Processing kodak motion picture films, module 3 analytical procedures

APPARATUS
All volumetric glassware should meet all “Class A”
specifications, as defined by American Society for Testing
and Materials (ASTM) Standards E 287, E 288, and E 969,
unless otherwise stated.
Pipette, (50-mL)
Separatory funnels, (250-mL)
Beakers, (250-mL)
Exhaust hood
METROHM 536 Titrator or equivalent with a DOSIMAT
and a 20-mL burette
Platinum indicator electrode, BECKMAN, Model 39273
or equivalent
Double junction reference electrode, ORION Model
900200 or equivalent
Filling solutions:
– ORION No. 900002 (inner chamber)
– ORION No. 900003 (outer chamber)
Burette, (25-mL) / (visual method only)
Magnetic stirrer / (visual method only)
REAGENTS
Use ACS Reagent Grade reagents unless specified
otherwise.
Polystyrene Sulfonate, (0.1%)
Butyl Acetate
Ferroin Indicator
Sulfuric Acid, H 2SO 4, (1.0 N)
Sulfato Cerate, (NH 4) 2Ce(NO 3) 6, (0.05N) standardized to
4 places past the decimal point
Sodium Chloride, NaCl
PROCEDURE
Extraction of the Developing Agent, CD-3, with
Butyl Acetate
1. Pipette 50.0 mL (potentiometric titration) or 50.0 mL
(visual titration) of sample into a 250-mL separatory
funnel (No. 1).
2. Add 5.0 g NaCl to the separatory funnel.
3. Add 2 mL of 0.1% polystyrene sulfonate solution.
Stopper the funnel and mix, by gently swirling or
shaking, until all the salt completely dissolves.
4. Add 50 mL of butyl acetate. Swirl the funnel for 30
seconds. Stopper the funnel, invert and vent through
the stopcock. Shake separatory funnel No. 1,
horizontally, for a few seconds; invert and vent the
funnel through the stopcock. Continue to shake
vigorously for 30 seconds. The funnel should be
vented at least 2 times.
5. Allow the layers to separate. Gently swirling the
funnel will aid breaking up any emulsion at the
aqueous-nonaqueous interface.
6. After separation of the layers occurs, transfer the lower
(aqueous) layer, as completely as possible, including
any emulsion that fails to separate, into another
250-mL separatory funnel (No. 2).
7. Swirl separatory funnel No. 1. Drain any additional
lower (aqueous) layer that separates into separatory
funnel No. 2. Save the top (butyl acetate) layer in
separatory funnel No. 1.
8. Add 50 mL of butyl acetate to separatory funnel No. 2.
Swirl the funnel for 30 seconds. Stopper the funnel;
invert and vent through the stopcock. Shake the funnel
horizontally for a few seconds; invert and vent through
the stopcock. Continue to shake the funnel vigorously
for 30 seconds, venting at least 2 times.
9. After the layers separate, discard the lower (aqueous)
layer as completely as possible. Swirl the funnel and
discard any additional aqueous layer that separates,
taking care not to lose any of the butyl acetate layer.
Discard any emulsion layer that fails to separate.
Note: Additional separation time may be needed for
highly seasoned samples.
10. Transfer the contents of separatory funnel No. 2 (butyl
acetate layer) into funnel No. 1 (which contains the
first butyl acetate layer).
4 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03