Name: RAFAEL, DUNE VIENIS KAREN N.

Year &
Section: BS-Pharmacy 4A
Date Performed: November 20, 2009 Rating:
____________________

Activity No. 3
PHENOL

Objectives:
1. To detect the presence of phenol by performing Millon’s test, bromine water
test, ferric chloride test, hypochlorite test and Melzer’s benzaldehyde test,
2. To understand the principles behind each test, and
3. Interpret the results after performing each method of detection.

Data:
Tests Observation/Results
1. Millon’s Test Actual: From white to pink with white precipitate
Ideal (+): The solution gives a distinct red color of
diluted 1:100,000 (Warren, 1921).
Blank (-): The solution gives no distinct red color.

2. Bromine Water Actual: No changes were observed in the bromine

Test water.
Ideal (+): Excess of the bromine water produces a
yellowish white, crystalline precipitate (Warren,
1921).
Blank (-): The excess of the bromine water produces
no yellowish white, crystalline precipitate.
3. Ferric chloride Actual: After ferric chloride was added, the solution
Test changed its color to yellow. Upon the addition of
sulfuric acid, the solution turned its color from black
to white.
Ideal (+): Very dilute ferric chloride solution added
drop by drip, imparts a blue-violet color to aqueous
carbolic acid (phenol) solutions. Addition of dilute
sulfuric acid changes this color to yellow(Warren,
1921).
Blank (-): No changes are observed/no characteristic
change of color from blue-violet to yellow is
observed.
 4. Hypochlorite Test Actual: Dark blue precipitate was formed from a
brownish solution.
Ideal (+): The solution gives a blue color upon gentle
warming. Very dilute carbolic acid (phenol) solutions
after some time give only a green to blue-green color
(Warren, 1921).
Blank (-): The solution gave no characteristic change
of color to blue or green to blue-green color.

5. H. Melzer’s Actual: After the addition of 2 mL sulfuric acid, the

Banzaldehyde Test
Data Analysis
solution turned to orange; when 10 mL of distilled
water was added, three (3) layers were formed in the
solution:
• Upper layer – Colorless
• Middle layer – Orange
• Lower layer – Orange
After the addition of Potassium hydroxide (KOH), the
color of the three layers changed:
• Upper layer – Lavender
• Middle – Colorless
• Lower – Light Orange
Ideal (+): The mixture, at first yellowish brown, will
become dark red. At the same time a red resinous
substance will appear unless the solution is too dilute.
When 10 mL (cc) of cold water and enough potassium
hydroxide solution is added, it gives a distinct violet-
blue color. To obtain this coloring-matter, the solution
should be acidified, extracted with ether and
evaporate the solvent (Warren, 1921).
Blank (-): In absence of phenol concentrated sulfuric
acid produces a dark brown color with benzaldehyde.
Alkalies dissolve the pure crystals withour color but, if
these solutions are exposed to air, oxidation takes
place and a red or red-violet color appears. Probably,
benzaurine, dihydroxy-triphenyl-carbinol, is first
formed. This compound is a brick red crystalline
powder soluble in akalies with a violet color(Warren,
1921).

Millon’s Test
Though a very delicate test, it is not characteristic of carbolic acid, because
several other aromatic compounds behave similarly to carbolic acid. This is true
derivatives of mon-acid phenols like the three cresols, salicylic acid, para-hydroxy-
benzoic acid, para-hydroxy-phenyl-proprionic acid and tyrosine.

Bromine Water Test

Excess of bromine water produces a yellowish white, crystalline precipitate,
even with very dilute carbolic acid solutions. It is a very delicate test for carbolic
acid. Phenol dilutes 1:50,000 yields, after some time, a precipitate made up in part
of well-formed crystals.

Ferric Chloride Test

Very dilute ferric chloride solution, added drop by drop, imparts a blue-violet
color to aqueous carbolic acid solutions. Addition of dilute hydrochloric or sulfuric
acid changes this color to yellow. This test is not as delicate as Millon’s test and
Bromine Water test. It is entirely negative in presence of mineral acids. The limit of
delicacy is about 1:1000.

Hypochlorite Test
Gentle warming will produce a blue color. Very dilute carbolic acid solutions
after some time give only a green to blue-green color. F.A. Fluckiger (1879) allows
bromine vapor to come into contact with the phenol solution which has been mixed
with a little ammonium hydroxide solution in a porcelain dish.

H. Melzer’s Benzaldehyde Test

The mixture, at first yellowish brown, will become dark red. At the same time
a red resinous substance will appear, unless the solution is too dilute. When cold
water is water is added (10 mL/cc) and enough potassium hydroxide solution gives
a distinct alkaline reaction. If carbolic acid is present, a violet-blue color will appear.
In absence of phenol concentrated sulfuric acid produces a dark brown color with
benzaldehyde.

Answers to Questions:

1. List down several products and the level of phenols found in each (ppb-parts
per billion):

• Salicylic acid
• Para-hydroxy-benzoic acid
• Para-hydroxy-phenyl-acetic acid
• Aniline
• Para-hydroxy-phenyl-proprionic acid

1. How are phenol levels tested in wastewater?

Phenol levels in waste water are tested by high-performance liquid

chromatography with chemiluminescence detection(Huang, 2005).

Conclusion
Concentrated carbolic acid coagulates and destroys the constituents of the
human body, especially proteins and protoplasmic structures. It has therefore a
very strong caustic action. But its action is not merely local, for after absorption it
shows an affinity particularly for the central nervous system, brain and spinal cord.
In man, the period of stimulation is very slow in appearing. In chronic poisoning,
after repeated small doses of carbolic acid, degeneration of the kidneys and liver is
a result of absorption. With these basic facts about carbolic acid or phenol
intoxication, it poses a great concern for pharmacists on how to manage such
cases. It is important that as a future pharmacist that I should be knowledgeable
about this subject matter. Through this activity, I conclude that carbolic acid could
be detected by conducting Millon’s test, Bromine Water test, Ferric chloride test,
Hypochlorite test and H. Melzer’s Benzaldehyde test.

Bibliography
Huang, C., Zhou, G., Peng, H., & Gao, Z. (2005). Simultaneous determination of N,N-
dimethylaniline and phenol in wastewater by high-performance liquid
chromatography with chemiluminescence detection. Retrieved November 27, 2009,
from Cat.inist.fr: http://cat.inist.fr/?aModele=afficheN&cpsidt=16781950

Warren, W. H. (1921). Laboratory Manual for the Detection of Poisons and Powerful
Drugs. New Jersey: Read Books.