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( Reaffirmed 2003 )
METHODS OF MEASUREMENT OF EMISSIONS FROM STATIONARY SOURCES
PART 6 AMMONIA
Supplied by Book Supply Bureau to CSIR E JOURNALS Consortium for internal use by subscribing member only.
0 BIS 1999
BHAVAN, 9 BAHADUR SHAH ZAFAR NEW DELHI 110002
Ammonia is one of such pollutants. which may become chronic with repeated exposure to its vapours. it shall be done in accordance with IS 2 : 1960 ‘Rules for rounding off numerical values (revised)‘. after the draft finalized by the Air Enviromnent Protection Sectional Committee had been approved by the Chemical Division Council. The composition of the technical committee responsible for preparation of this standard is given in Annex A. . This standard details two methods for determination of ammonia from stationary sources.Air Environment Protection Sectional Committee. The undesired impacts of pollutants on flora and fauna is of high concern to scientists and technologists. CHD 32 FOREWORD This Indian Standard was adopted by the Bureau of Indian Standards. eyes and respiratory tracts. Supplied by Book Supply Bureau to CSIR E JOURNALS Consortium for internal use by subscribing member only. Keeping these in view. in particular and to common people. observed or calculated. in general. discharged in air mainly by fertilizer industry. Ammonia is known to be causing irritant to skin. plethods for measurement of ammonia has gained importance. if the final value. is to be rounded off. In reporting the result of a test made in accordance with this standard.
The ammonia content in the sample is determined by titration of the distillate with a dilute standard sulphuric acid solution. The upper detection limit may be extended by increasing the strength of the titrant acid solution. 1 TITRATION given in Leak-proof vacuum pump. The sample solution is buffered at pH 9. the editions indicated were valid.3 Interferences Ammonium salts will liberate ammonia during distillation to give high ammonia concentration. All standards are subject to revision. 4. Method A .4 Apparatus 4.4.4 Valve Needle valve or equivalent to adjust accurately in the range of 0.4. capable of drawing upto 5 l/min air under the sampling conditions.4.4.IS 11255 ( Part 6 ) : 1999 Zndian Standard OFEMISSIONS METHODSOFMEASUREMENT FROMSTATIONARYSOURCES PART 6 1 SCOPE This standard prescribes two methods namely.3 mg of ammonia in a 60 1 gas sample.7 Glass Wash Bottle Containing distilled water to rinse the impingers connecting tubes. These can be removed by filtration of the gas sample before its passage into the impingers. 4 METHOD A 4. 4. 4. corresponding to a concentration of about 5 mg/Nm”.5 to 5 l/min.4.43 Pump Supplied by Book Supply Bureau to CSIR E JOURNALS Consortium for internal use by subscribing member only. 4. and flow rate METHOD . 4. At the time of publication.4.5 to 5 l/min.6 Dry Gas Meter Sufficiently accurate to measure the sample volume within 1 percent. 4. for determination of ammonia from stationary sources.Titration method and Method B . 3 TERMINOLOGY For the purpose of this standard. definitions IS 4167 shall apply.2 Range and Sensitivity This method may be used to detect as little as 0. 2 REFERENCES The following standards contain provisions which through reference in this text. fitted with a thermometer and a pressure gauge/manometer to measure the metering temperature and pressure. 4167: 1980 5182 (Part 5) : 1975 Title Glossary of terms relating to air pollution (first revision) Methods for measurement of air pollution: Part 5 Sampling of gaseous pollutants AMMONIA 4. constitute provision of this standard.1 Principle Ammonia is collected in dilute sulphuric acid solution in two all-glass impingers to form ammonium sulphate. 4.2 Impinger Three standard large impingers [see IS 5 182 (Part 5)] connected in series and placed in an ice bath.Nessler reagent method/Spectrophotometric method. 4.5 with borate buffer and distilled into a solution of boric acid.8 Polyethylene Storage Bottles With 100 ml capacity to store the impinger samples. This is avoided through preliminary distillation step. orifice-meter or other suitable device to measure flow rate in the range of 0. Acidic and alkaline gases in the gas sample may interfere during titration.034 mg of ammonia in the sample. with an internal diameter of 5 to 6 mm with a heating system to prevent condensation and a filtering medium at the sample inlet end to remove particulate matter (end packed with glass or quartz wool). The lower detection limit is about 0.4.1 Probe Chemical resistant glass tube.5 Rotameter Rotameter. and parties to agreements based on this standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below: IS No. 4.
4. To this.1 Water Deionized or distilled water.11 Erlenmeyer Flask 500 ml capacity. if needed.5. if needed.1 N Sulphuric Acid) Dilute 2.1 ml sub division.34 mg of ammonia. 10 H20) in 500 ml of water. Prepare such mixed indicator solutions. add 88 ml of 0. once in a month.5.5 Reagents 4. 4. GASMETER H NEEDLE VALVE FIG.7 Standard Sulphuric Acid Titrant 0.5. 4. Leave the final impinger dry.410 pH Meter 4.12 Burette 25 ml and 50 ml capacity with 0. 4.02 N.6 Procedure 4. One ml of acid solution is equivalent to 0. Borate Buffer Solution Dissolve 4. add 10 ml of mixed indicator solution and dilute to 1 1.5 Mixed Indicator Solution Dissolve 200 mg of methyl red indicator in 100 ml of 95 percent ethyl alcohol or isopropyl alcohol. AMMONIA SAMPLINGTRAIN 1 2 .IS11255(Part6):1999 4.4. Mix the two solutions. 4. 1.6.4 Neutralization Sodium hydroxide.1 N sulphuric acid into each of the first two impingers. Check the sampling train for leakage at the sampling site by plugging the probe inlet and creating a vacuum Supplied by Book Supply Bureau to CSIR E JOURNALS Consortium for internal use by subscribing member only.5. sulphuric acid to 100 ml Dilute 200 ml of 0. Connect all the three impingers in series and place in the ice bath. 4. using the mixed indicator. Assemble the train as shown in Fig. Standardize this by titrating against a known amount of sodium carbonate that has been incorporated in the boric acid solution.9 Distillation Apparatus Borosilicate glass flask of 1 000 ml capacity attached to a vertical condenser so that the outlet tip may be submerged below the surface of the acid solution in the receiving flask.1 N sulphuric acid to 1 1. 4.6 Absorbent Solution Dissolve 20 g of boric acid (HsBOs) in ammonia-free distilled water.8 ml of concentrated with distilled water. 4. Agent IN.1 Preparation of Sampling Train Pour 30 ml of 0.4.5. free of ammonia.5.1 N sodium hydroxide and dilute to 1 1. 4. 4. 4.75 g of borax (NaiB&.53. Dissolve 100 mg of methylene blue in 50 ml of 95 percent ethyl alcohol or isopropyl alcohol.2 Absorbing Solution (0. Prepare once in a month.
At the end of the sampling. vb = volume in ‘ml of 0.7. Remove the probe from the stack and disconnect it from the train. 4.3 Sample Recovery Disconnect the impingers. Correct the sample volume measured by the dry gas meter to normal conditions (298“K and 760 mm Hg ) on dry basis by using.IS 11255 ( Part 6 ) : 1999 corresponding to 250 mm mercury column..02 N sulphuric acid solution by titrating against a known amount of sodium carbonate in the boric acid absorbent indicator solution. it shall be stored in a cool place. Position the tip of the probe at the first sampling point within the stack.6. Rinse the two impingers and the connecting tube with ammonia-free distilled water and add the washings into the shipment bottle. 4. 4. x (V-VdXf Vi. Lower the collected distillate free of contact with delivery tube and continue distillation for 2 min to clean condenser and delivery tube. turn off the pump and record the final reading of the gas meter.6. Pm = average gauge pressure in mm Hg of gas sample through dry gas meter. t m= = volume in m3 of dry sample measured in the gas meter under meter conditions.34 = mg of ammonia equivalent 0. continue the sampling for a total period of 30 min. 4.02 N sulphuric used for the sample. 3 . Neutralize to approximately pH 7 with sodium hydroxide using a pH meter and make this volume upto about 500 ml with distilled water. = saturated vapour pressure of steam at h. Distill at the rate of 6 to 10 ml/min and collect the distillate into the Erlenmeyer flask containing the indicator boric acid absorbent solution.1 Dry Gas Volume Supplied by Book Supply Bureau to CSIR E JOURNALS Consortium for internal use by subscribing member only. Add ice into the ice bath during the sampling to maintain the temperature of the gases leaving the impinger train at 20°C or less.02 N sulphuric used for the blank. within acceptable. 4.4 Ammonia Distillation Transfer the contents of the shipment bottle quantitatively into a distillation flask and make the volume upto to about 400 ml with distilled water.2 Ammonia Concentration Calculate the concentration following equation: c_o34 of ammonia using the .5 Analysis Titrate ammonia in distillate with standard 0. Maintain the sample flow rate at about 2 Ymin by operating the valve. m3. and f= V” = volume of dry gas sample. Carry a blank through all steps and apply the necessary correction to the results. Record the metering temperature and pressure at 5 min intervals. v= to 1 ml of acid acid volume in ml of 0.6.02 N sulphuric acid titrant until indicator turns to a pale lavender. 4.7. Pa = atmospheric pressure in mm Hg during sampling period.02 N sulphuric acid . Standardize the 0. In the same manner. Pour 50 ml of absorbent solution (indicator boric acid solution) in the Erlenmeyer flask and place it below the condenser of distillation apparatus with the tip of the delivery tube below the surface of the absorbent solution. 4. factor of 0. Collect at least 200 ml distillate. in mg/Nm3 of ammonia in where c= concentration gas sample.7 Calculations 4. Pour the contents of the first two impingers into a polyethylene shipment bottle. = * x 760 m where V” = volume in m3 of dry gas sample under normal conditions. v. Connect the distillation flask to the distillation apparatus.6.the following equation: _ Pa+i+P” V” = v. A leakage 1 percent of the sampling rate is rate. Record the metering temperature and pressure between 2 to 3 min of sampling. average temperature in ‘C of gas sample through dry gas meter. 0.2 Sample Collection Insert the sampling probe into the stack. Without stopping the pump.6 Calibration Use approved methods and equipments to calibrate dry gas meter and rotameter. Record the initial reading of the dry gas meter. sample shall be analyzed immediately. shift the tip of the probe to the second point.02 N sulphuric acid.1 N sulphuric acid). Carry blank run with the sampling reagent (0. Add 25 ml of borate buffer solution and adjust the pH to 9. Start the pump and maintain the sample flow rate at about 2 Vmin.6. drawing the sample from 6 different points within the duct. In case of delay. Draw the sample for 5 min from the first point. Preferably. consisting of distillation and titration steps.5 with 6 N sodium hydroxide using apH meter. and P.
5 g of potassium iodide in 260 ml of cold water.3 Ammonia Emission Calculate the emission of ammonia from the stack as follows: E = 10-3C x On where E= c= ammonia emission rate. g/h. and decant the clear liquid. 5 ml. 5.1 Principle Ammonia is collected in a dilute sulphuric acid solution in a midget impinger to form ammonium sulphate. Other interferences are not known. 5. 5. Filter and allow to cool. The solution is reacted with Nessler reagent to produce a yellow-brown complex. 1. This method is sensitive. 4.8 ml of concentrated sulphuric acid (18 M) to 1 1 with distilled water to form 0. 5. This method does not distinguish between free and combined ammonia.6 Quality of Reagents Unless specified otherwise.8 Absorbing Solution Dilute 2. The range of application of this method is 0.4 Spectrophotometer 1 cm. mg/Nm3 (dry).4.80 mg of ammonia in a 10 1 air sample.5 Volumetric Flasks 50 ml. NESSLER 5 METHOD B METHOD/SPECTROPHOTOMETRIC METHOD 5. 5. 5. NOTE . Attach the 4 . Cells REAGENT Supplied by Book Supply Bureau to CSIR E JOURNALS Consortium for internal use by subscribing member only. Absorption peak may shift with concentration. Dissolve 62. calibrated. concentration of ammonia in the exhaust gas.IS 11255 ( Part 6 ) : 1999 4.5. 200 ml. 10 ml and 20 ml.1 Water Double distilled water.2 Impingers and Standard Midget Impinger All glass. 5. 5. 5.5. On = exhaust gas flow rate.5.1 Battery Operated Personal Air Sampling Pump Capable of drawing 1 1 of air per minute through 10 ml of absorbing solution.6 Pipette 0.The Nessler reagent shall be handled with caution because of its toxicity and corrosive properties.5.O ml.4 Apparatus 54. add the mercuric chloride solution to 250 ml of the iodide solution until a slight permanent red precipitate is formed. NOTE .002 mg of ammonia.3 Interferences Ammonium salts will react with Nessler reagent to give a false high reading.5 Ammonium Sulphate 5. 100 ml.5. but ammonium salts can interfere.7.4. Add this solution to the potassium iodide-mercuric chloride solution and make up to 1 1 with distilled water.4 Potassium Iodide 5. 5.7. 54.1 mg to 0.5. pure chemicals and distilled water (see IS 1070) shall be employed in the tests. Discard solution after a week.5. distillation and analysis have not been reported.3 Spectrophotometer 5. Dissolve the precipitate with the remaining iodide solution and again add mercuric chloride slowly until a red precipitate remains. One ml of this solution contains 20 ltg of ammonia. The ammonia concentration is determined by reading the absorption of the yellow-brown solution at 440 nm and comparing it with a standard curve. 5. Preliminary studies have indicated that the accuracy of the procedure is + 5 percent at 100 mg/Nm” and + 10 percent at 20 mg/Nm3.‘Pure chemicals’ shall mean that do not contain impurities which affect the results of analysis.1 Sampling Add 10 ml of absorbing solution to each midget impinger including one for the blank.5.6 Nessler Reagent Dissolve 35 g mercuric chloride in 500 ml of hot water. Dissolve 150 g of potassium hydroxide in 250 ml of distilled water.1 N sulphuric acid.7 Standard Ammonium Sulphate Solution Dissolve 77.2 Range and Sensitivity The nessler reagent is sensitive to as little as 0.3 Potassium Hydroxide 5.7 Procedure 5. Nm3/h (dry).5 Reagents 5. 5. These can be removed by filtration of the air before its passing into the absorption tube. 50 ml and 100 ml.4.6 mg of ammonium sulphate (desiccated overnight) in distilled water and make up to 1 1.8 Precision and Accuracy The precision and accuracy of the procedure involving sampling. free of ammonia. 1 000 ml glass stoppered. Gradually. and 54.5 ml.2 Mercuric Chloride 5.4. Stir thoroughly and allow to stand a day or so.7 Graduated Cylinders 25 ml.
7. Shake. 30 ml and 40 ml Supplied by Book Supply Bureau to CSIR E JOURNALS Consortium for internal use by subscribing member only. light absorbance in a spectrophotometer at 440 nm.2.9 Calculation Ammonia.8 Calibration and Standardization of the standard ammonium sulphate solution and process in the same manner as described in 57. Treat the blank in the same manner as the sample. 5. and V = volume in litre of air corrected to 25’C and 760 mm Hg. mg/Nm3 where M = mass in ug of ammonia from the standard curve minus blank value.2 Colour Development Dilute the sample to 50 ml with distilled water in a volumetric flask and shake well. = $ Dilute samples of 5 ml. . 5. add 2 ml of Nessler reagent to the latter flask and determine absorbance after 10 min at 440 nm in a spectrophotometer using a 1 cm cell.IS 11255 ( Part 6 ) : 1999 bubbler to a personal air sampling pump and draw air through the bubbler at a rate of 1 Vmin for 10 to 15 min. Determine. Prepare a standard curve of absorbance versus mg of ammonia. Record the volume of air sampled. 5. Take 1 ml of this solution and make up to 50 ml with distilled water in another volumetric flask. 10 ml. 20 ml.
BHARDWAI S. NAMBI DR T. BHARGAVA (Alternate) REPRESENTATIVE SHRIA~HOKBHATIA DR A. Haridwar Department of Industrial Development. SINGH Add1 Director (Chem). V. GURLJMOOR’IHY (Alternafe) REPRESEWATIVE SHRIS. K. AGGARWAL SHRI RAKESHAGGARWAL(Alfernate) DR R. Mumbai Bharat Heavy Electricals Ltd. New Delhi Cement Manufacturers’ Association. BAPAT DR S. Mumbai Indian Chemical Manufacturers’ Association. RAJAGOPALAN. V. RAO (Ahmate). AGGARWAL SHRI S. DAS SHRI C. Nagpur National Institute of Occupational Health. Calcutta Hindustan Lever Ltd. JHAVAR (Alternate) REPRESENTATIVE DR P. New Delhi Central Fuel Research Institute. NAIR (Alfernate) DR G. DR S. D. C. Mumbai Directorate General of Factory Advice Services and Labour Institutes. DR T. (Alternate) DR V. GHOSH SHRI P. New Delhi Asea Brown Boveri Ltd. Dhanbad Envirotech Instruments Private Ltd. RAMAKRISHNA SHRIM. S. K. BIS DR (MS) B. SINGH D. N. C. NARANG K. SENGWTA DR C. BIS (Ex-oficio Member) Member-Secretary DR R. BHASKAR S&R[ A. V. Dhanbad Coal India Ltd. SHARMA (Alternate) DR K. VISHWANAIHAN Supplied by Book Supply Bureau to CSIR E JOURNALS Consortium for internal use by subscribing member only. S. PATEL SHRI RAM GOPAL SHRI C. Calcutta Industrial Toxicological Research Centre. Calcutta National Organic Chemical Industries Ltd. Lucknow Indian Oil Corporation Ltd (R&D Centre). NAND (Alternate) SHRISATINDER KUMAR MAIRA SHRI SANTANU KUMAR(Alternate) DR A. CHD 32 Representing Central Pollution Control Board. K. Ministry of Industry. Faridabad Ministry of Environment and Forest. Ahmadabad National Thermal Power Corporation Ltd. L. Mumbai The Fertilizer Association of India.IS 11255 Part 6 ) : 1999 ( ANNEX A (Foreword) COMMITTEE Air Environment Chairman Stiar DIUPBISWAS Members DR B. NIGAM REPRESEIWAT~VE COMPOSITION Protection Sectional Committee. New Delhi The Dharamsi Moraxji Chemical Company Ltd.. (Alternate) REPRESENTATIVE SHRIR. New Delhi Steel Authority of India Ltd. SHRI JANARDAN SINCH (Alternate) REPRESENTATIVE DR 9. Delhi Bhabha Atomic Research Centre. SWAMINATHAN DR S. MAHADEVAN (Alrernate) SHRID. Delhi Central Pollution Control Board. New Delhi Director General. Director (Chem) . New Delhi National Environmental Engineering Research Institute. S. Mumbai Central Mining Research Institute. G. N. K. M. K. New Delhi Confederation of Indian Industry. SHASTRI SHRI N. S.
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