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Introduction
19 6. A
600 - 900 °C. However, this is not a universal temperature range. After
carbonisation the product is subjected to physical or chemical activation.
The oxidation step selectively erodes the surface, increasing the surface
area and porosity leaving the carbon surface full of surface groups having
specific affinities and a highly porous carbon skeleton with numerous capillaries,
which provide an immense internal surface area (Hashimoto et. al.).
19 6. A
There are many existing companies all over the world, which are
producing a wide range of activated carbons for a variety of gas phase and liquid
phase applications such as gas separation, gas purification, solvent recovery,
colour and odour removal and purification. Some of the internationally known
producers of PAC and GAC are Pittsburgh Activated Carbon, Union Carbide and
Westvaco (U.S.A) , Sutcliff and Speakmann, Bergwerkseverband GmbH
(Jungeten et. al.), LURGI & Degussa (Germany) and Norit Activated Carbon
(Neatherland). The raw material used by most of these producers is bituminous
and anthracite coals. The general steps involved in the GAC or PAC production
are:
19 6. A
coconut shells, saw dust and rice husk were found to be suitable for gas phase
adsorption whereas those prepared from South Arcot lignite , Kutch lignite , non
caking Samla coal, soft wood, and certain other shells showed good
decolourising properties. These carbons had comparatively lower surface area
than the commercially available carbons but their decolourising power was
comparable. Naidu et.al. at National Environmental Engineering Research
Institute, Nagpur, obtained activated carbon from coke fine having N 2 -BET
surface area of 526 m 2 /g and bulk density of 0.660 g/cm . It showed a good
decolourising power but required much higher contact time for maximum removal
of organic carbon from wastewater. Srivastava and co-workers prepared cheap
carbonaceous adsorbent material from fertiliser waste and the product was found
to have a very good adsorption potential form substituted phenols.
19 6. A
structure similar to graphite are formed. The X-ray spectrographs interpreted
these structures as micro crystallites consisting of fused hexagonal rings of
carbon atoms (Wolff W. F.). The diameter of the planes making up the micro
crystallite is estimated to be 150 A0 and the distance between micro crystallites
ranges from 20-50 °A (Garten et. al.).
Chemical Structure
Surface Chemistry
The Fourier-Transform Infrared infrared spectrophotometric analysis
shows the presence of many functional groups on the surface of activated
carbon. They are carboxyl groups, phenolic hydroxyl groups, quinone type
carbonyl groups, normal lactones, fluorescien type lactones, cyclic peroxides,
19 6. A
carboxylic acid, anhydrides etc. Observations of (Mattson et. a!.) the internal
reflectance spectroscopic examination of activated sugar carbons, suggested the
presence of a pair of adjacent carboxylic acid groups. But according to Gorten
and Weiss, no acidic group of such strength as a carboxylic group is present on
the surface of activated carbon. They proposed the presence of lactones of the
fluorescien type to explain the reaction of diazomethane to form hydrolyzable
esters.
Preservation of Carbon
Air sample at a flow rate of 200 ml/min is passed through a glass tube
packed with activated charcoal. The organic vapours were absorbed onto the
charcoal. The collected vapours are desorbed using carbon disulfide (CS2) and
19 6. A
SEM of F-300 Grade Activated Carbon
183.1
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19 6. A
RSIC,NAGPUR
SAMPLE CODE - F300
Thu Sep 26 16!l7:29 1996
oo Number of (ample scans: 32
u> Number of background scans: 32
Resolution: 4.000
Sample gain: 1.0
Mirror velocity: 0.6329
Aperture: 69.08
Detector: DTGS KBr
Beamsplitter! KBr
Source: IR
88
87
Wavenumbers (cm-1)
The Organic Vapour Sampler model Envirotech APM 850 used for
collecting the samples is described below.
Sampling Assembly:
Activated charcoal tube
The charcoal tube is made of a glass with both ends flame sealed, 70 mm
long with an outside diameter of 6 mm & an inside diameter of 4 mm containing
two sections of 0.35 mm to 0.85 mm of activated charcoal. The adsorbing
section contains 100 mg of charcoal & the back up section 50-mg, specially
designed for large loading capacity of Volatile Organic Compounds. Provided two
sections separated by intent glass tape plugs. Glass beads are packed before
front section of the tube for proper distribution of air, entering into the tube.
This tube has one inlet and two outlets. While sampling inlet is attached to
filter adopter and outlet is connected to suction pump through orifice controlled
Teflon nozzle while other outlet connected to 'u' tube manometer through
184
provided nozzles for pressure measurement. All connections of the tube are
done with the help of silicon tubes. Two sections provided in this tube can be
separated out by removing springs for desorption/extraction of adsorbed organic
compounds separately. Ground glass joints male and female type have been
provided to facilitate assembling and dissembling of the tube.
Rubber caps need to be used for sealing all three opening of the tubes
after sampling and regeneration.
The pressure drop across the tube shall not exceed 3 Kpa (25 mm Hg) at
the flow rate of 200 ml/min recommended for sampling.
Extraction Assembly :-
Desorption Bulb :
A round bottom glass flask of 25-ml capacity provided with ground glass
connector suitable to fit into both sections of the charcoal tube.
Syringes :
19 6. A
Sample Analysis
19 6. A
Equivalence of Gas Chromatograph Stationary Phases
SP-2330 and SP-1000 columns can also be used for the determination of
Volatile Organic Compounds. The suitability of the column shall be verified by
testing with 2 or more columns of dissimilar packing to ensure the absence of
interferences.
Sampling
Connect mains cable in the socket provided on the rear side of the
sampler. Remove rubber caps of Activated Charcoal tube and fit it in the
"hydrocarbon nozzle" with the help of silicon tube. Silicon tube of nozzle marked
as "pressure" is connected to 2 nd connection of the tube. Take carbon monoxide
or other gases indicator tube and break glass seal from both end of the tube and
fit it in the nozzle marked with carbon monoxide. Use metallic folding stand for
holding the tubes straight. Take initial reading of the time totalizer. Now switch on
the power supply and see that indicator ON/OFF switch glows. Switch 'ON' the
equipment and check flow in both the tubes with the help of rotameter by
connecting silicon tube of nozzle marked with the flow to the tip of connected
hydrocarbon/ carbon monoxide tube. Record flow reading on the note sheet.
Flow is maintained constant in the equipment with the help of needle type
orifices. Generally flow rate 100 to 200 ml/min is maintained in both the tubes.
Higher flows can also be maintained by choosing different size of needle orifices.
After noting the flow, attach filter adopter loaded with filter on each tube to avoid
entry of particulates in the tubes, which may increase pressure drop and reduce
19 6. A
the adsorption efficiency beyond acceptable limits. Sampling frequency may
vary from 3-8 hrs at traffic junctions/sampling site depending on vehicular
density/peak hours. While operating if no flow is observed check needle fitted in
the Teflon nozzle. It is expected that needle may be chocked, replace needle in
such cases. After operation for desired period check the flow reading and switch
off the suction pump and note the final time totalizer reading. Now take out the
charcoal tube and seal all three openings with the help of supplied plugs after
marking sampling date, time and location on sealed tube. Now this tube needs to
be sent to lab for analysis. Ensure storing of tube at low temperature (sub
ambient temperature) to avoid migration of sorbed compounds from one section
to another. CO tube is removed and concentration of CO is noted by comparing
the colour with provided chart.
Extraction
Open the sealed exposed Activated charcoal tube and separate the
sampling tube's back up section and front section of modular activated charcoal
tube. Extract sampled organic compounds separately from front section &
backup section. Desorption need to be carried out using desorption bulbs. Take
10 ml of AR Grade CS 2 or suitable elutant as prescribed in standard analysis
method in desorption bulb. Remove the glass tape from sampling tube and
attach with desorption bulb with the help of provided male-female glass
connector. Extraction is carried out by ultrasonication or it can be carried by
shaking. The desorption bulb containing 10 ml elutant CS 2 & exposed activated
charcoal is sonicated for 15 min. Repeat the same procedure for the backup
section using different desorption bulb. Filter extracted solvent if particles are
visible after desorption use 25-mm diameter glass fibre filter & provided funnel
and sample vial. Use only transparent elutant for injecting in the Gas
Chromatograph.
19 6. A
Analysis
The transparent elutant obtained after extraction was used for gas
chromatograph analysis.
1 pi of Mix standard (BTX = 100 ng/pl) was injected into the Gas
Chromatograph. Replicates of fixed volume of Mix standard was introduced to
get a chromatograph for evaluating precision.
Mix standard was diluted with carbon disulphide (CS2) in 1:1 proportion
and injected under the same GC condition in triplicate to get reproducibility.
In a similar way sample and spiked sample was also injected to get a
repeatable peak pattern.
19 6. A
1
Area = /2 x h x W (mm2)
h Height of a peak
W = Width of peak at half height
In case of very narrow or sharp peaks only height was considered and
taken as area of a peak.
19 6. A
Table 1
GC response for standard solution (100 ng/pl)
19 6. A
GC response for Standard + Sample (1.1)
19 6. A
Precautions :
1) During the sampling if the pressure drop increases more than 25 mm Hg,
check the activated charcoal tube packing, loosen the glass beads and glass
tube plug.
3) After the extraction of the sample, the concentrated tubes (sample tubes)
should be sealed properly with Aluminium foil to keep the sample volume
constant.
4) Extraction and analysis of the sample should be done on the same day.
5) If the samples are not to be analysed within 8 hrs, store tem in a sealed metal
or glass container placed either in dry ice or in a freezer maintained at -20°C,
in order to minimize migration of analyte from one section of the tube to
another.
19 6. A
References :
Faust, S.D. and Aly, O.M.; in "Adsorption processes for water treatment" pp.
168-170, Butterworth Publishers (1987).
Juntgen H., Klein Jurgen, Knoblauch K., Schroten Hans-Jurgen, and Schulze
Joachim in Chemistry of Utilization, llnd Supplementary Volume, Chapter -30,
Editor. Elliott Martin A.; 2144-2145 (1981).
19 6. A
19 6. A
Choudhury, S.B., Banerjee, D.K., Dutta A.C., Mazumdar S., Ray A.K. and
Prasad M.;
Srivastava S.K. and Tyagi, Renu ; Fresenius Environ. Bull., 3(1), 12-17
(1994)
Walker, P.L., Jr., "Carbon An Old But New Material", Am. Scientist, 50, 250
(1962)
Garten, V.A. and Weiss, D.E., Rev. Pure Appl. Chem., 7, p 69, (1957)
Yenkie, M.K.N, and Natarajan, G.S.; Sep. Sci. & Technol. 28(5), 1177-1190
(1993)
Mattson, J.S., Mark, H.B. Jr., Malbin, M.D., Weber, W.J. Jr. and Crittenden,
J.C., J. Colloid Interface Sci., 31, 116 (1969)
Coughlin, R.W., Ezra, F.S. and Tan, R.N. ; J Colloid Interface Sci., 28, 386
(1968).
Organic emissions profile for a light duty diesel vehicle. Atmo. Env. Vol.33
(Nov 1998) No.5, pg. No. 797
19 6. A
ORGANIC VAPOUR SAMPLER
196.1
NO. Details
1QC
SAMPLE VIAL
FILTER
ADOPTER
Details Details
VQCs :-
1. BENZENE
2. T O L U E N E
3. p - X Y L E N E
A. tn-XYLENE
5. o - X Y L E N E
FlG,2(g):CHR0MAT0GRAM FOR MIX STANDARD FlG.2 (b): C HROMATOGR AM FOR MIX STANDARD-*- SOLVENT(1-1)
F1G.2: (C):CHR0MAT0GRAM FOR AIR SAMPLE FIG.2 ( d) '• C H ROM ATOGRA M FOR STANDARD* SAM PL E( 1:1)
19 6. A