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
water droplets adhere to the inside walls of the glassware after one minute of draining, it is not sufficiently clean. Only an unbroken film of water should remain. Burets and pipets should drain in a vertical position. Volumetric flasks are inverted with the bottom at a slight angle from the horizontal, so that drops on the bottom will drain away. If burets and pipets are clean, they generally do not have to be dried before being used with standard solutions. The slight amount of water which remains after rinsing and draining is removed by rinsing two or three times with small amounts of the solution to be used, allowing the buret or pipet to drain completely between rinses. If it is necessary to have volumetric vessels dry, a gentle stream of clean air can be used. Acetone should not be used as a drying agent because of the likelihood of trace amounts left in glassware causing unwanted absorption in ultraviolet methods of analysis. Use of Volumetric Glassware 1. General Instructions a. Effects of Temperature on Glassware and Solutions: Glassware—The temperature at which volumetric vessels are calibrated is 20°C (68°F). For the greatest precision and accuracy, all measurements should be made at this temperature. Since this condition may not be practicable, it is important to consider the magnitude of the errors introduced into volumetric procedures by using standard solutions at temperatures other than 20°C (68°F). The change in capacity of glass volumetric apparatus with temperature is, at the most, only 1 part in 10,000 for each 5°C change in temperature in the region of 20°C. This source of error generally may be disregarded. Solutions—Whereas the change in capacity of glassware with temperature generally may be disregarded, it is not to be confused with the change in volume of a solution with temperature. The effect of temperature on volume is shown in Table 2. To attain accuracy of approximately 0.1 percent it is necessary that the solution be at 20 ± 2°C (68 ± 3.6°F) when measured. The change in concentration of standard solutions is also affected by temperature. It may become of such magnitude as to introduce appreciable errors. In general, the more concentrated the solution the more serious the change. The coefficient of expansion of dilute aqueous solutions of different electrolytes is practically the same for similar concentrations and hence, the values given in Table 2 serve as a general index of their behavior. b. Meniscus In the use of graduated cylinders, pipets, burets, and flasks, the lowest point of the meniscus should be taken as the reading. See Figures 1 and 2. Opaque solutions, however, must be measured by reading at the top of the meniscus. Another special case is the determination of specific gravity. The top of the meniscus is read because the hydrometer is calibrated on that basis. Figure 1 Reading the Meniscus on a Pipet or Volumetric Flask F002_0901AC Figure 2 Reading the Meniscus on a Buret F002_0900AC Correct Line of Vision Excessive Volume 2 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 Deficient Volume Low Reading Correct Line of Volume High Reading
In observing the lowest point on the meniscus it is very important that the line of vision be in the same horizontal plane as the bottom of the meniscus. This is easily ascertained if the graduations on the glassware extend at least halfway around the tube. The eye is correctly positioned when both front and back portions of the graduation coincide (Figures 1 and 2). The meniscus may be seen more clearly if a small white card with a rectangular black patch is held behind the meniscus. Raise or lower the card until the bottom of the meniscus is clearly outlined (Figure 3). Figure 3 Outlining the Meniscus F002_0904AC 2. Pipets Pipet specifications are established on the basis of a pipet's ability to deliver (TD) a known volume of distilled water (20°C [68°F]) within the specified tolerances. Pipets meeting the volume shown in Table 1 have been used successfully. The pipets conforming to these requirements are defined as “Class A.” However, experience has shown that some pipets marked “Class A” do not meet delivery time specifications. Other pipets having shorter delivery time than “Class A” meet “Class A” volume tolerances. Pipets meeting “Class A” volume tolerances but not meeting delivery time requirements may be used for analytical purposes as long as the analyst understands and practices the following instructions on the use of pipets: a. Cleanliness Use a clean pipet. The pipet does not have to be dry, but must be perfectly clean and free from grease so that drops of the solution will not adhere to the walls, causing the pipet to deliver less than the rated volume. Any contaminant may affect the results. b. Perfect Tip Use a pipet with a perfect tip. A pipet with a broken or chipped tip must be discarded since it will deliver a volume other than the rated volume when the tip is touched against the wall of the receiving vessel. c. Rinsing (or Seasoning) With one hand holding the pipet and the other hand holding a rubber bulb, squeeze the bulb, place it over the upper end of the pipet and release slowly. Draw a small portion of the solution into the pipet, i.e., about 20 percent of the volume of the pipet, then remove the bulb and cap the pipet with the forefinger. See Figure 4. Place the pipet in a horizontal position, and rotate it, permitting the solution to wet the walls to a point about two inches above the calibration mark. Do not permit the top of the mouthpiece to become contaminated with solution, which in turn may contaminate the bulb. Discharge the solution through the tip, and repeat the rinsing with another portion of the solution. Note: If the solution being pipeted is a standardized reagent, the reagent is drawn into the pipet from a clean beaker which was rinsed once with reagent. To prevent contamination of the reagent, the pipet should not be placed into the stock bottle. Figure 4 How to Use a Rubber Bulb for Pipeting B. Release bulb and liquid will be drawn up slowly. If suction ceases before pipet is full, remove bulb, recompress, and reapply. F002_0905GC A. Dip pipet tip into liquid. Compress rubber bulb in left hand, and slip bulb over end of pipet. C. When liquid rises above calibration mark, remove bulb and place index finger of right hand to end of pipet. Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 3
- Page 215 and 216: Potentiometric Determination of Eth
- Page 217 and 218: Titrimetric Determination of Ferric
- Page 219 and 220: Iodometric Determination of Ferricy
- Page 221 and 222: Potentiometric Determination of Fer
- Page 223 and 224: Iodometric Determination of Formali
- Page 225 and 226: Spectrophotometric Determination of
- Page 227 and 228: Titrimetric Determination of Hypo I
- Page 229 and 230: Potentiometric Determination of Iod
- Page 231 and 232: Potentiometric Determination of Pot
- Page 233 and 234: Titration Note: For preparation of
- Page 235 and 236: Titrimetric Determination of Persul
- Page 237 and 238: Spectrophotometric Determination of
- Page 239 and 240: APPARATUS Spectrophotometer with a
- Page 241 and 242: APPENDIX B Effect of Temperature in
- Page 243 and 244: Potentiometric Determination of Sil
- Page 245 and 246: Potentiometric Determination of Sod
- Page 247 and 248: Iodometric Determination of Total S
- Page 249 and 250: Titrimetric Determination of Total
- Page 251 and 252: Table 2 Contribution of Constituent
- Page 253 and 254: Determination of Sulfite in KODAK R
- Page 255 and 256: CALCULATIONS Na2SO3 , g/L = (mL B -
- Page 257 and 258: Colorimetric Determination of Thioc
- Page 259 and 260: APPENDIX A Calibration of Spectroph
- Page 261 and 262: Analysis Order for Photographic Pro
- Page 263 and 264: Procedure for Electroplating a Silv
- Page 265: The Selection, Care, and Use of Vol
- Page 269 and 270: 4. Graduated Cylinders and Tip-up P
- Page 271 and 272: 6. Microburets Microburets equipped
- Page 273 and 274: Table 1 Required Tolerance for Volu
- Page 275 and 276: pH Measurement of Photographic Proc
- Page 277 and 278: Temperature Equilibration All sampl
- Page 279 and 280: Low-range pH Measurements (pH 1-7)
- Page 281 and 282: Preparation of Control Buffers 1. p
- Page 283 and 284: Standardization of pH Meter - Low p
- Page 285 and 286: Reference Electrode Care/Rejuvenati
- Page 287 and 288: Potentiometric Titrations for Photo
- Page 289 and 290: difference corresponds to the poten
- Page 291 and 292: Determination of Residual Thiosulfa
- Page 293 and 294: APPENDIX A Calibration Procedure Th
- Page 295 and 296: Determination of Silver in Thiosulf
- Page 297 and 298: Note: The appropriate amounts of 0.
- Page 299 and 300: The Determination of Specific Gravi
- Page 301 and 302: Instructions for Performance Checks
- Page 303 and 304: Processing KODAK Motion Picture Fil
water droplets adhere to the inside walls of the<br />
glassware after one minute of draining, it is not<br />
sufficiently clean. Only an unbroken film of water<br />
should remain. Burets and pipets should drain in a<br />
vertical position. Volumetric flasks are inverted with<br />
the bottom at a slight angle from the horizontal, so that<br />
drops on the bottom will drain away. If burets and<br />
pipets are clean, they generally do not have to be dried<br />
before being used with standard solutions. The slight<br />
amount of water which remains after rinsing and<br />
draining is removed by rinsing two or three times with<br />
small amounts of the solution to be used, allowing the<br />
buret or pipet to drain completely between rinses. If it<br />
is necessary to have volumetric vessels dry, a gentle<br />
stream of clean air can be used. Acetone should not be<br />
used as a drying agent because of the likelihood of<br />
trace amounts left in glassware causing unwanted<br />
absorption in ultraviolet methods of analysis.<br />
Use of Volumetric Glassware<br />
1. General Instructions<br />
a. Effects of Temperature on Glassware and<br />
Solutions:<br />
Glassware—The temperature at which<br />
volumetric vessels are calibrated is 20°C (68°F).<br />
For the greatest precision and accuracy, all<br />
measurements should be made at this<br />
temperature. Since this condition may not be<br />
practicable, it is important to consider the<br />
magnitude of the errors introduced into<br />
volumetric <strong>procedures</strong> by using standard<br />
solutions at temperatures other than 20°C<br />
(68°F). The change in capacity of glass<br />
volumetric apparatus with temperature is, at the<br />
most, only 1 part in 10,000 for each 5°C change<br />
in temperature in the region of 20°C. This source<br />
of error generally may be disregarded.<br />
Solutions—Whereas the change in capacity of<br />
glassware with temperature generally may be<br />
disregarded, it is not to be confused with the<br />
change in volume of a solution with<br />
temperature. The effect of temperature on<br />
volume is shown in Table 2. To attain accuracy<br />
of approximately 0.1 percent it is necessary that<br />
the solution be at 20 ± 2°C (68 ± 3.6°F) when<br />
measured.<br />
The change in concentration of standard<br />
solutions is also affected by temperature. It may<br />
become of such magnitude as to introduce<br />
appreciable errors. In general, the more<br />
concentrated the solution the more serious the<br />
change. The coefficient of expansion of dilute<br />
aqueous solutions of different electrolytes is<br />
practically the same for similar concentrations<br />
and hence, the values given in Table 2 serve as a<br />
general index of their behavior.<br />
b. Meniscus<br />
In the use of graduated cylinders, pipets, burets,<br />
and flasks, the lowest point of the meniscus<br />
should be taken as the reading. See Figures 1<br />
and 2. Opaque solutions, however, must be<br />
measured by reading at the top of the meniscus.<br />
Another special case is the determination of<br />
specific gravity. The top of the meniscus is read<br />
because the hydrometer is calibrated on that<br />
basis.<br />
Figure 1<br />
Reading the Meniscus on a Pipet or Volumetric Flask<br />
F002_0901AC<br />
Figure 2 Reading the Meniscus on a Buret<br />
F002_0900AC<br />
Correct Line<br />
of Vision<br />
Excessive<br />
Volume<br />
2 <strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03<br />
Deficient<br />
Volume<br />
Low<br />
Reading<br />
Correct Line<br />
of Volume<br />
High<br />
Reading