this section, and all information put forward,

should clarify the experiment presented. This experiment combines multiple

previous experiments by other researchers into one experiment, serving the

purpose of identifying an element indirectly through the property of specific heat.


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Problem Statement

Problem Statement:

To determine whether an unidentified sample is molybdenum, using the

intensive property of specific heat.

Hypothesis:

The unidentified metal is molybdenum, determined using specific heat

values to an alpha value of 0.1 and a percent error of 7%.

Data Measured:

This experiment will measure the temperature of each body of water, and

the temperature of the known and unknown sample before and after it is

submerged in the cooler body of water. All temperatures are measured in

degrees Celsius. The masses of the metal samples will be measured in grams.

To analyze the data, the specific heat of the unknown metal will be compared to

the specific heat of molybdenum in a two-sample t test, with the specific heat

measured in J/g * C.

There are various variables needed to calculate specific heat. The variable

s represents specific heat in J/g * C and m represents the mass of the sample in

grams. tf represents the final temperature of the system, which is going to be the

temperature recorded when the metal rod and water in the calorimeter meet

equilibrium, in C. ti represents the initial temperature of the metal or water. On

one side of the equation, these variables apply to the water in the calorimeter. On

the other side, they apply to the metal sample. The specific heat on the water

side of the equation will be waters known specific heat value, 4.184. It is also
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important to note the mass of the water will be determined based on the milliliters

or water added to the calorimeter, as the density of water is one gram per one

milliliter.
Barber-Coles-Monteiro 10

Experimental Design

Materials:

Loaf Pan (2) Molybdenum Samples (Material A)


Scale (0.0001 g precision) (2) Unknown Metal Samples (Material B)
Tongs Vernier Temperature Probe (0.01 C)
Hot Plate Vernier LabQuest
Thermometer (0.1 C) Timer
Hot Mitt (4) 100mL Graduated Cylinder
(4) PVC Calorimeters Microsoft Excel

Procedure:

1. Using Microsoft Excel, randomly assign each sample to one of thirty trials.
Ensure that each sample is used in 15 trials. Do this for both materials A
and B. (see Appendix B)

2. Fill the loaf pan approximately half full with water.

3. Place the loaf pan on a hot plate, turn the hot plate on high, and bring the
water somewhere between 95-105 C.

4. Set up the Labquest (see Appendix C).

5. Using a scale, measure the mass of the sample and record it.

6. Using tongs, place the metal rod into the boiling water within the loaf pan
for 60 seconds. Using the thermometer, record the temperature of the
water in the pan at this point as the initial temperature of the metal for
each trial.

7. For trials using the known metal samples, measure out 45 ml of room
temperature water using a graduated cylinder. For trials using the
unknown metal samples, measure out 37 ml of room temperature water
using a graduated cylinder. Note how much water was measured. Pour
this water into the appropriate calorimeter (see Appendix A for how to
create the calorimeters).

8. Record the temperature of the water in the calorimeter after the


temperature probe has reached equilibrium with the water as the initial
temperature of the water. Keep the temperature probe in the water.

9. Using the tongs, place the hot metal rod into the calorimeter. Be sure to
replace the lid on the calorimeter
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10. Record the temperature of the water in the calorimeter after 45 seconds
as the final temperature.

11. Use the recorded values to calculate the specific heat of the metal (see
Appendix D for example calculation).

12. Repeat steps 5-11 for all trials.

Diagram:

Figure 2. Calorimeter Setup

Figure 2 shows the setup used in this experiment. Not pictured are the

tongs, hot plate, metal samples, and loaf pan.


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Data and Observations

Data:

Table 2
Data from the Specific Heat Molybdenum Trials
Molybdenum
Change in Temp. Specific
Initial Temp. (C)
Equilibrium (C) Heat
Trial Rod Mass (g)
Temp. (C) (J/g x
Water Metal Water Metal
C)
1 B 21.3 99.3 24.5 3.20 -74.8 42.7913 0.188
2 A 21.3 99.3 24.4 3.10 -74.9 42.7114 0.182
3 A 22.6 99.5 25.5 2.90 -74.0 42.7076 0.173
4 B 22.2 99.5 25.0 2.80 -74.5 42.7953 0.165
5 A 26.7 99.3 29.2 2.50 -70.1 42.7115 0.157
6 B 26.8 99.3 29.5 2.70 -69.8 42.7913 0.170
7 A 25.4 98.6 28.2 2.80 -70.4 42.7077 0.175
8 B 25.0 98.6 27.4 2.40 -71.2 42.7953 0.148
9 B 26.8 99.2 28.9 2.10 -70.3 42.7912 0.131
10 A 26.2 99.2 28.7 2.50 -70.5 42.7117 0.156
11 B 25.8 99.0 28.3 2.50 -70.7 42.7914 0.156
12 A 25.9 99.0 28.5 2.60 -70.5 42.7134 0.163
13 A 25.4 99.3 28.1 2.70 -71.2 42.7076 0.167
14 B 25.1 99.3 27.9 2.80 -71.4 42.7953 0.173
15 B 23.7 99.5 26.5 2.80 -73.0 42.7907 0.169
16 A 24.1 99.5 27.0 2.90 -72.5 42.7119 0.176
17 B 23.8 94.3 26.9 3.10 -67.4 42.7949 0.202
18 A 23.6 94.3 26.5 2.90 -67.8 42.7066 0.189
19 A 23.6 93.0 26.6 3.00 -66.4 42.7068 0.199
20 A 23.6 90.1 26.1 2.50 -64.0 42.7161 0.172
21 B 23.7 93.0 27.2 3.50 -65.8 42.7954 0.234
22 B 23.7 90.1 26.5 2.80 -63.6 42.7938 0.194
23 A 23.6 97.1 26.4 2.80 -70.7 42.7146 0.175
24 B 23.7 97.1 26.3 2.60 -70.8 42.7888 0.162
25 A 23.9 99.1 26.8 2.90 -72.3 42.7072 0.177
26 B 23.8 99.1 26.8 3.00 -72.3 42.7921 0.183
27 B 23.2 95.5 26.5 3.30 -69.0 42.7865 0.210
28 B 23.3 97.2 26.7 3.40 -70.5 42.7921 0.212
29 A 23.2 95.5 26.1 2.90 -69.4 42.7108 0.184
30 A 23.4 97.2 26.3 2.90 -70.9 42.7033 0.180
31 B 22.9 91.3 26.0 3.10 -65.3 42.7901 0.209
Barber-Coles-Monteiro 13

Change in Temp. Specific


Initial Temp. (C)
Equilibrium (C) Heat
Trial Rod Mass (g)
Temp. (C) (J/g x
Water Metal Water Metal
C)
32 A 22.8 91.3 25.8 3.00 -65.5 42.7096 0.202
33 A 21.9 98.9 24.8 2.90 -74.1 42.7065 0.173
34 B 21.6 98.9 25.0 3.40 -73.9 42.7939 0.202
35 B 22.2 99.3 25.6 3.40 -73.7 42.7897 0.203
36 B 22.1 99.2 25.9 3.80 -73.3 42.7925 0.228
37 B 21.8 99.2 24.8 3.00 -74.4 42.7896 0.177
38 B 21.8 98.5 25.0 3.20 -73.5 42.7929 0.192
39 B 21.6 98.9 24.9 3.30 -74.0 42.7897 0.196
40 A 22.4 99.3 25.5 3.10 -73.8 42.7101 0.185
41 A 22.2 99.2 25.5 3.30 -73.7 42.7052 0.197
42 B 21.7 98.8 25.2 3.50 -73.6 42.7934 0.209
43 B 21.8 98.9 25.1 3.30 -73.8 42.8059 0.197
44 A 22.0 99.2 25.0 3.00 -74.2 42.7099 0.178
45 A 21.9 98.5 25.3 3.40 -73.2 42.7058 0.205
46 B 22.0 99.0 25.7 3.70 -73.3 42.8036 0.222
47 B 21.9 99.1 25.1 3.20 -74.0 42.7987 0.190
48 A 21.7 98.9 24.7 3.00 -74.2 42.7095 0.178
49 B 22.3 99.3 25.4 3.10 -73.9 42.7987 0.185
50 A 21.7 98.8 25.1 3.40 -73.7 42.7052 0.203
51 A 22.0 98.9 25.1 3.10 -73.8 42.7141 0.185
52 A 22.1 99.0 25.1 3.00 -73.9 42.7131 0.179
53 A 21.9 99.1 24.9 3.00 -74.2 42.7154 0.178
54 A 22.5 99.3 25.6 3.10 -73.7 42.7124 0.185
55 A 22.8 99.1 25.9 3.10 -73.2 42.6833 0.187
56 B 22.6 99.1 25.6 3.00 -73.5 42.7946 0.180
Average 23.2 97.8 26.2 3.01 -71.6 42.7512 0.185

Table 2, above, compiles all the data collected from the samples known to

be Molybdenum, as well as the specific heat of each trial.


Barber-Coles-Monteiro 14

Table 3
Data from the Specific Heat Trials of the Unknown Metals
Unknown Metal
Change in Temp.
Initial Temp. (C) Equilibrium Specific
Trial Rod Temp. (C) Mass (g) Heat
Water Metal (C) Water Metal (J/g x C)
1 A 21.7 99.3 32.7 11.0 -66.6 75.2389 0.344
2 A 24.3 99.5 35.0 10.7 -64.5 75.2392 0.346
3 B 21.8 99.3 33.1 11.3 -66.2 75.6435 0.354
4 A 27.2 99.3 37.8 10.6 -61.5 75.2321 0.359
5 B 24.2 99.5 34.9 10.7 -64.6 75.6510 0.344
6 B 27.1 99.3 37.9 10.8 -61.4 75.6429 0.365
7 A 26.0 98.6 36.7 10.7 -61.9 75.2322 0.361
8 A 27.8 99.2 37.4 9.6 -61.8 75.2408 0.324
9 A 28.7 100.1 37.4 8.7 -62.7 75.2315 0.289
10 A 27.7 99.0 38.0 10.3 -61.0 75.2398 0.352
11 A 26.5 99.3 37.2 10.7 -62.1 75.2310 0.359
12 B 26.0 98.6 36.1 10.1 -62.5 75.6511 0.335
13 B 27.8 99.2 37.8 10.0 -61.4 75.6425 0.338
14 B 29.0 100.1 38.7 9.7 -61.4 75.6497 0.328
15 A 25.6 99.5 36.4 10.8 -63.1 75.2399 0.357
16 A 23.8 94.3 35.8 12.0 -58.5 75.2338 0.428
17 B 27.8 99.0 37.7 9.9 -61.3 75.6433 0.335
18 A 25.8 93.0 36.0 10.2 -57.0 75.2419 0.373
19 B 26.6 99.3 36.6 10.0 -62.7 75.6518 0.331
20 B 25.3 99.5 35.9 10.6 -63.6 75.6428 0.346
21 B 23.7 94.3 36.0 12.3 -58.3 75.6518 0.438
22 B 25.5 93.0 35.9 10.4 -57.1 75.6444 0.378
23 B 25.5 90.1 34.6 9.1 -55.5 75.6507 0.340
24 B 26.0 97.1 34.9 8.9 -62.2 75.6444 0.297
25 B 25.6 99.1 35.9 10.3 -63.2 75.6520 0.338
26 A 25.6 90.1 36.4 10.8 -53.7 75.2348 0.419
27 A 26.0 97.1 36.5 10.5 -60.6 75.2422 0.361
28 B 25.5 95.5 35.6 10.1 -59.9 75.6444 0.350
29 A 25.7 99.1 36.2 10.5 -62.9 75.2338 0.348
30 A 25.6 95.5 35.4 9.8 -60.1 75.2423 0.340
31 A 25.2 97.2 35.7 10.5 -61.5 75.2397 0.356
32 A 25.1 91.3 35.8 10.7 -55.5 75.2337 0.402
33 B 24.8 97.2 35.3 10.5 -61.9 75.6440 0.352
34 B 25.1 91.3 34.9 9.8 -56.4 75.6504 0.360
35 A 21.2 98.9 32.7 11.5 -66.2 75.2400 0.362
Barber-Coles-Monteiro 15

Equilibrium Change in Temp Specific


Initial Temp. (C) Mass
Trials Rod Temp. (C) Heat
(g)
Water Metal (C) Water Metal (J/g x C)
36 A 23.2 99.3 34.8 11.6 -64.5 75.2337 0.375
37 B 21.6 98.9 34.1 12.5 -64.8 75.6432 0.400
38 A 23.6 99.2 35.4 11.8 -63.8 75.2409 0.386
39 A 24.1 99.2 34.9 10.8 -64.3 75.2340 0.350
40 A 23.4 98.5 35.4 12.0 -63.1 75.2399 0.397
41 B 23.6 99.3 36.3 12.7 -63.0 75.6503 0.418
42 A 24.0 98.8 35.0 11.0 -63.8 75.2331 0.360
43 B 24.2 99.2 36.6 12.4 -62.6 75.6435 0.411
44 A 23.7 98.9 35.5 11.8 -63.4 75.2562 0.388
45 A 24.0 99.0 35.3 11.3 -63.7 75.2458 0.370
46 B 24.2 99.2 35.7 11.5 -63.5 75.6500 0.376
47 B 24.0 98.5 35.7 11.7 -62.8 75.6428 0.386
48 B 24.4 98.8 35.5 11.1 -63.3 75.6502 0.364
49 A 25.8 99.1 35.1 9.3 -64.0 75.2533 0.303
50 A 24.1 99.3 36.1 12.0 -63.2 75.2357 0.396
51 A 24.1 99.1 35.4 11.3 -63.7 75.2343 0.370
52 B 24.1 98.9 36.1 12.0 -62.8 75.6667 0.396
53 B 24.3 99.0 35.3 11.0 -63.7 75.6690 0.358
54 B 24.2 99.1 36.6 12.4 -62.5 75.6546 0.411
55 B 25.1 99.3 36.6 11.5 -62.7 75.6443 0.380
56 B 24.9 99.1 37.1 12.2 -62.0 75.6445 0.408
Average 25.0 97.9 35.9 10.9 -62.0 75.4435 0.365

Table 3 shows the data collected during the trials of the unknown

samples, with the specific heat also calculated.


Barber-Coles-Monteiro 16

Observations:

Table 4
Observation Data from the Specific Heat Trials of the Molybdenum Samples
Molybdenum Observations
Trial Metal Calorimeter Observations
1 B 2 One minute transfer
2 A 1 One minute transfer
Approximately 30 second transfer, switched
3 A 1 tongs
Approximately 30 second transfer, switched
4 B 2 tongs
Approximately 20 second transfer, early temp
5 A 1 reading (known moved first)
Approximately 20 second transfer, early temp
6 B 2 reading (known moved first)
Approximately 30 sec transfer. Calorimeter
7 A 1 tipped over, increasing time in air.
Approximately 30 sec transfer. Took longer to
8 B 2 get into calorimeter than normal.
9 B 2 20 sec transfer, but smooth.
20 sec transfer, took longer in air than other
10 A 1 samples.
11 B 2 Flawless transfer (20 seconds)
12 A 1 Flawless transfer (20 seconds)
13 A 1 20 sec transfer
14 B 2 20 sec transfer
15 B 2 30 second transfer
16 A 1 30 second transfer
17 B 2 Smooth transfer
18 A 1 Smooth transfer
19 A 1 Smooth transfer
20 A 1 Smooth transfer
Lid failed to sit properly on calorimeter
21 B 2 immediately, but did after being forced on.
22 B 2 Smooth transfer
23 A 1 Smooth transfer
24 B 2 Smooth transfer
25 A 1 Smooth transfer 20 seconds
26 B 2 Smooth transfer 20 seconds
27 B 2 Smooth transfer
28 B 2 15 sec fast transfer
29 A 1 Smooth transfer
Barber-Coles-Monteiro 17

Trial Metal Calorimeter Observations


30 A 1 15 sec fast transfer
31 B 2 Smooth transfer, a little extra time in the air.
32 A 1 Smooth transfer
33 A 1 Smooth efficient transfer (16 seconds)
34 B 2 Smooth efficient transfer (16 seconds)
35 B 2 Smooth efficient transfer
36 B 2 Smooth transfer
37 B 2 Took a while on transfer
Good transfer, thermometer turned off during
38 B 2 reading
39 B 2 Smooth transfer (no corresponding Unknown)
40 A 1 Smooth efficient transfer
41 A 1 Smooth transfer
42 B 2 18 sec smooth transfer
43 B 2 Okay transfer
44 A 1 Took a while on transfer
Good transfer thermometer turn off during
45 A 1 reading
46 B 2 Smooth transfer
47 B 2 10 second, very good transfer
Rough transfer, hit calorimeter before going
48 A 1 inside (no corresponding Unknown)
49 B 2 Smooth transfer
50 A 1 18 sec smooth transfer
51 A 1 Okay transfer
52 A 1 Smooth transfer
53 A 1 10 second gold transfer
54 A 1 Smooth transfer
55 A 1 Smooth transfer
56 B 2 Smooth transfer

Table 4, above, shows the qualitative observations of each trial of the

known metal samples. The times of transfer are approximate and are measured

from when all four metals tested at a time were in the water for one minute to

when the fourth sample was placed into its calorimeter.


Barber-Coles-Monteiro 18

Table 5
Observation Data of the Specific Heat Trials of the Unknown Metals
Unknown Metal Observations
Trial Metal Calorimeter Observations
1 A 3 One minute transfer
2 A 3 30 second transfer switched tongs
3 B 4 One minute transfer
20 second transfer early temp reading (known
4 A 3 moved first)
5 B 4 30 second transfer switched tongs
20 second transfer early temp reading (known
6 B 4 moved first)
7 A 3 30 sec transfer
8 A 3 20 sec transfer
Dropped before making it to calorimeter, no
simultaneous Molybdenum trials, odd temp
9 A 3 spike around 20 seconds (0.3C).
10 A 3 Flawless transfer (20 seconds)
11 A 3 20 sec transfer
12 B 4 30 sec transfer
13 B 4 20 sec transfer
14 B 4 No corresponding molybdenum trials
15 A 3 30 second transfer
16 A 3 Smooth transfer
17 B 4 Flawless transfer (20 seconds)
18 A 3 Smooth transfer (took while longer)
19 B 4 20 sec transfer
20 B 4 30 second transfer
21 B 4 Smooth transfer
22 B 4 Took longer smooth transfer
23 B 4 Fell twice
24 B 4 Fell on transfer to calorimeter
25 B 4 Smooth transfer 20 seconds VIDEO
26 A 3 Smooth transfer
27 A 3 Smooth transfer
28 B 4 Smooth transfer
29 A 3 Smooth transfer 20 seconds VIDEO
30 A 3 Took long time on transfer
31 A 3 15s fast transfer
32 A 3 Smooth transfer
33 B 4 15s fast transfer
34 B 4 Smooth transfer, a little extra time in air.
Barber-Coles-Monteiro 19

Trial Metal Calorimeter Observations


35 A 3 Smooth efficient transfer (16 seconds)
36 A 3 Smooth efficient transfer one corner exposed
37 B 4 Smooth efficient transfer (16 seconds)
38 A 3 Smooth transfer
39 A 3 Smooth transfer
Good transfer. Thermometer turned off during
40 A 3 reading.
Smooth, efficient transfer. One corner of the
sample was exposed above water in loaf
41 B 4 pan.
42 A 3 18 sec smooth transfer
43 B 4 Smooth transfer
44 A 3 Okay transfer
45 A 3 Smooth transfer
46 B 4 Smooth transfer
Good transfer thermometer turn off during
47 B 4 reading
48 B 4 18 sec smooth transfer
49 A 3 10 second gold transfer
50 A 3 Slightly longer transfer
51 A 3 Smooth transfer
52 B 4 Okay transfer
53 B 4 Dropped twice on transfer
54 B 4 10 second gold transfer
55 B 4 Smooth transfer
56 B 4 Smooth transfer

Table 5 shows the qualitative observations of the unknown trials. The

transfer times are approximate and are measured the same way as the unknown

trials were, as they were conducted simultaneously. No notable photographs

were taken.
Barber-Coles-Monteiro 20

Data Analysis & Interpretation

This research was done in order to determine if an unknown sample is

molybdenum by comparing the specific heat of the known molybdenum samples

to the specific heat of the unknown metal samples. This was done by

constructing calorimeters and measuring the specific heats of metal samples.

Specific heat is measured in Joules over grams times degrees Celsius.

In order to ensure reliable data, there must be a control, there must be

randomness, and there must repetition. The control in the experiment was finding

the specific heat of the known molybdenum samples, to allow for accounting for

error introduced through flaws in the procedure and materials. The order the

trials were run was randomized using Excel. Each metal was subject to 56 trials,

a sample size large enough to ensure the central limit theorem applies and the

data is normal, which is verified more thoroughly later.

Table 6
Percent Error of the Known Molybdenum Trials
Perc. Perc. Perc. Perc.
Trial Trial Trial Trial
Error Error Error Error
1 -24.71% 16 -29.47% 31 -16.45% 46 -11.19%
2 -27.02% 17 -19.06% 32 -19.24% 47 -23.91%
3 -30.89% 18 -24.57% 33 -30.98% 48 -28.71%
4 -33.86% 19 -20.33% 34 -19.03% 49 -26.18%
5 -37.12% 20 -31.13% 35 -18.80% 50 -18.64%
6 -31.92% 21 -6.39% 36 -8.76% 51 -25.94%
7 -29.86% 22 -22.52% 37 -29.03% 52 -28.42%
8 -40.68% 23 -30.17% 38 -23.38% 53 -28.72%
9 -47.43% 24 -35.36% 39 -21.51% 54 -25.83%
10 -37.47% 25 -29.27% 40 -25.93% 55 -25.28%
11 -37.77% 26 -26.97% 41 -21.04% 56 -28.17%
12 -34.97% 27 -15.82% 42 -16.31% AVG -26.08%
13 -33.13% 28 -15.12% 43 -21.33%
14 -30.99% 29 -26.32% 44 -28.71%
15 -32.49% 30 -27.86% 45 -18.09%
Barber-Coles-Monteiro 21

Table 6 on the previous page shows the percent error for all trials of the

known metal. Percent error was monitored during the experiment in order to

make sure that the experiment was delivering consistent results. The range of

the percent error of the molybdenum samples is 41.03 percent.

Table 7
Percent Error for the Trials of the Unknown Metal
Perc. Perc. Perc. Perc.
Trial Trial Trial Trial
Error Error Error Error
1 37.77% 16 71.12% 31 42.41% 46 50.24%
2 38.38% 17 33.99% 32 60.83% 47 54.58%
3 41.62% 18 49.26% 33 40.74% 48 45.48%
4 43.78% 19 32.31% 34 44.15% 49 21.19%
5 37.41% 20 38.28% 35 44.90% 50 58.39%
6 45.94% 21 75.03% 36 50.03% 51 47.98%
7 44.20% 22 51.11% 37 60.05% 52 58.49%
8 29.57% 23 36.02% 38 54.27% 53 43.22%
9 15.75% 24 18.72% 39 40.11% 54 64.58%
10 40.85% 25 35.20% 40 58.63% 55 52.17%
11 43.74% 26 67.77% 41 67.24% 56 63.26%
12 34.06% 27 44.52% 42 43.83% AVG 45.80%
13 35.13% 28 39.89% 43 64.35%
14 31.06% 29 39.25% 44 55.21%
15 42.77% 30 36.01% 45 47.96%

Table 7 shows the percent errors from the trials of the unknown samples.

The range of the percent error of the unknown samples is 59.27 percent. These

percent errors are consistently much higher than the ones in the known

molybdenum trials. In fact, the difference in the averages is 71.6 percent.

The control tests yielded a specific heat value that was on average 0.158

(J/g x C). However, it is known that the actual specific heat of molybdenum is

0.25 (J/g x C). In order to correct for the errors led to this discrepancy, the

difference of these two values, 0.065 (J/g x C), was added to every specific heat
Barber-Coles-Monteiro 22

data point collected for both metals before any further analysis was performed.

This adjustment means that the average percent error for the known

molybdenum samples is 0.45%, and the average percent error for the unknown

samples is 71.85%.

Before any statistical analysis test is run, various descriptive statistics and

graphs can be analyzed. The first to be analyzed will boxplots of the data, as well

as the quartile data.

Figure 3. Box Plot of the Specific Heat Values of Molybdenum

Figure 3 shows the boxplot for the specific heat values of the molybdenum

samples. The median specific heat and true specific heat values appear close to

each other, having a difference of only 0.002 (J/g x C). The box plot appears to

be mostly normally distributed, with a slight right skew. The data points all lie

between 0.299 (J/g x C) and 0.196 (J/g x C), giving the data a range of 0.103

(J/g x C).
Barber-Coles-Monteiro 23

Figure 4. Box Plot of the Specific Heat Values of the Unknown Samples

Figure 4 shows the boxplot for the specific heat values of the unknown

samples. The median specific heat and true specific heat values appear relatively

far from each other, having a difference of 0.175 (J/g x C). The box plot appears

to be mostly normally distributed, with a slight right skew, similar to that of the

molybdenum trials. The data points lie between 0.503 (J/g x C) and 0.354 (J/g x

C), giving the data a range of 0.149 (J/g x C).

Before running a statistical test, it is helpful to verify that the data tested is

normal. Normal probability plots are one method used to determine if the data

comes from a normally distributed population.


Barber-Coles-Monteiro 24

Figure 5. Normal Probability Plot of the Specific Heat Molybdenum Trials

Figure 5 shows the normal probability plot for the molybdenum specific

heat trials. As seen in the figure, the data appears to be roughly linear. This

means that the data can reasonably be modeled using a normal distribution.

Figure 6. Normal Probability Plot of the Specific Heat Unknown Trials


Barber-Coles-Monteiro 25

Figure 6 shows the normal probability plot for the unknown metal specific

heat trials. Again, the data also appears to be roughly linear and can be modeled

with a normal distribution.

The appropriate statistical test in this situation is a two-sample t test,

because the specific heat of different samples from two different populations of

uncertain standard deviation is being compared. These populations are the

unknown metal trials and the known metal trials.

In order to run a two-sample t test numerous conditions must be met. The

first condition is that the data comes from a simple random sample. In this case,

the Excel randomization acts to make sure that the data is a random sample. The

second condition that must be met is that the data comes from a normally

distributed population, and there must be enough data to satisfy the central limit

theorem. As shown above by the normal probability plots, the data appears to be

for the most part normally distributed. The sample size, 56, is also large enough

that it can be concluded that the data is normal by the central limit theorem. The

third condition is that the samples are from independent populations. This

experiment was designed to keep the four rods isolated from each other, and

thus independent. All conditions for the test have been met, so a two-sample t

test can be run.

For a two sample t-test to be run, first a null and alternative hypothesis

must be stated.
Barber-Coles-Monteiro 26

0 : =

0 : =

Figure 7. Null and Alternative Hypothesis

In figure 7, the null hypothesis, H , states that the true mean of the specific
o

heat values of the known molybdenum samples (k) is the equivalent to the true

mean of the specific heat values of the unknown samples (u). The alternative

hypothesis, H , states that the mean of the true specific heat values of the known
a

molybdenum samples (k) is not equivalent to the mean of the true specific heat

values of the unknown samples (u). The equation for a t-test, as well as a

sample calculation, is shown in appendix D.

Figure 8. TI-Nspire Two-Sample t Test Results

Figure 8, above, contains the results from the two-sample t test run on the

specific heat values, as well as a graph of the p-value, where the portion of the t

distribution represented by the p-value is shaded. This region is so small that the

shaded portion is not visible. The t value of -36.1791 means that the shaded

region starts 36.1791 standard deviations from the mean.


Barber-Coles-Monteiro 27

The null hypothesis was rejected, because the p-value of 3.96 x10-56 is

less than the level of 0.1. This means that it is highly unlikely the unknown

metal has the same specific heat as molybdenum. If the null hypothesis were

true, that is, if the true mean for the specific heat of the unknown metal was 0.25

(J/g x C), there is only a 3.96 x 10-54% chance that the average reading of 0.430

(J/g x C) could occur by chance. Since these results are so unlikely to occur by

chance, it can be concluded that the unknown samples do not have the same

specific heat as molybdenum.


Barber-Coles-Monteiro 28

Conclusion

This experiment was intended to identify whether a metal sample was

molybdenum. During the experiment, metal samples were heated and then

placed in a calorimeter to measure their specific heats. A two-sample t test was

then carried out on the specific heat data. The hypothesis that the metal sample

was molybdenum was rejected. The unidentified metal samples are not

molybdenum. This conclusion was drawn due to both the difference in mean

specific heats and the physical differences of the metal samples.

The two-sample t test determined that there was a less than 3.96 x 10 % -54

chance that the difference in mean specific heats would occur by chance alone, if

the samples were in fact molybdenum. The unlikeliness of this occurring,

combined with physical differences observed in the metals from known

molybdenum samples, allow the hypothesis to be rejected with certainty. The

unknown metal samples are not molybdenum.

The calorimeters used in this experiment were bespoke, and hand-built

out of PVC by the researchers. PVC is not designed to insulate heat. While the

design of the calorimeters attempted to counter this shortcoming by wrapping the

pipe in insulation, and was further benefited by the presence of water, which is a

poor conductor of heat, there were still many exposed areas of the pipe that may

have leaked heat into the environment. This heat loss means that the readings of

the calorimeters were not perfectly accurate. This was a minor shortcoming

experiment of the experiment, especially in comparison to the main source of

heat loss in the experiment: the heat lost while transferring the samples from the
Barber-Coles-Monteiro 29

boiling water to the calorimeters. Heat energy always moves towards equilibrium

in its environment, and, while exposed, the samples released heat in pursuit of

equilibrium with the lab air. This introduced error into the experiment. Although

the statistical analysis process attempted to account for the errors due to heat

loss by adding a correction factor, the correction was not exact and thus some

error remained.

Further, error was introduced by the failings of the researchers to carry out

the experiment perfectly. The metal samples were repeatedly dropped while

attempting to transfer them from the boiling water to the calorimeters. This

resulted in the metal samples spending a greater amount of time in the air, thus

losing more heat to the air before being placed into the calorimeters.

Furthermore, the samples were held by metal tongs, and heat transferred from

the metal samples to the tongs. Also, the amount of time required to transfer the

samples from the boiling water to the calorimeters varied, causing variation in the

amount of heat released into the air. Once in the PVC, some heat from the

samples transferred to the PVC pipe and not the water, resulting in more loss of

heat during the transfer. These errors could be reduced by using more secure

tongs or by placing the calorimeters closer to the source of the boiling water.

Despite this, the results are still in line with the existing scientific

knowledge as referenced in the review of literature section. The property of

specific heat proved to be a good metric for determining the identity of a sample.

Also, the behavior of the heat within the calorimeters and outside them was in
Barber-Coles-Monteiro 30

line with how it was explained in the literature. These similarities to previously

published results lend credence to the results of this experiment.

Further tests could be used to ID this element, including chemical tests

and tests of other intensive properties such as tensile strength and density, but

those are beyond the range of this experiment. The design of this experiment

could also be used by other researchers to design a more sophisticated test of

specific heat, using superior calorimeter and refined transfer techniques.


Barber-Coles-Monteiro 31

Application

Molybdenum is a rare and precious element, and the fact that it is

essential for life as well as being very durable makes it desirable as jewelry.

Figure 9. Drawing View of the Ring

Figure 9 shows the SolidWorks drawing view output of the ring, which is

useful in actually constructing the jewelry piece.

Figure 10. Isometric View of the ring


Barber-Coles-Monteiro 32

Figure 10 shows a 3-dimensional rendering of the ring, which includes a

faux diamond-shaped setting for aesthetic effect. The ring has a mass of 0.1

pounds, and molybdenum sells for $30 a pound, so the rings raw materials

would cost approximately $3.00.


Barber-Coles-Monteiro 33

Acknowledgements
We would like to thank Stuarts family and Elisas mother for financing this

experiment. Without the materials we would not be able to conduct the

experiment.
Barber-Coles-Monteiro 34

Appendix A: Constructing the Calorimeters

Materials:

20 in. in. diameter PVC Pipe


Hand saw
(8) in. PVC Endcaps
14 in. in. diameter polyethylene pipe insulation
Drill
4 mm Drill Bit
Scissors
8 Wire Coat Hangers
Cutting Pliers

Procedure:

1. Using the saw, cut a five inch segment of PVC pipe.

2. Using scissors, cut the insulation into a 3.5 inch segment.

3. Place one end cap on each onto PVC segment.

4. Slide one segment of insulation over each segment of PVC.

5. Using the drill with the 4 mm drill bit in place, drill a hole in the top of
another end cap, approximately one centimeter from the edge.

6. Place this cap onto the open end of the PVC pipe.

7. Repeat steps 1-7 for all four calorimeters.

8. Use the cutting pliers to separate the bottom, straight segment of the wire
hanger from the top.

9. Use the pliers to bend the wire hangers around the edges of the bin,
locking them in place.
Barber-Coles-Monteiro 35

Appendix B: Randomization with Excel

Materials:

Microsoft Excel 2010

Procedure:

1. Open a new workbook in Microsoft Excel.

2. Type the values 1-30 in their respective boxes in Column A.

3. In column B, alternate between letters A and B for each box, to indicate


which sample will be assigned to which trial.

4. In cell C1, type rand().

5. Use autofill to copy the random number generation command into cells
C2-C30.

6. Select cells B1-B30 and C1-C30, and right click on the selection. From the
list of options in the context menu, place the mouse over Sort and select
Custom Sort.

7. In the custom sort box, ensure that the Column drop down is set to
Column C, the Sort On box is set to Values and the Order box is set
to Smallest to Largest. The resulting order of As and Bs will indicate
which sample is assigned to which trial.

8. Repeat these steps for the other group of metals.


Barber-Coles-Monteiro 36

Appendix C: LabQuest Setup

Materials:

Vernier Labquest
(4) Vernier Labquest Temperature Probe

Procedure:

1. Plug a temperature probe into each slot on the back of the Labquest.

2. Turn the Labquest on.

3. Click the duration on the screen that appears.

4. In the prompt that appears, change the duration to 180 seconds and press
OK.

5. Select the Data Collection Tab.

6. Begin data collection.


Barber-Coles-Monteiro 37

Appendix D: Formulas and Sample Calculations

The calculation for determining specific heat was performed on every data

point. The formula used to calculate specific heat is shown blown, where smetal is

the specific heat of the metal, mmetal is the mass of the metal, timetal is the initial

temperature of the metal, tf is the final temperature, tiwater is the initial temperature

of the water, swater is the specific heat of the water, and mwater is the mass of the

water.

( ) = ( ( ))

A sample calculation is shown.

( ) = ( ( ))

42.7913 (24.5 99.3)


= (4.184( ) 45 (24.5 21.3))

= 0.188

Figure 11. Sample Calculation of Specific Heat

Figure 11, above, shows the calculations to determine specific heat of the

metal sample using the data collected in trial number one of the Molybdenum

data collection.

As well as specific heat, a test was done to determine the percent

error of each trial. This was used to ensure consistency in the results. The

following formula was used to calculate this, where the experimental value is the

value determined in the lab, and the true value is the published value for the

metal.
Barber-Coles-Monteiro 38


= 100

An example calculation using values from the experiment is shown on the

next page.


= 100


0.344 ( ) 0.25( )
= 100

0.25 ( )

= 37.77%

Figure 12. Sample Calculation of Percent Error

Figure 12 shows the example calculation of percent error.

Finally, a two-sample t test was conducted. The equation for this test is

shown below:


=
( )2 ( )2

+

In this equation, t stands for the t value of the test, stands for the mean

of the samples, s stands for the standard deviation of the sample population, and

n stands for the number of samples in each sample population. The subscript m

means that that number represents the known molybdenum population and the

subscript u means that the value represents the unknown metal population. A

sample calculation using the formula is carried out below.


=
( )2 ( )2

+
Barber-Coles-Monteiro 39


0.2498 ( ) 0.4295( )
=
2
(0.0196 ( )) (0.0316 ( ))2
+
56 56

= 36.971

Figure 13. Example Calculation of a Two-Sample t Test

Figure 13 on the previous page shows the calculations required to execute

a two-sample t test.
Barber-Coles-Monteiro 40

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