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    © All Rights Reserved
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    8 views43 pages

    Lab - SOP PH

    Uploaded by

    Mehmet Diler
    SOP

    Copyright:

    © All Rights Reserved
    Download as PDF or read online from Scribd
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    Franklin Township Municipal Sanitary Authority Laboratory Standard Operating Procedures Effective Date: April 15, 2010 Revisions: July 28, 2006 (original) June 21, 2007 (rev. 1) January 4, 2010 (rev. 2) April 14, 2010 (rev. 3) Approving Name: Kevin Kaplan ‘Title: Assistant Manager Approving Signature: Date: ‘The analyst has read, understands and is performing the methods as writen in these SOPs. ‘Analyst Name (rin) Init Analyst Signature Date: ‘able of Contents: Pase Distibution List 1 Identification of Methods 1 “Ammonia Distillation of, 2 Neslerzation Method 5 Total Suspended Solids 9 pH 2 Dissolved Oxygen 15 cBop 18 Chlorine, Residual 2 Fecal Califor “Membrane Filtration Technique 30 Multiple Tube Fermentation (AI Medium) 36 Tol Solids 2 Disribtion List, Jes Brucker - Manager Gene Greco - Plant Superintendent Kevin Kaplan - Assistant Manager isillation of, - Standard Methods (SM). 184 ed 4590-NH3 B, ‘esslerization Method - Standard Methods (SM), 18° ed. 4500-NH3 C. ‘Chlorine, Residual (4500-C1 G.)- DPD Colorimetric ‘DH Blecrometrc Method (Standard Methods 18*ed. 4500-1 B.) “TSS - Total Suspended Solid Dried at 103 - 105 °C (Standard Methods 18% ed. 2540 D.) ‘CBOD - Carbonnceous Biochemical Oxygen Demand, BODS (Standard Methods 15% ed 5210) Dissolved Oxygen - Membrane Electrode Method (Standard Methods 18* ed. 4500.0 G.) Fecal Coliform ‘Membrase Filtration Technique (Standard Methods 18%ed 9222 D. Membrane Filter Technique) “Multiple Tube Fermentation - Fecal Coliforms (Biosolids) in A-1 Broth (Standard ‘Methods 18 ed. 9221 E) Ammonia, Distil ‘Scope: lation i require preliminary step to the Nessleization Method (4500 NH3 C) forthe valuation of wastewater samples. The ammonia released inthe distillation process i eaptured {na solution of boric acid and can be determined colorimetrically by nesslerzation using @ spectrophotometer - The samples ae buffered ata pH of 9.5 with a borate buffer solution to decrease hydrolysis of eyanates and organic nitrogen compounds. This is a colorimetic test in ‘which an inereas in color is proportional to an increase inthe concentration of ammonia (NH3- ™, ‘Sample Handlire, Preservation and Preparation: Distillation is performed on 24 hour, 8 hour composites samples and/or grab samples of influent and/or effluent wastewater. If the samples ae not tested immediately after distillation, they are place in plastic o glass containers and stored in the sample refigerator. of (4800-NH3 B) ‘Composite samples during compositing are kept reftigerated near 4 degree Celsius. After collection samples are stored in a refrigerator near 4 deprees Celsius. Upon collection, samples are dechlorinated using either sodium thiosulfate or sodium sulfite, ‘Samples that are to be distilled immediately following collection are not preserved otherwise 1 ‘lof 1+ 1 H2S04 is added per liter of sample (or an amount equivalent for the sample volume) so that a pH of less than 2 is achieved. ‘Disillation Apraratus and Equipment: 1. Several borosilicate glass flasks of 500 mi capacity ae attached to vertical water cooled ‘condensers with the outlet tps submerged below the surface ofthe receiving solution (ori acd. 2. Blectromantle heating units with temperature adjustments capable of causing the sample tw boi 3. pH meteor litmus paper 4. Boiling chips 5. Receivirg flasks Reagents: Ammonia fee water - distilled water passed through a Bamstead Easy Pure ion-exchange system 2 and prepared as needed. Ammonia free water is used forall reagents, standards, laboratory contol samples and blanks. ‘Borate buffer solution - 88 mls of 0.1N NaOH solution and 4.75 g of sodium tetraborate (Na2B407 * 10 H20) is added to 500 ml of ammonia free water, then diluted tol liter. [Boric acid solution - 20 ¢ of boric acid diluted to 1 liter. (0.4% Thymol Blue indicating solution 1+ 1 Sulfuric Acid solution - Equal parts of Sulfuric Acid and reagent grade water are added together stored in glass container. Safety Note: Acid into water! Sodium Thiosulfate (dechlorinating agent) - dissolve 0.35 g of Na2S203 * $ H20 into 50 ml of reagent grade water and dilute to 100 ml, Add 0.5 ml to sample to remove 1 mg/L of residual chlorine. Sodium aydroxide solution: (GIN NaOH - 4.0 g of NaOH diluted to | liter with reagent grade water, SN NaOH - 200 g of NaOH diluted to | liter with reagent grade water. Equipment Preparation: Adjust 2250 ml volume of distilled water toa pH of 9.5 with SN sodium hydroxide solutcn Place into distillation unit along with some boiling chips and 12 mls of borate buffer solution, ‘This mixture is used to steam out the distillation apparatus to eliminate traces of ammonia. Procedure: ‘An adequate amount of sample volume (approximately 1 L) is checked fora residual chlorine ‘and an aopropriate amount of thiosulfate solution is added for dechlorination. Add 0.1 ml ‘o sample t) remove 0.2 mg/L of residual chlorine. 12 ml ofborate buffer solution, 2-3 drops of 0.4% thymol blue indicating solution and boiling chips are added to a 250 mi dechlorinated sample ina distillation unit. The sample should tur blue if pi is in the 9.5 range. If nt, the sample needs to be adjusted to that pH range with the ‘appropriate (SN) sodium hydroxide solution using a pH meter. Tur on heating mantle to an pproprite temperature and distil off into a 50 ml boric acid solution toa total volume of 250, ‘ml. The ip of condenser needs to be submerged into the receiving solution. During the lst ‘minute cr two of distillation, lower the receiving solution as to cleanse the condenser and delivery tube. Quality Control Distillation should include: a blank, laboratory control sample, duplicate, spike duplicate spike and a 10 2pm ammonia standard. Refer tothe Quality Manual for additional QA/QC requirements and information. Standards: Using a Class A pipet, 10 mi of 1000 ppm stock ammonia standard is diluted to 500 ml with reagent grade water in a volumetric flask, Added I ml of +1 Sulfuric Acid solution, then further iluteto |. (10 ppm final concentration) Refer to Ammonia, Nesslerization Method 4500-NHL C. following this section. Notes: ‘Standard, LCS and all QA/QC should be distilled off s a sample. Determine the ammonia concentration by the Nesslerzation Method Standard Methods 18" ed. 4500-NIB C, Ammonia, Nesslerization Method of (Standard Methods 18% ed. 4500-NH3 C.) ‘Scope: thas been established by the Authority that this method, following distillation, is applicable for ‘the determination of ammonia in it's wastewater influent and effluent samples. A spectrophotometer with alight path of Sem set ata wavelength of 425 nm can determine ‘ammonia concentration between 0.1 ppm and 5.0 ppm. Absorbance is measured and conforms to ‘Beer's Law having a linear curve ‘Upon addition ofthe Nessler’s Reagent, @ light yellow color in the sample is indicative ofa low ‘ammonia concentration. Color increase is proportional with ammonia concentration ‘The calculated detection limits are 0.05 ppm. The lowest concentration that the Authority will report is <0.1 ppm. The upper limit for this curve is 5.0 ppm. Sample concentrations above this amount need tobe diluted to concentration from mid-range to the upper concentration of the curve. Arminimam of a4 point standard curve willbe ran, not including the blank. The correlation ‘coefficient (r value) shall be no les than 0.9980, ee Analysis is performed on 24 hour, hour composites samples and/or grab samples of influent ‘and/or eluent wastewater. Ifthe samples are not tested immediately following distillation, they ‘are stored in the sample refigerator at 4 degrees Celsius ‘Composite samples during compositing are kept refrigerated near 4 degree Celsius. After collection samples are stored in a reftigerator near 4 degrees Celsius ‘Upon collection, samples are dechlorinated using either sodium thiosulfate or sodium sulfite. ‘Samples that are to be distilled immediately following collection are not preserved otherwise 1 ml of 1+ 1 H2S04 is added per ltr of sample (or an amount equivalent forthe sample volume) 0 that apH of less than 2 is achieved and the sample i distilled and analyzed at alter time within 2 weeks of sample collection or sooner if required by regulation ‘Standards are prepared atthe same temperature and reaction time (approximately 10 minutes) as used forthe samples. ‘Standards: Preparation ofthe standards are as follows: 1 100 OL 3 100 03 5 100 05 5 50 10 10 50 20 15 50 30 20 50 40 25 50 50 CCV preparation: smls of 10 pm Standard Diluted to (mls) inal concentration (ppm) 2 100 02 45 100 45 ‘A.0.2_ppmand 4.5 ppm standards are used as a continuing calibration verification (CCV). CCVs are to be alternated between high and low. Any CCV is acceptable to use if the low CCV isin the lower 20% of the curve but not more than 5 times the lowest quantitation level andthe high (CCV is within the upper 20% of the curve, Procedure: Let samples and standards stout a room temperature for approximately 1 hour. “Make up sandards in the concentration range stating at 0.1 ppm to 5.0 ppm, Use different concentration forthe curve. Warm up spectrophotometr for 10 minutes. Set a 425 nm wavelength Zero spectophotometer with ised water according o manufactures directions located on the instrumentitself Set spectrphotomete tothe Absorbance reading. us the stndard curve starting wih the lowest concentration through the highest ‘Use a 50.0ml sample ora portion diluted with reagent grade wate. ‘Add a few drops of SN sodium hydroxide solution to neutalize the boric acid solution. ‘Add I ml of Nessler Reagent. Run the LS, blank and samples wth all QA/QC. Rana CCV and a blank every 10 samples and atthe end ofthe analysis. ‘Mix thoroughly and lt stand 10 minutes for color development. Record absorbance readings. Using absrbance versus concentration, calculate the cuve corelation coefficient (R vale). += 0.9980 or betters acceptable ‘Calelate and report concentration of NH-N from curve on datasheet. Example analysis run: Reagent Flank (Boric Acid) CCV (029 ppm) Effluent sample 1 Effluent sample 2 Effluent sample 3 Effluent sample 3 duplicate Eflvnt simple 3 spike Event sample 3 duplicate spike Inflows ample Inert sample 2 Infoent ample 3 ccv Blane Apparatus Spectrophotometer- Spectonic 200+ pil meter Class A pet: 1m 50 ml beakers 50 ml graduate cylinders ‘Reagents: ‘Ammonia free distilled water (Reagent grade) Nessler Reagent - purchased SN sodiun hydroxide solution -20 g of NaOH diluted to 100 ml with reagent grade wate. ‘Stock ammonium solution - Dissolve 3.819 g anhydrous NHACI, dried at 100 degrees Celsius, in ‘ammonia fee distilled water, and dilute to 1 L 1.00 ml= 1.00 mg N= 1.22 mg NEB. 7 Standard ammonium solution - Dilute 10.ml of stock ammonium solution to 1 L with reagent grade water. 1 ml=10 ppm N= 12.2 ppm NH3. gasoc: Refer to page 31 of the Laboratory Quality Manual. Control limits are 43 times the standard deviation for CCVs, Control limits for laboratory control samples (LCS) are set by the manufacture, Refer to their documentaton for limits. Duplicate samples with values beyond 3.27 times the average value are considered “Not ‘Acceptable ‘Spike concentrations (refer to page 30 ofthe Laboratory Quality Manual) ive Act Refer to page 31 of the Quality Manual. Data outside the limits is considered “Not Acceptable” and the analyst isto flag the data, check for enors ard take corrective action. (QA/QC results that are more than +2 times the standard deviation but less than 43 times are acceptable but the analyst should check for eror. ‘Reporting of Results: Refer tothe Quality Manual Equations: img NH3-NL=Cx A/B x DIE total volume (50 ml) sample volume used C= concentration from curve sample volume originally distilled Aistllate volume collected including boric acid solution ‘The ratio DIE only applies ifthe original sample volume and the distilled sample volume are not the same, mg NH3-N/L = Concentration of Sample x (Total Volume ~ Sample Volume used) = Concentration of Sample x (50 ml + Sample Volume used) Dilutions for Standards: (Concentration of A) x (Volume of A) = (Concentration of B) x (Volume of B) Total Suspended Solids Dried at 103 - 105 °C (Standard Methods 18% ed. 2540 D.) ‘Scope: ‘A well-mixed composite sample of wastewater influent or effluent is filtered through a weighed ‘standard glass-fiber filter and the residue retained on the filter is dried to a constant weight at 103 te 105°C. The increase in weight of the filter represents the total suspended solids. This method is appropriate forthe examination of wastewater. Inteferences: Exclude large floating particles or submerged gathered masses of nonhomogeneous materials from. the sample if it is not representative ofthat sample. Limit the sample size to that yielding no more than 200 mg residue. For samples high in dissolved solids thoroughly wash the filter to ensure the ‘removal of dissolved material. Prolonged filtration times resulting from filter clogging may produce. ‘high results owing o increased colloidal materials captured on the clogged filter. ‘Sample Handling. Preservation and Preparation: Analysisis performed on 24 hour or 8 hour composites samples of influent and effluent wastewater. Ifthe samples are not tesed within 1 hour after sampling, they are placed in plastic containers thet have leak-proof tops and stored inthe sample reftigerator at 4 degrees Celsius. All samples will be ‘analyzed within 24 hours of collection. Reagents: Distilled water Apparatus: Drying oven, for operation at 103 t0 105°C. Analytical balance, 10 to 200 g capacity, capable of weighing up to 0.0001 g (0.1 mg). Filtration apparatus (vacuum pump with reservoir) or aspirator. Gooch crucibles, 25-ml to 40-ml capacity each with their own unique identification. Desiccator, provided with a desiccant containing a color indicator of moisture concentration. Graduated cylinders, 25-ml, $0-ml, 100-ml, 250-mi, $00-ml Glass-fibe filter disks, 2.4 em to 4.7 em; Whatman grade934AH, Gelman type AE, Millipore type ‘APAO, or equivalent. Suction Flask, 250-ml Dish tongs Forceps, smoothed-tip, ‘reparation of glass-fiber filter disk: ‘The glas-fber filter disk is inserted rough side up in the Gooch crucible using the forceps. Discard ‘any filters that are toro contain holes. Do not handle the glass fiber filters. ‘Conneet to filtration apparatus and turn on vacuum, ‘Wash disk with three successive 25-ml portions of reagent-grade water. Continue suction until all races of water are removed. Discard rinse filtrate from filter flask. Remove Gooch crucible and transfer tothe drying over fora period of 1 hour. ‘Remove from drying oven and transfer tothe desiceator. Let crucible cool to room temperature in desiccator. Proves ‘Select crucible and weigh 3 times on an analytical balance. Record crcibleidentiffeation and weights ‘Connect filtration apparatus and begin suction, ‘Wet the filter witha small volume of reagent-grade water to seat it ‘Stir or mix sample thoroughly, remove the appropriate volume into a graduated cylinder and filter. ‘Tae appropriate volume would be that which would yield between 2.5 and 200 mg or residue If filtration time exceeds 10 minutes, decrease the sample volume or use a larger filter to ensure & representative sample can be filtered. Rinse with three suecessive 10-ml volumes of reagent-grade water, allowing complete drainage ‘between washings and continue suction for about 2 minutes after filtration is complete. ‘Samples with high dissolved solids may require additional washings. [Remove the crucible from the filtration apparatus and transfer tothe drying oven fort least 1 hour at 103 t0 105°C, ‘After drying is complete, transfer to the desiccator and allow to cool to room temperature. Select crucible and re-weigh 3 times on an analytical balance. Record crucible identification and weights. Alternatively, the crucible, if dried overnight, cn be weighed one time instead of 3. Caleulation: OWE Wi x 1000. img total suspended solids = Sample volume, mi where: WE= the final weight ofthe crucible, mg Wi the initial weight of the crucible, mg. Each sarple will be analyze with two crucibles with equivalent volumes. The average ofthe tw- results wil be reported, 10 owioc: ‘Two crucibles per sample. ‘One sample must be run in duplicate (total of 4 crucibles). ‘A reference weight (20g) in the range ofthe weight ofthe samples and crucibles nnst be weighed ‘onthe analytical balance prior to running samples to check it's precision ard accuracy, Refer tothe Quality Manual ‘The laboratory will keep a calibration certificate demonstrating the traceability to NIST standards and the weights must be ASTM type 1, 2, or 3 (Class $ or S-1). Reference weights will be re= certified every 5 years and documented pH, Electrometric Method (Standard Methods 18" ed. 4500-H' B.) Introduccion: 1H isa mathematical expression of the intensity ofthe acid or alkaline condition of a sampie. The term “pH” is defined asthe negative logarithm of the hydrogen ion concentration, and is generally represened with a scale from Oto 14 pH units. ‘Water is made up ofboth hydrogen ions (H+) and hydroxyl ions (OH-). Because water is made up ofthese wo ions, any solution which contains water (called an aqueous solution) always has both hhydzoges ions and hydroxyl ions, The pH scale is a means of showing which ion has the greater intensity, ‘AtapH of 70, the intensities ofhydrogen and hydroxyl ions are equal and solution is said tbe pH ‘neutral. When the pH is less than 7.0, the intensity ofthe hydrogen ions is greater than tht of the hydroxyl ions and the solution is said to be acidic. When the pH is greater than 7.0, the hydroxyl ions have the greater intensity and the solution is efered to as alkaline or basic. ‘The pH measuring instrument is calibrated potentiometrically with an indicating (glass) electrode and reference cell using NIST buffers having assigned values. ‘pH monitoring and controls importants the operation of wastewater treatment plants. This method is applicable for the analysis of wastewater. Sampling: (Only grab samples may be taken for pH measurement. Itis very important that the samples be well ‘mixed and representative of the plant flow. Each sampling point should have it’s own sample colletion devices and container in order to prevent cross-contamination. Preservation: ‘The pH must be measured as soon after collection as possible. There isnot approved method of sample preservation for pH samples. Ifthe time lag between sample collection and testing exceeds '30 minutes, the samples should be discarded and fresh samples collected, ‘Sample Containers: Polyethylene, polypropylene or glass. ‘Sample Container Preparation: All sample collection containers and bottles should be cleaned thoroughly with soap and water on ‘regular basis and rinsed well. A final rinsing shouldbe 3 times with distilled water and allowed ‘ody. ‘Equipment: ‘pH meter, readable oat least 0.1 pH nit with temperature probe. Beakers Electrode, combination Magnetic stimer and sting bar. Reagents: pH buffer solutions: pH of 4,7 & 10 ‘Calibration; Tum on pH meter and allow instrument to warm up. Calibrate according to manufacturers instruction found inthe laboratory. Insert pH probe into 7.00 pH buffer solution. Record mV and temperature. Remeve pH probe from the buffer solution, rinse with dsilled water and carefull blot the probe dy Place probe into «10.00 pH buffer solution. Record mV and temperature Remove pH probe fom the buffer solution, rinse wit dsiled water and carefully blot the probe dry. 7. Place probe into a 4.00 pH buffer solution. Record mY and temperature, 8. Check calibration with a laboratory control sample (LCS). Procedure: ‘Tum on pH meter and allow instrument to warm up. Remove pH probe from buffer solution, [Rinse pH prebe with distilled water and blot the probe dry Insert probe into a beaker containing the sample along witha stirring bar. ‘Tum on magnetic stirer and str sample at a moderate rate Record pH reading and temperature. ‘After usage, um pH meter on “standby”. aloe: ‘Check calibration with afresh 7.00 buffer solution daily 3B ‘Run a laboratory control sample. ‘Duplicate samples should be run on every 10* sample. ‘Laboratory bench sheets must be maintained that document the date and time the sample was ‘collected, the analyst, method number, result and temperature of sample. ‘Refer to he Quality Manual ‘Interferences: ‘The glass electrode is relatively fee from interferences due to color, turbidity, colloidal matter, oxidants, ductanta or high salinity, except fora codium error at ahigh pH. This error ata pH above 10 may be reduced by using a special “low sodium error” electrode. Itis nt typical forthe treatment ‘plant to analyze samples above the pH of 10. Since both ph, itself, as well asthe measurement of pH are temperature dependent, iis important ‘that temperature compensation be performed on all saraples and thatthe temperatures of buffers and samples beas similar as possible. ‘Notes: Record temperature along with pH. ‘Check the pH probe for cracks and the appropriate amount of filling solution. ‘Calibration should be a 3 point calibration Replace buffer solution daly Do not use expired buffer solutions. Discard used buffer solutions. ‘Watch for eric results. ‘Reporting of Data: Report pH values to the nearest 0.1 pH unit. Record temperature of samples with pH values. 4 Dissolved Oxygen, Membrane Electrode Method (Standard Methods 18 ed. 4500-0 G) ‘This method is applicable forthe determination ofthe amount of dissolved (or ftee) oxygen present in water or wastewater. Membrane electrodes provide an excellent method for DO analysis in polluted waters, highly colored waters, and strong waste eflucats, An accuracy of 40.1 mg DO/L ‘and a precision of £0.05 mg DOL can be obtained, ‘The membrane electrode procedure utilizes a meter and electrode, and is based on the rate at which ‘oxygen molecules diffuse (or passthrough) a membrane covering a set of electrodes. The oxygen ‘molecules react with an internal filling solution to develop a small electrical charge between the clectrodes which can be read on a meter. The readings on the meter correspond directly to the ‘amount of DO preseat in the sample, ‘Sampling: Samples are o be analyzed immediately. Samples willbe grab samples. ‘Samples must be representative, Sampling location where mixing is through andthe wastewater is ‘uniform. ‘Sampling should be done at the same time of each day. ‘Sample Containers: Grab samples in gla 300-ml BOD bottles with stoppers. BOD botts should be washed thoroughly with soap and water, rinse well with tap water, then a final rinse Gx) with distilled water, Equipment & Apparatus: DO meter DO electrode (probe) Electrode membrane kit BOD bottes, 300-ml Reagents: ‘The addition of an excess of sodium sulfite (Na2S03), and a trace of cobalt chloride (CoCI2) to distilled water ina full 300-ml BOD bottle will yield a sample with zero DO. Calibration: ‘The probe must be ar calibrated before each use Shake of excess watec/condensation ftom the probe. Wait $ mimes. ‘Check barometer for atmospheric pressure reading (mm Hg). ‘Off of char find the calibration value forthe pressure reading ‘Check temperature (°C) of air in BOD bottle containing 50-ml of distilled water. (Off of char find the value for DO at 100% humidity t that temperature. Maliple ppm DO value time pressure value to find value to calibrate the meter to. Pressure calibration value x ppm DO value = value to calibrate the meter to. ‘To enter the value into the DO meter: ‘Turn the kncb ofthe DO meter to “CALIBRATE”. Push “SKIP, the meter thin will show “CALIBRATE IN MG/L?” Push “CONFIRM”, the meter will show “ENTER CAL VALUE” “LAST = 8.xx MG/L” Push “t" or “Wand hold button until the calibration value is shown. Push “CONFIRM, the meter will show “CALIBRATED TO 8.xx”. ‘Turn the kncb to O2/TEMP. Calibration is complete. Refer to manufacturer’ instructions located in the laboratory. Atmospheric Pressure Chat: mmiie Calibration value mmHg Calibration value 168 L010 745 0,980 188 1.005 71 0975 160 1.000 BI 0970 156 0.995 Ba 0.965 152 0.990 70 0.960 188 0.985 DOMTemperature Chat: ‘Temp2C — ppmDO ‘Temp.2C — ppmDO 18.0) 9.50 240 850 185 9.40 245 8.45 190 9.30 250 840 195 9.25 23.5 830 200 9.20 260 820 205 9.10 265 als 210 9.00 270 810 215 8.90 215 8.00 20 880 280 790 25 875 285 785 20 870 20 780 238 860 16 ‘Reporting Data: ‘There are no calculations for this method. The DO concentration is read directly from the meter. aoc: A laboratory control sample and duplicate sample is run each analysis or every 10 samples, Whichever is more frequent. Refer tothe Quality Manual Interferences: ‘There are very few substances which will interfere with the DO method when utilizing the ‘lectrometic meter. Salinity caused by dissolved inorganic salts (such as industrial or ‘manufacturing processes) can influence the probe's readings. Reactive compounds and gases (like hydrogen sulfide and other sulfur compounds) can interfere with the eading by reducing probe sensitivity. Chlorine residual can create a positive interference. Biochemical Oxygen Demand, BODS (Standard Methods 18" ed. 5210 B.) In the presenve of free oxygen, aerobic bacteria use the organic matter found in wastewater as “food”. The BOD test isan estimate ofthe “food” available in the sample. The more “food” present in the waste, the more Dissolved Oxygen (DO) will be required. The BOD test measures, the strength cf the wastewater by measuring the amount of oxygen used by the bacteria as they stabilize the organic matter under controlled conditions of time and temperature, ‘The BOD tes is used to measure waste loads to treatment plants, determine plant efficiency Gin temas of BOD removal) , and conto plant processes. Iti also used to determine the effects of discharges on receiving waters. A major disadvantage ofthe BOD tests the amount of time (5 days) required to obtain the results. In many biological treatment plants, the facility effluent contains large numbers of nitrifying ‘organisms which are developed during the treatment process. These organisms ean exert an ‘oxygen demand as they convert nitrogenous compounds (ammonia and organic nitrogen) to more stable forms (nitrites and nitrates). At least pat ofthis oxygen demand is normally messured in @ five day BOD. Sometimes itis advantageous to measure just the oxygen demand exerted by organic (aronaceots) compounds, excluding the oxygen demand exerted by the nitrogenous compounds. To accomplish this, the ntifying organisms can be inhibited from using oxygen by te addition of nitifcation inhibitor to the samples. The results termed “Carbonaceous Biochemical Oxygen Demand”, or CBOD. This method is appropriate forthe analysis of ‘wastewater. An aliquot of sample is placed into a BOD bottle containing aerated dilution water. The DO content is determined and recorded and the botle is incubated inthe dark of five days at 20°C. At the end ofthe five days, the final DO content is determined and the difference between the 1 DO reading is calculated. The decrease in DO is corrected for sample dilution and represents the biochemical oxygen demand ofthe sample. ‘Sampling: ‘Samples can be either grab or composite. Composite samples are taken of influent and effluent ‘wastewater a the treatment plantas specified by the NPDES permit. Samples are taken at points ‘where they ate well-mixed and proportional tothe amount of the flow. ‘Sample Preservation: ‘Testing should be started as quickly as possible. During compositing, samples will be stored at ‘or near 4°C in plastic containers. These containers will be of adequate volume in proportion to the plant flow and sample aliquot volume. Samples may be Kept for no more than 48 hours before beginning the BOD test. The 48 hours starts when the very first aliquot of a composite is colleted. ‘Sample storage containers should be cleaned thoroughly between samples. Itis recommended that they be acid cleaned on a regular basis to prevent residue buildup which occurs overtime. Each sampling point should have its own storage container. Containers should be clean and dry before a new set of composite samples are stored in them. Pretreatment of Samples: ‘Samples with extreme pH values and samples containing disinfectants such as residual chlorine ‘must be treated prior to testing. ‘Samples which have pH values higher than 7.5 or lower than 6.5 must be neutralized to ap Iherween 6.5 and 7.5 before this test is performed. Neutralized samples mus be seeded forthe BOD test. Reagerts: Phosphate buffer solution: Dissolve 8.5 g KH2POS , 21.75 g K2HPO4, 33.4 g Na2HPO4 * 7H20, and 1.7 g NH4CI in about 500 ml distilled water and dilute tolL, The pH should be 7.2 without further adjustment. Discard reagent (or any ofthe following reagents) ifthere is any sign of biological growth inthe stock bottle Magnesium sulfate solution: Dissolve 22.5 g MeSO4 *71120 in distilled water and dilute to 1 L. Calcium chloride solution: Dissolve 27.5 g CaCI? in distilled water and dilute to IL. Ferric chloride solution: Dissolve 0.25 g FeC13*6H20 in distilled water and dilute to IL. Sodium hydroxide solution: Dissolve 40 g NaOH in distilled water and dihte to 1 L, (IN concentration) Sulfuri act solutio ‘Add 28 ml 1o 1 Lof distilled water and mix. {1'N concentration) Sodium sulfite solution: Dissolve 0.1575 g Na2S03 in 100 mi distilled water. This solution is not stable. Prepare daily Nitvification inhibitor: _2-chloro-6-(tichloro methyl) pyridine. Bought from Fisher ‘Scientific or Hach, Glucose-glutamic acid solution: Dry reagent-grade glucose and reagent-grade glutamic acid ‘at 103°C for | hour. Add 150 mg glucose and 150 mg 19 glutamic acid to distilled water and dilute to 1 L. Prepare fresh immediately before use. This can also be purchased from Fisher Scientific. Ammonia chloride solution: Dissolve 1.15 g NH4CI in about 500 ml of distilled water, adjust pH to 7.2 with NaOH solution, and dilute to 1 L. Solution contains 0.3 mg Nim. BOD Seed: Commercially bought ‘Preparation of Dilution Water; Using a3 Lot larger bottle, add I ml of each phosphate buffer, magnesium chloride, calcium chloride and fei chloride solutions per iter of distilled, deionized water. The pH of dilution the water should be around 7.00. Adjust with IN NaOH or H2SO4 solutions if necessary. ‘Saturate with DO before using by vigorously shaking the dilution water bottle or by aerating. ‘The DO should be approximately 8 mg/L. at room temperature. Store at 20°C in a dark area such as the BOD incubator or in a cabinet. tis very important thatthe distilled water used for dil contaminants such as copper and chlorine which could i water be of high grade and fre from bit the growth of bacteria ‘Equipment: BOD bottles, 300 ml with stoppers and water seal caps. DO meter with probe. Incubator: sir, thermostatically controlled at 20 1°C. Exclude all light to prevent possibility of photosynthetic production of DO. Graduated cylinders, various capacities. Pipets, various capacities Pipet bulb Magnetic ster and sirng bars pH meter and probe Dilton water ote, 3 oF larger Brette graducted to 0.1 ml 250 ml Eclenmeyer flask Determination of Sample Size: ‘The BOD test relies on a measurable depletion of DO over a 5 day period of time. Because most samples of wastewater willhave a BOD higher than the amount of oxygen available inthe BOD bottle during the incubation period, the samples must be diluted. This dilution is done by adding

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