CHAPTER 4

OTHERS
INSTRUMENTATION

WATER ANALYSIS
INSTRUMENTATION
DMT 40133 INSTRUMENTAL ANALYSIS OF FOOD
 LEARNING OUTCOME
• At the end of this course, students able to
• Explain water analysis Instrumentation
• Water quality
• Water quality parameters
• Applications of water analysis in food industry
• Common techniques used for water analysis
• Prepare solutions and samples according to a set
method used in water analysis.
 WATER QUALITY
• Water quality is the physical, chemical and biological characteristics of water
Physical Chemical Biological
temperature pH algae
turbidity dissolved oxygen phytoplankton

• Water quality testing is an important part of environmental monitoring. When water

quality is poor, it affects not only aquatic life but the surrounding ecosystem as well.
• These parameters are relevant not only to surface water studies of the ocean, lakes
and rivers, but to groundwater and industrial processes as well.
• Water quality monitoring define as the sampling and analysis of water constituents
and conditions. These may include:
• Introduced pollutants, such as pesticides, metals, and oil
• Constituents found naturally in water that can be affected by human sources, such as
dissolved oxygen, bacteria, and nutrients.
• Contaminants that may be in untreated water include:
• microorganisms (viruses and bacteria)
• inorganic contaminants (salts and metals)
• pesticides and herbicides
• sediments
• organic chemical contaminants from industrial processes and
petroleum use
• radioactive contaminants

• Water quality depends on :

1. The local geology & ecosystems
2. Human uses (sewage dispersion, industrial pollution)
Water quality parameters
• Temperature
• Dissolved Oxygen(DO)
• Biochemical oxygen demand (BOD)
• Chemical oxygen demand (COD)
• Electrical Conductivity (also see salinity)
• Total suspended solids (TSS)
• pH
• Color of water
• Taste and odor
• Turbidity
• Dissolved metals and salts (sodium, chloride, potassium, calcium, manganese, magnesium)
• Microorganisms such as fecal coliform bacteria (Escherichia coli), Cryptosporidium, and Giardia lamblia
• Nutrients, such as nitrogen and phosphorus
• Dissolved metals and metalloids (lead, Mercury (element),arsenic, etc.)
• Dissolved organics: Colored Dissolved Organic Matter (CDOM), Dissolved Organic Carbon (DOC)
• Pesticides
What does each water quality
measurement mean？
• Water temperature:
• one of the critical parameters that is used to assess our river/stream for
aquatic habitats’ health.
• Many organisms, especially fish, are sensitive to temperature changes in
the river water.
• Fish can be classified into 3 categories based on their sensitivity to water
temperature (cold water, mixed water and warm water).
• Water temperature does not change as fast as air temperature (Figure 1),
but because of this, smaller increases in water temperatures can have
more of a negative impact on the water quality and ecosystems that
depend on this water.
• Turbidity:
• Turbidity of water is a measurement of the clarity of water that is affected by the
presence of solids, small particles/sediments, or pollutants.
• The more sediments in the water, the more turbid the water is; so our drinking
water is low in turbidity compared to water in the lakes.
• Turbidity can be useful as an indicator of the effects of runoff from construction,
agricultural practices, logging activities, stormwater, and wastewater discharges.

Fish in turbid water (left), and fish in clear water (right)

pH:
• pH level is a measurement of the acidity or alkalinity of water. Level of pH can indicate
chemical changes in water, and the biological availability of nutrients in water.
• A safe level of pH of water ranges between 6.5 and 8.5 units. pH levels higher than 8.5
become highly basic, while pH levels below 6.5 become highly acidic for water quality.
• The pH values in the stream water change due to human activities or due to submerged
plants and animals. The effluent discharges that come from industry, stormwater and
wastewater treatment plants and quarries may have higher or lower pH levels that in turn
change the pH of the stream water.
• High acidity or alkalinity deteriorates water quality for both aquatic and recreational
purposes and may cause irritation or damage to skin or eyes. Prolonged exposure of
aquatic species to higher or lower pH may some times have fatal consequences.
• Chlorides:
• Chlorides are salts often present in areas of urban development. Chlorides in
water usually occur as a result of the use of water softeners, road salt, and
drainage of swimming pools. The majority of the time, many creeks and streams
display chloride levels above the Draft Canadian Water Quality Guideline (128
mg/L).
• Conductivity:
• Conductivity is a measure of the ability of water to pass an electrical current.
• Conductivity is useful as a general measure of stream water quality. Each stream
tends to have a relatively constant range of conductivity that, once established,
can be used as a baseline for comparison with regular conductivity measurements.
Significant changes in conductivity can be an indicator that a discharge has
occurred or some other source of pollution has entered a stream.
• Dissolved Oxygen:
• Dissolved oxygen (DO) is a measure of the amount of oxygen dissolved in
the water (percent or milligrams of oxygen per litre of water).
• Oxygen solubility in water = ranging from 6 to 14 mg/L
• Aquatic insects and fish that live in streams need sufficient dissolved
oxygen to survive and thrive.
• Stream waters gain oxygen from the atmosphere and from plants as a
result of photosynthesis
• Microorganisms consume oxygen during the breakdown of organic
material from both natural and man-made sources.
• The amount of dissolved oxygen in the river water can be affected by a
range or factors and processes going on in the river.
• The concentration of DO in a sample is significantly influenced water by:
• Temperature: As water temperature increases, DO decreases (i.e., as
water gets warmer, it holds less oxygen)
• Salinity: As water salinity increases, DO decreases (i.e., as water gets
saltier, it holds less oxygen).
• Atmospheric Pressure: As pressure increases, DO also increases (i.e.,
water holds less oxygen as increase the altitude).
• The concentration of dissolved oxygen in ocean water is
typically between 7 and 8 milligrams per liter (mg/L).
• Below 4 mg/L, organisms will begin to react either avoiding
or migrating out of the area.
• Less than 0.2 mg/L - unable to support most forms of life.
Biological Oxygen Demand
• Biochemical oxygen demand, or BOD, measures the amount of oxygen consumed
by microorganisms in decomposing organic matter in stream water.
• A test is used to measure the amount of oxygen consumed by these organisms
during a specified period of time (usually 5 days at 20 C).
• The greater the BOD, the more rapidly oxygen is depleted in the stream. This
means less oxygen is available to higher forms of aquatic life.
• Sources of BOD include leaves and woody debris; dead plants and animals; animal
manure; effluents from pulp and paper mills, wastewater treatment plants,
feedlots, and food-processing plants; failing septic systems; and urban
stormwater runoff.
Chemical Oxygen Demand
• The amount of oxygen consumed to chemically oxidize organic
water contaminants to inorganic end products.
• COD is expressed in mg/L, which indicates the mass of oxygen
consumed per liter of solution.
• COD is the most popular alternative test to BOD for establishing the
concentration of organic matter in wastewater samples.
• The COD test only takes a few hours to complete, giving it a major
advantage over the 5-day BOD test.
• COD can test wastewater that is too toxic for the BOD test.
 Quantitative water
Purpose Normal value
analysis
Summary Relative acidic or basic
Surface water: 6.5 to
level of the solution.
pH 8.5
(hydrogen ion
Groundwater: 6 to 8.5
concentration)

Sum of total dissolved

solids (TDS) and up to 500 mg/l (WHO2
Total Solids (TS)
suspended solids (TSS) 2003)
in water.

Drinking water: 0.005 to

Conductivity (Ionic Measurement of total
0.5S/m
Contamination) dissolved solids (TDS)
(www.lenntechn.com)
Quantitative water
Purpose Normal value
analysis

Measure of total viable

Total Bacterial Count (can proliferate) 100 CFU/ml
organisms in water

Amount of dissolved
oxygen needed to meet
Biochemical Oxygen
the demand of aerobic 1 mg/l
Demand (BOD)
microorganisms in
water

Amount of dissolved
oxygen required to
Chemical Oxygen 10 mg/l
cause chemical
Demand (COD) (hannainst.com)
oxidation of the organic
material in water
 Applications of water analysis in food industry
• Water is important to the food processing industry because it is present in all
foods.
• When water is used as a food ingredient, its quality can affect the properties of the
food, including texture, shelf stability, appearance, aroma and flavor.
• When water as a processing aid, water may be used for conveying, heating,
cooling, rinsing, dissolving, dispersing, blanketing, diluting, separating, steam
generation and other activities.
• Both microbiological and chemical parameters should be tested.
• Microbial analyses should include total counts and coliforms.
• Chemical tests should include pH, water hardness, heavy metals,
pesticides, iron and nitrates.
Common techniques used for water analysis

• WINKLER (TITRATION) METHOD / DILUTION METHOD

• MONOMETRIC METHOD (METER & PROBE)
 METHODS OF DO TEST
1. WINKLER (TITRATION) METHOD / DILUTION METHOD

1. MONOMETRIC METHOD (METER & PROBE)

 1. WINKLER METHOD
• The Winkler method involves filling a sample bottle
completely with water (no air is left to bias the test).
• The dissolved oxygen is then "fixed" using a series of
reagents that form an acid compound that is titrated.
• Titration involves the drop-by-drop addition of a
reagent that neutralizes the acid compound and
causes a change in the color of the solution.
• The point at which the color changes is the "endpoint"
and is equivalent to the amount of oxygen dissolved in
the sample.
2. METER AND PROBE METHOD
• A dissolved oxygen meter is an electronic device that converts signals
from a probe that is placed in the water into units of DO in milligrams
per liter.
• Most meters and probes also measure temperature.
• The probe is filled with a salt solution and has a selectively permeable
membrane that allows DO to pass from the stream water into the salt
solution.
• The DO that has diffuse (slowly) into the salt solution changes the
electric potential of the salt solution and this change is sent by electric
cable to the meter, which converts the signal to milligrams per liter on a
scale that the volunteer can read.
EXAMPLE OF DO INSTRUMENTS

DISSOLVED OXYGEN METER

WATER TEST 2: BOD (BIOCHEMICAL OXYGEN
DEMAND)

◻ BOD Definition = How fast biological organisms use up

oxygen in a body of water
◻ Not a precise quantitative test

◻ Expressed in milligrams of oxygen consumed per litre of

sample (mg/L) during 5 days of incubation at 20 °C
 METHODS OF BOD TEST
MONOMETRIC METHOD
DILUTION METHOD
• Dilution
• Undiluted

TYPICAL BOD VALUE

🞑 Wastewater BOD5 ≈ 250 mg/L
🞑 Effluent BOD5 from wastewater < 30 mg/L
🞑 Industrial wastewater = 30,000 mg/L
 METHODS OF BOD TEST
• 1. DILUTION METHOD
• Very small amount of micro-organism seed is added to each sample being tested

• This seed is typically generated by diluting organisms with buffered dilution water

BOD test is carried out by diluting the sample with oxygen saturated dilution water,
inoculating (vaccinated) it with a fixed aliquot of seed, measuring the dissolved oxygen (DO)
and then sealing the sample to prevent further oxygen dissolving in.

• The sample is kept at 20 °C in the dark to prevent photosynthesis (and thereby the addition
of oxygen) for five days, and the dissolved oxygen is measured again.

• The difference between the final DO and initial DO is the BOD.

◻ BOD can be calculated by:
🞑 Undiluted
◻ Initial DO - Final DO = BOD

🞑 Diluted
◻ ((Initial DO - Final DO)- BOD of Seed) x Dilution Factor
◻ Dilution factor refers to the ratio of the volume of the initial
(concentrated) solution to the volume of the final (dilute)
solution, DF = V2 ÷ V1.
 2. Manometric method (METER & PROBE)
• This method is limited to the measurement of the oxygen consumption due only
to carbonaceous oxidation. Ammonia oxidation is inhibited.
• The sample is kept in a sealed container fitted with a pressure sensor.
• A substance that absorbs carbon dioxide (typically lithium hydroxide) is added in
the container above the sample level.
• The sample is stored in conditions identical to the dilution method.
• Oxygen is consumed and, as ammonia oxidation is inhibited, carbon dioxide is
released.
• The total amount of gas, and thus the pressure decreases because carbon
dioxide is absorbed.
• From the drop of pressure, the sensor electronics computes and displays the
consumed quantity of oxygen.
 EXAMPLE OF MONOMETRIC
INSTRUMENT

BOD METER & PROBE

 ADVANTAGES
◻ The main advantages of MONOMETRIC method
compared to the DILUTION method are:

1. Simplicity: no dilution of sample required, no

seeding, no blank sample.
2. direct reading of BOD value.
3. continuous display of BOD value at the current
incubation time.
 WATER TEST 3: COD
( CHEMICAL OXYGEN DEMAND)
• The amount of oxygen consumed to chemically oxidize organic
water contaminants to inorganic end products.
• COD is expressed in mg/L, which indicates the mass of oxygen
consumed per liter of solution.
• COD is the most popular alternative test to BOD for establishing the
concentration of organic matter in wastewater samples.
• The COD test only takes a few hours to complete, giving it a major advantage
over the 5-day BOD test.
• COD can test wastewater that is too toxic for the BOD test.
METHODS OF COD TEST
1. TITRATION METHOD
TITRATION
METHOD
 1. TITRATION METHOD
• A sample is refluxed in strongly acidic solution with a known excess of
potassium dichromate (K2Cr207).
• After digestion the remaining unreduced K2Cr207 is titrated with ferrous
ammonium sulphate to determine the amount of K2Cr207 consumed and
the oxidizable matter is calculated in terms of oxygen equivalent.
• This procedure is applicable to COD values between 40 and 400 mg/L.
• Higher COD values can be obtained by careful dilution or by using higher
concentrations of dichromate digestion solution
• The COD value may be calculated then from the difference of the originally
added quantity of dichromate and the remainder, which is determined by
the quantity of the added ferrous till titration endpoint.
 2. COLORIMETRIC METHOD
• In Colorimetric method, sample is digested in a COD Reactor for 2 hours.
• COD material in that sample is oxidized by the dichromate ion. The result is the
change in chromium from the hexavalent (VI) to the trivalent (III) state.
• Both chromium species exhibit a color and absorb light in the visible region of the
spectrum.
• This method covers the ranges from 0 to 15000 mg/L 02:
1) 0- 150 mg/L near 420 nm
2) 0-1000 (1500) mg/L near 600 nm
3) 0-15000 mg/L near 600 nm
Official Reporting Method, (dichromate)
• In the 400 nm region the dichromate ion (Cr2072-) absorbs strongly while the chromic
ion (Cr3+) absorbs much less. In the 600 nm region it is the chromic ion that absorbs
strongly and the dichromate ion has nearly zero absorption.
• Advantages in using this method include high accuracy, certifiable results and abate
chloride interference.
 APPLICATIONS
• Most applications of COD determine the amount of :

• organic pollutants found in surface water

• (e.g. lakes and rivers) or wastewater

• making COD a useful measure of water quality.

• The COD tests oxidizes organic compounds by the action of

strong oxidizing agents under acid conditions
EXAMPLE OF COD INSTRUMENTS

COD Meter and Multiparameter

Photometer for Wastewater
Analysis
EXAMPLE OF COD INSTRUMENTS
 BOD vs COD
1. Biologically decompose 1. Chemically decompose organic
organic waste waste.
2. Amount of oxygen that require 2. total measurement of all
for the bacteria to degrade the chemicals (organics & in
organic components present in organics) in the water / waste
water / waste water. water
3. BOD values are always lower 3. COD values are always higher
than the COD values. than the BOD values.
4. BOD contains only bio 4. COD includes both
degradable. biodegradable and non-
biodegradable substances
5. The BOD tes takes 5-day to
complete 5. The COD test only takes a few
hours to complete
Prepare solutions and
samples according to
a set method used in
water analysis.
• Samples must be taken
from locations that are
representative of the
water source, treatment
plant, storage facilities,
distribution network,
points at which water is
delivered to the consumer,
and points of use.