STANDARD OPERATING PROCEDURE (SOP) FOR TIAN SIANG OIL MILL PAHANG LABORATORY

NAME :NURUL HAZWANI BT MOHAMAD :FAMEZA BT REHAN PROGRAMME: EH220 LI DURATION: 2 MONTHS 2010276264 2010811842

SUPERVISOR: MR. RIZALMAN BIN ABD RAHIM COMPANY ADDRESS : TIAN SIANG OIL MILL (PAHANG) SDN. BHD. KG. TERSANG, BATU MALIM, 27610 RAUB, PAHANG.

1. Crude Palm Oil (CPO) Test 1.1 Objectives a) To determine the percent of moisture content in the CPO. b) To determine the content of Free Fatty Acid (FFA) in the CPO. c) To determine the percent of deterioration of bleach ability index (DOBI) in the CPO. d) To ensure that the content of each parameter did not exceed the given limit. 1.2 Limitation Table PARAMETER Moisture Free Fatty Acid (FFA) Deterioration (DOBI) Table 1.1 of Bleachability Index LIMIT (%) 0.25 < 5.00 2.30

1.3 Materials and Apparatus 1.3.1 MOISTURE CONTENT a) 100 mL beaker b) 250 mL beaker c) Hot plate / heater d) Electronic weighing scale e) Tap water f) Crude palm oil (CPO) g) Goggles h) Gloves i) Mask j) Safety helmet 1.3.2 FFA CONTENT a) 100 mL beaker b) 150 mL conical flask c) 10 mL pipette d) 15 mL burette e) Electronic weighing scale f) Hot plate / heater g) Retort stand h) Phenolphthalein i) Isopropyl Alcohol (IPA) j) Sodium Hydroxide (NaOH) k) Crude palm oil (CPO) l) Goggles m) Gloves n) Mask o) Safety helmet

1.3.3 DOBI a) 100 mL beaker b) 250 mL beaker c) 25 mL volumetric flask d) Dropper e) Electronic weighing scale f) Precision cells g) Spectrophotometer machine h) Tissue / clean cloth i) 2,2,4-trimethylpentane j) Crude palm oil (CPO) k) Goggles l) Gloves m) Mask n) Safety helmet

1.4 Procedure 1.4.1 MOISTURE CONTENT (< 0.25%) a) Take 100 mL of crude palm oil sample from the production line or storage tank or dispatch section. b) Measure the weight of an empty beaker (100 mL beaker) by using the electronic weighing scale. c) Add 20 mL of crude palm oil sample into the weighed empty beaker. d) Measure the weight of the beaker after sample is added in order to get the weight of the sample. ( ) Where; ( ) ( ( ) ) ( ) ( ) ( ) ( ) ( )

e) Heat the loaded beaker on the hot plate for 1-2 minute/s. f) Add approximately 200 mL of tap water into the 250 mL beaker (this is for the cooling of the heated beaker). g) After heated, cool the heated beaker in the tap water. h) Measure the weight of the cooled beaker by using the electronic weighing scale. ( Where; ( ( ( ) ) ) ( ) ( ) ( ) ) ( ) ( )

1.4.2 FFA CONTENT (<5.00%) a) Take the remaining sample of CPO from part 1.4.1. b) Measure the weight of an empty conical flask by using the electronic weighing scale. c) Add approximately 3g of crude palm oil sample into the conical flask. d) To get the exact weight of the sample, measure the weight of the loaded conical flask. ( ) Where; ( ) ( ( ) ) ( ) ( ) ( ) ( ) ( )

e) Add 1 mL of phenolphthalein (indicator) into the conical flask and swirl. f) Add 50 mL of Isopropyl Alcohol (IPA) into the conical flask and swirl. g) Heat the conical flask on the hot plate for 1-2 minute/s. h) Pipette 15 mL of Sodium Hydroxide (NaOH) into the 15 mL burette. i) Titrate the heated mixture with NaOH until the color of the mixture turn to CPOs color (reddish orange color). j) Record the reading of the burette after the titration. ( ) ( ) ( ) Where;

( )

( )

1.4.3 DOBI (>2.30%) Step 1: Preparation of solution A. a) Take the remaining sample of CPO from part (1.4.2). b) Measure the weight of an empty volumetric flask. c) Add approximately 0.1g of sample into the volumetric flask. d) Add 2,2,4-trimethylpentane into the volumetric flask until it reach the calibration point. e) Shake the volumetric flask until the solution is perfectly mixed. Step 2: Preparation of the spectrophotometer machine. a) Switch on the spectrophotometer machine. b) Press Main Menu button. Select Data Menu at the option list. c) Then, prepare the precision cells by rinsing the cell with 2,2,4-trymethylpentane. d) After rinsed, fill three-quarter of the precision cells with 2,2,4-trymethylpentane. e) Wipe away any finger print or dust on the surface of the precision cells. f) Insert the precision cells in the spectrophotometer with the clear part perpendicular to the laser direction. g) Then, press Auto Zero button and wait until the reading on the panel is equal to 0.0000. Step 3: DOBI testing. a) By using the same precision cells from step 2, rinse the precision cells using solution A. b) Fill three-quarter of the precision cells with solution A. c) Wipe away any finger print or dust on the surface of the precision cells. d) Insert the precision cells in the spectrophotometer with the clear part perpendicular to the laser direction. e) Then, press Start button and wait until the panel show its reading. f) Record the reading.

1.5 Results 1.5.1 MOISTURE CONTENT (<0.25%) NO. Time t, CPO(b),g CPO(bs),g CPO(s),g CPO(bh),g CPO(ac),g % moisture

(00:00:00) hour 1. 2. 3. Table 1.2 1.5.2 FFA CONTENT (<5.00%) NO. Time (00:00:00) 1. 2. 3. Table 1.3 1.5.3 DOBI (>2.30%) NO. Time (00:00:00) 1. 2. 3. Table 1.4 t, hour % DOBI t, hour 2.56 2.56 2.56

CPO(cf),g CPO(cfs),g CPO(s),g NaOH,mL Numerity % FFA

2. Kernel Test 2.1 Objectives a) To determine the moisture content in the kernel. b) To determine the impurities content in the kernel. c) To ensure that the moisture and impurities content in the kernel do not exceed the given limit. 2.2 Limitation Table PARAMETER Moisture Impurities (dirt and shells) Table 2.1 LIMIT (%) <7.00 <6.00

2.3 Materials and Apparatus 2.3.1 MOISTURE CONTENT a) Basin b) Moisture meter c) Cup electrode d) Tissue e) Kernel f) Goggles g) Gloves h) Mask i) Safety helmet

2.3.2 IMPURITIES ( DIRT AND SHELLS) a) Basin b) Weighing scale c) A clean cloth / tray ( 45 75 ) cm d) Goggles e) Gloves f) Mask g) Safety helmet

2.4 Procedure 2.4.1 MOISTURE (<7.00%) a) Take kernel sample from production line or bunker or dispatch section. b) Sort out from the sample approximately 10-20 kernels. c) Wipe the kernels until it is fully dried. d) Fill the lower part of the cup electrode with the dried kernels until it is full. e) Connect the upper part of the cup electrode and close it tightly by twisting the hand wheel of the cup electrode. f) Connect the cup electrode to the moisture meter by using the connecting wire. g) Press the red check button and ensure that the meter needle reach the red zone on the meter. h) Press white measuring button and take the reading.

2.4.2 IMPURITIES (<6.00%) a) Take kernel sample from production line or bunker or dispatch section. b) Weight 1kg / 1000g of kernel sample by using the manual weighing scale. c) Spread the weighed kernel sample on the clean cloth or the tray. d) Sort out any dirt such as shells, half crack nut, small fibers and etc. e) Weight the dirt by using the manual weighing scale. () ( ) () ( ) ( ) ( )

2.5 Results 2.5.1 MOISTURE CONTENT (<7.00%) NO. Time (00:00:00) 1. 2. 3. Table 2.2 t, hour % moisture

2.5.2 IMPURITIES (<6.00%) NO. Time (00:00:00) 1. 2. 3. Table 2.3 t, hour K(s),g D(i),g % impurities

3. Dry Decanter Cake Test 3.1 Objectives a) To determine the moisture content in the dry decanter cake. b) To ensure that the moisture content in the dry decanter cake do not exceed the given limit.

3.2 Limitation Table PARAMETER Moisture Table 3.1 LIMIT (%) < 12 - 20

3.3 Materials and Apparatus a) Scooper b) Weighing scale c) Moisture meter d) Cup electrode e) Decanter cake f) Goggles g) Gloves h) Mask i) Safety helmet

3.4 Procedure a) Take dry decanter cake sample from bunker or dispatch section. b) Let it cool to room temperature for about an hour. c) Then, fill the lower part of cup electrode with the cooled dry decanter cake until it is full. d) Connect the upper part of cup electrode and close it tightly by twisting the hand wheel. e) Connect the cup electrode to the moisture meter by using the connecting wire. f) Press the red check button and ensure that the meter needle reach the red zone on the meter. g) Press white measuring button and take the reading.

3.5 Results NO. Time (00:00:00) 1. 2. 3. Table 3.2 t, hour % moisture

4. Oil Losses Test 4.1 Objectives a) To determine the percent of oil loss by extracting oil from fibers (press), oil room, dry decanter cake and sludge. b) To ensure that the losses of oil do not exceed the given limit. 4.2 Limitation Table PARAMETER Moisture Oil losses wet basis (OLWB) Oil losses dry basis (OLDB) LIMIT (%) 30 35 Sludge and cake (<14.00) Fiber (<7.00) Not of solid (NOS) 59 65 Table 4.1

4.3 Materials and Apparatus a) 250 mL beaker b) Crucible pot c) Filter paper d) Borosilicate glass e) Thimble filter f) Southlete extractor g) Align condenser h) Extraction apparatus i) Oven j) Electronic weighing scale k) Tap water l) Hexane m) Goggles n) Gloves o) Mask p) Safety helmet

4.4 Procedures a) Take sample of pressed fiber from press section. b) Take sample of decanter cake from decanter dryer. c) Take sample of sludge from sludge tank. d) Weight three empty crucible pots by using the electronic weighing scale. e) Fill one pot with approximately 5g of fibers, one pot with approximately 30g of decanter cake and the other one with approximately 30g of sludge. f) Weight each of the pot again by using the electronic weighing scale. g) Heat all of the pots in the oven. Fibers = 4 minutes Decanter cake = 5 minutes Sludge = 4 hours

h) After heated, weight each of the pot again by using the electronic weighing scale. i) From this step, the moisture can be calculated already:

( ) ( ) ( )

( ) ( ) ( )

Step 2: Preparation of hexane. a) Weight three empty borosilicate glasses by using the electronic weighing scale one by one. b) Fill each of the borosilicate glass with 250 mL of hexane. Step 3: Extraction process. a) Insert each heated sample into the thimble filter. b) Insert the thimble filter into the southlete extractor and connect it to the align condenser at the extraction apparatus. c) Connect the bottom of the southlete extractor to the borosilicate glass that containing the hexane. d) Place borosilicate properly on the heater while connecting it to the southlete extractor. e) Connect the align condenser with tap water pipe by using the tubes. f) Open the tap and let the tap water flow through the tube as well as the align condenser. g) Heat the borosilicate glass with the level of hotness at 4. h) Heat the borosilicate glass until all the oil from the sample being extracted out and the hexane dried. i) After the oil being extracted, weight the borosilicate glass again by using the electronic weighing scale. j) Calculate the parameters.

( )

( ) ( ) ( ) ( ) ( ) ( ) ( )

4.5 Results Samples Time t, hours 1. Fibers 2. Decanter cake 3. Sludge Table 4.2 (a) t,hours A,g B,g C,g D,g E,g F,g G,g H,g

Samples

Time

% moisture

% OLWB

% OLDB

% NOS

1. Fibers 2. Decanter cake 3. Sludge Table 4.2 (b)

5. Kernel Losses Test 5.1 Objectives a) To determine the losses of kernel from fiber cyclone, stage (1&2) and clay bath. b) To make sure that the losses do not exceed the given limit. 5.2 Limitation Table SECTION Fiber cyclone Stage (1&2) Clay bath Table 4.1 LIMIT (%) <2.00 <2.00 <2.00

5.3 Materials and Apparatus a) Plastic bag b) A clean cloth / tray ( 45 75) cm c) Manual weighing scale d) Goggles e) Gloves f) Mask g) Safety helmet

5.4 Procedure 5.4.1 Fiber cyclone (fiber) a) Take sample of fibers from fiber cyclone by using the plastic bag. b) Weight 1kg / 1000g of the sample by using the manual weighing scale. c) Spread the sample on the clean cloth / tray. d) Sort out any nut and kernel from the fibers. e) Weight the nut and kernel by using the manual weighing scale.

( )

5.4.2 Stage (1&2) a) Take sample from stage (1&2) using plastic bag. b) Weight 1kg / 1000g of the sample by using the manual weighing scale. c) Spread the sample on the clean cloth / tray. d) Sort out any kernel from the sample. e) Weight the kernel by using the manual weighing scale.

( )

5.4.3 Clay Bath a) Take sample from clay bath outlet by using the plastic bag. b) Weight 1kg / 1000g of the sample by using the manual weighing scale. c) Spread the sample on the clean cloth / tray. d) Sort out any kernel, broken kernel and nut from the wet shell. e) Weight each of them by using the manual weighing scale.

5.5 Results NO. TIME, 00:00:00 Fiber cyclone 1. 2. 3. Table 4.2 SECTION, % Stage Clay bath

6. Cracking Efficiency Test (RM 1 & 2) 6.1 Objectives a) To determine the cracking efficiency of the ripper mill. 6.2 Materials and Apparatus a) Plastic bag b) A clean cloth / tray ( 45 75) cm c) Manual weighing scale

6.3 Procedures a) Take sample from ripper mill (1&2) by using the plastic bag. b) Weight 1kg / 1000g of sample by using the manual weighing scale. c) Spread the sample on the clean cloth / tray. d) Sort out any nut, whole kernel, broken kernel and shell. e) Weight each of them by using the manual weighing scale. f) Calculate the percent of nut, whole kernel, broken kernel and shell.

6.4 Results NO. TIME,00:00:00 Nut Whole kernel 1. 2. 3. Table 5.1 RESULTS,% Broken kernel Shell Cracking efficiency

7. Pressing Efficiency Test 7.1 Objectives a) To determine the pressing efficiency of the pressing machine. b) To ensure that the fruits are press to the level of fully dried. 7.2 Limitation Table PARAMETERS Nut Broken nut Whole kernel Broken kernel Shell Fiber Table 6.1 7.3 Materials and Apparatus a) Plastic bag b) A clean cloth / tray ( 45 75) cm c) Manual weighing scale LIMITS, % >35.00 <6.00 <1.50 <1.50 <1.50 >50.00

7.4 Procedure a) Take sample from pressing machine that is / are working on that day. b) Weight 1/2kg / 500g of sample by using the manual weighing scale. c) Sort out any nut, broken nut, whole kernel, broken kernel and shell from the fiber. d) Weight each of them. e) Calculate the percentage.

7.5 Results NO. TIME, 00:00:00 Nut Broken nut 1. 2. 3. Table 6.2 PARAMETERS, % Whole kernel Broken kernel Shell Fiber

8. Boiler Water Test 8.1 Objectives a) To find the concentration of Sulphite presence in the Boiler Water. b) To find the concentration of Phosphate presence in the Boiler Water. c) To find the concentration of Caustic Alkalinity presence in the Boiler Water. d) To find the concentration of Total Dissolved Solid (TDS) in the Boiler Water. e) To find the Total Hardess of the Boiler Water. f) To know the pH of the Boiler Water. g) To find the concentration of Phosphate presence in the Boiler Water. h) To find the concentration of Silica presence in the Boiler Water. i) To find the concentration of Chloride presence in the Boiler Water.

8.2 Limitation Table Parameters Sulphite Phosphate Caustic alkalinity Total Dissolved Solid (TDS) Total Hardness pH Silica Chloride Table 7.1 Limits 20 60 ppm 20 70 ppm 300 700 ppm < 1200 ppm < 1 ppm 10.5 11.5 < 90 ppm < 300 ppm

8.3 Materials and Apparatus a) 100 mL beaker b) 150 mL conical flask c) 50 mL burette d) Retort Stand e) Dropper f) TDS Tester g) Color Comparator h) pH Indicator Strips i) Iron rod j) Test tube k) Boiler water (sample) l) Hydrochloric Acid 6N (HCl) m) Starch Indicator n) Potassium Iodide N/63 (KI2) o) Phosphate Reagent p) Distilled Water q) Phenolphthalein Indicator r) Barium Chloride (BaCl2) s) EDTA 50 t) Sulphuric Acid (H2SO4) u) Tablet of Hardness Yes or No v) Acid Reagent w) Solochrome Black Indicator x) Ammonium Buffer Solution y) Silica 3 Reagent z) Molybdate Reagent aa) Citric Acid Reagent bb) Potassium Chromate (K2CrO4) cc) Silver Nitrate (AgNO3)

8.4 Procedures 8.4.1 Sulphite a) Take the Boiler Water sample from the Boiler. Ensure that the sample water still hot. b) Pour 50 mL of Boiler Water sample into a 150 mL conical flask. c) 1 mL of Hydrochloric Acid 6N (HCl) and 2 mL of Starch Indicator. d) Shake the conical flask until the solution is mixed completely. e) Pour the 50 mL burette with Potassium Iodide N/63 (KI2) until it full. f) Titrate the solution with Potassium Iodide N/63 (KI2) by using the burette until the color turns blue. g) Record the reading of the burette after titration. h) Calculate the titration reading: Titration reading = (50 mL - reading of the burette after titration) i) Calculate the concentration of Sulphite presence in the Boiler Water: Concentration of Sulphite presence (in ppm) = Titration reading 20 j) Record the results. 8.4.2 Phosphate a) Take the Boiler Water sample from the Boiler. Ensure that the sample water still hot. b) Pour 0.5 mL of Boiler Water sample into a test tube. c) Add 5 mL of Distilled Water into the test tube. d) Put 1 packet of Phosphate Reagent and shake it until the reagent completely dissolved in water. e) Use Color Comparator (Phosphate-Phosver III) to get the reading. f) Record the result. 8.4.3 Caustic Alkalinity a) Take the Boiler Water sample from the Boiler. Ensure that the sample water still hot. b) Pour 50 mL of Boiler Water sample into a 150 mL conical flask. c) Add 4 droplets of Phenolphthalein Indicator and 1 mL of Barium Chloride (BaCl2).

d) Shake the conical flask until the solution is mixed completely. e) Pour the 50 mL burette with Sulphuric Acid (H2SO4) until it full. f) Titrate the solution with Sulphuric Acid (H2SO4) by using the burette until the color turns grey. g) Record the reading of the burette after titration. h) Calculate the titration reading: Titration reading = (50 mL - reading of the burette after titration) i) Calculate the concentration of Caustic Alkalinity presence in the Boiler Water: Concentration of Caustic Alkalinity presence (in ppm) = Titration reading 100 j) Record the results. 8.4.4 Total Dissolved Solid (TDS) a) Take the Boiler Water sample from the Boiler. Ensure that the sample water still hot. b) Pour 100 mL of Boiler Water sample into a 100 mL beaker. c) Use TDS Tester to test the TDS of the water. d) Record the reading shown on the TDS Tester. 8.4.5 Total Hardness ( Method 1) a) Take the Boiler Water sample from the Boiler. Ensure that the sample water still hot. b) Pour 50 mL of Boiler Water sample into a 100 mL beaker. c) Take 1 tablet of Tablet Hardness Yes or No and put it into the water sample. d) Stir the water by using an iron rod until the tablet completely dissolved in the water. e) If the color of the water turns green, it means that the Total Hardness = 0, no need to proceed the test. f) If the color of the water turns red, titrate the solution with EDTA 50 by using a burette until the color turns blue. Pour the 50 mL burette first with EDTA 50 until it full n pour the sample into a 150 mL conical flask. g) Record the reading of the burette after titration. h) Calculate the titration reading: Titration reading = (50 mL - reading of the burette after titration)

i) Calculate the Total Hardness of the Boiler Water: Total Hardness of the Boiler Water = Titration reading 10 j) Record the results. Method 2 a) Take the Boiler Water sample from the Boiler. Ensure that the sample water still hot. b) Pour 50 mL of Boiler Water sample into a 150 mL Conical Flask. c) Add 5 droplets of Solochrome Black Indicator and 5 droplets of Ammonium Buffer Solution. d) Shake the conical flask until the solution is mixed completely. e) If the color of the water turns green, it means that the Total Hardness = 0, no need to proceed the test. f) If the color of the water turns red, titrate the solution with EDTA 50 by using a burette until the color turns blue. Pour the 50 mL burette first with EDTA 50 until it full n pour the sample into a 150 mL conical flask. g) Record the reading of the burette after titration. h) Calculate the titration reading: Titration reading = (50 mL - reading of the burette after titration) i) Calculate the Total Hardness of the Boiler Water: Total Hardness of the Boiler Water = Titration reading 10 j) Record the results.

8.4.6 pH a) Take the Boiler Water sample from the Boiler. Ensure that the sample water still hot. b) Pour 50 mL of Boiler Water sample into a 100 mL beaker. c) Take 1 strip of pH Indicator Strip and soak it into the water sample. d) Wait for a while and compare the color change shown on the pH Indicator Strip to get the pH reading. e) Record the result.

8.4.7 Silica a) Take the Boiler Water sample from the Boiler. Ensure that the sample water still hot. b) Pour 0.5 mL of Boiler Water sample into a test tube. c) Add 5 mL of Distilled Water into the test tube. d) Put 1 packet of Acid Reagent and shake the tube until the reagent completely dissolved in water. e) Put 1 packet of Molybdate Reagent and shake the tube until the reagent completely dissolved in water. f) Put 1 packet of Citric Acid Reagent and shake the tube until the reagent completely dissolved in water. g) Put 1 packet of Silica 3 Reagent and shake the tube until the reagent completely dissolved in water. h) Use Color Comparator (Silica) to get the reading. Concentration of Silica presence (in ppm) = reading 10 i) Record the result. 8.4.8 Chloride a) Take the Boiler Water sample from the Boiler. Ensure that the sample water still hot. b) Pour 50 mL of Boiler Water sample into a 150 mL Conical Flask. c) Add 4 droplets of Phenolphthalein Indicator and shake the conical flask until the solution is mixed completely d) Pour the 50 mL burette with Sulphuric Acid (H2SO4) until it full. e) Titrate the solution with Sulphuric Acid (H2SO4) by using the burette until the color turns colorless. f) Add 2 mL of Potassium Chromate (K2CrO4) into the colorless solution. g) Shake the conical flask until the solution is mixed completely. h) Pour the 50 mL burette with Silver Nitrate (AgNO3) until it full. i) Titrate the solution with Silver Nitrate (AgNO3) by using the burette until the color turns Orange. j) Record the reading of the burette after titration.

k) Calculate the titration reading: Titration reading = (50 mL - reading of the burette after titration) l) Calculate the concentration of Chloride presence in the Boiler Water: Concentration of Chloride presence (in ppm) = Titration reading 20 m) Record the results.

8.5 Results Result Time (00:00:00) (00:00:00)

Test Sulphite Phosphate Caustic Alkalinity Total Dissolved Solid Total Hardness pH Silica Chloride

Limit 20 60 20 70 300 700 < 1200 <1 10.5 11.5 < 90 < 300

Table 7.2

9. Silica Remover Water Test 9.1 Objectives a) To find the concentration of Silica presence in the Silica Remover Water. b) To find the Total Hardess of the Silica Remover Water. 9.2 Limitation Table Parameters Silica Total Hardness Table 8.1 Limits < 5 ppm < 1 ppm

9.3 Materials and Apparatus a) Test tube b) Color Comparator c) 100 mL beaker d) Iron rod e) 150 mL Conical Flask f) 50 mL burette

g) Dropper h) Silica Remover Water sample i) Molybdate Reagent j) Acid Reagent

k) Citric Acid Reagent l) Silica 3 Reagent

m) EDTA 50 n) Tablet Hardness Yes or No o) Solochrome Black Indicator p) Ammonium Buffer Solution

9.4 Procedures 9.4.1 Silica a) Take the Silica Remover Water sample from the Silica Remover. b) Pour 5 mL of Silica Remover Water sample into a test tube. c) Put 1 packet of Acid Reagent and shake the tube until the reagent completely dissolved in water. d) Put 1 packet of Molybdate Reagent and shake the tube until the reagent completely dissolved in water. e) Put 1 packet of Citric Acid Reagent and shake the tube until the reagent completely dissolved in water. f) Put 1 packet of Silica 3 Reagent and shake the tube until the reagent completely dissolved in water. g) Use Color Comparator (Silica) to get the reading. h) Record the result. 9.4.2 Total Hardness ( Method 1) a) Take the Silica Remover Water sample from the Silica Remover. b) Pour 50 mL of Silica Remover Water sample into a 100 mL beaker. c) Take 1 tablet of Tablet Hardness Yes or No and put it into the water sample. d) Stir the water by using an iron rod until the tablet completely dissolved in the water. e) If the color of the water turns green, it means that the Total Hardness = 0, no need to proceed the test. f) If the color of the water turns red, titrate the solution with EDTA 50 by using a burette until the color turns blue. Pour the 50 mL burette first with EDTA 50 until it full n pour the sample into a 150 mL conical flask. g) Record the reading of the burette after titration. h) Calculate the titration reading: Titration reading = (50 mL - reading of the burette after titration) i) Calculate the Total Hardness of the Silica Remover Water: Total Hardness of the Silica Remover Water = Titration reading 10 j) Record the results.

Method 2 a) Take the Silica Remover Water sample from the Silica Remover. b) Pour 50 mL of Silica Remover Water sample into a 150 mL Conical Flask. c) Add 5 droplets of Solochrome Black Indicator and 5 droplets of Ammonium Buffer Solution. d) Shake the conical flask until the solution is mixed completely. e) If the color of the water turns green, it means that the Total Hardness = 0, no need to proceed the test. f) If the color of the water turns red, titrate the solution with EDTA 50 by using a burette until the color turns blue. Pour the 50 mL burette first with EDTA 50 until it full n pour the sample into a 150 mL conical flask. g) Record the reading of the burette after titration. h) Calculate the titration reading: Titration reading = (50 mL - reading of the burette after titration) i) Calculate the Total Hardness of the Silica Remover Water: Total Hardness of the Silica Remover Water = Titration reading 10 j) Record the results. 9.5 Results Result Time (00:00:00) (00:00:00)

Test Silica Total Hardness

Limit <5 <1

Table 8.2

10. Softener Water Test 10.1 Objectives a) To know the pH of the Softener Water b) To find the Total Hardess of the Softener Water 10.2 Limitation Table Parameters pH Total Hardness Table 9.1 10.3 Materials and Apparatus a) 100 mL beaker b) pH Indicator Strip c) Iron rod d) 50 mL burette e) 150 mL conical flask f) Dropper g) Softener Water sample h) Tablet Hardness Yes or No i) EDTA 50 Limits 6.8 7.0 < 1 ppm

j) Solochrome Black Indicator k) Ammonium Buffer Solution

10.4 10.4.1 pH

Procedure

a) Take the Softener Water sample from the Softener. b) Pour 50 mL of Softener Water sample into a 100 mL beaker. c) Take 1 strip of pH Indicator Strip and soak it into the water sample. d) Wait for a while and compare the color change shown on the pH Indicator Strip to get the pH reading. e) Record the result. 10.4.2 Total Hardness (Method 1) a) Take the Softener Water sample from the Softener. b) Pour 50 mL of Softener Water sample into a 100 mL beaker. c) Take 1 tablet of Tablet Hardness Yes or No and put it into the water sample. d) Stir the water by using an iron rod until the tablet completely dissolved in the water. e) If the color of the water turns green, it means that the Total Hardness = 0, no need to proceed the test. f) If the color of the water turns red, titrate the solution with EDTA 50 by using a burette until the color turns blue. Pour the 50 mL burette first with EDTA 50 until it full n pour the sample into a 150 mL conical flask. g) Record the reading of the burette after titration. h) Calculate the titration reading: Titration reading = (50 mL - reading of the burette after titration) i) Calculate the Total Hardness of the Softener Water: Total Hardness of the Softener Water = Titration reading 10 j) Record the results. Method 2 a) Take the Softener Water sample from the Softener. b) Pour 50 mL of Silica Remover Water sample into a 150 mL Conical Flask. c) Add 5 droplets of Solochrome Black Indicator and 5 droplets of Ammonium Buffer Solution.

d) Shake the conical flask until the solution is mixed completely. e) If the color of the water turns green, it means that the Total Hardness = 0, no need to proceed the test. f) If the color of the water turns red, titrate the solution with EDTA 50 by using a burette until the color turns blue. Pour the 50 mL burette first with EDTA 50 until it full n pour the sample into a 150 mL conical flask. g) Record the reading of the burette after titration. h) Calculate the titration reading: Titration reading = (50 mL - reading of the burette after titration) i) Calculate the Total Hardness of the Softener Water: Total Hardness of the Softener Water = Titration reading 10 j) Record the results.

10.5

Results Result Time (00:00:00) (00:00:00)

Test pH Total Hardness

Limit 6.8 7.0 <1

Table 9.2

11. BOD Test 11.1 Objectives a) To find the Biochemical Oxygen Demand (BOD) content in the Raw Palm Oil Mill Effluent

11.2

Theory

Why choose BOD at 30 C for 3 days instead BOD at 20 C for 5 days: 1. To stimulate tropical climate condition 2. To shorten the incubation period so that more samples can be analyzed 3. The effect of nitrification is minimal 4. Extensive lab experiment have shown that BOD at 30 C for 3 days is slightly higher than BOD at 20 C for 5 days Calculation of BOD: BOD (mg/L) = [A B C E ] D where A: Initial Dissolved Oxygen Content (DO-1) of the diluted sample B: Final Dissolved Oxygen Content (DO-3) of the diluted sample C: Blank value = [Initial DO of Dilution Water blank sample final DO of Dilution Water blank sample] D: Dilution factor (50 or 100) E: Average Seed control

11.3

Materials and Apparatus a) 10 L water container b) 50 mL measuring cylinder c) 250 mL beaker d) Aquarium Air Pump e) Electronic Clock Timer f) Dropper

g) pH Indicator Strips h) 500 mL measuring cylinder i) j) DO Meter BOD Bottles (Wheaton type)

k) Hot Plate l) Stirrer HTS 1003

m) Alluminium Wrapper n) BOD Incubator o) Distilled water p) Ferric Chloride Solution (FeCl3.6H2O), q) Magnesium Sulphate Solution (MgSO4.7H2O) r) s) Calcium Chloride Solution (CaCl2), Phosphate Buffer Stock Solution

t) Polyseed BOD Innoculum PK/50 u) Effluent Water sample from Pond 11 (Settling) and Pond 12 (Maturity) v) Sulphuric Acid (H2SO4) w) Sodium Hydroxide (NaOH)

11.4

Procedures Section A Preparation of Aeration Water a) Pour 5 L of distilled water into a 10 L water container. b) Add 5 mL each of Ferric Chloride Solution (FeCl3.6H2O), Magnesium Sulphate Solution (MgSO4.7H2O), Calcium Chloride Solution (CaCl2), and Phosphate Buffer Stock Solution into the water container by using a 50 mL measuring cylinder. c) Pour 150 mL of distilled water into a 250 mL beaker. d) Put 1 capsule of Polyseed BOD Innoculum PK/50 into the beaker. e) Connect an Aquarium Air Pump to the water container and the beaker to allow aeration process occurs. Switch on the Aquarium Air Pump and set the Electronic Clock Timer to 2 hours. f) Let the process run for 2 hours. Section B Preparation of Effluent Water Sample a) Take the Effluent Water sample from Pond 11 (Settling) and Pond 12 (Maturity). b) Pour 250 mL of each water samples into the 250 mL beaker. c) Check the pH of each water samples by using a pH Indicator Strips. It should be in a range of (6.5 8.2). d) If the pH exceeds 8.2, then add Sulphuric Acid (H2SO4) by using a dropper into the water sample to reduce the pH.If the pH lowers than 6.5, add Sodium Hydroxide (NaOH) by using a dropper to increase the pH. Section C Dilution of Water Sample a) Pour 10 mL of water sample (Pond 12) into a 500 mL measuring cylinder. b) Add distilled water which taken from the water container (prepared in Section A) into the measuring cylinder until it full. c) Close the measuring cylinder and shake slowly until it mixed completely. d) Repeat step 1 until step 3 for water sample (Pond 11).

Section D a) Take out 8 BOD Bottles (Wheaton type), label each of it and pour the Seed Solution which taken from the beaker (prepared in Section A) into the bottles according to the measurement below:

Label Blank 5 mL 10 mL 15 mL FD 50 FD 100 11 50 11 100

Volume of Seed Solution used 0 mL 5 mL 10 mL 15 mL 2 mL 2 mL 2 mL 2 mL Table 10.1

b) Add distilled water which taken from the water container (prepared in Section A) into the Blank, 5 mL, 10 mL, and 15 mL bottles until it full. c) Add Pond 12 water sample (prepared in Section C) into the FD 50 bottle until it full. d) Record the volume of Pond 12 sample water (prepared in Section C) left in the measuring cylinder and times by 2: G = sample water left 2 e) Pour distilled water from the water container (prepared in Section A) into that measuring cylinder until it reach G. f) Add Pond 12 water sample (prepared in step 5) into the FD 100 bottle until it full. g) Repeat step 3 for the 11 50 bottle and step 4 until step 6 for 11 100 bottle by using Pond 11 water sample (prepared in Section C). h) Stir all the water samples in BOD bottles by using the Hot Plate Stirrer HTS 1003 for about 1 minute for each bottle.

i) Use DO Meter to measure the Dissolved Oxygen Content for day 1 (DO-1) in each of the water sample. (unit in mg/L) j) Close the BOD bottles with its Pennyhead stoppers/cap and wrap the head with Alluminium Wrapper. k) Set the BOD Incubator at 30 C and put all the water samples in the BOD Incubator for 3 days. l) Record the Dissolved Oxygen Content for day 3 (DO-3) in each of the water sample after 3 days by using the DO Meter. m) Calculate the Biochemical Oxygen Demand (BOD) content in Pond 12 and Pond 11s water sample and record the results.

11.5

Results DO-1 (mg/ L) DO-3 (mg/L)

Label of the Sample Blank 5 mL 10 mL 15 mL FD 50 FD 100 11 50 11 100

Table 10.2

12. Dilution 12.1 Objectives a) To find the percentage of oil, water, and sand in the sample taken from Apollo Tank, Under Flow, and Distributor

12.2

Limitation Table Limit (in %) Oil 40 45 8 10 50 55 Table 11.1 Water 30 40 < 80 20 30 Sand < 30 12 20 25

Sample Crude Oil Under Flow Distributor

12.3

Materials and Apparatus a) 100 mL beaker b) Thermometer c) Iron rod d) 10 mL centrifuge tube e) Centrifuge 80-2 f) Samples from Apollo Tank (crude oil), Under Flow, and Distributor

12.4

Procedures a) Take the samples from Apollo Tank (crude oil), Under Flow, and Distributor. b) Pour each of the samples into the 100 mL beaker. c) Measure the temperature for every sample by using a thermometer. d) Stir the samples by using an iron rod until it mixed completely. e) Pour each of the samples into the 10 mL centrifuge tube until it full. f) Put all the centrifuge tubes into the Centrifuge 80-2. g) Set up the Centrifuge 80-2:

Speed = 10 100 rpm Time = 20 minutes h) Switch on the Centrifuge 80-2. i) Record the results of oil, water, and sand layer after 20 minutes for each of the samples.

12.5

Results Result

Sample

Temperature (C)

Oil(in %)

Water(in %)

Sand(in %)

Crude Oil Under Flow Distributor Table 11.2