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    Filter Extraction For Heavy Metals and Benzo (A) Pyrene: DR Rajendra Prasad

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    Filter Extraction For Heavy Metals and Benzo (A) Pyrene: DR Rajendra Prasad

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    Research material and environment related resource is available free on http://ecrd.in/, please visit to get the best resource on web for environment training. http://learntech.in/ has developed this environment learning portal, you can visit the Leaders in E Learning development in India to explore more ideas on learning.

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    Research material and environment related resource is available free on http://ecrd.in/, please visit to get the best resource on web for environment training. http://learntech.in/ has developed this environment learning portal, you can visit the Leaders in E Learning development in India to explore more ideas on learning.

    Copyright:

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    59 views14 pages

    Filter Extraction For Heavy Metals and Benzo (A) Pyrene: DR Rajendra Prasad

    Uploaded by

    ECRD
    Research material and environment related resource is available free on http://ecrd.in/, please visit to get the best resource on web for environment training. http://learntech.in/ has developed this environment learning portal, you can visit the Leaders in E Learning development in India to explore more ideas on learning.

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    of 14

    Filter Extraction For

    Heavy Metals and


    Benzo(a)pyrene
    Dr Rajendra Prasad
    <[email protected]>
    Ambient Air Quality Standards of Notified Parameters and
    Range of Analysis in Methods Recommended

    S.No. Parameters Applicable Standard Range of the Analytical Methods


    1. SO2 50 g/m3 (6 g/m3 to 1025 g/m3)
    2 NO2 40 g/m3 (9 g/m3 to 900 g/m3)
    3 NH3 100 g/m3 (20 g/m3 to 700 g/m3)
    4 O3 100 g/m3 (20 g/m3 to 20,005 g/m3)
    5 Pb 0.5 g/m3 (0.01 g/m3 to 2.5 g/m3)
    6 Ni 20 ng/m3 (5 ng/m3 to 1000 ng/m3)
    7 As 6 ng/m3 (100 ng/m3 to 1500 ng/m3)for 10 m3 sample
    8 CO 2000 g/m3 (1144 g/m3 to 114400 g/m3)
    9 Benzene 5 g/m3 (1g/m3to10mg/m3)
    10 Benzo(a)pyrene 1ng/m3 (3 ng in extracted sample LDL)
    Benzene Analysis
     Capilliary Column 624 having coating Cynopropyl Pheylpolysiloxane
    length 30m, ID-0.25mm coating thickness 1.4 mm – 1No.
     CS2 Benzene free – 500ML
     Benzene (Chromatography Grade) – 250ml
     We will be sending ultrasonically extracted samples for analysis of
    Benzene at your set up for its analysis.
     We suggest following conditions to be set on GC while analysis
    A
     N2 gas flow – 30ml/min
     H2 gas flow – 30ml/min
     Air flow - 300ml/min
    B. We need to inject at least 5ul sample or 10 ul sample
    C. Set injection port temp – 250 oC
    D Set FID Temp - 300oC
    Benzo(a)pyrene
     Four circles of 3.6cm diameter are cut from exposed filters
     These are kept in 30ml micro Soxhlet apparatus on glass wool (to prevent
    carbon particles going in to solvent)
     Put 30ml fluorescence free Cylohexane
     Extracted solvent is evaporated to 2ml in current of nitrogen
     This 2ml extract is send to lab for analysis of Benzo(a)pyrene
     Analysis is done after passing extract through a chromatographic column
    12cm long prepared by slurring activated alumina with toluene. Elution is
    carried out using toluene. Collected elutant is air evaporated and final
    volume is made as 5ml in toluene
     Fluorescence emission measurement of peak heights are now made at 307
    & 387nm using Fluorimeter
     Blank filter paper is also run as above
     Standard is analyzed and peak heights are obtained for various range of
    concentration and a calibration graph is prepared.
     Obtained peak height of sample is used to find out concentration of
    Benzo(a)pyrene with the help of calibration curve.

    Area taken for analysis 40.7 cm2 Total Exposed Area of filter 406.5cm2
    Area factor for multiplication 406.5/40.7 = 9.99 say 10
    Solvent Extraction of Benzo(a)pyrene
    followed by HPLC/GC analysis

    Soxhlet Apparatus GC, Capillary Column


    Condenser

    Water Out

    Water In

    Sample
    s

    Flask

    Solvent
    Heavy Metals Pb,Ni and As in Particulates Collected

    on Glass Micro Fiber Filter Paper From Ambient Air

     It is desirable to take 24 hrs sample of Particulates on 8 x10’’ Filter Paper


     Extraction of filter paper:
     Take a strip of exposed filter as 2.5 x 17.5cm for urban sample 5.0 x 17.5cm for rural
    sample
     This strip need to be ashed in low temperature asher (If not available leave the filter in
    oven at 250oC for 1hr at least
     Transfer ashed filter in extraction tube
     Take 125ML Erlenmeyer flask with 24/40 female Joint . Put 8mL concentrated HCL and
    32ML 40% HNO3. Attach this flask to extraction tube and connect a Allihn condensor
    and reflux it for 3hrs
     Now remove the extraction tube condenser. Extracted liquid is evaporated on hot plate
    till volume is reduced to about 2ML
     Leave the contents overnight for cooling .
     Now transfer the contents to 15ML centrifuge (2000 rpm) tube with 3 washing by 5-10
    drops by 1:20HCI for 30 minutes
     Transfer supernant liquid in the polypropylene tube with cap and send to AAS for
    analysis.
     Dilution of this sample may be done using 1:10 HCI as per requirements.
     For analysis of Arsenic Hydride Converter is required with AAS fitted with Graphite
    Furnace..
    Analysis of Arsenic in particulates
    Collected from Ambient Air
     Range: Concentration as low as 0.1 g/m3 or 100ng/mg can be
    measured in 10m3 sampled air
     Since limit of arsenic is 6ng/m3 it is difficult to analyzed the
    arsenic concentration in such low concentration for small
    duration sample.
     For Arsenic sampling duration need to be 24hrs 8hrs sample
    must not be analyzed.
     Arsenic present in particulates as Arsenic Oxide and arsenate
     Particulate are dissolved in HCI. Extract is made to react with KI
    and SnCI2. This give trivalent arsenic.
     This trivalent Arsenic is reduced to Arsine (ASH3) by Zinc in
    acidic solution in Gutzeitt generator. This Arsine is passed
    through H2S scrubber which contain glass wool impregnated with
    lead acetate and then into absorber containing silver diethyl
    thiocarbamate dissolved in pyridine. Here reaction take place
    and red soluble complex is formed which is directly proportion to
    the Arsenic. Intensity of this colour is measured at 535nm.
    Analysis of Arsenic in particulates
    Collected from Ambient Air
     Extraction of Filter
     Take filter strip 2.5cm x 17.5cm in flask. + 6N HCI digest
    90.95oC on water bath for 1hr. Cool and add 6N NaOH.
    Now add 1ML KI and 8 drops of stanus chloride and mix.
    Allow 15 minute for reduction of Arsenic in Trivalent state.
    Cool solution in ice bath at 4oC Impregnate glass wool with
    lead acetate. 15ML lead acetate is good for 4cm length of
    glass wool.
     Take 3ML of silver diethyl thiocarbamate solution in
    absorber tube. Add 3gm of Zinc to the flask and immediate
    connect to scrubber-absorber assembly allow 90minute for
    complete evolution of Arisen gas. Color will form which is
    directly proportional to the concentration of Arsenic. Blank
    should also be handled in the also above. Read
    absorbance against blank at 535nm.
    Ozone
     Range 0.01 to 10PPM
     Absorbing Solution:
     13.6gmKH2PO4+14.2gm Na2HPO4 +10gm KI make up
    contents up to 1000cc by distilled water. Adjust pH 6.8 .
    Leave solution in dark place overnight before use.
     I2 Stock:
     0.025M(0.05N)Dissolve 16gm KI and 3.173gm of I2 and
    make up this by distilled water up to 500ML.
     I2 working 0.001M
     Take 4ML of 0.025 M I2 in 100mL flask and dilute it with
    absorbing solution up to the mark
    Calibration Curve Preparation
     Take 4.09 mL 0.001 M I2 solution and dilute it up to
    100mL using absorbing solution this will be
    1ulO3/mL
     Take 10ML flask and put 1mL 2mL 3mL 5mL 8mL
    10mL solution and make up to 10mL using
    absorbing solution
     Read absorbance at 352nm against distilled water
    and plot the calibration curve
     Analysis
     Read absorbance of exposed sample against blank and
    find out concentration of 03ul/mL
    Making of SO2 Trap for Ozone
    sampling
     Take glass micro fiber filter 8*10 inches and cut a
    piece of 400 cm2
     Drop 15 ml aqueous solution of 2.5gm chromium
    trioxide mixed with 0.7 ml conc. H2SO4
     Dry this in oven at 90 degrees for 1 hour
     Quickly cut circles of 6mm dia and store in airtight
    glass bottle.
     Fill these circles in trap after filling glass fibers just
    before sampling.
    CALCULATION
    cal factor x 48 x 1000 x 25
     O3 (ug/m3) = ---------------------------
    Vol. of air (lit) x 24.45 x 10
     Thank you

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