Wall Wash

WALL WASH TEST PROCEDURE
FIRST TEST : ALPHA COLOUR TEST

REASON : VISUAL MEASUREMENT OF THE COLOUR OF ESSENTIALLY LIGHT LIQUIDS
PROCEDURE:
1) PREPARE STANDARD COLOUR SOLUTION IN A TEST TUBE.
METHOD: 100ml DI WATER + 1ml ALPHA 500 STANDARD SOLUTION/PKLATINUM COBALT SOLUTION FOR A COLOUR STANDARD NO: 5
100ml DI WATER + 2ml ALPHA 500 STANDARD SOLUTION/PKLATINUM COBALT SOLUTION FOR A COLOUR STANDARD NO:10
100ml DI WATER + 3ml ALPHA 500 STANDARD SOLUTION/PKLATINUM COBALT SOLUTION FOR A COLOUR STANDARD NO: 15
2) IN ANOTHER TEST TUBE TAKE 100ml OF WALL WASH SOLUTION ( PASS THRU FILTER PAPER IF VISIBLE TURBIDITY )
3) COMPARE BOTH TEST TUBES.
HINT : VIEW BOTH TUBES FROM THE TOP HAVING A BLACK BACK GROUND.
IF COLOUR LIES BETWEEN TWO COLOUR STANDARDS , REPORT THE DARKER OR THE RANGE BETWEEN WHICH IT LIES.
SECOND TEST : TEST FOR HYDROCARBONS ( WATER MISCEBILITY TEST )

REASON : HYDRO CARBON INSOLUBLE IN WATER.WILL RESULT IN CLOUDINESS IN THE MIXTURE.
PROCEDURE:
1) 50ml WALL WASH + 50ml DI WATER IN TEST TUBE.INVERT,STAND FOR 20 MINS.(Other Combinations 40mlWW+60mlDI, 25mlWW+75mlDI, & 10mlWW+90mlDI )
2) STANDARD SOLUTION FOR COMPARISON.50ml MEOH USED FOR WW+50mL DI WATER.INVERT STAND FOR 20 MINS.( USE SAME COMBINATION AS USED ABOVE )
HINT : PLACE TUBES ON BLACK SURFACE.DARKEN THE ROOM.SHINE A WIDE BEAM 6INCH FROM THE SIDE.LOOK FROM ABOVE
CLOUDINESS COULD BE DUE TO GRADUATION ON TUBE IS BLUE,COLUMN IS DIRTY,BULKHEAD IS DAMP.
IF INTENSE BEAM IS USED EVEN STANDARD SOLUTION SHOWS A FAINT WHITISH TRACE.
THIRD TEST ( METHOD 1 ) : TEST FOR CHLORIDES

REASON : FOR DETECTING CHLORIDE IONS.
PROCEDURE:
1) USE SAME SOLUTION FROM THE SECOND TEST.IF NO HYDROCARBONS ARE FOUND.
2) ADD 5 DROPS OF SILVER NITRATE SOLUTION.
3) INVERT AND OBSERVE IF TURBIDITY IS FORMED.
4) STANDARD SOLUTION:
1ml 100PPM CHLORIDE STANDARD SOLUTION + 25 ml MEOH + 75 ml DI WATER = 1 PPM CHLORIDE SOLUTION.
2ml 100PPM CHLORIDE STANDARD SOLUTION + 25 ml MEOH + 75 ml DI WATER = 2 PPM CHLORIDE SOLUTION. AND SO ON FOR HIGHER PPM.
HINT: PLACE ON DARK BACKGROUND, DARKEN ROOM, LOOK FROM TOP, USE WIDE BEAM 12 INCH FROM SIDE.
THIRD TEST ( METHOD 2 ) : TEST FOR CHLORIDE IONS
REASON : FOR DETECTING CHLORIDE IONS.
PROCEDURE :
TEST TUBE ' A ' TEST TUBE ' B ' TEST TUBE 'C '
1) 20ml DI WATER 20ml DI WATER 20ml DI WATER
2) 5ml WALL WASH 5ml MEOH USED IN WW 0.25ml 100 PPM CHLORIDE STANDARD
SOLUTION FOR 5 PPM CHLORIDE STANDARD.
3) 1ml 20% NITRIC ACID 1ml 20% NITRIC ACID 1ml 20% NITRIC ACID
4) 1ml( 0.1 )10% SILVER NITRATE 1ml( 0.1 )10% SILVER NITRATE 1ml( 0.1 )10% SILVER NITRATE
SOLUTION SOLUTION SOLUTION
5) CAP ALL TUBES AND INVERT SEVERAL TIMES.
6) ALLOW TO STAND FOR 10 MINS IN THE DARK.
7) COMPARE TUBES ' A ' AND ' B '
8) CHECK TUBE FOR CONTAMINATION.SHOULD BE CLEAR.
HINT : VIEW AGAINST BLACK BACKGROUND.

STANDARD SOLUTION : 2 PPM = 0.12 ml 100 PPM CHLORIDE STANDARD TO TEST TUBE 'C' IN STEP NO 2
: 10 PPM = 0.5 ml 100 PPM CHLORIDE STANDARD TO TEST TUBE 'C' IN STEP NO 2
: 15 PPM = 0.75 ml 100 PPM CHLORIDE STANDARD TO TEST TUBE 'C' IN STEP NO 2
FOURTH TEST : PERMANGANATE TIME TEST

REASON : FOR IMPURITIES IN THE WALL WASH
PROCEDURE :
1) PREPARE POTASSIUM PERMANGATE SOLUTION ( KMNO4 ).
0.1 gm KMNO4 CRYSTALS + 500 ml DI WATER ( SUITABLE FOR 1 WEEK )
2) 50 ml WALL WASH PLACED IN CONSTANT TEMPARATURE BATH OF 15 DEG C.
3) ADD 2 ml OF KMNO4 SOLUTION TO THE WALL WASH.INVERT, RETURN TO THE BATH.START THE STOP WATCH.
4) SAME PROCEDURE FOR STANDARD MEOH SOLUTION.
5) TAKE THE TIME DOWN WHEN THE COLOUR CHANGES FROM PINK TO YELLOW FOR BOTH THE TUBES.
6) CALCULATE PTT = WW TIME / STANDARD TIME x 120 MINS
HINT : PROTECT THE TUBE FROM LIGHT.
FIFTH TEST : ACID WASH FOR AROMATIC HYDRO CARBONS

REASON : DETERMINATION OF THE ACID WASH FOR AROMATIC HYDROCARBONS.
PROCEDURE :
1) FILL A TEST TUBE WITH 7 ml OF SULFURIC ACID OF STRENGTH AS IN TABLE GIVEN BELOW.
2) ADD SUFFICIENT WALL WASH TO BRING THE VOLUME TO 28 ml AND INSERT STOPPER AND SHAKE VIGOROUSLY FOR 40 TO 50 SEC.
3) ALLOW TO STAND FOR THE TIME SPECIFIED IN TABLE AWAY FROM SUNLIGHT
4) INVERT ONCE AND COMPARE TO THOSE OF STANDARDS.
5) SEE TO NEAREST NUMBER OF STANDARD ADD PLUS OR MINUS IF ABOVE OR BELOW TO THE CLOSEST.
HINT : COMPARE WITH WHITE BACKGROUND OR DAYLIGHT.
TABLE 1 ACID STRENGTHS AND STANDING TIME
SAMPLE ACID STRENGTHS STANDING TIME
) Benzene, All ASTM Grades

) Tolune, All ASTM Grades
GROUP 1 ) Xylene, Nitration Grades 96 15
) Xylene , 5˚
) Xylene , 10˚
GROUP 2 ) Xylene , Industrial Grade 96 5

) Refined solvent Naptha
GROUP 3 ) Hi-Flash solvent 78 5

) Heavy solvent naptha

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WALL WASH TEST PROCEDURE

FIRST TEST : ALPHA COLOUR TEST

SECOND TEST : TEST FOR HYDROCARBONS ( WATER MISCEBILITY TEST )

THIRD TEST ( METHOD 1 ) : TEST FOR CHLORIDES

HINT : VIEW AGAINST BLACK BACKGROUND.

FOURTH TEST : PERMANGANATE TIME TEST

HINT : PROTECT THE TUBE FROM LIGHT.

FIFTH TEST : ACID WASH FOR AROMATIC HYDRO CARBONS

HINT : COMPARE WITH WHITE BACKGROUND OR DAYLIGHT.

TABLE 1 ACID STRENGTHS AND STANDING TIME

SAMPLE ACID STRENGTHS STANDING TIME

) Benzene, All ASTM Grades

GROUP 2 ) Xylene , Industrial Grade 96 5

GROUP 3 ) Hi-Flash solvent 78 5

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