Processing kodak motion picture films, module 3 analytical procedures
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Processing kodak motion picture films, module 3 analytical procedures

Processing kodak motion picture films, module 3 analytical procedures Processing kodak motion picture films, module 3 analytical procedures

motion.kodak.com
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22.07.2013 Views

REPRODUCIBILITY Customer Standard Deviation, 1sc & 95 Percent Confidence Estimate (not including bias) The Reproducibility or customer standard deviation (1sc ) is an estimate of the variability a customer could expect when submitting a sample to any Photoprocessing Quality Services laboratory, where any trained analyst could test the sample using any instrument on any day. The 95 percent confidence estimate (calculated using the customer standard deviation) around a single test result will include the mean value 95 percent of the time. Four analysts analyzed four Accelerator tank samples, on two different days. Duplicate analyses were performed on each sample, on each of the two days. These samples were: 1. A “fresh” Accelerator tank solution prepared with all components at their respective “working tank” aim concentrations. 2. A “seasoned” Accelerator tank solution analyzed as received as 3.55 g/L PBA-1. 3. The same “seasoned” solution, as in number 2, above, analyzed in the same manner, after making a standard addition of 1.2327 g/L PBA-1. Sample “Fresh” (prepared at 3.31 g/L) “Seasoned” As Received “Seasoned” plus Standard Addition Mean (g/L PBA-1) N PBA-1 Reproducibility Standard Deviation, 1s c (g/L PBA-1) 95 Percent Confidence Estimate (g/L PBA-1) 3.31 16 0.104 ± 0.22 3.55 16 0.022 ± 0.05 4.81 16 0.040 ± 0.09 Bias Bias is a statistically significant deviation of the mean from the known mix level at a 95 percent confidence level. It is determined for fresh samples only. Bias was not determined for this sample because the component concentration level was not determined independently of the test method. No statistically significant bias was found at the 95 percent confidence level. Recovery Recovery is used for seasoned samples, since the component concentration level was not determined independently of the test method. It is defined as the calculated mean for the seasoned sample with a standard addition of the component minus the mean for the seasoned sample, divided by the actual amount of the standard addition. It is expressed as a percentage. Statistically, the recovery of 102.21 percent was significantly different from 100 percent at the 95 percent confidence level, however it was judged not to be practically significant. APPARATUS Metrohm E536 Autotitrator or equivalent Orion Silver-Silver Sulfide Electrode, Catalog No. 941600 or equivalent (Note: DO NOT use a silver billet or bar electrode as prepared in SLM-1295) Orion Double Junction Reference Electrode, Catalog No. 90-02-00 or equivalent Pipet (50.0 mL) Tip-up pipet (10 mL) Graduated Cylinder (250 mL) All volumetric glassware should meet all Class A specifications, as defined by American Society for Testing and Materials (ASTM) Standards E 287, E288, and E969, unless otherwise stated. REAGENTS All reagents should be ACS Reagent Grade unless otherwise specified. 10 N Sodium Hydroxide, NaOH 0.0500 N Silver Nitrate, AgNO3 (standardized to four decimal places) Water, Type I Reagent - This method was developed using reagent water equivalent to or purer than Type I grade, as defined in ASTM Standard D 1193. Other grades of water, e.g., reverse osmosis (RO), demineralized, or distilled water, may give equivalent results, but the effects of water quality on method performance have not been studied. 2 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03

PROCEDURE A. Preparation of Sample 1. Pipet (wipe the pipet before leveling) 50.00 mL of sample into a 400 mL beaker containing a magnetic stir bar. 2. Using a tip-up pipet, add 10 mL of 10 N sodium hydroxide to the beaker containing the sample. Caution Caustic, avoid contact with skin and eyes. In case of contact, flush with water. 3. Place the beaker on a magnetic stirrer and set a timer for 3 minutes. 4. After the solution has stirred for 3 minutes, add 250 mL of reagent water to the beaker from a graduated cylinder. B. Titration of Sample 1. Titrate the solution with 0.0500 N silver nitrate, using a METROHM E536 Titrator or equivalent. Caution Silver nitrate is poisonous, causes burns, and stains skin. Avoid contact. a. Set the following parameters on the METROHM E536Titrator: Potentiograph E536 Control Setting Titration mode mV/pH Horizontal chart span 750 mV Auto Control 8 min/100% volume 20 MV x 100 -1 mV /pH 100% °C Auto Indicator electrode Silver/silver sulfide Reference electrode Model 900200 or equivalent Dosimat 655Control Setting Buret Size 20 mL Mode Switch Mode 1 b. Place the beaker on the METROHM titrator stand and add a magnetic stir bar. Place the electrodes in the beaker. (NOTE: The titrant delivery tip should be placed so that the titrant flows past the reference electrode before the platinum electrode.) Set the stirrer speed to stir rapidly without splashing or creating a vortex. Titrate the solution with standardized 0.0500 N silver nitrate through the inflection. c. Determine the end point using concentric arcs (refer to Method ULM-0003-01, Potentiometric Titrations for Photoprocessing Solutions or any subsequent revisions.) If a microprocessor controlled titrator is used, the endpoint will be picked automatically. A typical titration curve is shown in Figure 1. Figure 2 S-shaped Curves Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 3 −350 −500 −650 + MiliVolts − −800 MiliLiters F002_1126GC

PROCEDURE<br />

A. Preparation of Sample<br />

1. Pipet (wipe the pipet before leveling) 50.00 mL of<br />

sample into a 400 mL beaker containing a magnetic<br />

stir bar.<br />

2. Using a tip-up pipet, add 10 mL of 10 N sodium<br />

hydroxide to the beaker containing the sample.<br />

Caution<br />

Caustic, avoid contact with skin and eyes. In case of<br />

contact, flush with water.<br />

3. Place the beaker on a magnetic stirrer and set a timer<br />

for 3 minutes.<br />

4. After the solution has stirred for 3 minutes, add<br />

250 mL of reagent water to the beaker from a<br />

graduated cylinder.<br />

B. Titration of Sample<br />

1. Titrate the solution with 0.0500 N silver nitrate, using<br />

a METROHM E536 Titrator or equivalent.<br />

Caution<br />

Silver nitrate is poisonous, causes burns, and stains<br />

skin. Avoid contact.<br />

a. Set the following parameters on the<br />

METROHM E536Titrator:<br />

Potentiograph E536<br />

Control<br />

Setting<br />

Titration mode mV/pH<br />

Horizontal chart span 750 mV<br />

Auto Control 8<br />

min/100% volume 20<br />

MV x 100 -1<br />

mV /pH 100%<br />

°C Auto<br />

Indicator electrode Silver/silver sulfide<br />

Reference electrode Model 900200 or<br />

equivalent<br />

Dosimat 655Control Setting<br />

Buret Size 20 mL<br />

Mode Switch Mode 1<br />

b. Place the beaker on the METROHM titrator<br />

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

electrodes in the beaker. (NOTE: The titrant<br />

delivery tip should be placed so that the titrant<br />

flows past the reference electrode before the<br />

platinum electrode.) Set the stirrer speed to stir<br />

rapidly without splashing or creating a vortex.<br />

Titrate the solution with standardized 0.0500 N<br />

silver nitrate through the inflection.<br />

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

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

Titrations for Photoprocessing Solutions or any<br />

subsequent revisions.) If a microprocessor<br />

controlled titrator is used, the endpoint will be<br />

picked automatically. A typical titration curve is<br />

shown in Figure 1.<br />

Figure 2 S-shaped Curves<br />

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

−350<br />

−500<br />

−650<br />

+ MiliVolts<br />

−<br />

−800<br />

MiliLiters<br />

F002_1126GC

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