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Solids, Colour, Turbidity

& Conductivity
Presented by:
M S Bhatti
Guru Nanak Dev University, Amritsar

December 7, 2021 1
Physical characteristics:
2

 Solids: floating, settable, colloidal, dissolved


 Odour

 Temperature

 Density or specific gravity

 Colour

 Turbidity

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TDS with conductivity
Suspended solids with turbidity in settled
secondary effluent.

How they are related

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Solids
• Total solids at 103 to 105 C
• Total dissolved solids at 180 C for clean water
• Volatile solid analysis at 550 C to measure the
biological activity (MLSS & MLVSS) in municipal
sludge.

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1. Total Solids dried at 103 to 105 degree C

2. Total dissolved solids dried at 180 C


3. Total Suspended Solids at 103-105 C
4. Fixed & Volatile Solids Ignited at 550 C
5. Settleable solids for semisolids &
sludge

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Significance of Solids
• Water with high dissolved solids are of inferior quality
– A limit of 500 mg/l is desirable in drinking water
• Highly mineralized water is also unsuitable for many industrial
applications
• Water with high suspended solids may be aesthetically
unsatisfactory (for bathing!)
• Solids analysis is important
– in the control of biological and physical wastewater treatment
processes
– for assessing compliance with regulatory requirements
• Fixed and volatile solids are used to represent active biomass
in the mixed liquor in activated sludge process
– Volatile and fixed solids do not precisely distinguish organic and
inorganic matter –many mineral salts also volatilize

8 December 7, 2021
Solids
Total solids (TS): Material residue left behind after evaporation
of a sample and its subsequent drying in a oven at a defined
temperature to constant weight
Total suspended solids (TDS): Portion of the material residue of
a sample retained by a filter
Total dissolved solids (TDS): Portion of the material residue of a
sample that passes through a filter
Fixed solids: Residue of TS or TSS or TDS left after ignition for a
specified time at a specified temperature
Volatile solids: weight loss on ignition
Settleable solids: Material settling out of suspension within a
defined period

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Temperature and duration of drying
10

 Temperature at which the residue is dried and duration of


drying are very important - influences
 Weight loss due to volatilization of organic matter
 Weight loss from loss of mechanically occluded water and
water of crystallization
 Weight loss from loss of gases (heating converts
bicarbonates into carbonates and release CO2, and
decomposes carbonate to release CO2)
 Weight loss from chemical decomposition and weight gain
from oxidation
 Usually duration of drying is adjusted to obtain constant
weight of the residue
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Temperature and duration of drying

• Drying temperatures in practice

• 103-105C

• 180±2C

• For estimating fixed solids the residue is


usually ignited at 550±50C to constant
weight in a muffle furnace
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Sample handling, preservation and preparation

• If acceptable, avoid large floating particles or submerged


agglomerates of non-homogenous materials while sampling
• Resistant glass or plastic bottles, provided the material in
suspension of the sample does not adhere to walls, are used for
holding the samples
• Analysis of samples is started as soon as possible (impractical to
preserve sample)
• To minimize microbiological decomposition refrigerate sample at 4
C
• Before taking sample disperse floating oil and grease with a blender
• Choose sample size/volume to give 2.5 to 200 mg of residue

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Sample handling, preservation and preparation

Evaporation dishes of 100 mL capacity of one of


the following material are used:
– Porcelain (9 cm dia.)
– Platinum
– High silica glass

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Sample handling & preparation
Preparation of the evaporation dish
– Heat clean dish to 103-105C/180±2C/550±50C for 1 hour
depending on the temperature of drying and on the need for
ignition of the residue
– Storing the heated dish in desiccator until needed
– Weighing the dish immediately before use for initial weight -
balance capable of weighing to 0.1 mg is required

Transfer measured volume of well mixed sample into pre-weighed dish


and evaporate to dryness on a steam bath or drying oven
– For evaporation in a oven, use temperature 2C below boiling
point to prevent splattering

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Sample evaporation, and drying to constant
weight and ignition of residue

Once evaporated to dryness, dry the sample at least for 1


hour in a oven at 103-105C or 180±2C as required and
cool the dish in a desiccator to balance temperature and
weight

Use repeat cycles of drying, cooling in desiccator and


weighing until constant weight.
– Weight loss <4% or 0.5 mg whichever is less between
two successive drying cycles is acceptable

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Fixed & Volatile Solids ignited at 550 C

Ignite the dried residue of the dish to constant weight in a


muffle furnace at 550±50C
– Raise the furnace temperature to desired level prior to
inserting the sample and ignite for 15-20 minutes
– Air cool the dish partially and then transfer into
desiccator for final cooling in dry atmosphere, then
weight the dish
– Use repeat cycles of drying, cooling in desiccator and
weighing until constant weight is obtained

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Total solids
Well mixed sample is evaporated in a weighed dish and dried to
constant weight in a oven at 103-105C
Increase in weight of dish represents total solids

Total solids (mg / L) 


 A  B  1000 B is weight of empty dish
Sample volume (mL) A is weight of dish with residue

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Total dissolved solids
Filter well mixed sample through a fiber filter and evaporate filtrate in
weighed dish and dry to constant weight at 180±2C
– Filtrate from TSS determination can also be used
Increase in dish weight represents TDS
TDS ( mg / L) 
 A  B   1000 B is weight of empty dish
Sample volume ( mL) A is weight of dish with residue

• Highly mineralized samples may require prolonged drying, proper


desiccation and rapid weighing
– Significant concentrations of calcium, magnesium, chloride and/or
sulfate can be hygroscopic and cause problem
• Samples high in bicarbonate may require careful and prolonged
drying to ensure complete conversion to carbonate
• Glass fiber filter disks, filtration apparatus with membrane filter
funnel or Gooch crucible, and suction flask may be needed
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Total suspended solids
• Filter well mixed sample through a weighed standard glass fiber
filter and dry the residue retained on the filter to constant weight
at 103-105C
– In case of filter clogging and prolonged duration of filtration take
difference of TS and TDS as TSS
Increase in dish weight is represented by
TSS (mg / L) 
 A  B  1000 B is weight of empty dish
Sample volume (mL) A is weight of dish with residue

• In case of samples with high dissolved solids, thoroughly wash the


filter to ensure removal of dissolved material
• Clogging and prolonged filtration can produce high results due
excessive solids capture
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Fixed and volatile solids

• Dried residue left in the dish during TS, TDS and TSS is ignited to
constant weight at 550±50C in a muffle furnace
• Solids left after ignition represent fixed solids (total fixed solids
from TS, total dissolved fixed solids from TDS and total suspended
fixed solids from TSS)
• Fixed solids can be calculated by

Fixed solids (mg / L) 


 B  C  1000
Sample volume (mL )

B is weight of dish after ignition


C is weight of the empty dish

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Fixed and volatile solids

• Weight lost on ignition represent volatile solids (total


volatile solids from TS, total dissolved volatile solids from
TDS and total suspended volatile solids from TSS)

Volatile solids (mg / L) 


 A  B  1000
Sample volume (mL)

B is weight of dish after ignition


A is weight of dish after drying

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Settleable solids
Determined & reported on either volume (mL/L) or weight (mg/L)
basis
Measurement on volume basis requires an Imhoff cone
– Fill Imhoff cone to 1-L mark with sample and settle for 45 min.
– Gently stir sides of the cone with a rod by spinning and settle for
another 15 minutes
– Record volume of the settled solids in the Imhoff cone
Measurement on weight basis (indirect method)
– Determine total suspended solids of well mixed sample
– Pour >1-L of sample into a glass vessel of >9 cm dia. to depth >20cm
– Let it stand quiescent for one hour
– Without disturbing settled or floating material siphon out 250 ml from
vessel center and determine its TSS as non-Settleable TSS
Settleable solids = TSS – non-Settleable TSS
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Sludge volume index (SVI)
• Volume in mL occupied by 1 g of a suspension after 30 min. settling
settled sludge volume (mL / L)  1000
SVI 
suspended solids concentration (mg / L)

• Applications:
1. Used to monitor settling characteristics of activated sludge and other
biological suspensions
2. Determined for the mixed liquor of the aeration tank of the ASP
3. Determine SS concentration of a well mixed sample of suspension
4. Determine the 30 min. settled sludge volume

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Applications of solids data in
Environmental Engineering:

• Suitability of potential supplies


• Need for water softening
• Corrosion control through pH adjustment
which depends on solids
• Design of Primary sedimentation tank

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Turbidity
measures the light transmitting
properties of water
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Turbidity
• Water quality standard: < 5 NTU
• Indicates clarity of water
• Optical property due to the presence of colloidal matter like
– Clay, silt, finely divided organic and inorganic matter, plankton
and other microscopic organisms etc.
• Causes light to be scattered and absorbed
• Clarity of water is important for
– Producing products destined for human consumption
– Potability
– Water bodies condition and productivity
• Coagulation, settling and filtration are needed for the
removal of turbidity and clarity of water

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Significance of Turbidity
• Aesthetic
• Filterability: Slow and rapid sand filter
• Hindrance in Disinfection

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Principle of Nephlometric Turbidity:

• For measurement intensity of light scattered in one


particular direction (at right angles to the light path)
by the sample under defined conditions is compared
with that by a standard reference suspension under
the same conditions

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Nephelometer: Principle & Operation
• A light source - tungsten filament lamp (now IR lamp for
coloured samples)
• Photoelectric detector and a readout device
– Should have spectral peak response between 400-600 nm
• Sample tube
– should be of colourless glass
– should be devoid of scratches or etches
– Light (both incident and scattered) travel distance through the
sample should be <10 cm
• Sensitivity should be <0.02 NTU
• Should allow several ranges of turbidity measurement
(0-1; 0-10; 0-100; 0-1000)

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Turbidity measurement
• Should be measured on the same day of sampling
– If unavoidable sample can be stored in dark up to 24 hours
– Storage for longer periods can cause irreversible changes in
turbidity
• Sample free of debris and rapidly settling coarse sediments,
after vigorous shaking, should be transferred into sample
tube
• Dirty glassware, presence of air bubbles and vibrations can
affect the results
• Water colour due to dissolved substances that absorb
colour can lower the turbidity measurement ??
• Higher the intensity of the scattered light higher is the
turbidity

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Standard unit of turbidity:
• Initially 1 mg SiO2/l = 1 unit of turbidity
• Now Formazin polymer suspension is used
• Preparation of standard stock suspension
• Dissolve 1.000 g of hydrazine sulfate, (NH2)2.H2SO4 (carcinogenic), in
turbidity free water and dilute to 100 ml
• Dissolve 10.000 g hexamethylene tetramine, (CH4)6NH4, in turbidity
free water and dilute to 100 ml
• Mix 5 ml of hydrazine sulfate solution and 5 ml of hexamethylene
tetramine solution in a 100 ml volumetric flask and allow it to stand
for 24 hours at 25±3C
• Dilute the mixer with turbidity free water to 100 ml to obtain
standard stock suspension of 400 NTU turbidity
– Can stand for one month
– Can be used for daily preparation of standard reference suspensions
of other turbidities (dilute with turbidity free water)

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Turbidity measurement
• Calibration of the turbidity meter:
– Follow manufacturer’s instructions
– Run at least one standard reference suspension in each of the ranges
• Turbidity measurement
– When turbidity expected is <40 NTU measure turbidity of the sample
directly
– When expected turbidity is >40 NTU dilute the sample to get 30-40
NTU range of turbidity and then measure

A is NTU measured of diluted sample


A  (B  C)
NTU  B is volume of the diluted sample
C C is volume of the sample diluted

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Application of turbidity data:

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Colour
Reflects age of the wastewater: light
brownish gray to gray and then to
black (anaerobic conditions) also
known as septic conditions
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Colour
35

Could be due to the presence of natural metallic ions


(iron and manganese), humus and peat materials,
plankton, weeds and industrial wastes
True colour: colour of water from which turbidity has
been removed
Apparent colour: includes the colour contributed by
colloidal and suspended matter
Usually visual comparison method is used for potable
water
Instrumental methods (spectrophotometric method) are
appropriate for unusual colours of industrial wastes

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 Iron gives colour in water supply
 Surface water is more coloured
 Colour intensity increases with increase in
pH. Recording pH with colour is advised.
 Industries like dye, textile, pulp & paper
produce wide varieties of colour

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Pretreatment of sample
• Needed to remove turbidity prior to colour
determination.
• Centrifugation and filtration can be used for the
pretreatment.
• Filtration can remove some of the true colour
• Results of centrifugation may vary with sample
nature and size and speed of the centrifuge
• The pretreatment method used should be reported
with the results.
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Colour comparator by Nessler tubes:

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Visual comparison method
39

• Good for potable water and for water with colour


due to naturally occurring materials
• Sample colour is compared with the known
concentrations of coloured solutions or with special
properly calibrated glass colour discs.
• One unit of colour is produced by 1 mg of platinum
(K2PtCl6) per liter in the form of chloroplatinate
ion.

December 7, 2021
Standard colour solution:
• Colour standard of 500 units colour is prepared by dissolving
1.246 g K2PtCl6 (equivalent to 500 mg of metallic platinum)
and 1.000 g of crystallized cobaltous chloride CoCl2.6H2O in
distilled water and 100 ml of HCl and adjusting final volume to
1000 ml
• From this colour standards desired colour is prepared by
dilution with distilled water
• Colour of the glass discs are also calibrated with the colour
standards of platinum-cobalt

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Requirements

• Filtration system comprising of filtration flasks, filter


crucible of 40 µm pore size, crucible holder, calcined filter
aid and vacuum system
• Spectrophotometer with effective operating range of 400-
700 nm and absorption cells of 10 mm light path
• Filtered sample is used.
• Results are expressed in terms of dominant wavelength/ on
the basis of this hue of the sample.
• Luminance
• Purity

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Colour hues for dominant wavelengths
Dominant wavelength Hue
range
400-465 Violet
465-482 Blue
482-497 Blue-green
497-530 Green
530-575 Greenish yellow

575-580 Yellow
580-587 Yellowish orange

587-598 Orange
598-620 Orange-red
620-700 red
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Steps in Spectrophotometric method
• Take two portions of 50 ml for sample.
• Adjust pH of one portion to 7.6 (should not change volume by
beyond 3%)
• Remove suspended solids by centrifuging
• Prepare each of the two portions of the sample through filtration
• Assemble the filtration set-up
• Prepare suspension of 0.1 g of calcinated filter aid in 10 ml of
sample and filter through the filter crucible for forming precoat in
the crucible
• To 35 ml of the sample add 40 mg of calcinated filter aid and filter
through precoat crucible while applying vacuum
• Waste the filtrate as long as it is not clear and after that collect 25
ml filtrate

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Spectrophotometric method
• Measure light transmittance of the filtered sample on
spectrophotometer
• Clean an absorption cell with detergent and rinse first with
distilled water and then with filtered sample twice and fill
the cell with sample
• Clean the exterior of the cell with lens paper and transfer
the cell to spectrophotometer
• Measure transmittance after setting 100% transmittance on
distilled water blank at the three different wavelengths
against each of the 10 or 30 ordinate numbers
• Tabulate the transmittance values under X,Y and Z columns
against the ordinate numbers

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Ordinates for spectrophotometric colour determinations
Ordinate No. X Y Z
Wavelength (nm)
2 435.5 489.5 422.2
5 461.2 515.2 432
8 544.3 529.8 438.6
11 564.1 541.4 444.4
14 577.4 551.8 450.1
17 588.7 561.9 455.9
20 599.6 572.5 462.0
23 610.9 584.8 468.7
26 624.2 600.8 477.7
29 645.9 627.3 495.2
Multiplying 0.09806 0.10000 0.11814
factor
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Spectrophotometric method:
Find tristimulus values X, Y and Z by summing up transmittances
under X, Y and Z columns and multiplying with appropriate
factor
The tristimulus value Y is percent luminance
Find trichromatic coefficients x and y by
X Y
x y
X Y  Z X Y  Z
Using chromaticity diagram determine dominant wavelength
and purity (in percent) corresponding to the trichromatic
coefficient values x and y
Using the table of colour hues for dominant wavelength ranges
find colour hue corresponding to the dominant wavelength

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Expression of results:

• Express colour characteristics (as pH 7.6 and


at original pH) in terms of dominant
wavelength (nm), luminance & purity along
with spectrophotometer, bandwidth and
number of selected ordinates 30/10.

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Conductivity

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Conductivity
• Numerical expression of the ability of an aqueous solution to
carry electric current
• Depends on the presence and concentration of ions and their
valence and mobility and temperature
– Inorganic acids, bases and their salts are relatively good
conductors
– Organic molecules are in general poor conductors
• Actually resistance is measured and reciprocal of it is taken as
conductance

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Conductivity: Units of expression
• Expressed in reciprocal ohms or mhos or
µmhos/cm
– In SI units it is expressed in Siemens
(milliSiemens/meter)
– 1 mS/m = 10 µmhos/cm
• Temperature affects conductivity
– increases by 1.9% per every 1C temperature increase
in of standard KCl solution

• Conductivity is measured and expressed at 25C


December 7, 2021 50
Conductivity meter: Instrument detail
• Includes a source of alternate current, Wheatstone bridge, null
indicator and conductivity cell, and thermometer of 23-27C range
to nearest 0.1C
– Range can be checked with standard KCl solutions
• Conductivity cell can be platinum electrode type or a non-platinum
electrode type
• Platinum electrode type
– In case of new cells, electrodes need cleaning (chromic-sulfuric acid
mixture) and platinizing before use
– In case of erratic readings, electrodes need cleaning and re-platinizing
– When not in use thoroughly rinse the electrodes and keep inserted in
distilled water
• Non-platinum electrode type
– Durable common metals like stainless steel electrodes
– Need calibration
Error of measurement should be <1% or 1 µmhos/cm
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Standard potassium chloride solution
• Conductivity water is used for preparing KCl solution and for
various other purposes in the experiment
– Should have <1 µmhos/cm conductivity
• 1M 111,900 µmhos/cm
• 0.1 M 12,900 µmhos/cm
• 0.01 M 1,413 µmhos/cm
• 0.001 M 147 µmhos/cm
• 0.0001 M 14.94 µmhos/cm
Standard potassium chloride solution
– 0.01M KCl solution - 745.6 mg anhydrous KCl solution in
conductivity water in one liter of final volume
– Stored in glass-stopper borosilicate glass bottle.
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Conductivity measurement
Rinse the cell with two or three portions of sample
Adjust sample’s temperature to 25±0.1C
Measure sample’s resistance (Rm) and temperature (tC)
Estimate conductivity at 25C of the sample by
1,000,000  C
K
Rm 1  0.0191 t  25 
Conductivity measured at tC (Km) can be corrected to conductivity at
25C (K) by
K m 1,000,000  C
K
1  0.0191 t  25

Here temperature coefficient of water sample is considered same that


of standard KCl solution
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Observations:
 Fresh distilled water has 0.5 to 2 µmhos/cm
 With storing it increases to 2-4 µmhos/cm due to CO2
and even ammonia absorption
 Conductivity of potable water is in the range of 50-1500
micro mho/cm
 Industrial wastewaters conductivity can be even >10000
micro mho/cm
 Conductivity measurement is used
1. To signal exhaustion of ion-exchange resins
2. For rapid determination of large changes in inorganic content
of waters and wastewaters
 Dissolved solids concentration is related to conductivity
by an empirical multiplying factor (0.55 to 0.9)
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THANKS

December 7, 2021 55

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