Prepared By:epa.ie/licences/lic_eDMS/090151b2801f649a.pdfA: SOP 001: Determination of Suspended...

WASTEWATER TREATMENT PLANT

TESTING PROCEDURES AND MONITORING SCHEDULE 2006 -2007

Prepared By: -

Environment Section, Westmeath County Council,

County Buildings, Mullingar,

Co. Westmeath.

JUNE 2006

Wastewater Treatment Plant TESTING PROCEDURES AND MONITORING SCHEDULE

2006 -2007

Approval Sheet.

Name Title Date

Murty H a n k

Sean O'Laoide

Revision History.

Rev No Change control record No

Details Effective Date Authors Name

00 New Anne Bonner

Circulation. Area Engineers Relevant DOS

STANDARD OPERATING PROCEDURES

A: SOP 001: Determination of Suspended Solids.

B: SOP 002: Determination of PH

C: SOP 003: Determination of Sludge Volume Index

D: SOP 004: Determination of Dissolved Oxygen.

E: SOP 005: Determination of the Biological Oxygen Demand.

F: SOP 006: Determination of the Chemical Oxygen Demand.

G: SOP 007: Determination of Ammonium in Liquids.

H: SOP 008: Determination of Nitrate.

I: SOP 009: Determination of Orthophosphate.

J: SOP 010: Determination of Total Phosphorus.

K: SOP 011: Determination of Total Kjeldahl Nitrogen.

L: SOP 012: Determination of Total Nitrogen.

M: SOP 013: Determination of the Method of Detection Level.

N: SOP 014: Construction and Analysis Control Charts.

0: SOP 015: Collection of Samples Procedure and Schedule for Sampling and

Testing of the Wastewater treatment Plants in County Westmeath.

Standard Operating Procedures Number 001 Rev. 03

Page 1 of 3

Title Standard Operating Procedures for the determination of Suspended Solids

Written By :Anne Bonner Rev By: Darran Killian Approved By :

1.0 Introduction

Wastewater suspended solids may be determined by filtering a sample through a glass fibre filter disk. The residue retained in the filter is dried to constant weight at 103-105°C. The suspended matter determination is extremely valuable in the analysis of wastewaters. Laboratory determination of suspended solids in the influent; aeration basins and final effluent are standard measurements used to indicate treatment plant efficiency. This procedure is performed as per Standard Methods for the examination of Wastewater and water (20th edition)

2.0 Responsibility

It is the responsibility of the Executive Scientific Officer to ensure that the laboratory technicians execute the procedure.

3.0 Laboratory Equipment

Glass Fibre filter disk. Filtration Apparatus. Reagent grade water. Suction flask of sufficient capacity for sample size collected. Vacuum pump. Dessicator with desiccant containing a colour indicator of moisture concentration. Drying oven at 103-105 °C. Glass pipette. Weighing balance

4.0 Laboratory Procedure 4.1 Preparation of glass —fibre filter disk 4.1.1 Insert disk in filtration apparatus (wrinkled side up). 4.1.2 Apply vacuum and wash disk with three successive 20ml portions of reagent

grade water continue suction to removes all traces of water, and discard washings.

4.1.3 Remove filter from filtration apparatus and transfer to oven 4.1.4 Dry in oven at 103-105 °C for 1 hour 4.1.5 Cool in dessicator to balance temperature and weigh 4.1.6 Repeat cycle of drying, cooling, desiccating and weighing until a constant weight is

obtained. 4.1.7 Store in dissector until needed


Page 2 of 3



4.2 Collection and Preservation of Samples

Refer to Stand Methods For The Examination Of Water And Wastewater 20th Edition

4.3 Selection of filter and sample size. 4.3.1 Choose sample volume to yield between 2.5 and 200mg dried residue 4.3.2 If volume filtered fails to meet minimum yield increases volume up to 1000mI 4.3.3 If complete filtration takes longer than 10 minutes, increase filter size or decrease

volume filtered 4.4 Sample Analysis. 4.4.1 Assemble filtering apparatus and filter and begin suction 4.4.2 Wet filter with a small volume of reagent water to seal it 4.4.3 Shake sample thoroughly and using a graduated cylinder pour a measured

volume onto the sealed glass fiber filter. 4.4.4 Wash with three successive 10mI volume of reagent water, using a wash bottle

allowing complete drainage between washings, and continue suction for about three minutes after filtration is complete

4.4.5 Carefully remove filter from filtration apparatus. 4.4.6 Dry for at least one hour at 103-105 °C in an oven, cool in a dessicator to

balance temperature and weigh 4.4.7 Calculate results using the following equation

mg total suspended solids/L = (A-B)*1000 Sample vol.

Where

A= weight of filter + dried residue, (mg) B = weight of filter, (mg)

4.4.8 Record results on appropriate data sheets


Page 3 of 3



5.0 Calibration See Calibration Standard operating procedure

6.0 Quality/Technical Knowledge Method: See Standard methods 2540D, Edition 20th, 1998 Interferences: see Standard methods 2540A.2,2540B.1 and 2540D.1 b. 7.0 Safety/Environmental Gloves, safety glasses and appropriate PPE must be worn during sampling and sample handling Wastes generated must be handled and disposed of in an appropriate manner

Change Control Record

SOP No.

SOP REV No.

Change originated from Change authorised by Details of Change

SOP Title

D t


Page 1 of 2

Title Standard Operating Procedures for the determination of pH in wastewater using the Orion 720A

Written By :Anne Bonner Rev By: Darran Killian Approved By:

1.0 Introduction

Practically every phase of water supply and wastewater treatment, e.g. acid-base neutralisation, water softening, precipitation, coagulation, disinfections, and corrosion controls pH dependant. At given temperature the intensity of the acidic or basic character of a solution is indicated by pH or Hydrogen ion activity.

A pH meter consists of a potentiometer, a glass electrode, a reference electrode and a temperature-compensating device. A circuit is completed though the potentiometer when the electrodes are immersed in the test solution. The pH 720A is capable of reading pH or millivolts and has a scale expansion that permits reading to 0.01 pH Unit This procedure is performed as per Standard methods for the Examination of Wastewater and water (20th Edition)

2.0 Responsibility



pH Meter (Orion 720A) 150m1 glass beaker. Buffer solutions (pH 4, 7, 10) Distilled water. Magnetic Stirrer

4.0 Procedure 4.1 Calibration Procedure

4.1.1 See Calibration Standard Operating Procedure



4.3 Test Procedure


Page 2 of 2

Title Standard Operating Procedures for the determination of pH in wastewater using the Orion 720A

Written By :Anne Bonner Rev By: Darran Killian Approved By:

4.3.1 Place sample into a clean 250m1 glass beaker. 4.3.2 Add a stirring bar. 4.3.3 Place the beaker on top of a magnetic stirrer. 4.3.4 Place the electrodes in sample solution and record the pH value when READY is

indicated or when the electrode signal is stable. Temperature is displayed in the prompt line.

4 Quality /Technical Knowledge

Method: See Standard Methods, Section 4500-H B, Edition 20th 1998 and Instruction manual for pH 720A Orion pH meter

Trouble Shooting: See Standard Methods, section 4500-H B (5), Edition 20th, 1998 and the Instruction manual for the pH 720A Orion pH meter pg 51-57

5 Safety/ Environmental

Gloves, safety glasses and appropriate PPE must be worn during sampling and sample handling

6 Appendix

Calibration Record for Orion 720A PH monitoring results should be placed in appropriate data sheets.

Change Control Record SOP No

SOP REV No. Change originated from

Change authorised by

Details of Change

SOP Title

Date

Standard Operating Procedures Number WWT-003 Rev:001

Page l of 4

Title Standard Operating Procedures for the determination of Sludge Volume Index in wastewater

Written by: Anne Bonner Approved by:

1.0 Introduction The sludge volume index (SVI) is the volume in millimeters occupied by 1g of a suspension after 30 min settling. SVI typically is used to monitor settling characteristics of activated sludge and other biological suspensions. This procedure is performed as per Standard methods for the Examination of Water and Wastewater (20th Edition) 2.0 Responsibility It is the responcibility of the Executive Scientific Officer to ensure that the laboratory technicicans execute the procedure. 3.0 Laboratory Equipment. Drying oven set at 103°C-105°C Analytical Balance Dissector with desiccant containing a color indicator of moisture concentration Glass fibber filter disks GFC 70mm Filtration Apparatus Suction Flask of sufficient capacity for sample size collection Vacuum Pump Reagent water One Litre Imhoff Cone. Stopwatch 4.0 Laboratory Procedure.

4.1 General Procedure 4.2 Frequency of testing 4.3 Sample Analysis

4.1 General Procedure

Determine the 30 min settled sludge volume

4.1.1 Fill an imhoff cone to 1L mark with a well-mixed sample from the aeration tank.

4.1.2 Settle for 30 min. 4.1.3 Record volume of settled solids in the cone in millimeters per litre. 4.1.4

Standard Operating Procedures Page 2 of 4 Number WWT-003 Rev 001 Title Standard Operating Procedures for Written by: Anne Bonner the determination of Sludge Volume Index Approved by: in wastewater

If the settled matter contains pockets of liquid between large particles, estimate volume of these and subtract from the total volume. The practical lower limit of measurement depends on sample composition and generally is in the range of 0.1-1.0 ml/I where separation of settable materials occur do not estimate the floating material as settable material.

Step 4

Calculation.

MI settleable solids/I = ml total suspended solids/I – ml solids/1

3.1.1 Frequency

Daily

3.1.2 Tools

3.1.3 Support N/A

•

Standard Operating Procedures Page 3of 4 Number WWT-003 Rev 001 Title Standard Operating Procedures for Written by:Anne Bonner the determination of Sludge Volume Index Approved by: in wastewater

Test Procedure

Step 1

Determine the suspended solids concentration of a well-mixed sample of the suspension (SOP WWT001) 3.2 Task # 2 Determine the 30 min settled sludge volume

3.2.1 Frequency

Daily 3.2.2 Tools Imhoff Cone Stirring Rods 3.2.3 Support N/A

Test Procedure Step 1 Fill an imhoff cone to 1 L mark with a well-mixed sample from the aeration tank Step 2 Settle for 30 min, Record volume of settled solids in the cone in millimeters per litre. Step 3 If the settled matter contains pockets of liquid between large particles, estimate volume of these and subtract from the total volume. The practical lower limit of measurement depends on sample composition and generally is in the range of 0.1-1.0 ml/I where separation of settable materials occur do not estimate the floating material as settable material. Step 4 Calculation

Standard Operating Procedures Page 4of 4 Number WWT-003 Rev 001 Title Standard Operating Procedures for Written by: Anne Bonner the determination of Sludge Volume Index Approved by: in wastewater

MI settleable solids/I = ml total suspended solids/I – ml solids/I

3.2 Task # 3 Calculation of Sludge Volume Index

3.2.1 Frequency

Daily

3.2.2 Tools

Results from the determination of suspended solids (mg/1) and settled sludge volume index (ml/1)

3.2.3 Support N/A

Test Procedure

Step 1

Calculation

SVI = Settled sludge volume (ml/I *100 Suspended Solids mg/I

Step 2

Record results on appropriate log sheets as attached

5.0 Quality/ Technical Knowledge

Precision is determined by the precision achieved in the suspended solids measurement, the settling characteristics of the suspension and variables associated with the measurement of the settled sludge volume. Method See Standard Methods Sections 2710 d, Edition 18th, 1992.

6.0 Safety/ Environmental

Gloves safety glasses and appropriate PPE must be worn during sampling and sample handling Wastes generated must be handled and disposed of properly

Change control Record Change Control Record No 99/1

SOP No

SOP REV No.

Change originated from

Change authorised by Details of Change

SOP Title

Date

Standard Operating Procedures Page 1 of 3 Number 004 Rev.02 Standard Operating Procedures for the Written by: Anne Bonner Determination of the Dissolved Rev By Darran Killian Oxygen. Approved b :

1.0 Introduction

Dissolved Oxygen (DO) levels in liquids depend on the physical, chemical and biological activities in the liquid. The analysis for DO is a key test in wastewater treatment process control. Membrane electrodes provide an excellent method for DO analysis in strong wastewater. In membrane electrodes the diffusion current is linearly proportional to the concentration of molecular oxygen. The current can be converted easily to concentration units (e.g. mg/1) by a number of calibration procedures. This procedure is performed as per the Standard Methods for the analysis of waters and waste waters (18th edition). DO should preferably be measured using an electrode membrane at the sampling site. It should be noted that a delay in DO analysis leads to meaningless and grossly misleading results.

2.0 Responsibility

It is the responsibility of the Executive scientific officer to ensure that the laboratory technicians execute this procedure.


CellOx 325 DO probe InoLab Oxi Level 2 DO meter OxiCal —SL air calibration vessel Magnetic Stirrer

4.0 Laboratory Procedures

4.1 Calibration of DO meter & probe. 4.1.1 Connect the DO probe to the meter 4.1.2 Put the D.O. probe into the air calibration vessel (the

sponge in the air calibration vessel must be moist not wet)

4.1.3 Press the "CAL" key repeatedly until the calibration mode appears

4.1.4 Press the "Run/Enter" key. Auto read is activated, AR flashes.

4.1.5 As soon as a stable value is reached, AR stops flashing. Thus the calibration is finished and the probe symbol indicates the relative slope determination and probe evaluation.

4.1.6 Press "M" key to change to the measuring mode.


4.2 Determination of DO of a sample 4.2.1 Switch on the DO meter, and calibrate as per section 4.1

4.2.2 Press the "M" key until the oxygen concentration is displayed in mg/I

4.2.3 Immerse the probe into the sample, add a stirring bar and place sample on top of magnetic stirrer.

4.2.4 When the reading on the DO meter has stabilised, record this results as actual DO result.

4.3 Maintenance of DO Probe

4.3.1 Disconnect probe from meter 4.3.2 Unscrew membrane head. 4.3.3 Rinse probe head with deionised water. 4.3.4_ Clean counter electrode carefully with a paper towel and

dry it. 4.3.5 Immerse probe head including the counter electrode into

cleaning solution RUG for 1 to 3 min 4.3.6 Rinse probe head several times with deionised water.

4.3.7 Water counter electrode for at least 10 min in distilled water

4.3.8 Shake off water droplets 4.3.9 Moisten new membrane with some drops of electrolyte

solution ELY/G 4.3.10 Fill membrane head with electrolyte solution 4.3.11 Remove air bubbles by carefully knocking 4.3.12 Rinse probe head with electrolyte solution. 4.3.13 Screw Probe head onto the shaft 4.3.14 Hold sensor inclined, excess solution is pushed out 4.3.15 Screw on probe head finger tight with a paper towel 4.3.16 The filling should possibly be free of air bubbles.

5.0 Quality / Technical knowledge

Method: See standard methods, section 4-129 (4500-OG) 20th Edition. And instruction manual for CellOx 325 DO probe and InoLab Oxi Level 2 DO meter.


6.0 Safety / Environment

Gloves, Safety Glasses and appropriate PPE must be worn during sampling, and sample handling.

7.0 Appendix

See data sheet plant monitoring calibration sheet for CellOx325 DO probe and InoLab Oxi Level 2 DO meter.

Standard Operating Procedures Page 1 of 7 Number 005 Rev.02 Standard Operating Procedures for the Written by: Anne Bonner Determination of the Biological Oxygen Rev By Darran Killian Demand. Approved by:

1.0 Introduction

The Biochemical Oxygen Demand (BOD) determination is a test in which

standardised laboratory procedures are used to determine the relative

oxygen requirements of waste waters effluents and polluted waters. The

test measures the molecular oxygen utilised during a specified incubation

period for the biochemical degradation of organic material (carbonaceous

demand) and the oxygen used to oxidise inorganic materials such as

sulphides and ferrous iron. It also may measure the amount of oxygen used

to oxidise reduced forms of nitrogen unless their oxidation is prevented by

an inhibitor.

2.0 Responsibility

It is the responsibility of the Executive scientific officer to ensure that the

laboratory technicians execute this procedure.


Cell-Ox 325 DO probe

InoLab Oxi Level 2 DO meter

OxiCal –SL air calibration vessel

Magnetic Stirrer

Incubator set @ 20°C and dark

BOD bottles and lids

Standard Operating Procedures Page 2 of 7 Number 005 Rev.02 Standard Operating Procedures for the Written by: Anne Bonner Determination of the Biological Oxygen Rev By Darran Killian Demand. Approved by:

4.0 Laboratory Procedures

4.1 Calibration of DO meter & probe.

4.1.1 Connect the DO probe to the meter

4.1.2 Put the D.O. probe into the air calibration vessel (the

sponge in the air calibration vessel must be moist not

wet)

4.1.3 Press the "CAL" key repeatedly until the calibration mode

appears

4.1.4 Press the "Run/Enter" key. Auto read is activated, AR

flashes.

4.1.5 As soon as a stable value is reached, AR stops flashing.

Thus the calibration is finished and the probe symbol

indicates the relative slope determination and probe

evaluation.

4.1.6 Press "M" key to change to the measuring mode.

4.2 Determination of DO of a sample

4.2.1 Switch on the DO meter, and calibrate as per section 4.1

4.2.2 Press the "M" key until the oxygen concentration is

displayed in mg/I

4.2.3 Immerse the probe into the sample, add a stirring bar and

place sample on top of magnetic stirrer.

4.2.4 When the reading on the DO meter has stabilised; record

this results as actual DO result.

Standard Operating Procedures Page 3 of 7 Number 005 Rev.02 Standard Operating Procedures for the Written by: Anne Bonner Determination of the Biological Oxygen Rev By Darran Killian Demand. Approved b :

4.3 Maintenance of DO Probe

4.3.1 Disconnect probe from meter

4.3.2 Unscrew membrane head.

4.3.3 Rinse probe head with deionised water. 4.3.4 Clean counter electrode carefully with a paper towel and dry it.

4.3.5 Immerse probe head including the counter electrode into cleaning solution RL/G for 1 to 3 min

4.3.6 Rinse probe head several times with deionised water.

4.3.7 Water counter electrode for at least 10 min in distilled water

4.3.8 Shake off water droplets

4.3.9 Moisten new membrane with some drops of electrolyte solution ELY/G

4.3.10 Fill membrane head with electrolyte solution

4.3.11 Remove air bubbles by carefully knocking

4.3.12 Rinse probe head with electrolyte solution.

4.3.13 Screw Probe head onto the shaft

4.3.14 Hold sensor inclined, excess solution is pushed out

4.3.15 Screw on probe head finger tight with a paper towel

4.3.16 The filling should possibly be free of air bubbles.


4.4 Sampling and storage

4.4.1 Grab Samples

4.4.1.1 If analysis is begun within 2h of collection,

cold storage is unnecessary. If analysis is not

started with 2 hours of sample collection, keep

samples at or below 4°C and report length and

temperature of storage with the results. In no case

start analysis more than 24hour after grab sample

collection.

4.4.2 Composite Samples

4.4.2.1 Keep samples at or below 4°C during

compositing. Limit compositing period to 24hours.

Use the same criteria as for the storage of grab

samples.

4.5 Analysis

4.5.1 Sample pre treatment

4.5.1.1 Check pH of sample to ensure pH is

between 6 and 8.5. Alter pH with sulphuric acid or

sodium hydroxide of such strength that the quality

of reagent does not dilute the sample by more than

0.5%. Always seed samples that have been pH

adjusted.


4.5.1.2 If samples have been chlorinated but have

no detectable chlorine level, seed the dilution

water. If residual chlorine is present, dechlorinate

the sample and seed dilution water.

4.5.1.3 Samples containing more than 9mg/I DO at

20°C may be encountered in cold waters or in

waters where photosynthesis has occurred. To

prevent loss of oxygen during incubation reduce

DO to saturation at 20°C by bringing sample to

20°C while aeration with clean air source.

4.5.1.4 Bring sample to 20°C +/- 1°C before making

dilutions.

4.5.1.5 If nitrification inhibition is required, add 3mg 2-

chloro-6-(trichloro methyl) pyridine to each 300ml

BOD bottle.

4.5.2 Dilution

4.5.2.1 Make several dilutions of sample that will

result in a residual DO of at least 1 mg/I and a DO

uptake of at least 2mg/I after a 5day incubation.

4.5.3 Determination of initial DO

4.5.3.1 Determine initialDO using methods

described in section 4.2


4.5.4 Dilution Water Blank

4.5.4.1 Use a dilution water blank as a rough check

on quality of unseeded dilution water and

cleanliness of incubation bottles. Together with

each batch of samples incubate a bottle of

unseeded dilution water. The DO uptake should

not be more than 0.2mg/I

4.5.5 Incubation

4.5.5.1 Incubate bottles at 20°C +/- 1 °C for 5 days

in a dark container.

4.5.6 Determination of final DO

4.5.6.1 Determine final DO using method described

in section 4.2

4.5.7 Calculations

4.5.7.1 Where water is unseeded BODS = (D1-

D2)/P

4.5.7.2 Where water is seeded BOD 5 = ((D1-D2)-

(B1-B2)f) / P

Where..

D1 is the DO of diluted sample immediately after

preparation


D2 is the DO of diluted sample after 5d incubation at

20oC

P is the decimal volumetric fraction of sample used

B1 is the DO of seed control before incubation

B2 is the DO of seed control after incubation

F is the ration of seed in diluted sample to seed in seed

control

5.0 Quality / Technical knowledge

Method: See standard methods, section 5210 201h Edition. And instruction

manual for CellOx 325 DO probe and InoLab Oxi Level 2 DO meter.

6.0 Safety / Environment

Gloves, Safety Glasses and appropriate PPE must be worn during

sampling, and sample handling.

Standard Operating Procedures Page 1 of 2 Number 006 Rev. 003 Standard Operating Procedures for the Written by: Anne Bonner determination of Chemical Oxygen Rev By: Darran Killian Demand Approved by:

1.0 Introduction

Chemical oxygen demand (COD) is defined as the amount of a specific oxidant that reacts with the sample under controlled conditions. The quantity of oxidant consumed is expressed in terms of its oxygen equivalence. This procedure is performed in Standard Methods for the examination of water and Wastewater, (20th Edition)

2.0 Responsibility



HACH DR/2400 Spectrophotometer HACH COD Reactor COD reagent vials. Distilled water. 2ml glass pipette.

• 4.0 Laboratory Procedure



4.2 Instrument set-up.

4.2.1 Touch "HACH PROGRAMS" on screen of DR/2400 4.2.2 Select program "430 COD LR" (0mg/I – 150mg/I COD) or "435 COD HR" (0mg/I – 1500mg/1). 4.2.3 Touch "START" on screen of DR/2400.

Standard Operating Procedures Page 2 of 2 Number 006 Rev. 003 Standard Operating Procedures for the Written by: Anne Bonner determination of Chemical Oxygen Rev By: Darran KillianDemand Approved by:

4.3 Sample Analysis

4.3.1 Homogenize sample for 30 seconds in a blender 4.3.2 Preheat COD reactor to 150°C 4.3.3 Add 2ml of sample to appropriate ranged vial. 4.3.4 Add 2ml of distilled water to appropriate ranged vial (blank). 4.3.5 Immediately cap and invert to mix. 4.3.6 Place the vials in the COD reactor for 120 minutes. 4.3.7 After 120 minutes allow the vials to cool to room temperature.

4.3.7.1 Clean the outside of the "blank" vial and insert it into the HACH spectrophotometer. Touch "Zero" on the screen.

4.3.7.2 Clean the outside of the "sample" vial and insert it into the HACH spectrophotometer. Touch "Read" on the screen.

4.4 Calibration.

See Calibration Standard Operating Procedure.


Method See Standard methods Sections 5220-A. Edition 20th, 1998 Also see hand book on HACH DR/2400 Spec, Method 8000(Oxygen Demand, Chemical)


Gloves, safety glasses and appropriate PPE must be worn during sampling and sample handling Wastes generated must be disposed of correctly


SOP No



Details of Change

SOP Title

Date

Standard Operating Procedures Page 1 of 2 Number 007

Rev.003 Standard Operating Procedures for the Written by: Anne Bonner determination of Ammonium in liquids Rev by: Darran Killian

Approved b :

1.0 Introduction

Nitrogen can be found in nature, in the form of ammonium (NH4'). Nesslers reagent will combine with ammonium ions to form a characteristic yellow colour, which is measured at 425nm.

2.0 Responsibility



HACH DR/2400 Spectrophotometer. 25ml Sample Cells. Mineral stabiliser. Polyvinyl Alcohol Dispersing Agent. Nesslers Reagent. Distilled Water. 25ml Graduated cylinder. 1 ml Pipette Pipette bulb

4.0 Laboratory Procedure 4.1 Sample collection and preservation.


4.2 Sample Analysis

4.2.1 Touch "HACH PROGRAMS" on screen of DR/2400 4.2.2 Select program "380 N, Ammonia, Ness" 4.2.3 Touch "START" on screen of DR/2400. 4.2.4 Convert expression of result on screen from NH3-N to NH4

+ 4.2.4 Fill a 25ml graduated cylinder with sample 4.2.5 Fill a 25ml graduated cylinder with distilled water. (blank) 4.2.6 Add three drops of mineral stabiliser to each cylinder, and mix.

Standard Operating Procedures Page 2 of 2 Number 007

Rev.003 Standard Operating Procedures for the Written by: Anne Bonner determination of Ammonium in liquids Rev by: Darran Killian

Approved b :4.2.7 Add three drops of polyvinyl alcohol dispersing agent to each cylinder and mix. 4.2.8 Pipette 1 ml of Nesslers reagent into each cylinder and mix. 4.2.9 Touch the timer icon to begin a one minute countdown. 4.2.10 Pour each solution into a round sample cell. 4.2.11 When the timer beeps, place the blank into the cell holder. 4.2.12 Touch "ZERO" the display will show 0.00mg/I NH3-N 4.2.13 Place the prepared sample cell into the cell holder. 4.2.14 Touch "READ" the result will appear on screen.

4.3 Calibration.

Refer to Calibration standard operating procedure


Also see hand book on HACH DR/2400 Spec, Method 8038, Nitrogen, Ammonia (Nesslers method)



Wastes generated must be disposed of correctly


SOP No



Details of Change

SOP Title

Date

Standard Operating Procedures Page 1 of 2 Number 008 Rev 003 Title Standard Operating Procedures for Written by: Anne Bonner the determination of Nitrate Approved by:

1.0 Introduction

Cadmium metal reduces nitrates in the sample to nitrite. The nitrite ion reacts in an acidic medium with sulfanilic acid sulfanilic acid to form intermediate diazonium salt. The salt couples with gentisic acid to form an amber coloured solution.

2.0 Responsibility

It is the responcibilty of theExecutive Scientific officer to ensure that the laboratory technicians execute the procedure.


HACH Spectrophotometer DR/2400. NitraVer Nitrate Reagent 25ml sample cell. Distilled water.

4.0 Laboratory Procedure

4.1 Sample Preservation.

4.1.1 Collect samples in clean glass or plastic bottles 4.1.2 Cool samples may be stored for up to 24 hours at 4°C or lower.

4.1.3 To store for longer periods add 2ml of Conc. Sulphuric acid to every litre of sample, and store at 4°C or lower.

4.1.4 Warm samples to room temperature, and adjust pH to 7 with 5N ® Sodium Hydroxide before analysis.

4.1.5 Correct the test result for volumne additions by dividing the total volumne (acid+base+sample) by the original volumne and multiplying the result by this factor.

4.2 Sample Analysis.

4.2.1 Touch "Hach Programs" on screen. 4.2.2 Select program "355 N, Nitrate HR". 4.2.3 Touch "Start" on screen. 4.2.4 Fill a round sample cell with 25ml of sample. 4.2.5 Add the contents of one NitraVer Nitrate Reagent powder pillow to

the sample cell. 4.2.6 Touch the timer icon 4.2.9 Touch "OK" (a one minute timer begins) 4.2.10 Shake the cell vigorously until the timer beep

Standard Operating Procedures Page 2 of 2 Number 008 Rev 003 Title Standard Operating Procedures for Written by: Anne Bonner the determination of Nitrate Approved by:

4.2.11 When the timer beeps, touch the timer icon again. 4.2.12 Touch "OK" (a five minute timer begins) 4.2.13 When the timer beeps, fill a second cell with 25ml of sample (this is

the blank). 4.2.14 Wipe the Blank sample cell and place it into the Hach DR/2400 4.2.15 Touch "Zero" 4.2.16 Wipe the prepared sample and place it in the Hach DR/2400 4.2.17 Touch "Read" 4.2.18 Result is expressed as mg/I NO3

--N

4.3 Accuracy test

4.3.1 For proof of accuracy, use a Nitrate Nitrogen Standard Solution in place of the sample.

5 Quality/ Technical Knowledge

METHOD see Standard Methods Sections 4500-NO3-E. , Edition 20th, 1998. Also see handbook on HACH DR/2400 Spec, method 8039. 6 Safety/ Environmental

Gloves, safety glasses and appropriate PPE must be worn during sampling and sample handling. Wastes generated must be handled and disposed of properly

Change Control Record No 99/1

SOP No


Change authorised by Details of Change

SOP Title

Date

Standard Operating Procedures Page 1 of 2 Number 009 Rev.003 Title Standard Operating Procedures for Written by: Anne Bonner the determination of Ortho-phosphate in Approved by: liquids

1.0 Introduction

Ammonium molybdate and potassium antimonyl tartrate react in acid medium with orthophosphate to form a heteropoly acid – phosphomolybdic acid – that is reduced to intensely colored molybdenum blue by ascorbic acid This procedure is performed in Standard Methods for the examination of water and Wastewater, (20th Edition)

2.0 Responsibility



HACH DR/2400 Spectrophotometer 25ml Sample Cells PhosVer 3 Phosphate Reagent Distilled Water. 1:1 Hydrochloric acid Solution Pre washed and dried filter paper



4.2 Sample Analysis

4.2.1 Touch "HACH PROGRAMS" on screen of DR/2400. 4.2.2 Select program "490 P Reactive PV". 4.2.3 Touch "START" on screen of DR/2400. 4.2.4 Convert expression of results on screen from mg/I PO43- to mg/I P. 4.2.4 Filter sample and blank, this is necessary if the sample is turbid. 4.2.5 All glassware and sample bottles should be washed in 1:1 hydrochloric acid and

then rinsed in distilled water. 4.2.6 Fill a sample cell with 25ml of sample. 4.2.7 Add the contents of one PhosVer 3 Phosphate Reagent to the cell. 4.2.8 Immediately cap and invert to mix. 4.2.9 Touch the timer icon. A two minute reaction period will begin.

Standard Operating Procedures Page 2 of 2 Number 009 Rev.003 Title Standard Operating Procedures for Written by: Anne Bonner the determination of Ortho-phosphate in Approved by: liquids

4.2.10 Fill another sample cell with 10ml of sample (this is the blank). 4.2.11 When the timer beeps, wipe the blank and place it into the cell holder.

4.2.12 Touch "ZERO" on the screen of the DR/2400. 4.2.13 Wipe the prepared sample and place it in the cell holder. 4.2.14 Touch "READ" on the screen of the DR/2400. 4.2.15 Result will then be displayed as mg/i PO4

3 4.3 Calibration.

Refer to Calibration standard operating procedure


Sample turbidity may interfere with analysis. Remove by filtration before analysis. Method See Standard methods Sections 4500-P E. Edition 20th, 1998 Also see hand book on HACH DR/2400 Spec, Method 8048(Reactive Phosphorous range 0-2.5 mg/1)



Wastes generated must be disposed of correctly


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Standard Operating Procedures Page 1 of 2 Number 010 Rev 02 Standard Operating Procedures for the Written by: Darran Killian determination of Total Phosphorus Rev By: Anne Bonner

Approved b :

1.0 Introduction

Phosphorus can exist in many different forms. The total phosphorus analysis converts organic and inorganic forms of phosphorus to orthophosphate, which can then be analysed using standard operating procedures for orthophosphate.

2.0 Responsibility



HACH DR/2400 Spectrophotometer. Total Phosphorous Test N Tube Reagent set. Distilled water COD Reactor 2ml pipette 5ml pipette

4.0 Laboratory Procedure 4.1 Sample Collection and Preservation


4.2 Sample Analysis 4.2.1 Touch "HACH PROGRAMS" on screen of DR/2400 4.2.2 Select program "536 P Total/AH PV TNT 4.2.3 Touch "START" on screen of DR/2400. 4.2.4 Analysis range is between 0.06 and 3.5mg/I PO4

3 , perform a series of dilutions to ensure that the sample total phosphorous range will be between these values. 4.2.5 Add 5ml of sample to a total and acid hydrolysable test vial.

4.2.6 Add the content of one Potassium persulphate powder pillow for phosphonate to the vial.

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4.2.7 Cap tightly and shake to dissolve. 4.2.8 Place the vials into the preheated COD reactor at 150°C. 4.2.9 Touch the timer icon, a 30 minute heating period will begin. 4.2.10 When the timer beeps, remove the vials from the COD reactor, and allow to cool. 4.2.11 When cooled, ass 2ml of 1.54N NaOH standard solution to the vial. Cap and mix. 4.2.12 Wipe the outside of the vial with a damp cloth, followed by a dry one, to remove

fingerprints or other marks. 4.2.13 Install the 16mm adaptor in the HACH spectrophotometer. 4.2.14 Touch ZERO on the screen, the display will show 0.00 mg/I PO4

3" 4.2.15 Add the contents of one PhosVer 3 powder pillow to the vial. 4.2.16 Cap tightly and shake to mix for 15 seconds. 4.2.17 Touch the timer icon, a two minute reaction period will begin. 4.2.18 After the timer beeps, wipe the outside of the vial and place it in the HACH spectrophotometer. 4.2.19 Touch READ, the result will appear as mg/I PO4

3-

4.3 Calibration.

See Calibration standard operating procedure

4.0 Quality/ Technical Knowledge Also see hand book on HACH DR/2400 Spec, Method 8190, PhosVer 3 with acid persulphate digestion method.



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Standard Operating Procedures Page 1 of 3 Number 011 Rev 02 Title Standard Operating Procedures for Written by: Darran Killian the determination of Total Kjeldahl Rev by: Anne Bonner Nitrogen Approved by:

1.0 Introduction The term Total Kjeldahl Nitrogen refers to the combination of ammonia and organic nitrogen. However, only the organic nitrogen compounds appearing as organically bound nitrogen in the tri-negative are determined in this analysis. Nitrogen in this form is converted into ammonium salts by the action of sulphuric acid and hydrogen peroxide. The ammonia is then analysed by a modified Nessler method test.

2.0 Responsibility



HACH DR/2400 Spectrophotometer HACH Digesdahl Digestion Apparatus 100ml Digesdahl digestion flask. Concentrated Sulphuric Acid Boiling Chips 50% Hydrogen peroxide Distilled Water Filtration apparatus Filter paper. TKN Indicator solution. 8N Potassium Hydroxide 1 N Potassium Hydroxide 25ml Sample cells

• Mineral stabiliser Polyvinyl Alcohol Dispersing agent Nessler Reagent



4

4.2 Sample Digestion

4.2.1 Transfer a pre-measured amount of sample into a 100mI digesdahl digestion flask. See HACH manual for correct volumes

Standard Operating Procedures Page 2 of 3 Number 011 Rev 02 Title Standard Operating Procedures for Written by: Darran Killian the determination of Total Kjeldahl Rev by: Anne BonnerNitrogen Approved b :

4.2.2 Add 3ml of concentrated Sulphuric acid to the volumetric flask and two or more boiling chips.

4.2.3 Turn the temperature dial on the digesdahl apparatus to a heat setting of 440°C 4.2.4 When the proper temperature is reached turn on the water to the aspirator and ensure there is suction to the fractionation column.

4.2.5 Place the flask weight, followed by the fractionating column with funnel on the flask. 4.2.6 Place the flask on the heater and heat until the sulphuric acid boils. 4.2.7 Boil for 4 more minutes. Do not boil to dryness. 4.2.8 Add 10ml of 50% Hydrogen Peroxide to funnel at top of apparatus.

4.2.9 After addition of hydrogen peroxide is complete, boil off excess hydrogen peroxide by heating for one more minute.

4.2.10 Take the flask off the heater and allow the flask to cool 4.2.11 Dilute the digest to 100ml 4.2.12 If the sample has visible turbidity, filter or wait until the turbidity settles. 4.2.13 Digest an equal amount of distilled water as the blank. 4.3 Sample Analysis. 4.3.1 Touch "HACH PROGRAMS" on the screen of the DR/2400 4.3.2 Select program "399 NITROGEN TKN" 4.3.3 Touch "START" on the screen of the DR/2400 4.3.4 Select the appropriate analysis volume of the digested sample (see HACH

manual for correct volume) 4.3.5 Pipette the analysis volume from the sample and the blank into separate 25ml

mixing graduated cylinders. 4.3.6 Add one drop of TKN indicator to each cylinder. 4.3.7 If the aliquot is less than 1 ml proceed to step. 4.3.9 4.3.8 If the aliquot is greater than 1 ml add drops of 8N KOH to each cylinder until the

first flash of blue colour appears. 4.3.9 Add 1 N KOH to each cylinder one drop at a time, until the first permanent blue colour appears. 4.3.10 Fill both cylinders to the 20ml mark. 4.3.11 Add three drops of mineral stabiliser to each cylinder, and mix. 4.3.12 Add three drops of polyvinyl alcohol dispersing agent to each cylinder. 4.3.13 Fill both cylinders to the 25ml mark with distilled water. 4.3.14 Pipette 1 ml of Nesslers Reagent to each cylinder. 4.3.15 Touch the timer icon on the DR/2400. A two minute reaction period will begin, 4.3.16 When the timer beeps, pour the contents of each cylinder into separate 25ml sample cells. 4.3.17 Wipe the blank and place into the cell holder. 4.3.18 Touch "ZERO" on the screen of the DR/2400, the display will show 0mg/I TKN 4.3.19 Wipe the prepared sample and place it into the cell holder. 4.3.20 Touch "READ" on the screen of the DR/2400.

Standard Operating Procedures Page 3 of 3 Number 011 Rev 02 Title Standard Operating Procedures for Written by: Darran Killian the determination of Total Kjeldahl Rev by: Anne BonnerNitrogen Approved by:

4.3.21 Results will appear in mg/I TKN. 4.3.22 Calculate sample TKN as follows.

Mg/I TKN= 75 x Result from DR/2400 Sample taken for digest x Analysis volume of digested sample

4.4 Calibration

Refer to Calibration standard operating procedure.


Refer to HACH Digesdahl Digestion Apparatus manual and HACH DR/2400 Spectrophotometer manual



Wastes generated must be disposed of correctly 6.0 Appendix

Results obtained are recorded in the monthly data sheets


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Standard Operating Procedures Page 1 of 3 Number 012 Rev 002

Title Standard Operating Procedures for Written by: Anne Bonner the determination of Total Nitrogen Approved by:

1.0 Introduction

An alkaline persulfate digestion converts all forms of nitrogen to nitrate. Sodium metabisulfite is added after the digestion to eliminate halogen oxide interferences. Nitrate then reacts with chromotropic acid under strongly acidic conditions to form a yellow complex with an absorbance maximum at 410nm.

2.0 Responsibility



HACH DR/2400 Spectrophotometer Test 'N' TubeTm HR Total Nitrogen Reagent Set Adapter, 16mm Cell COD Reactor Glass Pipets Distilled Water Primary Standard Set, for Kjeldahl Nitrogen Ammonia Nitrogen Standard Solution.


4.1.1 Collect samples in clean plastic or glass bottles. 4.1.2 Best results are obtained with immediate analysis4.1.3 Preserve the sample by reducing pH to 2 or less with concentrated sulphuric acid4.1.4 Store at 4°C or less. 4.1.5 Preserved samples may be stored up to 28 days. 4.1.6 Warm samples to room temperatre and neutralize with 5 N Sodium Hydroxide before analysis.

4.1.7 Correct the test result for volume additions.

4.2 Sample Digestion

4.2.1 Turn on the COD reactor. Heat to 103-106°C 4.2.2 Add the contents of one Total Nitrogen Persulphate reagent powder pillow to

each of two HR Total Nitrogen Digestion reagent vials.



4.2.3 Add 0.5ml of sample to a vial (this is the prepared sample). 4.2.4 Add 0.5ml of deionised water included in the kit to a second vial (this is the reagent blank) 4.2.5 Cap both vials and Shake vigorously for at least 30 seconds to mix. 4.2.6 Place the vials in the reactor and heat for exactly 30 minutes at 103-106°C. 4.2.7 After 30 minutes remove the hot vials from the reactor and cool to room temperature. 4.3 Sample Analysis

4.3.1 Select program 395 N, Total HR TNT on the HACH spectrophotometer. 4.3.2 Touch Start button. 4.3.3 Add the contents of one total nitrogen reagent A powder pillow to each vial. 4.3.4 Cap the tubes and shake for 15 seconds. 4.3.5 Touch the timer icon, then OK on the HACH spectrophotometer. A three minute

reaction period will begin. 4.3.6 After the timer beeps, remove the caps from the vials and add one TN reagent B

powder pillow to each vial. 4.3.7 Cap the tubes and shake for 15 seconds 4.3.8 Touch the timer icon, then OK on the HACH spectrophotometer. A two minute

reaction period will begin. 4.3.9 After the timer beeps, remove the caps from two TN reagent C vials and add 2ml of

digested, treated sample to one vial. Add 2 ml of digested treated reagent blank to the second TN reagent C vial.

4.3.10 Cap the vials and invert ten times to mix. Use slow, deliberate inversions for complete recovery

4.3.11 Touch the timer icon, then OK. A five minute reaction period will begin. 4.4 Sample Measurement

4.4.1 Install the 16mm adapter into the HACH spectrophotometer. 4.4.2 Wipe the reagent blank and place it into the adapter. 4.4.3 Touch Zero the display will show 0 mg1I N 4.4.4 Wipe the reagent vial and place it into the adapter. 4.4.5 Touch Read. Results will appear in mg1l N

4.5 Blanks for Colorimetric Measurement

4.5.1 The reagent blank may be used repeatedly for measurement using the same lots of

reagents 4.5.2 Store the reagent blank in the dark at room temperature for a maximum of 7

days. 4.5.3 If a small amount of white floc appears prior to the end of one week, discard and

prepare a new one.



4.3 Calibration

Refer to Calibration standard operating procedure.


HACH DR/2400 Spectrophotometer manual



6.0 Appendix

Results obtained are recorded in the monthly data sheets


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Standard Operating Procedures Page 1 of 1 Number 013 Rev.001 Standard Operating Procedures for the Written by: Darran Killian determination of the Method Detection Rev By Anne Bonner Level Approved by:

1.0 Introduction

The Method Detection Level (MDL) measures the smallest amount that can be detected, after proceeding through the complete analytical method.

2.0 Responsibility


3.0 Laboratory Procedure 3 1 Determine the Instrument Detection Level (IDL) by consultation with the

instruments instruction manual. 3.2 Estimate the MDL by reference to the IDL. 3.3 Add a constituent to reagent water, or to the matrix of interest, to make a

concentration near the estimated MDL. 3.4 Prepare and analyse seven portions of this solution over a period of at least three

days to ensure that MDL determination is more representative than measured performance sequentially.

3.5 Calculate the standard deviation of the seven points for the solution with concentration near the estimated MDL.

3.6 Repeat measurements in the range of one to five times the calculated MDL. 3 7 From a table of the one-sided t distribution select the value of t for (7 – 1) = 6

degrees of freedom and at the 99% level; this value is 3.14. 3.8 Multiply 3.14 by the standard deviation to achieve the desired MDL.

4.0 Safety/ Environmental Gloves, safety glasses and appropriate PPE must be worn during sampling and sample handling Wastes generated must be disposed of correctly

5.0 Quality/Technical Knowledge

Method: See Standard methods 1030C, Edition 201h, 1998

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Standard Operating Procedures Page 1 of 3 Number 014 Rev.02 Standard Operating Procedures for the Written by: Darran Killian Construction and analysis of Control Rev By Anne Bonner Charts Approved by:

1.0 Introduction

Control charts are constructed to analyse accuracy of analysis in the laboratory.. 2.0 Responsibility


4.0 Control Chart Construction

4.1 Reagent Blank Control Chart.

4.1.1 Plot a scatter chart with RB sample number on the X-axis and concentration of analyte of interest on the Y-axis.

4.1.2 Determine the warning level (standard deviation x 2) and control level (standard deviation x 3) and illustrate these levels on the chart.

4.1.3 Refer to Control Chart Analysis section X to interpret results.

4.2 Laboratory Fortified Blank Control Chart.

4.2.1 Plot a scatter chart with LFB sample number on the X-axis and percentage recovery of analyte of interest on the Y-axis.

4.2.2 Determine the warning level (standard deviation x 2) and control level (standard • deviation x 3) and illustrate these levels on the chart.


4.3 Laboratory Fortified Matrix Control Chart.

4.3.1 Plot a scatter chart with LFM sample number on the X-axis and percentage recovery of analyte of interest on the Y-axis.



4.4 Laboratory Intercomparison Samples Control Charts.

4.4.1 Plot a scatter chart with LIS sample number on the X-axis and performance score of analyte of interest on the Y-axis.

Standard Operating Procedures Page 2 of 3 Number 014 Rev.02 Standard Operating Procedures for the Written by: Darran Killian Construction and analysis of Control Rev By Anne Bonner Charts Approved by:

4.4.2 Determine the warning level (standard deviation x 2) and control level (standard deviation x 3) and illustrate these levels on the chart. 4.3.3 Refer to Control Chart Analysis section X to interpret results.

4.5 External Company Instrument and Equipment Calibration Control Charts.

4.5.1 Plot a scatter chart with LIS sample number on the X-axis and performance score of analyte of interest on the Y-axis.


4.3.3 Refer to Control Chart Analysis section X to interpret results. 5.0 Control Chart Analysis 5.1 Control Limit (3 x Standard deviation)

5.1.1 If one measurement exceeds a control limit, repeat the analysis immediately. If the repeat measurement is with in the CL continue analysis

5.1.2 If it exceed the control limit, discontinue analyses and correct the problem. 5.1.3 After correcting the problem, re-analyse the sample analysed between the last in-

control measurement and the out of control one. 5.2 Warning Limit (2 x Standard deviation)

5.2.1 If two out of three successive points exceed a warning limit, analyse another sample. If the next point is within the warning limit, continue analysis.

5.2.2 If the next point exceeds the warning level, evaluate potential bias and correct the problem.

5.2.3 After correcting the problem, reanalyse the sample analysed between the last in-control measurement and the out of control one.

5.3 Standard Deviation

5.3.1 If four out of five successive points exceed the standard deviation, or are decreasing or increasing order, analyse another sample. If the next point is less than the standard deviation, or changes the order continue analysis.

5.3.2 Otherwise discontinue analysis and correct the problem. 5.3.3 After correcting the problem, reanalyse the sample analysed between the last in-

control measurement and the out of control one.

Standard Operating Procedures Page 3 of 3 Number Rev.02 Standard Operating Procedures for the Written by: Darran Killian Construction and analysis of Control Rev By Anne Bonner Charts Approved by:

5.4 Trending 5.4.1 If seven successive samples are on the same side of the central line, discontinue

analysis and correct the problem. 5.4.2 After correcting the problem, reanalyse the sample analysed between the last in-

control measurement and the out of control one.


Refer to Stand Methods For The Examination Of Water And Wastewater 20th Edition. Section 1020




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Standard Operating Procedures Page 1 of 3 Number 015 Rev.02 Standard Operating Procedures for the Written by: Anne Bonner collection of samples at the wastewater Rev By Anne Bonner treatment plants in County Westmeath Approved by:

1.0 Introduction

It is essential when sampling that the best sample is obtained by careful collection. To ensure that the relative proportions or concentrations of all pertinent components will be the same in the samples as in the materials being sampled and that the samples will be handled in such a way that no significant change in the composition occurs before the test are made. The following are the procedures for the collection of samples from the wastewater treatment plants within County Westmeath.

2.0 Responsibilitv


3.0. Materials.

3.1 Instrumentation and equipment

On-site refrigerated composite samples for inlet and outlet (smaller treatment plants use portable composite samplers).

3.2 Supplementary Equipment

1 litre azlon wide neck bottle indelible marker

field sheet telescopic sampling device

3.3 Safety Equipment

Disposable gloves Safety clothing First aid kit Disinfectant wipes

Standard Operating Procedures Page 2 of 3 Number 015 Rev.02 Standard Operating Procedures for the Written by: Anne Bonner collection of samples at the wastewater Rev By Anne Bonnertreatment plants in County Westmeath Approved by:

4.0 Sample Collection

4.1 Sample identification and test request

4.1.1 The sample bottle should be labelled with DOC COC 01 to prevent misidentification

4.1.2 Sampling containers should be identified 4.1.3 A sampling report and test request form should also be completed for

each sample container.

4.2 Sampling Frequency.

4.2.1 The sampling frequency for the wastewater treatment plants is attached.

4.3 Wastewater Sample Collection.

4.3.1 Sample collection in the aeration basin 4.3.1.1 The sample collected should be representative of the aeration tank

conditions.

4.3.2 Sample collection by composite sampler 4.3.2.1 The sampler takes a sample of effluent over a 24 hour period 4.3.2.2 The sample integrity is maintained by maintaining the sample at 4

degrees centigrade by use of a refrigerator or ice packs where no refrigeration is present.

4.3.3 Sample collection by portable composite samplers

4.3.3.1 The portable samplers are used in plants were no fixed samplers are

installed. 4.3.3.2 The samplers are set-up to take samples over a 24-hour period. 4.3.3.3 In order to maintain the integrity of the samples and minimise the

effect of elevated temperatures on the sample the following day hours should be avoided 00.01 – 24.00

4.3.3.4 The hourly samples should be taken from 10.00 to 9.00 hours the following day. Then just after 9.00 the 24 hour single composite sample should be collected.

Standard Operating Procedures Page 3 of 3 Number 015 Rev.02 Standard Operating Procedures for the Written by: Anne Bonner collection of samples at the wastewater Rev By Anne Bonnertreatment plants in County Westmeath Approved by:

5.0: Sample Preservation. 5.1 Transport

5.1.1 This is only relevant to the smaller treatment plants that have no laboratory on site.

5.1.2 All samples should be transported to the laboratory in a transport box capable of retaining the temperature at 4 degrees centigrade and protecting samples from dark.

5.1.3 All samples should be delivered to the laboratory tightly sealed and labeled with the local authority. 5.2 Preservation

5.2.1 The time interval between collection and analysis should be as short as possible

5.2.2 If immediate analysis is not possible preservation of samples may be necessary

5.2.3 Storage at 4 degrees centigrade is often adequate. 5.2.4 Use chemical preservatives only when they are shown not to

interfere with the sample.5.2.5 Choose the preservative with due regard because the

preservation technique for one parameter may not necessarily be the same for another.

5.2.6 Preservation techniques are limited to PH control, chemical addition, the use of amber and opaque bottles, refrigeration and freezing.

6.0 Safety Precautions.

6.1 During the wastewater sampling all personnel must wear safety boots and latex gloves at all times

6.2 Due care and attention should be taken at all times.

7.0 Sample Observation and Records

7.1 On each sampling occasion the technician should note observations and record in a comment sheet

7.2 The technician should report any problems to the Senior Executive Engineer, Executive Engineer and Executive Scientist


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WESTMEATH COUNTY COUNCIL WASTEWATER TREATMENT PLANT SAMPLING SCHEDULE 2006

Sample Type Grid Ref pH BOD COD SS Total N Nitrate Total P Ortho-P Ammonium SSV DO Temp Cond Sampling Sampling frequency Risk based mg/I mg/I mg/I mg/I N mg/I N mg/I P mg/I P mg/I NH4 ml 30min mg/I oC uS1cm3 frequency based based on regs and on plant on UWWT Regs plant performance performance Athlone WWTW

Inlet * * * * * * * * * Monthly Monthly Low Aeration * * * Monthly Monthly Low Outlet * * * * * * * * * Monthly Monthly Low Upsteam * * * * * * Monthly Monthly Low Downstream 1 km * * * * * Monthly Monthly Low BaUymore VVWTW

Inlet * * * * * * * * * Monthly Monthly Low Aeration * * * Monthly Monthly Low Outlet * * * * * * * Monthly Monthly Low Upsteam * * * * * * Monthly Monthly Low Downstream 10m * * * * * * * Monthly Monthly Low Kilbeggan WWTW Inlet * * * * * * Monthly 2 times/month High Aeration * * * Monthly 2 times/month High Outlet * * * * * * * * Monthly 2 times/month High Upsteam * * * * * Monthly 2 times/month High Downstream 2km * * * * * * * Monthly 2 times/month High Moat+e WWTW Inlet * * * * * Monthly 2 times/month High Aeration * * * Monthly 2 times/month High Outlet * * * * * * * * Monthly 2 times/month High Upstream East * * * * * Monthly 2 times/month High Upstream West * * * * Monthly 2 times/month High Downstream 10m * * * * * * Monthly 2 times/month High Downstream 2km * * * * Monthly 2 times/month High Rochfortbridge WWTW Inlet * * * * * * * Monthly 2 times/month High Aeration * * * Monthly 2 times/month High Outlet * * * * * * * * * Monthly 2 times/month High Upsteam * * * * * * Monthly 2 times/month High Downstream 2km * * * * * * Monthly 2 times/month High T y r r e U s p ~ s s Inlet * * * * * * * Monthly 2 times/month HighAeration 1 * Monthly 2 times/month High Aeration 2 * * * Monthly 2 times/month High Outlet 1 * * * * * * Monthly 2 times/month High Outlet 2 * * * * * * Monthly 2 times/month High Outlet * * * * * * * Monthly 2 times/month High Upsteam * * * * * * * Monthly 2 times/month High Downstream * * * * Monthly 2 times/month High


Sample Type Grid Ref pH BOD COD SS Total N Nitrate otal P Ortho-P Ammonium SSV DO Temp Cond Sampling Sampling frequency Risk based mg/I mg/I mg/I mg/I N mg/1 N mg/I P mg/I P mg/I NH4 ml 30min mg/I oC uS/cm3 frequency based based on regs and on plant on UWWT Regs plant performance performance MuHingar

Inlet * * * * * * NH3 daily (TP and COD monthly) Monthly High Risk Aeration * daily Monthly High Risk Outlet * * * * * * * * daily (TP and COD monthly) Monthly High Risk Upsteam * * * * * * * * monthly Monthly High Risk Downstream * * * * * * * * monthly Monthly High Risk Kinnegad Inlet * * * NH3 between 6 and 12 times yearly Monthly High Risk Aeration * * between 6 and 12 times yearly Monthly High Risk Outlet * * * * * * between 12 and 24 times yearly Monthly High Risk Upsteam * * * * * * * * monthly Monthly High Risk Downstream * * * * * * monthly Monthly High Risk Killucan Inlet * * * * NH3 between 6 and 12 times yearly Monthly Med Risk Aeration * between 6 and 12 times yearly Monthly Med Risk Outlet * * * * * * between 12 and 24 times yearly Monthly Med Risk Upsteam * * * * * * * monthly Monthly Med Risk Downstream * * * * monthly Monthly Med Risk

Delvin Inlet * * * * NH3 between 6 and 12 times yearly Monthly High Risk Aeration * between 6 and 12 times yearly Monthly High Risk Outlet * * * between 12 and 24 times yearly Monthly High Risk Upsteam * * * * * * monthly Monthly High Risk Downstream * * * * * * * * monthly Monthly High Risk Clonmelion Inlet * * * * NH3 between 6 and 12 times yearly 2 times/month High Risk Aeration * * between 6 and 12 times yearly 2 times/month High Risk Outlet * * * * * * between 12 and 24 times yearly 2 times/month High Risk Upsteam * * * * * * monthly 2 times/month High Risk Downstream * * * * * monthly 2 times/month High Risk

Castlepollard Inlet * * * NH3 between 6 and 12 times yearly 2 times/month High Risk Aeration * * between 6 and 12 times yearly 2 times/month High Risk Outlet * * * between 12 and 24 times yearly 2 times/month High Risk Upsteam * * * * * * * monthly 2 times/month High Risk Downstream * * * * * * * monthly 2 times/month High Risk


Sample Type Grid Ref pH BOD COD SS Total N N i t r a t P Ortho-P Ammonium SSV DO Temp Cond Sampling Sampling frequency Risk based mg/1 mg/1 mg/1 mg/I N mg/1 N mg/I P mg/I P mg/1 NH4 ml 30min mg/ oC uS/cm3 frequency based based on regs and on plant on UWWT Regs plant performance performance Ballynacarrigy Inlet * * * * NH3 between 6 and 12 times yearly 2 times/month High Risk Aeration * between 6 and 12 times yearly 2 times/month High Risk Outlet * * * * * between 12 and 24 times yearly 2 times/month High Risk

Upsteam * * * * * * monthly 2 times/month High Risk

Downstream * * * * * * * monthly 2 times/month High Risk Muttyfarnham Inlet * * NH3 between 6 and 12 times yearly 2 times/month High. Risk Aeration * between 6 and 12 times yearly 2 times/month High. Risk Outlet * * * * * * between 12 and 24 times yearly 2 times/month High. Risk Upsteam * * * * * * monthly 2 times/month High. Risk Downstream * * * * * monthly 2 times/month High. Risk Collnstown Outlet * * * * NH3 between 12 and 24 times yearly 2 times/month High Risk Downstream * * * * * * monthly 2 times/month High Risk Rathamey (Co. houses) Aeration * NH3 * between 6 and 12 times yearly 2 times/month Low Risk Outlet * * * * * between 6 and 12 times yearly 2 times/month Low Risk M'pass (Co. houses)

NH3 2 times/month Hlgh Risk Rathowen (Co. Houses) Outlet * * * NH3 between 6 and 10 times yearly 2 times/month High Risk Donore Aeration * NH3 between 6 and 10 times yearly 2 times/month High Risk Outlet * * * between 6 and 10 times yearly 2 times/month Baflinahowen Outlet High Risk 1 times/month Glasson High Risk Outlet * * * * * between 6 and 10 times yearly 1 times/month

W E S T M E A T H C O U N T Y C O U N C I L W A S T E W A T E R T R E A T M E N T P L A N T S A M P L I N G S C H E D U L E 2 0 0 6

Sample Type Grid Ref pH BOD COD SS Total N Nitrate otal P Ortho-P Ammonium SSV DO Temp Cond Sampling Sampling frequency Risk based mg/I mg/I mg/l mg/I N mg/I N mg/l P mg/l P mg/l NH4 ml 30min mg/l oC uS/cm3 frequency based based on regs and on plant on UWWT Regs plant performance performance Bagynacarrigy

Inlet * * NH3 between 6 and 12 times yearly 2 times/month High Risk Aeration * * between 6 and 12 times yearly 2 times/month High Risk Outlet * * between 12 and 24 times yearly 2 times/month High Risk Upsteam * * * * * * * monthly 2 times/month High Risk Downstream * * * * * * monthly 2 times/month High Risk

Multyfarnham Inlet * * * NH3 between 6 and 12 times yearly 2 times/month High. Risk Aeration * between 6 and 12 times yearly 2 times/month High. Risk Outlet * * * * * between 12 and 24 times yearly 2 times/month High. Risk Upsteam * * * * * * * monthly 2 times/month High. Risk Downstream * * * * * * monthly 2 times/month High. Risk Collinstown Outlet * * * * NH3 between 12 and 24 times yearly 2 times/month High Risk Downstream * * * * * monthly 2 times/month High Risk Ratharney (Co. houses) Aeration * NH3 * between 6 and 12 times yearly 2 times/month Low Risk Outlet * * * * between 6 and 12 times yearly 2 times/month Low Risk Wpass (Co. NH3 2 times/month Hlgh Risk Rathowen (Co. Houses) Outlet * * * * NH3 between 6 and 10 times yearly 2 times/month High Risk Donore Aeration * NH3 between 6 and 10 times yearly 2 times/month High RiskOutlet * * * between 6 and 10 times yearly 2 times/month

.haven Outlet High Risk * * * * * 1 times/month

rt High Risk Outlet * * * * * between 6 and 10 times yearly 1 times/month

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