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
g. Titration After the initial reading is made and the final drop removed, the standard solution is added to the titration vessel with constant swirling. See Figure 7 for the proper way to turn a stopcock. As the end point is approached, the rate of addition is decreased, until finally the titrant is added dropwise or as split drops. At this point, tilt the vessel and remove each drop by touching the tip with the wall of the vessel at a level just above the surface of the liquid. Tilt the vessel slightly more to rinse in the drop. Generally the end point is defined as a specified color change that persists for at least 15 seconds. When the end point has been reached, there should be no final drop to remove. If an end point is not sharp, or if it is unfamiliar, it may be difficult to decide when the end point has been reached. Then after a drop, record the buret reading, add another drop, and note the change produced in the indicator. Continue this procedure until the specified color change has occurred. Figure 7 How to Turn a Stopcock Thumb and forefingers wrap around handle of stopcock to turn cock and apply inward pressure to keep the plug seated. F002_0907AC Seating pressure absorbed by last two fingers pushing against tip of buret. h. Drainage Error Unless the titration to the end point has been slow and gradual, wait 30 seconds before taking the final reading of the meniscus, so that the effect of further drainage will be negligible. Read meniscus at eye level. i. Cleaning Buret Clean the buret with cleaning solution. Prevent the concentrated cleaning solution from coming into contact with the stopcock lubricant. A convenient way to clean burets without removing any of the stopcock lubricant is to invert them in a pipet jar containing enough cleaning solution to fill the buret to the stopcock. After a few minutes, rinse inside and out with tap water, then rinse three times with small quantities of reagent water. Store in a vertical position. j. Capping Capping the buret with an inverted test tube will aid in preventing evaporation of the solution and contamination by dust. If the solution is not alkaline and does not contain fluorides or phosphates in acid solution, it is generally safe to allow the solution to stand in the buret. A full buret will stay clean longer than a dry or partially filled buret. k. Greasing Stopcock (glass stopcocks) If the stopcock sticks or leaks, remove the old lubricant by wiping with a cloth, using methanol or acetone if desired. Replace with fresh “Lubriseal”. Apply only a thin film since too much lubricant may plug the hole. Unless the parts of the stopcock are dry before lubricating and sealing the plug, the seal may be defective. Teflon stopcocks are not to be greased. l. Offset Tip A buret with an offset tip is useful when titrating with a potentiometer or when the apparatus is crowded into a small space. m. Plugged Tip Occasionally a buret tip becomes plugged with a small amount of lubricant. The plug can be expelled in the following manner: Open the stopcock so that the pressure of the liquid column is on the plugged tip. Insert the tip in a beaker of warm water. If this treatment does not dissolve the plug, it will be necessary to disassemble the stopcock and thoroughly clean the buret with cleaning solution, after which the stopcock must be relubricated. In certain instances the use of a thin wire probe (pipet probe), or buret wire, is a satisfactory means of unplugging buret tips. 6 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03
6. Microburets Microburets equipped with 1.00-, 5.00-, or l0.00-mL syringes are used in some methods where microtitrations are performed. Follow the manufacturer's instructions for care and use of the microburet and any additional instructions that may be included in the method. 7. Volumetric Flasks Volumetric flasks are generally graduated “to contain” (TC) known volumes of solutions and should never be used “to deliver” (TD) known volumes unless they have been so calibrated. Volumetric flasks are used to make up solutions to a given volume. Use Class A flasks. See Table 1 for tolerances. Analysts should understand and practice the following instructions for the use of volumetric flasks. a. Safety Volumetric flasks are fragile, and when shaken, should be held at both the neck and bottom. A flask should never be shaken when held at the neck only. When inserting a stopper, hold at the neck rather than at the bottom. b. Cleanliness Use a clean flask. It usually does not have to be dry, but it must be clean. Rinse the entire interior of the flask two or three times with distilled water prior to use. c. Diluting to Volume Add the solution to be diluted to the flask, and add distilled water or specified diluent to bring to volume. While raising the meniscus to the graduation mark, hold the mark at eye level and add the last few drops from a wash bottle or from a small pipet. Stopper and invert 6 to 12 times to assure homogeneity. Care should be taken when making the initial inversion. Some solutions have a tendency to effervesce, and loss of the solution may result if the stopper is not held firmly in place. If such is the characteristic of the solution being mixed, a momentary removal of the stopper (flask in an upright position) prior to the second inversion will release the gas pressure formed and avoid possible loss. d. Cleaning and Storing Clean the flask with Alconox or a similar cleaning solution. It is not necessary to fill the volumetric flask with cleaning solution. If a generous portion is placed in the flask and the flask is stoppered, cleaning will be accomplished if the flask is shaken and inverted several times so as to keep the walls moistened with cleaning solution. After a thorough rinse inside and out with tap water, rinse 3 times with small quantities of reagent water. Store in an inverted position with the bottom slightly inclined. If the bottom is horizontal, the flask may not drain completely. Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 7
- 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 and 266: The Selection, Care, and Use of Vol
- Page 267 and 268: In observing the lowest point on th
- Page 269: 4. Graduated Cylinders and Tip-up P
- 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
6. Microburets<br />
Microburets equipped with 1.00-, 5.00-, or l0.00-mL<br />
syringes are used in some methods where<br />
microtitrations are performed. Follow the<br />
manufacturer's instructions for care and use of the<br />
microburet and any additional instructions that may be<br />
included in the method.<br />
7. Volumetric Flasks<br />
Volumetric flasks are generally graduated “to contain”<br />
(TC) known volumes of solutions and should never be<br />
used “to deliver” (TD) known volumes unless they<br />
have been so calibrated. Volumetric flasks are used to<br />
make up solutions to a given volume. Use Class A<br />
flasks. See Table 1 for tolerances.<br />
Analysts should understand and practice the following<br />
instructions for the use of volumetric flasks.<br />
a. Safety<br />
Volumetric flasks are fragile, and when shaken,<br />
should be held at both the neck and bottom. A<br />
flask should never be shaken when held at the<br />
neck only. When inserting a stopper, hold at the<br />
neck rather than at the bottom.<br />
b. Cleanliness<br />
Use a clean flask. It usually does not have to be<br />
dry, but it must be clean. Rinse the entire interior<br />
of the flask two or three times with distilled<br />
water prior to use.<br />
c. Diluting to Volume<br />
Add the solution to be diluted to the flask, and<br />
add distilled water or specified diluent to bring<br />
to volume. While raising the meniscus to the<br />
graduation mark, hold the mark at eye level and<br />
add the last few drops from a wash bottle or from<br />
a small pipet. Stopper and invert 6 to 12 times to<br />
assure homogeneity. Care should be taken when<br />
making the initial inversion. Some solutions<br />
have a tendency to effervesce, and loss of the<br />
solution may result if the stopper is not held<br />
firmly in place. If such is the characteristic of the<br />
solution being mixed, a momentary removal of<br />
the stopper (flask in an upright position) prior to<br />
the second inversion will release the gas<br />
pressure formed and avoid possible loss.<br />
d. Cleaning and Storing<br />
Clean the flask with Alconox or a similar<br />
cleaning solution. It is not necessary to fill the<br />
volumetric flask with cleaning solution. If a<br />
generous portion is placed in the flask and the<br />
flask is stoppered, cleaning will be<br />
accomplished if the flask is shaken and inverted<br />
several times so as to keep the walls moistened<br />
with cleaning solution. After a thorough rinse<br />
inside and out with tap water, rinse 3 times with<br />
small quantities of reagent water. Store in an<br />
inverted position with the bottom slightly<br />
inclined. If the bottom is horizontal, the flask<br />
may not drain completely.<br />
<strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 7