BENZENE

Method Gas Chromatograph (IS: 5182, Part XI, 1982)

Principle
A measured volume of air is drawn through silica gel by means of a personal sampler. Any
benzene vapour present, in the sampled air is observed. The silica gel is shaken with
isopropyl alcohol, which disrobes benzene quantitatively. The components of alcohol layer
are separated by gas liquid chromatography ove polypropylene glycol (PPG) 400 using
flame ionization detection.
Apparatus
Gas Chromatograph: - Any suitable gas chromatograph with flame ionization detector.
Column Conditions: - One set of suitable column conditions is given below: Length x ID
:
3.6 m x 3mm
Stationary phase
:
PPG-400
Solid support
:
Chromosorb W acid washed
(180 m 250 m)
Stationary phase/support
:
0.25
Detector
:
Flame Ionization Detector (FID)
Column temperature
:
750 C
Injection part temperature
:
750 C
Carrier gas
:
Nitrogen (Hydrogen may also be used)
31/h
Sample injection
:
10 l
Lower detection limit
:
0.1 ml (vapour)/m3 (0.3 mg/m3)
Personal Sampler: - Consisting of portable, battery powered, intrinsically safe pump,
with adsorption tube and a flow meter in the range of 0.5 to 1.5 l/m. Any other
suitable portable flame proof suction device with absorption tube and flow meter
capable of measuring at a sampling rate in the range of 0.5 to 1.5 l/m may also be
used.

Silica Gel: - 300 to 600 m size, chromatography grade. Active for at least 16 hours at
190 50 C, preferably in a vacuum oven. Allow to cool in a desiccator without
desiccant. Do not open the desiccator until the gel is to be used.
Benzene: - Analytical reagent grade
Iso-propyl Alcohol (IPA): - Free from benzene, analytical reagent grade.
Sample
It is recommended that such quantity of air is used that approximately 50 g of benzene
vapor is absorbed on the silica gel. For a benzene concentration of 1 ml (vapor)/m3
the volume of air to be passed through is approximately 20 liters. Normally, a
sample volume of 20 to 30 litres is sufficient. However, while determining extremely
low concentrations, up to 70 litres of air may be sampled if the ambient temperature
is below 260 C and relative humidity less than 70 %. Beyand these limits the
humidity of air may interfere as water absorbed on the silica gel may displace
trapped benzene. This displacement starts interfering when the silica gel has
absorbed 0.15-g water per gram of silica gel. Therefore, 0.12 g water per gram of
silica gel may be taken as an allowable maximum and the maximum sample sized
may be calculated as follows: V = 12 x 103 M / HC
Where,
V = Maximum allowable volume in litres of air sample
M = Mass in g of silica gel used
H = Relative humidity of the atmosphere, percent
C = Concentration of water vapor in air saturated with water vapor at the temperature
of test and 101.3 kPa, mg/l
Calibration
Prepare five calibrating solutions of benzene in iso-propyl alcohol containing 15, 25, 125
and 500 mg/l benzene. Pipette 20 ml of each solution into separate stoppered bottles
containing 10 g of silica gel, shake for two minutes and allow settling for at least five
minutes.

Analyze alcohol layer on gas chromatograph and plot the benzene peak height/area
against concentration of benzene in g/20 ml.
Procedure
Fill the adsorption tube with 5-15 g of silica gel. Mount the tube in the holder, read the
timer and start the pump. Pass requisite volume of air sample through the tube at
rate not exceeding 1.5 l/m. Transfer the silica gel to a 50-ml bottle. Add 20 ml isopropyl alcohol, stopper, shake for two minutes and allow to settle for at lest five
minutes. Analyze the alcohol layer for benzene using conditions identical to those
for calibration. Measure the area of benezene peak. Read from calibration graph the
concentration of benzene in iso-propyl alcohol in micro grams per 20 ml.
Calculation
Calculate the benzene vapor content per cubic meter of air at 00 C and 101.3 kPa (1.013
mbar, 760 mercury) by means of any of the following equations: Benzene, mg/m3

= 101.34 (273 + T)
273 p Ft

Benzene, ml (vapor)/m3 = 101.3 A (273 + T)

348 x 273 p Ft
Where,
A = Concentration of benzene in IPA, read from the calibration curve, g/20 ml
T = Temperature in 00 C of the air
P = Atmospheric in kPa pressure
F = Flow rate in 1/min during sampling and
T = Time in minutes of sampling
Note: - In case barometers calibrated in pascals are not available, express pressure in
milibar or millimeters of mercury and replace the factor 101.3 by 1013 or 760, respectively.