Air Pollution Monitoring

Methods of Measurement – Main Requirements

Rakesh Agarwal

Envirotech Instruments Pvt. Ltd.
envirotech@vsnl.com

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National Ambient Air Quality Standards
POLLUTANT TIME WEIGHTED AVERAGE INDUSTRIAL RES. RURAL OTHER METHOD

PM10 ug/m3 PM2.5 ug/m3
LEAD ug/m3 ARSENIC ng/m3 NICKEL ng/m3

ANNUAL 24 HOUR ANNUAL 24 HOUR
ANNUAL 24 HOUR

50 80 40 60
05 1.0 06 20
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GRAVIMETRIC TEOM BETA-ATTN. GRAVIMETRIC TEOM BETA-ATTN
ACID EXTRACTION & AAS

Definitions of PM10 & PM2.5

Inhalable particles enter the respiratory tract. Thoracic particles travel past the larynx & reach the gas exchange region of the lungs. PM10 Particle size distribution closely resembles the thoracic distribution with a D50 at 10m. PM2.5 size distribution with D50 at 2.5m AD It is important to note that particle sizes referred above are NOT physical particle sizes but Aerodynamic Diameters.

• Aerodynamic Diameter is defined as the diameter of a spherical particle
with a settling velocity equal to that of the particle in question, but with a density of 1g/cm3.
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PM10
Standard Annual 60 g/m3 24 Hr. 100 g/m3

BIS 5182(Part-23):2006
 Cyclonic Separation of Coarse Fraction  Flow rate 1m3/min  Flow Control with Auto Shut off if flow rate drops below 0.85m3/min.

 Gravimetric determination done by finding out mass of PM10 dust accumulated on filter paper and dividing it by volume of air passed in sampling period.  So far no BIS method available for Impactor based low flow rate Instruments
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PM10
 Trace Metals can be analyzed from the 8x10 GF/A Filter:
 Lead  Arsenic  Nickel

 In new standard sampling flow rate has not been specified thus sampling can be done at high flow rate (1.0 m3/min) or at low flow rate 1.0 m3/hr.  LOWER Flow rate instrument implies need for more accurate Balance.

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Envirotech APM 460NLDX
Main Features:
•Flow rate automatically controlled to compensate for Dust loading on the filter. •Auto Shut-off if flow rate drops below 0.85m3/min. •Only instrument that conforms to BIS •Low Noise and Brushless Blower

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PM2.5
 Standard Annual 40 g/m3 24 Hr. 60 g/m3 Concern for PM2.5 originated in 1994 – 95 as a consequence of Scientific studies sponsored by USEPA that correlated health impact with Air Pollution. There is no standard method prescribed so far by BIS or CPCB. USEPA standardized and published a design of PM2.5 Impactor at a flow rate of 1m3/hr. Most instruments are based on this design. Since dust sample is collected at low flow rate a sensitive balance accurate up to 1g may be needed to weigh collected dust. Special effort needed to get reliable PM2.5 values:
    Filter Handling & Conditioning Weighment Static Charge Volatility of PM2.5
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   

Monitoring Fine Particulates (PM2.5) in Ambient Air
• Precautions
– Minimize exposure of the filters to open air. Keep them covered in the filter carriers provided. – The membrane is fragile take care to handle the filter only on its edge using blunt tweezers. – Weigh the filters on a micro-balance with a resolution of at least 0.01mg. – Re-weigh the filters a few times to confirm repeatability of the weight. Reject the readings if they vary by more than 0.1mg. – EPA recommends that a Blank Filter be processed to keep track of drifts and artifacts.
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Monitoring of PM2.5 Procedure & Precautions
• Preparation of FILTER
– The Membrane is fragile – handle the filters only with a blunt tweezer and touch ONLY the support ring. Assign filter identification numbers. – Establish a system of filter batch numbers & lookout for fakes. – Equilibrate each filter for at least 24 hrs. in a controlled environment having:
• Temperature 15 - 30 degrees C • Humidity 20-45%

– Weigh each filter & record its initial weight. A balance with 0.01mg accuracy is required.
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Monitoring of PM2.5 Procedure & Precautions
• Preparation of WINS IMPACTOR
– Remove the WINS IMPACTOR assembly from the instrument and open its two halves by unscrewing them. – Open the Impactor Well and clean oil residues using a clean tissue. – Place a fresh 37mm dia. GF/A filter in the well cavity. – Pour a few drops of Silicone Oil to wet the filter surface – about 1ml. Of oil is sufficient. Note: this is a special low vapour pressure oil. – Re-assemble the well cover and WINS Impactor assembly.
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Monitoring of PM2.5 Procedure & Precautions
• Installation of Filter in Cassette
– The membrane filter is loaded in a Filter Cassette for ease in handling and protection. This task should be performed in a clean room or lab. – Open the filter cassette – the top half is just press fitted over the bottom part. – Use a blunt tweezer to place a pre-weighed membrane filter over the backing screen of the cassette. – Place the cassette cover over filter and gently press it into place. – Place the cassette in the carrier box provided with the instrument.
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Monitoring Particulates in Ambient Air - Procedure & Precautions
• Operation
– Install pre-weighed filter, record Dry Gas-Meter reading and turn ON the sampler flow. – Allow it to establish normal running temperature and check flow rate. – If sampling rate is outside acceptable limits check for leaks, filter displacement etc. – Record sample information - site location, Sample date, Filter ID No. – On completion of sampling period record Dry GasMeter reading. – Carefully remove the filter cassette and store in an appropriate carrier.

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Monitoring Particulates in Ambient Air - Procedure & Precautions
• Post Operation
– Work out the average flow rate. – Record any factors such as meteorological conditions, construction activity, dust storm etc. that might affect your results. – Transport the filter to the equilibrating environment as soon as possible. – Equilibrate the filter under the same conditions for at least 24 hours. – Immediately after equilibration weigh and record the post sampling filter weight along with filter ID.
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Heavy Metals (Pb, As &Ni)
• • • • Extract contents of Filter Paper. Use EPM 2000 Filter to avoid Matrix effects. Analyze Extract with AAS Only High Volume Samplers can provide sufficient sample for Analysis

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Extraction of Filters for Heavy Metal Analysis
– 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 – 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 – Extracted liquid is evaporated on hot plate till volume is reduced to 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..
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Benzo(a)pyrene
Applicable standard 1 ng/m3

 Majority of Polcyclic Aromatic Hydrocarbons (long chain and high molecular weight compounds) found adhered with particulates. Thus filter dust can be extracted using Soxhlet Apparatus for 6-8 hrs and extract analyzed on HPLC for PAH compounds including Benzo(a)pyrene.  BIS 5182 (part12) 2004 gives detailed procedure.  Sample should be wrapped in Al-foil and stored in a refrigerator. Exposure to light can cause photo-oxidation.  Usually a Sampler with High Flow rate – 1m3/min can provide a sufficient sample for analysis.

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Sulfur Dioxide (SO2)
Standard Annual 50 g/m3 24 Hr. - 80 g/m3

West & Gaeke Method – BIS 5182 (2) 2001
• SO2 in ambient air is collected in a solution of Tetrachloromercurate (TCM). SO2 reacts with TCM where Disulfitomercurate Compelx is formed. • The disulfito mercurate is treated with Formaldehyde and Acid bleached Pararosaniline to give a violet colour of Pararosaniline Methyl Sulfonic acid. • The intensity of the colour is measured on a spectrophotometer at 560nm wavelength against blank.

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Sulfur Dioxide (SO2)
West & Gaeke Method – BIS 5182 (2) 2001
• Range: Nominally 25 to 1050ug/m3. Conc. Below 25 can be measured by sampling larger volume of Air. • Lower Limit of detection of SO2 in 10ml absorbing reagent is 0.75ug. • Interferences: – NOx – eliminated by 1ml of 0.06% Sulphamic Acid. – Ozone – decomposed by allowing the solution to stand prior to analysis. – Trace Metals – Add EDTA to absorbing reagent prior to sampling

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Nitrogen Dioxide(NO2)
Standard Annual 40 g/m3 24 Hour 80 g/m3

BIS 5182 (part 6) 2006 • Absorbing Reagent: Solution of Sodium
Hydroxide & Sodium Arsenite. • Analysis: The absorbed NO2 is determined by reacting the nitrite ion with Sulphanilamide in the presence of Phosphoric acid and “coupling” it with NEDA. Intensity of colour is measured at 540 nm against blank using Spectrophotometer. • Range: 6 to 750 g/m3
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Nitrogen Dioxide(NO2)
BIS 5182 (part 6) 2006 • Analysis Range: 0.04 to 2.0ug/ml of soln. • Absorption Efficiency: 82% • Interferences:
– Small interference from NO and CO2 – SO2 – eliminated by converting to Sulphate by adding Hydrogen Peroxide during analysis.

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Ozone (O3)

Standard Annual 100 g/m3 1 Hr. 180 g/m3

Ambient Air is drawn through a midjet impinger containing 20ml 1% Potassium Iodide prepared in a neutral (pH 6.8) buffer composed of Na2HPO4 and KH2 PO4. The iodine liberated in the absorbing solution is determined Spectrophotometrically by measuring the tri-iodide ion at 352nm. Analysis must be completed within 30 min to 1hr after sampling. Interferences of other oxidants (SO2 & NO2 ) must be removed before sampling

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Ammonia (NH3)
Applicable standard 100 - 400 g/m3

• Ammonia is collected in dilute Sulfuric Acid solution where ammonia reacts with H2SO4 & gives Ammonium salt. When Nessler Reagent (K2HgI4) is added to this solution Orgeno Brown product in colloidal form is formed which has to be quickly determined colormetrically at 425nm wavelength. • Indo Phenol Blue method is also used for measurements of NH3. • Both methods are giving comparable results.
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Carbon Monoxide(CO)
Applicable standard 2(8hr)- 4(1hr) mg/m3

 In AAQ Standard measurement method for CO has been specified as NDIR. Thus NDIR based analyzer need to be used for monitoring of CO.  Analyzer need to be accurate up to 0.1 PPM. No other method is acceptable and can give reliable satisfactory results.  Alternatively an Air sample collected in Tedlar bag at low flow rates from a field station can be analyzed in lab for CO.
 Electrochemical sensor based systems may be used for short periods.
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Benzene(C6H6)
Standard Annual 5 g/m3

• Benzene from ambient air is collected on Activated Charcoal for specified period at very low flow rates (50-100ml/min)and later adsorbed organic compounds are Thermally Desorbed to find out concentration of Benzene using Gas Chromatograph fitted with capillary column. • BIS 5182 (Part 11) 2006 gives the details. • Ambient Benzene can only be analyzed using a high resolution GLC coupled with ATD System.
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Air Quality Monitoring
Sampling Period:
8 Hr. or 24 Hr as per standard. All parameters must be monitored simultaneously. If the sampler has operated for 75% of the time collected sample can be considered as valid sample.

 Monitoring must be done twice a week on nonconsecutive days of the week. Total 104 days monitoring must be done in a year to work out annual averages. Values must not be reported if calculated concentrations are less than the detection limits of the analysis method used.
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Selection of Monitoring Location
• Representative Site • The site should be away from major pollution sources • The site should be away from absorbing surfaces – such as a large water body. • It is expected to remain a representative site over a long time and no land use changes, rebuildings etc. are foreseen in near future.

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Physical requirements of the monitoring site
  • OPEN FROM ALL SIDES. For traffic pollution monitoring the sample intake should be 3 m above the street level.

Sampling in the vicinity of unpaved roads and streets results in entrainment of dust into the samplers from the movement of vehicles. Locate Sampler about 200m away from such sources.

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Logistics of the monitoring site
 Easy access to the site
 Anytime – day / night  Throughout the year.

 Site sheltering and facilities such as electricity of sufficient rating should be available.
Ground Connection / Earthing Voltage

It should be vandal proof

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To Ensure Data Reliability
Quality of Equipment Maintenance & Calibration Genuine & Good Quality Consumables
Filter Papers Reagents Distilled Water

Manpower Training
Sample Collection Analysis

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Equipment needed for complying with new Standard
Respirable Dust Sampler
PM10 Metals – Lead, Arsenic, Nickel PAH

Fine Particle Sampler – PM2.5 Gaseous Sampling Attachment or APM433
SO2 Nox Ozone , Ammonia

Additional Equipment
Benzene CO

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Thank you…
For more info on Envirotech Products visit www.envirotechindia.com

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