ID: 909160045nromoef.gov.in/Environment_Reports/Reports/4-814-2010-RO... · Web viewSilver nitrate (0.0141 N): Dissolve 2.395 gm AgNO3 and dilute to 1000 ml standardize against NaCl,

Environmental Monitoring at DLF Emporio Mall, Vasant Kunj, New Delhi

INTRODUCTION

The Environmental Monitoring was carried out by the environment team of Spectro Analytical Labs Ltd. at DLF Emporio Mall, Vasant Kunj, New Delhi. Being a construction and development company DLF is very much concern about to reduce the environmental impact due to its Operational and Constructional activity. The present work is to concerning the existing environmental condition with respect to water, waste water, air and noise levels. Environmental monitoring programme is a vital process of any management plan of the operational & development. This helps in signaling the potential problems that resulting from the project and will allow for prompt implementation of effective corrective measures. The environmental monitoring will be required for the construction and operational phases. The main objectives of environmental monitoring area are:

To assess the changes in environmental conditions,

To Monitor the effective implementation of mitigation measures,

Warn significant deteriorations in environmental quality for further prevention action.

In order to meet the above objectives the following parameters need to be monitored: Water Quality ,

Ambient Air and Noise quality

Scope of work and the detail of the sampling are given in following pages.

Spectro Analytical Labs Limited New Delhi Page 1 of 37


SCOPE OF WORKThe scope for performing the environments monitoring is already mentioned in the work order, which is briefly given for ready reference.

Site Visit for Physical verification of the current status of construction and compliance to stipulated conditions in the Environmental Clearance (EC) order/letter

Consultation with the site in-charge as well as the design in-charge to identify the gaps between the actual status and EC conditions assist in the preparation of six-monthly reports

During construction stage, the following on-site monitoring to be carried out:

a) Monitoring of Soil at the project site

b) Collection and Analysis of the Groundwater from the project site

c) Monitoring of Ambient air quality for the parameters namely PM 10, PM 2.5, Sulphur dioxide (“SO2”) & Oxides of Nitrogen (“NO2”), Carbon Monoxide (“CO”), Ozone (“O3”), Lead (“Pb”), Ammonia (“NH3”), Benzene (“C6H6”), Benzopyrene (“BaP”), Arsenic (“As”), and Nickel (“Ni”), at the project siteMonitoring of Ambient Noise Level Monitoring (24-hrs, day & night Leq) at two locations (one at the project site & other within the boundary of the project site).

During operation stage the following on-site monitoring to be carried out:

1. Monitoring of DG stack emission from project site

2. Monitoring of DG Noise level (inside the DG room and 0.5 m away from the DG room)

3. Collection and Analysis of Wastewater (Influent & effluent) samples of Sewage Treatment Plant (STP) from the project site.

4. Monitoring of Ambient air quality for the parameters namely PM 10, PM 2.5, Sulphur dioxide (“SO2”) & Oxides of Nitrogen (“NO2”), Carbon Monoxide (“CO”), Ozone (“O3”), Lead (“Pb”), Ammonia (“NH3”), Benzene (“C6H6”), Benzopyrene (“BaP”), Arsenic (“As”), and Nickel (“Ni”), at the project site

5. Monitoring of Ambient Noise Level Monitoring (24-hrs, day & night Leq) within the project boundary.



INSTRUMENTS & APPARATUSAir (Particulate Matter, PM 10) Monitoring Instrument

Instrument Make Model No. InstrumentIdentification

No.

Range and Sensitivity

SPM/RSPM Gases

Respirable Dust

Sampler (RDS)

M/s. Spectro Instruments Pvt. Ltd. – New Delhi

SLE -RDS 103/SLE -GA 133

SAL/RDS/10 0.02 – 01.8 m3/min±0.02

m3/min

0.2 – 3 LPM

± 0.2 LPM

Filter Paper Details

APPRATUS MAKE SIZE SIZE PRODUCTCATEGORY NO.

Filter Paper M/S Whatmann International Ltd.

20.3 x 25.4cm GF/ACAT NO. 1820-866

Air (Particulate Matter, PM 2.5) Monitoring Instrument

Instrument Make Model No. InstrumentIdentification

No.

Range and Sensitivity

PM

Fine Particulate Sampler

M/s. Spectro Lab

Equipments Pvt. Ltd.

SLE-FPS 105

SAL/FPS/01&2 16.67 LPM

Filter Paper Details

APPRATUS MAKE SIZE SIZE PRODUCTCATEGORY NO.

Filter Paper M/S Whatmann International Ltd.

47 mm GF/A & EPM 2000



Noise (Sound) Measuring InstrumentInstrument Make Model No. Instrument

IdentificationDetection

LimitIntegrated Sound Level Measurement Instrument Standard Accessories

Baseline Technologies

2001A0907-980

SAL/NOISE/INT/692

Lo 30-100dBHi 60-130dB



Testing Methods Followed


S.No. Particular Testing Method to be Followed

1 Ambient Air Monitoring ParameterA PM 10 IS-5182 (part – 23) 1973, Handbook of Methods in

Environment Studies (Vol 2) Published by ABD Publication

– Jaipur

B PM 2.5

C SO2 (Sulfur Dioxide) IS 5182 (Part – II) 1969, with Improved West & Gaeke

MethodD NO2 (Nitrogen Dioxide) Modified Jacobs – Hochheiser Method / Arsenite Method

E Carbon Monoxide (as CO),

(mg/m3)

Gas Chromatography

F Ozone (as O3) (µg/m3) Chemical Method

GLead (as Pb) (µg/m3)

AAS Method after sampling on EPM 2000 or equivalent

filter paper

H Ammonia (as NH3) (µg/m3) Chemiluminescence

I Benzene (as C6H6) (µg/m3) Gas chromatography based continuous analyzer

J Benzo (O) Pyrene (as BaP)

(ng/m3)

Solvent extraction followed by HPLC/GC analysis

K Arsenic (as As) (ng/m3) AAS Method after sampling on EPM 2000 or equivalent

filter paperL Nickel (as Ni) (ng/m3)

2 Noise Level MeasurementA Noise Level in dB (A) for

continuous 24 hours

Operational Manual of Noise level Meter, Model No. SL

5868 issued by Baseline Technologies

3 Water Analysis

Standard Method for the Examination of Water & Wastewater, 21st Edition, Edited by Lenore S. Clesceri,

Arnold E. Greenberg, Andrew D. Eton is followed for analysis.

4 Soil Analysis: As per Protocol: FAO / IS: 2720


Abbreviations used in the Report

RSPM = Respirable suspended particulate Matter (< 10 micron sized particle)

SPM = Suspended Particulate Matter

GL = Ground Level;

SO2 = Sulfur Dioxide

NO2 = Nitrogen Dioxide

AAQ = Ambient Air Quality

CO = Carbon Monoxide

DW = Drinking Water

WW = Wastewater



RESULTS OF AMBIENT AIR QUALITY




ID: 1110050061 Ambient Air Analysis Report

Name of the Project - REGENCY PARK PROPERTY MANAGEMENT SERVICES

PRIVATE LIMITED, “Emporio-Shopping Mall” at Plot No. 4,Vasant Kunj, Nelson Mandela Road, New Delhi

Name & Address of the Company - DLF Centre, 9th Floor, Sansad Marg, New Delhi- 110001.Name of the Site - Vasant Kunj (Emporio Mall)Location of Sampling Point - Near the Garden Area of MallDate of Sampling - 16.10.2011Sampling Started at - 3.00 PM (16.10.2011)

.201 Sampling Completed at - 3.00 PM (17.10.2011)Actual Time of Sampling (minutes) - 1440Av. Flow Rate for SPM (m3/min.) - 1.11Total Volume of Air Sampled for SPM (m3)

- 1584Average Ambient Temperature (oC) - 27Purpose of Monitoring - To Assess Pollution Load

PARAMETERS RESULTS Limits as per CPCB (MOEF)

Industrial,Residential, Rural

& other areas

Ecologically SensitiveArea (notified by

Central Government)

Particulate Matter PM 2.5 (µg/m3) - 72 60 60Particulate Matter PM 10 (µg/m3) - 112 100 100Sulphur Dioxide (as SO2) (µg/m3) - 8.3 80 80Oxides of Nitrogen (as NO2) (µg/m3) - 28.3 80 80Carbon Monoxide (as CO), (mg/m3) - 1.34 02 02Ozone (as O3), (µg/m3) - 27.3 100 100Lead (as Pb), (µg/m3) - N.D. 1.0 1.0Ammonia (as NH3), (µg/m3) - 18.4 400 400Benzene (as C6H6), (µg/m3) - N.D 05 05Benzo (O) Pyrene (as BaP), (ng/m3) - N.D 01 01Arsenic (as As) (ng/m3) - N.D 06 06Nickel (as Ni) (ng/m3) - N.D 20 20

Protocol – IS: 5182 (Pt - 4, 6 & 23) / IS: 2488, IS-13270


RESULTS OF NOISE MONITORING



ID: 1110050061AMBIENT NOISE MONITORING REPORT (DLF Emporio)

Location : Near The Garden AreaDate : 16/10/2011 to 17/10/2011


Time Hourly LeqdB (A) Result dB (A)

MIDNIGHT 55.2 Leq(24) 61.7

1:00 AM 53.6 L10 65.82 51.6 L50 64.43 51.4 L90 62.34 48.0 Lday 62.85 48.0 Lnight 58.36 49.7 Ldn 65.47 49.5 Lmax 66.08 50.9 Lmin 48.09 54.910 58.011 61.5

12 NOON 63.313 64.614 65.615 65.816 64.1 17 64.618 66.019 65.620 63.221 63.522 61.8 23 58.5

Area Category of Area Limits in day (dB) Limits in Night (dB)A Industrial 75 70B Commercial 65 55C Residential 55 45D Silence Zone 50 40


RESULTS OF WATER ANALYSIS



ID: 1110050061

(Inlet Water of STP – Emporio)

S.No Tests Results Protocol

1. pH Value 7.08 IS-3025 (Pt-11): 1984

2. COD, mg/l 397.21 APHA 5220-(COD)-C

3. BOD (at 270C for 3 days), mg/l 138 IS-3025 (Pt-44): 1993

4. Total Suspended Solids, mg/l 220 APHA 2540-Solids-D

5. Total Dissolved Solids, mg/l 1790 IS: 3025 (Pt-16): 1984

6. Oil & Grease, mg/l 11 APHA 5520–(O & G)-B

( Outlet Water of STP – Emporio)

S.No Tests Results Protocol

1. pH Value 7.78 IS-3025 (Pt-11): 1984

2. COD, mg/l 27.13 APHA 5220-(COD)-C

3. BOD (at 270C for 3 days), mg/l 10 IS-3025 (Pt-44): 1993

4. Total Suspended Solids, mg/l 8.0 APHA 2540-Solids-D

5. Total Dissolved Solids, mg/l 2124 IS: 3025 (Pt-16): 1984

6. Oil & Grease, mg/l 4.0 APHA 5520–(O & G)-B



ID: 1110050061

RESULTS OF RAW WATER AS PER IS: 10500-1991 (DLF Emporio)

TESTS RESULTS LIMITS (MAX) PROTOCOLSDesirable Extended

Colour, Hazen Units

<5.0 5 25 IS- 3025(Pt-4): 1983

Odour Unobjectionable Unobjectionable IS- 3025(Pt-5): 1983

Taste Agreable Agreeable IS- 3025(Pt-7&8): 1984

Turbidity, NTU

<1.0 5 10 IS- 3025(Pt-10): 1984

pH Value 7.45 6.5 to 8.5 IS- 3025(Pt-11): 1984

Total Dissolved Solids, mg/l

508 500 2000 IS- 3025(Pt-16): 1984

T. Hardness (asCaCO3), mg/l

164 300 600 IS- 3025(Pt-21): 1983

Residual Free Chlorine, mg/l

0.1 0.2 (Min) When Chlorinate 45 of IS-3025: 1964

Chlorides (as Cl), mg/l

156.54 250 1000 IS-3025(Pt-32): 1984

Total Iron (as Fe), mg/l

0.10 0.3 1.0 32 of IS- 3025: 1964

Fluorides (as F), mg/l

0.34 1.0 1.5 APHA-4500-D-F

BACTERIOLOGICAL TESTS

TESTS RESULTS LIMITS PROTOCOLSColi form Organism/100ml (MPN)

<2.0 10 (Max) IS: 1622-2003

E. Coli/100ml Absent Absent IS: 1622-2003



MONITORING AND ANALYSIS METHODOLOGY

The IS methods are followed to decide the monitoring stations, analysis of different sample and

also alternative methods are used, where the cross verification is required.

[A] Ambient Air Quality Monitoring:Two Respirable Dust Samplers (RDS) with gaseous attachment have been used for RSPM/SPM

Sampling. RDS with Gaseous attachment assembly is used for the collection of gaseous

pollutants such as SO2, NO2 and CO. The details of the instrument used for sampling is

mentioned in the separate annexure under the heading of details of Instruments & Apparatus. For

the measurement of fine particulate matter having an aerodynamic dia. Less than or equal to a

nominal 2.5 micrometer (PM2.5). Draw ambient air at a constant flow rate of 16.67 Lpm .Total

volume of the sampled air is automatically computed by the sampler from the measured

sampling flow rate .the mass concentration of PM 2.5 particles in the ambient air is computed by

dividing the total mass of collected particles by the total volume of sample air and is expressed

in micro grams per cubic meter of air.37mm glass fiber filter and 1 ml of diffution oil or silicon

oil.

For the collection of PM2.5 particulate matter we use 47mm PTFE (polytetrafluoro ethylene).

The ambient air enter the sampler air inlet and pass through the size selective inlet particles

larger then 10micro are separated . it then moves through down tube to the impacter where

particles larger then 2.5 micro are cut off.the particles smaller then 2.5 micro are then collected

on a filter paper (47mm PTFE ) mounted in a filter cassette and kept in a holder .

[B] Water Quality Survey: Water samples were collected in Pre-sterilized sampling container. Chemical and Bacteriological

analysis was carried out as per standard Methods for water and Wastewater Analysis, Published

by IS, APHA, etc.

[C] Noise Level Measurement:

Instant sound level meter is used for the collection of data related to noise for continuous 24

hours and for D.G. Set. The details of the instrument used for the sampling is mentioned in the

separate annexure under the heading of Details of instruments & Apparatus.



METHODOLOGY OF AMBIENT AIR QUALITY



RESPIRABLE PARTICULATE MATTER

PrincipleAmbient air laden with suspended particulates enters the system through the inlet pipe. As the air passes through the cyclone, coarse, non-Respirable dust is separated from the air stream by centrifugal forces acting on the solid particles. The separated particles fall through the cyclone’s conical hopper and collected in the sampling bottle placed at its bottom. The fine dust forming the repirable fraction of the total suspended particulate matter passes through the cyclone and is carried by the air stream to the filter paper clamped between the top filter cover and the filter adopter assembly. The respirable dust is retained by the filter and the carrier air exhausted from the system through the blower.

RESPIRABLE SIZE CUT OFFThe repirable dust standard recommended by the Central pollution Control Board is a 10 micron cut off size for respirable dust measurement. Moreover, the respirable tract like any other inspection centrifugal separation system retains particulates with varying densities at different levels. This implies that even relatively finer dust particles of materials having a higher specific gravit5y are likely to be retained in the upper respiratory tract while large particulates of lighter materials are likely to pass deeper into the respiratory system.II) Procedure of sample collection:Following steps are involved in the collection of samples;

a) Open the shelter of Respirable Dust Sampler (RDS), loosen the wing nuts and remove the retaining ring from the filter holder.

b) Mount a pre-weighted and numbered glass fibers filter paper in position with the rough side up and tighten the wing nuts.

c) Allow the RDS to run for the specified length of time (24 hrs)d) During the sampling time, flow rate should be taken hourlye) At the end of sampling remove the filter form the mount very carefully.f) Fold the filter in half upon itself with the collected materials enclosed within.g) Place the folder filter in a clean, tight envelope and mark it for identification.h) Place the filter in a desicator.

ANALYSIS OF SAMPLES:In a lab. remove the filter from the desicator and take out the filter paper from the envelope. Examine the inside surface of filter paper and with the pair of tweezers; remove any accidental objects such as insects. Dry the filter paper by keeping on watch glass in hot air oven at 1050 C for about one hour. Equilibrate the exposed filters for about one hour in desicator. Carry the desicator to the balance and weight on the analytical balance to the nearest 0.1-milligram.

I) Calculation of volume of air sampled:V =Q x TWhere V= Air volume sampled (m3 )Q = Average flow rate ( m3 per minute)T = Sampling Time (in minutes)



Q = (Q1 + Q2) 2

Q1 = Initial sampling rate indicated by the orifice meter at the start of samplingQ2 = Final sampling rate indicated by the orifice meter just before the end of sampling.

II) Calculations of mass concentration of Responded particulate Matter (RPM):The mass concentration of RPM may be calculated as follows:

(Fw – Iw) x 106

RPM (μg/m3) = -------------------- V

Where Fw = Final weight of exposed filter paper in grams.Iw = Initial weight of unexposed filter paper in grams.V = Air volume sampled in cubic meter.

Weight of dust retained by the cyclone SPM (μg/m3) = RPM (μg/m3) + ------------------------------------------- Volume of air sampled, m3



METHODS FOR DETERMINATION OF OXIDES OF NITROGEN IN AMBIENT AIR

PrincipleThe collection and fixation of nitrogen dioxide in air is done by scrubbing a known volume of air through a solution of basic sodium arsenate. The absorbed nitrogen dioxide is determined calorimetrically as the azo dye by using it to diazotize sulphanilamide in the presence of phosphoric acid at a pH of less than 2 and then coupling it with N-(1-Naphthyl)-ethylenediamine dihydrochloride. The method is standardized statically by using NaNO2 standard. Standardization is based upon the empirical observation that 0.74 mole of NaNO2 produces same colour as 1 mole of NO2. The absorbance of the highly colored azo dye is measured on a spectrophotometer at a wavelength of 540 nm.

Range and SensitivityAnalysis in the range of 0.04 to 2.0 μg/ml can be performed by this method. The monitoring range of the method is 9 to 750 μg/ml. However, under certain conditions, with a sampling rate of 2.0 LPM for 24 hours, a sampling efficiency of 82% the range of the method is 9 to 450 μg/m3. Nitrogen dioxide in the range of 420-750 μg/m3 is accurately measured by 1.1 dilution of the collected sample.

THE GASEOUS SAMPLING ATTACHMENTSA trapping is drawn from the suction side of the blower below the orifice plate assembly to provide suction for sampling air through a set of impingers. These impingers are housed in a separate enclosures and kept in an ice tray.The separate enclosure and ice tray insulate the impingers from ambient temperature and heat generated in the motor of the blower. It has Gas Manifold and Rotameter to allow setting up of independent sampling rates through each of impingers.The gaseous sampling attachment can easily be detached from the main sampler and transported and stored independently.

CALCULATIONI) The concentration of nitrogen dioxide in microgram per meter cube in the sample

may be calculated as follows: (A-Ao) x F x Vf NO2 (μg/m3 ) = --------------------- Va x Vt x 0.82

Where A= Sample AbsorbanceAo= Reagent blank absorbance

INTERFERENCESulphur dioxide is a major interference due to nitric oxide is positive while that due to carbon dioxide is negative. Interference from sulphur dioxide can be eliminated by converting it to sulphuric acid by the addition of hydrogen peroxide.



SULPHUR DIOXIDE

Principle:When sulphur dioxide from the air is absorbed in a sodium tetrachloromercurate solution it forms a stable sodium dichloro-sulphitomercurate solution. The amount of sulphur dioxide is then estimated by the colour produced when pararosaniline hydrochloride is added to the solution. The magenta colour is produced and estimated at 560 nm.

Range & SensitivityThe measurement should be reported to the nearest 0.005 ppm at concentration below 0.15 ppm and to the nearest 0.01 ppm above 0.15 ppm.

Interference Ozone and nitrogen dioxide interfere if presents in the air sample at concentration greater than sulphur dioxide. Interference of nitrogen dioxide is eliminated by adding 0.06 percent sulphamic acid in the absorbing reagent. Nitrogen dioxide interference may also be eliminated by adding 0.1 tuluidine after sample collection. Heavy metals interfere by oxidizing dichloro-sulphitomercurate during sampling collection. The interference is eliminated by adding EDTA in the absorbing reagent.

Procedure for gaseous sampling

8 hour sampling:Place 30 ml of Tetra-Chloro-Mercurate (TCM) absorbing solution in the standard impinger. Connect the sampling tube leading for manifold of High Volume Sampler. Check the flow rate from rotameter; maintain the flow rate to accurately 1 LPM throughout the sampling period. Shield the absorbing reagent from the direct sunlight during the sampling and after sampling. During hot weather sampling is to be conducted by keeping the impingers impregnated in ice cubes.

24 hourly samplingPlace 50 ml of (TCM) solution in a large impinger and collect the sample at 1 LPM. Determine the air volume by multiplying the airflow rate by the time in minutes. The solution after the sample collection are relatively stable. At the temperature of 250C and above, the losses of SO2

occurs. Therefore, it is advisable to store the samples at 50 C till the analysis.

Analysis of samplesAfter receiving the sample in the lab. check the volume of absorbing media and record it. Normally the volume of absorbing reagent is likely to be reduced as a result of evaporation losses. Make up the evaporation loss by adding fresh, boiled cooled distill water.Pipette 10 ml of aliquot from the sample into a 25 ml volumetric flask. Prepare a blank solution by measuring 10 ml of unexposed Tetra-Chloro-Mercurate (TCM) solution into 25 ml volumetric flask. Then add 1 ml sulphamic acid and allow to stand for 10 minutes for reaction, then ad 2 ml of formaldehyde and 2 ml of working parasaniline solution. Mix up thoroughly and make up it with freshly boiled and cooled distilled water to the volume. Take absorbance of the sample after 30 minutes at 560 nm on a spectrophotometer after setting the spectrophotometer at 0.00 absorbance with blank.



CalculationI) The concentration of sulphur dioxide in microgram per meter cube in the sample may

be calculated as follows: (A-Ao) x F x Vf SO2 (/m3) = ---------------------- Va x Vt

A= Sample AbsorbanceAo = Reagent blank absorbanceF = Calibration factor (g / absorbance unit)Vf = Final volume of Sample (ml)Va = Volume of air sampled (cubic meter)Vt = Volume of sample taken for analysis

II) Conservation of microgram/m3 sulphur dioxide to parts per million (PPM) may be calculated as follows:

SO2 ppm = g SO2/3 x 3.82 x 10-4



Ammonia (as NH3)

Principle: Ammonia is collected in 0.1 N Sulphuric Acid Solution (H2SO4) in a midget impinger to form ammonium sulphate. The solution reacted with nessler reagent to produce a yellow brown complex & determine by colorimetric method at the wavelength 440 nm.Procedure: Sampling: Take 20 ml of absorbing solution in midget impinger. Attach the impinger to air sampling pump & draw air through impinger at a rate of 1 lpm for 1hr to 24 hrs. Record the volume of air sample. Analysis: Take the sample in 50 ml volumetric flask containing 2 ml of alkaline tartrate and makeup to the mark with distilled water. Add 2 ml of nessler reagent to the flask & determine absorbance after 10 minutes at 440 nm in a spectrophotometer. Treat the blank in the same manner as the sample.Calculation: Ammonia, g/m3 = Abs ́ F ́ 10 6

VF- FactorV- Volume of air sampled, liter 106 – Conversion from liter to cubic meter

Carbon monoxide (as CO)

SAMPLING: Take the gaseous sample into a bladder through a suction pump.

ANALYSIS: Analyze it on the Gas Chromatograph.

CALCULATION:

Concentration of CO (ppm) = Sample Area x conc.of CO2 in Standard x vol. of standard

Standard Area x vol. of sample

Ozone in Ambient Air (O3)

Principle: Micro amounts of ozone and other oxidant librated iodine when absorbed in a 1% solution of potassium iodide buffered at pH 6.8 ± 0.2. The iodine is determined spectrophotometrically by measuring the absorption of triiodide ion at 352 nm.

Range and Sensitivity: This method covers the manual determination of oxidant concentration between 0.01 to 10 ppm (0.019-19.6mg/m3) as Ozone.

Reagent: 1. Double Distilled Water2. Absorbing Solution: (1% KI in 0.1 M Phosphate Buffer). Dissolve 13.6 gm of potassium

dihydrogen phosphate (KH2PO4), 14.2 gm of disodium hydrogen phosphate (NaHPO4) or 35.8 gm of the dodecahydrate salt (NaHPO4.12H2O) and 10 gm of potassium iodide in sequence and dilute the mixture to 1 lt with double distilled water.



3. Stock Solution: (0.025M) I2 Dissolve 16gm potassium iodide and 3.173gm of resublimed iodine successively and dilute the mixture to exactly 500ml with DDW.

4. 0.001M I2 Solution: Take 4ml of the 0.025 M stock solution into a 100ml low volumetric flask and dilute to the mark with absorbing solution.

5.Procedure:Take 10ml of the absorbing solution to a midget impinger. Sample at 0.5 to 3 l/m for up to 30 minutes. Calculate the total volume of the air sample, also measure the air temperature and pressure. Do not expose the absorbing reagent to direct sunlight.

Analysis: If appreciable evaporation of the absorbing solution occurs during sampling, add double distilled water to bring the liquid volume to 10ml.Within the 30 to 60 minutes after sample collection, read the absorbance in a cuvette at 352 nm against a reference cuvette containing DDW.Measure the absorbance of the unexposed reagent and subtract the value from the absorbance of the sample.

Calculation: The concentration of O3 (ppm) = Total µl ozone per 10 ml Volume of air sample in liter



Lead in Ambient Air (as Pb)

Principle of the Method: Airborne dust samples are collected on cellulose membrane filters (EPM 2000). The filters samples are ashed using nitric acid to destroy the organic matrix and solubilize the lead. The lead content of the ashed material is determined by atomic absorption spectroscopy.

Range and Sensitivity: By atomic absorption the detection limit for lead in aqueous solution about 0.1 g/ml. assuming the ashed sample is diluted to 10 ml this would correspond to 1 g of lead/filter. The optimum working range for Pb extends up to about 10 g/ml.

Reagents: 1. Purity. ACS reagent grade chemicals or equivalent shall be used in all tests. References to

water shall be understood to mean double distilled water or equivalent.2. Care in selection of reagents and in following listed precautions is essential if low blank

values are to be obtained.3. Conc. Nitric acid (68 to 71%) redistilled specific gravity 1.42.

Nickel in Ambient Air (as Ni)

Principle of the Method: Samples are collected by drawing a known volume of air through a membrane or glass fiber filter. The filter samples are ashed, extracted with acid, and the analysis is subsequently made by atomic absorption spectroscopy using 23.9 nm nickel line.Range and Sensitivity: This method is applicable to the determination of nickel in quantities of 0.1 to 20 g of nickel/ml of solution.Reagents:

1. Purity. ACS reagent grade chemicals or equivalent shall be used in all tests. References to water shall be understood to mean double distilled water or equivalent.

2. Care in selection of reagents and in following listed precautions is essential if low blank values are to be obtained.

3. Conc. Hydrochloric Acid (36.5 – 38.0%).4. Conc. Nitric Acid (69.0-71.0%).5. Nickel Shot.6. Perchloric acid 72%.7. Hydrochloric acid 1:10. Dilute 100 ml of conc acid to one liter with water.8. Perchloric-Nitric acid Mixture. Add 10 ml of conc perchloric to 90 ml of conc nitric.9.

Benzo[a]Pyrene (BaP) in Ambient AirPrinciple of the Method: This rapid method, for the measurement of Benzo[a]Pyrene (BaP) in air samples, is based on the chromatographic separation of air samples extracts on and activated alumina column using a polar solvent, toluene, as the eluting agent. The concentration of hydrocarbon in the eluates is determined from fluorescence emission measurements made on the eluates.

Range and Sensitivity: The method can measure concentrations in a prepared air sample extract or fraction over the range of 0 to 0.25 micrograms of BaP of solution.



Reagents: 1. Cyclohexane. Spectrograde Cyclohexane.2. Activated carbon.3. Alumina. 100 to 200 mesh size, is heated for 24 hrs in an oven at 1400C before use.4. Toluene. 5. Benzo[a]Pyrene(BaP).6. Standard solutions of BaP. Solutions of BaP are prepared containing 0.005, 0.010, 0.015,

0.020 and 0.025 g/1ml in fluorescence-free toluene. Weigh accurately 1.25 mg of BaP on a micro balance and dissolve in 250 ml of Spectrograde toluene. Measure accurately 1.0 ml of this stock solution and dilute to 1000 ml with Spectrograde toluene. Repeat this with 2.0, 3.0, 4.0 and 5.0 ml portions of stock solution, diluted in each case to 1000 ml.

Procedure: The chromatographic columns are setup in a fume hood and complete preparation of column and elution procedure is carried out there. Fluorescence readings are made while the elutions are in progress.Using a clean metal punch of cork borer, 4 corcles of 35.5 mm diameter are cut from the high volume glass fiber sample. These represent 1/10.5 of the total effective area of the filter. These are placed in a microsoxhlet extractor on top of a wad of glass wool which prevents the carbon particles from being washed over into the extract and avoids subsequent filtration. The area chose, in this case, amounts to ca 10% of the filter. After 6 to 8 hr extraction with fluorescence-free cyclohexane, the solvent extract is evaporated carefully in a current of nitrogen to 2 ml.A chromatographic column is then prepared by slurrying the activated alumina with toluene and filling the tube to a depth of 12.0 cm. the concentrated extract is placed on the alumina and after rinsing with a further 1 ml of toluene, elution os carried out using toluene from beginning to end. The first 25 ml of eluate are discarded and 3 ml fractions are collected thereafter up to a total of about 30 fractions. Each fraction is scanned separately in the fluorimeter and those fractions containing BaP and BkF are combined for further measurement.Having combined all the fractions containing BaP and BkF, these are carefully evaporated and made up to a final volume of 5.0 mol in toluene. Fluorescence emission measurements of peak heights are now made using excitation wavelength 307 and 384 nm.A blank determination is carried out on the glass fiber filter, glassware and reagents.Calibration and Standards: Standards curves of fluorescence emission, in arbitrary units, are prepared for the various concentrations of both BaP and BkF at the two exciting wavelengths 384 and 307 nm. i.e., the optimum excitation wavelengths for BaP and BkF. These are prepared by plotting the height of the peaks against the concentration. The fluorescence emission intensities of air sample extracts or fractions are also measured using the same two exciting wavelengths.Similar calibration curves are obtained when standard solutions are made up in eyelohexane. The sensitivity is noticeable less in toluene than in cyclohexane solution. The emission of BaP with 384 excitation, is higher than the emission of BkF with 384 excitation, so that the toluene based BaP measurement is somewhat better than a measurement made in cyclohexane.Calculation:Since the fluorescence emission intensity of BkF is much greater than that of BaP when a mixture of the two is excited at 307 nm, the reading at this wavelength is essentially due to BkF. Having determined the concentration of BkF, one can calculate the effect of this hydrocarbon when a mixture is excited at 384 nm after which the BaP concentration may be calculated. Thus:-

The concentration of BkF (g/ml) = Emission of Sample at 307 nm excitation



Slope of BkF standard curve at 307 nm excitation

The concentration of BaP (g/ml) = Emission of Sample at 384 nm – (conc. BkF X Slope BkF standard curve at 384 nm excitation)

Slope of BaP standard curve at 384 nm excitation



METHODOLOGY OF WATER ANALYSIS



METHODOLOGY OF PHYSIO-CHEMICAL ANALYSIS OF WATERpHFor most practical purposes, the pH of aqueous solutions can be taken as negative logarithm of hydrogen ion activity. pH values from 0 to 7 are disminishingly acidic, 7 to 14 increasingly alkaline and 7 is neutral.The pH of nature water usually lies in the range of 4.4 to 8.5. its value is governed largely by the carbon dioxide / bicarbonate / carbonate equilibrium. It may be affected by humic substances by changes in the carbonate equilibria due to the bio-activity of plants and in some cases by hydrolysable salts. The effect of pH on the chemical and biological properties of liquids makes its determination very important. It is used in several calculations in analytical work and its adjustment is necessary for some analytical procedures.The determination of pH by conventional chemical means is not practicable and the equilibria, which are involved, depend to some extent temperature. The precise accepted scale of pH must therefore be based on an agreed primarily standard. The colorimetric indicator methods can be used only if approximate pH values are required. The pH determination is usually done by electrometric method, which is the most accurate method and free of interferences.Electrometric Method:The pH is determined by measurement of the electromotive force of cell comprising an indicator electrode (an electrode responsive to hydrogen ions such as glass electrode) immersed in the test solution and a reference electrode (usually a mercury calomel electrode) contract between the test solution and the reference electrode is usually achieved by means of a liquid junction, which forms a part of the reference electrode. The emf of this cell is measured with pH meter. This is a high impedance electrometer calibrated in terms of pH.Apparatus:Glass Electrode:This must be compatible with the pH meter used and must be suitable for the particular application. Special electrodes are available for pH values greater than 10 and for use at temperature greater than 600 C. combined glass/reference electrodes are also available and are convenient to use.Reference Electrode:The mercury/ calomel electrode is widely used but the silver/ silver chloride electrode may be preferably on account of it being more reproducible and more reliable. Less concentrated solutions of KCL (3.5 M KCL or 350 gm/litre) are more satisfactory as filling solutions than the saturated solution often used because problems due to logging of the electrode or the liquid junction will be avoided. To prevent dissolution of the silver chloride film, the potassium chloride filling solution of Ag/ AgCl electrodes should be saturated with AgCl.PH Meter:Both mains and battery operated models are available, the alter type can be used for field measurements. The most accurate pH meters can be read to better than ± 0.005 pH unit.Reagents:1.Buffer solution for pH 4.0: Dissolve 10.12 gm potassium dihydrogen phthalate dried at 1100

C in freshly distilled water and dilute to one litre at 250C.2. Buffer solution for pH 6.8: dissolve 3.388 gm anhydrous KH2PO4 and 3.533 gm Na2HPO4

both of which have been dried overnight at between 1100C and 1300C in water an dilute to 1 litre at 250C. The distilled water should be freshly boiled, cooled and free from CO2.



3. Buffer Solution for pH 9.2: Dissolve 3.80 gm Na2B4O7. 10 H2O in water dilute to 1 litre to 250C.NOTE: In general analytical reagent grade chemicals are satisfactory for the preparation of these solutions. Commercial buffer tablets are available in the market for the preparation of solution of above pH values (Each tablet dissolved in 100 ml gives the buffer solution of required pH).Procedure:1. Standardize the pH meter according to the manufacture’s instructions.2. Select a standard buffer solution with a pH value close to that of the water to be tested.3. Set the temperature control to the temperature of the buffer.4. Set the meter to the pH of the buffer at that temperature.5. Check the electrode response by measuring a second standard buffer solution of different pH.6. Wash the electrode thoroughly first with distilled water and then with the sample.7. Set the temperature control to the temperature of the sample.8. Immerse electrodes in the sample and record the pH after stabilizing the system.Note:Between measurements, the electrodes are kept in distilled water. New or dried out glass electrodes should prepared for the use by soaking in 0.1 N HCL for 8 hours or according to the maker’s instructions.

COLOUR

Out line: Colour is measured by visual comparison of the sample with colour standard. One unit of colour is that produced by 1 mg of platinum per litre in the form of chloroplatinate ion.

Procedure: Prepare standard colour solution of various Hazen units by diluting standard chloroplatinate solution with distilled water to 50 ml, observe the colour of the sample by filling a matched nessler cylinder to the 50 ml mark with water and compare it with standard.

Calculation: Colour unit = (50 x A)/ B

Where, A = Estimated colour of diluted sampleB = Volume in ml of sample taken for dilution

ODOUR

Out line: The type of odours present in water & wastewater will vary widely. The types of odour shall be described by judging the degrees of sweetness, pungency, smokiness and rottenness of the odour.

Procedure: As soos as possible after collection of sample, fill a bottle half full of sample, insert the stopper and shake for 2-3 second and then quickly observed the order. The sample taken observation of odour shall be at room temperature.



TASTE

Procedure: Prepare dilution series, take the 15 ml sample in a 50 ml beaker and pair each sample with known blank sample and present to each panelist. Ask the panelist to hold water at 400C in as much quantity as is comfortable to several second and discharg it with out swallowing.

TURBIDITY

Outline: It is based on comparison of the intensity of light scattered by the sample under defined conditions with the intensity of light scattered by a standard reference suspension under the sample conditions. The higher the intensity of scattered light, the higher the turbidity.

Procedure: Shake the sample to disperse the solids wait until air bubbles disappear. Pour sample into turbidity meter tube and read turbidity directly from the instrument scale, which is calibrated by standard solution.

TOTAL DISSOLVED SOLIDS (FILTRABLE) SOLIDSPrinciple:A known volume of filterable sample is evaporated and dried in a weighing dish at 1050 C to constant weight the increase in weight over the empty dish represent the dissolved solids.Apparatus:1. Evaporating dishes, 50, 100ml capacity (Preferably porcelain or silica).2. Pipettes 25, 50 ml capacity.3. Water bath and oven.4. Balance to weigh up to 4th decimal.Procedure:The known volume (V) of filtered sample in a previously ignited and weighted basin (W1). Evaporate to dryness on a steam bath and further dry at 1500 C for one or two hours in an oven. Cool in desicator and weight (W2). Repeat by further heating for 15 minutes and cooling unit successive results do not differ by more than about 0.4 mg.Calculation:

Dissolved solids mg/l = (W2 – W1) x 1000 V

Where W2 = Weight of residue and dish W1 = Weight of empty and dry dish V = Weight of sample



(TSS)TOTAL SUSPENDED SOLIDSProcedure: Take well-mixed 100 ml sample and filter through a pre-weighed standard glass

fiber filter paper and the residue retained on the filter is dried to a constant weight at 103 to 1050C. The increase in weight represents the total suspended solids.

(BOD) BIOCHEMICAL OXYGEN DEMANDThe biochemical oxygen demand test is based on mainly bio assay procedure which measures the Dissolved oxygen consumed by micro organism while assimilating and oxidizing the organic matter under aerobic conditions.

Procedure: Take appropriate quantity of water sample in one liter. Volumetric flask and dilute upto mark with dilution water. Mix well. Rinse BOD bottles with diluted sample and fill up these bottles with diluted sample. Stopper the bottles immediately after removing the air bubbles. Determine the dissolve oxygen of one bottle. And keep one set of bottle for 3 days incubation at 270±10C. After three days determine the Dissolve oxygen. Carry out a blank determination along with each sample.

(COD) CHEMICAL OXYGEN DEMAND A sample is refluxed is strongly acid solution with a known excess of K2Cr2O7. After digestion, the remaining unreduced K2Cr2O7 is titrated with ferrous ammonium sulphate to determine the amount of K2Cr2O7 consumed. And oxidizable organic mater is calculated in terms of oxygen equivalent.

Procedure: Place 50 ml sample or smaller sample portion diluted to 50ml in a refluxing flask. Add 1g HgSO4 and very slowly add 5 ml sulphuric acid reagent with mixing to dissolve HgSO4. Add 25 ml of K2Cr2O7 solution and mix. Attach flask to condenser and then on cooling water add remaining sulphuric acid reagent (70 ml) through open end of condenser. Mix reflux mixture, cover open end of condenser with beaker and reflux for 2 hrs cool and wash down condenser with 50 ml D/W. Dilute and cool the room temterature. Titrate excess K2Cr2O7 with FAS using 0.1 to 0.15 ml (2-3 drops) ferroin indicator up to reddish brown end point. In the same manner reflux and titrate a blank with same reagents and a volume of D/W.

Calculation: COD as mg O2 / L = (A-B) X M X 8000 ml Sample

A= ml FAS used for blankB= ml FAS used for Sample.M= Molarity of FAS

OIL & GREASEDissolved and emulsified oil and grease is extracted from water by solvent trichlorotrifluorethane or petroleum benzene and estimation is made gravimetrically.

Procedure: Transfer suitable quantity of sample to a separating funnel. Acidify to pH 2 by adding Conc HCl. Carefully rinse the measuring cylinder with 30 ml solvent and add the solvent washings to the separating funnel. Shake vigorously for 2 minutes or gently for 5-10 minutes. Let the layers separate. Drain the solvent layer through



a funnel containing solvent moistened filter paper and Na2SO4 into a clean tared flask or beaker, wash filter or beaker. Extract two more times with 30 ml solvent each time. Collect extracts in tared flask or beaker. Wash filter paper with 10-20ml solvent. Distill off solvent over water bath at 70°C and evaporate of all solvent. Cool the beaker in a desiccator and weigh.

Calculation:

Oil & Grease mg/l = M x 1000 V

M = Mass in mg of residueV = Volume in ml of sample taken

HARDNESSWater hardness is the traditional measure of the capacity of water to react with soap, hard water requiring a considerable amount of soap to produce lather. Hardness of water is not a specific constituent but a variable and complex mixture of cations and anions. The principle hardness causing ions are calcium and magnesium. The degree of hardness of drinking water has been classified in term of the equivalent CaCO3 concentration as follows: Soft 0-60 mg/l, Medium 60-120 mg/l, Hard 120-180 mg/l & Very Hard > 180 mg/lHardness many also be discussed in term of carbonate (Temporary) & non-carbonate (Permanent) hardness. Carbonate hardness can be removed or predicated by boiling. This type of hardness is responsible for the deposition of scale in hot water pipes and kettles. Non-carbonate hardness is caused by the association of the hardness causing cations with Sulphate, chloride or nitrate. It cannot bye removed by boiling public acceptability of the degree of hardness may very considerably from community to community, depending on local condition.

EDTA TITRIMATRIC METHOD Principle:In alkaline condition EDTA reacts with Ca and Mg to form a soluble chelated complex. Ca & Mg ions develop wine red color with Eriochrom Black T under alkaline condition. When EDTA is added as a titrant, the Ca & Mg divalent ions get complexed resulting in sharp change from wine red to blue, which indicates end point of the titration. The pH for this titration has to be maintained at 10 + 0.1. At a high pH i.e. about 12 Mg ion of color from pink to purple which indicates the end point of the reaction.Interferences:Metal ions do interfere but can be overcome by addition of inhibitors.Reagents:1. Buffer Solution: Dissolve 16.9 gm NH4Cl in NH4OH. Add 1.25 gm magnesium salt of EDTA to obtain sharp change in indicator and to 250 ml. If magnesium salt of EDTA is unavailable, dissolve 1.179 gm disodium salt of EDTA (AR grade) and 780 mg MgSO4. 7H2O or 644 mg MgCl2 6H2O in 50 ml distilled water. Add to above solution of NH4Cl in NH4OH and dilute to 250 ml.2. Inhibitor:Dissolve 4.5 gm hydroxylamine hydrochloride in 1000 ml 95% ethyl alcohol or isopropyl alcohol.3. Erichrom Black T Indicator:



Mix 0.5 gm dye with 100gm. NaCl to prepare dry powder.4. Murexide Indicator: Prepare a ground mixture of 200 mg of murexide (ammonium purpurate) with 100gm of solid NaCl.5. Sodium Hydroxide 2 N:Dissolve 80 gm NaOH and dilute to 1000 ml.6. Standard EDTA solution 0.01 M:Dissolve 3.723 gm EDTA sodium salt and dilute to 1000ml. Standardize against standard calcium solution, 1 ml = 1mg CaCO3.7. Standard calcium solution:Weight accurately 1.0 gm AR grade CaCO3 and transfer to 250 ml conical flask. Place a funnel in the neck of a flask and add 1+1 HCl till CaCO3 dissolves completely. Add 200 ml distilled water and boil for 20-30 min. to expel CO2. Cool and add methyl red indicator. Add NH4OH3 N dropwise till intermediate orange color develops. Dilute 1000 ml to obtain 1 ml = 1 mg CaCO3.Procedure:A. Total Hardness:1. Take 25 or 50 ml mixed in porcelain dish or conical flask.2. Add 1-2 ml buffer solution followed by 1 ml inhibitor.3. Add a pinch of Eriochrome Black T and titrate with standard EDTA (0.01 M) till wine red color changes to blue. Note down the volume of EDTA required. (A) 4. Run a reagent blank. Note down the volume of EDTA…………….(B).5. Calculate volume of EDTA required by sample, from volume of EDTA required in step 3 & 4.C = (A-B)6. Calculate as follows:Total hardness

As CaCO3 mg/l = CxDx1000 ml sample

Where C = Volume of EDTA required by sample. D = mg CaCO3 per 1.0 ml. EDTA (0.01m) used as titrant.B. Calcium Hardness: 1. Take 25 or 50 ml sample in porcelain dish.2. Add 1 ml NaOH to raise ph to 12.0 and a pinch of murexide indicator.3. Titrate immediately with EDTA till pink color changes to purple. Note the volume of EDTA used (A’).4. Run a reagent blank. Note the ml of EDTA (B’) required and keep it aside to compare end points of sample titrations. 5. Calculate as follows:

Calcium hardness as CaCO3 = C x D x 1000 ml sample

Where C’ = Volume of EDTA used by sampled (A’- B’) D = mg Caco3 per 1.0 ml EDTA (0.01 M) used for titration.C. Magnesium Hardness as CaCO3 mg/l = total hardness asCaCO3 mg/l- Ca hardness as CaCO3 mg/l.D. Alkaline (Carbonate) Hardness and Non Alkaline (Non Carbonate) Hardness.These types of hardness can be calculated from hardness and alkalinity data as follows:



If total hardness as CaCo3 > Total alkalinity as Caco3

Then1. Alkalinity Hardness = Total Alkalinity2. Non-alkaline hardness = Total hardness- Total alkalinity

If total hardness as CaCO3 < Total alkalinity as CaCO3

Then,i) Alkaline Hardness = Total Hardnessii) Non-Alkaline Hardness = Nil

FLUORIDE

Outline: The Spadns colorimetric method is based on the reaction between fluoride and zirconium dye lake, Fluoride reacts with dye lake, dissociating a portion of it into a colorless complex anion and the dye. As the amount of fluoride increases, the color produced becomes progressing lighter.

Procedure:1) Prepare fluoride standards in the range of 0 to 1.4 mg/l by diluting standards fluoride

solution. Add 10 ml mixed acid zirconyl spadns reagent, mix and dilute to 50 ml with D/W. Set photometer to zero absorbance with reference solution and absorbance readings of standards. Plot a curve of mg fluoride - absorbance relationship.

2) Take 25 ml sample or a portion of sample, add 10 ml mixed acid zirconyl spadns reagent, mix and dilute to 50 ml with D/W and read absorbance at 570 nm. Determine concentration of fluoride from curve.

Calculation: mg F/l = A . ml sample

A = µg F from Curve CHLORIDE

Chloride ion is generally present in natural water. The presence of chloride in natural waters can be attributed to dissolution of salt deposits, discharges of effluents from chemical industries, irrigation drainage, contamination from refuge leachates and sea water intrusion in coastal areas. The salty taste produced by chloride depends on the chemical composition of the water. A concentration of 250 mg/L may be detectable in some waters containing sodium ions. A high chloride content has a deleterious effect on metallic pipes as structure as well as on agriculturalal plants.Principle:Chloride is determined in a neutral or slightly alkaline solution by titration with standard silver nitrate using potassium chromate as an indicator. Silver chloride is quantitatively precipitated before red silver chromate is formed.



Interference: If the sample is too colored or turbid to allow the end point to be readily detected. This interference may be reduced by alum flocculating followed by filtration prior to the estimation of chloride.Reagents:1. Potassium Chromate Indicator: Dissolve 50 g K2crO4 in distilled water. Add AgNO3 till definite red precipitate is formed. Allow standing for 12 hrs. filter and dilute to 1000 ml2. Silver nitrate (0.0141 N): Dissolve 2.395 gm AgNO3 and dilute to 1000 ml standardize against NaCl, 0.141 N. 1 ml of 0.141 N AgNO3 = 0.5 mg Cl.3. Sodium Chloride 0.141 N: Dissolve 824.1 mg NaCl (dried at 1400 C) and dilute to 1000 ml. 1 ml = 0.5 mg Cl4. Special reagent to remove color and turbidity: Dissolve 125 g A1K (SO4)2, 12 H2O or AINH4 (SO4)2,.12 H2O and dilute to 1000 ml Warm to 600 C and ad 5 ml conc.NH4OH slowely.Allow to stand for 1 hr.Solution should be free from Cl.Procedure:1. Take 100 ml sample and adjust the pH between 7.0 and 8.02. Take 50 ml well mixed sample adjusted to pH 7.0 – 8.0 and add 1.0 ml K2CrO4.

3. Titrate with standard AgNo3 solution till AgCrO4 starts precipitating.4. Standardize AgNO3 against standard NaCl.5. For better accuracy titrate distilled water (50 ml) in the same way to establish reagent blank.6. Calculate the follows:

Chloride mg/l = (A-B x N x 35.45 x 1000) ml sample

Where A = ml AgNO3 required for sample. B = ml AgNO3 required for sample. N = Normality of AgNO3 used.

RESIDUAL FREE CHLORINEOut line: Residual chlorine reacts under acid conditions with o-tolidine to give a yellow

colour which is matched against standard colours.

Procedure: Use 5 ml neutral ortho-toludine and 5 ml buffer stabilizer reagent with 100ml sample. Place the neutral ortho-toludine and buffer stabilizer mixture in a beaker on a magnetic stirrer. Mix and add sample to the reagents with gentle stirring, Measure the absorbance at 625 nm.

Calculation: (OD x GF x 1000)/ Sample taken = Residual free chlorine, mg/l

IRONBeing the fourth most abundant element by weight in the earth's crust, it occurs mainly in the divalent and trivalent state in water. The presence of iron in natural water can be attributed to the dissolution of rocks and minerals, acid mines drainage, landfill leachates, sewage and engineering industries. The presence of iron in drinking water supplies is objectionable for a number of reasons. Under pH condition existing in drinking water supply. ferrous sulphate is unstable and precipitate as insoluble ferric hydroxide which settles out as a rust colored silt. Such water often tastes unpalatable even at low concentration (0.3 mg/L) and stains laundry and



plumbing fixtures. Iron also promotes the growth of 'Iron bacteria'. These microorganisms serive their energy from the oxidation of ferrous to ferric and in the process deposit a slimy coating on the piping. Principle: The ferric form of iron is reduced to ferrous form by boiling with hydrochloric acid and hydroxylamine hydrochloride. Upon adding 1, 10 phenanthroline (between pH 3.3 and 3.3) form a soluble chelated complex of orange red color. Intensity of the color is directly proportional to concentration of iron present in the sample. Interference: Strong oxidizing agents such as CN, KO2, polyphosphates, Cr, Zn in conc. exceeding 10 times the Fe conc. Co and Cu if 5 mg/L Ni if 2 mg/L color and organic matter. constitutes sources of interference in the development of color. Boiling with HCI and addition of hydroxylamine -hydrochloride remove interference due to CN, PO4 and other oxidizing agents. The metal ions get complexed with phenanthroline. Apparatus: 1) HCl conc. 2) Hydroxylamine HCl solution -Dissolve 10 gm NH2OH. HCl in 100 ml distilled water. 3) Ammonium acetate buffer: Dissolve 250 gm ammonium acetate in 150 ml distilled water. Add 700 ml conc. glacial acetic acid. Final volume will be slightly more than 1000 ml. 4) Phenanthroline solution: Dissolve 100 mg 1, 10 -phenanthroline monohydrate = in 100 ml distilled water. Warm slightly or add 2 drops conc. HCl if necessary. 1 ml of this solution can chelate 100 mg iron. 5) Stock iron solution: Add 20 ml conc. H2SO4 to 50 ml distilled water and dissolve -1.404 gm Fe (NH4) (504) 2.6H2O add dropwise 0.1N KMnO4 till faint pink color persists. Dilute to 100 ml.,1 ml. = 200 g FeProcedure: 1. Take suitable aliquot about 50 ml (having 2 mg/L Fe) of well-mixed sampled in 125 ml conical flask. 2. Add 2 ml conc. HCl followed by 1 ml Hydroxylamine -hydrochloride solution. 3. Add 2-3 glass beads and boil for 20-25 min. to ensure dissolution of Fe. 4. Cool to room temp. and transfer to nessler's tube. 5. Add 10ml ammonium acetate buffer and 2 m11, 10-phenanthroline solutions. 6. Dilute to 100 ml and mix well. 7. Prepare blank by substituting the sample by distilled water. 8. For soluble iron determination, take known volume of filtered sample, acidify by adding 2 ml conc. HCl per 100 ml of sample and treat form step 5 onwards for color developing. 9. Prepare calibration curve taking standard iron solution in the same way in the range, 1 000-4000 g /L with 1 cm light path. 10. Measure the developed color after 10 min. at 510 nm. 11. Calculate the conc. 0 total or soluble Fe present in the sample form calibration curve and express as mg/L.



TOTAL COLIFORMSThe coliform group consists of several genera of bacteria belonging to the family of Enterobacteriaceae. This group is defined as all facultative anaerobic, gram (-), nor-spore forming rod shaped bacteria, lactose fermenting with acid and gas within 48 hrs. at 370C.“When multiple tubes are used in the fermentation technique results at the examination of replicate tubes and dilutions are reported in the term of the Most Probable Number (MPN) of organisms present”.Procedure:

(a) Presumptive test- i) Inculate a 5 tube series having 10 ml. Mac’Conkey broth double strength and 10 tube having 10 ml Macconkey broth single strength and Durham’s tubes by adding water sample 10 ml. in 5 tubes of double strength, and 1 ml., & 0.1 ml in each 5 tube of single strength respectively.ii) Incubate all the tubes at 370C for 24-48 hrs.iii) Examine each tube after the end of the incubation period for acid and gas formation.iv) Production of gas within 48 hrs in the inner fermentation tubes constitutes a positive presumptive test and absence of gas shows negative test.

(b) Confirmatory test- i) Transfer a loopful of suspension by the all-primary fermentation tubes showing acid and gas to a 10-ml. tube of BGB broth containing Durham’s tube.ii) Incubate the tubes at 370C for 48 hrs.iii) Formation of acid and gas in Durham’s tube shows positive test.

(c) Completed test- i) Positive BGB tubes streak with the help of a loop on Mac’ Conkey Agar plate.ii) Incubate all the tubes at 37 for 24 hrs.iii) Typical pink, pale yellow color colonies show positive results that will ferment the lactose broth.iv) Gram Staining – Gram negative bacilli.

Computing and RecordingNumber of the Coliform can be obtained by using MPN table.

E-ColiE-Coli is gram (-), aerobic, facultative anaerobic, rod shaped, lactose, fermenting and belongs to Enterobacterioaceae family. It is a member of indigenous fecal flora of warm blooded animals. Its occurrence is considered a specific indicator of fecal contamination and possible presence of enteric pathogen.Media:

1) Mac’ Conkey Broth

2) Mac’ Conkey Agar

3) Peptone Water

4) BGB Broth

5) Kovac’s Reagent



Procedure:1. Submit all the presumptive fermentation tubes from Coliform tests showing growth, gas

or acidity within 48 + 3 hours.

2. Sub culture from all the positive Mac Conkey Broth tube on to BGB Broth tubes and incubate at 44.5 0C for 48 hours.

3. Sub culture from all the positive tubes of BGB Broth into tubes of peptone water.

4. Incubate at 44.5 0C for 48 hours.

5. At the end of incubation period test for indole production by adding a few drops of Kovac’s reagent.

Results: Positive tubes will give pink color or reddish ring while negative tubes will give yellow color rings with Kovac’s reagent.


Documents

ID: 909160045nromoef.gov.in/Environment_Reports/Reports/4-814-2010-RO... · Web viewSilver nitrate (0.0141 N): Dissolve 2.395 gm AgNO3 and dilute to 1000 ml standardize against NaCl,