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LSD-NEERI- Water Quality Analysis.pdf

This document provides information on various methods for analyzing water quality parameters. It discusses the importance of measuring dissolved oxygen, biochemical oxygen demand, and bacteriological parameters like total coliform and fecal coliform. The principles, procedures, calculations, and sources of error for estimation of these parameters using standard methods are explained in detail. The document also discusses other water quality parameters like pH, conductivity, total dissolved solids, color and their significance in assessing water quality for different uses. Standards for classification of inland surface waters according to the Central Pollution Control Board are also presented.

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Water Quality Analysis Laboratory Methods Dr. (Mrs.) Leena Deshpande National Environmental Engineering Research Institute (NEERI), Nagpur Council of Scientific & Industrial Research, New Delhi, Govt. of India
Clouds Water bodies Water quality Atmospheric Constituents Surface runoff Leachates from Soil and Rocks Dispersion & Dissolution in Water
Quality changed Non-abstractive uses Water Ground Water Sea Water Abstractive Uses Domestic Irrigation Industrial Quantity returned Quantity lost Inland Surface Water
Water Transport Sea In-land Waters Food • Fishing • Sea Food • Pond Food • Lean Period River bed crops Recreation • Swimming • Sunbath & Swimming • Picnic Spot • Water Sports • Pilgrimage Eco-system • Conservation • Rejunvetion • Technical interferences • Technological Interventions Non-abstractive uses
Adverse Effects of Impurities Problems ¾ Aesthetically not acceptable and Palatability decreases ¾ Health related problems ¾ affect mucous membrane ¾ gastro-intestinal irritation ¾ Dental and skeletal fluorosis ¾ Methaemoglobinemia ¾ Encrustation in water supply structure ¾ Adverse effects on domestic use Constituents Responsible • Clay, Silt, Humus, Colour • pH • Hardness, TDS, Ca, Mg, SO4 • Fluoride • Nitrate • Hardness, TDS • Ca, Mg, Cl
¾ Eutrofication of the waterbody ¾ Taste, discolouration and corrosion of pipes fittings and utensils ¾ Promotes iron bacteria ¾ Corrosion in water supply system ¾ Carcinogenic effect ¾ Toxic effect ¾ Formation of chlorophenols with chlorine ¾ Imparts unpleasant taste and odour after chlorination ¾ Water-borne diseases • Zoo & Phyto, Phosphate, Nitrate • Iron, Mn, Cu, Zn, Alkalinity • Fe & Mn • pH, Cl • Cr, As • Cd, Pb, Hg • Phenols • Oil & grease • Bacteria & viruses Adverse Effects of Impurities
Contamination / Pollution 9 During its traverse water picks up impurities in varying amounts 9 Gases from atmosphere 9 Inorganic and organic salts from top soil and geological strata 9 During its traverse water get contaminated by inorganic and organic salts sometimes beyond desirable limits Pollution 9 Presence of undesirable substances in the quantities which are harmful to man vegetation or property is referred to as pollution 9 Quality of water depends upon quality and quantity of inorganic and organic salts present in water
Safe Water/ Wholesome Water Aesthetically acceptable Chemically safe Organic substances absent Free from bacteria Radioactive elements absent
Water Quality Assessment È To measure concentration of the constituents in quantity for characterisation of water for different uses È Of the various parameters in potable water few are objectionable even when present in very small quantity È Others if only present in unusual quantities as to relegate the water from the potable to the unusable class È The analyst familiar with water quality characterisation will often select parameters to be measured based on experience and intuition
Water Analysis - Key Factors Factors Reporting the values Proper Labeling Sampling Selection of Parameters Precision and accuracy of method selected Preservation
Water Quality Assessment : Potable & Industrial Uses Parameters Physical Inorganic OR Chemical Toxic Metals Organic, Nutrient & Demand Alpha emitter Beta emitter Biology Radioactive elements Bacteriological Phytoplankton Zooplankton Total Coliform Faecal Coliform BOD COD Phenols Oil & Grease Pesticides Nitrate Copper Chromium Cadmium Zinc Lead Mercury Iron Manganese Temperature PH Colour Conductivity Odour Total Dissolved Taste Solids Turbidity Hardness Fluoride Calcium Alkalinity Magnesium Nitrate Chloride Phosphate Sulphate
¾ Irrigation 9 pH 9 Conductivity 9 Sodium & Potassium 9 Nutrients 9 Specific compounds ¾ Industries 9 As per specific requirement ¾ Domestic Consumption 9 As per BIS Standards ¾ Water Bodies 9 As per CPCB guidelines Water Quality Consideration
S. No. Characteristics A’ B’ C’ D’ E’ 1. Dissolved Oxygen, mg/L, Min 6 5 4 4 - 2. Biochemical Oxygen Demand, mg/L, Max 2 3 3 - - 3. Total Coliform Organisms*, MPN/100 mL, Max 50 500 5000 - - 4. Total Dissolved Solids, mg/L, Max 500 - 1500 - 2100 5. Chlorides (as Cl), mg/L, Max 250 - 600 - 600 6. Colour, Hazen Units, Max 10 300 300 - - 7. Sodium Absorption Ratio, Max - - - - 26 8. Boron (as B), mg/L, Max - - - - 2 9. Sulphates (as SO4), mg/L, Max 400 - 400 - 1000 10. Nitrates (as NO3), mg/L, Max 20 - 50 - - 11. Free Ammonia (as N), mg/L, Max - - - 1.2 - 12. Conductivity at 25oC, micromhos/cm, Max - - - 1000 2250 13. pH value 6.5-8.5 6.5-8.5 6.5-8.5 6.5-8.5 6.5-8.5 14. Arsenic (as As), mg/L, Max 0.05 0.2 0.2 - - 15. Iron (as Fe) , mg/L, Max 0.3 - 50 - - 16. Fluorides (as F), mg/L, Max 1.5 1.5 1.5 - - 17. Lead (as Pb), mg/L, Max 0.1 - 0.1 - - 18. Copper (as Cu), mg/L, Max 1.5 - 1.5 - - 19. Zinc (as Zn), mg/L, Max 15 - 15 - - Classification of Inland Surface Waters (CPCB Standards) •If the coliform count is found to be more than the prescribed tolerance limits, the criteria for coliforms shall be satisfied if not more than 20 percent of samples show more than the tolerance limits specified, and not more than 5 percent of samples show values more than 4 times the tolerance limits. Further, the faecal coliform should not be more than 20 percent of the coliform. Source : Indian Standard (IS:2296-1982). A’ Drinking water source without conventional treatment but after disinfection D’ Propagation of wild life, fisheries B’ Outdoor bathing (organised) E’ Irrigation, industrial, cooling, controlled C’ Drinking water source with conventional treatment followed by disinfection waste disposal
¾ All living organisms depend upon oxygen to maintain the metabolic processes that produce energy for growth and reproduction ¾ Dissolved oxygen is important in precipitation and dissolution of inorganic substances in water Need ¾ To assess quality of raw water ¾ To check on pollution ¾ Determination of biological changes by aerobic or anaerobic organisms ¾ D.O. is the basis of BOD test to evaluate pollution potential of wastes ¾ All aerobic biological wastewater treatment processes ¾ Important factor in corrosion. Dissolved Oxygen
Principle ¾ Oxygen present in sample oxidizes the divalent manganous to its higher valency which precipitates as a brown hydrates oxide after addition of NaOH and KI ¾ Upon acidification, manganese revert to divalent state and liberates Iodine from KI equivalent to D.O. content in the sample ¾ The liberated Iodine is titrated against standard (N/40) solution of Sodium thiosulphate using starch as an indicator. Methodology The Winkler method with Azide modification
Procedure ¾ Collect sample in BOD bottle ¾ 2 ml MnSO4+ 2 ml Alkali iodide-azide+close stopper ¾ Mix well + allow the ppt to settle ¾ Add 2 ml concentrated H2SO4 + mix well till ppt dissolves ¾ Take 203 ml (Correspond to 200 ml) sample in a conical flask+titrate against Sodium thiosulphate (0.025 N) till pale yellow colour + starch + titrate till blue to colourless Calculation ¾ 1 ml of 0.025N Na2S2O3 = 0.2 mg of O2 ¾ D.O. in mg/l =(0.2 x 1000) x ml of thiosulphate 200 Results : D.O. mg/l
Interferences ¾ Ferrous ion ¾ Ferric ion ¾ Nitrite ¾ Microbial mass ¾ High suspended solids To reduce interferences, modification in the estimation procedures are suggested ¾ Alsterberge azide : Nitrite, higher concentration of ferric ions ¾ Redeal Stewart : Ferrous ion ¾ Alum / Flocculation : High suspended solids ¾ Copper Sulphate Sulfamic acid flocculation : Biological flocs ¾ Alkaline Hypochlorite : Complex of sulphur compound
A bioassay test, involving measurement of oxygen consumed by micro-organisms while stabilizing biologically decomposable organic matter under aerobic conditions Need ¾To determine the pollution load of waste water ¾The degree of pollution in water sources ¾Self purification capacity of sources ¾Designing of treatment facilities ¾Efficiency of waste water treatment methods Biochemical Oxygen Demand
Methodology Principle ¾ The BOD test is based upon determinations of dissolved oxygen ¾ It can be measured directly ¾ In general, a dilution procedure is applied.
Procedure Preparation of dilution water ¾ Aerate the required volume of D.W. by bubbling compressed air for 1-2 days to attain D.O. saturation ¾ Add 1 ml each per litre of dilution water Phosphate buffer Magnesium sulphate Calcium chloride Ferric chloride ¾ Mix well ¾ In case, waste not expected sufficient bacterial population, add seed (2 ml settle sewage / litre of dilution water)
Determination of D.O. i) Samples and ii) Blank, on initial and after 5 days ¾ 2 ml MnSO4 + 2 ml Alkali-iodide-azide+stopper immediately ¾ Mix well + allow the ppt. to settle ¾ Add 2 ml concentrated H2 SO4 + mix well till ppt. dissolve ¾ Take 203 ml (correspond to 200 ml) sample in a conical flask ¾ Titrate against sodium thiosulphate (0.025 N) till pale yellow colour + starch solution + blue colour + titrate till colourless
Observations D0 = D.O. in sample on 0th day D1= D.O. in sample on 5th day C0 = D.O. in Blank on 0th day C1 = D.O. in Blank on 5th day C0 – C1 = D.O. depletion in dilution water alone D0 – D1 = D.O. depletion in sample + dilution water (D0 - D1) - (C0 – C1) = D.O. depletion due to microbes
Calculation 1 ml of 0.025 N sodium thiosulphate = 0.2 mg of Oxygen D.O. in mg/l = (0.2 x 1000) x ml of thiosulphate 200 B.O.D. in mg/l (D0-D1) – (C0-C1) mg x Decimal fraction of sample used Results B.O.D. 5 days at 200 C = mg/l
Interferences ¾ Ferrous ion ¾ Ferric ion ¾ Nitrate ¾ Microbial mass ¾ High suspended solids ™ Lack of nutrients in dilution water ™ Lack of acclimated seed organisms ™ Presence of heavy metals ™ Presence of toxic materials
Bacteriological Analysis Bacteria Single cell microscopic organisms lacking chlorophyll Coliform group Contamination • Insanitary condition of surrounding area • Unhygienic practices • Discharge/seepage of sewage and domestic wastewater Need • Impact on water quality • Potability for human consumption • To prevent water-borne diseases • To assess the quality of raw and treated water • Specially to detect Faecal Contamination Bacteriological analysis : mainly includes estimation of • Total coliforms • Faecal coliforms
Methodology Approved techniques generally used as per "Standard Methods for the examination of water and wastewater” – .Membrane Filter (MF) – Multiple Tube Dilution (MTD) MF-technique Principle Biochemical reactions are used to detect the various groups of micro-organisms MF-technique - Merits • Results in 24 hours (MTD - 48 to 96 hours) • Larger volume of samples can be tested (MTD - less volume) • Results with greater precision (MTD - MPN) • Require less laboratory space (MTD – More space) • Easy processing (MTD – Tedious) • Useful during normal and emergencies (MTD – Difficult in emergencies) Limitations : Samples with more turbidity
Colour Coloured water is not acceptable for drinking (Aesthetic as well as toxicity reasons) Industrial wastewater require colour removal before discharge into water courses Definition • The term colour means true colour that is the colour of water from which turbidity has been removed. True colour of water is due to dissolved material • Apparent colour is due to suspended matter as well as due to substances on solution removed by filtration Unit for Measurement of colour • Unit for colour measurement is based on platinum cobalt scale Contd...
Methods for Colour Measurement Visual Comparison Method • Colour of the sample is determined by visual comparison with known concentration of coloured colutions prepared by diluting stock platinum cobalt solution • OR properly calibrated glass coloured disk is used for comparison • This method is useful for potable water and water in which colour is due to naturally occuring materials • This method is not applicable to most highly coloured industrial wastewater Spectrophotometric Method • This method is applicable to potable and waste both domestic and industrial • In this method light absorbed or transmitted is measured at dominant wavelength of a particular hue of sample • Spectrophotometer should have an effective operating range from 400 to 700 nm before measurement remove turbidity either by filtration or by centrifuging • Colour hues for dominant wavelengths ranges are Contd...
Definition Measure of the ability of aqueous solution to carry an electric current # Concentration of ions # Mobility # Valency # Temperature Degree of Minerilization Effect on plants and animals Check purity of distilled water Monitoring seasonal variation of raw water or wastewater Determine sample size for chemical analysis Check results of chemical analysis Estimate TDS µ mho/cm or µs/cm Conductance is measured between two spacially fixed and chemically inert platinum electrodes Unit Conductivity Measurement Conductance(G) ∝ Area (A) ∝ 1/Distance (L) G = K(A/L) A = 1cm2 L = 1 cm G = K K is called conductivity or specific conductance Conductivity Meter Significance
Total Dissolved Solids Definition Portion of Solids that passes through a filter of 2.0 µm or smaller pore size Significance Palatability decreases Gastro intestinal irritation Unsuitable for many industrial uses Evaporation at 180 + 20C Calculations Method Evaporation Method •Yield values for TDS closer to obtained through summation •At this temp. all mechanically occluded water is lost •Some samples may require prolonged drying and desiccation Conductivity
• pH = - log10 [H+] = log10 1/[H+] OR [H+] = 10-pH This method has advantage because all states of acidity and alkalinity of solutions with respect to hydrogen and hyroxide ions can be expressed by a series of positive numbers between 0 to 14 [ H+] (10o) 10-1 10-2 10-3 10-4 10-5 10-6 10-7 10-8 10-9 10-10 10-11 10-12 10-13 10-14 pH 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 pOH 14 13 12 11 10 9 8 7 6 5 4 3 2 1 0 [OH-]10-14 10-13 10-12 10-1110-10 10-9 10-8 10-7 10-6 10-5 10-4 10-3 10-2 10-1 10-0 • Chemical reactions depend on pH • Water Supply and Waste Water Treatment • Water Softening ,Precipitation., Coagulation, Disinfection, Corrosion Control,Alkalinity and CO2 Measurement and fluoride activity • Electrometric method - Using pH meter and electrodes • e.m.f. produced in glass electrode system varies linearly with pH • pH meter is calibrated potentiometrically with electrode system using standard buffers having assigned values so that pH = - log10 [H+] • pH Hydrogen Ion Exponent 6.5 - 8.5 Definition Significance Measurement pH Meter
Sources • Fertilizers and manure • Decayed vegetable • Animal feedlots • Municipal wastewater and sludge disposal to land • Industrial discharges • Leachates from refuse dumps • Septic systems and • N-fixation from atmosphere by bacteria and lightning Nitrate
Chloride Presence in Natural Waters • Dissolution of salt deposits • Discharges of effluents • Oil well operations • Sewage discharges • Irrigation drainage • Sea water intrusion in coastal areas
Chloride Methodology : An Argentometric Method • Principle Chloride is determined in a natural 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. 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 blank N = Normality of AgNO3 used
Methods for Nitrate Estimation A) Ultraviolet Spectrophotometric Method • Useful for uncontaminated natural waters and potable water supplies that have low organic content • Follows Beer’s law upto 11 mg/L as N • Interferences - Dissolved Organic Matter - Surfactants - Nitrite and Hexavalent Chromium • Procedure - Filter the sample - Add 1 ml of 1N HCl per 50 ml of sample - Read absorbance or tranmittance at 220 nm and 275 nm - Set 0 absorbance or 100% tranmittance with distilled water
B) Nitrate Electrode Method • Useful for Nitrate concentration range of 0.14 to 1400 mg/L NO3-N • Interferences - Chloride and bicabonate with weight ratios to NO3-N 10 or 5 respectively - NO2, CN, Sulphide, Br, I, Chlorite and Chlorate
C) Phenoldisulphonic Acid (PDA) Method • Nitrate reacts with Phenoldisulphonic acid to produce nitro derivatives that in alkaline solution rearranges its structure to form yellow colored compound with characteristics that follows Beer’s law • Chloride interferes seriously which can be overcome by precipitation of chloride with Ag+ as AgCl
Fluoride Significance Dual significance in water High concentration of F- causes dental Fluorosis Concentration 0.8 mg/L results in dental Carries Essential to maintain F- concentration between 0.8 mg/L to 1.0 mg/L in drinking water
Fluoride Methods Colorimetric SPADNS Method Principle: Under acidic conditions fluorides (HF) react with zirconium SPADNS solution and the lake (colour of SPADNS reagent) gets bleached due to formation of ZrF6 . Since bleaching is a function of fluoride ions, it is directly proportional to the concentration of fluoride. It obeys Beers law in a reverse manner. Ion Selective Electrode Method Principle: The fluoride sensitive electrode is of the solid state type, consisting of a lanthanum fluoride crystal; in use it forms a cell in combination with a reference electrode, normally the calomel electrode. The crystal contacts the sample solution at one face and an internal reference solution at the other. A potential is established by the presence of fluoride ions across the crystal which is measured by a device called ion meter or by any modern pH meter having an expanded millivolt scale. Calculate mg F- / L present in the sample using standard curve
Sulphate Significance • Occurs in natural water • High concentration of Sulphate laxative effect (enhances when sulphate consumed with magnesium) • Problem of scaling in industrial water supplies • Problem of odour and corrosion in wastewater treatment due to its reduction to H2S
Sulphate Method Spectorphotometric Method Principle: Sulfate ions are precipitated as BaSO4 in acidic media (HCl) with Barium Chloride. The absorption of light by this precipated suspension is measured by spectrophotometer at 420 nm or scattering of light by Nephelometer Calculate mg / L SO4 = mg SO4 x 1000 ml sample
Ammonia • Ammonia is present naturally in surface and wastewaters. Its concentration is generally low in ground waters because it adsorbs in soil particles and clays and is not leached readily from soils. • It is produced largely by de-amination of organic nitrogen containing compounds and by hydrolysis of urea • In the chlorination of water, chlorine reacts with ammonia to form mono and dichloramines (combined residual chlorine) • Ammonia concentration in water vary from less than 10µg in some natural surface and ground waters to more than 30 mg/L in some wastewaters
Methods for Ammonia Estimation A) Nesslerization Method • Direct nesslerization method is useful for purified natural water and highly purified wastewater effluents with very light color and having NH3-N concentrations more than 20 µg/L • Applicable to domestic wastewater only when errors of 1 to 2 mg/L are acceptable • The graduated yellow to brown colors produced by nessler-ammonia reaction absorb strongly over wide wavelength range • Low ammonia concentration of 0.4 to 5 mg/L can be measured with acceptable sensitivity in wavelength region from 400 to 425 nm with 1cms light path • A light path of 5 cm extends measurements of ammonia concentrations range of 5 to 60 µg/L
• The reddish brown color at ammonia levels approaching 10 mg/L may be measured in the wavelength region of 450 to 500 nm • Thus, the proper selection of light path and wavelength permits the photometric determination of ammonia concentrations over a considerable range • Carefully prepared nessler reagent may respond under optimum conditions to as low as 1µg NH3-N/ 50mL (100µg/L). However, reproducibility below 100 µg/L may be erratic • Interferences - Turbidity, color , magnesium and calcium
B) Ammonia Selective Electrode Method • The ammonia selective electrode uses a hydro-phobic gas permmeable membrane to separate the sample solution from an electrode internal solution of ammonium chloride • Dissolved ammonia is converted to NH3(aq) by raising pH to above 11 with a strong base, which diffuses through membrane and changes the internal solution pH that is sensed by a pH electrode • The fixed level of chloride in the internal solution is sensed by a chloride ion-selective electrode that serves as the reference electrode • Applicable to the measurement of 0.03 to 1400 mg NH3-N/L in potable and surface waters and domestic and industrial wastes • High concentrations of dissolved ions affect the measurements but color and turbidity do not. • Interference - Amines are a positive interference - Hg and silver interfere by complexing with ammonia
C) Titrimetric Method • The method is used only on samples that have been carried through preliminary distillation • Titrate ammonia in distillate using standard 0.02N Sulphuric acid with boric acid indicator solution
Phosphates • Phosphate occurs in traces in many natural waters, and often in appreciable amounts during periods of low biologic productivity. Waters receiving raw or treated sewage agricultural drainage, and certain industrial waters normally contain significant concentrations of phosphate.
Methods for Phosphorus Estimation A) Vanadomolybdophosphoric Acid Method • In a dilute orthophosphate solution, ammonium molybdate reacts under acid conditions to form a heteropoly acid. In the presence of vanadium, yellow vanadomolybdophosphoric acid is formed. The intensity of yellow color is proportional to phosphate concentration • Minimum detectable concentration is 0.2 mg P/L in 1 cm cell • Interferences - Silica and arsenate cause positive interference if the sample is heated - Negative interferences are caused by fluoride, thorium, bismuth, sulphide, thiosulfate, thiocyanate or excess molybdate - Blue color is caused by ferrous iron but this does not affect results if its concentration is less than 100 mg/L - Sulphide interference may beremoved by oxidation with bromine water
Procedure - Sample pH adjustment if pH 10 - Removal of excessive color by shaking with activated carbon - Color development with vanadate-molybdate reagent - Measurement of color absorbance at wavelength of 400 to 490 nm
B) Stannous Chloride Method • Molybdophophoric acid is formed and reduced by stannous chloride to intensely colored molybdenum blue • This method is more sensitive than above method and minimum detectable concentration is about 3 µg P/L • Interferences - Silica and arsenate cause positive interference if the sample is heated - Negative interferences are caused by fluoride, thorium, bismuth, sulphide, thiosulfate, thiocyanate or excess molybdate - Blue color is caused by ferrous iron but this does not affect results if its concentration is less than 100 mg/L - Sulphide interference may beremoved by oxidation with bromine water • Procedure - Sample pH adjustment if pH 10 - Color development with molybdate reagent - Measurement of color absorbance at wavelength of 690 nm
Limit of Iron and Manganese in Drinking Water • As per WHO guidelines for domestic water, iron should not exceed the limit of 0.3 mg/l • Above 200mg/l iron is toxic to human health • Manganese concentration as per WHO guideline is 0.05 mg/l • However average manganese level in drinking water range from 5 to 25 ug/l • At concentration exceeding 0.15 mg/l, manganese imparts undesirable taste
Iron and Manganese • Presence of excess of iron and manganese in water causes discoloration, turbidity and deposits • Iron and manganese bearing water have astringent metallic or bitter taste • Precipitation of iron and manganese imparts colour to water from yellow to brownish black, which becomes objectionable to consumers • Manganese concentration ranging from 8-14 mg/l is toxic to human • Excess of iron facilitates growth of iron bacteria which causes blocking of pipes, meters etc.
Limit of Iron and Manganese in Drinking Water • As per WHO guidelines for domestic water, iron should not exceed the limit of 0.3 mg/l • Above 200mg/l iron is toxic to human health • Manganese concentration as per WHO guideline is 0.05 mg/l • However average manganese level in drinking water range from 5 to 25 ug/l • At concentration exceeding 0.15 mg/l, manganese imparts undesirable taste
Methods for Detection of Iron and Manganese in Water • Atomic Absorption spectrophotometer (AAS) • Inductively Coupled Plasma (ICP) • Colorimetric method In colorimetric method iron is detected at wavelength 510 nm and manganese is detected at 525 nm. 1. Iron:- Phenanthroline method 2. Manganese:- Persulphate method Periodate method
Determination of Metals Inductively Coupled Plasma-Atomic Emission Spectrometer
ICP TORCH •Radio frequency 27-49 MHz 700-1599 W •Gas- Argon
Steps involved in the analysis of aqueous samples by ICP-AES
Procedure Instrument set up •Warm up for 30 min •Check the alignment of plasma torch •Make Cu/Mn ratio adjustment •Calibrate instrument using calibration standards and blank •Aspirate the standard and blank for 15s •Rinse with calibration blank for at least 60s to eliminate any carryover from previous standards •Ensure the concentration values within the 5% error
Analysis of samples •Analysis the samples using calibration blank •Analyse samples alternately with analyses of calibration blank • Rinse at least for 60s •Examine each analysis of the calibration blank to verify that carry over memory effect is no more •Make appropriate dilutions of the sample to determine concentrations beyond the linear calibration Instrument quality control •Reanalyse one or more samples analysed just before termination of the analytical run •Use this analysis to verify accuracy and validity of the calibration standards
End Point pH Alkalinity D e f i n i t i o n Sluggish response due to coating of soap, oily matter in potentiometric Colour, Turbidity with indicator method Significance Acid neutralizing capacity of water •Treatments of water and wastewater •Interpretation and control of water and waste water treatment processes Interference Carbonate Bicarbonate Hydroxyl Borates Phosphates Silicates Other Bases Due to All Titratable Bases Potentiometric titration Titration using indicator Total Alkalinity 4.5 Phenolphthalein Alkalinity 8.3 M e a s u r e m e n t
Turbidity General • Turbidity in water is caused by suspended matter such as Clay Silt Finely divided organic and inorganic matter Soluble coloured organic compounds Plankton and other microscopic organisms Definition • Turbidity is an expression of the optical property that causes light to be scattered and absorbed • It is not possible to correlate turbidity with the weight concentration of suspended matter because light scattering properties of the suspended particulate matter depends upon size, shape and refractive index of the particulates Contd...
Significance • Clarity of water is important for human consumption • Manufacturing processes such as beverages, and many food products need clear water Unit for Turbidity Measurement • Previously standard method for measurement of turbidity was based on the Jackson Cnadle turbidimeter • The lowest turbidity value that can be measured by this instrument is 25 J.T.U. • Need was felt to measure turbidity values even less than one unit because turbidities of treated water usually fall within the range of 0 to 1 unit • Different types of secondary instruments were developed to measure turbidity values in low range Contd...
• The results obtained with different types of secondary instruments frequently do not match closely with one another, even though the instruments are precalibrated against Jackson Candle turbidimeter, because of fundamental differences in optical systems • Nephelometers developed for measuring low turbidities give comparatively good indications of the intensity of light scattered at right angles to the incident light, and are specified as the standard instrument for measurement of low turbidities • The prescribed for turbidity measurement by Nephelometer is Nephelometric Turbidity Units (N.T.U.) • Formazin polymer is used as the reference turbidity standard suspension • Because there is no direct relationship between the intensity of light scattered at 90O angle and Jackson candle turbidity there is no basis for the practice of calibrating a Nephelometer in terms of candle units • However specific concentration of formazin polymer suspension defined as 40 NTU turbidity has an approximate turbidity of 40 JTU Contd...
Method Nephelometric • Nephelometric method of turbidity measurement is based in a 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 same conditions • Higher the intensity of scattered light the higher the turbidity • Turbidimeter with a tungston filament lamp as a light source for illuminating the sample and a photoelectric detector with a read out device is a system used for turbidity measurement by turbidimeter • Meter is designed to prohibit stray light reaching to detector • Short warm period is necessary to make the instrument free from significant drift • Clear colourless glass tube is used for sample Contd...
Hardness Definition • Total Hardness is defined as the sum of the calcium and magnesium concentrations, both expressed as calcium carbonate, in mg/L • Originally water hardness was under stood to be a measure of the capacity of eater to precipitated soap • Soap is precipitated chiefly by calcium and magnesium ions present. Other prevalent cations also precipitate soap but they often are in complex forms and minimal concentration Significance • Scale formation in boilers, pipes and cooking utensils • Adverse effect on domestic use • Encrustation in water supply structure • Cathartic and diuretic effect Contd...
Type • Carbonate hardness • Non carbonate hardness Methods of Analysis Hardness by calculation • Calcium can be estimated by AAS, ICP and EDTA titrimetric methods • Magnesium can be estimated by AAS, ICP and Gravimatric method Total Hardness by Calculation : mg CaCO3 / L = 2.497 [Ca mg/L] + 4.118 [Mg mg/L] Contd...

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LSD-NEERI- Water Quality Analysis.pdf

  • 1.
    Water Quality Analysis LaboratoryMethods Dr. (Mrs.) Leena Deshpande National Environmental Engineering Research Institute (NEERI), Nagpur Council of Scientific & Industrial Research, New Delhi, Govt. of India
  • 2.
    Clouds Water bodies Water quality Atmospheric Constituents Surfacerunoff Leachates from Soil and Rocks Dispersion & Dissolution in Water
  • 3.
    Quality changed Non-abstractive uses Water Ground Water SeaWater Abstractive Uses Domestic Irrigation Industrial Quantity returned Quantity lost Inland Surface Water
  • 4.
    Water Transport Sea In-land Waters Food • Fishing •Sea Food • Pond Food • Lean Period River bed crops Recreation • Swimming • Sunbath & Swimming • Picnic Spot • Water Sports • Pilgrimage Eco-system • Conservation • Rejunvetion • Technical interferences • Technological Interventions Non-abstractive uses
  • 5.
    Adverse Effects ofImpurities Problems ¾ Aesthetically not acceptable and Palatability decreases ¾ Health related problems ¾ affect mucous membrane ¾ gastro-intestinal irritation ¾ Dental and skeletal fluorosis ¾ Methaemoglobinemia ¾ Encrustation in water supply structure ¾ Adverse effects on domestic use Constituents Responsible • Clay, Silt, Humus, Colour • pH • Hardness, TDS, Ca, Mg, SO4 • Fluoride • Nitrate • Hardness, TDS • Ca, Mg, Cl
  • 6.
    ¾ Eutrofication ofthe waterbody ¾ Taste, discolouration and corrosion of pipes fittings and utensils ¾ Promotes iron bacteria ¾ Corrosion in water supply system ¾ Carcinogenic effect ¾ Toxic effect ¾ Formation of chlorophenols with chlorine ¾ Imparts unpleasant taste and odour after chlorination ¾ Water-borne diseases • Zoo & Phyto, Phosphate, Nitrate • Iron, Mn, Cu, Zn, Alkalinity • Fe & Mn • pH, Cl • Cr, As • Cd, Pb, Hg • Phenols • Oil & grease • Bacteria & viruses Adverse Effects of Impurities
  • 7.
    Contamination / Pollution 9During its traverse water picks up impurities in varying amounts 9 Gases from atmosphere 9 Inorganic and organic salts from top soil and geological strata 9 During its traverse water get contaminated by inorganic and organic salts sometimes beyond desirable limits Pollution 9 Presence of undesirable substances in the quantities which are harmful to man vegetation or property is referred to as pollution 9 Quality of water depends upon quality and quantity of inorganic and organic salts present in water
  • 8.
    Safe Water/ Wholesome Water Aesthetically acceptable Chemicallysafe Organic substances absent Free from bacteria Radioactive elements absent
  • 9.
    Water Quality Assessment ÈTo measure concentration of the constituents in quantity for characterisation of water for different uses È Of the various parameters in potable water few are objectionable even when present in very small quantity È Others if only present in unusual quantities as to relegate the water from the potable to the unusable class È The analyst familiar with water quality characterisation will often select parameters to be measured based on experience and intuition
  • 10.
    Water Analysis -Key Factors Factors Reporting the values Proper Labeling Sampling Selection of Parameters Precision and accuracy of method selected Preservation
  • 11.
    Water Quality Assessment: Potable & Industrial Uses Parameters Physical Inorganic OR Chemical Toxic Metals Organic, Nutrient & Demand Alpha emitter Beta emitter Biology Radioactive elements Bacteriological Phytoplankton Zooplankton Total Coliform Faecal Coliform BOD COD Phenols Oil & Grease Pesticides Nitrate Copper Chromium Cadmium Zinc Lead Mercury Iron Manganese Temperature PH Colour Conductivity Odour Total Dissolved Taste Solids Turbidity Hardness Fluoride Calcium Alkalinity Magnesium Nitrate Chloride Phosphate Sulphate
  • 12.
    ¾ Irrigation 9 pH 9Conductivity 9 Sodium & Potassium 9 Nutrients 9 Specific compounds ¾ Industries 9 As per specific requirement ¾ Domestic Consumption 9 As per BIS Standards ¾ Water Bodies 9 As per CPCB guidelines Water Quality Consideration
  • 13.
    S. No. CharacteristicsA’ B’ C’ D’ E’ 1. Dissolved Oxygen, mg/L, Min 6 5 4 4 - 2. Biochemical Oxygen Demand, mg/L, Max 2 3 3 - - 3. Total Coliform Organisms*, MPN/100 mL, Max 50 500 5000 - - 4. Total Dissolved Solids, mg/L, Max 500 - 1500 - 2100 5. Chlorides (as Cl), mg/L, Max 250 - 600 - 600 6. Colour, Hazen Units, Max 10 300 300 - - 7. Sodium Absorption Ratio, Max - - - - 26 8. Boron (as B), mg/L, Max - - - - 2 9. Sulphates (as SO4), mg/L, Max 400 - 400 - 1000 10. Nitrates (as NO3), mg/L, Max 20 - 50 - - 11. Free Ammonia (as N), mg/L, Max - - - 1.2 - 12. Conductivity at 25oC, micromhos/cm, Max - - - 1000 2250 13. pH value 6.5-8.5 6.5-8.5 6.5-8.5 6.5-8.5 6.5-8.5 14. Arsenic (as As), mg/L, Max 0.05 0.2 0.2 - - 15. Iron (as Fe) , mg/L, Max 0.3 - 50 - - 16. Fluorides (as F), mg/L, Max 1.5 1.5 1.5 - - 17. Lead (as Pb), mg/L, Max 0.1 - 0.1 - - 18. Copper (as Cu), mg/L, Max 1.5 - 1.5 - - 19. Zinc (as Zn), mg/L, Max 15 - 15 - - Classification of Inland Surface Waters (CPCB Standards) •If the coliform count is found to be more than the prescribed tolerance limits, the criteria for coliforms shall be satisfied if not more than 20 percent of samples show more than the tolerance limits specified, and not more than 5 percent of samples show values more than 4 times the tolerance limits. Further, the faecal coliform should not be more than 20 percent of the coliform. Source : Indian Standard (IS:2296-1982). A’ Drinking water source without conventional treatment but after disinfection D’ Propagation of wild life, fisheries B’ Outdoor bathing (organised) E’ Irrigation, industrial, cooling, controlled C’ Drinking water source with conventional treatment followed by disinfection waste disposal
  • 14.
    ¾ All livingorganisms depend upon oxygen to maintain the metabolic processes that produce energy for growth and reproduction ¾ Dissolved oxygen is important in precipitation and dissolution of inorganic substances in water Need ¾ To assess quality of raw water ¾ To check on pollution ¾ Determination of biological changes by aerobic or anaerobic organisms ¾ D.O. is the basis of BOD test to evaluate pollution potential of wastes ¾ All aerobic biological wastewater treatment processes ¾ Important factor in corrosion. Dissolved Oxygen
  • 15.
    Principle ¾ Oxygen presentin sample oxidizes the divalent manganous to its higher valency which precipitates as a brown hydrates oxide after addition of NaOH and KI ¾ Upon acidification, manganese revert to divalent state and liberates Iodine from KI equivalent to D.O. content in the sample ¾ The liberated Iodine is titrated against standard (N/40) solution of Sodium thiosulphate using starch as an indicator. Methodology The Winkler method with Azide modification
  • 16.
    Procedure ¾ Collect samplein BOD bottle ¾ 2 ml MnSO4+ 2 ml Alkali iodide-azide+close stopper ¾ Mix well + allow the ppt to settle ¾ Add 2 ml concentrated H2SO4 + mix well till ppt dissolves ¾ Take 203 ml (Correspond to 200 ml) sample in a conical flask+titrate against Sodium thiosulphate (0.025 N) till pale yellow colour + starch + titrate till blue to colourless Calculation ¾ 1 ml of 0.025N Na2S2O3 = 0.2 mg of O2 ¾ D.O. in mg/l =(0.2 x 1000) x ml of thiosulphate 200 Results : D.O. mg/l
  • 17.
    Interferences ¾ Ferrous ion ¾Ferric ion ¾ Nitrite ¾ Microbial mass ¾ High suspended solids To reduce interferences, modification in the estimation procedures are suggested ¾ Alsterberge azide : Nitrite, higher concentration of ferric ions ¾ Redeal Stewart : Ferrous ion ¾ Alum / Flocculation : High suspended solids ¾ Copper Sulphate Sulfamic acid flocculation : Biological flocs ¾ Alkaline Hypochlorite : Complex of sulphur compound
  • 18.
    A bioassay test,involving measurement of oxygen consumed by micro-organisms while stabilizing biologically decomposable organic matter under aerobic conditions Need ¾To determine the pollution load of waste water ¾The degree of pollution in water sources ¾Self purification capacity of sources ¾Designing of treatment facilities ¾Efficiency of waste water treatment methods Biochemical Oxygen Demand
  • 19.
    Methodology Principle ¾ The BODtest is based upon determinations of dissolved oxygen ¾ It can be measured directly ¾ In general, a dilution procedure is applied.
  • 20.
    Procedure Preparation of dilutionwater ¾ Aerate the required volume of D.W. by bubbling compressed air for 1-2 days to attain D.O. saturation ¾ Add 1 ml each per litre of dilution water Phosphate buffer Magnesium sulphate Calcium chloride Ferric chloride ¾ Mix well ¾ In case, waste not expected sufficient bacterial population, add seed (2 ml settle sewage / litre of dilution water)
  • 21.
    Determination of D.O. i)Samples and ii) Blank, on initial and after 5 days ¾ 2 ml MnSO4 + 2 ml Alkali-iodide-azide+stopper immediately ¾ Mix well + allow the ppt. to settle ¾ Add 2 ml concentrated H2 SO4 + mix well till ppt. dissolve ¾ Take 203 ml (correspond to 200 ml) sample in a conical flask ¾ Titrate against sodium thiosulphate (0.025 N) till pale yellow colour + starch solution + blue colour + titrate till colourless
  • 22.
    Observations D0 = D.O.in sample on 0th day D1= D.O. in sample on 5th day C0 = D.O. in Blank on 0th day C1 = D.O. in Blank on 5th day C0 – C1 = D.O. depletion in dilution water alone D0 – D1 = D.O. depletion in sample + dilution water (D0 - D1) - (C0 – C1) = D.O. depletion due to microbes
  • 23.
    Calculation 1 ml of0.025 N sodium thiosulphate = 0.2 mg of Oxygen D.O. in mg/l = (0.2 x 1000) x ml of thiosulphate 200 B.O.D. in mg/l (D0-D1) – (C0-C1) mg x Decimal fraction of sample used Results B.O.D. 5 days at 200 C = mg/l
  • 24.
    Interferences ¾ Ferrous ion ¾Ferric ion ¾ Nitrate ¾ Microbial mass ¾ High suspended solids ™ Lack of nutrients in dilution water ™ Lack of acclimated seed organisms ™ Presence of heavy metals ™ Presence of toxic materials
  • 25.
    Bacteriological Analysis Bacteria Single cellmicroscopic organisms lacking chlorophyll Coliform group Contamination • Insanitary condition of surrounding area • Unhygienic practices • Discharge/seepage of sewage and domestic wastewater Need • Impact on water quality • Potability for human consumption • To prevent water-borne diseases • To assess the quality of raw and treated water • Specially to detect Faecal Contamination Bacteriological analysis : mainly includes estimation of • Total coliforms • Faecal coliforms
  • 26.
    Methodology Approved techniques generallyused as per "Standard Methods for the examination of water and wastewater” – .Membrane Filter (MF) – Multiple Tube Dilution (MTD) MF-technique Principle Biochemical reactions are used to detect the various groups of micro-organisms MF-technique - Merits • Results in 24 hours (MTD - 48 to 96 hours) • Larger volume of samples can be tested (MTD - less volume) • Results with greater precision (MTD - MPN) • Require less laboratory space (MTD – More space) • Easy processing (MTD – Tedious) • Useful during normal and emergencies (MTD – Difficult in emergencies) Limitations : Samples with more turbidity
  • 27.
    Colour Coloured water isnot acceptable for drinking (Aesthetic as well as toxicity reasons) Industrial wastewater require colour removal before discharge into water courses Definition • The term colour means true colour that is the colour of water from which turbidity has been removed. True colour of water is due to dissolved material • Apparent colour is due to suspended matter as well as due to substances on solution removed by filtration Unit for Measurement of colour • Unit for colour measurement is based on platinum cobalt scale Contd...
  • 28.
    Methods for ColourMeasurement Visual Comparison Method • Colour of the sample is determined by visual comparison with known concentration of coloured colutions prepared by diluting stock platinum cobalt solution • OR properly calibrated glass coloured disk is used for comparison • This method is useful for potable water and water in which colour is due to naturally occuring materials • This method is not applicable to most highly coloured industrial wastewater Spectrophotometric Method • This method is applicable to potable and waste both domestic and industrial • In this method light absorbed or transmitted is measured at dominant wavelength of a particular hue of sample • Spectrophotometer should have an effective operating range from 400 to 700 nm before measurement remove turbidity either by filtration or by centrifuging • Colour hues for dominant wavelengths ranges are Contd...
  • 29.
    Definition Measure of theability of aqueous solution to carry an electric current # Concentration of ions # Mobility # Valency # Temperature Degree of Minerilization Effect on plants and animals Check purity of distilled water Monitoring seasonal variation of raw water or wastewater Determine sample size for chemical analysis Check results of chemical analysis Estimate TDS µ mho/cm or µs/cm Conductance is measured between two spacially fixed and chemically inert platinum electrodes Unit Conductivity Measurement Conductance(G) ∝ Area (A) ∝ 1/Distance (L) G = K(A/L) A = 1cm2 L = 1 cm G = K K is called conductivity or specific conductance Conductivity Meter Significance
  • 30.
    Total Dissolved Solids Definition Portion ofSolids that passes through a filter of 2.0 µm or smaller pore size Significance Palatability decreases Gastro intestinal irritation Unsuitable for many industrial uses Evaporation at 180 + 20C Calculations Method Evaporation Method •Yield values for TDS closer to obtained through summation •At this temp. all mechanically occluded water is lost •Some samples may require prolonged drying and desiccation Conductivity
  • 31.
    • pH =- log10 [H+] = log10 1/[H+] OR [H+] = 10-pH This method has advantage because all states of acidity and alkalinity of solutions with respect to hydrogen and hyroxide ions can be expressed by a series of positive numbers between 0 to 14 [ H+] (10o) 10-1 10-2 10-3 10-4 10-5 10-6 10-7 10-8 10-9 10-10 10-11 10-12 10-13 10-14 pH 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 pOH 14 13 12 11 10 9 8 7 6 5 4 3 2 1 0 [OH-]10-14 10-13 10-12 10-1110-10 10-9 10-8 10-7 10-6 10-5 10-4 10-3 10-2 10-1 10-0 • Chemical reactions depend on pH • Water Supply and Waste Water Treatment • Water Softening ,Precipitation., Coagulation, Disinfection, Corrosion Control,Alkalinity and CO2 Measurement and fluoride activity • Electrometric method - Using pH meter and electrodes • e.m.f. produced in glass electrode system varies linearly with pH • pH meter is calibrated potentiometrically with electrode system using standard buffers having assigned values so that pH = - log10 [H+] • pH Hydrogen Ion Exponent 6.5 - 8.5 Definition Significance Measurement pH Meter
  • 32.
    Sources • Fertilizers andmanure • Decayed vegetable • Animal feedlots • Municipal wastewater and sludge disposal to land • Industrial discharges • Leachates from refuse dumps • Septic systems and • N-fixation from atmosphere by bacteria and lightning Nitrate
  • 33.
    Chloride Presence in NaturalWaters • Dissolution of salt deposits • Discharges of effluents • Oil well operations • Sewage discharges • Irrigation drainage • Sea water intrusion in coastal areas
  • 34.
    Chloride Methodology : AnArgentometric Method • Principle Chloride is determined in a natural 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. 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 blank N = Normality of AgNO3 used
  • 35.
    Methods for NitrateEstimation A) Ultraviolet Spectrophotometric Method • Useful for uncontaminated natural waters and potable water supplies that have low organic content • Follows Beer’s law upto 11 mg/L as N • Interferences - Dissolved Organic Matter - Surfactants - Nitrite and Hexavalent Chromium • Procedure - Filter the sample - Add 1 ml of 1N HCl per 50 ml of sample - Read absorbance or tranmittance at 220 nm and 275 nm - Set 0 absorbance or 100% tranmittance with distilled water
  • 36.
    B) Nitrate ElectrodeMethod • Useful for Nitrate concentration range of 0.14 to 1400 mg/L NO3-N • Interferences - Chloride and bicabonate with weight ratios to NO3-N 10 or 5 respectively - NO2, CN, Sulphide, Br, I, Chlorite and Chlorate
  • 37.
    C) Phenoldisulphonic Acid(PDA) Method • Nitrate reacts with Phenoldisulphonic acid to produce nitro derivatives that in alkaline solution rearranges its structure to form yellow colored compound with characteristics that follows Beer’s law • Chloride interferes seriously which can be overcome by precipitation of chloride with Ag+ as AgCl
  • 38.
    Fluoride Significance Dual significance inwater High concentration of F- causes dental Fluorosis Concentration 0.8 mg/L results in dental Carries Essential to maintain F- concentration between 0.8 mg/L to 1.0 mg/L in drinking water
  • 39.
    Fluoride Methods Colorimetric SPADNS Method Principle:Under acidic conditions fluorides (HF) react with zirconium SPADNS solution and the lake (colour of SPADNS reagent) gets bleached due to formation of ZrF6 . Since bleaching is a function of fluoride ions, it is directly proportional to the concentration of fluoride. It obeys Beers law in a reverse manner. Ion Selective Electrode Method Principle: The fluoride sensitive electrode is of the solid state type, consisting of a lanthanum fluoride crystal; in use it forms a cell in combination with a reference electrode, normally the calomel electrode. The crystal contacts the sample solution at one face and an internal reference solution at the other. A potential is established by the presence of fluoride ions across the crystal which is measured by a device called ion meter or by any modern pH meter having an expanded millivolt scale. Calculate mg F- / L present in the sample using standard curve
  • 40.
    Sulphate Significance • Occurs innatural water • High concentration of Sulphate laxative effect (enhances when sulphate consumed with magnesium) • Problem of scaling in industrial water supplies • Problem of odour and corrosion in wastewater treatment due to its reduction to H2S
  • 41.
    Sulphate Method Spectorphotometric Method Principle: Sulfateions are precipitated as BaSO4 in acidic media (HCl) with Barium Chloride. The absorption of light by this precipated suspension is measured by spectrophotometer at 420 nm or scattering of light by Nephelometer Calculate mg / L SO4 = mg SO4 x 1000 ml sample
  • 42.
    Ammonia • Ammonia ispresent naturally in surface and wastewaters. Its concentration is generally low in ground waters because it adsorbs in soil particles and clays and is not leached readily from soils. • It is produced largely by de-amination of organic nitrogen containing compounds and by hydrolysis of urea • In the chlorination of water, chlorine reacts with ammonia to form mono and dichloramines (combined residual chlorine) • Ammonia concentration in water vary from less than 10µg in some natural surface and ground waters to more than 30 mg/L in some wastewaters
  • 43.
    Methods for AmmoniaEstimation A) Nesslerization Method • Direct nesslerization method is useful for purified natural water and highly purified wastewater effluents with very light color and having NH3-N concentrations more than 20 µg/L • Applicable to domestic wastewater only when errors of 1 to 2 mg/L are acceptable • The graduated yellow to brown colors produced by nessler-ammonia reaction absorb strongly over wide wavelength range • Low ammonia concentration of 0.4 to 5 mg/L can be measured with acceptable sensitivity in wavelength region from 400 to 425 nm with 1cms light path • A light path of 5 cm extends measurements of ammonia concentrations range of 5 to 60 µg/L
  • 44.
    • The reddishbrown color at ammonia levels approaching 10 mg/L may be measured in the wavelength region of 450 to 500 nm • Thus, the proper selection of light path and wavelength permits the photometric determination of ammonia concentrations over a considerable range • Carefully prepared nessler reagent may respond under optimum conditions to as low as 1µg NH3-N/ 50mL (100µg/L). However, reproducibility below 100 µg/L may be erratic • Interferences - Turbidity, color , magnesium and calcium
  • 45.
    B) Ammonia SelectiveElectrode Method • The ammonia selective electrode uses a hydro-phobic gas permmeable membrane to separate the sample solution from an electrode internal solution of ammonium chloride • Dissolved ammonia is converted to NH3(aq) by raising pH to above 11 with a strong base, which diffuses through membrane and changes the internal solution pH that is sensed by a pH electrode • The fixed level of chloride in the internal solution is sensed by a chloride ion-selective electrode that serves as the reference electrode • Applicable to the measurement of 0.03 to 1400 mg NH3-N/L in potable and surface waters and domestic and industrial wastes • High concentrations of dissolved ions affect the measurements but color and turbidity do not. • Interference - Amines are a positive interference - Hg and silver interfere by complexing with ammonia
  • 46.
    C) Titrimetric Method •The method is used only on samples that have been carried through preliminary distillation • Titrate ammonia in distillate using standard 0.02N Sulphuric acid with boric acid indicator solution
  • 47.
    Phosphates • Phosphate occursin traces in many natural waters, and often in appreciable amounts during periods of low biologic productivity. Waters receiving raw or treated sewage agricultural drainage, and certain industrial waters normally contain significant concentrations of phosphate.
  • 48.
    Methods for PhosphorusEstimation A) Vanadomolybdophosphoric Acid Method • In a dilute orthophosphate solution, ammonium molybdate reacts under acid conditions to form a heteropoly acid. In the presence of vanadium, yellow vanadomolybdophosphoric acid is formed. The intensity of yellow color is proportional to phosphate concentration • Minimum detectable concentration is 0.2 mg P/L in 1 cm cell • Interferences - Silica and arsenate cause positive interference if the sample is heated - Negative interferences are caused by fluoride, thorium, bismuth, sulphide, thiosulfate, thiocyanate or excess molybdate - Blue color is caused by ferrous iron but this does not affect results if its concentration is less than 100 mg/L - Sulphide interference may beremoved by oxidation with bromine water
  • 49.
    Procedure - Sample pHadjustment if pH 10 - Removal of excessive color by shaking with activated carbon - Color development with vanadate-molybdate reagent - Measurement of color absorbance at wavelength of 400 to 490 nm
  • 50.
    B) Stannous ChlorideMethod • Molybdophophoric acid is formed and reduced by stannous chloride to intensely colored molybdenum blue • This method is more sensitive than above method and minimum detectable concentration is about 3 µg P/L • Interferences - Silica and arsenate cause positive interference if the sample is heated - Negative interferences are caused by fluoride, thorium, bismuth, sulphide, thiosulfate, thiocyanate or excess molybdate - Blue color is caused by ferrous iron but this does not affect results if its concentration is less than 100 mg/L - Sulphide interference may beremoved by oxidation with bromine water • Procedure - Sample pH adjustment if pH 10 - Color development with molybdate reagent - Measurement of color absorbance at wavelength of 690 nm
  • 51.
    Limit of Ironand Manganese in Drinking Water • As per WHO guidelines for domestic water, iron should not exceed the limit of 0.3 mg/l • Above 200mg/l iron is toxic to human health • Manganese concentration as per WHO guideline is 0.05 mg/l • However average manganese level in drinking water range from 5 to 25 ug/l • At concentration exceeding 0.15 mg/l, manganese imparts undesirable taste
  • 52.
    Iron and Manganese •Presence of excess of iron and manganese in water causes discoloration, turbidity and deposits • Iron and manganese bearing water have astringent metallic or bitter taste • Precipitation of iron and manganese imparts colour to water from yellow to brownish black, which becomes objectionable to consumers • Manganese concentration ranging from 8-14 mg/l is toxic to human • Excess of iron facilitates growth of iron bacteria which causes blocking of pipes, meters etc.
  • 53.
    Limit of Ironand Manganese in Drinking Water • As per WHO guidelines for domestic water, iron should not exceed the limit of 0.3 mg/l • Above 200mg/l iron is toxic to human health • Manganese concentration as per WHO guideline is 0.05 mg/l • However average manganese level in drinking water range from 5 to 25 ug/l • At concentration exceeding 0.15 mg/l, manganese imparts undesirable taste
  • 54.
    Methods for Detectionof Iron and Manganese in Water • Atomic Absorption spectrophotometer (AAS) • Inductively Coupled Plasma (ICP) • Colorimetric method In colorimetric method iron is detected at wavelength 510 nm and manganese is detected at 525 nm. 1. Iron:- Phenanthroline method 2. Manganese:- Persulphate method Periodate method
  • 55.
    Determination of Metals InductivelyCoupled Plasma-Atomic Emission Spectrometer
  • 57.
    ICP TORCH •Radio frequency 27-49MHz 700-1599 W •Gas- Argon
  • 58.
    Steps involved inthe analysis of aqueous samples by ICP-AES
  • 59.
    Procedure Instrument set up •Warmup for 30 min •Check the alignment of plasma torch •Make Cu/Mn ratio adjustment •Calibrate instrument using calibration standards and blank •Aspirate the standard and blank for 15s •Rinse with calibration blank for at least 60s to eliminate any carryover from previous standards •Ensure the concentration values within the 5% error
  • 60.
    Analysis of samples •Analysisthe samples using calibration blank •Analyse samples alternately with analyses of calibration blank • Rinse at least for 60s •Examine each analysis of the calibration blank to verify that carry over memory effect is no more •Make appropriate dilutions of the sample to determine concentrations beyond the linear calibration Instrument quality control •Reanalyse one or more samples analysed just before termination of the analytical run •Use this analysis to verify accuracy and validity of the calibration standards
  • 62.
    End Point pH Alkalinity D e f i n i t i o n Sluggishresponse due to coating of soap, oily matter in potentiometric Colour, Turbidity with indicator method Significance Acid neutralizing capacity of water •Treatments of water and wastewater •Interpretation and control of water and waste water treatment processes Interference Carbonate Bicarbonate Hydroxyl Borates Phosphates Silicates Other Bases Due to All Titratable Bases Potentiometric titration Titration using indicator Total Alkalinity 4.5 Phenolphthalein Alkalinity 8.3 M e a s u r e m e n t
  • 63.
    Turbidity General • Turbidity inwater is caused by suspended matter such as Clay Silt Finely divided organic and inorganic matter Soluble coloured organic compounds Plankton and other microscopic organisms Definition • Turbidity is an expression of the optical property that causes light to be scattered and absorbed • It is not possible to correlate turbidity with the weight concentration of suspended matter because light scattering properties of the suspended particulate matter depends upon size, shape and refractive index of the particulates Contd...
  • 64.
    Significance • Clarity ofwater is important for human consumption • Manufacturing processes such as beverages, and many food products need clear water Unit for Turbidity Measurement • Previously standard method for measurement of turbidity was based on the Jackson Cnadle turbidimeter • The lowest turbidity value that can be measured by this instrument is 25 J.T.U. • Need was felt to measure turbidity values even less than one unit because turbidities of treated water usually fall within the range of 0 to 1 unit • Different types of secondary instruments were developed to measure turbidity values in low range Contd...
  • 65.
    • The resultsobtained with different types of secondary instruments frequently do not match closely with one another, even though the instruments are precalibrated against Jackson Candle turbidimeter, because of fundamental differences in optical systems • Nephelometers developed for measuring low turbidities give comparatively good indications of the intensity of light scattered at right angles to the incident light, and are specified as the standard instrument for measurement of low turbidities • The prescribed for turbidity measurement by Nephelometer is Nephelometric Turbidity Units (N.T.U.) • Formazin polymer is used as the reference turbidity standard suspension • Because there is no direct relationship between the intensity of light scattered at 90O angle and Jackson candle turbidity there is no basis for the practice of calibrating a Nephelometer in terms of candle units • However specific concentration of formazin polymer suspension defined as 40 NTU turbidity has an approximate turbidity of 40 JTU Contd...
  • 66.
    Method Nephelometric • Nephelometric methodof turbidity measurement is based in a 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 same conditions • Higher the intensity of scattered light the higher the turbidity • Turbidimeter with a tungston filament lamp as a light source for illuminating the sample and a photoelectric detector with a read out device is a system used for turbidity measurement by turbidimeter • Meter is designed to prohibit stray light reaching to detector • Short warm period is necessary to make the instrument free from significant drift • Clear colourless glass tube is used for sample Contd...
  • 67.
    Hardness Definition • Total Hardnessis defined as the sum of the calcium and magnesium concentrations, both expressed as calcium carbonate, in mg/L • Originally water hardness was under stood to be a measure of the capacity of eater to precipitated soap • Soap is precipitated chiefly by calcium and magnesium ions present. Other prevalent cations also precipitate soap but they often are in complex forms and minimal concentration Significance • Scale formation in boilers, pipes and cooking utensils • Adverse effect on domestic use • Encrustation in water supply structure • Cathartic and diuretic effect Contd...
  • 68.
    Type • Carbonate hardness •Non carbonate hardness Methods of Analysis Hardness by calculation • Calcium can be estimated by AAS, ICP and EDTA titrimetric methods • Magnesium can be estimated by AAS, ICP and Gravimatric method Total Hardness by Calculation : mg CaCO3 / L = 2.497 [Ca mg/L] + 4.118 [Mg mg/L] Contd...