Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public.

इंटरनेट मानक

“!ान $ एक न' भारत का +नम-ण”Satyanarayan Gangaram Pitroda

“Invent a New India Using Knowledge”

“प0रा1 को छोड न' 5 तरफ”Jawaharlal Nehru

“Step Out From the Old to the New”

“जान1 का अ+धकार, जी1 का अ+धकार”Mazdoor Kisan Shakti Sangathan

“The Right to Information, The Right to Live”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता है”Bhartṛhari—Nītiśatakam

“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 5182-6 (2006): Methods for Measurement of Air Pollution,Part 6: Oxides of nitrogen [CHD 32: EnvironmentalProtection and Waste Management]

IS 5182 (Part 6) :2006

Indian Standard

METHOD FOR MEASUREMENT OF AIR POLLUTIONPART 6 OXIDES OF NITROGEN

(First Revision )

ICS 13,040.20

0 BIS 2006

November 2006

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002Price Group 3

Environment Protection and Waste Management Sectional Committee, CHD 32

FOREWORD .

This Indian Standard (First Revision) was adopted by the Bureau of Indian Standards, after the draft finalized by theEnvironment Protection and Waste Management Sectional Committee had been approved by the Chemical DivisionCouncil.

The standard was originally published in 1975. Based on the technological development in this area since last threedecades, the committee decided to revise the standard. In this revision, details of the sampling apparatus and requiredglassware; precision and accuracy and also 4 h sampling have been incorporated.

The method is generally specific for nitrogen dioxide. In high temperature combustion processes, some other oxides ofnitrogen and yielded which further oxidize to nitrogen dioxide in air at ordinary temperatures. So, the method isemployed to determine the nitrogen oxide contents in the atmosphere as nitrogen dioxides.

There is no 1S0 Standard on this subject. In the preparation of this standard, considerable assistance has beenderived from the following publications.

a)

b)

c)

CHRISTIE (AA) er, al. Field method for the determination of nitrogen dioxide in air. Analyst, 95:510-524(1970).

MAGESON, (J H) et, al. Evaluation of the sodium arsenite method for measurement of NOZin ambient air,J.A.P.C.A., 27:553-556 (1977).

JACOB, (MB) and HOCHHEISER (S). Continuous sampling and untra-micro detmnination of nitrogen dioxidein air. Anal. Chem. 30:426 (1958).

The composition of the Committee responsible for formulating this standard is given in Amex A.

In reporting the results of a test or analysis made in accordance with this standard, if the final value, observed orcalculated, is to be rounded off, it shall be done in accordance with IS 2:1960 ‘Rules for rounding offnumerical values(revised)’.

IS 5182 (Part 6) :2006

Indian Standard

METHOD FOR MEASUREMENT OF AIR POLLUTION

I

PART 6 OXIDES OF NITROGEN

(First Revision )

1 SCOPE

1.1 This standardprescribes a method for measurementof nitrogen oxides (as NOZ)in ambient air.

1.2 This method is applicable for 4 to 8 h integratedsampling of N02 in ambient air.

2 REFERENCES

Thefollowingstandardscontainprovisionswhichthroughreferme inthistextconstituteprovisionsof thisstandard.At the time ofpublication the editions indicated were valid.All standards are subject to revision and parties toagreements based on this standard are encouraged toinvestigate the possibility of applying the most recenteditions of the standards indicated below:

1S No. Title

1070:1992 Reagent grade water (thirdrevision)

2303 (Part 1/ Sec 1) : Grading glass for alkalinity:1994 Part 1 Hydrolytic resistance,

Section 1 Hydrolytic resistance ofglass grains at 98°C — Method oftest and classification (jirstrevision)

4167:1980 Glossary of terms relating to airpollution (first revision)

3 TERMINOLOGY

The definitions given in IS 4167 shall apply.

4 PRINCIPLE

Ambient nitrogen dioxides are collected by bubbling airthrough a solution of sodium hydroxide and sodiumarsenite. The concentration of nitrite ion (NOZ)producedduring sampling is determined calorimetrically by reactingthe nitrite ion with phosphoric acid, sulphanilamide andN-( 1-naphthyl)-ethy lenediamine di-hydrochloride(NEDA) and measuring the absorbance of the highlycoloured azo-dye at 540 nm.

5 RANGE

The nominal range of the method is 6 to 750 ~g N02 /m’

(0.003 to 0.4 ppm). The range of the analysis is 0,04 to2.0 lLgN02hi fOllowingBeer’sLawthroughoutthisrange[Oto l.Oabsorbanceunits).Underthespecifiedconditions~f 50 ml of abaorbiligrea@n~ a samplingrateof 200 cm3/pin for 24 h and a sampli#tg,eflickncy of 82 percent, therange of the method ia,“therefore;6 to 420 pg N02/m3(0.003 to022 ~). Nlkgen dioxide concentrations in*e range of 420 ‘to 750 @m3 (0.22 to 0.4 ppm) areaccurately measured by 1 : 1 dilution of the collectedsample,

6 INTERFERENCES

6.1 Nitric oxide (NO) is a positive interfiit and carbondioxide (C02) is a negative intefierant. The average errorresulting from normal ambient concentrations on NO andCOZis small for most monitoring situations and does notnecessitate applying a correction to measurements obtainedwith the method.

6.2 Potential interference from sulphur dioxide (SOZ)iseliminated by converting any S02 to sulphate usinghydrogen peroxide during analysis.

7 SAMPLE PRESERVATION

Collected samples are stable for at least six weeks at roomtemperature 25 + 2“C. Stored samples should be tightlysealed to prevent absorption of NOz from the atmosphere.

8 APPARATUS

8.1 Sampler — A sampler consists of the followingcomponents.

8.1.1 Sample Inlet — Teflon or glass tube with an invertedteflon or gl=s fimnel at the sampling point to prevententrance of precipitation.

8.1.2 Absorber — Standard glm”smidjet impinger shallbe used for sampling purpose. The glass impingers shallbe made from Class HGB 3 glass conforming toIS 2303 (Part l/See 1). Dimensional details of midjetimpinger shall be as given in Fig. 1,

8.1.3 Moisture Trap — The outlet impinger, a moisturetrap made up of glass or polypropylene tube loosely packed

1

IS 5182 (Part 6) :2006

.

.

220

5

1 mm RestrictingOrifke

130

—

II

I

+-

41DX70D15ml

Impinging Tube

20ml

+

25 ml

l’-20 ml

23 ID X 26 OD

Tube

15 ml

i

10.ml

i

5 ml

All dimensions in millimetres.

FIG. 1 STANDARDIMPINGERFORAIR SAMPLING

with dry silica gel to trap moisture shall be available insampler. This shall also protect the flow control device.The trap shall be packed with fresh dry glass silica gelbefore the start of each sampling period.

8.1.4 Flow Control Device — Any device capable ofmaintaining a constant flow through the sampling solutionbetween 200-1000 cm3/min. A convenient flow controldevice is hypodermic needle of specific gauge 10mm longused as a critical orifice or a needle valve.

8.1.5 Air Pump — Capable of maintaining a vacuum ofat least 0.6 atmosphere across the flow control device.This value is based on the critical pressure differential

0.53 atmosphere plus a safety factor to slow for wiiationsin atmospheric pressure and minor variations in pumpperformance.

8.1.6 Flow Meter — Properly calibrated flow meter formeasuring air flow rates in the range of 200-2000 cm3/min. The use of a mass flow meter is particularlyconvenient since no corrections are required when usedunder temperature and pressure conditions that differ fromthe conditions under which it is calibrated (See 12.1).

8.1.7 Flow Measurement Standard — Precision wet testmeter ( 1 litre/revolution), bubble flow meter, or otherreliable standard.

8.2 Spectrophotometer — Capable of measuringabsorbance at wavelength 540 nm equipped with 1 cmoptical path length cells.

8.3 Analytical Glassware

8.3.1 Volumetric Flasks — 50 ml, 100 ml, 250 ml,500 ml and 1000 ml.

8.3.2 Pipettes — 1 ml, 2 ml, 10 ml, 50 ml; volumetricpipettes of 2 ml and 1 ml shall be graduated in 1/10 ml.

9 REAGENTS

9.1 General

9.1.1 Unless specified otherwise, pure chemicals andreagent grade water (see IS 1070) shall be used in thetests.

NOTE — ‘Pure Chemicals’ shall mean chemicals that do not

contain impurities which affect the ‘results of analysis.

9.2 Absorbing Reagents — Dissolve 4.0 g of sodiumhydroxide in distilled water, add 1.0 g of sodium arseniteand dilute to 1000 ml with distilled water.

9.3 Hydrogen Peroxide, 30 percent,

9.4 Hydrogen Peroxide Solution — Dilute 0.2 ml of30 percent hydrogen peroxide to 250 ml with distilledwater. This solution may be used for one month, ifrefrigerated and protected from light.

9.5 N-(I-Naphthyl)-Ethylenediamine Di-Hydrochloride(NEDA) – 1 percent aqueous solution should have onlyone absorption peak at 320 nm over the range of 260-400nm. NEDA showing more than one absorption peak ofthis range is impure and should not be used.

9.6 NEDA Solution — Dissolve 0.500 g of NEDA in500 ml of distilled water. The solution is stable for onemonth if refrigerated and protected from light.

I

2

9.7

9.8

9.9

Phosphoric Acid, 85 percent.

Sodium Arsenite

Gt/JT/ON—Arsenic compounds are highly toxic and should be

handled with extreme care. Avoid contact with skin and especially

with eyes. Avoid generating dust or breathing dust. Keep away

from food. Wash imrds at=lerhading it. Do not take internally.

Sodium Hydroxide

9.10 Sodium Nitrite — Assay of 97 percent NaNOz orgreater.

9.11 Sodium Nitrite Stock Solution (1 000 pg NO;ml)— Dissolve 1.500g of desiccated sodium nitrite in distilledwater and dilute to 1000 ml such that a solution containing1000 ~g NO;ml is obtained. The amount of NaNOz to beused if the assay percent is less than 100 percent, iscalculated as follows:

G = 1.5001Awhere

G = amount of NaN02 in g;.

1.500 = gravimetric conversion factor; and

A = assay, percent (should be 97 or greater).

NOTE — This stock solution can be stored for six weeks, if

refrigerated.

9.11.1 Sodium Nitrite Solution (10 pg NOz/ml) — Pipette5 ml of the stock solution (see 9.11) in to a 500 mlvolumetric flask and dilute to volume with distilled water,

9.11.2 Sodium Nitrite Solution (1 pg NO~ml) — Pipette25 ml of the solution (see 9.11.1) in to a 250 ml volumetricflask and dilute to volume with absorbing reagent solution(see 9.2), prepare fresh daily.

9.12 Sulphanilamide — Melting point 165 to 167”C.

9.13 Sulphanilamide Solution — Dissolve 20.0 g ofsulphanilamide in 700 ml of distilled water. Add withmixing 50 ml of 85 percent phosphoric acid and dilute to1000 ml.

NOTE — This solution is stable for one month, if refrigerated.

10 PROCEDURE

10.1 Sample Collection

10.1.1 Four Hourly Sampling

10.1.1.1 Assemble the sampling apparatus at the samplingsite. Components upstream from the absorber may beconnected where required with teflonlsilicon tubing;

IS 5182 (Part 6) :2006

glass tubing with dry ball joints; or glass tubing withbutt-to-butt joints with teflon or polypropylene. Addexactly 30 ml of absorbing reagent to the calibratedabsorber. Disconnect the fi,mnel. Connect the calibratedflow meter, measure the flowrate before sampling andrecord as F,. Start sampling only after obtaining art initialflowrate of 1litre per minute. Ensure packing of ice aroundbubbler for low temperature to improve absorptionetliciency. For effective cooling thermoelectric coolingwith thermostat to maintain temperature of absorbingreagent at 10-15°C should be used for better absorptionet%ciency.

10.1.1.2 Sample for 4 hours

Record the exact sampling time by recording initial time(t,)and final time (t)of sampler. Measure and record theflowrate ~ ) before the sampling and flowrate @ afler thesampling. Seal the collected samples after making it up to30 ml using distilled water and transport to the laboratoryfor analysis.

10.1.2 24-Hourly Sampling

10.1.2.1 Assemble the sampling apparatus at thesampling site. Components upstream ffom the absorbermay be connected, where required, with teflon/silicontubing; glass tubing with dry ball joints; or glass tubingwith butt-to-butt joint with tygon, teflon or polypropylene.

Add exactly 30 ml of absorbing reagent to the calibratedabsorber. Disconnect the fi,mnel, connect the calibratedflow meter, measure the flowrate before sampling andrecord as F,. Start sampling only after obtaining an initialflowrate in this range. Sampling rate need to be chosendepending upon expected range of concentration.

10.1.2.2 Sample for 24 hours

Record the exact sampling time in minutes by recordinginitial (ti)and final (t)time of sampling. Measure andrecord the flowrate before ~ )and after ~~) the sampling.Seal the collected samples after making it up to 30 mlusing distilled water and transport to the laboratory foranalysis.

10.2 Analysis

10.2.1 Pipette 10 ml of the collected sample into 50 mlvolumetric flask. Now add 1 ml of hydrogen peroxidesolution, 10 ml of sulfanilamide solution, and 1.4 ml ofNEDA solution using pipette, with thorough mixing afterthe addition of each reagent and make up to 50 ml withdistilled water.

10.2.2 Prepare a blank in the same manner using 10 ml ofun-exposed absorbing reagent. After a 10 min colourdevelopment interval, measure and record the absorbance

3

IS 5182 (Part 6) :2006

at 540 nm against the prepared reagent blank. DetermineNOZfrom the calibration curve (see 12.3). Samples withan absorbance greater than 1.0 must be reanalyzed aflerdiluting an aliquot of the collected samples with an equalquantity of un-exposed absorbing reagent.

NOTES

1 A randomly selected 5-10 percent of the samples should be

reanalyzed as apart of an internal quality assurance program.

2 A known concentration ofN02 solution may analyze with sample

as an internal quality assurance program.

11 CALCULATIONS

11.1 Air Volume

Calculate the volume of air drawn for sample as follows:

~= J+&a —x(tf-ti) x60x 103

2

where

~ = volume of air sample, m3;

j = air flowrate before sampling,litreperminute;J = air flowrate after sampling, litre per minute;

ti = initial time in hours;

tf = final time in hours;10-q= conversion of Iitre to m3;and

60 = conversion of hours to min.

If the temperature and pressure conditions at the time ofthe initial and final air flowrate measurements aresubstantially different from the condition under which theflow meter was calibrated. appropriate corrections to theflowrate measurements may be made to improve theaccuracy of the resultant N02 concentration measurement.The mathematical form of these correction depends onthe type of flow meter used; consult an appropriatereference for guidance.

11.2 NOZConcentration in Analyzed Sample

Determine ~g N02/ml graphically from the calibrationcurve or compute from the slope and intercept values.

11.3 N02 Concentration in Air Sample

Calculate NOZas ~g per cubic metre of air as follows:

where

NO,= NOZconcentration in analyzed sample, pg;[Graph Factor x (Sample Abs.-Blank Abs)]

D = dilution factor (D = 1 for no dilution: D= 2 for1:1 dilution);

V, = final volume of sampling solution, ml;

4

~ = volume of air sample, ml;

0.82= sampling efficiency; and

~ = aliquot taken for analysis.

11.4 The N02 concentration as ppm shall be calculatedas follows:

NOZ,ppm = (N02~g/m3) x 5.32x 104

12 CALIBRATION

12.1 Flow Meter

measurement device:meter, or otlqf

25°C and ?60 toti. ‘,, 1! )), ,”,:

12.2 Absorber,<,

Calibratetnidjetglass impingeras follow

a)

b)

c)

\

Pipette 3Smldistikd waterabsorbingreagentusing5 ml calibrated pipette and check correctness ofmarking on impinger.

Use 3 mm thickness metal disk and check gapbetween bottom and tip of the impinger, 3 mm diskmust not be loose after fitting head of impinger.

Use three drill bits of 0.9 mm 1.0 mm and 1.1 mmand check bore size of nozzle, Bore size has to be1.0 mm with tolerance of O.lmm. Impingers mustbe cleaned thoroughly fortnightly and a~o beforeattempting calibration. Grease must be put on mouthof impinger while using.

12.3 Spectrophotometer

12.3.1 Prepare calibration curve using 1 pg/ml workingstandards (see 9.11.2) in accordance with the analyticalprocedure given in 12.3.2. Measure and record theabsorbance for each calibration standard (O, 1,2,3,4, 5,6,7,8,9, 10, 12, 15,20 ~g N02).

12.3.2 Plot absorbance (y-axis) versus the correspondingconcentration in pg NOz/50 ml solution (x-axis). Draw orcompute the straight line best fitting the data to obtain thecalibration curve.

13 PRECISION AND ACCURACY

Based on results from a collaborative study the withinlaboratory standard deviation is 8 @m3 (0.004 ppm) andthe between laboratory standard deviation is 11 pg/m’(0.006 ppm) over the range of 50 to 300 pgNO~m3 (0.027to 1.16 ppm). Based on results from a collaborative studythe method has an average bias of 3 percent over the rangeof 50 to 300 pg N02/m3 (0.027 to 0.16 ppm).

—.—. — ..———..

IS 5182 (Part 6): 2006

ANNEX A(Foreword)

COMMITTEE COMPOSITION

EnvironmentProtectionandWasteManagement Sectional Committee, CHD 32

Organization

In personal capacity (#O/f 4, CR, Park, New Delhi 110019)

Bhabha Atomic Research Centre, Mumbai

Bharat Heavy Electrical Limited, Hardwar

Cement Manufacturers’ Association, New Delhi

Central Fuel Research Institute, Dhanbad

Central Leather Research Institute, Chennai

Central Pollution Control Board, New Delhi

Confederation of Indian Industries. New Delhi

Crop Care Federation of India, New Delhi

Delhi College of Engineering, Delhi

Department of Civil Engineering, Indian Institute of Technology, New Delhi

Directorate General of Factory Advice Service and Labour Institute, Mumbai

Directorate General of Health Services, New Delhi

Engineers India Limited, New Delhi

Envirotech Instruments Private Limited. New Delhi

Federation of Indian Chambers of Commerce & Industry (FICCI), New Delhi

Gujarat Pollution Control Board, Ahmedabad

Hindustan Lever Limited, Mumbai

Indian Chemical Manufacturers’ Association, Mumbai

Indian Council of Agricultural Research, New Delhi

Indian Council of Medical Research, New Delhi

Indian Oil Corporation Limited, Faridabad

Industrial Toxicology Research Centre, Lucknow

5

Representative(s)

PROFDILIP BISWAS(Chairman)

DR (SHRIMATI)G. G. PANDIT

DR 1. V. SARADHI(Alternate)

DR N. G. SHRIVASTAVA

DR K. C. NARANG

DR L, C. RAM

DR S. RAJAMANI

DR S. D, MAKHIJANI

DK C. S. SHARMA(Alternate I)

DR S. K. TYAGI(Alternate II)

SHRIA. K. GHOSE

SHRI R. P. SHARMA(Alternate)

SHRI P. N. PARMESHWARAN

DR RAKESHMEHROTRA

SHRI V. K. MINOCHA (Alternate 1)

DR (SHRIMATI)A, MANOAL (Alternate 11)

DR MUKESHKtiARE

DR ATUL MITTAL (Ahernafe I)

DR ARVINrJNEMA (Alternate 11)

SHRI S, S. GAUTAM

SHRI BRIJ MOHAN (Alternate)

DR (SHRIMATI)MADHURI SHARMA

SHRI B. B. LAL

SHRI SUSHEELSADH (Alfernate)

SHRI RAKESHAGARWAL

DR RAJENORAPRASAD(Alternate)

Ms ANTARAROY

SHRI D. C. DAVE

SHRI B. B. DAVE

SHRIADITYA JHAVAR(Ahernate)

SHRI V. N. DAS

SMRIA. A. PANJWANI(Alternate)

DR R. C. MAHESHWARI

DR H. N. SAIYAD

DR M. P. SINGH

DR S. K. BHARGAVA

IS 5182 (Part 6): 2006

lPCL, Vadodaxa

Ministry of Defence (R&D), DRDO, New Delhi

Ministry of Environment and Forests, New Delhi

Ministry of Non-Conventional Energy Sources, New Delhi

Municipal Corporation of Greater Mumbai, Mumbai

National Institute of Occupational Health (lCMR), Ahmedabad

National Environmental Engineering Research Institute, Nagpur

National Thermal Power Corporation Limited, New Delhi

NCCBM, New Delhi

Reliance Industries Limited, Mumbai

Shrirans Institute of Industrial Research, New Delhi

SGS India Limited, Chennai

Steel AuthoI@’ of India Limited, New Delhi

Thapar Centre for Industrial Research& Development, Patiala

The Fertilizer Association of India, New Delhi

Town & Country Planning Organization, Ministry of Urban

Development, New Delhi

BIS Dkctorate General

SHRIANUPAMDESAI

SHRI MIHIR BANEIUi (A[temafe)

SHRIJ. C. KAPOOR

REPRESENTATWE

SHRI VINOD KUMARJAIN

DY CITY ENGINEERCIVIL (ENVT)

DEPUTYEXECUTWEENmNaER,

(EMISSIONINVBNTORYGROUP)(Alternate)

DR V. KRiat+rdAMURTHY

DR A. K. MUKHERJEE(Alternate)

DR V. 1. PANOIT

DR TAPANNANDY (Alternate)

SHRI R. GOPAL

SHRI M. S. BIiAOWAT

DR S. N. PATI (Akrnate)

SHRI E. SUNDERAaAN

DR U.K. SAROOP(Alternate)

SHRIV. G, NAIRDR JAGDISHKIJMAR(Alternate)

SHRI S. FLw

SHR[V. M. SHASTRI

SHR]K. B. LAL (Alternate)

DR MAHESHWARROY

DR S. K. CHAKRABORTY(Alternate)

DR (SHRIMATi)B. SWAMINATHAN

DR S. NAND (Alternate)

SHRI K. K. JOADDER

DR SANTOSHV{DHYA DHARAN (Alternate)

DR U. C. SRWASTAVA,Director & Head (CHD)

[Representing Director General (Ek-oficio)]

Member Secretary

SHRI N. K. PAL

Director (Chem), BIS

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This Indian Standard has been developed from Dot: No. CHD 32 (1270).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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