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LABORATORY MANUAL

P.T. BUDI ACID JAYA

Ketapang, Indonesia

This document is the property of GLOBAL WATER ENGINEERING (GWE) Ltd. and GmbH, Hong Kong & Germany. It shall not be copied, reproduced, transmitted or communicated to third parties without the explicit agreement of GLOBAL WATER ENGINEERING. International Conventions of Berne (1886) - Paris (1896) Berlin (1908) Berne (1914) Rome (1928) Brussels (1948) Stockholm (1967) Paris (1971). Universal Copyright Convention of Geneva (1952) Paris (1971).

Rev. 0

08 May 2008

PROJ. No.3460

LUDSTADT, GERMANY

May 08, 2008

LABORATORY ANALYSIS MANUAL

CLIENT:

PROJECT:

WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
1/20

: Patrick Enriquez

LABORATORY ANALYSIS Analytical and Test Procedures Following procedures are generally used by GLOBAL WATER ENGINEERING (GWE) for the determination and analyses of different process operation parameters to monitor and operate the Wastewater Treatment Facilities. For more information we also recommend to refer to the Standard Methods for the Examination of Water and Waste Water by the American Public Health Association (APHA). Chapter

1 2 3 4 5 6

Suspended Solids (TSS, SV, TSSV, SVI) Volatile Fatty Acids (VFA) Chemical Oxygen Demand (COD) Biochemical Oxygen Demand (BOD) Standard Sludge Activity Test (SAT) Alkalinity Test

Date
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Laboratory Analysis

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WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
2/20

: Patrick Enriquez

1.

SUSPENDED SOLIDS 1.1 Total Suspended Solids (TSS) 1.1.1 Objective: To determine and quantify the amount of undissolved particulate sample. 1.1.2 Laboratory Equipment and other materials Perforated porcelain funnel (also known as Bchner funnel), 3 pcs (100 mm diameter) Rubber stopper/adaptor, 6 pieces 250-ml Erlenmeyer flask with side tubulation, 6 pieces General purpose oven, ca. at least 4 ft3 capacity, 30 150oC, 1 unit Portable vacuum pump, 1 unit Petri dishes 60 mm, 10 pieces Analytical balance (Ohaus Explorer), 1 unit Glass Desiccator ( 250 mm) with plate, 1 set Desiccator gel, 1 pack Silica gel grains with indicator, 1 kg Laboratory smooth tip filter forceps, 2 pieces Thick-walled rubber tubing ( 7 mm), 3 m Tongs, 2 pieces Membrane filters or glass microfiber filters, 600 pieces, 90-mm diameter 1.1.3 Chemical reagents 1.1.4 None matter in a

Note: The Total Suspended Solids (TSS) can be measured by two methods: A) by Filtration (using vacuum pump, evaporating dish or crucible paper) B) by Centrifuge and filter

1.1.5

Frequency of Analysis - Twice or thrice per day (once per shift)

Date
08/05/2008

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LABORATORY ANALYSIS MANUAL

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WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
3/20

: Patrick Enriquez

1.1.6

Procedure: A.1 By Filtration using evaporating dish or crucible A.1.1 Determine the dry solids content of the unfiltered sample. Follow procedures for the Dry Solids Determination. A.1.2 Filter a known volume of sample, usually 15-20 ml is required, into a filter paper (Whatman GF/C or Scheel SS No. 595 or equivalent) A.1.3 Transfer the filtrate into a pre-weighed dish. A.1.4 Determine the dry solids of the dish with the filtrate sample. Follow procedure for the Dry Solids Determination. A.1.5 Calculate for the TSS using the formula: TSS (g/l) = DS sample (g/l) - DS filtrate or supernatant (g/l) A.2 By Filtration using filter paper A.2.1 Prepare filter paper (Whatman GF/C or Scheel SS No. 595 or equivalent) and heat it to 105C (5C) for one hour. A.2.2 After heating, store and cool filter paper in a dessicator (provided with dessicant). Record the weight of filter paper as X1. A.2.3 Pipette a measured volume of sample (ml), usually 15-20 ml, and pour into a pre-weighed filter paper including the washing done on the pipette. A.2.4 Dry the filter paper with sample in the drying oven at 105 C ( 5C) for at least one hour. A.2.5 Cool the filter paper with the dried sample in a dessicator. Record the weight as X2. A.2.6 Calculate the TSS using the formula: TSS (g/l) = (X2 - X1) * 1000 ml of sample B.1 By Centrifuge (Applicable for samples with high TSS and for sludge samples i.e. Anaerobic)

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LABORATORY ANALYSIS MANUAL

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WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
4/20

: Patrick Enriquez

B.1.1 Measure volume of sample (ml), usually 15-20 ml, and pour into a centrifuge vial. B.1.2 Centrifuge the sample at 2,000 g for 10 minutes. B.1.3 Discard the supernatant. B.1.4 Wash the residue with distilled water. Repeat washings three (3) times. B.1.5 Transfer the residue into a pre-weighed evaporating dish where the weight is labeled as (X1). B.1.6 Determine the dry solids content of the sample. Follow procedures for dry solids determination. Record weight as (X2). B.1.7 Compute for TSS using the formula: TSS (g/l) = (X2-X1) * 1000 ml of sample 1.2 Total Settleable Suspended Solids (SV, TSSS, SVI) 1.2.1 Objective To determine and quantify the amount of settleable suspended solids in a sample. 1.2.2 Laboratory Equipment and other materials 1.2.3 Analytical balance (Capacity 100 g; Readability = 0.0001 g) Temperature control drying oven (30 - 220C) Crucibles with cover 25-ml capacity Evaporating dish 25-ml capacity Hot plate Crucible tong with Teflon tip Dessicator with dessicant Filtering apparatus Vacuum pump Filter paper (e.g. Whatman GF/C or Scheel SS No. 595 or equivalent) Imhoff cone with stand (Capacity = 1000 ml)

Chemical reagents None

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LABORATORY ANALYSIS MANUAL

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WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
5/20

: Patrick Enriquez

1.2.4

Note: The settleable suspended solids or sludge which are only part of the Total Suspended Solids (TSS), are determined after one (1) hour sedimentation (only half hour for aerobic sludge) of a mixed liquor sample (volume at 1000 ml) in a cone-shaped Imhoff flask.

1.1.5

Frequency of Analysis - Twice or thrice per day (once per shift)

1.2.6

Sludge Volume or Solids Settling Volume (SV) 1.2.5.1 1.2.5.2 1.2.5.3 1.2.5.4 Fill the Imhoff cone with a well-mixed sample up to 1000 ml mark. Gently agitate with stirring rod the sample near the sides of the cone. Allow the sludge (anaerobic) or solids to settle for one hour. Record the volume of the sludge or solids that have settled down in the cone. If the sludge consists of settling and floating layers, both layers should be measured. Express SV results as: SV (ml/l) = Total volume of sludge (settling + floating) 1000 ml sample

1.2.5.5

1.2.6.

Concentration of Settleable sludge (g/l sludge) is determined from the difference between dry solids content of the supernatant liquid and of the settled sludge. 1.2.6.1 Determine the dry solids content of the settled sludge. Follow procedure for the dry solids determination. The dry solids content of the settled sludge should be labeled X3. Determine the dry solids content of the supernatant liquid. Follow procedure for the dry solids determination. The dry solids content of the supernatant liquid should be labeled X4. Calculate for the total settleable suspended solids (TSSS) expressed as:

1.2.6.2

1.2.6.3

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LABORATORY ANALYSIS MANUAL

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WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
6/20

: Patrick Enriquez

TSSS (g/l) = X3 - X4 1.2.7. Sludge Volume Index (SVI) - gives the relation between the volume of the sludge (SV) and the concentration of the sludge (TSSS) SVI (ml sludge/g sludge) = SV TSSS 1.3 Volatile (or Volatizable) Suspended Solids (VSS) 1.3.1 Objective To determine and quantify the amount of Volatile Suspended Solids in a sample and to assess the growth of bacteria in the sludge (organic matter fraction present in the sludge). 1.3.2 Laboratory Equipment 1.3.3 All equipment for TSS determination Muffle type furnace (maximum temp. 1100C)

Chemical Reagents and other materials NONE

1.3.4

Procedure 1.3.4.1 1.3.4.2 Follow the procedure for TSS analysis. Record the value of X2 (refer to TSS analysis section). After analyzing the TSS of the sample, place the dish or crucible with the sample for four hours in a muffle furnace having a temperature of 650C (5C). Cool the dish or crucible with the sample in the dessicator and weigh. The weight should be labeled as X3.

1.3.4.3

Calculate the TSS using the formula: Note: When doing method of filtration using evaporating dish or crucible, suspended ash is taken as the difference below the unfiltered sample and the filtrate. VSS (mg/l) = (X2 - X3) x 1,000,000 ml of sample

Date
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LABORATORY ANALYSIS MANUAL

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WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
7/20

: Patrick Enriquez

1.3.5

Frequency of Analysis - Once per week during start-up/twice per month during normal operation

1.4

Volatile Settleable Suspended Solids (VSSS) 1.4.1 Objective To determine and quantify the amount of Volatile Settleable Suspended Solids in a sample. 1.4.2 Laboratory Equipment 1.4.3 All equipment for TSSS determination Muffle type furnace (maximum temp. = 1100C)

Chemical Reagents and other materials NH4NO3 solution (10%)

1.4.4

Procedure 1.4.4.1 Determine the Total Settleable Suspended Solids (TSSS) of the sample. Follow procedure for Total Settleable Suspended Solids Determination. Determine the Settleable ash of the sample. The settleable ash should be the difference between the ash content of the settled sludge and the supernatant liquid. This is determined in the same way as Settleable Suspended Solids (TSSS) where however, the dried samples are ashed prior to weighing. Follow procedure for the Ash Determination. Calculate for the Volatile Settleable Suspended Solids (VSSS), expressed as: VSSS (g/l) = TSSS - Settleable Ash

1.4.4.2

1.4.4.3

1.4.5

Frequency of Analysis - Once per week during start-up/twice per month during normal operation

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LABORATORY ANALYSIS MANUAL

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WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
8/20

: Patrick Enriquez

2.

VOLATILE FATTY ACIDS (VFA) 2.1 Objective To provide information concerning the anaerobic degradation of organic matter and the environmental conditions best suited for optimum activity of the methane-producing bacteria. 2.2 Principle Volatile Fatty Acids and alcohol can be distilled by means of steam distillation in acid medium usually until pH 2 to 3. The result of the pH reduction is that bi-carbonate (HCO3-) is converted to CO2 gas and the fatty acids are transformed into their nondissociated form (molecules) in solution. Hereafter, the sample is boiled to expel CO2 gas while the fatty acids remain in the solution. The sample is cooled and titration is carried out with NaOH and phenolphthalein. 2.3 Methods 2.3.1 2.3.2 2.3.3 2.4 Using Steam Distillation: (Kjeltec Steam Distillation Apparatus) and Titration Using Direct Heating / Distillation and Titration Using Simple Titration

Laboratory Equipment and other materials 2.4.1 Steam Distillation Method and Titration Kjeltec Steam Distillation unit with its accessories (also used for TKN), 1 set Erlenmeyer flasks, 250 ml capacity, 10 pieces Erlenmeyer flasks, 500 ml capacity, 10 pieces Hot plate with stirrer, heating surface 16 in2 Iron stand with double sided titration clamps, 1 set Titration burettes (5 ml and 10 ml capacity, 4 pieces each) Anti-bumping beads (1 pack)

2.5

Chemical Reagents 2.5.1 Steam Distillation and Titration phenolphthalein C20H14O4 indicator 100 ml (or phenolphthalein C20H14O4 100 g , 95% ethanol CH3CH2OH solution 1 L) Concentrated Sulfuric acid H2SO4, 4 L 0.1 N Sodium Hydroxide NaOH solution (standardized), 4 L

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LABORATORY ANALYSIS MANUAL

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PROJECT:

WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
9/20

: Patrick Enriquez

2.6

Procedure 2.6.1 Steam Distillation Method 2.6.1.1 Bring 50 ml waste water sample into the Kjeltec digestion tube. 2.6.1.2 Add 5 ml concentrated H3PO4 or H2SO4 to bring the pH to 2. 2.6.1.3 The steam distillation is carried out with a Kjeltec distillation apparatus (Follow the distillation procedures in the Kjeltec manual). 2.6.1.4 During distillation, the first 15 ml is discarded. 2.6.1.5 Collect 300 ml distillate in a 500 ml Erlenmeyer flask. 2.6.1.6 The total distillate is boiled for about 3 min. in a Pyrex Erlenmeyer flask to expel the dissolved CO2. Use anti-bumping beads to prevent bumping. 2.6.1.7 After cooling, 5 drops of phenolphthalein are added and the distillate is titrated with 0.1 N NaOH. 2.6.1.8 Titration is carried out until the sample shows a persistent pale or light pink. 2.6.1.9 Calculation of the VFA concentration: The amount of VFA is expressed as mg acetic acid/l sample. mg CH3COOH/liter = ml NaOH x N titer NaOH x 60 x 20 where: ml NaOH = N titer = 60 = 20 = ml of titer used 0.1 N NaOH molecular weight of acetic acid (CH3 COOH) multiplication factor to know the amount of VFA in 1 liter.

2.6.2.10 Calculation of the VFA concentration: VFA expressed as mg CH3COOH = ml NaOH used x N titer NaOH x 60 100 ml sample / 1 liter 1000 ml

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LABORATORY ANALYSIS MANUAL

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WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
10/20

: Patrick Enriquez

2.7 Frequency of Analysis - Twice or thrice per day (once per shift)

3.

CHEMICAL OXYGEN DEMAND (COD) 3.1. Objective The Chemical Oxygen Demand (COD) test is widely used as a means of measuring the organic strength of municipal and industrial wastes. 3.2. Principle The chemical oxygen demand (COD) determination provides a measure of the oxygen equivalent of that portion of the organic matter in a sample that is susceptible to oxidation by a strong oxidant. Therefore the organic matter is destroyed by a mixture of chromic and sulfuric acid. The excess amount of potassium dichromate is measured by backtitration. 3.3. Laboratory Equipment and Glassware COD reflux apparatus consisting of 250 ml Erlenmeyer flask with ground-glass 24/40 neck (Corning Brand), 6 pieces 300 mm jacket (Liebeg, Corning 2360), West or equivalent water cooled condenser with 24/40 ground-glass joint, 6 pieces Hot plate with sufficient power to produce at least 1.4 W/cm2 (can accommodate at least 6 of 250 ml Erlenmeyer Flasks), 1 unit 50 ml glass beakers, 10 pieces 250 ml capacity Erlenmeyer flask, 10 pieces 50 ml capacity automatic/self zeroing titration burette with 1 liter glass bottle (amber color) reservoir including rubber bulb, 1 set 1000 ml capacity reagent bottles (amber color), 6 pieces Rubber aspirator, 3 pieces Reagent spatula, 3 pieces Volumetric Dispensers (plunger type, e.g. Optifix Brand), 2 pieces 3.4. Reagents 3.4.1 Standard potassium dichromate solution 0.25 N : dissolve 12.259 g K2Cr207, primary standard grade, previously dried at 103C, in 1000 ml distilled water. Sulfamic acid is added (240 mg/l) to avoid eventual interference of nitrites.

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LABORATORY ANALYSIS MANUAL

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WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
11/20

: Patrick Enriquez

Standardization: Pipette 10 ml standard K2Cr2O7 Add 10 ml distilled water, 3g KI, 2g NaHCO3 Add 5 ml HCl slowly while swirling Store mixture in a dark place for 5 minutes Titrate against 0.1N standard Na2S2O3 N K2Cr2O7 = 3.4.2 Sulfuric acid reagent Concentrated H2SO4 containing 10g Ag2SO4/l is prepared. One to two days are required for the complete dissolution of the Ag2SO4. 3.4.3 Standard ferrous ammonium sulfate solution 0.10 N : dissolve 39.2 g Fe (NH4)2 (SO4)2.6 H2O in distilled water. Add 20 ml of concentrated H2SO4 and dilute to 1.0 liter. The titer of this solution must be determined daily against the standard potassium dichromate solution. Standardization: Dilute 10 ml standard K2Cr2O7 to about 100 ml with distilled water Add 30 ml concentrated H2SO4 , cool Titrate with standard Ferrous Ammonium Sulphate (FAS) solution using 2-3 drops (0.10-0.15 ml) Ferroin indicator. N FAS = Vol. of K2Cr2O7 * N of K2Cr2O7 Volume of titer 3.4.4 Ferroin indicator solution Dissolve 1.485 g of 1, 10-phenanthroline mono-hydrate and 695 mg of FeSO4.7H2O in 100 ml water. 3.4.5 Mercuric sulfate Addition of 0.4g HgSO4 is enough to complex all the chlorides as HgCl42-, at concentrations below 2000 mg/l. For higher chloride concentrations, dilution of the sample or addition of a higher amount of HgSO4 is required. N Na2S2O3 * Volume of titer 10 ml

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LABORATORY ANALYSIS MANUAL

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WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
12/20

: Patrick Enriquez

3.5

Procedure 3.5.1 Put 0.4g HgSO4 in a digestion flask. Add 20.0 ml sample, or an aliquot diluted to 20.0 ml with distilled water and mix. See Table. Volume of Sample Distilled Water (ml) (ml) Blank 0 20 UASB Influent 2 18 UASB Effluent 10 10 Final Effluent 20 0 Note : The diluted sample should have a COD between 0 and 700 mg/l. 3.5.2 Add : 10 ml K2Cr207, 0.25 N 30 ml H2SO4 + Ag2SO4 solution Swirl thoroughly after adding the acid while cooling the solution using running tap water. Keep the distillation flask slightly inclined while adding the acid and also while swirling and cooling. Caution: Mix reflux mixture thoroughly before applying heat to prevent heating of flask bottom that could result to sudden cracks of the flasks and a possible blowout of flask contents. 3.5.4 3.5.5 3.5.6 3.5.7 3.5.8 3.5.9 Make a blank sample i.e. 20 ml of distilled water and prepare it with the same chemicals. Provide the flasks with water cooled condensers. Bring the flasks with samples in the heating mantle. Cover the open end of the condensers with a small beaker to prevent foreign materials from entering the refluxing mixture. Re-flux the samples for 2 hours at 150C. Let it cool and rinse the condenser with approximately 20 ml of distilled water. Titration is carried out in the 250 ml Erlenmeyer flask. Titrate the excess dichromate with standard Fe(NH4)2(SO4)2.6H2O) using 0.5 ml Ferroin as indicator. Sample

3.5.3

3.5.10 Take as the end point the sharp color change from blue-green to reddish brown, even though the blue-green may reappear within a few minutes.

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LABORATORY ANALYSIS MANUAL

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Ketapang, Indonesia
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13/20

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3.5.11 Calculation mg/l COD = (a - b) N x 8000 ml sample where: a = ml Fe (NH4) 2 (SO4)2 used for the blank b = ml Fe (NH4) 2 (SO4)2 used for the sample N = normality of Fe (NH4)2 (SO4)2 Remarks: A distinction is made between: CODs : CODt : CODss : Note: To evaluate the accuracy of procedure and quality of reagents with standard KHP solution. % Recovery = Actual COD of KHP solution Theoretical COD of KHP solution Theoretical COD of KHP solution: 1 Liter solution = 500 mg/l COD For better COD results, % Recovery should be more than 1.0 3.6. Frequency of Analysis - Twice or thrice per day (once per shift) soluble COD, determined on a centrifuged or filtered sample total COD, determined on the total sample suspended solids COD: CODss = CODt - CODs

4.

BIOCHEMICAL OXYGEN DEMAND (BOD) 4.1 Introduction The biochemical oxygen demand determination constitutes an empirical test, in which standardized laboratory procedures are used to determine the relative oxygen requirements of the sample. Comparison of BOD-values may not be made unless the results have been obtained under identical test conditions.

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PROJECT No: BY

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Ketapang, Indonesia
HONGKONG MANILA

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14/20

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4.2

Method for the Determination of the BOD by OxiTop Control 4.2.1 Principle

OxiTop systems, offers a unique, modular and mercury-free instrument system. It is not only suitable for BOD determination, but also for measuring biodegradability and deple-tion. The advantages of OxiTop and OxiTop Control: simple operation, improved controllability and non-toxicity, and measuring ranges of up to 400 000 mg/l BOD (with OxiTop Control OC 110). As the measured pressure is automatically converted the values can be directly read as mg/l BOD.
4.2.2 Laboratory Equipment and Glassware

BOD auto-check measurement systems OxiTop Control, 6 measuring points, 1 unit consists of OxiTop BOD controller OxiTop measuring heads inductive strirring system, sample bottles stirring bars Sodium Hydroxide NaOH pellets rubber sleeves 164 ml and 432 ml overflow measuring flasks nitrification inhibitor Thermostatic cabinet (temperature range from 4 to 40oC) 180 liters, 1 unit 4.2.3 Reagents

Di-potassium hydrogen phosphate K2HPO4, 500 g Potassium dihydrogen phosphate KH2PO4, 250 g Magnesium sulfate heptahydrate MgSO4.7H2O, 500 g Iron (III) chloride hexahydrate FeCl3.6H2O, 250 g Calcium chloride dehydrate CaCl2, 1 kg Ammonium chloride NH4Cl, 500 g 4.3 Frequency of Analysis - Once or twice per week

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WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
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15/20

: Patrick Enriquez

5.

STANDARD SLUDGE ACTIVITY TEST (SAT) 5.1 Objective: 5.1.1 5.1.2 5.1.3 To determine the activity of the sludge through the rate of biogas production in function of time. To calculate initial COD loading of conditioned wastewater into the MUR. To evaluate or assess the presence of toxic substances and inhibition of the methane bacteria.

5.2 Procedure: 5.2.1 Collect a representative sample of digested sludge in a 2.0-liter Erlenmeyer flask. Store sample for about 24 hours at 35C (e.g. in a heated room, in an oven or incubator at 35C, or in a hot water bath). Analyze sludge sample for the following analyses: - Sludge settling Volume (SV) - pH and Temperature - Initial VFA 5.2.3 5.2.4 Take 500-ml sludge sample into a 1.0-Liter Erlenmeyer flask. Add 500 ml distilled water. Stir the mixture with a stirring rod or in a magnetic stirrer. Test substrate to be added to sludge sample: - 4.69 g Glacial Acetic acid (HAC) or 1.28 g anhydrous Sodium acetate (NaAC), equivalent to 5.0 g COD. or - Raw waste water, equivalent to 5.0 g COD or - Suspected toxic substances, equivalent to 5.0 g COD 5.2.5 5.2.6 Stir while neutralizing the sludge mixture to pH 7.0 with 1.0 N NaOH. Connect the Erlenmeyer flask according to the illustration:

5.2.2

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a. Close Erlenmeyer flask with a rubber stopper. Note: Preferably after flushing the headspace with N2 (nitrogen) gas. Put the Erlenmeyer flask on a magnetic stirrer, in a heated room or incubator at 35C. Allow to stir gently as possible, just to keep the sludge in suspension. b. Let the gas bubble through a NaOH solution (10%) to absorb CO2. Methane gas is not absorbed. c. Collect the gas in a graduated measuring cylinder of 2.0 1 or more. The cylinder is placed in a container with acidified tap water (+ HCl or H2SO4 until pH 2.0). 5.2.7 Monitor and record the methane gas production by measuring the water displacement. Start in the morning, follow the methane gas production till the evening, and continue the next day. Put the results in a graph as follows :

5.2.8

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LABORATORY ANALYSIS MANUAL

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Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
17/20

: Patrick Enriquez

5.2.9

Express the max. gas production rate during phase 3) as : l CH4/l sludge.d Convert methane volume to volume at 0C, 1.013 bar; normally this comes to multiplying with 0.9, when the gas temperature in the gas cylinder is : 25C (0.9) = 273 273 + 25

Nl CH4/l sludge.d (Nl : normal liter) Since production of 0.350 Nl CH4 corresponds to 1.0 g COD removed, express sludge activity (by multiplying with 1/0.35) as: g COD removed/l. sludge.d Measure the sludge concentration (TSS and VSS), and express the result per g VSS sludge: g COD removed/g VSS.d or COD rem./g TSS.d

Date
08/05/2008

DESCRIPTION
Laboratory Analysis

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LUDSTADT, GERMANY

May 08, 2008

LABORATORY ANALYSIS MANUAL

CLIENT:

PROJECT:

WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
18/20

: Patrick Enriquez

5.2.10

Interpretation of the results digested municipal sludge 0 -0.05 g COD removed/g VSS.d 0.05 - 0.10 0.1 - 0.2 > 0.2 methanogenic sludge from MUR 0.5 g COD removed/g VSS.d 0.5 - 1.0 > 1.0 : : : poor sludge average sludge good sludge : : : : very poor sludge poor sludge average sludge good sludge

The sludge activity (g COD rem./g VSS.d) reflects the sludge-loading rate, which can be applied during start-up. 5.3 Laboratory Equipment and other materials Erlenmeyer flask, 1 L, 1 piece Measuring cylinder, 1 L, 1 piece Thermometer 10/110C, 2 pieces Magnetic stirring bar, 5 pieces Rubber stopper fit for 100 ml Erlenmeyer flask, 1 pieces Rubber stopper fit for 1 L Erlenmeyer flask, 1 pieces Cork borer, 1 piece Glass tube 7 mm, 6 length, 4 pieces Silicone rubber tubing ( 7 mm), 1.4 m Retort stand base 300 x 150mm, 1 piece Support rod, 1000 mm, 1 piece Rod clamp, 1 piece Support ring with bosshead 100mm, 1 piece 5.4 Frequency of Analysis Will be determined by the number of possible toxic compounds in the wastewater during biological start-up

Date
08/05/2008

DESCRIPTION
Laboratory Analysis

REV
0

BY
PE

CHD

LUDSTADT, GERMANY

May 08, 2008

LABORATORY ANALYSIS MANUAL

CLIENT:

PROJECT:

WASTEWATER TREATMENT
PROJECT No: BY

BUDI ACID JAYA

Ketapang, Indonesia
HONGKONG MANILA

PLANT 3460
Process Engineer

SHT
19/20

: Patrick Enriquez

6.

ALKALINITY TEST 6.1 Objective 6.1.1 6.1.2 6.1.3 To determine the acid-neutralizing capacity of a wastewater sample, expressed as mg CaCO3/L. To estimate the acceptable VFA concentration suitable for the type of wastewater. To evaluate or assess toxicity effect brought by certain high concentration of VFA. Target VFA/Alkalinity ratio inside the methane reactor is 0.30. 100 mL beaker Iron stand with base Iron clamp 25 ml burette Stir plate with magnetic stirrer (optional) Portable pH meter

6.2

Objective -

6.3

Reagents 0.1 N H2SO4 solution 0.1 N NaOH solution

6.4

Procedure Prepare 50 mL of wastewater sample into a 100 mL beaker. Indicate pH start of sampling then titrate it with 0.1 N H2SO4 until pH 4.0. Record mL of H2SO4 from pH start to pH 4.0. Then titrate until pH 3.3 3.5. Boil the sample for 3 minutes. After 3 minutes, wait for the sample to cool to room temperature. Then, titrate with 0.1 N NaOH until pH 4.0. Titrate again until pH 7.0 (Record the mL of 0.1 N NaOH from pH 4.0 to pH 7.0).

VFA= ml NaOH (pH 4.0-7.0) x N NaOH x 50,000 ml sample if VFA > 180 mg/l, then multiply the value by 1.5 Alkalinity = ml H2SO4 (pH start-pH 4.0) x 2,500 ml sample

Date
08/05/2008

DESCRIPTION
Laboratory Analysis

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PE

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