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Processing kodak motion picture films, module 3 analytical procedures

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PROCEDURE<br />

A. Sample Treatment<br />

1. Pipet 10.0 mL of sample into a l00-mL volumetric<br />

flask containing approximately 50 mL of reagent<br />

water.<br />

2. Bring to volume with reagent water and invert the<br />

flask 6 to 9 times to mix.<br />

3. Pipet 10.0 mL from the l00-mL volumetric flask into a<br />

250-mL beaker containing 100 mL of reagent water<br />

and a magnetic stir bar.<br />

4. Add 10 mL of 7.0 N sulfuric acid from a tip-up pipet.<br />

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

stirrer.<br />

B. Titration<br />

1. Set the following parameters on the METROHM<br />

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 (U%) OFF<br />

Indicator electrode Silver/Sulfide Ion<br />

Selective, Orion<br />

Model 941600 or<br />

equivalent<br />

Reference electrode Double-Junction, Orion<br />

Model 900200 or<br />

equivalent<br />

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

stand and add a magnetic stir bar. Place the electrodes<br />

in the beaker. (NOTE: The titrant delivery tip should<br />

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

electrode before the silver/silver 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 silver nitrate through the<br />

inflection.<br />

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

to Method ULM-0003-01, Potentiometric Titrations<br />

for Photoprocessing Solutions, or any subsequent<br />

revisions. If a microprocessor-controlled titrator is<br />

used, the endpoint will be picked automatically.<br />

CALCULATIONS<br />

For NH 4 Br;<br />

g/L NH 4 Br = (mL AgNO 3) (N AgNO 3) (eq wt NH 4Br) (10) (1000)<br />

(mL sample)(1000)<br />

Where<br />

mL AgNO3 = volume of AgNO3 in millilitres required to<br />

reach the equivalence point<br />

N = normality of the AgNO3 in milliequivalents per<br />

millilitre (meq/mL)<br />

eq wt = equivalent weight of ammonium bromide in<br />

milligrams per milliequivalent (97.9 mg/meq)<br />

10 = dilution factor for sample<br />

mL sample = millilitres of sample pipetted in step 1 of part A<br />

of procedure<br />

1000 = factor to convert meq to eq in the numerator<br />

and mL to L in the denominator<br />

If mL 0.0492 N AgNO 3 = 10.34 mLs:<br />

(10.34) (0.0492) (97.9) (10) (1000)<br />

g/L NH4Br =<br />

(10.00) (1000)<br />

= 49.8 g/L NH4Br Figure 2 S-shaped Curves<br />

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

+150<br />

0<br />

−150<br />

+ MiliVolts<br />

−<br />

−300<br />

6 MiliLiters<br />

5<br />

4<br />

3<br />

2<br />

1<br />

F002_1123GC

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