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Permanganate Time Test Method BASIC WALL WASH PROCEDURE THESE PROCEDURES DESCRIBE THE BASIC METHODS FOR COLLECTING AND TESTING CONTAMINANTS PRESENT ON THE TANK COATINGS OF A SHIP.. C

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WALL-WASH TEST PROCEDURES

1 BASIC WALL-WASH PROCEDURE

2 Chloride Test Method

3 Hydrocarbon Test Method

4 Permanganate Time Test Method

BASIC WALL WASH PROCEDURE

THESE PROCEDURES DESCRIBE THE BASIC METHODS FOR COLLECTING AND TESTING CONTAMINANTS

PRESENT ON THE TANK COATINGS OF A SHIP

THE TANK BULKHEADS ARE CONTACTED WITH TEST METHANOL AND THE WASHINGS ARE COLLECTED

IN A GLASS JAR VIA A SPECIALLY SHAPED FUNNEL (ALL CLEANED TO METHANOL STANDARD)

THE METHANOL IS THEN SUBJECTED TO ANALYTICAL TESTS METHANOL IS USED IN PERFORMING

WALL WASHES BECAUSE IT IS A SOLVENT WHOSE PROPERTIES ARE MOST SENSITIVE TO

CONTAMINANTS

EQUIPMENT REQUIRED

I/ WASHING BOTTLE-POLYTHENE, 500ml CAPACITY

2/ METHANOL CLEAN SAMPLE BOTTLES WITH PLASTIC LINED CAPS

3/ PLASTIC FUNNEL FOR COLLECTING WALL WASH

4/ PLASTIC DISPOSABLE GLOVES

REAGENT

APPROVED TEST METHANOL OF PRIME QUALITY USE APPROXIMATELY 50 ml OF METHANOL

FOR EACH AREA TESTED MARKS ON THE SIDE OF THE WASH BOTTLE WILL AID THIS

TANK TEST AREAS THE NUMBER OF TANK AREAS WHICH SHOULD BE TESTED WILL VARY AND WILL DEPEND UPON THE

CONSTRUCTION, COATING AND CONDITION OF THE TANK AS A MINIMUM, TESTS ARE TO BE

TAKEN THAT REPRESENT 4 "WALL" AREAS AND IS T0 BE A FAIR REPRESENTATION OF THE TANK,

AS SUCH THIS SHOULD INCLUDE POOR AS WELL AS GOOD AREAS, AND INCLUDE FRAMES, TO GIVE

A TOTAL OF 6 TO 8 TEST AREAS

CHLORIDE TEST METHOD REFERENCES FOR THE FOLLOWING TEST METHOD WERE TAKEN FROM

"STANDARD METHOD OF TEST SMA-68-62:

THIS TEST IS DESIGNED TO DETECT THE PRESENCE OF CHLORIDES IN METHANOL (OR OTHER

WATER SOLUBLE ORGANIC LIQUIDS) THE CHLORIDE ION IS REACTED WITH THE NITRATE

SOLUTION TO PRECIPITATE SILVER CHLORIDE THE ADDITION OF NITRIC ACID IS TO ENSURE

THE DISPERSING OF ANY SUSPENDED MATTER IN THE METHANOL SAMPLE, WHICH WILL GIVE A

POSITIVE INTERFERENCE WITH THE TEST

ANY CHLORIDES THAT ARE MIXED WITH THE SILVER NITRATE (AgNo3) WILL REACT TO GIVE A

MILKY SOLUTION, WHICH WOULD BE APPARENT WHEN COMPARED TO THE STANDARD SOLUTION

THE FOLLOWING RATIOS SHOULD BE USED WHEN MIXING THE SAMPLES

TEST SAMPLES

WALL WASH METHANOL 30ml

NITRIC ACID (HN03) 1ml

SILVER NITRATE (AgNo3) l/2ml

STANDARD SAMPLES

TEST METHANOL 30ml NITRIC ACID (HN03) 1ml SILVER NITRATE(AgNo3) l/2ml

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AGITATE THOROUGHLY AND ALLOW TO STAND FOR 15 MINUTES COMPARE EACH SAMPLE WITH THE

"STANDARD" SAMPLE, IF IT APPEARS "CLEAR AND BRIGHT" IT PASSES THE TEST IF IT

APPEARS "MILKY" THEN CHLORIDES ARE PRESENT IN

THE SAMPLE

NOTE THIS TEST CAN ALSO BE RUN ON THE FRESH WATER USED FOR TANK CLEANING TO GIVE AN

INDICATION OF THE QUALITY OF THE FRESH WATER USED

TESTING PROCEDURE

I/ USING THE PLASTIC BOTTLE, SQUIRT APPROXIMATELY 50 ml OF THE TEST METHANOL ON THE TEST SECTION, AT LEAST 4 FEET ABOVE THE TANK FLOOR AND IN A STREAM APPROXIMATELY

4 INCHES WIDE ALLOW THE METHANOL TO RUN DOWN THE WALL AND COLLECT IN THE SAMPLE JAR VIA THE FUNNEL

2/ PLASTIC DISPOSABLE GLOVES SHOULD BE WORN, AND CARE SHOULD BE TAKEN THAT THE INSIDES OF THE WALL WASH SAMPLES, FUNNEL, BOTTLE NECK, OR THE INSIDE OF THE

BOTTLE TOP IS NOT TOUCHED AS THE HUMAN BODY PERSPIRES, THE PERSPIRATION CONTAINS CERTAIN AMOUNTS OF CHLORIDES (AS SODIUM CHLORIDE - SALT) IT IS THEREFORE CRUCIAL NOT TO CONTAMINATE THE WALL WASH^WITH PERSPIRATION

3/ BEFORE CARRYING OUT ANY OF THE TEST PROCEDURES IT IS ESSENTIAL TO HAVE CLEAN GLASSWARE AND EQUIPMENT, IT SHOULD BE CLEANED AS FOLLOWS :

A/ WASH WITH SOAP AND WATER

B/ RINSE WITH TAP WATER TO REMOVE THE SOAP

C/RINSE WITH D.I WATER TO REMOVE THE TAP WATER

D/RINSE WITH METHANOL BEFORE USE

HYDROCARBON TEST METHOD REFERENCES FOR THE FOLLOWING TEST WERE TAKEN FROM

ASTM D1722/TEST METHOD BP-3-73 THIS TEST IS DESIGNED TO DETECT THE PRESENCE OF HYDROCARBONS IN THE METHANOL WALL WASH SAMPLE GENERALLY IT IS A TEST TO DETERMINE THE MISCIBILITY OF WATER WITH

METHANOL IT IS A GOOD TEST FOR HYDROCARBON AS THEY ARE ALL RELATIVELY INSOLUBLE IN WATER WHEN METHANOL IS DILUTED WITH WATER, ANY HYDROCARBONS PRESENT WILL CREATE A TURBIDITY TO THE SAMPLE THE SAMPLE SHOULD BE SHAKEN VIGOROUSLY AND ALLOWED TO

STAND IF THE SAMPLE IS "CLEAR AND BRIGHT " WHEN COMPARED TO THE STANDARD SOLUTION THEN IT PASSESS THE TEST IF THE SAMPLE IS HAZY OR APPEARS "MILKY WHITE" THEN

HYDROCARBONS ARE PRESENT IN THE SAMPLE

THE FOLLOWING RATIOS SHOULD BE USED WHEN MIXING THE SAMPLES

WALL WASH METHANOL 10ml TEST METHANOL 10ml

D.I WATER 30ml DI WATER 30ml

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PERMANGENATE TIME TEST METHOD REFERENCES FOR THE FOLLOWING TEST METHOD WERE TAKEN FROM

ASTM-D1363-67 ASTM-D1363-58 SMA-43-65 THIS TEST IS APPLICABLE TO:

METHANOL / ETHANOL / PROPANOL / BUTANOL / ACETINE / METHYL ETHYL KETONE /

METHYL ISOBUTYL / MONO ETHYLENE GLYCOL

THIS TEST IS DESIGNED TO CALCULATE THE PRESENCE OF IMPURITIES IN THE METHANOL, WHICH WILL EFFECT

AS IMPURITIES SOME OF THE OXIDIZING AGENTS ARE ETHYLENE AND UNSATURATED HYDROCARBONS, OR

IN GENERAL, LIGHT ENDS OF THE CRUDE METHANOL

THE PRESENCE OF CARBON MONOXIDE (CO) WILL CAUSE A DECREASE IN TIME

THE STANDARD SOLUTION REPRESENTS THE COLOUR OF THE END POINT TO WHICH THE SAMPLE

SOLUTION FADES IN THE KMn04 TEST

THE COLOUR OF THE STANDARD SAMPLE (AS PER ASTM) IS "PINK ORANGE"

THE COLOUR OF THE TEST SAMPLE, IN THE BEGINNING OF THE TEST IS "PINK"

.THE "PERMANGENATE TIME", IS THE TIME TAKEN FROM ADDING THE KMn04 (POTASSIUM CHLORIDE), FOR

THE "PINK" TO CHANGE TO "PINK ORANGE" (THAT OF THE STANDARD)

FOR METHANOL THIS TIME IS TO BE 60 MINUTES PLUS IN ORDER TO PASS

FOR M.E.G THIS TIME IS TO BE 30 MINUTES PLUS IN ORDER TO PASS

CONSTANT TEMPERATURE FOR THIS TEST IS 15 DEGREES CENTIGRADE

NOTES :

I/ CLEAN GLASS WARE IS ABSOLUTELY ESSENTIAL AS COMMON CONTAMINANTS SUCH AS SOAP IN WASHING, AND OIL WILL GIVE A FAILED RESULT

2/ THE TEST IS A MEASURE OF THE TIME OF A CHEMICAL REACTION AND AS SUCH TEMPERATURE

PLAYS AN IMPORTANT ROLE -AN INCREASE IN TEMPERATURE CAUSES AN INCREASE IN RE-ACTION

TIME, AS DOES A DECREASE IN TEMPERATURE CAUSE A DECREASE IN RE-ACTION TIME THE CORRECT

AND CONSTANT TEMPERATURE FGOR THIS TEST IS 15 DEGREES CENTIGRADE

3/ THE SAMPLE TUBES SHOULD BE CLEANED AS SOON AS THE ANALYSIS IS COMPLETE, AS THE

MANGANESE DIOXIDE FORMED TENDS TO STAIN THE INSIDE OF THE TUBE BROWN AND IS VERY

DIFFICULT TO REMOVE THIS SHOULD BE CLEANED WITH HYDROCHLORIC ACID (ASTM1363-58)

4/ IN ORDER TO MAINTAIN THE REQUIRED TEMPERATURE, A CONSTANT TEMPERATURE WATER BATH WITH

LID SHOULD BE USED, FOR ALL THE SAMPLE TUBES AND THE STANDARD THE WATER TEMPERATURE

SHOULD BE STABLE AT 15 DEGREES CENTIGRADE.

5/ THE COMMENCING TIME OF THE TEST IS WHEN THE KMn04 IS ADDED.

6/ THE PRESENCE OF LIGHT ALSO ADVERSELY EFFECTS THE TIME TEST, CONSEQUENTLY THE TUBES

SHOULD BE KEPT IN A LIGHT FREE (DARK) PLACE, AND INSPECTED ONLY AT THE END OF EITHER THE

30 MINUTES OR 60 MINUTES INTERVAL, (DEPENDING ON THE TIME TEST BEEN CARRIED OUT).THE

FOLLOWING RATIOS SHOULD BE USED WHEN MIXING THE SAMPLES:

TEST SAMPLES

WALL WASH METHANOL .25 ml

POTASSIUM CHLORIDE (KMn04) 1 ml

STANDARD SAMPLE

WALL WASH METHANOL 25 ml POTASSIUM CHLORIDE (KMn04) 1 ml

REMOVE THE TUBES AND INSPECT THEM AGAINST THE STANDARD AFTER THE REQUIRED TIME

LIMIT HAS EXPIRED

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