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Processing kodak motion picture films, module 3 analytical procedures

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Potentiometric Determination of Iodide in Reversal Color Developers<br />

ECR-925A<br />

Process ECN-2 ECP-2D VNF-1/LC RVNP<br />

Formulas — — DR-150/151 * DR-150<br />

* This method was developed for a process other than VNF-1 and RVNP<br />

that did not contain sodium thiocyanate. Thiocyanate is a well-known<br />

interferent to halide determinations when using a silver ion titration, due<br />

to co-precipitation. A significant high bias could exist when applying this<br />

procedure to determine bromide in developers containing thiocyanate.<br />

PRINCIPLE<br />

A sample of developer is made highly alkaline to prevent the<br />

formation of an emulsion during the extraction of CD-3 and<br />

RA-1 with chloroform. After the extraction, the aqueous<br />

phase is acidified with glacial acetic acid. The solution is<br />

then titrated potentiometrically with a silver nitrate solution<br />

using silver billet and double junction electrodes. The<br />

inflection point is determined by applying the concentric<br />

arcs technique.<br />

The addition of sodium chloride alters the shape of the<br />

potentiometric curve such that the end point determined by<br />

this technique is slightly beyond the actual inflection point.<br />

However, the concentric arcs technique is used because it<br />

produces more reliable results than other techniques for<br />

determining the location of the end point. The difference<br />

between the determined end point and the actual inflection<br />

point is fairly constant and is calibrated out. See Figure 1 for<br />

a typical titration curve.<br />

Figure 1 Typical Iodide Titration Curve in Reversal<br />

Color Developers<br />

mV<br />

1100<br />

1000<br />

900<br />

800<br />

700<br />

0 5.00 10.00 15.00 20.00<br />

F002_0939AC<br />

mL Standardized 0.005 N Silver Nitrate<br />

This method requires handling potentially hazardous<br />

chemicals. Consult the Material Safety Data Sheet for each<br />

chemical before use. MSDS's are available from your<br />

chemical supplier.<br />

This method uses chloroform-a highly toxic solvent and<br />

suspected carcinogen. The following strict precautions must<br />

be observed when using chloroform:<br />

1. An exhaust (fume) hood must be used that provides<br />

100-ft/min minimum average air face velocity. The<br />

greatest laboratory hazard presented by chloroform is<br />

through inhalation. The odor threshold of chloroform<br />

(50 ppm) is much higher than its threshold limit value<br />

(TLV) of 2 ppm. Therefore, since there is no odor<br />

warning, toxic levels can be present without an<br />

analyst's awareness.<br />

2. Impervious gloves should be worn when handling<br />

chloroform. Chloroform can cause defatting, and<br />

subsequent cracking of the skin. In addition, this<br />

defatting can make the skin more susceptible to<br />

dermatitis from other sources.<br />

3. Eye protection, in the form of safety glasses or goggle<br />

must be worn by the analyst. Chloroform vapors can<br />

cause irritation of the eye—especially to the<br />

conjunctiva (the eye's membrane covering). Splashing<br />

of the liquid into the eye can be painful. If it occurs<br />

despite precautions, wash the eye immediately and<br />

seek medical attention.<br />

4. Keep chloroform away from heat and open flames.<br />

Although not a flammable substance, chloroform may<br />

break down to phosgene (COCl2 ), which further<br />

decomposes to hydrochloric acid and carbon<br />

monoxide after inhalation into the body.<br />

5. Local regulations must be adhered to regarding the<br />

use and/or disposal of chloroform. Regulations<br />

concerning chloroform use may vary from one locality<br />

to another. It is the responsibility of the laboratory<br />

supervisor to be aware of, and follow, these<br />

regulations.<br />

<strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 1

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