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Cross-border network for knowledge transfer and innovative development in wastewater treatment WATERFRIEND HUSRB/1203/221/196 1st HUSRB Students Meeting

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Title: Cross-border network for knowledge transfer and innovative development in wastewater treatment WATERFRIEND HUSRB/1203/221/196 1st HUSRB Students Meeting


1
Cross-border network for knowledge transfer and
innovative development in wastewater
treatment WATERFRIEND HUSRB/1203/221/196 1st
HUSRB Students Meeting
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Wastewater and certain methods for its
analysis Božo Dalmacija, Jasmina Agbaba, Malcolm
Watson University of Novi Sad Faculty of
Sciences, Trg Dositeja Obradovica 3, 21000 Novi
Sad
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Wastewater - water which is contaminated in any
way during use.
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  • Water polluters

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According to its origin, wastewater can be
classed as
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  1. municipal wastewater - water used in households,
    institutions, schools, hospitals, etc.
  2. industrial wastewater - used water from
    industrial plants
  3. wastewater from livestock facilities (farms) -
    usually wet manure removed from breeding pigs and
    so on
  4. atmospheric waste water - rainfall which flows
    from the city and industrial areas and which can
    contain various materials found locally and
  5. drainage wastewater from landfills containing
    municipal and other waste.

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Municipal wastewater
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  • Long term constant composition in a region, as a
    result of the standard of living and way of life
    of the population.
  • Pollution amounts and loads may be expressed
    using norms, i.e. standard values per unit
    population
  • (PE - Population Equivalent)

Table 1. Pollution by PE
Parameter Unit Value
BOD5 g/PE.day 60
COD g/PE.day 120-150
Suspended matter g/PE.day 70-90
Total phosphor g/PE.day 12-15
Total nitrogen g/PE.day 2.5-3
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  • The amount and composition of municipal
    wastewater shows typical variations during the
    day as a result of the rhythm of life of the
    population.
  • Certain variations in flow and composition may
    also occur during the year.

rainy period
Flow m3/s
dry period
S M T W T F
S
Figure 1. Usual daily and weekly variation of
municipal wastewater
Rural centres - below 150 l / capita per day,
Urban areas - 200 l / capita per day.
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  • The smaller the sewage system and the lower the
    population served by the sewage system, the
    greater the daily variation, i.e. the greater the
    ratio between the maximum and medium flows

Figure 2. Daily fluctuations in municipal
wastewater flow 34500 m3/day suspended matter
9620 kg/day BOD5 7420 kgO2/day total nitrogen
1620 kgN/day
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Parameter Variation Settleable fraction()
pH 7.5-8.5
Dry extract, mg/l 500-1500 10
Total suspended solids, mg/l 150-500 50-70
BOD5, mgO2/l 100-400 25-40
COD, mgO2/l 300-1000 25-40
TOC, mg/l 100-300
Total nitrogen, mgN/l 30-100 8-12
NH4-N, mgN/l 20-80 0
NO2-N, mgN/l lt1 0
NO3-N, mgN/l lt1 0
Detergents, mg/l 6 13 0
Total phosphor, mgP/l 4 18 10 20
Lipids, mg/l 50 120 8 20
Table 2. Characteristics of municipal wastewater
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Industrial wastewater
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  • Industrial wastewaters often have variable
    character, both in quantity and in quality.

Wastewaters vary by type of industry, but also
frequently between the same type of factory, as a
consequence of differences in production
techniques, raw materials, hours worked, etc.
Figure 3. Example of an industrial wastewater
daily flow
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  • Industrial wastewater can be divided into four
    categories depending on its quality and method of
    formation
  • technological wastewater
  • specific wastewater
  • useful discharge
  • occasional discharge

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  • The quantity and quality of industrial wastewater
    depends on
  • industrial activity, plant capacity and raw
    materials used
  • ability to recycle or separate different
    wastewater streams
  • daily wastewater amounts of each type
  • average and maximum daily amounts (frequency and
    duration) of water
  • average and maximum flows of pollutants
    (frequency and duration) for each specific waste
    discharge.

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Monitoring of wastewater
  • The selection of monitoring parameters depends on
    the
  • manufacturing process,
  • raw materials and
  • chemicals used in the plant/factory.
  • Wide range of monitoring frequencies according
    to the needs and depending on the risk posed to
    the recipient ecosystem, and in accordance with
    the monitoring approach undertaken.

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  • Large numbers of factories/companies - various
    pollutants in their wastewater.
  • Analytically irrational and economically
    unjustified to analyse all possible pollutants.
  • Parameters are therefore grouped according to the
    activities performed by the polluter and
    currently applied technology.
  • In all these cases, there is a certain number of
    parameters common to this type of wastewater -
    "general parameters".

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Table 3. General wastewater parameters
Parameter Parameter
Flow - daily average (m3/day) Fixed and volatile solids ignited at 550 C(mg/l)
Air temperature (oC) Loss on ignition (mg/l)
Water temperature (oC) Suspended matter (mg/l)
Colour (description or as spectral adsorption coefficient (SAC)) COD (dichromate method), homogenised sample (mg O2/l)
Odour (description) COD (dichromate method), filtered and settled sample (mg O2/l)
Visible material (description) BOD5, homogenised sample (mg O2/l)
Settleable solids (after 2 hours) (ml/l) BOD5 filtered and settled sample (mg O2/l)
pH Total nitrogen (mg N/l)
Dry residue (mg/l) Total phosphorus (mg P/l)
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  • Specific parameters - parameters that
    characterize different activities, technological
    processes, and in some cases differences in
    production organization.
  • These parameters are defined after examining the
    production process and defined for wastewaters in
    certain factories or companies.

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Table 4. Examples of specific parameters by
industrial activity
Activity Specific parameter analysed in this wastewater
Agriculture Agriculture
Livestock Pig farms Poultry ammonium ion (mgN/l) organic nitrogen (mgN/l) total coliform bacteria For farms greater than 40000 poultry, 2000 pigs (larger than 30 kg) or 750 sows, the following should also be determined Cu compounds (mg/l) Zn compounds (mg/l)
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Activity Specific parameter analysed in this wastewater
Food manufacturing Food manufacturing
Production, processing and preservation of meat and meat products oil and grease (mg/l) sodium (mg/l) chlorides (mg/l) surface active agents, (mg DBS/l) total coliform bacteria fecal coliform bacteria
Processing and preservation of fish and fish products oil and grease (mg/l) sodium (mg/l) chlorides (mg/l) surface active agents (mg DBS/l)
The production of vegetable and animal oils and fats oil and grease (mg/l) surface active agents (mg DBS/l) sulphates (mg/l)
Processing and preservation of milk oil and grease (mg/l) surface active agents (mg DBS/l) m- and p-alkalinity (mVal/l) m- and p-acidity (mVal/l)
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Activity Specific parameter analysed in this wastewater Specific parameter analysed in this wastewater
Tanning and leather production Tanning and leather production Tanning and leather production
Tanning and dressing of leather, manufacture of luggage, handbags, saddles, harness and footwear Tanning and dressing of leather, manufacture of luggage, handbags, saddles, harness and footwear - chrome (mg/l) - if chrome tanning agents are used - aluminium (mg/l) - if white tanning used - calcium (mg/l) - sodium (mg/l) - sulphates (mg/l) - m- and p-alkalinity (mVal/l) - m- and p-acidity (mVal/l) - toxicity ()
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Activity Specific parameter analysed in this wastewater
Manufacture of basic metals and fabricated metal products Manufacture of basic metals and fabricated metal products
Manufacture of fabricated metal products, except machinery and equipment Depending upon the technology used to protect the metal products, the following need to be determined - all metals present in the different reagents such as preparation, cleaning and activating metal products Fe, Mn, Zn, Cd, Sn, cyanides, F, Cr, etc. coating metals Cr (all forms), Zn, Ni, Ag, Al, Pb, Ti, B, Sn, etc. post processing Cr, Zn, Co, etc. m- and p- alkalinity or acidity (mVal/l) toxicity ()
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  • Flow measurements
  • quality of wastewater irrelevant if quantity not
    known
  • Closed pipe flow
  • magnetic, ultrsonic generally require pipe to be
    kept full
  • Open channel
  • Primary measuring device weir/flume
  • non contacting level measuring device
    radar/ultrasonic
  • easier maintenance, easier to use

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  • Preliminary wastewater testing - quick
    qualitative or semi-quantitative tests, carried
    out by spectroscopic, micro - and macro chemical
    methods.
  • Full program of work based on the preliminary
    results, a methodolgy must be made for the
    analyst to follow when analyzing the samples.

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  • Preliminary testing - allows the analyst to
    correctly determine
  • the amount of water required for testing,
  • the number of special samples to be taken,
  • specific requirements for the taking and storage
    of individual samples,
  • the proper selection of analytical methods, and
  • any links between the presence of one component
    or water property with the absence of an other.

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wastewater sampling strategy
interpretation
wastewater sampling
characterisation
data analysis
prep.
meas.
assess.
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Sampling
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  • Proportional to time. Take the same amount of
    sample (?qconstant) at the same time interval
    (?tconstant) and the composite sample is defined
    by a certain time interval.
  • Proportional to flow.
  • Take different amounts of sample proportional to
    the wastewater flow (?qk?Q) at the same time
    interval (?tconstant)

Figure 4. Different sampling possibilities
  • Take the same amount of sample (?qconstant) at
    different time intervals depending on the
    wastewater flow (?tk?Q).

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Tabela 5. Sample definitions
Sample Sampling method
Grab Sample taken at a certain time and place
Composite A mixture of samples taken to be proportional to the flow
Spatial composite Mixture of samples taken at one general location at various points, e.g. at the aeration basin, the settling tank, etc.
Cumulative Same amount of sample taken at same time intervals.
If the wastewater sample is not representative,
either at the time of sampling or the time of
analysis, even the most careful analysis will not
be useful.
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  • According to the nature of the components that
    need to be determined, samples can be classified
    into two groups
  • samples taken for the determination of
    characteristics and contents which change in
    contact with air, and
  • samples taken for the determination of properties
    that do not change in contact with air.

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Water samples for air-sensitive parameters
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  • Require the use of specific sampling methods - to
    avoid sample contact with air, sample containers
    must be immediately sealed or conserved.
  • Separate samples must be taken for the
    determination of air sensitive components, such
    as acidity/alkalinity, ammonia and ammonium
    ions, CO2, Fe2 and Fe3, dissolved oxygen,
    nitrites, residual chlorine, chlorine demand, pH,
    hardness, phenols, H2S and sulphides, SO2,
    sulphites and bisulphites.
  • It is even necessary to carry out some analyses
    on the spot, during or immediately after taking
    the sample (dissolved gases, pH, suspended
    solids).

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Water samples for air-non sensitive parameters
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  • Composite sample is usually taken - it is still
    necessary to take precautions against possible
    contamination of the sample solids from the air.
  • From one composite sample, the following
    parameters may be determined organic substances,
    suspended solids, nitrates, phosphates, calcium
    and magnesium, sulphates, total iron and other
    metals.
  • Separate samples are taken for the determination
    of substances extracted by some solvent (grease,
    suspended matter, detergents).

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  • Samples taken for wastewater parameters which do
    not change in contact with the air may or may not
    be filtered prior to analysis, depending on the
    nature and quantity of insoluble material, and
    the applied method of measurement.
  • According to the purpose of the investigation and
    the components to be determined, analysis might
    include
  • only the aqueous phase,
  • only the solid phase, or
  • the entire system.

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  • For the analysis of gaseous wastewater components
    (oxygen, CO2, H2S), prior filtration of the
    sample is not allowed, in order to prevent the
    loss of these components.
  • If filtration is not allowed, as outlined in the
    analytical method, the precipitate may be
    separated by centrifugation, clarification by
    standing, etc.

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  • An intelligent and meaningful concept of
    laboratory analysis includes

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  • Today, there are many known methods for the
    qualitative detection and quantitative
    determination of pollutants in wastewater, and
    they are continuously improving.
  • The choice of method depends on the
  • purpose and goals of the wastewater investigation
    and the information desired,
  • from the concentration of components determined
    (the maximum allowable concentrations of
    pollutants prescribed by regulations are often
    highly relevant),
  • the type of results required (approximate,
    accurate and correct results),
  • the instrument and chemicals that are available,
  • to possible analytical limitations due to
    interference and others.

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Methods can be classified according to their
purpose
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  • Reference (standard) methods
  • Rapid or screening methods
  • Routine methods
  • Automated methods
  • Modified methods

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Reference (standard) methods
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  • Standards of the International Organization for
    Standardization (ISO),
  • Standard Methods for the Examination of Water and
    Wastewater published by the American Public
    Health Organization (APHA),
  • American Waterworks Association (AWWA)
  • Water Pollution Control Federation (WPCF),
  • Environmental Protection Agency (EPA) .

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Rapid or screening methods
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  • used for preliminary testing of a large number of
    samples, as an expedient means of determining
    whether any sample must be subjected to
    additional testing with more accurate methods.

Routine methods
  • official or standard, but may be modified to be
    better suited for application with a large number
    of similar samples.

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Automated methods
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  • using automated equipment, which can also be
    official or rapid methods.

Modified methods
  • can be are official or standard methods that have
    been modified in order to simplify them or adapt
    them to different types of samples from the
    original planned method, or to remove abnormal
    interfering substances.

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  • Non-standard methods, and those that are
    published by reputable scientific journals or
    research companies.
  • The choice of optimal method is very important
  • compliance with the quality assurance program
    based on scientific and technical information,
  • consideration of practical requirements
  • (time and cost of wastewater analysis, the
    accuracy and precision of analytical instruments,
    and the experience and skills of the analyst,
    etc).

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  • Simple, quick and inexpensive determination of
    multiple parameters .

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  • If there is a choice between several good
    methods, preference is given to
  • the method recommended by the relevant
    international organizations,
  • methods validated by interlaboratory tests
    conducted in accordance with international
    protocols,
  • methods validated in the required concentration
    range,
  • methods which are often applied, are simple, fast
    and economical,
  • methods applicable to samples similar to those
    investigated,
  • methods applicable to different sample types, and
    materials and
  • methods which allow for the traceability of each
    result.

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Analytical method selection
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The most important quality parameters of an
analytical method
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  • Accuracy is defined as the degree of agreement
    with the actual measured or expected value.
  • Accuracy is measured by comparing the response of
    the method to the real value, and is expressed as
    the recovery.
  • Analysis of a Certified Reference Material CRM
  • Determination of percentage yield - Recovery
  • Comparison with other methods already confirmed
    to be accurate

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  • Precision is the degree of mutal agreement
    between individual measurements made under the
    same conditions.
  • Can be expressed using different statistical
    indicators
  • standard deviation,
  • relative standard deviation (RSD).

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Limit of Detection (LoD) and Limit of
Quantitation (LoQ)
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  • Instrument detection limit (IDL) the
    concentration of analyte that gives a signal five
    times the signal/noise ratio
  • Method detection limit (MDL, LoD) lowest
    concentration of an analyte which can be measured
    and reported with 95 confidence that the analyte
    concentration is greater than zero.
  • Criterion of detection CD t0.95(f) Sbl v (1
    1/n)
  • Limit of detection LoD 2 CD
  • t0.95 from Students table
  • (f) number of measurements used for Sbl
  • Sbl - standard deviation of blank
  • n number of blanks during routine analysis (2)

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  • Practical quantitation limit (PQL, LoQ), the
    lowest concentration that can be determined
    reliably in the laboratory using routine
    procedures.
  • LoQ Xaverage blank 10 Sbl
  • LoQ Xaverage blank 5 LoD
  • Xaverage blank average value of blank or sample
    with extremely low level of analyte
  • Sbl standard deviation of blank

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  • Specific methods allow determination of one
    analyte, irrespective of the presence of other
    components
  • Selective methods allow for the determination of
    more than one similar analytes at the same time,
    irrespective of the presence of other potentially
    interfering components
  • May be necessary to remove or mask such
    interferences.

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  • Method sensitivity characterises a method or
    instruments ability to differentiate two
    different concentrations of an analyte at a
    certain degree of confidence.
  • Sensitivity is expressed by the slope of the
    calibration curve
  • y f(x), which expresses the relation between
    the output signal and analyte concentration.

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  • Linearity within the working range of the method,
    the analytical signal should have a linear
    dependence on the analyte concentration.
  • Linearity determined by drawing a calibration
    curve
  • At least 6 points required
  • Each point should be replicated at least twice
  • Validation of the method should encompass the
    entire linear

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  • Repeatability is the property of a method
    describing how close the results of repeated
    consecutive measurements of the same analyte are,
    using the same procedure, analyst, instrument,
    place and within a short time period.
  • Reproducibility is the property of a method
    describing how close the results of repeated
    measurements of the same analyte are, using a
    different analyst, different reference standards,
    and different instruments and laboratories, over
    a longer period of time.

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  • Analytical robustness describes how sensitive a
    method is to slight changes in conditions such as
    temperature, pH, reagent concentrations,
    reaction times, etc.
  • The more robust a method, the less like it is to
    be overly sensitive to small variations in
    laboratory conditions.

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After validation
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  • Permanent control of experimental conditions to
    maintain method performance at an established
    level
  • Internal controls of LoD, accuracy, precision,
    comparison with results from authorised methods
  • Validation must be repeated whenever a method is
    modified or changed (extension of range,
    different reagents, additional matrices, etc)

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ANALYTICAL PUZZLE
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Hvala na pažnji! Thank you for your
attention! Köszönöm a figyelmet!
Presentation/lecture has been produced with the
financial assistance of the European Union. The
content of the presentation/lecture is the sole
responsibility of University of Novi Sad,
Faculty of Technology and can under no
circumstances be regarded as reflecting the
position of the European Union and/or the
Managing Authority.
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