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Processing kodak motion picture films, module 3 analytical procedures

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APPARATUS<br />

Spectrophotometer with a tungsten lamp<br />

1-cm Silica Cell<br />

All volumetric glassware should meet all Class A<br />

specifications, as defined by American Society for Testing<br />

and Materials (ASTM) Standards E 287, E 288, and E 969,<br />

unless otherwise stated.<br />

REAGENTS<br />

All reagents should be ACS Reagent Grade unless otherwise<br />

specified.<br />

KODAK Anti-Calcium, No. 4<br />

Molybdenum Reagent<br />

1.0 N Sulfuric Acid, H 2 SO 4<br />

PROCEDURE<br />

A. Treatment of Sample<br />

1. Add, from a tip-up Pipet, 5 mL of KODAK Anti-<br />

Calcium No. 4 to a 100 mL volumetric flask<br />

containing a magnetic stir bar. (Allow 15 seconds for<br />

the tip-up pipet to drain.)<br />

2. Start stirring moderately. Pipet (wipe the pipet before<br />

leveling) 3.00 mL of Color Developer solution into<br />

the flask.<br />

3. Set, but do not start, a timer for five minutes.<br />

4. Add, from a tip-up pipet, 10 mL of molybdenum<br />

reagent to the flask. Immediately start the timer.<br />

5. To the flask, add, from a graduated cylinder, 80 mL of<br />

1.0 N sulfuric acid that is at room temperature<br />

(20.0°C-24.0°C).<br />

6. Remove the stirring bar and dilute the solution to its<br />

final 100.0 mL volume with 1.0 N sulfuric acid.<br />

7. Stopper the flask and invert it five times to complete<br />

mixing.<br />

B Absorbance Measurement<br />

1. Zero the spectrophotometer vs. air.<br />

2. After four minutes have elapsed, rinse and fill a 1-cm<br />

silica cell with the molybdenum blue solution<br />

(Step A.7, above).<br />

3. Place the cell in the sample compartment of the<br />

spectrophotometer and measure the solution<br />

absorbance at 725-nm (AR) at exactly five minutes<br />

after the addition of the molybdenum reagent in<br />

Step A.4, above. Record the absorbance.<br />

Note: Do not place the cell in the spectrophotometer for<br />

longer than one minute.<br />

CALCULATIONS<br />

y=mx+b<br />

Definition of the equation is found in the Regression section<br />

of Appendix A.<br />

Where:<br />

mg/L RA-1 = m (A 725 )+b<br />

Each laboratory should establish its own regression equation<br />

based on a set of calibration standards. Appendix A explains<br />

this calibration procedure. The regression equation may be<br />

different for each spectrophotometer. A typical regression<br />

equation line for the effluent is described by the following<br />

equation:<br />

Example:<br />

m = slope of the calibration line<br />

[(mg/L) RA-1 / ABU @725 ]<br />

A 725 = Absorbance of sample at 725 nm<br />

b = the intercept of the calibration line<br />

with the y-axis (mg/L RA-1)<br />

mg/L RA-1 = 143.3 (A 725 ) – 4.355<br />

A 725 = 0.847<br />

mg/L RA-1 = 143.3 (0.847) - 4.355<br />

= 117.0<br />

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

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