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1. CONTROL OF ABSORBANCE TEST.

PART 1

STEP 1: DRY POTASSIUM DICHROMATE  AT 120°C FOR THREE HRS,


STEP 2 : BLANK : PREPARED  0.005M H2SO4 ( 0.30 ML CONC. H2SO4 IN
1100 ML DIS.WATER). ((BLANK)) 100 ml
STEP 3: THEN TAKE OUT 100 ML OF THE SAME SOLUTION.
STEP 4: DISSOLVE 57 - 63 MG OF POTASSIUM DICHROMATE  TO THE 1000
ML OF ABOVE MADE SOLUTION. ((SAMPLE))
STEP 5: SCAN THE SAMPLE AND BLANK  400 TO 220 NM AND  OBSERVE
THE OD (ABS) AT FOLLOWING NM  VIZ  .. 235, 257, 313 & 350.
STEP 6 : CALCULATE % TOLERANACE LIMIT  AS FOLLOWS
 
% TOLERANACE LIMIT FOR Abs at 235,257,313,350 nm = (ABS/ WT OF
POT.DICHROMATE TAKEN) * 10* 1000

 WHERE 10= PATH LENGTH OF THE CUVETTE in mm


& 1000 = VOLUME TAKEN

Weight of Pot.. DICHROMATE (K2Cr2O7):

WL                           ABS         % TOLERANCE LIMIT            PERMTD. RANGE


235 NM:                                                  122.9  -  126.2
257 NM:                                                  142.4  -  145.7
313 NM:                                                    47.0  -  50.3
350 NM:                                                   104.9 - 108.2

PART 2

STEP 1: BLANK: PREPARED  0.005M H2SO4 ( 0.27 ML CONC. H2SO4 IN


1000 ML DIS.WATER). ((BLANK)) 900 ml
STEP 2: THEN TAKE OUT 100 ML OF THE SAME SOLUTION.
STEP 3: DISSOLVE 57 -63 MG OF POTASSIUM DICHROMATE TO THE 100
ML OF ABOVE MADE SOLUTION. ((SAMPLE))
STEP 4: DO AUTO ZERO OF SAMPLE AND BLANK AT 430 NM AND 
OBSERVE THE OD (ABS) AT FOLLOWING NM  VIZ 430 NM.
STEP 5 : CALCULATE % TOLERANACE LIMIT  AS FOLLOWS

% TOLERANACE LIMIT FOR Abs at 430 nm = (ABS/ WT OF


POT.DICHROMATE TAKEN) * 10* 100

WHERE 10= PATH LENGTH OF THE CUVETTE


& 100 = VOLUME TAKEN

 Weight of Pot. DICHROMATE (K2Cr2O7):


WL                           ABS             % TOLERANCE LIMIT    PERMTD. RANGE
430 NM: 15.7 - 16.1
  2.  STRAY LIGHT TEST
STD KCL DRIED AT 120°C FOR 1 HOUR, DISSOLVED 1.2 gm OF KCl IN 100
ml DIS.WATER.
SCANNED THE SOLUTION IN THE SPECTRUM MODE FROM 210 TO 190 NM
DIS. WATER AS BLANK
FOUND THE ABSORPTION WAS MORE THAN 2.0 AT 200 NM.
 
 
3. RESOLUTION POWER
1. DISSOLVE 0.5 ml OF TOLUENE IN 50 ml OF HEXANE. THEN TAKE OUT 1
ml OF THIS SOLUTION & MIX WITH 50 ml OF HEXANE AGAIN. THIS IS THE
SOLUTION PREPARED FOR RESOLUTION POWER.
2. SCANNED THE SAMPLE FROM 275 – 260 NM, HEXANE AS BLANK.
3. FOUND THE ABSORPTION MAXIMA NEAR ABOUT 269 NM &
MINIMA AT 266 NM
4. RATIO OF THE MAXIMA AND MINIMA SHOULD BE MORE THAN 1.5 
 
4. Control Of Wavelength
VERIFY THE WAVELENGTH SCALE USING THE ABSORPTION MAXIMA OF
HOLMIUM PER CHLORATE SOLUTION R, THE LINE OF THE HYDROGEN OR
DEUTERIUM DISCHARGE LAMP OR THE LINES OF MERCURY VAPOURS ARE
SHOWN IN THE TABLE SHOWN. PERMITTED TOLERANCE IS ±1 NM FOR THE
ULTRAVIOLET RANGE & ±3 NM FOR THE VISIBLE RANGE. SUITABLE CERTIFIED
REFERENCE MATERIALS MAY ALSO BE USED.

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