prepartion of the picric acid:

1.to take phenol of 5 grams&1o ml 0f the h2so4,7ml hno3.

2.to take round bottam flask of 100 ml added 5 ml phenol andmix with h2so4 stir
it magentic stirar
A note on proportions: 0.8grams of phenol are reacted for every 1.5ml of Nitric
acid and 1ml of sulfuric acid.
25grams of powdered phenol are weighted and added to a 250ml beaker containing
31.25ml (57.81g) of concentrated sulfuric acid. The mixture is stirred and than
heated on a hotplate at 100C for 30 minutes until it becomes dark colored, indi
cating the formation of phenol-4-sulphonic acid. This is than chilled to -5C on
a water bath with salt added, becoming a cold viscous syrup, to which 47ml of ch
illed (-5C) nitric acid are added inside a fume cupboard, making sure that the m
ixture is not allowed to warm up prior to the addition of the acid. Within a few
minutes a vigorous reaction will occur which will produce large amounts of nitr
ogen dioxide, a red colored (poisonous!) gas. One must be very careful with sput
tering during this reaction.
The reaction is allowed to subside and than the mixture (which has now become a
thin, orange/yellow liquid) is heated on a water bath for one and a half hours,
with occasional shaking
When the heating is complete the mixture is allowed to cool down and 313ml of co
ld water are added, causing the Picric Acid to crystallize out of the mixture. T
he mixture is cooled to 5C so as to precipitate most of the remaining Picric aci
d, and than is quickly filtered and washed with 1200mL of cold distilled water s
o as to remove any traces of the nitration acids.
The filtrate appears as the fine yellowish mass of crystals seen to the left. Yi
eld is approximately 40grams for the 25 grams of phenol that was started out wit
h. These crystals are high purity and have all of the properties attributed to r
eagent grade Picric Acid. However, they can be purified:
Making use of Phenol's high water solubility, and the higher solubility of dini
tro and mononitroPhenol, the Picric Acid can be purified to near analytical grad
e by re-crystallization from a solvent mixture of 1 volume ethanol and 2 volumes
water, roughly 9ml of solvent being required per gram of Picric Acid.
The crystals are than removed by vacuum filtering, are vacuum dried in a dissec
tor, and form into a nearly yellow mass of mp 123C.
It is advisable to store Picric Acid wet with at least 30% water and in rubber
stoppered flasks.

This acid may be used for other synthesis, such as Ammonium Picrate (C6H2.ONH4.(
NO2)3) Ammonium picrate, also called ammonium piconitrate, Explosive D, or carba
zoate is a commonly used safety explosive which is insensitive enough to be used
in shells that penetrate armor and detonate inside it. It requires a substantia
l shock to cause it to detonate, slightly less than that required to detonate am
monium nitrate. In many ways it is much safer than picric acid, since it does no
t have the tendency to form hazardous unstable salts when placed in metal contai
ners. Vdet 7100M/s. It is made by dissolving picric acid crystals in 15 parts ho
t, steaming distilled water and adding clear ammonia in excess, allowing the exc
ess ammonia to evaporate (excess ammonia should not be used as it will form a re
d precipitate that is more sensitive than pure Ammonium Picrate. Yellow ammonium
picrate can be obtained from red picrate by recrystallizing it several times fr

om water. It also eventually changes into the yellow form if stored as a concent
rated solution. Keep this material as dry as possible). The powder remaining sho
uld be ammonium picrate. The water should not be heated, as ammonium picrate is
sensitive to heat. Vacuum distillation and open evaporation are relatively safe
ways to extract the picrate. Ammonium picrate most commonly appears as bright ye
llow crystals, and is soluble in water. These crystals should be treated with th
e care due to all shock sensitive materials. Some illegal salutes have been foun
d to contain ammonium picrate, which makes them much more hazardous. Equation go
es as follows:
NH3H2O + C6H2(NO2)3OH ---> C6H2(NO2)3ONH4 + H2O
Melts at 271C, impact sensitivity is 20% less impact than TNT, and relative streng
th is 93 - 100% TNT in the trauzl test.
ALTERNATIVE SYNTHESIS:
Picric Acid can also be produced from Phenol derivatives such as Salicylic and
Acetylsalicylic acids. The procedure is exactly the same as the one outlined abo
ve, except a smaller amount of Salicyclic (0,6grams per 1mL H2SO4 and 1,5mL HNO3
) our Acetylsalicylic (0,5g per 1mL H2SO4 and 1,5mL HNO3) acids are used. This i
s important because Acetylsalicylic acid is the active ingredient in aspirin and
can be obtained by dissolving them in hot ethanol (20 500mG pills per 100mL), f
iltering out the buffers, and allowing the pure acid to crystallize out. The rea
ction than goes:
H2SO4
C9H8O4 -------> C2H4O2 + C7H4O2
(The sulfuric acid breaks down the acetylsalicylic acid to acetic and salicylic
acid)
Or if Salicylic acid is used,
C7H4O2 + H2O ---> C6H6O + CO2
(Salicylic acid with heat source converts to carbolic acid (phenol) and carbon d
ioxide; (in presence of water from 98% H2SO4)
Or the formed phenol just sulfonates rapidly. From Phenol-4-sulfonic acid onwar
ds the reaction proceeds as outlined above.
The Nitric Acid can also be substituted by adding 15 grams Sodium Nitrate per 8
0mL H2SO4.
With the NaNO3/H2SO4 nitrating system (H2SO4 already present) without any exter
nal cooling; the phenolsulfonic acid
compound readily nitrates to a polynitro compound (2,4,6-trinitrophenol).
Yet another way of preparing picric acid is by the conversion of benzene direct
ly into picric acid in one step. This was patented by Mueller Teeters in 1948 (U
S pat. 2,455,322): 1g of mercuric nitrate is added to 60mL of 70% nitric acid wh
ich is than stirred and added to 23 mL of benzene. The mixture is than heated fo
r several hours and distilled. Benzene will distill over first, then nitrobenzen
e, and finally a mixture of dinitrobenzene and dinitrophenol will come over slow
ly. The distillation is continued until these volatile organics are removed. The
remaining residue is filtered while hot to remove any impurities and allowed to
crystallize. the picric acid that should have crystallized can be purified by r
ecrystallizing from hot water.
Picric Acid can be used alone or in the synthesis of picrate salts such as, for
example:
Potassium Picrate.