Qualitative and Quantitative Analysis for Determination of

Formaldehyde Contents in a Given Solution.

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Formaldehyde is a gas which condenses at – 21 C. It is very soluble in
water and a 30 to 40 % aqueous solution of formaldehyde is known as formalin.
When and aqueous solution of formaldehyde is allowed to stand, or is
evaporated to dryness, an insoluble polymerized, paraformaldehyde, (HCHO)2, is
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produced. When this substance is heated to a temperature of 140 C another
insoluble product, trioxymethylene, (HCHO)3 is formed.
In order to detect formaldehyde in complex mixtures it must be removed
by distillation either with water or steam. If presents as a polymerized or
condensation product, a little dilute sulfuric acid is added to the distilling flask.

Qu a l i t a t i v e T e s t s :
In common with other aldehydes and ketones, formaldehyde gives a violet
color with Schiff’s reagent. It forms condensation compounds with
phenylhydrazine, hydroxylamine and semicarbazide, and unites directly with
ammonia, sodium bisulphate and hydrocyanic acid. The most characteristic
special tests are,

Hehner’s Test:
A little of the solution containing formaldehyde is mixed with an equal
volume of pure milk and the mixture is poured on to the surface of concentrated
sulfuric acid to which a trace of ferric chloride has been added. A violet ring is
formed after a few minutes at the junction of the two liquids.

Lyon’s Test:
Lyon modifies the above test to make it capable of detecting one part of
formaldehyde in 4,000,000. Beef peptone is used instead of milk. To two test
tubes are added 2 c.c. of the solution under examination, containing 25
milligrams of beef peptone, and the sulfuric acid to which a trace of ferric chloride
has been added is poured carefully down the side of the tubes so as to form a
layer at the bottom. One tube is allowed to stand until the color zone develops. If
the other is shaken to mix the contents a uniform violet color is produced.

Phenol Test:
A drop of dilute aqueous solution of phenol is added to the formaldehyde
solution and the mixture is poured on the surface of concentrated sulfuric acid in
a test-tube. In the presence of formaldehyde a crimson ring is formed at the
junction of the two liquids. Only a trace of phenol must be present.

Schryver’s Test:
10 c.c. of solution containing formaldehyde is added to 2 c.c. of a freshly
made and filtered 1% solution of phenylhydrazine hydrochloride. To this mixture
is added 1 c.c. of a fresh 5% solution of ferricyanide , followed by 4 c.c. of
concentrated hydrochloric acid. A brilliant Magenta color develops, which
reaches its full intensity in a few minutes and lasts for several hours.

Qu a n t i t a t i v e M e t h o d s :
These methods involve the reaction of formaldehyde with ammonia and
iodine.

Hexamethylenetetramine Method:
A measured volume of the solution, e.g. 5 c.c., is placed in stoppered
bottle and 50 c.c. of normal ammonium hydroxide solution are added. The bottle
is closed and allowed to stand for some hours. The ammonia and formaldehyde
react in accordance with the equation,

6HCHO + 4NH3 &+ ) N4 + 6H2O

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The unused ammonia is determined by the titration with normal acid. This
method is simple but its accuracy is limited.

Romijn’s Method:
10 c.c. of the formaldehyde solution is weighed in a stoppered weighing
bottle, washed into a 500 c.c. flask and diluted to the mark with distilled water, 5
c.c. of this solution is transferred to a stoppered bottle and about 30 c.c. of
normal sodium hydroxide solution added, followed by an excess of decinormal
iodine solution, that is, sufficient to give the solution a distinctly yellow color. The
interaction of iodine and formaldehyde to give hydroiodic acid and formic acid,

HCHO + I2 + H2O +,+&22+

The contents of bottle are mixed well and if necessary more iodine solution is
added. After about an hour, decinormal sulfuric acid is added and the unused
iodine determined by titration with sodium thiosulphate solution. Each c.c. of
decinormal iodine used up is equivalent to 0.0015 gram of formaldehyde.

The above test methods will help you in determining the formaldehyde contents in solution and on fabric. If you have any
suggestions and questions about any test method please do not hesitate to contact at following emails.
fisa6@hotmail.com
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fisa6@cityonline.net.pk