Procedure for Analysis of Treated Effluent

• Objective:To lay down a Laboratory procedure for the analysis of Treated Effluent.

• Scope:This standard operating procedure is applicable for formulation plant of pharmaceutical company.

• Responsibility: ETP chemist shall be responsible for testing of Treated Effluent.
• COD :  Chemical Oxygen Demand
• D.O :Dissolved Oxygen
• FAS : Ferrous Ammonium Sulfate
• BOD : Biochemical Oxygen Demand
• Abbreviations & Definitions:
• Accountability:Head-Engineering and QA shall be accontable for compliance of the SOP.
• Procedure
  • Biochemical Oxygen Demand
    • Apparatus:
      • BOD bottles
      • BOD Incubator
• Prepare reagents as per SOP titled “Preparation and Handling of Solutions in ETP Laboratory”, Annexure-I.
• Mix the solution by inverting bottle few times and allow settling the precipitate.
• Add 2 ml MnSO₄ solution and 2 ml of alkali azide solution to the sample collected in 300 ml BOD bottles.
• Determination of Dissolved Oxygen:
• Determine the D.O content of another bottle immediately.
• Keep one bottle for 3 days in the incubator at 27°C and determined its D.O. after three days.
• Fill two BOD Bottle (300 ml each).with the above solution.
• Take suitable portion of sample in a volumetric flask and dilute to one litre with dilution water. Mix thoroughly.
• Adjust pH of the dilution water to 7.0 by using NaOH or HCl.
• Add 1 ml each of phosphate buffer, Magnesium sulphate, Calcium Chloride and Ferric Chloride solution for each litre of dilution water and mix thoroughly.
• Prepare dilution water in a glass container by bubbling compressed air in distilled water for about 2 hrs.
• Similarly for blank, take 2 bottles for dilution water .determine D.O.content of one bottle immediately and determine the D.O. of another bottle after 3 days incubation (27°C)
• Titrate 200 ml of the above solution with 0.025 N sodium thiosulphate using starch indicator.
• Then add 2 ml of conc. H₂SO₄ to dissolve precipitate.Restopper the bottle and mix by inverting bottle few times.
• Calculations:
•  BOD mg/litre=           (D1-D5) – (B1-B5)  _/ % of Sample
• Where,
• D1= ml of 0.025N sodium thiosulphate consumed by sample
• D2= 0.025 N sodium thiosulphate consumed after incubation of sample
• B1= ml of 0.025 N sodium thiosulphate consumed by blank
• B2= ml of 0.025 N sodium thiosulphate consumed by incubation of sample.

• Chemical Oxygen Demand
• Apparatus
• Reflux Condenser
• ml flat bottomed flasks with standard joint
• Heating mantle (hot plate)
• Prepare reagents as per SOP titled “Preparation and Handling of Solutions in ETP Laboratory”, Annexure-1.
• Take 10 ml standard K₂Cr₂O₇ solution in flask. To that add 20 ml of sample or suitable portion. Make up to 200 ml with distilled water.
• Add 1g or a pinch of mercuric sulphate powder and several glass beads.
• Add 30 ml of sulfuric acid reagent with mixing to dissolve HgSO₄.
• Attach flask to the reflux condenser and turn on cooling water .Reflux for 1.5 to 2 hrs.

CAUTION:    Mix reflux mixture thoroughly before applying heat to prevent local heating of the flask bottom and a possible blowout of flask contents.

• Disconnect condenser and dilute mixture with 80 ml distilled water.
• Cool to room temperature and titrate excess K₂Cr₂O₇ with FAS, using 0.10to 0.15 ml ferroin indicator. End point is wine red colour.
• Calculations:
• COD as mg O2/L =     (A-B) X M X 8000   X dilution factor* / ml of sample
• Where, A = ml FAS used for blank
• B = ml FAS used for sample
• M = Molarity of FAS
• * = If sample is diluted

• Total Suspended Solids
• Apparatus
• Vacuum pump
• Filtration assembly
• Filtered discs
• Silica or Gooch crucible
• Glass Desiccator
• Insert disc with wrinkled side up in filtration apparatus and apply vacuum .Wash disc with reagent grade water.
• Take suitable amount of sample and filter it. Wash the filter paper with 10 ml reagent grade water and continue applying vacuum for about three min. after filtration is complete.
• Remove filter paper from filtration apparatus and carefully transfer to an aluminium disc as a support. Remove the crucible and filtration combination from crucible adapter if Gooch crucible is used.
• Dry at 103 to 105°C in an oven, cool in a desiccator to balance temperature and weigh. Repeat the cycle until a constant weight is obtained or weight change is less than 4%.
• Calculations:
• mg total suspended solids/L =   A-B x 1000 / ml of sample
• Where, A = Weight of filter + dried residue, mg, and
• B  = Weight of filter, mg.

• Then add 10 ml CCl₄, shake well and allow standing for 5 minutes. Repeat the procedure for 3-4 times i.e. add total 30-40 ml of CCl₄.
• Take 50 ml of sample in a separating funnel and add 2-3 ml conc. HCl.
• Weigh 100 ml silica or glass dish.
• Prepare reagents as per SOP titled “Preparation and Handling of Solutions in ETP       Laboratory”, Annexure- I.
•  Water bath
• Silica or Glass dish
• Filter paper
• Separatory funnel
• Apparatus
• Oil & Grease
• B  = Weight of Dish, mg.
• Where, A = Weight of Dried residue + Dish, mg, and
• mg total dissolved solids/L = A-B x 1000 / ml of sample
• Calculations:
• Transfer total filtrate(with washings) to a weighing evaporating dish and evaporate to dryness in a drying oven at 180° + 2°C,cool on desiccator and weigh. Repeat the cycle until a constant weight is obtained or weight change is less than 4%.
• Total Dissolved Solids
• Apparatus
• Filter discs
• Filtration Apparatus
• Membrane filtration funnel
• Gooch crucible
• Drying Oven
• Insert disc with wrinkled side up in filtration apparatus and apply vacuum .Wash disc with reagent grade water.
• Heat clean dish in an oven at 180°C, cool in a desiccator and weigh immediately before use.
• Take suitable volume of sample and filter. Wash with 30 ml reagent grade water allowing complete drainage.
• Take the lower layer through separating funnel in dish and discard the remaining part.
• Evaporate CCl₄ or Petroleum ether on water bath and take the final weight of dish after cooling in a desiccator.
• Calculations:
• Oil & Grease, mg/L =    (A-B) X 1000000  _/ V
• Where,
• A= final weight of dish in gram.
• B= Initial weight in gram.
• C= Volume of sample in ml.
• pH
• Apparatus:
• pH meter
• Beakers
• Prepare standard solution of 4.0,7.0 and 9.2 pH by using pH buffer tablets in 100 ml distilled water for each tablets.
• Operate pH meter as per SOP and standardize with standard pH buffer solutions.
• Determine the pH of the effluent at Different stages viz.Equilisation Tank (S1), Flash mixer (S2), Primary Clarifier (S3) and Treated water (S4).

NOTE: Standardize the pH meter with standard buffer solutions every day before Operation.

• Forms and Records
• Logbook For ETP Plant-Treated Effluent – Annexure-I
• Distribution
• Master Copy: Documentation Cell
• Controlled Copies : Engineering, Quality Assurance, ETP Laboratory

• History

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