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Processing kodak motion picture films, module 3 analytical procedures

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Reference Electrode Care/Rejuvenation<br />

For new reference electrodes, withdraw the filling solution<br />

and refill the electrode with 3.5 M KCl (calomel electrodes)<br />

or 3.5 M KCl saturated with AgCl (Ag/AgCl electrodes).<br />

At the beginning of each shift/day, the KCl filling solution<br />

should be withdrawn and the electrode refilled with fresh<br />

3.5 M KCl (calomel electrodes) or 3.6 M KCl saturated with<br />

AgCl (Ag/AgCl electrodes).<br />

When poor performance of the pH measurement system is<br />

not improved with substitution of a new pH electrode,<br />

reference electrode junction clogging may be the problem,<br />

especially where inaccurate or unsteady readings are<br />

obtained. If there is a possibility the filling solution may have<br />

become contaminated, refill with fresh KCl and recheck the<br />

system. Frit-type junctions can be checked for flow by<br />

pressing just the tip of the reference electrode gently against<br />

a paper towel several times. A small wet spot will be visible<br />

if the junction is flowing.<br />

For clogged calomel reference electrodes, warm (not<br />

above 50°C) a solution of 3.5 M KCl diluted 1 part to 9 with<br />

distilled water, and soak the electrode junction for 1/2 hour.<br />

Drain the electrolyte and replace with fresh 3.5 M KCl, and<br />

retest the electrode.<br />

For Ag/AgCl reference electrodes, a 10-minute soak in<br />

10 percent NH 4OH can remove precipitated AgCl from the<br />

junction. It is important that the electrode have filling<br />

solution present when trying this procedure. Higher<br />

concentrations of NH 4OH or longer periods of soaking<br />

should be avoided as in some types of Ag/AgCl reference<br />

electrodes damage to the reference element may occur.<br />

As with glass electrodes, more severe <strong>procedures</strong> are not<br />

recommended as they are costly and, in many cases, do more<br />

to damage the electrode than to improve its performance.<br />

Reference Electrode Accuracy Check<br />

Liquid-junction potential error in reference electrodes can be<br />

assessed * by determining the pH of the NIST equimolar<br />

phosphate buffer (See pH 7 Equimolar Phosphate Reference<br />

Buffer in APPENDIX A) at two ionic strengths differing by a<br />

factor of 10. The meter is standardized with the NIST<br />

phosphate buffer (pH 7, full strength), and the NIST<br />

phthalate buffer (pH 4) as in APPENDIX B. Dilute 110 mL<br />

of the NIST phosphate buffer (pH 7) to 1 L with distilled<br />

water, and measure the pH of the diluted buffer. The meter<br />

reading should be 7.065 ± 0.010 pH units for a properly<br />

functioning reference junction. †<br />

* J.A. Illingsworth, A Common Source of Error in pH Measurements;<br />

Biochem. J. (1981) 195, 259.<br />

† Additional methods for reference electrode evaluation can be found in:<br />

C.C. Westcott pH Measurements; Academic Press: New York (1978)<br />

pp. 65-70.<br />

APPENDIX D<br />

RECOMMENDED COMMERCIALLY<br />

PREPARED BUFFER SOLUTIONS AND THEIR<br />

SOURCES<br />

NIST Reference Buffers<br />

1. pH 1.68, 500 mL, Radiometer America Order No.<br />

511M001<br />

2. pH 4.01, 500 mL, Radiometer America Order No.<br />

511M002 (European No. S1316)<br />

3. pH 6.86, 500 mL, Radiometer America Order No.<br />

511M003 (European No. S1346)<br />

4. pH 9.18, 500 mL, Radiometer America Order No.<br />

511M006 (European No. S1336)<br />

In the U.S., above buffers are available from:<br />

Radiometer America<br />

810 Sharon Drive<br />

Westlake, OH 44145<br />

1-800-736-0600<br />

In Europe, they are manufactured by and available from:<br />

Radiometer A/S<br />

Emdrupvjet 72<br />

Copenhagen NV<br />

Denmark<br />

Calibrating Buffers<br />

1. pH 4, 20-L cube, VWR Scientific, CAT No. 34170-155<br />

2. pH 7, 20-L cube, VWR Scientific, CAT No. 34170-158<br />

VWR Scientific<br />

P.O. Box 483<br />

Bridgeport, NJ 08014<br />

800-932-5000<br />

3. pH 10,20-L cube, Fisher Scientific, CAT No.<br />

SB-115-20<br />

Fisher Scientific Company<br />

50 Fadem Road<br />

Springfield, NJ 07081-3193<br />

800-766-7000<br />

Control Buffers<br />

1. pH 3.63, gallon, SPI CAT No. 1750<br />

Also available in 120-mL and quart volumes<br />

2. pH 11.43, gallon, SPI CAT No. 6805<br />

Also available in 120-mL and quart volumes<br />

These control buffers are manufactured for Kodak by:<br />

Solution Plus, Inc.<br />

2275 Cassens Drive, Suite 147<br />

Fenton, MO 63026<br />

314-349-4922<br />

<strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 11

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