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Processing kodak motion picture films, module 3 analytical procedures

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Titration of the Developing Agent with Sulfato<br />

Cerate<br />

Note: The end-point of the titration step can be determined<br />

either potentiometrically (Step 1 below) or visually (Step 2<br />

below).<br />

1. Potentiometric Titration<br />

a. Add 5 drops of ferroin indicator and a magnetic<br />

stir bar to the 250-mL beaker (from steps 6 & 7<br />

of the Back-Extraction of the Developing Agent<br />

procedure).<br />

Note: Do not omit the ferroin, it aids the<br />

definition of the end point.<br />

b. Set the following parameters, if using a<br />

METROHM 536 titrator:<br />

Titration mode mV/pH<br />

Horizontal chart span 750 mV<br />

Autocontrol OFF<br />

Maximum titration speed 15 min/100% volume<br />

Vertical chart span 400 mm/100% volume<br />

Automatic titration stop<br />

(U%)<br />

Indicator electrode<br />

Reference electrode<br />

OFF<br />

Platinum, BECKMAN,<br />

Model 39373 or equivalent<br />

Double-junction ORION,<br />

Model 900200 or equivalent<br />

c. Place the 250-mL beaker on the METROHM<br />

titrator stand. Place the electrodes in the beaker.<br />

(NOTE: The titrant delivery tip should be placed<br />

so that the titrant flows past the reference<br />

electrode before the platinum electrode.) Set the<br />

stirrer speed to stir rapidly without splashing or<br />

creating a vortex. Titrate the solution with<br />

standardized 0.05 N sulfato cerate through the<br />

inflection.<br />

d. Determine the end point using concentric arcs.<br />

(Refer to Universal Method ULM-0003-01,<br />

Potentiometric Titrations for Photoprocessing<br />

Solutions, or any subsequent revisions.) Record<br />

the end point as mL A.<br />

e. Add 100 mL of 1.0 N sulfuric acid to a second<br />

250-mL beaker containing a magnetic stir bar.<br />

Add 5 drops of ferroin indicator.<br />

f. Place the second beaker on the METROHM<br />

titrator stand and titrate through the inflection<br />

point with standardized 0.05 N sulfate cerate.<br />

Record any measurable end point as mL B.<br />

(This is the blank. This determination needs to<br />

be performed only once, if a series of analyses<br />

will be performed.)<br />

2. Visual Titration:<br />

a. Place the 250-mL beaker (from steps 6 & 7 of<br />

the Back-Extraction of the Developing Agent<br />

procedure) on a magnetic stirrer. Add 5 drops of<br />

ferroin indicator. Turn the magnetic stirrer on<br />

and adjust the setting so that the solution stirs<br />

vigorously but without creating a vortex or<br />

splashing.<br />

b. Using a 25-mL burette, titrate the solution with<br />

standardized 0.05 N sulfato cerate to the first<br />

green color that persists for 15 seconds. Add the<br />

titrant dropwise when within an estimated 2 mL<br />

of the end point, allowing sufficient time for<br />

mixing before making another addition. Record<br />

the end point as mL A.<br />

c. Add 100 mL of 1.0 N sulfuric acid to a second<br />

250-mL beaker containing a magnetic stir bar.<br />

Add 5 drops of ferroin indicator and place the<br />

beaker on a magnetic stirrer. Turn the magnetic<br />

stirrer on and adjust the setting so that the<br />

solution stirs vigorously without creating a<br />

vortex or splashing.<br />

d. Titrate the solution to the first light blue color<br />

that persists for 30 seconds. Record the end point<br />

as mL B. (This is the blank. This determination<br />

needs to be determined only once, if a series of<br />

analyses will be performed.)<br />

<strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 5

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