WASTE WATER HOLDING BHD.

Internship Report
Characterization of Sludge
Florian Michael Gehring & Mohd Farhan Ariff

1.02.2011
1

Inhalt
1. Introduction............................................................................................................3
2. Timetable................................................................................................................4
3. Experimental procedure.........................................................................................6
3.1. Total, Volatile and Fixed Solids.........................................................................6
3.1.1. TS...............................................................................................................6
3.1.2. VS, FS.........................................................................................................6
3.2. Total, Volatile and Fixed Suspended Solids......................................................7
3.2.1. TSS.............................................................................................................7
3.2.2. VSS, FSS......................................................................................................7
3.3. Sludge Volume Index........................................................................................7
3.4. Chemical Oxygen Demand (Preparation of the Stock Solution).......................8
3.5. Alkalinity (Preparation of the Stock Solution)..................................................8
3.6. pH..................................................................................................................... 9
3.7. Moisture...........................................................................................................9
4. Results and Discussion..........................................................................................10
4.1. Total, Volatile and Fixed Solids.......................................................................10
4.2. Total, Volatile and Fixed Suspended Solids....................................................11
4.3. Sludge Volume Index......................................................................................11
4.4. Chemical Oxygen Demand..............................................................................12
4.5. Alkalinity.........................................................................................................13
4.6. pH................................................................................................................... 15
4.7. Moisture.........................................................................................................16
5. Summary...............................................................................................................16
6. Problems...............................................................................................................17
6.1. Temperature...............................................................................................17
6.2. Oxygen........................................................................................................17
6.3. pH................................................................................................................ 17
6.4. Retention Time............................................................................................17
2

7. Proposal for solution.............................................................................................18

7.1. Tracer..........................................................................................................18
7.2. Is the sludge in the anaerobic digester hermetically sealed?......................18
7.3. Digester is overfilled...................................................................................18
7.4. Sludge is to inconstant................................................................................18
7.5. Problems with the temperature.................................................................18
8. References............................................................................................................18
3

1. Introduction
The Jelutong Sewage Treatment Plant is one ofthe biggest waste water treatment
plants, based on the SBR technology, all over the world. It was constructed on the
reclaimed land (14.7 hectars) and designed to treat 1.2 million Population Equivalent
(PE). The maximum capacity is 270 m³/day. The JSTP would be required to generate
an effluent quality less than 20 mg/L BOD, 50 mg/L TSS and 10 mg/L of total
ammonium nitrogen plus nitrate nitrogen with a limit of 5 mg/L ammonia nitrogen.
The plant can reduce phosphorous in the biological step in the future.

JSTP

Figure 1: Location of Jelutong Sewage Treatment Plant (JSTP)

The JSTP consists of the inlet works, preliminary treatment, biological treatment,
prethickening tank, sludge holding tank, sludge thickening process, sludge digester,
sludge dewatering process and sludge disposal.

There are two anaerobic sludge digesters on the JSTP and only one is in operating
state. The other digester has not been used. The gas which arises in the digester is
used to generate electricity in a generator. The anaerobic digesteris equipped with
heating and mixing facilities which use the electricity from the generator.

The mixing in the anaerobic digester is performed with compressed biogas. They used
a heat exchanger to get a constant temperature in the digester. The temperature
depends between 30°C and 38°C.

One problem of the plant is the bad biogas quality. Due the bad methane rate I
picked up 7 sludge samples from different places of the JSTP and analyzed it in the
laboratory at the UniversitiSains of Malaysia. With my results and my knowledge I
want to find a solution for this problem.
4

2. Timetable
In cooperation with Dr. Suffian and Mr. Farhan I created a timetable for my work.

The first step was the orientation. In this step I read a lot of books and visited many
websites with information about the anaerobic digestion and there microorganism.
The books, which I have read, are listed in table 1.

Table1: List of books

Titel ISBN-10
Anaerobic Sludge Digestion 0-943-24413-7
The Microbiology of Anaerobic Digesters 0-471-20693-8
Wastewater Sludge Processing 0-471-70054-1
Sludge Management and Disposal 0-135-01248-1
Recycling and Reuse of Sewage Sludge 0-727-72992-6
Methods of Characterization of Sewage Sludge 9-027-71782-6
Taschenatlas der Umweltchemie 3-131-03111-5

After thisstep I discussed with Farhan and Dr. Suffian, which places are the best to
pick up our samples and which measurements we have to do. We defined 7 places
(figure 1, grease removal, biological treatment (sequencing batch reactors tank),
sludge thickening, sludge digester (influent and effluent), sludge dewatering process
and also disposal of sludge) and our measurements (TS, VS, FS, TSS, TVS, TFS, COD,
Alkalinity, Moisture, pH, and SVI). All samples were stored in refrigerator at
UniversitiSainsMalaysia civil engineering lab.
5

4
7
3
6
5

Figure 2: Sewage treatment flow diagram and sample points

The second step was to pick up the sludge and analyze it in the laboratory.

The last step was to discuss the results and make some improvement proposals.
6

3. Experimental procedure
3.1. Total, Volatile and Fixed Solids

3.1.1. TS
I. Prepare two evaporating dishes by cleaning and ignition at 500°C
for 1 hour in a muffle furnace.
II. Cool, desiccate, weigh, and store dish in desiccator until ready
for use.
III. Transfer sample to prepared dish, weigh (weight of wet sample
plus dish) and evaporate to dryness on a steam bath or in a
drying oven. Choose a sample volume that will yield a residue
between 2.5 and 200 mg. If necessary, add successive sample
portions to the same dish. When evaporating in a drying oven,
lower temperature to approximately 98°C to prevent splattering.
IV. Dry evaporated sample for at least one hour at 103 to 105°C.
V. Cool dish in a desiccator to balance temperature and weight
(weight of dry solids).
VI. Repeat cycle of drying at 103 to 105°C, cooling, desiccating, and
weighing until a constant weight is obtained, or until weight less
than 4% of previous weight.
A−C
VII. Calculate: Total Solids , as % by weight = ∗100
B−C
A=weight of dried resid ue plusdish [ mg ]
B=weight of wet residue plusdish[ mg]
C=weight of dish[ mg]

3.1.2. VS, FS
I. After total solids have been performed, ignite sample and dish
for 20 minutes at 500°C in muffle furnace. (Perform analysis in
triplicate)
II. Let dish cool partially in desiccator with cover off until most of
the gas has dissipated (approx. 2 minutes). Close desiccator to
complete cooling.
III. Weigh cool dish.
A−B
IV. Calculate: Volatile Solids ,as % Total Solids= ∗100
A−C
7

B−C
¿ Solids , as % Total Solids= ∗100
A−C
A=weight of residue plusdish before burning[mg]
B=weight o f residue plus dishafter burning[mg]
C=weight of dish[ mg]

3.2. Total, Volatile and Fixed Suspended Solids

3.2.1. TSS
I. Seat prepared glass-fibre filters in filter manifold with distilled
water.
II. Select sample size that will yield between 10 and 200 mg residue.
Keep sample mixed.
III. Filter sample to dryness. If pipetting small volumes pipette into
approximately 10 mL of distilled water to ensure sample is well
distributed over filter. Do not use 10 mL of distilled water if
saving the filtrate if saving the filtrate for analysis of Total
Dissolved Solids.
IV. Transfer filter back to its original planchet with forceps and dry
filter plus planchet for 1 hour at 103°C.
V. Cool in desiccator and weigh (dry weight of solids plus filter and
planchet).
mg ( A−B )∗1000
VI. Calculate: TSS ,
L
=[ ]
sample volume [ mL ]
A=dry weight of solids plus filter∧ planchet [ mg ]
B=weight of filter plus planchet

3.2.2. VSS, FSS

I. After determination of total suspended solids, ignite filter plus
planchet at 500°C for 20 minutes.
II. Cool in desiccator and weigh (weight of burned solids plus filter
and planchet).
mg ( A−B )∗1000
III. Calculate: VSS , [ ]
L
=
sample volume [ mL ]
mg ( B−C )∗1000
FSS , [ ]
L
=
sample volume [ mL ]
A=weight of solids plus filter∧¿
planchet before burning[mg]
B=weight of solids plus filter∧¿
planchet after burning [mg]
8

C=weight of filter plus placnchet [mg]

3.3. Sludge Volume Index

IV. Take a sample of mixed liquor and determine its SS
concentration (MLSS)
V. Add sample of mixed liquor into a measuring cylinder of 1000 mL
capacity.
VI. Allow the sludge to settle for 30 minutes.
VII. The volume of settled sludge is read from the markings on the
cylinder.
mg V ∗1000
VIII. Calculate SVI , [ ]
L
=
MLSS
mL
V =volume of settled sludge , [ ]
L
mg
MLSS=mixed liquor ,[ ]
L

3.4. Chemical Oxygen Demand (Preparation of the Stock Solution)

I. Potassium dicromate + mercuric sulphate solution (for 1 liter).
Weight 10.216 gm potassium dichromate and heat it in oven
until 2 hours. Then add 500 mL distilled water plus 10.216 gm
potassium dichromate (heated) plus 167 mL H2SO4 with
concentration 98% pure plus 33.3 gm mercury sulphate.
II. Silver sulphate solution (Acid Reagent ) (for 1 liter)
One liter H2SO4 with concentration 98% pure plus 10.12 gm Ag
SO4

3.5. Alkalinity(Preparation of the Stock Solution)

I. N/50 H2SO4
N = Take 7 mL from H2SO4 with concentration 98% then dilute
with distilled water until 250 mL. In order to become N/50, take
20 mL from 250 mL from N, then dilute with distilled water until
1 liter.
II. 2. Methyl orange indicator ( C14H14N3NaO3S)
0.05gm methyl orange indicator were dilute in 100 mL distilled
water.
III. Phenolphthalein Indicator
0.08gm phenolphthalein indicator were dilute with 100 mL
methanol (CH3OH)
9

IV. To calculate the results of the total alkalinity use this formular.
1000
Total alkalinity (M) = mL H2SO4 (to pH 4.50) x
mL sample

3.6. pH
I. The pH meter is calibrated with buffer solutions (pH 4.01 and
7.01).
II. The electrode is rinsed with with distilled water and dried with a
piece of tissue paper.
III. The pH values of the samples (50 mL) are determined by
immersing the pH meter electrode into them.
(Note: The electrode is rinsed with distilled water and dried with
tissue paper before measuring each sample’s pH.)
IV. The results are compared with are compared with those
obtained with pH paper.
V. Results are recorded.

3.7. Moisture
Ten milliliter of the sewage sludge sample and the empty clean beaker were weighed
with the analytical balance separately. The sample then added into beaker, and oven-
dried at temperature 105°C for 24 hours. After that it cooled in the desiccator for
balance the temperature. Beaker was weighed after oven-dried and recorded the
reading of the weight.

A−B
Moisture Content= ∗100
A
10

4. ResultsandDiscussion
If we picked up the first samples for ouranalysis, the SBR was on.So it was possible to
pick up all our samples. At the second time the SBR was off, so it wasn’t possible to
pick up sample number 4. We have also a huge difference between some values from
the first to the second analysis. Perhaps it is possible, that when the SBR is off, the
sludge has different content and that’s the reason, why the values have a so huge
difference.

1.1. Total, Volatile and Fixed Solids

The table 2 shows the results of the TS, VS, and FS measurements.

Table 2: Results of the Total, Volatile and Fixed Solids

15thDecember 2010 17thJanuary 2011

Sample
TS [%] VS [%] FS [%] TS [%] VS [%] FS [%]
1 0,0575 73,7864 26,2136 0,0700 58,4615 41,5385
2 0,1050 55,7471 44,2529 0,1398 52,1073 47,8927
3 2,8333 76,4889 23,5111 2,8570 73,9840 26,0160
4 0,0711 63,4146 36,5854 - - -
5 2,7102 73,5615 26,4385 3,3578 69,7194 30,2806
6 3,0468 74,5714 25,4286 3,6740 72,7448 27,2552
7 5,7051 74,8495 25,1505 4,3778 94,2193 5,7807

During the digestion process, volatile solids are degraded to a certain extent and
converted into biogas. The sludge volume is hereby reduced and the supernatant is
returned to the plant. The degree of stabilization is often expressed as the percent
reduction in volatile solids, itself associated with either the SRT or the detention time
based on the untreated sludge feed.
The following empirical equation allows the estimation of the amount of volatile
solids destroyed.
Vd=13,7∗ln ( SRTdes )+ 18.9

Vd=Volatile Solids destruction [ % ]

SRTdes=the time of digestion

In the anaerobic sludge digester of the JSTP we have a retention time of 15 days, so
the volatile solids destruction is 56%. In my measurements the volatile solids after
the digestion has an average value of 73,6581%. Before the digestion the value is
lower than after. This means, that the volatile solids increase in the digester. The
11

microorganisms produce normally gas in the digestion process, so the volatile solids
decrease.

1.2. Total, Volatile and Fixed Suspended Solids

The results of the TSS, VSS, and FSS measurements are in table 3.

Table 3: Results of the Total, Volatile and Fixed Suspended Solids

15thDecember 2010 17thJanuary 2011

Sample TSS VSS FSS TSS VSS FSS
[mg/L] [mg/L] [mg/L] [mg/L] [mg/L] [mg/L]
1 152,00 112,00 40,00 194,00 188,00 6,00
2 114,00 78,00 36,00 1058,00 870,00 188,00
3 23126,00 17132,00 5994,00 24622,00 18282,00 6340,00
4 1476,00 1072,00 404,00 -  -  -
5 25780,00 15456,00 10324,00 29696,00 23036,00 6660,00
6 27190,00 19774,00 7416,00 56926,00 47814,00 9112,00
7 337873,00 297380,00 40493,00 6426,00 4569,00 1857,00

1.3. Sludge Volume Index

The table 4 shows the results of the sludge volume index measurements.

Table 4: Results of the SVI

15thDecember 2010 17thJanuary 2011

Sample
MLSS [mg/L] SVI [mL/g] MLSS [mg/L] SVI [mL/g]
1 40,00 130,00 6,00 166,70
2 36,00 55,56 188,00 531,91
3 5994,00 166,50 6340,00 149,84
4 404,00 445,54 -  - 
5 10324,00 96,86 6666,00 150,15
6 7416,00 134,89 9112,00 109,74
7 40493,00 4,89 1857,00 21,54

The results are also very inconstant. You can see a huge fluctuation between all the
sample points. For example sample 2, at the 15 th December the sludge volume index
was 55,56 mL/g and at the 17th January the sludge volume index was 531,91 mL/g

.
12

1.4. Chemical Oxygen Demand

The results of the Chemical Oxygen Demand measurement are in table 5.

Table 5: Results of the COD measurement

15thDecember 2010 17thJanuary 2011

Sample dilutionratio
COD [mg/L] COD [mg/L]
1 1:5 340 152
2 1:120 161 330
3 1:10 23250 27720
4 1:120 1045 -
5 1:120 19800 16800
6 1:10 21240 26760
7 1:120 1154 1490
The COD Values increase with the time in the plant. Normally they should increase till
the digester and after the digestion process they should decrease. But in our
measurements, the values increase till after the digester and on the disposal they
decrease. That’s not normal and something is going wrong in the digester.
13

1.5. Alkalinity
The results of the total alkalinity from the 15th December 2010 are in table 6.

Table 6: Results of the alkalinity measurements from the 15 th December 2010

Burette reading
Sample Type of
Volume of Total
Sample Volume Start End alkalinit
N/50 H2SO4 alkalinity
[mL] [± 0.05 mL] [± 0.05 mL] y
[mL]
0 9,7 9,7
Methyl-
1 50 0 8,8 8,8 185,4
orange
Average 9,27
9,7 14 4,3
Methyl-
2 50 8,8 11,6 2,8 71
orange
Average 3,55
14 19 5
Methyl-
3 50 11,6 14,8 3,2 82
orange
Average 4,1
19 21,3 2,3
Methyl-
4 50 14,8 17 2,2 45
orange
Average   2,25
21,3 24,2 2,9
Methyl-
5 50 17 19,4 2,4 53
orange
Average 2,65
24,2 26,8 2,6
Methyl-
6 50 19,4 21,7 2,3 49
orange
Average 2,45
26,8 31,6 4,8
Methyl-
7 50 21,7 25,6 3,9 87
orange
Average 4,35
14

The table 7 shows the values of the Alkanility measurement from the 17 th January
2011

Table 7: Results of the Alkalinity measurements from the 17 th January 2011

Burette reading Type of Total
Sample Start End Volume of alkalinit alkalinity
Sample y
Volume (mL) [± 0.05 [± 0.05 N/50 H2SO4
mL] mL] [mL]
0 9,3 9,3
Methyl
1 50 0 9,5 9,5 188
orange
Average 9,4
9,3 16,8 7,5
Methyl
2 50 9,5 15,8 6,3 690
orange
Average 6,9
16,8 18,6 1,8
Methyl
3 50 15,8 17,5 1,7 4200
orange
Average 1,75
Nil Nil Nil
Methyl
4 Nil Nil Nil Nil Nil
orange
Average Nil
18,6 21,6 3
Methyl
5 50 17,5 19,7 2,2 6240
orange
Average 2,6
21,6 23,1 1,5
Methyl
6 50 19,7 21,4 1,7 3840
orange
Average 1,6
23,1 26,5 3,4
Methyl
7 50 21,4 25,6 4,2 760
orange
Average 3,8

Between the sample points there is sometimes a higher fluctuation than 500%. The
results from the first measurements have each time a lower value than the results
from the second measurements. At the first and second sampling we collected the
same sludge, but measured each time different values. Very important for the
digestion is the ratio of volatile acids/alkalinity after the anaerobic digestion. This
ratio should amount less than 0.8. In the measurements from the 15 th December, the
total alkalinity is very low and between the digester influent and effluent the
15

difference of the total alkalinity is not high enough. In the second series of
measurements the values are much better. Here we have a higher difference
between the influent and effluent.

1.6. pH
The results of the pH measurements are in the table 8.

Table 8: Results of the pH measurement

pH
Sample
15th December 2010 17thJanuary 2011
1 7,54 8,02
2 7,08 8,37
3 7,88 8,13
4 7,22 - 
5 7,53 8,08
6 7,32 7,94
7 8,05 8,17

The pH values are very high. Normally the pH of sludge before and after the digester
depends between 6,5 and 7,5. In the second sampling the pH values are higher than
in the first sampling. And each value from the second sampling is higher than 7.5. This
has a negative influent of the microorganisms.
16

1.7. Moisture
Table 9: Results of the Moisture measurement

15thDecember 2010 17thJanuary 2011

Sample
MLSS [mg/L] SVI [mL/g] MLSS [mg/L] SVI [mL/g]
1 40,00 130,00 6,00 166,70
2 36,00 55,56 188,00 531,91
3 5994,00 166,50 6340,00 149,84
4 404,00 445,54  -  -
5 10324,00 96,86 6666,00 150,15
6 7416,00 134,89 9112,00 109,74
7 40493,00 4,89 1857,00 21,54

The values of the moisture content have also a huge difference. For example sample
2 130 mL/mg at 15th December and 532 mL/mg at the 17 th January. Maybe the set off
of the SBR has a direct influence of sample 2.

5. Summary
On the basis of the results of my measurements we can see that the sludge is very
inconstant. This imbalance has an influence on the anaerobic digestion and therefore
also of the gas production. The microorganisms need a constant sludge consistence, a
constant temperature and also a constant pH.
17

6. Problems
The JSTP anaerobic digester produces a bad gas rate. The biogas consistence is
normally 55-70% of methane, 30-45% carbon dioxide and a less of sulfur compounds.
But in the anaerobic digester the gas consists of 30-40% methane, 25-30% carbon
dioxide, 4-10% oxygen and 1% sulfur compounds. The other 20-25% was indefinable.

6.1. Temperature
The temperature should not depend more than 2°C. At the first time when I visited
the plant, the temperature in the digester was 30°C, at the second time it was 36°C
and at the third time it was 30 °C again. So the temperature difference is too high for
the microorganisms. If this temperature difference to high, the microorganism died.

6.2. Oxygen
Another problem is the oxygen in the anaerobic digester, because the oxygen is toxic
for the anaerobic microorganisms. I’m not sure if the digester is thick or if the mixing
facilities pump oxygen in the tank.

6.3. pH
In my measurements I assert that the pH is very high. The values liebetween 7.5 and
8.5. Normally the sludge has the same pH in the influent and effluent of a continuous,
anaerobic sludge digester. These values were also different.

6.4. Retention Time

In an anaerobic sludge digester the retention time amounts between 15 and 25 days.
Mr. Azman told me, that the retention time in the JSTP digester is 15 days. I’m not
sure if that is right, because at the effluent the volatile acid /alkalinity ratio is very
high. That means that the microorganisms have not enough time to destroy the
volatile acids.
18

7. Proposalforsolution
7.1. Tracer
To determine the real retention time of the sludge in the digester, you can use the
tracer method. You inject a tracer in the digester and wait so long, till the tracer is
coming out. After that you have the exact retention time of the sludge. So you can
see,if the sludge is long enough in the digester.

7.2. Is the sludge in the anaerobic digester hermeticallysealed?

There are some solutions in the internet to check the density of the digester. You
have to discharge the digester and then you can check, if the digester is thick.

7.3. Digester is overfilled

It should be possible that the anaerobic digester is to full. That could be also a reason
for the bad gas rate. In this case, you can use your second digester, to get a better
methane gas rate.

7.4. Sludge is to inconstant

In this case, you have to check discharger. Maybe there are industrial companies
which discharge intermittent high loaded wastewater into the drain.

7.5. Problems with the temperature

There are many hints to solute the problems with the temperature. Reasonable is it,
to make a new isolation around the digester. The isolation stabilized the
temperature. Now it is also easier to control the temperature.

8. References
 The books in table 1.
 www.iwk.com.my
 www.wikipedia.de
 www.google.de
 www.ecosia.de