DIAGRAM AND APPARATUS

Digital Titrator

pH/ISE meter

Delivery Tube

pH Electrode

Temperature Electrode

REAGENTS AND APPARATUS

EXPERIMENT 1: CARBON DIOXIDE TEST BY DIGITAL TITRATOR METHOD
USING SODIUM HYDROXIDE
REAGENTS
1. Phenolphthalein Indicator Powder Pillows
2. Sodium Hydroxide Titration Cartridge, 3.636 N
APPARATUS
1.
2.
3.
4.

Digital Titrator
Delivery tube for digital titrator
Erlenmenyer Flask, 125 mL
Erlenmenyer Flask, 250 Ml

EXPERIMENT 2: DISSOLVED OXYGEN TEST BY AZIDE MODOFICATION OF

WRINKLED METHOD
REAGENTS for 300ml BOD Bottle
1.
2.
3.
4.
5.
6.

Alkaline Iodide-Azide Powder Pillows

Manganous Sulfate Powder Pillows
Starch Indicator Solution
Sulfamic Acid Powder Pillows
Sodium Thiosulfate Titration Catridge, 0.2000 N
Sodium Thiosulfate Titration Catridge, 2.00 N

APPARATUS for 300 ml BOD bottle

1.
2.
3.
4.
5.
6.

Alkaline Iodide-Azide Powder Pillows

Manganous Sulfate Powder Pillows
Starch Indicator Solution
Sulfamic Acid Powder Pillows
Sodium Thiosulfate Titration Catridge, 0.2000 N
Sodium Thiosulfate Catridge, 2.00 N

Experiment 3 : pH and TEMPERATURE OF SAMPLE WATER

REAGENTS
1.
2.
3.
4.

Buffer solution pH 4
Buffer solution pH 7
Buffer solution pH 10
Deonized water.

APPARATUS
1. Platinum Series Combination pH electrode w/Temp
2. Sension 2 Poratble Ph/SE meter
3. Potassium Chloride Electrolyte Catridge

EXPERIMENTAL PROCEDURES
EXPERIMENT 1 : CARBON DIOXIDE TEST BY DIGITAL TITRATOR METHOD
USING SODIUM HYDROXIDE .
PROCEDURES
1. A sample volume and titration catridge was selected
2. A clean delivery tube was inserted into the titration catridge . The catridge was attach to
the titrator
3. The delivery tube was turned to ejects air and few of titrant was dropped. The counter to
zero was reset and wiped to tip
4. A sample water was collected directly into the titration flask by filled to the appropriate
mark
5. The contents of one Phenolphthalein Indicator Powder Pillow was added. Swirl to
mixed . Pink color was formed because no carbon dioxide is presented .
6. The delivery tube was placed into the solution and the flask was swirled. The knob was
turned on the titrator to add titrant to the solution. The flask was continue swirled and
titrant was added until the color changes to a light pink color that persists for 30 seconds
(pH 8.3). The number of digits displayed on the counter was written.
7. The concentration of CO2 sample water was calculated using the multiplier of 1.

EXPERIMENT 2: DISSOLVED OXYGEN TEST BY AZIDE MODIFICATION OF

WRINKLED METHOD
PROCEDURES:

1. A water sample in a clean 300ml BOD bottle was collected. The sample to overflow the
bottle for 2-3 minutes was allowed to make sure that air bubbles are not trapped.
2. The contents of one Manganous Sulfate Powder Pillow and one Alkaline Iodide-Azide
Reagent Powder Pillow were added.
3. The stopper was inserted immediately and without trapped air in the bottle. The bottle
was inverted several times to mixed. A flocculent precipitate was formed. It become
orange-brown because oxygen was presented. The flocs were settled slowly in salt water.
The settled takes about five minutes
4. The bottle was inverted several times again and waited for the flocs settled and the top
half of the solution was cleared again. To make sure the reaction of the sample and
reagents was completed wait until the floc settled
5. The stopper was removed and the content of one Sulfamic Acid Powder Pillow was
added. The stopper was replaced without trapped air in the bottle. To mixed inverted for
several times. The flocs was dissolved and a yellow color was leaved because oxygen
was presented.
6. . A sample water and Sodium Thiosulfate Titration Cartridge was selected that
corresponds to the expected dissolved oxygen (DO) concentration.
7. A cleaned delivery tube was inserted into the titration cartridge. The cartridge was
attached to the titrator body.
8. The delivery knob was turned to eject a few drops of titrant. The counter to zero was reset
and the tip was wiped.
9. A graduated cylinder was used to measure the 100ml of sample volume. The sample
volume was transferred into a 250ml Erlenmeyer flask.
10. The delivery tube tip was placed into the solution and the flask was swirled while titrated
with sodium thiosulfate to a pale yellow color.
11. Two 1 ml droppers of Starch Indicator Solution was added and swirled to mixed. A dark
blue color was developed.
12. The titration was continued to a colorless end point. The number of digits required was
recorded.
13. The amount of dissolved oxygen content in water sample was calculated.

Experiment 3 : pH and TEMPERATUR OF SAMPLE WATER

1. The Potassium Chloride Electrolyte Gel Cartridge was installed in the Platinum Series pH
Electrode.
2. The electrode was primed by pushing the dispenser button until gel comes out of the
reference junction. The excess gel was rinsed from the tip and the outlet with deionized
water.
3. The electrode was connected to the sension2 pH/ISE meter.
4. The meter was turned on by pressing I/O. The pH mV was pressed until the display shows
pH value.

5. The SETUP button was pressed. The up arrow was pressed for three times. The ENTER
button was pressed to toggle to the number of desired decimal places, then EXIT to leave
setup.
6. In two 50 ml beakers, the buffers of 4.0 and 7.0 pH or 7.0 and 10.0 pH was prepared.
7. The CAL was pressed. The display of Standard 1 was shown.
8. The electrode was rinsed in deionized water and blot dry.
9. The electrode was placed in pH 7.0 buffer. The ENTER was pressed.
10. A stable pH was determined, the display showed the Standard 2. The electrode was
removed from the beaker and was rinsed with deionized water and blot dry.
11. The electrode was placed in the 4.0 (or 10.0) pH buffer. The ENTER was pressed.
12. After the last calibration point has stabilized and the display reads Standard 3, the Exit
was pressed.
13. The display showed the store and the ENTER was pressed to store the calibration or EXIT
to leave the calibration mode without storing values.
14. The electrode was removed from buffer and rinsed with deionized water followed by a
small amount of sample and blot dry.
15. The electrode was placed in the sample.
16. The pH and temperature was recorded when they was stabilized.

REFERENCES
1. M Hamizura (Hassan, 2013) Faculty of Chemical Engineering, Chemical Engineering
Laboratory manual (CHE 331),Basic Water Quality, Page 1-9

APPENDICES
Original data sheet.