Procedure for Analysis of Treated Effluent

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  • 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
Date Revision

Number

 Reason for Revision
– 00 New SOP

 

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