Oil and Grease by Extraction/Gravimetric Method

1. Dry distillation flask constantly by 70C in the drying oven for 24 hours. After 24 hours drying, weight the distillation flask using analytical balance. This weight will be sign as W1 (weight of dry distillation flask without oil/grease). 2. Take a water sample by filling a clean 500 ml graduated separatory funnel to the 500 ml mark. 3. Using a pipet, add 4 ml of sulphuric acid standard solution, 14.5 N to the separatory funnel. Stopper and shake. 4. Add 30 ml of n-Hexane to the separatory funnel. 5. Shake the stoppered separatory funnel vigorously for two minutes. 6. Stand the separatory funnel upright in a support. Wait 10 minutes. 7. Insert a small cotton plug soaked with n-Hexane into the delivery tube of the separatory funnel. Drain the n-Hexane layer into the distillation flask. 8. Repeat steps 4 to 7 three times, then, discard the water layered. 9. Rinse the separatory funnel with n-Hexane to remove any oil film left on the funnel walls. 10. Place the flask, which contain of oil/grease and n-Hexane into the drying oven for 24 hour. 11. After 24 hour, weight the distillation flask using analytical balance. This weight will be sign as W2 (weight of oil/grease + dry distillation flask). 12. Then, the calculation of test result as follow:

Weight total (mg/l) =

W2- W1 Sample volume in litre

W2 = Weight of oil/grease + dry distillation flask W1 = Weight of dry distillation flask without oil/grease

*Adapted from Standard Methods for Examination of Water and Wastewater Method 1664, Revision A: N-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated NHexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry, February 1999. United States Environmental Protection Agency, Office of Water, Washington, D.C

Ammoniacal Nitrogen by APHA 2450 D Method

Sample and blank sample preparation

1. Pour 25 ml of sample into a 25 ml mixing graduated cylinder (the prepared sample). 2. Pour 25 ml of deionized water into a second cylinder (the blank). 3. Add the contents of one Ammonia Salicylate Reagent Powder Pillow to each cylinder. Stopper. Shake to dissolve. 4. After three minutes, add the contents of one Ammonia Cyanurate Reagent Powder Pillow to each cylinder. Stopper. Shake to dissolve.

Analysis was conducted using DR3000 HACH SPECTROPHOTOMETER

1. Enter the stored program number for ammonia nitrogen (NH3-N), salicylate method. Press: 385 READ/ENTER, the display will show: DIAL nm TO 655 2. Rotate the wavelength until displays shows: 655 nm. 3. Press: READ/ENTER, the display will show: mg/l NH3 Salic 4. Pour the blank into a sample cell. Place the cell into the cell holder. Close the light shield. 5. Press ZERO. The display will show: WAIT, then: 0.00 mg/l N-NH3 Salic. 6. Fill a second cell with the prepared sample. Place the cell into the cell holder. Close the light shield. 7. Press: READ/ENTER, the display will show: WAIT, then the result in mg/l ammonia as nitrogen (NH3-N) will be displayed.
*Adapted from Clin.Chim. Acta., 14 403 (1966) HACH Water Analysis Handbook. NITROGEN, AMMONIA (0 to 0.50 mg/l NH3-N) for water, wastewater and seawater