JJG18-095 (SOP For COD Measurement - HI Photometer) July 11

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SOP FOR MEASURING COD - JJG18 – 095

HANNA INSTRUMENTS PHOTOMETER
July 11th, 2018 Page 1 of 5
COD reactor and photometer instruction manuals must be read before use.
This protocol is based on both manuals.
1. SCOPE
This Standard Operation Procedure (SOP) must be used for accurate COD measurements. It should be carried out
by a lab operator.
2. DEFINITIONS
Chemical Oxygen Demand (COD): the Chemical Oxygen Demand is the amount of oxygen consumed to
chemically oxidize organic water contaminants to inorganic end products. This test is based on the fact that a strong
oxidizing agent, under acidic conditions, can fully oxidize almost any organic compound to carbon dioxide. COD is
expressed in mg O2/L, which indicates the mass of oxygen consumed per liter of solution.
3. EQUIPMENT AND SUPPLIES

• COD reactor and test tube heater
• COD and Multiparameter Bench Photometer
• 100 mL graduated cylinder
• 5 mL syringe
• 170 mL beaker
• Vials for COD measurement
• Distilled water
• 100 µL precision pipette
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4. SAFETY
• Please refer to COD Reactor Instruction Manual, section Health & Safety.
• Please refer to COD and Multiparameter Bench Photometer Instruction Manual, section Health & Safety.
• Safety equipment: Wear suitable eye protection and clothing when required and follow instructions carefully.
• Reagent spills: If a reagent spill occurs, wipe up immediately and rinse with plenty of water. If reagent
contacts skin, rinse the affected area thoroughly with water. Avoid breathing released vapors.
• Waste disposal: for proper disposal of reagent kits and reacted samples, refer to the Material Safety Data
Sheet (MSDS).
5. PROCEDURE
Reactor’s preparing for sample(s) digestion
• Turn the reactor ON using the power switch located on the rear panel. The green POWER LED will be
illuminated. Wait until unit displays the heater block temperature.
• Select the Program 166 for COD ranges of 0 – 150 mg/L; as it is expected for the POME of BBS Biogas
Plant.
• Select the Program 169 for COD ranges of 5 – 90 mg/L; as it is expected for the Reactor overflow and
Settling Pond overflow of BBS Biogas Plant.
• Press the ▲ or ▼ key to increase or decrease the reaction time up to two (2) hours; if necessary.
• Press the START button to start the heating mode. The yellow HEATING LED will illuminate.
• Wait until the reactor reaches the desired temperature.
Sample(s) dilution for POME only:

• Choose a homogeneous sample. Samples containing settleable solids need to be homogenized.
• Use the syringe to measure exactly 5 mL of POME sample. Pour the sample into the graduated cylinder.
• Complete up to 100 mL mark with distilled water (95 mL).
• Pour the solution in the large 170 mL beaker, replace the cap and invert several times to mix.
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• Sample dilution is complete.

• The dilution factor is: N = 100 / 5 = 20
Note: this dilution procedure is valid to POME samples with COD up to 300 000 mg/L. If the sample COD is beyond
300 000 mg/L, dilution factor must be higher.
Sample(s) digestion
• Remove the cap from two reagent vials.
• Add exactly 0,1 mL (100 µL) of sample to one vial (sample vial) and 0,1 mL (100 µL) of distilled water to
the other vial (blank vial), while keeping the vials at a 45-degree angle. Replace the cap tightly and mix by
inverting each vial a couple of times.
Warning: the vials will become very hot during mixing, be careful when handling them.
• Insert the vials into the reactor as soon as the desired temperature is reached and has stabilized (a beep
will signal that vials may be placed in the reactor).
• Press START to start the timer. Heat the sample(s) for 2 hours at 150°C.
• At the end of the digestion period, switch off the reactor. Wait for twenty (20) minutes to allow the vials to
cool to about 120°C.
• Invert each vial several times while still warm and then place them in the test tube rack.
Warning: the vials are still hot, be careful when handling them.
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• Leave the vials in the tube rack to cool to room temperature. Do not shake or invert them anymore otherwise
the samples may become turbid.
COD measurement:
• Turn the photometer ON via the ON/OFF power switch.
• In order to select the Oxygen Demand, Chemical HR (COD) method, press the METHOD key and a screen
with the available methods will appear.
• Press the keys to highlight the Oxygen Demand, Chemical HR (COD) method. Press Select.
• After the Oxygen Demand, Chemical HR (COD) method is selected, place the COD vial adapter in the cuvet
holder and ensure that the adapter is well fit inside.
• Place the blank vial into the holder and push it completely down.
• Press the Zero key and the instrument will perform a zero sequence. If the zero sequence was successfully
done, the display will show “-0.0-”. Now the meter is zeroed and ready for measurement.
• Remove the blank vial.

• Place the sample vial into the holder and push it completely down.
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• Press Read and the instrument will perform the reading.

• The instrument directly displays concentration in mg/L of oxygen demand.
6. COD CALCULATION FOR DILUTED SAMPLES

When performing the reading, pay attention to multiply the read value by the dilution factor in order to obtain the real
concentration of the COD in the original sample:
𝑟𝑒𝑎𝑙 𝐶𝑂𝐷 𝑖𝑛 𝑜𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑠𝑎𝑚𝑝𝑙𝑒 = 20 ∗ 𝐶𝑂𝐷 𝑟𝑒𝑎𝑑𝑖𝑛𝑔 𝑣𝑎𝑙𝑢𝑒

JJG18-095 (SOP For COD Measurement - HI Photometer) July 11

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SOP FOR MEASURING COD - JJG18 – 095

3. EQUIPMENT AND SUPPLIES

Sample(s) dilution for POME only:

• Sample dilution is complete.

• Remove the blank vial.

• Press Read and the instrument will perform the reading.

6. COD CALCULATION FOR DILUTED SAMPLES

𝑟𝑒𝑎𝑙 𝐶𝑂𝐷 𝑖𝑛 𝑜𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑠𝑎𝑚𝑝𝑙𝑒 = 20 ∗ 𝐶𝑂𝐷 𝑟𝑒𝑎𝑑𝑖𝑛𝑔 𝑣𝑎𝑙𝑢𝑒

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