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Standard Operation Procedure - Ru

1. 47 TITRATION PRECAUTIONS c ccccsssscecsssccecssseeecsscsensesseeeeseccsenseecseseeeccsssaeaessaaeseceseeasecssesaeccsssaeeaeseauaaecessaaaeess 48 REAGENTS AND SOLUTIONS ccssccssssseecesseeececssseseccssseeecsseseneeecseensecsesesecesseueesseseseecsuaaecseseeecesseenaesseenaaees 48 PROCEDURE BICARBONATE ccssssccccesscecessseecesssneeeeccssneeecssseneceseseeeeessensecesseaeecsesuuecseesanaaeseaesecesseaaeesseeeneess 48 CALCULATION o 49 PROCEDURE CARBONATE c 49 CALCULA TION tostadas a titanio 49 Standard Operation Procedure for detection of Potassium in water esses 50 Scope and application iR er IR RP ERR ve Rsde tint skies es entiers essi nutans 50 Storage Or samples ene eee ad e o M LU ET ir SE 50 Minimum detectable concentration 50 Jae p 50 REAGENTS erotische seb ae ee ee oe pe M mr 50 Operati Jri may u EE 51 Shu tdoWmiioc iternm eei ME MM M aasE 51 Operating precautions siii p ER PvE aea aeri as deae ER aa E EEE aE EEG Ran Ere 52 Standard Operation Procedure for detection of Sodium in water 53 Scope and application 3 coco I E REN sse neis EIU 53 Storage orLsamplessioenein e o o o E E
2. 21 CALIBRATION PROCEDURE Temperature Calibration 21 Standard Operation Procedure Manual for Analysis of Drinking water quality Page 1 of 64 OPERATIONAL PROCEDURE Pl 0o cccsecessscsssesescscscscscssscscscssscscscesscscscsssssssesesssasasasssasaasacssasavacecacacasecsueracesess 22 Standard Operation Procedure for detection of Color in water J 23 Ups ERR 23 SCOPE tac eo ir 23 RESPONSIBILITY dais 23 DEFINITIONS 225 cc20c5 2cessesas3t HPHHNS 23 HEALTH AND SAFETY D u A o o HRU T 23 CAUTION c P 23 PRINCIPLES 2 u io 24 APPLICATION tc 24 INTERFERENCE 2 reete S nu aa u entendiendo IM IPIE 24 APPARATUS Ute o O a Ds a 24 PREPARATION OF STANDARDS 24 PROCEDURE sans nu e us S EN na s E E EA E EE ET NE 25 CALCULATION S R u tes ec diui ee 25 Standard Operation Procedure for detection of Arsenic in water T T 26 PURPOSE te erii o e 26 SCOPE nose MEE EM 26 PRINCIPDIE terio
3. J 37 dilige tarta OS awaq ps qa aasawa O nea 37 SCOPE AND APPLICATO N e 37 RESPONSIBILITY ce e ni 37 SUMMARY OF METHOD L u L Ea uu uha A EEEO EERE 37 HEALTH AND SAFETY WASTE HANDLING 37 hudiidid Slc E 37 REAGENTS AND SOLUTIONS uu u oper Errat neo sderteweddnceceissneetunads aaa r ara aE Eiaa 38 PROCEDURE ai mem m ce D A 38 Standardization of Silver Nitrate Titrant a 38 SAMPLE PREPARATION is 39 Calculation sido Eden ME M UU MR 40 Standard Operation Procedure for detection of Total Hardness in water 41 PURPOSE 2 u ai tias MI MI E MA MEE e EVE EE 41 SCOPE AND APPLICATION s 41 RESPONSIBILITY eire tre ERROREM Eesti aibi titer eius 41 PRINCIPLE SUMMARY OF METHOD 41 HEALTH AND SAFETY WASTE HANDDLINQG eene enne enne nennen nennen nennt sse antennes esse sas tese s ete se ansn nna 41 hum iiie AA a iaa dk dat 42 TITRATION PRECAUTION kr 42 REAGENTS AND SOLUTIONS scm 42 duisi 43 CALCULATION E 43 Stan
4. Press ON to switch on the meter and the MEAS in indicator appear on the top of LCD Dip probe into the sample Ensure that the solution level is above its upper steel band Stir the probe gently in the sample to create a homogenous sample Allow time for the reading to stabilize Note the reading on the display Press MODE to toggle between conductivity and TDS measurement After noting EC value remove the electrode from the sample and rinse it with water distilled de ionized In case sample solution is viscous then wipe the electrode with the help water de ionized or distilled and tissue paper RFERENCES p 2 44 APHA 20 Ed Instruction Manual CON 510 RELATED DOCUM ENTS Procedure for Calibration program RELATED RECORD B Daily Calibration Record of EC meter ANNEXURE Standard Operation Procedure Manual for Analysis of Drinking water quality Page 22 of 64 Standard Operation Procedure for detection of Color in water Procedure for Operation and Calibration for Color Determination of Water by Visual Comparison Method PURPOSE To establish a procedure for examination of true not apparent color of water SCOPE This procedure is applicable for determination of true color of water only RESPONSIBILITY WAL Analyst Operation and Calibration WQL Manager Receiving sample log book entry and Implementation of this SOP WQ Consultant QC QA DEFINITIONS Apparent color i
5. Accessories Select 8 cell holder and click cell number of cell type icon to select the active cell position e Quantitative measurement window It has 4 parts standards measurement table unknown sample measurement table calibration curve and performance Total Iron Determination and Calibration Curve Sample preparation Pipette 10 00 mL of mixed acid zirconyl SPADNS reagent to each standard and mix well Avoid contamination Set photometer to zero absorbance with the reference solution and obtain absorbance readings of standards at 570nm Plot a curve of mg F versus absorbance Prepare a new standard curve whenever a fresh reagent or a different standard temperature is used After taking reading of all standards check the curve and R2 value R2 value must be 0 98 Once we calibration cure is produced and have satisfactory R2 value click in the unknown sample table and prepare the unknown sample as described in section10 2 1 RFERENCES e p 4 79 86 APHA 20 Ed e UVWIN 5 0 instruction manual ANNEXURE Nil Standard Operation Procedure Manual for Analysis of Drinking water quality Page 36 of 64 Standard Operation Procedure for detection of Chloride in water Standard Procedure for Chloride Analysis in Water by the Argentometric Method 4500 CI B APHA PURPOSE To establish a procedure for chloride determination in water SCOPE AND APPLICATION This method is based on Standard Methods 4500 CI B APHA
6. Titrate with standard silver nitrate titrant to a pinkish yellow end point Be consistent in end point recognition and record ml of titrant 1ml of AgNO3 is equal to 500 mg of chloride Factor of standardization is calculated as Factor F theoretical reading actual reading SAM PLE PREPARATION Allow samples to come to room temperature prior to analysis Shake the sample bottle for approximately five 5 seconds to ensure homogeneity of the water sample Fill burette to the 0 0 mark with 0 0141N silver nitrate titrant Use a Class A 50 ml graduated cylinder to measure 20 ml of sample Transfer the sample to a 50 ml beaker Measure the pH of sample and adjust pH of the sample as necessary to a pH between 7 10 with 0 01N sulfuric acid or 0 01N sodium hydroxide Add 1 ml of potassium chromate indicator to sample and mix well Titrate with standard silver nitrate titrant to a pinkish yellow end point i e the color persists throughout the sample and record ml of titrant on the chloride Be Standard Operation Procedure Manual for Analysis of Drinking water quality Page 39 of 64 consistent in end point recognition If more than 10 ml of silver nitrate titrant is required to reach a pinkish yellow end point dilution is necessary Deionized water is used as the diluent Calculation mg CI L A B F N 35450 ml of sample Where A ml titrant for sample B ml titrant for blank F Factor N normality of silver nitrate AgNO3 ti
7. Orthophosphate in excess of 25 mg L interferes by precipitating as silver phosphate Iron in excess of 10 mg L interferes by masking the end point In general if color is present in the sample it will mask the end point Aluminum Hydroxide AI OH 3 is used for pretreatment of highly colored samples REAGENTS AND SOLUTIONS 1N Sulfuric Acid Cautiously add 28 0 ml concentrated sulfuric acid to approximately 500 ml deionized water in a 1000 ml volumetric flask and mix Dilute to 1 L with deionized water Mix thoroughly Prepare on an annual basis or more often as needed 0 01N Sulfuric Acid Mix 10 ml of 1N sulfuric acid with deionized water and dilute to 1 L Store on lab shelf Prepare on an annual basis or more often as needed This solution is used to adjust the pH of the water sample to between 7 and 10 pH units 0 01N Sodium Hydroxide Cautiously dissolve 0 4 g sodium hydroxide pellets in approximately 500 ml of deionized water and dilute to 1 L with deionized water Store in a polyethylene bottle with a polyethylene screw cap on the lab shelf This solution is used to adjust the pH of the water sample to between 7 and 10 pH units Prepare on a semiannual basis or more often as needed Sodium Chloride NaCl Standard 0 0141N Dissolve 824 0 mg NaCl dried at 140 C in distilled water and dilute to 1000 mL Chloride 500 mg l Potassium chromate indicator solution Dissolve 50 g K2CrO4 in a little distilled water Add AgNOS soluti
8. control Standard Operation Procedure Manual for Analysis of Drinking water quality Page 31 of 64 Measurement tab Select single wavelength and edit 510 in the Mean wave length box Select identifier sample and standard number In other select duplicate to achieve more accurate data and edit 3 to have every measurement repeated 3 times Calibration Curve Select Abs f Conc in the curve equation box As per principle of the phenanthroline method we will have straight line equation therefore select equation order 1 Select ppm or mg l in the concentration unit box Select zero interception In curve evaluation box select R2 to have correlation coefficient Select concentration method in the calibration method menu Instrument in this tab we can interchange D2 lam and W lamp but T60 V spectrophotometer has only W lamp therefore we have to change nothing Accessories Select 8 cell holder and click cell number of cell type icon to select the active cell position e Quantitative measurement window It has 4 parts standards measurement table unknown sample measurement table calibration curve and performance Total Iron Determination and Calibration Curve Sample preparation e Take 20 ml iron sample add 4 ml buffer and 0 8 ml phenanthroline solution and take absorption after 15 minutes reaction time at 510 nm wavelength as described above pH of the sample should be 2 9 3 5 e After taking reading of all standards check the curve
9. sample and the measure display screen will indicate any fluctuation in the sample pH Standard Operation Procedure Manual for Analysis of Drinking water quality Page 14 of 64 e After noting pH value remove the electrode from the sample and rinse it with water distilled de ionized and place the electrode in potassium chloride solution In case sample solution is viscous then wipe the electrode with the help water de ionized or distilled and tissue paper RFERENCES p 2052 USP25 Manual pH meter CyberScan 6000 RELATED DOCUMENTS Procedure for Calibration program RELATED RECORD A Daily Calibration Record of pH meter ANNEXURE Nil Standard Operation Procedure Manual for Analysis of Drinking water quality Page 15 of 64 Standard Operation Procedure for detection of Turbidity in water Procedure for Operation and Calibration of TN100 Turbidity meter for Turbidity Examination PURPOSE To establish a procedure for operation and calibration of TN 100 turbidity meter for turbidity determination of water SCOPE This method is applicable to drinking surface saline and ground water in the range of turbidity from O to 1000 Nephelometric Turbidity Units NTU The working range of this method is 1 to 1000 NTU PRINCIPLE Standard Methods 2130 B The Nephelometric Method is based on a comparison of the intensity of light scattered by a sample under defined conditions with the intensity of light
10. 13 HEALTH AND SAFETY REOR RON in 13 CAUTIONS LI rrr 13 A Dn M M d 14 PROCEDURE TC 14 CALIBRATION PROCEDURE Auto Buffer Recognition aa 14 OPERATIONAL PROCEDURE ara dai 14 Standard Operation Procedure for detection of Turbidity in water sss 16 PURPOSE SS SSS ss A ens uie E RE M M Up 16 A usun usa 16 PRINCIPLES e 16 RESPONSIBILIDYS ua a aaa uk usa Suyana aaa Gawa unto an 16 HEALTH AND SAFE A n Sean ad a acted aaa 16 CATIA Md n nas 17 DILUTION nn aka m ua 17 PROCEDURE obesse oa trc son ec a iaa 18 Sample preparations x csccscacece 18 Calibration procedutre cient eric tea cod ees a de deu nets 18 OPERATIONAL PROCEDURE ti 19 Standard Operation Procedure for detection of Electical Conductivity in water 20 PURPOSE dort A tuat A eg ts ees ee eee MER EU 20 SCOPE Mc PH 20 PRINCIPLES t n S outs a tonus aku MR tr Sn RICE De end ee 20 RESPONSIBILTY ceiien a atate dedi ted b Catan p tbe Qu Fa un terested 20 HEALTH A D SAFETY unus saa an aqa a it n Ind ett pas UE 20 A A 20 PROCEDURE ate 21 CALIBRATION PROCEDURE Automatic Conductivity Calibration
11. 20 Ed 1998 and is applicable to ground drinking surface and saline waters domestic and industrial wastes The method is suitable for use in relatively clear waters when 0 15 to 10 mg Cl are present in the portion titrated RESPONSIBILITY WAL Analyst Operation and Calibration WAL Manager Receiving sample amp log book entry and Implementation of this SOP WQ Consultant QC OAWQL Analyst Operation and Calibration SUMMARY OF M ETHOD Ina neutral or slightly alkaline solution potassium chromate can indicate the end point of the silver nitrate titration of chloride Silver chloride is precipitated quantitatively before red silver chromate is formed HEALTH AND SAFETY WASTE HANDLING Wear personal protective equipment PPE including lab coat safety glasses and gloves when performing chloride analysis After analysis discard analyzed samples down the drain Retain unused sample until the sample has been reviewed and reported INTERFERENCES Substances in amounts normally found in potable waters will not interfere Bromide iodide and cyanide register as equivalent chloride concentrations Sulfide thiosulfate and sulfite ions interfere but can be removed by treatment with hydrogen peroxide If sulfide sulfite or thiosulfate is known to be present add 0 5 ml H202 and stir for 1minute prior to titration Standard Operation Procedure Manual for Analysis of Drinking water quality Page 37 of 64
12. B mg CaCO3 equivalent to 1 00 mL EDTA titrant or B ml of standard Ca solution ml of EDTA titrant RFERENCES e p 2 37 39 APHA 20 Ed ANNEXURE Nil Standard Operation Procedure Manual for Analysis of Drinking water quality Page 43 of 64 Standard Operation Procedure for detection of Nitrate in water Standard Operation Procedure for Nitarte N Examination in Water by lon Selective Electrode Method PURPOSE To establish a procedure for determination of nitrate N in water by ion selective electrode method SCOPE This method may be used for measuring solubilized nitrate in drinking water natural surface water and groundwater domestic and industrial wastewater PRINCIPLE The NO3 ion electrode is a selective sensor that develops a potential across a thin porous inert membrane that holds in place a water immiscible liquid ion exchanger The electrode responds to NO3 ion activity between about 10 5 and 10 1 M 0 14 to 1400 mg NO3 N L The lower limit of detection is determined by the small but finite solubility of the liquid ion exchanger RESPONSIBILITY WAL Analyst Operation and Calibration WAL Manager Receiving sample amp log book entry and Implementation of this SOP WQ Consultant QC OA METHOD SUM MARY Solubilized nitrate is determined potentiometrically using a nitrate ion selective electrode ISE in conjunction with a double junction reference electrode and a pH met
13. Conductivity in water Procedure for Operation and Calibration of CON 510 Conductivity meter for Electrical Conductivity Examination PURPOSE To establish a procedure for operation and calibration of CON 510 Conductivity meter for electrical conductivity determination of water SCOPE This procedure is applicable for operation and calibration of CON 510 Conductivity meter only PRINCIPLE The measurement of electrical conductivity EC in water results from ions in solution from dissolved salts Measurement of conductivity gives an estimate of the concentration of these dissolved salts Conductivity of an aqueous solution is the measure of its ability to carry an electric current by means of ionic motion This ability depends on the concentration mobility and valence ions present in solution and on the temperature of measurement RESPONSIBILITY WAL Analyst Operation and Calibration WQL Manager Receiving sample log book entry and Implementation of this SOP WQ Consultant QC QA HEALTH AND SAFETY Personal protective equipment including safety glasses and lab coats should be used CAUTIONS Protect the conductivity standard solution from air because of the absorption of atmospheric CO which may change the conductivity n Always rinse the probe with de ionized or distilled water before use and after each sample to remove any impurities adhering to the probe body Shake or air dry To avoid conta
14. E 53 Minimum detectable concentration 53 A aus 53 AGLI cp M M Ma 54 Op ratiolil e 54 Shutdown teet E ERI 55 Operating precautiOris c uu uu ee e ee a apa ete ains andes ei eae dess ocio rod Free EFES 55 Standard Operation Procedure for detection of Sulfate in water 56 PURPOSE 56 SCOPE Rm 56 RESPONSIBILITY e 56 PRINCIPeLER uuu 56 HEALTH AND SAEETY ll 56 CAUTION tam 56 INTERFERENCES S cc T m 57 nig gc M 57 REAGENTS AND E 1 aaikhyqaaaawaspasaqaypuwaqyaspuqwyankusqayaaqyakuwaqusaqqayausaquyqaqqyapayapuspaqqupusquswha 57 dieleznjicm hak ahua 57 Spectr photormetric setup c m 57 Turbidity meter set p x e tice tiec esee ai 58 Sulfate Determination and Calibration Curve 59 Standard Operation Procedure for detection of Cac
15. Loading Bung Devices e Take one hydrogen sulfide removal filter and insert into the bottom end of the bung e Take red filter slid and put one filter paper from red labeled pot ensuring the filter paper is evenly covering the hole and close the slid holder e Get bung and insert the red filter slide into the top slot e Take black arsenic filter slid put one filter paper from black labeled pot and insert black filter slid into lower slot Sample Preparation e Take flask and fill to the 50 ml mark with sample water e Take A1 powder sachet and pour into the flask e Drop A2 tablet carefully into the flask Reaction will start e Immediately push down the bung device firmly into the flask e Wait for 20 minutes After reaction time remove the black filer slid and proceed to next step Arsenic M easurement e Record corresponding color match from color chart to obtain result in ppb ug l e f test result reads above 500 ppb dilute the water sample with distilled water and repeat the process from 8 1 8 3 RFERENCES e Wag WE10500 arsenator operation manual ANNEXURE Nil Standard Operation Procedure Manual for Analysis of Drinking water quality Page 27 of 64 Standard Operation Procedure for detection of Residual Chlorine in water Procedure for Examination of Residual Chlorine in Water by Pool Tester PURPOSE To establish a standard operation procedure for residual chlorine determination in water SCOPE This met
16. applicable for operation and calibration of T60 V spectrophotometer only for total iron examination RESPONSIBILITY WAL Analyst Operation and Calibration WQL Manager Receiving sample amp log book entry and Implementation of this SOP WQ Consultant QC OA Principle The amount of iron present in a sample is determined by first reacting the iron with 1 10 phenanthroline to form a colored complex and then measuring the amount of light absorbed by this complex Beer s law can then be used to determine the concentration relative to absorption A ebc HEALTH AND SAFETY Personal protective equipment including safety glasses and lab coats should be used CAUTIONS 1 Protect the iron standard solution from air Always rinse cuvette with distilled water before use and after each sample to remove any impurities adhering to the cuvette body Shake or air dry To avoid contamination or dilution of sample rinse cuvette with a small volume of your sample solution Do not wipe the glass cuvette with any coarse material Standard Operation Procedure Manual for Analysis of Drinking water quality Page 30 of 64 INTERFERENCES Among the interfering substances are strong oxidizing agents nitrite phosphate and chromium in concentration exceeding 10 times that of iron cobalt and copper excess of 5 mg L and Nickel in excess of 2 mg L precipitate phenanthroline APPARATUS Spectrophotometer for use
17. nimiae e 26 RESPONSIBIUITY u S n n um n Su testet Riu eem 26 HEALTH pEyildhiee m 26 CAUTIONS n an n as u SD a Saa Sa a a naa u au at 26 GALIBRATION n tu u u oa Mum Du 27 Standard Arsenic solution preparation a 27 PROGEDURE 5 e RR LM mee 27 Loading UDnABAgerupc M 27 ll eet iO emendi esta E D M UN t IUE 27 Arsenic Measurement virer eR Ee Aeris ricas 27 Standard Operation Procedure for detection of Residual Chlorine in water 0 00 0 28 PURPOSE tera o a u u 28 xjeoril 28 adzscc OM 28 PRINCIPLES ELEM 28 RESPONSIBIL Vico A Butikussqa squa p yaq a E humb E R 28 a BP pvc 28 eec A ii 29 PROCEDURES cio A a on 29 Standard Operation Procedure for detection of Total Iron in water sss 30 PURPOSE a 30 xjeoplm 30 RESPONSIBLE PP 30 Jes 30 us inp pEvVdpd m 30 CAUTIONSu Ia M 30 INTER
18. not light within approximately 20 seconds release the switch and open the fuel valve one turn Allow the gas to disperse before continuing Press the ignition switch for a further 20 seconds This process may be repeated until successful ignition occurs 4 Set the filter select control to the desired position 5 Aspirate deionised water and set the readout to zero by adjusting the blank control 6 Aspirate a standard solution of slightly higher concentration than expected in the samples to be tested Adjust the fine and coarse control until a positive reading is obtained This is a nominal value to be used in optimising flame conditions 7 Adjust the fuel valve in a clockwise direction until a peak reading is obtained Standard Operation Procedure Manual for Analysis of Drinking water quality Page 54 of 64 8 For optimum performance the instrument should be allowed 15 minutes to warm up During this warm up period a blank deionised water sample should be aspirated Shutdown 1 Aspirate deionised water for at least ten minutes 2 If the shutdown is short term i e the instrument is to be used again the same day it is adequate to remove electrical power from the unit by pressing the power switch This will safely extinguish the flame 3 If the shutdown is longer term or if the laboratory is likely to be left unattended during the shutdown then the fuel supply should be turned off at source wait for the flame indicator to extingui
19. of actual Fluoride concentration Substance Conc mg L Type of error Alkalinity 5000 AP 01 Cr 7000 Fe 10 SO 200 Distillation is necessary for samples containing high concentration of dissolved solids The dissolved solids interfere with the fluoride analysis Alkalinity aluminum iron and sulfates have negative effect on the results while chloride and phosphate has positive effect APPARATUS Spectrophotometer for use at 570nm providing a light path of 1cm Acid washed glassware use conc HCI for cleaning all the glassware rinse with distilled water before use Standard Operation Procedure Manual for Analysis of Drinking water quality Page 34 of 64 REAGENTS AND SOLUTIONS Stock fluoride solution Dissolve 221 0mg anhydrous sodium fluoride NaF in distilled water and dilute to 1000 mL 100 mg l fluoride Standard fluoride solution Dilute 100 mL stock fluoride solution to 1000 mL with distilled water 10 mg l of fluoride Similarly prepare 0 5 1 0 1 5 and 2 0 mg l of F SPADNS solution Dissolve 958mg SPADNS sodium 2 parasulphophenylazo 1 8 dihydroxy 3 6 naphthalenedisulphonate in distilled water and dilute to 500 mL protect from light stable for 1 year Zirconyl acid reagent Dissolve 133mg zirconyl chloride octahydrate ZrOCI2 8H20 in about 25 mL distilled water add 350 mL conc HCI and dilute to 500 ml Mixed acid zirconyl
20. peak reading is obtained 8 For optimum performance the instrument should be allowed 15 minutes to warm up During this warm up period a blank deionised water sample should be aspirated Shutdown 1 Aspirate deionised water for at least ten minutes 2 If the shutdown is short term i e the instrument is to be used again the same day it is adequate to remove electrical power from the unit by pressing the power switch This will safely extinguish the flame 3 If the shutdown is longer term or if the laboratory is likely to be left unattended during the shutdown then the fuel supply should be turned off at source wait for the flame indicator to extinguish and then turn off the power This ensures that there is no gas left in the tubing to the unit Standard Operation Procedure Manual for Analysis of Drinking water quality Page 51 of 64 Operating precautions 1 The fuel gases used in the flame photometers are inflammable and therefore potentially hazardous Cylinders of fuel gas should always be stored and used in appropriate and safe ways 2 It is possible that a small quantity of fuel will escape from the instrument during the ignition sequence The amount of fuel is harmless although may smell slightly If the smell of fuel gas persists the instrument should be immediately shut down and locate source of the leakage in the hose joints 3 Do not leave the instrument running unattended while the flame is alight 4 The top of the in
21. scattered by a standard reference suspension under the same conditions The nephelometric instrument light source illuminates the sample and the intensity of the scattered light is measured at approximate right angles 90 30 to the path of the incident light for samples The higher the intensity of scattered light the higher the turbidity RESPONSIBILITY WAL Analyst Operation and Calibration WAL Manager Receiving sample amp log book entry and Implementation of this SOP WQ Consultant QC QA HEALTH AND SAFETY Wear proper protective equipment which includes safety glasses protective gloves and a lab coat when working in the active laboratory area Work under a fume hood and or in an adequate ventilated area to avoid inhaling vapors dust etc Standard Operation Procedure Manual for Analysis of Drinking water quality Page 16 of 64 Formazin polymer suspensions may be used as reference standards Formazin contains hydrazine sulfate which is a known carcinogen Take care in handling and disposal to avoid inhalation skin contact and ingestion After analysis discard analyzed samples down the drain Retain the unused sample until the sample has been reviewed and reported CAUTIONS NEVER pour liquid directly into the sample well of the instrument Always use a vial The instrument will only accurately measure the turbidity of a sample when vials sealed with the black caps are used The black cap serves as
22. FERENCES essentie cT 31 APPARATUS ii A r ated blo aan Recess Pie EE E aiii 31 REAGENTS AND SOLUTIONS 2 tuy a eaaa aaaea euet restes aaa EE De Pul EE E Eae Et 31 Mesue 31 Spectrophotomietric setup torte A rae ete RE ree nr nua rnc de escapade eren ache dudes 31 Total Iron Determination and Calibration Curve ll tete 32 Standard Operation Procedure Manual for Analysis of Drinking water quality Page 2 of 64 Standard Operation Procedure for detection of Fluoride in water J 33 PURPOSE SK ELTE 33 SCOPE c M N 33 Nasen bisce PR 33 PUMIVG MOS e EO DECEDERE OS OO D E EEE E I UE 33 HEALTH AND SAFETY mersinin 33 Dig kl D 34 bdiidddidel HH H 34 APPARATU BY 34 REAGENTS AND SOLUTIONS cernicus u cease au pon zu a A Qaqata q kashasqa awki qhana kaq 35 eledalc RMM 35 Spectrophotometric Setup PARRA 35 Total Iron Determination and Calibration Curve Ple acaicicnicicninicicninioninononn eerte 36 Standard Operation Procedure for detection of Chloride in water
23. Islamic Republic 4 4 N a Min istry of Rura Rehab WW v gt iral V ater Supply Sanitation ar IIT ion Prog Feberuary 201 Prepared by Ru WATSIP MRRD Water quality Lab Staff and Abdus Saboor WQ Consultant m unicef ts Table of Contents Introduction of RUWATSIP M RRD Water Quality Laboratory sss 6 Standard Operation Procedure for detection of Bacteriological parameters 7 Uis Pur RENI RTT S 7 A O e 7 D GTIAILIONSS sce coc xu Qu susu iaa olas 7 PRINGIPEE S OCTTCT e 8 RESPONSIBILITY ass at uu Sasa ibus acetate bua ctu DbD B due inen DER D ep adi sayis 8 HEALTH AND SAFED tddi ente Dr 8 IRI TERFEREDICES ac aia 9 MEDIA PREPARA ION ici 9 PROCEDUR Easier a a a A A A 10 A EEE A ME AE ce Ee akawa 10 Total Coliform Presumptive Test MPN Method a 10 Coliform Confirmation Test anu esses nnne een ennnnnnn aeaaaee a aE Ea aE nass ss ase asa agas 11 Escherichia Coli E Colias u 52 n nSn os nir A AO EORR A AANE EOE ia 11 Standard Operation Procedure for detection of pH in water 13 PURPOSE S y S D u n A aaa A 13 SCORE Sas e ES Po aS na n A 13 RESPONSIBILTY Suq u as ahua a AAA AAA 13 DEFINITIONS Senra u ia S skua ia
24. SE To establish a procedure for operation and calibration of T60 V spectrophotometer for sulfate determination in water SCOPE This procedure is applicable for operation and calibration of T60 V spectrophotometer only for sulfate examination RESPONSIBILITY WAL Analyst Operation and Calibration WQL Manager Receiving sample amp log book entry and Implementation of this SOP PRINCIPLE This method is used for the determination of sulphate ions Minimum detectable concentration is approximately 1 mg SO4 L Sulphate ion is precipitated in an acetic acid medium with Barium chloride BaCl2 so as to form Barium sulphate BaSO4 crystals of uniform size Light absorbance of the BaSO4 suspension is measured by a photometer or the scattering of light by Nephelometer HEALTH AND SAFETY Personal protective equipment including safety glasses and lab coats should be used CAUTIONS 1 Protect the sulfate standard solution from air Always rinse cuvette with distilled water before use and after each sample to remove any impurities adhering to the cuvette body Shake or air dry To avoid contamination or dilution of sample rinse cuvette with a small volume of your sample solution Do not wipe the glass cuvette with any coarse material Standard Operation Procedure Manual for Analysis of Drinking water quality Page 56 of 64 INTERFERENCES Color or suspended matter in large amounts will interfere S
25. SPADNS reagent Mix equal volumes of SPADNS solution and zirconyl acid reagent stable for 2 years Reference solution Add 10 mL SPADNS solution to 100 mL distilled water Dilute 7 mL conc HCI to 10 mL with distilled water and add to SPADNS solution stable for 1 year Set the instrument to zero with this solution PROCEDURE Spectrophotometric setup e Switch on the instrument and wait for initialization process e Select Quantitation tab in work place e Select parameter setting under measure menu e There are 5 tabs Measurement Calibration curve Instrument Accessories and Quality control Measurement tab Select single wavelength and edit 570 in the Mean wave length box Select identifier sample and standard number In other select duplicate to achieve more accurate data and edit 3 to have every measurement repeated 3 times Calibration Curve Select Abs f Conc in the curve equation box As per principle of the phenanthroline method we will have straight line equation therefore select equation order 1 Select ppm or mg l in the concentration unit box Select zero interception In curve evaluation box select R2 to have correlation coefficient Select concentration method in the calibration method menu Standard Operation Procedure Manual for Analysis of Drinking water quality Page 35 of 64 Instrument in this tab we can interchange D2 lam and W lamp but T60 V spectrophotometer has only W lamp therefore we have to change nothing
26. TE HANDLING Wear personal protective equipment PPE including lab coat safety glasses and gloves when performing analysis After analysis discard analyzed samples down the drain Retain unused sample until the sample has been reviewed and reported Standard Operation Procedure Manual for Analysis of Drinking water quality Page 41 of 64 INTERFERENCES Some meal ions interfere by causing fading or indistinct end points or y stoichiometric consumption of EDTA Suspended or colloidal organic matter also may interfere with the end point TITRATION PRECAUTIONS Conduct titration at or near room temperature The color change becomes impractically slow at the sample approaching freezing temperature Indicator decomposition become problem in hot water Dilute sample with distilled water to reduce CaCO3 concentration REAGENTS AND SOLUTIONS Buffer solution Dissolve 16 9g NHACI in 143 mL conc NH40H Add 1 25g magnesium salt of ethylenediaminetetraacetate EDTA and dilute to 250 mL with distilled water Store in a plastic bottle stoppered tightly for no longer than one month Alternative buffer Dissolve 1 179 g disodium salt of dthylenediaminetetraacetic acid dihydrate and 780 mg magnesium sulfate MgSO4 7H20 or 644 mg magnesium chloride MgCl2 6H20 in 50 mL distilled water Add this solution to 16 9 g NHACI and 143 mL conc ammonium hydroxide with mixing and dilute to 250 mL with distilled water Complexing agent Magnesium s
27. a few drops of methyl red indicator and adjust to the intermediate orange colour by adding 3N NH40H or 1 1 HCl as required Transfer quantitatively and dilute to 1000 mL with distilled water 1 mL Img CaCO3 Sodium hydroxide NaOH 1N Dissolve 4 0 gram of NaOH pellets in 100 ml of water Murexide ammonium purpurate indicator Prepare by mixing 200 mg murexide with 100 g solid NaCl and grinding the mixture to 40 to 50 mesh Titrate immediately after adding indicator because it is unstable under alkaline conditions Facilitate end point recognition by preparing a color comparison blank containing 2 0 mL NaOH solution 0 2 g solid indicator mixture and sufficient standard EDTA titrant 0 05 to 0 10 mL to produce an Unchanging color Standard Operation Procedure Manual for Analysis of Drinking water quality Page 61 of 64 PROCEDURE Take 10 mL sample Add 10 ml distilled water Add 0 4 mL 1M NoOH to give a pH of 12 0 to 13 0 Add 0 04 g of murexide indicator Because of the high pH used in this procedure titrate immediately after adding alkali and indicator Titrate with 0 01M EDTA titrant to change in colour CaL A X B X 400 8 cias sample CALCULATION A x B x 1000 Calcium hardness as mg CaCO L mL sample Where A mL titrant used EDTA B Factor mg CaCO3 equivalent to 1 00 mL EDTA titrant at the calcium indicator end point RFERENCES e p 3 64 65 APHA 20 Ed ANNEXURE Nil Standard Operat
28. alt of 1 2 cyclohexanediaminetetraacetic acid Add 250mg per 100 mL sample only if interfering ions are present and sharp end point is not obtained Indicator Dissolve 0 1 g Calmagite in 100 ml distilled water Standard EDTA titrant 0 01M Weigh 3 723g di sodium salt of EDTA dihydrate dissolve in distilled water and dilute to 1000 mL Store in polyethylene bottle Standard Calcium Solution Weigh 1 000g anhydrous CaCO3 in a 500 mL flask Add 1 1 HCI slowly through a funnel till all CaCO3 is dissolved Add 200 mL distilled water and boil for a few minutes to expel CO2 Cool and add a few drops of methyl red indicator and adjust to the intermediate orange colour by adding 3N NH4OH or 1 1 HCI as required Transfer quantitatively and dilute to 1000 mL with distilled water 1 mL 1mg CaCO3 Standard Operation Procedure Manual for Analysis of Drinking water quality Page 42 of 64 PROCEDURE Dilute 25 mL sample to 50 mL with distilled water Add 1 to 2 mL buffer to give a pH of 10 0 to 10 1 Add 1 to 2 drops of indicator solution and titrate with EDTA titrant to change in colour from reddish tinge to blue Select a sample volume that requires less then 15 mL EDTA titrant and complete titration within 5 min after buffer addition Standardize the EDTA titrant against standard calcium solution using the above procedure CALCULATION Total Hardness EDTA as mg CaCO3 L A x B x 1000 ml of sample where A mL EDTA titrated for sample
29. and R2 value R2 value must be gt 0 98 e Once calibration cure is produced with satisfactory R2 value click in the unknown sample table and prepare the unknown sample as described in section10 2 1 RFERENCES e p 3 76 78 APHA 20 Ed e UVWIN 5 0 instruction manual ANNEXURE Nil Standard Operation Procedure Manual for Analysis of Drinking water quality Page 32 of 64 Standard Operation Procedure for detection of Fluoride in water Procedure for Operation and Calibration of T60 V Spectrophotometer for Fluoride Determination by SPANDS Method PURPOSE To establish a procedure for operation and calibration of T60 V spectrophotometer for fluoride examination in water by SPANDS method SCOPE This procedure is applicable for operation and calibration of T60 V spectrophotometer for fluoride examination only This method is applicable to the measurement of fluoride in drinking surface and saline waters domestic and industrial wastes The method covers the range from 0 1 to about 1 4 mg L F RESPONSIBILITY WAL Analyst Operation and Calibration WQL Manager Receiving sample amp log book entry and Implementation of this SOP WQ Consultant QC QA Principle This method relies on the fact that when fluoride reacts with certain zirconium dyes a colorless complex anion and a dye are formed The complex which is proportional to the fluoride concentration tends to bleach the dye which therefore bec
30. ap and gently inverting it several times Discard the used sample and repeat the rinsing procedure two more times Fill the rinsed vial with the remaining portion approximately 10 ml of the grab sample up to the mark indicated in the vial Cap the vial with the supplied black screw cap Wipe the vial with the soft lint free cloth supplied Ensure that the outside of the vial is dry clean and free from smudges Wipe with a soft cloth to obtain an even distribution over the entire vial s surface Calibration procedure Place TN 100 T 100 turbidity meter on a flat and level surface Insert the CAL 1 standard 800 NTU into the sample well aligning the mark on the vial with the mark on the meter Press down vial until it snaps fully into the instrument Cover the vial using the light shield cap Press ON OFF key to switch the on the meter The meter goes to measurement mode after the power up sequence Select the calibration function of the instrument by pressing the CAL key once The CAL annunciator blinks momentarily and the meter prompt for the first calibration standard CAL 1 800 NTU Press READ ENTER key The CAL 1 800 NTU annunciator blinks for about 12 seconds while the instrument performs calibration of CAL 1 point When the instrument has completed calibration for this point it prompts you to insert the next calibration standard into the sample well CAL 2 100 NTU Repeat the calibration for CAL 2 CAL 3 amp CAL 4 cal
31. at 510nm providing a light path of 1cm or longer Acid washed glassware use conc HCI for cleaning all the glassware rinse with distilled water before use REAGENTS AND SOLUTIONS Ammonium acetate buffer solution Dissolve 250g NH4C2H302 in 150 mL water add 700 mL glacial acetic acid Since ammonium acetate may contain a significant amount of iron prepare new reference standards with each buffer preparation Phenanthroline solution dissolve 100mg 1 10 Phenanthroline monohydrate C12H8N2 H20 in 100 mL water by stirring and heating to 80 C without boiling discard if darkens or add 2 drops conc HCI to avoid heating Stock iron solution 200 mg L slowly add 20 mL conc H2SO4 to 50 mL water and dissolve 1 404g ferrous ammonium sulphate Fe NH4 2 SO4 2 6H20 add 0 1N KMnO4 dropwise until a faint pink colour persists dilute to 1 L with water and mix Use stock solution for further standards iron solution preparation using dilution formula C1V1 C2V2 C1 concentration of stock C2 concentration of required dilution standard and V1 volume of stock solution V2 volume of the dilution standard Prepare iron standards of 0 1 0 2 0 3 0 4 and 0 5 mg l concentration PROCEDURE Spectrophotometric setup e Switch on the instrument and wait for initialization process e Select Quantitation tab in work place e Select parameter setting under measure menu e There are 5 tabs Measurement Calibration curve Instrument Accessories and Quality
32. both seal and a light shield Air or other trapped gases should be removed before measurement DILUTION This dilution procedure is necessary only when your turbidity measurement is above 1000 NTU To measure the turbidity above 1000 NTU dilute the sample with turbidity free water Turbidity free water can be obtained by filtering deionized water through a lt 0 2um filter membrane with precision sized pores Measure the volume of the sample before dilution and record the value in ml Vs Take a known volume Vd of dilution water and add it to the sample Pour 10 ml of the diluted sample in a clean vial and measure the turbidity of the diluted sample Record this value in NTU Td Calculate the true turbidity T of the original sample in NTU using the following formula T Td Vs Vd Vs Example Dilute 20 ml of the original sample whose turbidity is above 1000NTU with 50 ml of dilution water Measure the turbidity of the diluted sample Ff the reading is 300 NTU the turbidity of the original sample is 1050 NTU In this case Td 300NTU Vs 20ml Vd 50ml so T 300 20450 20 300 70 20 21000 20 1050 Standard Operation Procedure Manual for Analysis of Drinking water quality Page 17 of 64 PROCEDURE Sample preparation Obtain a clean and dry sample vial Take care to handle the sample vial by the top Rinse the vial with approximately 10 ml of the sample water capping the vial with the black screw c
33. bration Make sure the electrode is properly connected Turn on the meter The ATC indicator will appear at the right hand side of the LCD to indicate that the temperature sensor is in good working condition If the ATC indicator does not light up see SETUP sub menu P3 3 to switch it on Press MODE key to select either conductivity or TDS mode Press CAL MEAS to enter either Conductivity or TDS calibration mode The CAL indicator appears above upper display While you are in conductivity or TDS calibration mode press MODE to enter into Temperature calibration mode The upper display show the current temperature reading and the lower display shows the factory default temperature value Standard Operation Procedure Manual for Analysis of Drinking water quality Page 21 of 64 Dip the ATC electrode into a solution of known temperature i e a constant temperature bath Allow about 3 5 minutes for the built in temperature sensor to stabilize its measured reading Adjust using the MI or MR key to set to the correct temperature value i e the temperature of the bath in increments of 0 1 C Maximum allowable offset temperature value is 5 0 C Once you have selected the correct temperature press ENTER key To abort or exit this calibration mode without confirming of the temperature calibration value DO NOT press ENTER key Press CA MEAS key instead and the meter automatically reverts back to the measurement mode OPERATIONAL PROCEDURE P
34. centration levels Standards should be stored in sealed plastic vessels and in high concentrations e g as a stock 1000ppm solution and dilutions prepared as required The long term storage of low concentration standards is not recommended due to degradation of ionic species Operation 1 Ensure that the drain trap has solution in it and that no air locks are present If necessary purge by adding deionised water and allowing the surplus to run away 2 Turn on the fuel supply at source i e cylinder and then switch on the photometer 3 Press the ignition switch and hold down Watch the flame indicator in the display window When this indicator is illuminated the flame is a light and the ignition switch can be released If the flame indicator does not light within approximately 20 seconds release the switch and open the fuel valve one turn Allow the gas to disperse before continuing Press the ignition switch for a further 20 seconds This process may be repeated until successful ignition occurs 4 Set the filter select control to the desired position 5 Aspirate deionised water and set the readout to zero by adjusting the blank control 6 Aspirate a standard solution of slightly higher concentration than expected in the samples to be tested Adjust the fine and coarse control until a positive reading is obtained This is a nominal value to be used in optimising flame conditions 7 Adjust the fuel valve in a clockwise direction until a
35. coli strains are harmless but some can cause food poisoning in humans Of the several types of bacteria in the total colifom group E coli does not typically reproduce in soil and water environments Their ability to survive for brief periods outside the body makes them an ideal indicator organism to test environmental samples for fecal contamination Colony A group of bacteria growing on a supporting surface The colony is considered to be the result of the growth and reproduction of a single cell Disinfection To destroy most but not necessarily all of the harmful or objectionable microorganisms by means of chemicals heat ultraviolet light etc Fermentation The process by which bacteria convert organic matter into carbon dioxide and water Fermentation Tube A container designed to allow easy identification of gas production Standard Operation Procedure Manual for Analysis of Drinking water quality Page 7 of 64 Fecal Coliform A subclass of the coliform bacteria which originate almost exclusively in the intestinal tract of warm blooded animals Inoculation The process by which a sample or seed culture is introduced into a system MPN The most probable number MPN of coliform or fecal coliform bacteria per unit volume of a sample It is expressed as the number of organisms which are most likely to have produced the laboratory results noted in a particular test Medium Media A substance or substances used to provide nutrients
36. concentration of blank from apparent sulphate concentration as determined above because the calibration curve is not a straight line this is not equivalent to subtracting blank absorbance from sample absorbance RFERENCES p 311 312 APHA 20 Ed e UVWIN 5 0 instruction manual Standard Operation Procedure Manual for Analysis of Drinking water quality Page 59 of 64 Standard Operation Procedure for detection of Cacium in water Procedure for Operation and Calibration of Calcium determination in Water PURPOSE To establish a procedure for Calcium determination in water SCOPE AND APPLICATION This method is based on Standard Methods 3500 Ca B EDTA titrimetric method and is applicable to ground drinking surface and saline waters domestic and industrial wastes RESPONSIBILITY WAL Analyst Operation and Calibration WQL Manager Receiving sample log book entry and Implementation of this SOP WQ Consultant QC QA PRINCIPLE SUMMARY OF METHOD When EDTA ethylene di amine tetra acetic acid or its salts is added to water containing both calcium and magnesium it combines first with the calcium Calcium can be determined directly with EDTA when the pH is made sufficiently high that the magnesium is largely precipitated as the hydroxide and an indicator is used that combines with calcium only Several indicators give a color change when all of the calcium has been complexed by the EDTA at a pH of 12 t
37. d in high quality paper or placed in containers prior to hot air sterilization All glassware except those in metal containers should be sterilized for a minimum of 60 minutes at 170 C Sterilization of glassware in metal containers should require a minimum of 2 hours Hot air sterilization should not be used for glassware containing media or other liquids The caps or stoppers of glassware sterilized in a hot air sterilizer should be partially loosened to prevent pressure buildup during sterilization Autoclave Sample bottles dilution water culture media and glassware may be sterilized by autoclaving at 121 C for 15 minutes The autoclaving process uses steam and pressure 15 psi for sterilization Care should be taken that the pressure has returned to zero prior to opening the autoclave to prevent injuries or loss of sterilized liquids The caps or stoppers of glassware sterilized in an autoclave or pressure cooker should be partially loosened to prevent pressure buildup inside the containers Coliform Presumptive Test MPN Method Homogenize water sample by gentle shaking Take 15 sterilized test tubes and divide into three sets each set of 5 To each test tube of 1 set add 10 ml of double strength MacConkey broth Whereas to gne and 3 set of tubes add 5 of single strength MacConkey broth To all set of tubes insert inverted Durham tubes cap each tightly and sterilize in autoclave After sterilization the tube are brought to room
38. d of water in which color is due to naturally occurring materials It is not applicable to most highly colored industrial wastewaters INTERFERENCE Even a slight turbidity causes the apparent color to be noticeably higher than the true color therefore centrifuge for 1 h unless it has been demonstrated that centrifugation under other conditions accomplishes satisfactory turbidity removal The color value of water is extremely pH dependent and invariably increases as the pH of the water is raised APPARATUS Nessler tubes matched 50 mL tall form pH meter for determining sample pH PREPARATION OF STANDARDS Dissolve 1 246 g potassium chloroplatinate K2PtCl6 equivalent to 500 mg metallic Pt and 1 00 g crystallized cobaltous chloride CoCI2x6H20 equivalent to about 250 mg metallic Co in distilled water with 100 mL conc HCI and dilute to 1000 mL with distilled water This stock standard has a color of 500 units Prepare standards having colors of 5 10 15 20 25 30 35 40 45 50 60 and 70 by diluting 0 5 1 0 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 6 0 and 7 0 mL stock color standard with distilled water to 50 mL in nessler tubes Protect these standards against evaporation and contamination when not in use Standard Operation Procedure Manual for Analysis of Drinking water quality Page 24 of 64 PROCEDURE Pour sample in a Nessler tube up to 50 mL mark Similarly fill three to four tubes with colour sta
39. d wait for initialization process e Select Quantitation tab in work place e Select parameter setting under measure menu Standard Operation Procedure Manual for Analysis of Drinking water quality Page 57 of 64 There are 5 tabs Measurement Calibration curve Instrument Accessories and Quality control Measurement tab Select single wavelength and edit 420 in the Mean wave length box Select identifier sample and standard number In other select duplicate to achieve more accurate data and edit 3 to have every measurement repeated 3 times Calibration Curve Select Abs f Conc in the curve equation box As per principle of the phenanthroline method we will have straight line equation therefore select equation order 1 Select ppm or mg l in the concentration unit box Select zero interception In curve evaluation box select R2 to have correlation coefficient Select concentration method in the calibration method menu Instrument in this tab we can interchange D2 lam and W lamp but T60 V spectrophotometer has only W lamp therefore we have to change nothing Accessories Select 8 cell holder and click cell number of cell type icon to select the active cell position Quantitative measurement window It has 4 parts standards measurement table unknown sample measurement table calibration curve and performance Turbidity meter setup Place TN 100 T 100 turbidity meter on a flat and level surface Place the sample vial inside the sample w
40. dard Operation Procedure for detection of Nitrate in water 44 PURPOSE e 44 SEO PES M n 44 PRINCIPLE coincida E a R da don ide eas aa sheds suet papata iaa EE dme n 44 RESPONSIBILITY tdi E 44 METHOD SUMMARY u uuu E 44 HEALTH AND SAFETYILuu S sta ee pee torio aksa deaur eee Dodd dia dudtvusedetedseadedabsatuebidebcudasandedenvenceceveanecteess 45 iid imei MM 45 REAGEN TS ive c 45 PROCEDURE e 46 Preparation of Calibration Curv uuu u u uu 1 nnn enne nennt nsn nn nena anas nass ssa i ttai as sisse ases saga sanas ania 46 Measurement OT sample steiere L rrt A calce aa eo doe ne aree kasa assia deca gd iuba 46 Standard Operation Procedure for detection of Bicarbonate amp carbonate in Waer 47 PURPOSES re 47 Standard Operation Procedure Manual for Analysis of Drinking water quality Page 3 of 64 so dpi d Beiden ss 47 RESPONSIBILITY ERR 47 PRINCIPLE amp SUMMARY OF METHOD uuu aa aaa ste asas apas no rana o nnns senten as essersi sese nnne nennen nn 47 HEALTH AND SAFETY WASTE HANDLING eseeseeeeee eren enne enne nennnnnn conan nan nnnn nnns nennen nenne nasse ensis 47 INTERFERENCE L uQ yau
41. e concentration The better flame photometers can be used to determine sodium levels approximating 100ug L With proper modifications in techniques the range of sodium measurement can be extended to 10ug L or lower Principle Trace amounts of potassium can be determined in either a direct reading of internal standard type of flame photometer at a wavelength of 766 5 nm Because much of the information pertaining to sodium applies equally to the potassium determination carefully study the entire discussion dealing with the flame photometric determination of sodium before making a potassium determination Reagents To minimize potassium pickup store all solutions in plastic bottles Shake each container thoroughly to dissolve accumulated salts from walls before pouring Reagent water Use this water for preparing all reagents and calibration standards and as dilution water Stock potassium solution Dissolve 1 907g KCI dried at 1109C and dilute to 1000mL with Water 1000mg l of K Intermediate potassium solution Dilute 10mL stock potassium solution with water to 100mL 10 mg l K Use this solution to prepare calibration curve in potassium of 1 to 10 mg L Standard Operation Procedure Manual for Analysis of Drinking water quality Page 50 of 64 Storage of standards Store solutions away from direct sunlight in a cool place ideally at temperatures below 259C Glass containers should not be used for storage as they can affect the con
42. e of arsenic contents from 10 ppb to 500 ppb PRINCIPLE Water sample is treated with reagents provided with Wag WE10500 Arsenator for 20 minutes and the gas produced during reaction changes color of the strip placed in cap of reaction bottle The color change of strip is then visually compared with chart having arsenic ranges RESPONSIBILITY WAL Analyst Operation and Calibration WQL Manager Receiving sample amp log book entry and Implementation of this SOP WQ Consultant QC OA HEALTH AND SAFETY Wear proper protective equipment which includes safety glasses protective gloves and a lab coat when working in the active laboratory area Work under a fume hood and or in an adequate ventilated area to avoid inhaling vapors dust etc After analysis discard analyzed samples down the drain Retain the unused sample until the sample has been reviewed and reported CAUTIONS NEVER open the reaction flask during the reaction time Ensure tight fitting of tri filter arsenic trap bung Standard Operation Procedure Manual for Analysis of Drinking water quality Page 26 of 64 CALIBRATION Standard Arsenic solution preparation e Prepare arsenic standard of 10 ppb 50 ppb and 100 ppb by taking 1ml 5ml and 10ml from arsenic stock solution 1000 ppb into 100ml volumetric flask and fill up to mark with distilled water Check the arsenic 10ppb 50ppb and 100ppb standards as described in 8 0 PROCEDURE PROCEDURE
43. e with a slope of 57 3 mV decade at 25 C should result Recalibrate electrodes several times daily by checking potential reading of the 10 mg NO3 N standard and adjusting the calibration control until the reading plotted on the calibration curve is displayed again Measurement of sample Transfer 10 mL sample to a 50 mL beaker add 10 mL buffer solution and stir for about 1 min with a magnetic stirrer Measure standards and samples at about the same temperature Immerse electrode tips in sample and record potential reading when stable after about 1 min Read concentration from calibration curve RFERENCES APHA 20 Ed p 4 114 16 User Manual ISE Thermo scientific RELATED DOCUMENTS Procedure for Calibration program ANNEXURE Nil Standard Operation Procedure Manual for Analysis of Drinking water quality Page 46 of 64 Standard Operation Procedure for detection of Bicarbonate amp carbonate in waer Procedure for Operation and Calibration of Bicarbonate and Carbonate Determination in Water PURPOSE To establish a procedure for Bicarbonate determination in water SCOPE AND APPLICATION This method is based on Standard Methods 2320 B Titration method and is applicable to ground drinking surface and saline waters domestic and industrial wastes RESPONSIBILITY WAL Analyst Operation and Calibration WAL Manager Receiving sample log book entry and Implementation of this SOP WQ Cons
44. ell and align the vial s index mark with the meter s index mark Push the vial until it is fully snapped in Cover the vial with the light shield cap b Turn on the meter by pressing the ON OFF key After the power up sequence the meter goes to measurement mode and the display blinks Rd for about 10 times The measured reading appears in the display If necessary place the second sample vial into the sample well Remember to align the vial s mark with the meter s index mark Standard Operation Procedure Manual for Analysis of Drinking water quality Page 58 of 64 Press READ ENTER key The display blinks Rd for several times and measured reading appears e Repeat steps 2 through 9 for all other samples Sulfate Determination and Calibration Curve a Take suitable volume of sample and dilute to 100mL into a 250mL Erlenmeyer flask b Add 20mL buffer solution mix well C Keep the flask constantly stirred with the help of stirrer Add 1 spatula BaCl2 crystals with Stirring Continue stirring for 1 minute after addition of BaCl2 d Pour suspension into an absorption cell of photometer a measure turbidity at 5 0 5 min e To correct for sample colour and turbidity run a blank to which BaCl2 is not added Note If buffer solution A was used determine sulphate concentration directly from the calibration curve after subtracting sample absorbance before adding BaCl2 If buffer solution B was used subtract sulphate
45. ementing water quality program across Afghan communities will extend the strategy policy and of water quality in providing safe drinking water for Afghan people Standard Operation Procedure Manual for Analysis of Drinking water quality Page 6 of 64 Standard Operation Procedure for detection of Bacteriological parameters Standard Operation Procedure MPN Method for Total Coliform Fecal Coliform and Escherichia Coli Examination in Water IS 1622 1981 Reaff 2003 PURPOSE To establish a procedure for determination of Coliform and E Coli in water SCOPE This method is used to examine coliform and E Coli in drinking water natural surface water and groundwater domestic and industrial wastewater DEFINATIONS Broth A mixture of chemicals which will encourage the growth of a specific organism or group of organisms Kovac s Reagent It is used to detect the presence of indole Used in the identification of bacteria Buffer A chemical which has the ability or capacity to neutralize acids or bases Coliform A group of bacteria which can be used as an indicator of pollution A major portion of this group live in the intestinal tract of warm blooded animals including human beings They are easy to identify and count in the laboratory because of their ability to ferment lactose E Coli A type of bacteria belonging to the fecal coliform group of bacteria found primarily in the gut and feces of warm blooded animals Most E
46. er equipped with an expanded millivolt scale mV or an ISE meter capable of being calibrated directly in terms of nitrate concentration Standards and samples are mixed with an ionic strength adjustment solution Standard Operation Procedure Manual for Analysis of Drinking water quality Page 44 of 64 Calibration is performed by analyzing a series of standards and plotting mV vs nitrate nitrogen concentration or by calibrating the ion meter directly in terms of nitrate concentration HEALTH AND SAFETY Personal protective equipment including safety glasses and lab coats should be used INTERFERENCES Chloride and bicarbonate ions interfere when their weight ratios to NO3 N are gt 10 or gt 5 respectively lons that are potential interferences but do not normally occur at significant levels in potable waters are NO2 CN S2 Br I CIO3 and ClO4 Although the electrodes function satisfactorily in buffers over the range pH 3 to 9 erratic responses have been noted where pH is not held constant Because the electrode responds to NO3 activity rather than concentration ionic strength must be constant in all samples and standards Minimize these problems by using a buffer solution containing Ag2SO4 to remove Cl Br I S2 and CN sulfamic acid to remove NO2 a buffer at pH 3 to eliminate HCO3 and to maintain a constant pH and ionic strength and AI2 SO4 3 to complex organic acids REAGENTS Nitrate calibratio
47. for the growth of bacteria Pathogenic Organisms Bacteria viruses protozoa etc which can cause disease in animals or human beings Sterilization Destruction or removal of all viable or living organisms PRINCIPLE Fecal coliform bacteria are non disease causing organisms which are found in the intestinal tract of all warm blooded animals Each discharge of body wastes contains large amounts of these organisms The presence of fecal coliform bacteria in a stream or lake indicates the presence of human or animal wastes The number of fecal coliform bacteria present is a good indicator of the amount of pollution present in the water RESPONSIBILITY WAL Analyst Operation and Calibration WQL Manager Receiving sample log book entry and Implementation of this SOP WQ Consultant QC QA HEALTH AND SAFETY Wear personal protective equipment including gloves lab coat and safety glasses and handle all chemicals with caution Work under fume hood to avoid inhaling vapors Standard Operation Procedure Manual for Analysis of Drinking water quality Page 8 of 64 Special care should be taken when working with autoclaves due to high temperature and pressures Face shields aprons and temperature resistant gloves should always be worn when opening or removing items from autoclaves Do not look directly into the UV light INTERFERENCES Samples may contain material that affects the color of the sample If thi
48. g water and waterborne diseases which can be prevented drinking water must be free from components which may adversely affect the human health Such components include minerals organic substances and disease causing microorganisms a large portion of the population in developing countries suffers from health problems associated with either lack of drinking water or due to the presence of microbiological contamination in water poor water quality is responsible for the death of children special under the five year old in the developing countries the problem is further aggravated by rapidly increasing population which results in poor water quality management Rural Water Supply Sanitation amp Irrigation Program RUWATSIP Ministry of Rural Rehabilitation and Development MRRD are responsible to provide safe drinking water across the country RuWATSIP Department with technical and financial support by UNICEF had inaugurated Water Quality Laboratory to target community and all water sources in provinces of Afghanistan and distribute safe drinking water for all Water quality Laboratory has two parts first one is Chemical Physical Lab and second part is Bacteriological lab water quality Laboratory inaugurated with a formal meeting and started their activities on 18 July 2011 27 Saratan 1390 UNICEF Kabul and RuWATSIP supplied these laboratories with necessary chemicals and Bacteriological equipment for testing of basic 29 water quality parameters Impl
49. health Avoid skin contact and do not inhale the fumes Chlorine should always be stored in cool dark dry and sealed containers and out of reach of children The toxicity or carcinogenicity of each reagent used in this method has not been precisely identified each chemical compound should be treated as a potential health hazard and exposure to these chemicals should be minimized PROCEDURE Place one tablet in the test chamber and add a few drops of the chlorinated water supply under test Crush the tablet then fill chamber with the chlorinated water supply under test Place more of the same water supply under test without a tablet in the second chamber This is the blank control for colour comparison The level of residual chlorine R in mg of chlorine per liter of water mg l is determined by comparing the colour of the water supply under test in chamber with the tablet added with the standard colours on the vessel chamber RFERENCES p 5 53 65 APHA 20 Ed Technical Note No 11 WHO 7 1 05 ANNEXURE Nil Standard Operation Procedure Manual for Analysis of Drinking water quality Page 29 of 64 Standard Operation Procedure for detection of Total Iron in water Procedure for Operation and Calibration of T60 V Spectrophotometer for Total Iron Examination PURPOSE To establish a procedure for operation and calibration of T60 V spectrophotometer for iron determination in water SCOPE This procedure is
50. hod is for the analysis of residual chlorine in drinking water DEFINITIONS When chlorine is dissolved in clear water in sufficient quantities will destroy most disease causing organisms without being a danger to people The chlorine however is used up as organisms are destroyed If enough chlorine is added there will be some left in the water after all the organisms have been destroyed this is called Free Chlorine Free chlorine will remain in the water until it is either lost to the outside world or used up destroying new contamination We call this measuring the Chlorine Residual PRINCIPLE The color comparator uses DPD 1 N N diethyl p phenylene diamine tablets that causes a color change to pink in the presence of chlorine RESPONSIBILITY WAL Analyst Operation and Calibration WQL Manager Receiving sample amp log book entry and Implementation of this SOP WQ Consultant QC QA HEALTH AND SAFETY Wear proper protective equipment which includes safety glasses protective gloves and a lab coat when working in the active laboratory area Work under a fume hood and or in an adequate ventilated area to avoid inhaling vapors dust etc Standard Operation Procedure Manual for Analysis of Drinking water quality Page 28 of 64 After analysis discard analyzed samples down the drain Retain the unused sample until the sample has been reviewed and reported CAUTIONS All forms of chlorine are harmful to
51. ibration standards After you successfully calibrate the CAL 4 standard 0 02 NTU the display shows STbY Standard Operation Procedure Manual for Analysis of Drinking water quality Page 18 of 64 e The meter is now ready for measurement e Figure 5 shows the complete calibration sequence OPERATIONAL PROCEDURE e Place TN 100 T 100 turbidity meter on a flat and level surface e Place the sample vial inside the sample well and align the vial s index mark with the meter s index mark e Push the vial until it is fully snapped in e Cover the vial with the light shield cap e Turn on the meter by pressing the ON OFF key e After the power up sequence the meter goes to measurement mode and the display blinks Rd for about 10 times e The measured reading appears in the display e f necessary place the second sample vial into the sample well Remember to align the vial s mark with the meter s index mark e Press READ ENTER key The display blinks Rd for several times and measured reading appears e Repeat steps 2 through 9 for all other samples RFERENCES e p 2 4 APHA 20 Ed e Instruction Manual TN 100 T 100 RELATED DOCUM ENTS Procedure for Calibration program RELATED RECORD e Daily Calibration Record of Turbidity meter ANNEXURE Nil Standard Operation Procedure Manual for Analysis of Drinking water quality Page 19 of 64 Standard Operation Procedure for detection of Electical
52. ion Procedure Manual for Analysis of Drinking water quality Page 62 of 64 References APHA 20 Ed 9221 B p 2 44 IS 1622 1981 Reaff 2003 USP25 P 2052 Manual pH Meter P 25 6000 CyberScan Bow m p Instruction Manual TN 100 T 100 Instruction Manual CON 510 APHA 20 Ed 1998 p 2 1 2 3 5 53 65 4 66 68 2 37 39 KNIGHT A G 1951 The photometric estimation of color in turbid waters J Inst Water i o gv wl Arsenator operation manual Wag WE 0500 10 Technical Note No 11 WHO 7 1 05 11 APHA 20 Ed p 4 79 86 4 79 86 12 UVWIN 5 0 instruction manual 13 UVWIN 5 0 instruction manual 14 ol O Vode dl e e la a 15 Aco Y oa Verd aga ala e als 5158 e ds sh 9 Sue Standard Operation Procedure Manual for Analysis of Drinking water quality Page 63 of 64
53. ium in water T 60 PURPOSE c 60 SCOPE AND APPLICATION eem 60 RESPONSIBILITY sccsscsstccccsbeccssecsscitacsacscuvastvnssstessscccebsneccadeacachstatbacdscdeaceddevneastcapssaasenssanccesdtscssedensdatedesdanccdiveanecsddes 60 PRINCIPLE amp SUMMARY OF METHOD c ccccessssecessncececseaeceecseaaeeceeeaaeecseaaaececseaeeeeeseaaaeceeeaaeceseaaaeeeeeseneeeeneaaas 60 HEALTH AND SAFETY WASTE HANDLING L 60 hididddid ecl 60 Standard Operation Procedure Manual for Analysis of Drinking water quality Page 4 of 64 TITRATION PRECAUTIONS s 22 3 cone tou od oac epa rientro ca ua ss asecesssstdetestscactenessceet st gnscdsseosdebeessadeneseeseegessys 61 REAGENTS AND SOLUTION Sarli 61 PROCEDURE 62 CALCULA TONE tada 62 PROTON CIN COS caricia lie io teta 63 Standard Operation Procedure Manual for Analysis of Drinking water quality Page 5 of 64 Introduction of RUWATSIP M RRD Water Quality Laboratory Afghanistan is confronted with a number of basic environmental health issues unsafe drinking water inadequate sanitation facilities poor water supply and hazardous waste water management poor water quality like chemical contamination and Microbial contamination Afghanistan has the highest child mortality rate every year the main cause of death is unsafe drinkin
54. mination or dilution of sample rinse probe with a small volume of your sample solution Standard Operation Procedure Manual for Analysis of Drinking water quality Page 20 of 64 PROCEDURE CALIBRATION PROCEDURE Automatic Conductivity Calibration Turn on the instrument and select conductivity mode by pressing MODE key Rinse the probe thoroughly with de ionized water and then rinse with a small amount of calibration standard Dip the probe into the calibration standard Immerse the probe tip beyond the upper steel band Stir the probe gently to create a homogenous sample Allow time for the reading to stabilized Press CAL MEAS to enter conductivity calibration mode The CAL indicator will appear in the upper right corner of the display The lower display will scan and locked the closest set calibration value momentarily Pressing before the set displayed value being locked will be prompted by an error message and remain in the calibration mode Wait for READY indicator to appear before pressing ENTER key to confirm calibration value The upper display will show dOnE once the calibration is successfully performed To abort calibration without confirming press CAL MEAS to revert back to measurement mode No calibration is performed at this stage To perform the next point calibration in the multi point calibration repeat step 1 7 again until all points have been calibrated if necessary CALIBRATION PROCEDURE Temperature Cali
55. n stock solution 100 mg L NO3 N Dissolve 0 7218 g of potassium nitrate dried for two hrs at 110 C and stored in a desiccator in reagent water and dilute to 1 L in a volumetric flask Store in a clean bottle This standard may also be purchased from a vendor Nitrate calibration standards Dilute 1 0 10 and 50 mL stock nitrate solution to 100 mL with water to obtain standard solutions of 1 0 10 and 50 mg NO3 N L respectively Buffer solution Dissolve 17 32 g Al2 SO4 318H20 3 43 g Ag2SO4 1 28 g H3BO3 and 2 52 g sulfamic acid H2NSO3H in about 800 mL water Adjust to pH 3 0 by slowly adding 0 10N NaOH Dilute to 1000 mL and store in a dark glass bottle Sodium hydroxide NaOH 0 1N Reference electrode filling solution Dissolve 0 53 g NH4 2SO4 in water and dilute to 100 ml Standard Operation Procedure Manual for Analysis of Drinking water quality Page 45 of 64 PROCEDURE Preparation of Calibration Curve Transfer 10 mL of 1 mg NO3 N L standard to a 50 mL beaker add 10 mL buffer and stir with a magnetic stirrer Immerse tips of electrodes and record millivolt reading when stable after about 1 min Remove electrodes rinse and blot dry Repeat for 10 mg NO3 N L and 50 mg NO3 N L standards Plot potential measurements against NO3 N concentration on semilogarithmic graph paper with NO3 N concentration on the logarithmic axis abscissa and potential in millivolts on the linear axis ordinate A straight lin
56. ndards which appear to correspond to the colour of the sample Compare colour of the sample with that of the standards by viewing vertically downwards while the tubes are placed on a white surface Use a colour comparator stand if available fthe sample colour exceeds 70 units dilute sample with distilled water in known proportions In case sample contains turbidity report result as apparent colour Measure pH of each sample CALCULATION Calculate color unit by following equation Color Units A x 50 B where A estimated color of a diluted sample B mL sample taken for dilution Report color results in whole numbers and record as follows Color Units Record to Nearest 1 50 1 51 100 5 101 250 10 251 500 20 Report sample pH RFERENCES e APHA 20 Ed 1998 p 2 1 2 3 e KNIGHT A G 1951 The photometric estimation of color in turbid waters J Inst Water Eng 5 623 ANNEXURE Nil Standard Operation Procedure Manual for Analysis of Drinking water quality Page 25 of 64 Standard Operation Procedure for detection of Arsenic in water Procedure for Operation and Calibration of Wag WE10500 Arsenator for Arsenic Determination in Water PURPOSE To establish a procedure for operation and calibration of Wag WE 10500 arsenator for the determination of arsenic in clean water matrix SCOPE This method is applicable to clean water matrix i e drinking surface saline and ground water in the rang
57. o 13 HEALTH AND SAFETY WASTE HANDLING Wear personal protective equipment PPE including lab coat safety glasses and gloves when performing analysis After analysis discard analyzed samples down the drain Retain unused sample until the sample has been reviewed and reported INTERFERENCES Under conditions of this test the following concentrations of ions cause no interference with the calcium determination Cu2 2 mg L Fe2 20 mg L Fe3 20 mg L Mn2 10 mg L Zn2 5 mg L Pb2 5 mg L Al3 5 mg L and Sn4 5 mg L Orthophosphate precipitates calcium at the pH of the test Strontium and barium give a positive interference and alkalinity in excess of 300 mg L may cause an indistinct end point in hard waters Standard Operation Procedure Manual for Analysis of Drinking water quality Page 60 of 64 TITRATION PRECAUTIONS Conduct titration at or near room temperature The color change becomes impractically slow at the sample approaching freezing temperature Indicator decomposition become problem in hot water REAGENTS AND SOLUTIONS Standard EDTA titrant 0 01M Weigh 3 723g di sodium salt of EDTA dihydrate dissolve in distilled water and dilute to 1000 mL Store in polyethylene bottle Standard Calcium Solution Weigh 1 000g anhydrous CaCO3 in a 500 mL flask Add 1 1 HCI slowly through a funnel till all CaCO3 is dissolved Add 200 mL distilled water and boil for a few minutes to expel CO2 Cool and add
58. ome suspended matter may be removed by filtration Silica in excess of 500 mg L will interfere and in waters containing large quantities of organic material it may not be possible to precipitate BaSO4 satisfactorily In potable waters there are no ions other than SO4 that will form insoluble compounds with barium under strongly acid conditions Make determination at room temperature variation over a range of 10 C will not cause appreciable error APPARATUS Spectrophotometer for use at 420nm providing a light path of 2 5 to 10 cm or turbidity meter Acid washed glassware use conc HCI for cleaning all the glassware rinse with distilled water before use REAGENTS AND SOLUTIONS Buffer solution A dissolve 30g Magnesium chloride MgCI2 6H20 5g Sodium acetate CH3COONa 3H20 1g Potassium nitrate KNO3 and 20mL acetic acid CH3COOH 9996 in 500mL distilled water and make up to 1000mL Buffer solution B required when the sample sulphate SO4 is less than 10mg L Dissolve 30g Magnesium chloride MgCl2 6H20 5g sodium acetate CH3COONa 3H20 1 0g of potassium nitrate KNO3 0 111 g of sodium sulphate Na2504 and 20mL acetic acid 9996 in 500mL distilled water an make up to 1000mL c Barium chloride crystals 20 30mesh d Standard sulphate solution dissolve 0 1479g anhydrous sodium sulphate Na2SO4 in distilled water and dilute to 1000mL 100mg Il PROCEDURE Spectrophotometric setup e Switch on the instrument an
59. omes progressively lighter as the fluoride concentration increases Inthe case of the fluoride ion reaction with Zr SPADNS sodium 2 parasulphophenylazo 1 8 dihydroxy 3 6 naphthalene disulphonate the resulting coloured complex is measured in a spectrophotometer at 570 nm HEALTH AND SAFETY Personal protective equipment including safety glasses and lab coats should be used Standard Operation Procedure Manual for Analysis of Drinking water quality Page 33 of 64 CAUTIONS The addition of the highly colored SPADNS reagent must be done with utmost accuracy because the fluoride concentration is measured as a difference of absorbance in the blank and the sample A small error in reagent addition is the most prominent source of error in this test nl Care must be taken to avoid overheating the flask above the level of the solution This is done by maintaining an even flame entirely under the boiling flask Always rinse cuvette with distilled water before use and after each sample to remove any impurities adhering to the cuvette body Shake or air dry To avoid contamination or dilution of sample rinse cuvette with a small volume of your sample solution Do not wipe the glass cuvette with any coarse material SPADNS Reagent is toxic and corrosive Use care while handling the reagent INTERFERENCES Concentration of substances causing 0 1mg L error at 1 0mg F L in SPANDS method overestimation underestimation
60. on Storage of samples To minimize sodium contamination stores all solution in plastic bottles Use small containers to reduce the amount of dry element that may be picked up from the bottle walls when the solution is poured Minimum detectable concentration The better flame photometers can be used to determine sodium levels approximating 100ug L With proper modifications in techniques the range of sodium measurement can be extended to 10ug L or lower Principle Trace amounts of sodium can be determined by flame emission photometry at the wavelength of 589 nm The sample is sprayed into a gas flame and excitation is carried out under carefully controlled and reproducible conditions The desired spectral line is isolated by the use of interference filters or by a suitable slit arrangement in light dispersing devices such as prisms or gratings The intensity of light is measured by a phototube potentiometer or other appropriate circuit The intensity of light at 589 nm is approximately proportional to the concentration of the element If alignment of the wavelength dial with the prism is not precise in the available photometer the exact wavelength setting which may be slightly more or less than 589 nm can be determined from the maximum needle deflection and then Standard Operation Procedure Manual for Analysis of Drinking water quality Page 53 of 64 used for the emission measurements The calibration curve may be linear but has a
61. on until a definite red precipitate is formed Let stand 12 h filter and dilute to 1000 ml with distilled water Standard silver nitrate titrant 0 0141M 0 0141N Dissolve 2 395 g AgNO3 in distilled water and dilute to 1000 mL 1 mL 500 ug Cl Store in brown bottle 1 00 ml 500 mg CI L Store in an amber bottle PROCEDURE Standardization of Silver Nitrate Titrant Set up titration apparatus Fill the burette to the 0 0 mark with the 0 0141N silver nitrate titrant Transfer 20 ml of the blank into a 50 ml beaker Standard Operation Procedure Manual for Analysis of Drinking water quality Page 38 of 64 Read the pH of the blank Adjust the pH of the blank as necessary to a pH between 7 10 with 0 01N sulfuric acid or 0 01N sodium hydroxide Add 1 0 ml potassium chromate K2CrO4 indicator solution Mix on the stir plate Titrate with standard silver nitrate AgNO3 titrant to a pinkish yellow end point and record ml of titrant used on the chloride Be consistent in endpoint recognition A consistent choice of endpoint is critical Use the standard solution endpoints as a reference and always titrate to the same point to achieve reproducibility from sample to sample Note A blank of 0 2 to 0 3 ml is usual Measure the pH of the Std NaCl sample and adjust if necessary to a pH between 7 10 with 0 01N sulfuric acid or 0 01N sodium hydroxide Add 1 0 ml potassium chromate K2CrO4 indicator solution Mix on the stir plate
62. rimary standard Na2CO3 at 250 C for 4 h and cool in a desiccator Weigh 2 65 transfer to a 1 L volumetric flask fill flask to the mark with distilled water and dissolve and mix reagent Do not keep longer than 1 week Standard hydrochloric acid 0 02N Initially prepare acid solution of approximate normality 0 1N by diluting 8 3ml concentrated HCI into 1L distilled water then dilute 200 00 mL 0 1N standard acid to 1000 mL with distilled water Standardize against 40 00 mL 0 05N Na2CO3 solution with about 60 mL water in a beaker by titrating potentiometrically to pH of about 5 Calculate normality Where A g Na2CO3 weighed into 1 L flask Homie Pe E B mL Na2C03 solution taken for titration and 33 90 amp E C mL acid used Use measured normality in calculations or adjust to 0 02N Phenolphthalein indicator Dissolved 0 1g in 100mL 95 ethyl alcohol Add 100mL distilled water Add dropwise 0 02N NaOH till faint pink colour appears pH 8 3 Methyl orange indicator Dissolve 0 1g and dilute to 200mL with distilled water pH 4 3 4 5 PROCEDURE BICARBONATE Take 10 mL sample Add 2 drops methyl orange indicator If light yellow color appears it indicate presence of bicarbonate Titrate against 0 02N HCI when color change to orange color stop titration note burette reading Standard Operation Procedure Manual for Analysis of Drinking water quality Page 48 of 64 CALCULATION Bicarbonate in mg l burette reading in ml
63. s SOP WQ Consultant QC QA DEFINITIONS A three point calibration involves calibrating the pH meter with three different buffers of known pH and then checking the pH meter against a pH 7 00 standard buffer to confirm the calibration Fill Solution Acts as an electrical conductor between the reference inside the electrode and the solution under test Wetting Cap The cap that covers and protects the tip of the electrode The wetting cap should stay on the tip of the electrode during periods of non use HEALTH AND SAFETY Personal protective equipment including safety glasses and lab coats should be used CAUTIONS Do not allow fill solution to run dry Add fill solution whenever the level falls more than 25 mm below the fill hole Do not leave the electrode in organic solvents as the tip and body may be damaged Keep the electrode of pH meter in 3M potassium chloride solution Do not wipe the glass electrode bulb with any coarse material lf there are signs of growth or contamination in buffer solutions then discard the solutions and prepare fresh Standard Operation Procedure Manual for Analysis of Drinking water quality Page 13 of 64 Buffer solution should not be used after 3 months nl INTERFERENCES The electrodes can be stored for up to one week in 25 mm of pH 7 0 or pH 4 0 buffer Never store the electrode in distilled water For longer storage periods remove the bulb protector fill the
64. s situation does arise compare inoculated trays to a control tray containing only water Test sensitivity maybe affected by taking the samples out of the incubator too soon ending with false negatives Test samples should be incubated forthe full term Autofluorescentplastic ware or glassware may produce false positives Check sample containers prior to sampling and processing MEDIA PREPARATION Single strength MacConkey medium Dissolve 35 0 g in 1 liter of distilled or deionized water Stir slowly until complete dissolution Dispense in tubes containing a Durham tube Sterilize in an autoclave at 121 C for 15 minutes After cooling the Durham tubes should not contain air Double strength MacConkey medium Dissolve 70 0 g in 1 liter of distilled or deionized water Stir slowly until complete dissolution Dispense 10 mL in 20 x 200 mm tubes without a Durham tube Sterilize in an autoclave at 121 C for 15 minutes Brilliant Green Bile Lactose medium Dissolve 20 0 g in 1 liter of distilled or deionized water Stir slowly until complete dissolution Sterilize in an autoclave at 121 C for 15 minutes Peptone Water Dissolve 10 0 g peptone water and 5 0 g NaClin 1 liter of distilled or deionized water Sterilize in an autoclave at 121 C for 15 minutes Standard Operation Procedure Manual for Analysis of Drinking water quality Page 9 of 64 PROCEDURE STERI Total LIZATION Hot Air Sterilizer All equipment should be wrappe
65. s the color of the whole water sample and consists of color from both dissolved and suspended components True color is measured after filtering the water sample to remove all suspended material The term color is used here to mean true color HEALTH AND SAFETY Personal protective equipment including safety glasses and lab coats should be used CAUTIONS Pretreatment for Turbidity Removal To determine color turbidity must be removed before analysis Methods for removing turbidity without removing color vary Filtration yields results that are reproducible from day to day and among laboratories However some filtration procedures also may remove some true color Centrifugation avoids interaction of color with filter materials but results vary with the sample nature and size and speed of the centrifuge When sample dilution is necessary whether it precedes or follows turbidity removal it can alter the measured color Acceptable pretreatment procedures are included with each method State the pretreatment method when reporting results 1 Standard Operation Procedure Manual for Analysis of Drinking water quality Page 23 of 64 PRINCIPLE Color is determined by visual comparison of the sample with known concentrations of colored solutions The unit of color being that produced by 1 mg platinum L in the form of the chloroplatinate ion APPLICATION The platinum cobalt method is useful for measuring color of potable water an
66. served report negative E Coli If gas bubbles seen in durham tubes inoculate loopful from BGLB broth to 5 ml of peptone water and incubate this peptone water test tube without durham tube at 44 5 C for 24 hours e After 24 hours add few drops of Kovac s reagent to the test tubes e f pink color ring formation is observed report E Coli as positive otherwise negative E Coli RFERENCES e APHA 20 Ed 9221 B e 1S 1622 1981 Reaff 2003 NOTE For the combination of positive tubes not appearing in Table 1 use the following formula No of positive tubes x 100 MPN 100 ml ml of sample in negative tubes x ml of sample in all tubes Standard Operation Procedure Manual for Analysis of Drinking water quality Page 11 of 64 MPN Index per m o 2 o 2 u o 2 o z 2 a E o MPN Index per Combination of positive tubes REFRENCE TABLE 1 M PN 100 ML Page 12 of 64 Standard Operation Procedure Manual for Analysis of Drinking water quality Standard Operation Procedure for detection of pH in water Procedure for Operation and Calibration of pH Meter CyberScan 6000 PURPOSE Toestablish a procedure for operation and calibration of pH meter SCOPE This procedure is applicable for operation and calibration of CyberScan 6000 pH meter only RESPONSIBILITY WAL Analyst Operation and Calibration WQL Manager Receiving sample amp log book entry and Implementation of thi
67. sh and then turn off the power This ensures that there is no gas left in the tubing to the unit Operating precautions 1 The fuel gases used in the flame photometers are inflammable and therefore potentially hazardous Cylinders of fuel gas should always be stored and used in appropriate and safe ways 2 It is possible that a small quantity of fuel will escape from the instrument during the ignition sequence The amount of fuel is harmless although may smell slightly If the smell of fuel gas persists the instrument should be immediately shut down and locate source of the leakage in the hose joints 3 Do not leave the instrument running unattended while the flame is alight 4 The top of the instrument chimney unit becomes very hot when running and can cause severe burns if touched 5 The exhaust gases from the flame are very hot and the area approximately 1 metre above the chimney must be avoided Never attempt to look down the chimney whilst the flame is running Always use the inspection window 6 The instrument uses potentially hazardous electrical supplies Never remove covers from the instrument without first ensuring that it has been isolated completely from the mains power supply Standard Operation Procedure Manual for Analysis of Drinking water quality Page 55 of 64 Standard Operation Procedure for detection of Sulfate in water Procedure for Operation and Calibration of T60 V Spectrophotometer for Sulfate Examination PURPO
68. strument chimney unit becomes very hot when running and can cause severe burns if touched 5 The exhaust gases from the flame are very hot and the area approximately 1 metre above the chimney must be avoided Never attempt to look down the chimney whilst the flame is running Always use the inspection window 6 The instrument uses potentially hazardous electrical supplies Never remove covers from the instrument without first ensuring that it has been isolated completely from the mains power supply Standard Operation Procedure Manual for Analysis of Drinking water quality Page 52 of 64 Standard Operation Procedure for detection of Sodium in water Procedure for Operation and detection of Sodium in water by Flame Emission Photometric Scope and application Sodium ranks sixth among the elements in order of abundance and is present in most natural water The levels may vary from less than 1 mg Na L to more than 500 mg Na L Relatively high concentrations may be found in brines and hard water softened by the sodium exchange process The ratio of sodium to total cations is important in agriculture and human pathology Soil permeability can be harmed by a high sodium ratio Persons afflicted with certain diseases require water with low sodium concentration A limiting concentration of 2 to3 mg L is recommended in feed water destined for high pressure boilers When necessary sodium can be removed by the hydrogen exchange process or by distillati
69. temperature To each test tube of 1 set containing double strength media add 10 ml water sample with sterilized pipette To 2 set of tubes add 1 ml sample and add0 1 ml water sample to 3 set of test tubes Incubate all above three set of test tubes at 37 1 Cfor 48 hours After the due time examine color change and gas formation in durham tubes Any tube with color change to yellow or gas formed in durham tubes are consider positive note the number of positive tubes in each set and find the MPN from table 1 If no color change or gas formation is observed discontinue the test and report less than 2 coliform 100 ml Standard Operation Procedure Manual for Analysis of Drinking water quality Page 10 of 64 Coliform Confirmation Test e In sterilized test tube insert inverted durham tube and add 10 ml of Brilliant Bile Green Lactose broth and transfer loopful from each individual positive tubes e Incubate the tubes at 37 1 C for 48 hours e Examine the tubes for gas formation No gas production observed disconnect the test and report as less than 2 Coliform 100 me MPN If gas is produced in durham tubes record the positive tubes out of 15 tubes as confirmed for coliform and proceed for E Coli test Escherichia Coli E Coli e Inoculate loopful from each confirmed positive BGBL broth test tube to 10 ml new BGBL media with durham tube and incubate at 44 5 C for 24 hours e Examine test tubes after 24 hours if no gas production ob
70. tendency to levels off at higher concentrations Reagents Deionized distilled water Use deionized distilled water to prepare all calibration standards and reagents and as dilution water Stock sodium solution Dissolve 2 542 g NaCl dried at 140 C and dilute to 1 000 ml with water 1 00 ml 1 00 mg Na Intermediate sodium solution Dilute 10 00 ml stock sodium solution to 100 ml with water 1 00 ml 100 ug Na This solution is used to prepare the calibration curve in the range 1 to 10 mg l sodium Storage of standards Store solutions away from direct sunlight in a cool place ideally at temperatures below 259C Glass containers should not be used for storage as they can affect the concentration levels Standards should be stored in sealed plastic vessels and in high concentrations e g as a stock 1000ppm solution and dilutions prepared as required The long term storage of low concentration standards is not recommended due to degradation of ionic species Operation 1 Ensure that the drain trap has solution in it and that no air locks are present If necessary purge by adding deionised water and allowing the surplus to run away 2 Turn on the fuel supply at source i e cylinder and then switch on the photometer 3 Press the ignition switch and hold down Watch the flame indicator in the display window When this indicator is illuminated the flame is a light and the ignition switch can be released If the flame indicator does
71. trant 20 ml volume of sample analyzed RFERENCES p 4 66 68 APHA 20 Ed 1998 ANNEXURE Nil Standard Operation Procedure Manual for Analysis of Drinking water quality Page 40 of 64 Standard Operation Procedure for detection of Total Hardness in water Procedure for Operation and Calibration of Total Hardness determination in Water PURPOSE To establish a procedure for total hardness determination in water SCOPE AND APPLICATION This method is based on Standard Methods 2340 C EDTA titrimetric method and is applicable to ground drinking surface and saline waters domestic and industrial wastes RESPONSIBILITY WAL Analyst Operation and Calibration WQL Manager Receiving sample amp log book entry and Implementation of this SOP WQ Consultant QC QA PRINCIPLE SUMMARY OF METHOD An excellent way to determine water hardness is to perform a complexometric titration using a standard ethylenediaminetetraacetic acid EDTA solution Due to steric hindrances EDTA will complex with calcium and magnesium in a one to one molar ratio The endpoint in this experiment will be determined using a calmagite indicator The indicator imparts a red color to the solution while there are calcium and magnesium ions that have not complexed with EDTA Once the endpoint has been reached and there is no more uncomplexed Ca or Mg the indicator will give a blue color No hint of red color will be left HEALTH AND SAFETY WAS
72. ultant QC QA PRINCIPLE amp SUM M ARY OF M ETHOD Alkalinity of sample can be estimated by titrating with standard hydrochloric acid 0 02N at room temperature using phenolphthalein and methyl orange indicator Titration to decolourisation of phenolphthalein indicator will indicate complete neutralization of OH and of CO3 while sharp change from yellow to orange of methyl orange indicator will indicate total alkalinity complete neutralisation of OH CO3 HCO3 HEALTH AND SAFETY WASTE HANDLING Wear personal protective equipment PPE including lab coat safety glasses and gloves when performing analysis After analysis discard analyzed samples down the drain Retain unused sample until the sample has been reviewed and reported INTERFERENCES Soaps oily matter suspended solids or precipitates may coat the glass electrode and cause a sluggish response Allow additional time between titrant additions to let electrode come to Standard Operation Procedure Manual for Analysis of Drinking water quality Page 47 of 64 equilibrium or clean the electrodes occasionally Do not filter dilute concentrate or alter sample TITRATION PRECAUTIONS Conduct titration at or near room temperature The color change becomes impractically slow at the sample approaching freezing temperature Indicator decomposition become problem in hot water REAGENTS AND SOLUTIONS Sodium carbonate solution 0 05N Dry 3 to 5 g p
73. wetting cap with KCI solution and push the wetting cap onto the tip of the electrode PROCEDURE CALIBRATION PROCEDURE Auto Buffer Recognition e Switch on the instrument and make sure auto buffer recognition is selected in the setup screen e Touch standardize on the screen to access the standardization screen e Immerse the pH electrode and temperature probe in buffer solution from the selected buffer group and stir gently and wait for 1 2 minute for thermal equilibrium The selected buffer group appears on the standardization screen e The screen will flash a beaker icon of the buffer solution you have selected When the reading is stable STABLE appears on the screen e Touch Confirm icon to standardize buffer The meter will return to pH measure screen e Repeat step 8 1 4 and 8 1 5 for other two buffer standards e After calibration place the electrode in potassium chloride solution OPERATIONAL PROCEDURE P e Immerse the rinsed electrode in the sample and stir gently e Touch measure to begin measuring your sample The meter will accept the reading and display STABLE e The measure screen provides readout of the current sample measurement Then the auto read function is active the meter will lock onto a reading when the meter recognizes it as stable The meter will not deviate from this reading until the measure button is touched e f the auto read mode is inactive then the meter will continuously monitor the pH of the
74. x 100 mg l Bicarbonate Alkalinity in m mole as bicarbonate burette reading in ml x 2 m mole alkalinity PROCEDURE CARBONATE If pH of the sample is above 8 3 it indicate the presence of carbonate in the water sample Take 10 mL sample Add 2 drops phenolphthalein indicator Appearance of pink color indicates presence of carbonate and pH 8 3 or above Titrate against 0 02N HCI when color change from pink to transparent stop titration note burette reading CALCULATION Carbonate in mg l burette reading x 100 RFERENCES e p 2 26 28 APHA 20 Ed ANNEXURE Nil Standard Operation Procedure Manual for Analysis of Drinking water quality Page 49 of 64 Standard Operation Procedure for detection of Potassium in water Procedure for Operation and detection of Potassium in water by Flame Emission Photometric Scope and application Potassium ranks seventh among the elements in order of abundance yet its concentration in most drinking water seldom reaches 100mg L Potassium is an essential element in both plant and human nutrition and occurs in groundwater as a result of mineral dissolution Storage of samples Do not store samples in soft glass bottles because of the possibility of contamination from leaching of the glass Use acid washed polyethylene or borosilicate glass bottles Adjust sample to pH 2 with nitric acid This will dissolve potassium salts and reduce adsorption on vessel walls Minimum detectabl

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