Wall Wash Test: 1. Preparation

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WALL WASH TEST

1. PREPARATION.
- Regent -
a) Pure Methanol (500ml/bottle)
b) Pure Water(Distillated Water)
c) Acetone(500ml/bottle)
d) 2%AgNO3 Solution(500ml/bottle)
e) 20%HNO3 Solution(500ml/bottle)
f) 10ppm(0.01mg/ml)Chlorine Standard Solution(500ml/bottle)
g) 0.02%KMnO4 Solution(500ml/bottle)-Store in dark place and keep cool temperature.

- Instrument -
a) Plastic Bottles(500ml x 2 bottles for Methanol washing / Pure Water Dropping)
b) Nessler - Tube ( 100 ml x 6 pcs )
c) Pipet ( 5 ml x 4pcs for AgNO3 / HNO3 / CL / KMnO4 respectively)
d) Shall x 2pcs ( for testing Non-volatile matters)
e) Disposable Vinyl gloves ( 200 sheets / 1 case )
f) Funnel x 1
g) Shoies Covers
h) A.P.H.A Color Standard ( No.3, 5, 8, 10) for Color Test
i) Black Colored Plate(for testing trubidity of HC/CL)
j) White Colored Plate(for testing turbidity Color)
k) Flash Light

2. WALL WASH BY METHANOL AND SAMPLING.


Before entering into cargo tank for sampling, the cargo tank has to be dried without humidity on the wall and gas freed.
The tank must be checked toxic gas/combustible gas/oxygen content by responsible officer and posted one man near
hatch cover.

* Test kits for WWT have to be stowed in closed bag or wooden box not to drop test kits into tank when going into
and coming out tank.
* Put the shoes covers and wear vinyl gloves
* Before taking sample,wash Funnel by methanol
* Take samples from four(4)parts of Fore / Aft / Port /Starboard bulkheads and in the area of 1 meter in height x
30cm in width at the position of 1.5meter from the bottom by methanol wash on the wall.
* It is desitable to take sample from reasonable area but don't take sample from nook corner which can not count
as standard value.
* The necessary quantity of sample from each cargo tank is about 250cc for Color/50cc,
HC/50cc, CL/50cc, PTT/50cc.

3. SAMPLE ANALYSIS.
a) Hydrocarbon Test
- Fill up 50cc of wall wash sample into 100cc Nessler-tube and add 50cc of Distilled water
- The mixture is shaken and allowed to stand for 20 minutes
- For avoiding any observational error or for checking purity of reagent,make a standard solution by pure
methanol 50cc + distilled water 50cc and compare with sample on the black plate.
- The standard solution for each ppm can be made by Methanol / 50cc+ AgNO3 / 2cc+ HNO3 / 2cc+ 10ppm
standard CL / 8cc ( for 2ppm, 4cc for 1 ppm) + Distilled water 38cc (for 2ppm) or 42cc(for 1ppm)
- If the sample is very clear as standard solution of zero ppm, it means zero ppm.
Nearly clear : 0.5 ppm
Little cloudy : 1 ppm
Not cloudy : 5 ppm
Cloudy(milky) : more than 10 ppm
b) Chloride Test
- Fill up Sample / 50cc + 20% HNO3 / 2cc + 2% AgNO3 / 2cc + Distilled water/46cc into 100cc Nessler-tube
- The mixture is shaken and allowed to stand for 10 minutes
- The mixture in the tube is compared with Standard solution on the Black plate
(Standard Solutions for each ppm)
ppm Methanol 20%HNO3 2%AgNO3 10ppm standard CL Distilled water Total
2 ppm 50 cc 2 cc 2 cc 8 cc 38 cc 100 cc
1 ppm 50 cc 2 cc 2 cc 4 cc 42 cc 100 cc
0.5 ppm 50 cc 2 cc 2 cc 2 cc 44 cc 100 cc
0.25 ppm 50 cc 2 cc 2 cc 1 cc 45 cc 100 cc

c) Permanganate Time test ( P.T.T )


- Fill up Sample / 50cc and add 0.02%KMnO4 / 2 cc into 100 cc Nessler - tube ( Sample )
- Fill up Methanol / 50cc and add 0.02% KMnO4 / 2 cc into 100 cc Nessler - tube ( Standard )
- The mixture is shaken and then wait until the color of violet turned orange
- The times required for P.T.T are as follow:
50 minutes over at 15 °C, or 30 minutes over at 25 °C, or 20 monutes over at 28 °C

Checking of color change:


Violet Light Violet Orange Light Yellow
<-----------------------? Minutes ?---------------------------->

d) APHA Color Test


- Fill up Sample / 50cc and add Methanol / 50cc into 100cc Nessler - tube
- Compare with APHA standard color(from No.1 to No.20)

e) Non-Volatile Matters Test ( NVM Test )


- For NVM test, wall of cargo tank has to be washed by Acetone instead of Methanol
- Put the sample in Shall on hot plate until Acetone vaporized completely and then check the residues such as oil
remained in Shalle.

4. FIGURES FOR TESTING HC / CL / PTT / COLOR TEST

a) Hydrocarbon Test b) Chloride Test

Pure water 36cc

46cc
50cc Pure water 50cc 10ppm CL 8cc
2cc 2% AgNO3 2cc
2cc 20% HNO3 2cc

Sample
Sample
50cc Methanol 50cc 50cc 50cc

Methanol

(Sample) (Standard ) (Sample) (Standard )


Zero ppm 2ppm
c) Permanganate Time Test d) APHA Color Test

50cc Methanol 50cc

2cc 2cc
KMnO4

Sample
Sample
50cc Methanol 50cc 50cc 50cc

Methanol

(Sample) (Standard ) (Sample) (Standard )

e) Non Volatile Matters Test ( NVM )

5. SPECIFICATION FOR WALL WASH ANALYSIS.


Cargo HC CL PTT Color Water Odor Remarks
MEG-1 Nil 2 ppm > 50 min/15°C < No. 5 > 500ppm max Nil DOW
MEG-2 Nil 0.2ppm > 50 min/15°C < No. 5 > Nil Nil PCT
Methanol Nil 2 ppm > 50 min/15°C < No. 5 > Nil Nil
SM Nil N/A N/A No.10 > N/A N/A

6. REMOVAL OF HYDROCARBON.
Result of WWT Tank Cleaning Methods
2ppm>HC Methanol spray
2ppm<HC<3ppm Toluene steaming 3hrs & Methanol spray
3ppm<HC<5ppm Toluene wash Steaming(within LEL) Methanol spray
5ppm<HC Re-cleaning with detergent or solvent depend on tank coating
*Detergent : B-4 , B-2, Caustic Soda
*Solvent : Toluene, PCE, Kerosene
*Others : Phosphoric Acid , Rust remover

7. REMOVAL OF CHLORIDE
Result of WWT Tank Cleaning Methods
2ppm>CL Steaming or Methanol spray
2ppm<CL<5ppm Methanol spray Steaming(within LEL)
5ppm<CL Hand wash or BW by Fresh water Steaming(within LEL) Methanol spray
* Before start Methanol spray, the purity of methanol in drum & Cleanness of Spray equipment have to be
tested
8. REMOVAL OF OXIDE RESIDUE (PTT)
Result of WWT (15°C) Tank Cleaning Methods
30 min < PPT < 50min Methanol spray
15 min < PPT < 30min Methanol Steaming Methanol spray
15 min > PPT Re-cleaning with detergent or solvent depend on tank coating

9. REMOVAL OF COLOR.
Result of WWT Tank Cleaning Methods
No. 5 < APHA < No.10 Methanol spray / 1 time
No.10 < APHA < No.15 Steaming & Methanol spray
No.15 < APHA Hot sea Butterworth Methanol spray
* Basically the color results from rusts on surface of cargo coating tank or EDC tank as last cargo

10. REMOVAL OF NVM RESIDUE.


Result of WWT Tank Cleaning Methods
Almost Nil Methanol spray
Normal Toluene wash Methanol wash
Too much Re-cleaning with detergent or solvent (Refer to item-6)

11. INSPECTION ITEMS FOR CARGOES.


CARGOES SURVEY ITEMS SPECIFICATION REMARKS
Acetone WWT NVM, Water
Benzene 1st Foot Vapor return
I-4 Butandiol 1st Foot sample to Lab NVM, Water N2 blanket
B.Acetate Visual Running 1st Foot NVM, Water
Chlorofoam WWT & 1st Foot Analysis NVM, Water N2 blanket
C.Hexanone 1st Foot sample to Lab NVM, Water N2 blanket
DIDP Running 1st Foot
DINP Running 1st Foot
DOP Visual Running 1st Foot
DMF 1st Foot Analysis NVM, Water N2 , Vapor return
DEC 1st Foot sample to Lab Color <10, water < 200ppm
EGMBE 1st Foot sample to Lab NVM, Water
2-EH Visual Running 1st Foot NVM, Water
Ethanol WWT & Foot sample HC & CL
E.Acrylate 1st Foot sample to Lab NVM, Vapor return
Hexane WWT & Foot sample NVM, Water
IBA 1st Foot sample to Lab NVM,
IPA WWT & Foot sample to lab CL / 5ppm , HC / nil
MEK WWT & Foot sample to lab NVM, Water
MTBE 1st Foot sample to Lab Color, Water
Phenol Running 1st Foot N2 , Vapor return
P.Xylene 1st Foot sample to Lab CL / 5ppm , HC / nil

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