CHE 029 L:

Analytical Chemistry
Laboratory
Prepared by:
Cindy Uy, RPh, MPA
OBJECTIVE:

At the end of the activity, you will be able to:

• Demonstrate the different analytical laboratory
techniques and operations.
• Explain the application of the different analytical
laboratory technique and operations.
• Identify the presence of groups IA and IIA metals
based on selected qualitative tests.
• Identify the presence of selected trace ions based on
selected qualitative tests.
• Analyze and discuss the specific tests that correspond
to the unknown metal or trace ion.
CHE 029 L:
Analytical Chemistry Laboratory

Analytical Laboratory
Techniques and Operations
A. Laboratory Gas Burner
A. Laboratory Gas Burner
A. Laboratory Gas Burner
Side questions
What is the color of the flame when the air vents are closed?
When the air vent of a Bunsen burner is closed, air for the
combustion reaction is only coming from the area near the top of the
burner. As a result, incomplete combustion occurs, and elemental
carbon is produced. The temperature of the flame is lower, and it is a
bright yellow, candle-like flame.

Did anything happen to the surface of the test tube in this flame?
Soot was deposited onto the surface of the test tube.
Side questions
What happens to the flame size when the gas control valve is
turned?
The gas valve controls the amount of gas entering the Bunsen
burner. Allowing more gas to enter the Bunsen burner creates a larger
flame. Flame increases in a clockwise turn and flame decreases with
a counterclockwise turn.

Describe the effect on flame as the air vents were opened.

Blue in color, produces less light, small and steady, does not
produce soot, has three zones, and burns noisily.
B. LABORATORY MEASUREMENTS

I. Volume
- 50ml Graduated cylinder
- 50ml Erlenmeyer
- 50ml Beaker
II. Mass
- triple beam balance
- top-loading balance
- Analytical balance
III. Length
- Ruler
Side questions
Side questions

Which piece of glassware will give you a more accurate measure

of liquid: the graduated cylinder, the Erlenmeyer flask, or the
beaker? Explain why.
Graduated cylinder will give you accurate measure of liquid
since it has zero or lesser error in volume or % error compared to the
other volumetric glassware.
II. MEASURING MASS

Analytical balance
II. MEASURING MASS

Top-loading balance Triple beam balance

Side questions
Side questions
Two students weighed a 125-mL beaker that had a weight of
80.562 g on a calibrated top-loading balance. Each student used
their own top-loading balance, recorded three weights for the
beaker, and then determined the average. Below are the results:

Graduated cylinder will give you accurate measure of liquid

since it has zero or lesser error in volume or % error compared to the
other volumetric glassware.
Side questions
a. Find the averages.
Student A’s recorded weights for the beaker: 80.56 g
Student B’s recorded weights for the beaker: 80.56 g

b. Which set of results matches the known weight of the beaker?

• Both have the same average weights which are closest or near accurate to
the known weight.

c. Which set of results is more precise?

• Set of results from Student A is more precise than Student B because the
recorded weights are closer to one another.

d. Which student has the more reliable balance?

• Since Student A has more precise recorded weights, Student A has more
reliable balance.
C. USE OF VOLUMETRIC
WARE

Pipet/ Pipette Buret/Burette

Side questions
D. DECANTATION
Side questions

Volume of the supernatant liquid: __80__ mL

Note: Answers may vary

Is there a difference in the volume measurement between before

and after decantation of the
liquid? Explain why or why not.
Yes, because only the liquid (supernatant liquid) was
decanted to the other container resulting to a difference of the
volume or lesser volume.
E. FILTRATION
Side questions

Volume of the Filtrate: __75__ mL

Note: Answers may vary

Is there a difference in the volume measurement between before

and after filtration of the liquid?
Explain why or why not.
Yes, because the residue remained in the filter paper resulting
to a difference of the volume or lesser volume of the liquid, which is
not the filtrate.
F. HEATING OF SOLUTION
Side questions

Was the NaCl solution successfully heated under 5 minutes? YES

Note: Answers may vary

What do you think will happen to the solution if it will be heated

more than the specified time in the procedure?
The temperature would increase and would reach the boiling
point of the solution. This may result to the evaporation of the
solution.
G. HEATING OF SOLUTION
pH paper
pH meter
Side questions

Which of the solutions is acidic, Solution A or Solution B or C?

Explain why.
Solution B because the red litmus paper remained the same in
color, or the blue litmus paper turns to red.
Note: Answers may vary

Which of the solutions is basic/alkaline, Solution A or Solution B

or C? Explain why.
Solution C because the blue litmus paper remained the same in
color, or the red litmus paper turns to blue.
CHE 029 L:
Analytical Chemistry Laboratory

IDENTIFICATION TESTS FOR

SELECTED TRACE IONS AND
METALS
Alkali Metals
GROUP IA: Alkali Metals
 Soft, with relatively low melting and boiling points
 Low density (float on water)
 Li , Na , K less dense than water
 Cannot be stored under water
 Hydroxides
- white ionic crystalline solids
- deliquescent except LiOH
 Oxides
- basic and water-soluble
 Halide
- soluble in water except LiF
Solution

Precipitate
White crystalline precipitate
Present ion Test/Reagent Theoretical
result

Na Magnesium
uranyl acetate
Pale yellow /
Lemon yellow
solution

Na Lead (II) nitrate White

precipitate
Prese Test / Theoretical result
nt ion Reagent
K Lead (II)
nitrate
Yellow precipitate

K Tartaric
acid
White crystalline precipitate
Present ion Test/ Theoretical
Reagent result
Sodium White
Li carbonate precipitate

Sulfuric acid White

Li precipitate
Flame Test

Golden
Yellow
Flame

Violet / Carmine /
Purple Crimson
Flame Red
Group IIA: Alkali Earth Metals
 Can be found in the Earth’s crust
 Widely distributed in rock structure
 Hydroxides
 Magnesium and Beryllium are water-insoluble
 Calcium , Strontium and Barium give strong basic
solution
 Carbonates , Phosphates , Sulfates , and Fluorides are insoluble
Present ion Test / Reagent Theoretical Result

Ca Acetic acid + White octahedral

Oxalic acid crystal precipitate
Present Test / Reagent Theoretical result
ion

Mg Potassium oxalate White precipitate

Present Test / Theoretical Result
ion Reagent
Potassium Yellow precipitate
Ba chromate
Flame Test

Brick
red
flame

Apple
Colorless
Green
flame
Flame
Flame Test
Group IB Metals
Coinage/noble metals
Properties

• occur in the free metallic state, and are relatively easy to

recover them form their ore
• are very malleable
• used throughout historical times to make decorative
vessels and jewelry
• employed for centuries as a measure of monetary wealth
and for the fabrication of coins
Group IIB Metals
Zinc group
Procedure B: TS 1
Unknown + NH4OH , added further with of HNO3

Azure blue solution Cupric amino sulphate [ Cu(NH3)4 SO4 ]

White precipitate Zinc hydroxide [ Zn(OH)2]
Colorless solution Cadmium.Ammonium sulphate complex
[Cd (NH4)4SO4 ]
White gelatinous solution Aluminum hydroxide [Al (OH)3 ]
Bluish green Nickel hydroxide [ Ni (OH)2 ]
Pink solution Cobalt hydroxide [ Co(OH)3 ]
Reddish brown Ferric hydroxide [ Fe(OH)3]
Procedure B: TS 2
Unknown + K4Fe(CN)6

Copper or Cupric ferrocyanide

Brick red or red-brown precipitate- {Cu4[Fe(CN)6]2}
White precipitate Zinc ferrocyanide {Zn4 [ Fe(CN)6]2 }
White flocculent precipitate Cadmium ferrocyanide { Cd2Fe (CN)6 }

Prussian blue precipitate Ferri-ferrocyanide { Fe4 [ Fe(CN)6]3 }

• Unknown + HCH3COO -----------------pale green [Fe(CH3COO)2] -------------ferrous
deep-red solution [ Fe(CH3COO)3] ------ferric ion.

• Unknown + NaF + alcoholic NH4CNS ---blue-green color at conjunction of two liquids ---Cobalt

• Unknown + HCl + H2O2 --------------- blue color which fades rapidly --------- Chromium