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Flame Test Experiment

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Name ___________________________ Date ___________________ Class __________________

Chapter 5 • Electrons in Atoms EXPERIMENT

FLAME TESTS FOR METALS


6
PURPOSE
To observe and identify metallic ions, using flame tests.
Text Reference
Section 5.3

Time Required BACKGROUND


30 minutes Have you ever wondered why a candle flame is yellow? The characteristic
yellow of a candle flame comes from the glow of burning carbon
Objectives fragments. The carbon fragments are produced by the incomplete
• Observe the flame test for combustion reaction of the wick and candle wax. When elements, such
seven different metallic as carbon, are heated to high temperatures, some of their electrons are
ions.
excited to higher energy levels. When these excited electrons fall back to
• Identify an unknown lower energy levels, they release excess energy in packages of light called
metallic element, using
photons, or light quanta. The color of the emitted light depends on its
the flame test.
energy. Blue light is more energetic than red light, for example. When
heated, each element emits a characteristic pattern of light energies,
Advance Preparation which is useful for identifying the element. The characteristic colors of
6M hydrochloric acid
light produced when substances are heated in the flame of a gas burner
Pour 150 mL concentrated
HCl into 150 mL of water. are the basis of flame tests for several elements.
In this experiment, you will perform the flame tests used to identify
several metallic elements.
Fill small labeled screw-top
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jars with chemicals for


groups of four students to
use at their lab stations. MATERIALS (PER PAIR)
safety goggles potassium nitrate, KNO3 t
Platinum wire is more
expensive, but also more 8 small test tubes calcium nitrate, Ca(NO3)2 t
durable, than nichrome wire. test-tube rack strontium nitrate, Sr(NO3)2 t
Nichrome wire can paper towel lithium nitrate, LiNO3
deteriorate rapidly, especially scoopulas copper(II) nitrate, Cu(NO3)2 t
if it is used in the hottest
50-mL beaker sodium nitrate, NaNO3 t
region of the burner flame.
platinum wire or nichrome barium nitrate, Ba(NO3)2 tc
wire loop 6M hydrochloric acid, HCl ct
gas burner unknown salt
cobalt-blue glass

SAFETY FIRST!
Review the safety procedures In this lab, the solutions you will be using contain harmful materials.
and caution the students Avoid skin contact with these chemicals. Observe all precautions,
about the corrosive nature of especially the ones listed below. If you see a safety icon beside a step in
acids before they begin to the Procedure, refer to the list below for its meaning.
work.
Caution: Wear your safety goggles. (All steps.)

Experiment 6 Flame Tests for Metals 49


Name ___________________________ Date ___________________ Class __________________
Caution: Hydrochloric acid is corrosive and can cause severe
burns. (Step 2.)
Caution: Do not taste any of the substances or touch them with
your hands. (Step 1.)
Caution: Do not at any time touch the end of the wire loop used
in the flame tests. This wire gets extremely hot and can cause
severe burns. (Steps 2–5.)
Note: Return or dispose of all materials according to the
instructions of your teacher. (Step 6.)

PROCEDURE
As you perform the experiment, record your observations in Data Table 1.
1. Place a test-tube rack on a paper towel. Write the chemical
name for each of the seven metal salts next to a position in the
rack where a test tube will be placed. Use scoopulas supplied
with each salt to place pea-sized samples of each metal salt
into a test tube. Place the tubes in the test-tube rack.
2. Pour about 15 mL of 6M HCl into a clean, labeled 50-mL
beaker. Dip the wire loop into the 6M HCl and then heat it in
the hot flame of a gas burner, as shown in Figure 6.1a. Continue
this procedure until no color comes from the wire when it is
put into the flame.
3. Dip the clean wire loop into a sample of metal salt and heat the
sample in the burner flame, as shown in Figure 6.1b. Record the
color of the flame in Data Table 1. Test the remaining samples,
cleaning the wire loop as described in Step 2, before each new
The solutions can be stored
sample is tested. Record your observations.
and reused or use the

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following disposal methods 4. View the flame colors produced by NaNO3 and KNO3 through
for chemical waste. cobalt-blue glass. Record your observations.
Disposal 1: NaNO3, KNO3, 5. Perform a flame test on your unknown salt. Record your
Ca(NO3)2, Sr(NO3)2, LiNO3,
observations.
Cu(NO3)2.
Disposal 2: HCl(aq). 6. Dispose of the unused portions of your samples as directed by
your teacher.
Disposal 3: Ba(NO3)2.

Figure 6.1a Figure 6.1b

50 Chemistry Laboratory Manual


Name ___________________________ Date ___________________ Class __________________

OBSERVATIONS
DATA TABLE 1: FLAME TESTS

Ion Flame Color

sodium, Na yellow

potassium, K violet and yellow

calcium, Ca2 brick red

barium, Ba2 green

strontium, Sr2 bright red

lithium, Li crimson

copper, Cu2 blue-green

sodium, Na (cobalt glass) none

potassium, K (cobalt glass) violet

unknown

ANALYSES AND CONCLUSIONS


1. List the elements that produced the most easily identified colors.
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Ca2, Ba2, Sr2, Li, Cu2 are quite easily identified.

2. Which elements are least easily identified? Explain.


Na and K are difficult to distinguish.

3. Which element produces the most intense color?


The color given by Sr2 is a very bright red and is probably the most intense.

4. Would flame tests be useful for detecting metal ions present in a mixture of metal
ions? Explain.
The detection of metal ions in mixtures would be difficult. For example, Li and Sr2

both give red flames and cannot be distinguished in a mixture.

Experiment 6 Flame Tests for Metals 51


Name ___________________________ Date ___________________ Class __________________

5. The energy of colored light increases in the order red, yellow, green, blue, violet.
List the metallic elements used in the flame tests in increasing order of the energy
of the light emitted.

Sr2 Li Ca2  2 2 


冢 red 冣 冢yellow
Na
冣 冢Bagreen
Cu
冣 冢violet
K

low energy y high energy

6. What is the purpose of using the cobalt glass in the identification of sodium and
potassium?
K nearly always gives a yellow flame because of the presence of trace amounts of Na.

Cobalt glass filters out the yellow, allowing the violet of K to be seen. The glass helps

to distinguish Na from K. If only Na is present, no flame is seen through the cobalt

glass. If K is present, violet light is seen through the glass.

GOING FURTHER
Do Research
In this lab, you observed that each element emits a unique color of light when heated
in a flame. If these light emissions were examined through a prism, you would observe
that the emitted light is actually composed of different wavelengths of light that may
lie in the violet region, the green region, or the red region of the visible spectrum. Each
element has a unique emission spectrum. Look up the emission spectra for the
elements tested in this lab. Do research on how scientists apply these emission
spectra to investigate the chemical composition of stars. For example, what is the

© Pearson Education, Inc., publishing as Pearson Prentice Hall. All rights reserved.
emission spectrum of the sun, and what does this spectrum reveal about the types of
elements in the sun?
Scientists compare the emission spectrum of the sun with the wavelengths of lines

emitted by elements in the laboratory to determine the kinds of elements in the sun. At

least 67 different elements have been detected in the sun’s emission spectrum. The sun

is mainly composed of helium and hydrogen.

52 Chemistry Laboratory Manual


Name ___________________________ Date ___________________ Class __________________

Chapter 5 • Electrons in Atoms EXPERIMENT

ENERGIES OF ELECTRONS
7

PURPOSE
Text Reference
To construct a simple flame spectrograph and measure a wavelength
Section 5.3 of light produced by the electronic excitations of sodium ions.

Time Required
40 minutes BACKGROUND
You should recall from Experiment 6 that flame tests are useful for
Objectives identifying metal ions that produce characteristic colors. Separating
• Construct a simple flame these characteristic colors into discrete wavelengths of light produces a
spectrograph.
pattern of individual lines that uniquely identifies the metal ion. This
• Measure the 589-nm pattern of lines is called an emission spectrum. With a reference source
flame omission line of the
of emission spectra, you would find it relatively easy to identify a
sodium ion.
particular metal ion.
You can separate the lines in the visible region of a flame emission
Advance Preparation spectrum by using an optical prism or a diffraction grating. A
6M hydrochloric acid
spectrograph is an instrument designed to produce electronic
Dilute concentrated HCl 1:1
with distilled water. excitations, separate the emitted light into its component wavelengths,
Approximately 200 mL will be and then record the wavelengths of emitted light. In this experiment,
required to meet the needs of you will construct a simple spectrograph and measure the wavelength of
15 student lab pairs. a strong excitation of sodium ions.
1M sodium chloride
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Dissolve 5.8 g of NaCl in 80


mL of distilled water and
dilute to 100 mL. MATERIALS (PER PAIR)
Other materials safety goggles watch glass
The width of the slit should 2 meter sticks platinum or nichrome wire
be 1 mm or less. The slit diffraction grating loop
height should be
cardboard piece with narrow gas burner
approximately 2 cm.
slit 6M hydrochloric acid, HCl ct
50-mL beaker 1M sodium chloride, NaCl

SAFETY FIRST!
In this lab, observe all precautions, especially the ones listed below. If
you see a safety icon beside a step in the Procedure, refer to the list below
for its meaning.
Caution: Wear your safety goggles. (All steps.)

Caution: Hydrochloric acid is corrosive and can cause severe


burns. (Step 2.)
Caution: Do not let your skin or clothing contact the burner
flame or the hot wire used in the flame tests. (Steps 2–4.)

Experiment 7 Energies of Electrons 53


Name ___________________________ Date ___________________ Class __________________
Caution: Exercise care when working with an open flame. Tie
back hair and loose clothing. Do not use the burner near
flammable materials. (Steps 2–4.)
Note: Return or dispose of all materials according to the
instructions of your teacher. (Step 7.)

PROCEDURE
As you perform the experiment, record your data and calculation results
in Data Table 1.
1. Set up the apparatus shown in Figure 7.1.

2. Pour approximately 15 mL of 6M hydrochloric acid, HCl, into a


50-mL beaker. Always cover the beaker with a watch glass
when the beaker is not being used. Clean the wire loop by first
dipping it into the HCl and then heating it in the hot flame of a
gas burner. Continue to dip and heat the wire until no color
comes from the wire as it is heated.
3. Dip the clean wire loop into the NaCl solution.
4. Place the wire loop in the burner flame. Observe the flame
through the slit in the cardboard and the diffraction grating, as
shown in Figure 7.1. You should see a series of lines to the left
and right of the slit. Pick out the brightest line to the left side of
the slit and have your partner record this position on the meter
stick as position A. Repeat this procedure on the right side of
the slit and record this as position B.
5. Measure the distance from the diffraction grating to the slit and
record this as distance Y.

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Use the following disposal
6. Dispose of the solutions as directed by your teacher.
methods for chemical waste.
Disposal 2: NaCl(aq).
Disposal 3: HCl(aq).

Left
image

A
B
90 Y
Right
80 image
Z
70

60

5 0
40
20
30
30 Movable 20
slit
40 10

50

60

Figure 7.1

54 Chemistry Laboratory Manual


Name ___________________________ Date ___________________ Class __________________

OBSERVATIONS
DATA TABLE 1: WAVELENGTH FOR THE SODIUM EMISSION LINE

left image (A) 15.0 cm

right image (B) 15.8 cm

distance X (average of left and right images) 15.4 cm

distance Y 40.0 cm

distance Z 42.9 cm

diffracting grating constant (d) 1.90  104 cm/line

sin  0.359

wavelength () 682 nm

ANALYSES AND CONCLUSIONS


1. Find the average of distances A and B (in centimeters). Record this answer as
distance X in your data table.

15.0 cm  15.8 cm
  15.4 cm
2

2. Calculate the distance Z, using the Pythagorean theorem. Refer to Figure 7.1 for
relationship of distances.
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Z  兹苶
X2  Y2苶
Record the value of Z in the data table.
Z 兹(15.4
苶苶 cm)2 苶
(40.0苶
cm)2

 兹237.1
苶苶 6 cm2苶
 16苶
00 cm2苶

 42.9 cm

3. Calculate sin , using the following relationship:


X
sin   
Z
Record sin  in the data table.
15.4 cm
sin ␪ 
42.9 cm
 0.359

Experiment 7 Energies of Electrons 55


Name ___________________________ Date ___________________ Class __________________

4. The wavelength () of the sodium flame emission line being investigated in this
experiment is given, in nanometers, by the Bragg equation:
1  107 nm

  d  sin   
1 cm 冣
1
d represents a diffraction grating constant: d   where n is the number of lines,
n
per centimeter, scribed on the diffraction grating. Calculate the value of d for your
grating and enter it in Data Table 1.
The number of lines per inch is often 13 400; d may be calculated
as follows:

1 in. 2.54 cm
d      1.90  104 cm/line (constant)
13 400 lines 1 in.

5. Compute the wavelength of the bright line you viewed on the meter stick, using
the Bragg equation. Record this value in the data table.
1  107 nm

  (1.90  104 cm)  (0.359)    682 nm
cm 冣
6. The accepted value of  for the observed transition is 589.0 nm. Calculate the
percent error in your value.

682 nm  589 nm
percent error    100  15.8%
589 nm

7. Identify the possible sources of error in your determination of .


The major source of error is the measurement of the values for X and Y.

8. How can a spectrographic experiment help identify a particular metal ion?

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The ions of each element give characteristic patterns of lines in the spectrograph.

Even elements that produce flame-test results that appear to the eye to be the same

color produce very different sets of flame emission lines.

GOING FURTHER
Do Research
Atomic absorption spectroscopy is one of the most sensitive methods available for the
detection of various metals. Do research to find out how this method is used to
quantify the amount of an element in a particular sample and compare the detection
limits of this method with other spectroscopic methods of analysis.
The detection limits of many modern atomic spectroscopic methods lie well below 1 ppm

for a number of metallic elements. The ultrasensitivity of this technique is a valuable asset

to scientists studying materials that contain only trace amounts of a given metal.

56 Chemistry Laboratory Manual


Name ___________________________ Date ___________________ Class __________________

Chapter 5 • Electrons in Atoms EXPERIMENT

INTRODUCTION TO THE
8 SPECTROPHOTOMETER
PURPOSE
To determine the absorption spectrum of an aqueous solution of
Text Reference chromium(III) ions.
Section 5.3

Time Required BACKGROUND


50 minutes
Many compounds absorb light from regions of the electromagnetic
spectrum. A spectrophotometer is a device designed to determine the
Objectives wavelengths of light that a compound absorbs. When an aqueous
• Examine the use of a
sample of a compound is placed in the light path of a
spectrophotometer to
study the light-absorbing spectrophotometer, the sample may absorb all the light, some of the
properties of a chemical light, or no light at all. The absorption of light depends upon the
substance. materials in the sample and the wavelength of the light. Light absorption
• Observe how the occurs at wavelengths whose energy corresponds to the energy
absorption of light by a necessary to cause electronic excitations of atoms, ions, or molecules in
compound varies with the the sample. From the spectrophotometer data, a graph can be made that
wavelength of light. plots the light intensity transmitted through the sample versus the
• Construct a graph of wavelength of the light; such a graph is called an absorption spectrum.
wavelength versus The range of wavelengths absorbed by the sample appear as bands of
absorption for an aqueous minimum intensity.
solution of chromium(III)
Absorption spectra are useful for two reasons. First, the absorption
nitrate.
spectrum of a substance is a unique characteristic of that substance.
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This makes the spectrum useful for the identification of unknown


Advance Preparation substances. Second, the intensity of the absorption bands can be related
0.02M chromium(III) nitrate to the concentration of the substance in the sample. Thus, the intensity
Dissolve 4.8 g of Cr(NO3)3 in of the absorption band can be used to determine the amount of a
900 mL of distilled water and
particular substance in a mixture.
dilute to 1 L.
In this experiment, you will determine the absorption spectrum of an
aqueous solution of chromium(III) ions.

MATERIALS (PER PAIR)


safety goggles plastic wash bottle
Spectronic 20 distilled water
spectrophotometer 0.02M chromium(III) nitrate,
2 small test tubes or 2 glass Cr(NO3)3 ti
cuvettes tissue paper
10-mL graduated cylinder

SAFETY FIRST!
In this lab, observe all precautions, especially the following ones. If you
see a safety icon beside a step in the Procedure, refer to the following list
for its meaning.

Experiment 8 Introduction to the Spectrophotometer 57


Name ___________________________ Date ___________________ Class __________________

Caution: Wear your safety goggles. (All steps.)

Caution: Chromium(III) nitrate is toxic and can irritate your


skin. (Steps 5–8.)
Note: Return or dispose of all materials according to the
instructions of your teacher. (Step 8.)

PROCEDURE
As you perform the experiment, record your percent transmittance data
in Data Table 1.
1. Turn on the spectrophotometer and allow it to warm up for
about 20 minutes.
Step 2. 2. Set the wavelength control knob to 375 nanometers (375 nm).
To avoid damage, the Adjust the amplifier control knob to produce 0 percent
spectrophotometer knobs transmittance (0%T) at this wavelength.
must not be twisted past the
3. Add 3 mL of distilled water to a clean, small test tube. Wipe the
point at which resistance is
encountered. Twisting the
outside of the tube with a tissue to make certain that it is clean
amplifier control knob and dry. Avoid getting fingerprints on the tube. Dislodge any air
counterclockwise past the bubbles present in the water by gently tapping the tube with a
resistance point turns the finger.
spectrophotometer off.
4. Place the tube in the sample holder and close the cover. Adjust
Step 4. the light control knob until the spectrophotometer reads
Show students how to tilt the 100%T.
bottom of the test tube
slightly to the right (facing 5. Remove the first sample from the spectrophotometer. Add
the spectrophotometer) to fit 3 mL of 0.02M chromium(III) nitrate, Cr(NO3)3, to another
into the holder. clean test tube. Use a tissue to clean and dry the tube. Insert the

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tube of chromium(III) nitrate into the sample holder. Close the
The energy of the radiation cover of the holder. Read the percent transmittance and record
striking the detector is not the reading in Data Table 1. Remove the sample from the
constant at all wavelengths, holder.
because the energy output of 6. Turn the wavelength dial to 400 nm. Use the amplifier control
the source is not constant.
knob to adjust the percent transmittance to 0%T. Place the
The amplifier control knob
opens or closes the slit to water sample in the holder. With the light control knob, adjust
bring the energy at the the meter to 100%T. Replace the water sample with the
detector to the constant chromium(III) nitrate sample. Measure and record the percent
value designated 100%T. transmittance at 400 nm.
Failure to adjust to 100%T at
7. For the remainder of the wavelengths listed in Data Table 1,
each wavelength will
produce an “absorption continue the procedure of setting 0%T, setting 100%T, and
spectrum” that includes the measuring the percent transmittance of the chromium(III)
energy profile of the source nitrate solution.
as well as the spectrum of 8. Unless directed otherwise by your teacher, return the aqueous
the absorbing species in the
chromium(III) nitrate to the dropper bottle.
sample solution.

Use the following disposal


method for chemical waste.
Disposal 6: Cr(NO3)3.

58 Chemistry Laboratory Manual


Name ___________________________ Date ___________________ Class __________________

OBSERVATIONS
DATA TABLE 1: PERCENT TRANSMITTANCE AND ABSORBANCE OF 0.02M
Cr(NO3)3 SOLUTION AT VARIOUS WAVELENGTHS

Wavelength (nm) % Transmittance (%T) Absorbance


375 64.0 0.194

400 48.5 0.314

405 47.0 0.328

415 46.5 0.333

425 53.2 0.274

440 60.0 0.222

455 71.5 0.146

470 80.0 0.097

490 82.5 0.084

500 83.0 0.081

520 72.0 0.143

530 67.5 0.171

540 63.0 0.201

550 58.5 0.233

570 54.0 0.268

575 53.0 0.276


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580 53.0 0.276

600 56.0 0.252

625 66.3 0.178

ANALYSES AND CONCLUSIONS


1. Graph percent transmittance versus wavelength. The curve you plot is the
absorption spectrum of chromium(III) ions in the visible region of the
electromagnetic spectrum.
2. At what wavelengths do chromium(III) ions absorb the maximum amounts of
light? What colors of light correspond to these wavelengths?
There are two absorption maxima (transmittance minima). One is at

about 420 nm and the other is at about 580 nm. These wavelengths

of light correspond to the wavelengths of violet (400–450 nm) and

orange (600–650 nm) light.

Experiment 8 Introduction to the Spectrophotometer 59


Name ___________________________ Date ___________________ Class __________________

100

80
Percent Transmittance (%T)

60

40

Sample Data:
Percent Transmittance (%T)
versus Wavelength (nm)
20

0
350 400 450 500 550 600 650

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Wavelength (nm)

Sample Data:
Absorbance (A)
Absorbance (A)

0.4 versus Wavelength (nm)

0.2

0
350 400 450 500 550 600 650
Wavelength (nm)

60 Chemistry Laboratory Manual


Name ___________________________ Date ___________________ Class __________________

3. Based on the answer to problem 2, would you expect a red solution to absorb or
transmit red light? Explain.
The previous answer suggests that colored solutions absorb light of a

complementary color. Blue Cr(NO3)3 solution absorbs orange light. (Orange is the

complement of blue.) A red solution absorbs green light (the complement of red)

and transmits red light. (A yellow solution would absorb its complement, yellow.)

4. The amount of light that is absorbed by a solution is commonly expressed either


in terms of percent transmittance, as in this experiment, or in terms of
absorbance (A). Absorbance is defined as: 2  log of percent transmittance
or
A  2  log %T
Given the relationship shown in the preceding formula, convert the percent
transmittance values in Data Table 1 to absorbance values. Plot a graph of
absorbance versus wavelength. Compare and analyze the shapes of the two
curves. Might it be more useful to use transmittance values sometimes and
absorbance values at other times? Explain the advantages and disadvantages of
using these different units.
An absorption maximum appears to be sharper than its corresponding transmittance

minimum. The concentration of a substance is directly proportional to the area under

the peaks in an absorbance spectrum, but not in a transmittance spectrum. For this

reason, analytical work is most often expressed in absorbance.


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Experiment 8 Introduction to the Spectrophotometer 61


Name ___________________________ Date ___________________ Class __________________

GOING FURTHER
Develop a Hypothesis
Based on the results of this lab, propose a hypothesis about how the absorption of
light by a solution of Cr(NO3)3 varies with the concentration of Cr3 ions in solution.
The amount of light absorbed is directly proportional to the concentration of the

absorbing species in solution.

Design an Experiment
Propose an experiment to test your hypothesis. In your protocol, include a method
for determining the concentration of Cr3 ions in an unknown solution of Cr(NO3)3.
If resources are available and you have your teacher’s permission, perform the
experiment.
Measure the absorption of a series of standard solutions of chromium(III) ions at the

wavelength of an absorption maximum determined in this experiment. Construct a plot

of absorption versus concentration. Draw a best-fit line through these points. The

concentration of chromium(III) solutions in an unknown solution can be determined by

measuring the absorption and reading its concentration from the graph.

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62 Chemistry Laboratory Manual

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