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Determination SMP

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Methodology for determination of Suspended Particulate

Matter (SPM) in the Atmosphere (High Volume Method).

PURPOSE

The purpose is to lay down a uniform and reliable method for measurement of Suspended
Particulate Matter (SPM) in the ambient air.

PRINCIPLE

Air is drawn through a size-selective inlet and through a 20.3 X 25.4 cm (8 X 10 in) filter
at a flow rate which is typically 1132 L/min (40 ft3 / min). Particles with aerodynamic
diameters less than the cut-point of the inlet are collected by the filter. The mass of these
particles is determined by the difference in filter weights prior to and after sampling. The
concentration of suspended particulate matter in the designated size range is calculated by
dividing the weight gain of the filter by the volume of air sampled (1,2).

OTHER ANALYSIS

Depending on the type of filter media used, filter samples can be analyzed for lead, ion,
organic and elemental carbon, extractable organic material, elements, radioactive
materials, inorganic compounds, and single particles.

RANGE AND SENSITIVITY

Lower Quantifiable Limit - For a 24-h sample duration at 1132 L/min, the detection
limit is determined by the reproducibility of the filter weight difference which shows a
standard deviation (sigma) of approximately + 2 mg. The three-sigma detection limit is
then approximately 3.5 g/m3. The three-sigma lower quantifiable limit depends on the
filter used and may be as high as 5 g/m3.

Upper Quantifiable Limit- For a 24-h sample duration at 1132 L/min, this is in the range
of 400 to 1000 g/m3. The exact value depends on the nature of the aerosol being
sampled : very small particles will clog the filter at a relatively low mass loading while
larger particles will fall off during sample transport at high concentrations.

Field Sampling- Tilt back the inlet and secure it according to manufacturer instructions.
Loosen the face-plate wing-nuts and remove the face plate. Remove filter from its jacket
and center it on the support screen with the rough side of the filter facing upwards.
Replace the face-plate and tighten the wing-nuts to secure the rubber gasket against the
filter edge. Gently lower the inlet. Inertial jet and cyclonic inlets must have their seals in
contact with the top of the face-plate. Look underneath the inlet just as it is coming into
contact with the face-plate to assure that this contact is being made may be necessary to
read just the position of the filter/motor assembly in the sample housing to obtain such a
seal. Excessively windy and wet conditions should be avoided when changing samples.
Pre-loading in a filter cartridge assembly, temporary remove the sampler to a protected
area, or a wind or rain shield may be used if, the sample must be changed in inclement
weather. Set the timer for the desired start and stop time. Replace the chart paper in the
flow recorder, if there is one, set the proper time, and measure the time and date on the
chart. For a manually flow controlled sampler turn on the motor for five minutes and
measure the exhaust pressure with a pressure gauge. Read the flow rate corresponding to
this exhaust pressure from the calibration curve record it on the data sheet. Turn off the
motor and assure that the timer is in its automatic mode. For automatically flow-controlled
units, record the designated flow rate on the data sheet. Record the reading of the elapsed
time meter. The specified length of sampling is commonly 8 hours or 24 hours. During
this period, several reading (hour) of flow rate should be taken.
After sampling is complete, record the final flow rate and the elapsed time in the same
manner. Subtract the initial elapsed time from the final elapsed time to determine sample
duration. Remove the face-plate by removing the wing-nuts. Fold the filter half lengthwise
by handling it along its edge with the exposed side inward. Insert filter in its jacket. Note
the presence of insects on the deposit, loose particles centered deposits, evidence of leaks,
and unusual meteorological conditions on the sheet. Mark the flow recorder chart, if any,
and return it with the data sheet.

CALCULATIONS

Calculation of Volume of Air Sampled

V = QT
V = Volume of air sampled in m3.
Q = Average flow rate in m3/minute

Calculation of Suspended Particulate Matter in Ambient Air

(Wr – Wi) x 106


----------------------------
SPM =
V

Where
SPM = Mass concentration of suspended particles in g/m3.
Wi = Initial weight of filter in g.
Wr = Final weight of filter in g.
V = Volume of air sampled in m3.
106 = Conversion of g to g.

REFERENCES

1. Robson, C.D. and K.E., Foster, 1962. Evaluation of air particulate sampling
equipment. Amer. Indust. Hyg. Assoc. Journal, 23:404.
2. Olin, J.G. and J.L. Kurz, 1975. High volume air samplers. Poll. Eng. 7(1):30.
3. Rehme K.A., C.F. Smith, M.I. Fitzsimmons, 1984. “ Investigation for use in the
determination of ambient particulate matter”. 048, Research Triangle Park, N.C.
4. Countess. R.J., 1974. Production of aerosol by high volume samples. J.Air Poll.
Cont. Assoc. 24-605.
5. King, R.B. and J. Toma, 1975 “Copper emissions from a high volume air sampler”
NASA Technical Memorandum, NASA-TM X- 71693.
6. Coutant, R.W., 1977. Effects of environmental variables on collection of
atmospheric sulfate. Environ. Sci. & Tech., 11:875.
7. Appel B.R.Y. Tokiwa. M. Haik and E.L. Kothny, 1984. Artifact particulate sulfate
and nitrate formation on filter media. Atmos. Environ. 18:409.
Methodology for Respirable Suspended Particulate Matter
(PM10) in ambient air (Cyclonic Flow Technique).

PURPOSE

The purpose is to lay down an uniform and reliable method for measurement of PM10
(Particulate matter less than 10 m diameter) in ambient air.

PRINCIPLE

Air is drawn through a size-selective inlet and through a 20.3 X 25.4 cm (8 X 10 in) filter
at a flow rate which is typically 1132 L/min. Particles with aerodynamic diameter less than
the cut-point of the inlet are collected by the filter. The mass of these particles is
determined by the difference in filter weights prior to and after sampling. The
concentration of PM10 in the designated size range is calculated by dividing the weight
gain of the filter by the volume of air sampled.

Other Analysis - Depending on the type of filter media used, filter samples can be
analyzed for lead, iron, organic and elemental carbon, extractable organic material,
elements, radioactive materials, inorganic compounds, and single particles.

Range and Sensitivity

Lower Quantifiable Limit - For a 24-h sample duration at 1132 L/min, the detection
limit is determined by the reproducibility of the filter weight difference which shows a
standard deviation (sigma) of approximately + 2mg. The three-sigma detection limit is
then approximately 3.5 g/m3. The three-sigma lower quantifiable limit depends on the
filter used and may be as high as 5 g/ m3.

Upper Quantifiable Limit - For a 24-h sample duration at 1132 L/min, this limit is in the
range of 400 to 1000 g/ m3. The exact value depends on the nature of the aerosol being
sampled : very small particles will clog the filter at a relatively low mass loading while
larger particles will fall off during sample transport at high concentrations.

Field Sampling- Tilt back the inlet and secure it according to manufacturer instructions.
Loosen the face-plate wing-nuts and remove the face plate. Remove filter from its jacket
and center it on the support screen with the rough side of the filter facing upwards.
Replace the face-plate and tighten the wing-nuts to secure the rubber gasket against the
filter edge. Gently lower the inlet. Inertial jet and cyclonic inlets must have their seals in
contact with the top of the face-plate. Look underneath the inlet just as it is coming into
contact with the face-plate to assure that this contact is being made may be necessary to
read just the position of the filter/motor assembly in the sample housing to obtain such a
seal. Excessively windy and wet conditions should be avoided when changing samples.
Pre-loading in a filter cartridge assembly, temporary removal the sampler to a protected
area, or a wind or rain shield may be used if, the sample must be changed in inclement
weather. Set the timer for the desired start and stop time. Replace the chart paper in the
flow recorder, if there is one, set the proper time, and measure the time and date on the
chart. For a manually flow controlled sampler turn on the motor for five minutes and
measure the exhaust pressure with a pressure gauge. Read the flow rate corresponding to
this exhaust pressure from the calibration curve record it on the data sheet. Turn off the
motor and assure that the timer is in its automatic mode. For automatically flow-controlled
units, record the designated flow rate on the data sheet. Record the reading of the elapsed
time meter. The specified length of sampling is commonly 8 hours or 24 hours. During
this period, several reading (hour) of flow rate should be taken.

After sampling is complete, record the final flow rate and the elapsed time in the same
manner. Subtract the initial elapsed time from the final elapsed time to determine sample
duration. Remove the face-plate by removing the wing-nuts. Fold the filter half lengthwise
by handling it along its edge with the exposed side inward. Insert filter in its jacket. Note
the presence of insects on the deposit, loose particles centered deposits, evidence of leaks,
and unusual meteorological conditions on the sheet. Mark the flow recorder chart, if any,
and return it with the data sheet.

CALCULATIONS

Calculation of Volume of Air Sampled

Calculation of PM10 in Ambient Air

PM10 = (Wr – Wi) x 106


----------------------------
V

Where

PM10 = Mass concentration of particular matter less than 10 micron


diameter in g/m3
Wi = Initial weight of filter in g.
Wr = Final weight of filter in g.
V = Volume of air sampled in m3.
106 = Conversion of g to g.

REFERENCES

1. Intersociety Committee. Methods of Air Sampling and Analysis, (3rd Edition) by


James. P. lodge, Sr. Editor. Lewis Publishers, Inc.
Methodology for measurement of CO/Hydrocarbon emission
from Petrol Driven vehicles by infrared analyzer.

PURPOSE

The purpose is to lay down an uniform and reliable method for measurement of Carbon
Monoxide and Hydrocarbon emission from petrol driven automobiles.

PRINCIPLE

Carbon monoxide and hydrocarbon concentration of gases in the exhaust gas from the
combustion engines is measured by a infrared detector in CO-HC analyzer. Both the gases
are measured simultaneously by the instrument. The CO concentration in percent by
volume is indicated on CO meter and HC concentration in n-hexane in parts per million
(PPM) by volume is indicated on HC meter. The detection method used by this instrument
is based on Non-dispersive infrared, single beam tamp stabilized Lead Selenide detector.
Special narrow hand interference filters are used to analyze the characteristic absorption
spectra of CO/HC.

SCOPE

This method is applicable for measurement of concentration of CO/Hydrocarbon emission


in petrol driven vehicles.

OPERATION PROCEDURE

1. Place the dust filters on sample line.


2. Connect the sampling probe and sampling tube with the instrument.
3. Make the power switch on.
4. Warm-up the instrument for 30 minutes.
5. Select the range for CO-HC
6. Check the electronic test pulse by pressing the relevant push button. It should
be in green zone.
7. Make the pump switch on and start the measurement.

CALIBRATION

Calibration is of vital importance in all automobile exhaust instruments otherwise all the
measurement and data obtained will be false and mis-representing. The procedures for the
calibration of CO-HC analyzer is as under :

Zero Calibration : Select the desired range of CO-HC analyzer and introduce fresh air
from the tip of sampling probe. Adjust the zero with the help of zero potentiometer/knob.
Similarly adjust the zero for HC also with the help of zero potentiometer for HC.

Span calibration :

1. Make the pump switch of the instrument off


2. Keep the CO range select switch to 10% CO and HC select switch to 2000
PPM respectively

3. Insert the nozzle of known concentration of span gas cane (cylinder) into the
calibration gas inlet of the instrument. Instrument will get purged with span
gas.

4. When the calibration gas is purged in the instrument, CO and HC meters


needles/display will indicate some higher values

5. If required, adjust CO span potentiometer to the concentration marked on CO


cylinder. For HC also adjust the span potentiometer as per the hexane value.
Hexane value for HC has to be converted as per span gas specification marked
on the gas cane.

6. After the calibration is over instrument can be put to automobile emission


measurement.

SPECIFICATIONS

1. Instrument range : CO – 0 - 2%
0- 10%
HC - 0- 500 / 0 – 2000 / 0-8000 PPM

2. Reproducibility : with 2% of full scale

3. Stability : with 2% of full scale

4. Response time : T – 90

5. Ambient tamp : 0 to 50 C

6. RH : 0 – 90 %

7. Calibration method : calibration by span gas

8. Instrument deviation : with in 30% full scale

Confirmity : Confirmation to 89/336 EFC directive on E.M. compatibility.

EN – 50081 – 1 Gerric Emission Standard 1992

EN – 50082 – 2 Gerric Immunity Standard 1992

72/23/ECG Low Voltage Safety Directive.


Methodology for determination of Nitrogen Dioxide
in the Atmosphere (Sodium Arsenite method)
PURPOSE

The purpose is to lay down an uniform and reliable method for sampling and analysis of
nitrogen dioxide in ambient air.

PRINCIPLE

Ambient nitrogen dioxide (NO2) is collected by bubbling air through a solution of sodium
hydroxide and sodium arsenite. The concentration of nitrite ion (NO2) produced during
sampling is determined colorimetrically by reacting the nitrite ion with phosphoric acid,
sulfanilamide, and N- (1-naphthyl)- ethylenediamine di-hydrochloride (NEDA) and
measuring the absorbance of the highly colored azo-dye at 540 n m.

The nominal range of the method is 9 to 750 g NO2/m3 (0.005 to 0.4 ppm3). The range of
the analysis is 0.04 to 2.0 g NO2 / ml, following Beer’s Law throughout this range (0 to
1.0 – absorbance units). Under the specified conditions of 50 ml of absorbing reagent, a
sampling rate of 200 cm3 / min for 24 hours, and a sampling efficiency of 0.82, the range
of the method is, therefore, 9 to 420 g /NO2 /m3 (0.005 to 0.22 ppm). Nitrogen dioxide
concentrations in the range of 420 to 750 g /m3 (0.22 to 0.4 ppm) are accurately
measured by 1 : 1 dilution of the collected sample.

Based on results from a collaborative study, the within laboratory standard deviation is 8
g /m3 (0.004 ppm) and the between laboratory standard deviation is 11 g / m3 (0.006
ppm) over the range of 50 to 300 g NO2 /m3 (0.027 to 1.16 ppm)4.

Based on results from a collaborative study, the method has an average bias of –3% over
the range of 50 to 300 g NO2 /m3 (0.027 to 0.16 ppm)4.

SCOPE

This method is applicable to 24 hours integrated sampling of NO2 in ambient air.

ANALYSIS OF NITROGEN DIOXIDE


(Sodium Arsenite Method)

Sodium Hydroxide : Dissolve 4.0 gm sodium Hydroxide in distilled water add 1.0 gm of
sodium arsenite and dilute to 1000 ml.

Sulphanilamide : Dissolve 20 gm sulphanilamide in 700 ml distilled water, add 50 ml


phosphoric acid ( 85%) and make it 1000 ml. This sol. Stable for one month if
refrigerated.
NEDA : N [ 1- Naphthyl ] ethylenediamine di-hydrochloride : Dissolve 0.5 gm of
NEDA in 500 ml distilled water or 0.1 gm in 100 ml distilled water. This sol. Stable for
one month if refrigerated (protected from light).

Hydrogen Peroxide : Dilute 0.2 ml of 30% H2O2 in 250 ml distilled water. This solution
may be used for one month.

Analysis :

Pipet 10 ml of the collected sample +1 ml H2O2 (0.02%) + 10 ml sulphanilamide +1.4 ml


NEDA; After mixing wait for 10 minutes. Prepare a blank also with unexposed absorbing
reagent. Record the absorbance at 540 nm.

Calculation :

Absorbance x Calibration factor x Vol. Of total Abs. Sol


NO2 ( g/m3) = ---------------------------------------------------------------------------
Total air volume passed x 0.82 x Sample taken for analysis
Methodology for determination of Sulphur Dioxide
in Air (Modified West and Gaeke Method)

PURPOSE

The purpose is to lay down an uniform and reliable method for determination of sulphur
dioxide (SO2) in ambient air.

PRINCIPLE

Sulpher dioxide from air is absorbed in a solution of potassium tetrachloro-mercurate


(TCM). A dichlorosulphitomercurate complex, which resists oxidation by the oxygen in
the air, is formed (5,6). Once formed, this complex is stable to strong oxidants such as
ozone and oxides of nitrogen and therefore, the absorber solution may be stored for some
time prior to analysis. The complex is made to react with pararosaniline and formaldehyde
to form the intensely colored pararosaniline methylsulphonic acid (7). The absorbance of
the solution is measured by means of a suitable spectrophotometer.

Concentration of sulphur dioxide in the range of 25-1050 g/m3 can be measured under
the conditions given are measure concentration below 25 g/m3 by sampling larger
volumes of air, but only if, the absorber efficiency of the particular system is first
determined and found to be satisfactory. Higher concentration can be analyzed by using
smaller gas samples of a suitable aliquot of the collected sampler. Beer’s law is followed
through the working range from 0.03 to 1.0 absorbance unit. This corresponds to 0.8 – 27
g of sulfite ion in 25 ml of final solution calculated as sulphur dioxide. The lower limit of
detection of sulpher dioxide in 10 ml absorbing reagent is 0.75 g based on twice the
standard deviation, which represent a concentration of 25 g/m3 in an air sample of 30
litres.

SCOPE

This method is applicable for the measurement of concentration of sulphur dioxide present
in ambient air.

Determination of SO2 in Ambient Air


(West and Gaeke Method)
Reagents :

(11) Absorbing Solution : TCM ( 0.04 M) : Dissolve 10.86 gms mercury


chloride(Hgcl2), 0.066 gms EDTA and 6 gms potassium chloride in 1000 ml
DH2O.

(12) Sulphamic Acid (0.6%) – Dissolve 0.6 gm Sulphamic Acid in 100 ml DH2O.

(13) Formaldehyde (0.2%) - Dilute 0.5 ml (35-40%) Formalin in 100 ml DH2O.

(14) P-Rosoniline Hydrochloride (Stock) : Dissolve 0.5 gms of PRH in 100 ml


distilled water for 48 hours and filter it.

PRA (Working Sol) : Mix 4 ml stock PRA sol +6 ml HCL (conc.) and
dilute to 100 ml.

Analysis :

20 ml sample + sulphamic Acid; wait for 10 minutes; after 10 minutes + 2 ml


formaldehyde + 2 ml PRA (working ) wait for 30 minutes.

After 30 minutes read the absorbance at 560 NM.

Abs x Cal. factor x Total sample vol. (20)


Calculation SO2 (g/m3) = -----------------------------------------------------------
Vol. of air (m3) x sample taken for analysis (20)

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