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A course in petroleum laboratory techniques.
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A course in petroleum laboratory techniques.
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A COURSE IN PETROLEUM LABORATORY TECHNIQUES A Project Presented to the Faculty of the School of Education The University of Southern California In Partial Fulfillment of the Requirements for the Degree Master of Science in Education by Robert Ulrich Fisher June 1950 UMI Number: EP46306 All rights reserved INFORMATION TO ALL USERS The quality of this reproduction is dependent upon the quality of the copy submitted. In the unlikely event that the author did not send a complete manuscript and there are missing pages, these will be noted. Also, if material had to be removed, a note will indicate the deletion. Dissertation Publishing UMI EP46306 Published by ProQuest LLC (2014). Copyright in the Dissertation held by the Author. Microform Edition © ProQuest LLC. All rights reserved. This work is protected against unauthorized copying under Title 17, United States Code ProQuest LLC. 789 East Eisenhower Parkway P.O. Box 1346 Ann Arbor, Ml 48106- 1346 £ 1 ' ' s ' / P 3 5 " P^°<V jT /u j project report, w ritten under the direction of the candidate’s adviser and approved by him , has been presented to and accepted by the F aculty of the School of Education in p a rtial fu lfillm en t of the requirements fo r the degree of M a s te r of Science in Education. ....... Adviser D ean ii TABLE OF CONTENTS CHAPTER PAGE PART I. LIGHT OILS HOW TO INSURE QUALITY IN LIGHT PETROLEUM DISTILLATES 1. PRELIMINARIES; HOW TO PERFORM THE INITIAL TESTS. . 2 . I. GRAVITY: How to determine the density of a petroleum product . . . . . . . . . . . . . . 2 2. COLOR: How to test with the Sayholt Chromometer . . . . . . . . . . . . . . . . . . 4 3. DOCTOR: How to test for mercaptans ...... 6 4. CORROSION: How to detect free and corrosive sulfur compounds. .......... 7 5. FLASH POINT: How to check the ignition temperature ............ ...... ........ 6 6. SOURCES FOR THIS CHAPTER: Where to get further assistance. 11 S. BOILING RANGE: HOW TO DISTILL LIGHT OILS ..... 13 1. EQUIPMENT: How to assemble the necessary apparatus •••••••••••.••••... 13 2. ACCESSORIES: How to minimize equipment errors. ••••••••••••••• ........ 14 3. SAMPLE: How to prepare the product for distillation. .... ............ •••••• 15 4. DISTILLATION: How to conduct the test.......... 17 ill CHAPTER PAGE 5. CALCULATION: How to obtain ’ ’evaporated” points. 19 6. PLOTTING: How to check your distillation ... 20 7. SOURCES FOR THIS CHAPTER: Where to get fur ther assistance 21 5. VOLATILITY: HOW TO OBTAIN THE REID VAPOR PRESSURE. 2g 1. APPARATUS: How to assemble the proper equip ment. 23 2. SAMPLE: How to prepare the gasoline for the test. • 24 3. TRANSFER: How to get the sample into the gasoline chamber. . . . . . . . . . . . . . . . 26 4. VAPOR PRESSURE: How to complete the test ... 26 5. SOURCES FOR THIS CHAPTER: Where to get fur ther assistance ........... ........ 28 4. GUM: HOW TO DETECT OXIDATION PRODUCTS.............. 31 1. OXIDATION STABILITY: How to determine the gum- forming tendencies of a gasoline in storage . . 31 2. ASTM GUM: How to determine the present gum content of a gasoline . . .. .. .. ... .. 34 3. AVIATION GUM: How to determine potential gum in an aviation gasoline 35 4. COPPER DISH GUM: How to determine accelerated gum in a gasoline 36 iv CHAPTER PAGE 5. SOURCES FOR THIS CHAPTER: Where to get fur ther assistance. . . . . . . . . . . . . . . . 38 PART II. HEAVY OILS HOW TO INSURE QUALITY IN HEAVY PETROLEUM OILS 5. PRELIMINARIES: HOW TO PERFORM ROUTINE TESTS ... 41 1. GRAVITY: How to determine the density of heavy oils • 41 2. BS&M: How to estimate water and sediment hy centrifuge .. .. ......... 42 3. WATER BY DISTILLATION: How to find the amount of water in heavy oils 43 4. PRECIPITATION NUMBER: How to discover the amount of sediment in lubricating oils .... 45 5. CLOSED CUP FLASH: How to check the flash point of oils. ........... 46 6. OPEN CUP FLASH AND FIRE: How to secure the Cleveland flash and fire points. ....... 48 7. POUR POINT: How to find the temperature at which an oil solidifies. ........... 50 8. COLOR: How to check the transparency of a dark oil 52 9. VISCOSITY: How to determine the Saybolt viscosity. •••••••• .......... .... 53 10. SOURCES FOR THIS CHAPTER: Where to get fur ther assistance. 58 CHAPTER PAGE 6. BOILING RANGE; HOW TO DISTILL HEAVY OILS.......61 1. GAS OIL: How to distill gas oil ....... 61 2. SPRAY OIL: How to distill spray oil . . . . . 66 3. CRUDE OIL: How to distill crude oil.......68 4. SOURCES FOR THIS CHAPTER: Where to get fur ther assistance.............* 71 7. CONCLUSION: HOW TO PERFORM SUPPLEMENTARY TESTS. . 73 1. CARBON RESIDUE: How to determine the carbon forming propensity of an oil • •••.•••. 73 2* ASH: How to find the ash content of oils. . . 76 3. SEDIMENT: How to determine the sediment by extraction ........... ........ . . 77 4. SOURCES FOR THIS CHAPTER: Where to get fur ther assistance. 79 BIBLIOGRAPHY: Special references of use to petroleum testers . . . . . . . . . . . . . . . . 81 vi PREFACE The trend in junior college education has long been toward more and more courses of a terminal nature. By this is meant not only finishing courses in the academic subjects, but also courses which prepare the student for one particular job in commerce or industry. It is primarily for this latter type of course that this syllabus is writ ten. 'Actually, however, the tests outlined here are quite similar to many of the experiments used in regular chemistry courses. The one basic difference is that in this syllabus the work all points toward a specific goal: helping the student to get a good job upon graduation. Thus, the sepa rate T T experiments” are not arranged so as to illustrate general physical or chemical principles, but in a functional order as the future Petroleum Inspector will perform them in his work. This course is the result of several years experience in petroleum laboratory work: of learning "the hard way", and of watching others not learn at all. Slips were col lected from fellow employees and from beginning testers. Complains of employers and foremen were listed and were sup plemented from personal experience. All of this pointed to ward the need for a manual to tell the inspector in simple vii language just how to do his job. No attempt is made to supplant the Standards of the American Society for Testing Materials. These test de scriptions are intended to be definitive guides for the use of executives, purchasing agents, engineers, and contract-makers. As such, they are necessarily nearly unreadable for the beginning tester. Unfortunately, they are often the only written guide available to him; the companyfs laboratory manual being merely a carbon copy of these directions. It is hoped that this syllabus will be a real step to ward fulfilling the needs of its future students. 1 PART I. • LIGHT OILS HOW TO INSURE QUALITY IN LIGHT PETROLEUM DISTILLATES This first part of the course is designed to acquaint you with the different methods and techniques used with gasolines, kerosines, and other light oils* You have all used gasoline in your cars, and most of you have seen kero- sine lamps. So the materials are familiar to you. You will find the work easy and different from any laboratory you have had. For here, the results you obtain will mean some thing to you, not just to the course. Good luck to youl 2 CHAPTER X. PRELIMINARIES *-HOW TO PERFORM THE INITIAL TESTS A. MOTIVATION: Rewards of performing preliminary tests on light oils. 1. ECONOMY OF TIME: Whenever, you find an oil that will not meet the initial requirements, you need perform no more tests on it. 2. FAVORABLE NOTICE: When you are the one who habi tually starts work on a sample first, you will attract approving comment. 3. VARIETY: Since the preliminary tests vary for dif ferent products, your tasks will not be monotonous repititions. B. DIRECTIONS: Some suggestions on how to get started testing light oils. 1. GRAVITY: How to determine the density of a petro leum product. a. Procure the following equipment.. (1) A transparent measuring cylinder of either 100 ml. or 250 ml. capacity. (2) Suitably sized hydrometers graduated in degrees API. (3) Ah ASTM Gravity Thermometer graduated from -5° to 215° F. Maintain the proper temperature for the sample and equipment. (1) If the sample has an estimated API gravity of less than 70°, cool it to 65° F. or less before starting the test. (2) If the sample has an estimated API gravity of more than 70°, cool it to 35° F. or less before starting the test. (Run the test in ice-water bath to keep the temperature low.) (3) A kerosine sample need not be cooled below room temperature regardless of its esti mated gravity. (4) If the sample Is a mixture of a petroleum product and some other liquid, take the gravity at 60° F. (5) Cool the cylinder, thermometer, and hydro meters to approximately the same temperature as the sample. Proceed with the test as follows: (1) Pour the sample slowly into the cylinder to avoid evaporation loss and formation of bubbles. (Remove any bubbles that do form by blowing gently over the oil surface.) (2) Carefully insert a hydrometer into the sample• (a) If the hydrometer floats too high in the liquid to be read, replace it with a hydrometer having a lower API range. (b) If the hydrometer sinks to the bottom of the cylinder, replace it with an other hydrometer having a higher API range. (3) Spin the hydrometer so that it will not stick to the edge of the cylinder. (4) Read the hydrometer while it is spinning. (a) If the sample is transparent, look through it to see where the surface cuts the hydrometer scale. (b) If the sample is not transparent, look at the scale from above and see where the surface apparently cuts it. Sub tract 0.1° API from this for the final reading. (5) Take the temperature of the sample. (6) Correct the observed gravity to the gravity at 60° F. (Use Table 1 in National Stand ard Petroleum Oil Tables.) COLOR; How to test with the Saybolt Chromometer, a. Provide all necessary equipment. (1) The Chromometer. (2) Flannel and filter paper, (3) Hie sample* Filter the sample to remove any water or sus pended material. Rinse the right-hand tube of the Chromometer with some of the oil to be tested, and allow it to drain. Close the pet-cock at the bottom of the tube and fill it to a depth of 12 inches. Determine the number of discs to be used. (1) Compare the color of oil at this depth to that of one-half disc in the left-hand tube, (a) If the oil color is lighter, use one- half disc for the remainder of the test. (b) If the oil color is darker, lower the oil level to 10.5 inches. (2) Compare the color of the oil at a depth of 10.5 inches to that of two discs in the left-hand tube. (a) If the oil color is lighter, use one disc for the remainder of the test. (b) If the oil_ color is darker, use two discs. Determine the color of the oil. (1) Put the proper number of discs in place. (2) Add more oil if necessary until the oil-color is darker than the disc color. (3) Lower the oil level to the various levels given in the table accompanying the instru ment and compare the colors. J (4) Report as the color of the oil the number corresponding to the depth of oil at which the two colors match. DOCTOR: How to test for mercaptans. a. Procure all equipment and materials. (1) A 4-ounce cylindrical bottle and cork to fit. (2) A supply of pure, dry flowers of sulfur. (3) The ’ ’ doctor” solution made up as follows: (a) -Dissolve 125 grams of sodium hydroxide in one liter of distilled water. (b) Add 60 grams of litharge (PbOg) and let stand with occasional shakings for at least a day. (c) Siphon off the clear liquid for use in the test. (4) Proceed with the test. (1) Add to the 4-ounce bottle 10 ml. of the sample and 5 ml. of the doctor solution. (2) Shake these together vigorously for about 15 seconds. (3) Add a very small pinch of the sulfur and shake again for 15 seconds. (4) Observe the sulfur while the solution settle out. (a) If either the sulfur or the sample is discolored, report the sample as "sour" (mercaptans present.) (b) If the sample Is unchanged in color and if the sulfur remains bright yellow report the sample as "sweet" (no mer captans present.) CORROSION: How to detect free and corrosive sulfur compounds. a. Procure the following equipment. (1) A 6-inch glass test tube. (2) Two freshly polished copper strips 1/2-inch wide by 3 inches long. (a) Polish one immediately before starting the test. (b) Polish the other Just before the test period is up. (3) A bath maintained at 122° F. (4) The sample of oil* h* Proceed with the test. (1) Place the polished copper strip in the test tube and add enough sample to cover it. (2) Place the test tube, loosely corked, in the bath and let it stand for three hours. (3) At the end of this time, remove the strip and compare it with the one just polished. (a) Report the test as "negative" if only extremely slight discoloration to the test strip is sho?m. (b) Report the test as "positive" if more than extremely slight discoloration is shown. FLASH POINT: How to check the ignition temperature. a. Set up the Tag tester in a suitable manner. (1) The test must be performed in a darkened room. (2) The tester must be level and steady. (3) The tester must be shielded on three sides to protect it from drafts. b. Equip the tester properly. (1) Provide two ASTM Flash Point Thermometers (range 20° to 230° F.) (2) Fill the water bath until it overflows. (3) Procure a microburner to heat the water. Prepare the sample for the test. (1) Float the oil cup on the water bath. (2) Add 50 ml. of cool sample to the oil cup. The oil cup will settle into position. (3) Destroy any air bubbles on the surface of the sample. (Use a piece of blotting paper for this.) (4) Place the cover of the tester in position. (5) Light the test flame and adjust it to the size of the white bead on the cover. Determine the flash point of the oil. (1) Record the initial temperature of the oil. (2) Place the lighted microburner in a central position in the base of the tester. (3) Adjust the flame so that the oil temperature o rises at the rate of 1.8 F. per minute as nearly as possible. (No faster than 2.0° F.; no slower than 1.6° F.) (4) When the oil temperature is 9° F. below its probable flash point, begin applying the test flame. (a) Turn the knob on the cover so as to introduce the test flame into the cup. (b) Immediately turn it back again. The full time consumed should be about one second. (c) Record the time and temperature at which the first test was made. (5) Repeat this application after each 1° tem perature rise of the sample. (6) Record the time and temperature of the oil when the flash point is reached. (a) There must be a distinct flash in the interior of the cup. (b) Disregard any bluish halo which may form around the test flame. (7) Divide the temperature rise of the oil, from the temperature at which the test flame was first introduced to the flash point temperature, by the time consumed in the process. (8) If this rate thus determined does not fall within the specifications, the test must be repeated, using a fresh sample. (a) The temperature of the water bath must be lowered by the addition of cool water until it is 15° F. below the previously determined flash point• (b) The microburner flame must he adjusted so that the heating rate will fall with in the proper limits* (c) In all other particulars, the flash point should he determined In the man ner described above. (9) Report at the flash point the temperature at which the oil first flashes during a test which is properly run. e. Turn off the microburner and allow the sample and apparatus to cool in position, f. Discard the cool sample and clean the apparatus in preparation for the next test. 6. SOURCES FOR THIS CHAPTER: Where to get further as sistance. a. ASTM Standards: D 287-29; D 156-38; D 484-40; D 130-30; D 56-36. b. Laboratory manuals and specifications of the various oil companies* C. ACTIVITY ASSIGNMENTS: Laboratory work to help you get started in petroleum testing-. 1* GASOLINE: Run the appropriate preliminary tests on several gasolines. 2. KEROSINE; Run the appropriate preliminary tests on several samples of kerosine. S. SPECIFICATIONS: Compare test results of gasolines and kerosines to State specifications* Determine which oils are safe for use. D. EVALUATION: A true-false test to determine your mastery of preliminary tests. (Place an X in the proper space for true or false.) T F 1. ( )( ) You should run gravities on all petroleum products at 60° F. ( )( ) To minimize temperature changes, you should pre-cool all apparatus to the same tem perature as the gasoline. 3. ( )( ) You should never use more than one color disc in determining the color of a kerosine. 4. ( ) ( ) If you run a doctor test, you need not run a corrosion test on the same sample. 5. ( )( ) You should not run a Tag flash test on gasoline. 13 CHAPTER 2. BOILING RANGE HOW TO DISTILL LIGHT OILS A. MOTIVATION; Benefits resulting from mastery of distil lation techniques. 1, LIFE OF EASE: While running distillations, you will be able to sit down on a comfortable chair, 2, COMPANIONSHIP: More than one person usually uses the same machine; you can en^oy yourselves while working• 3, NO EXTRA WORK: While running distillations, you cannot be assigned any ”odd jobs” for your nspare time.” B. DIRECTIONS: Some instructions on how to distill gaso lines. naphthas, and kerosines. 1. EQUIPMENT: How to assemble the necessary apparatus. a. Use the condenser bath provided (”Engler mach ine”) . b. Choose a 100 ml. distilling flask with a tight- fitting cork stopper on the distilling tube. (1) Select a flask that has been used before. (2) If a new flask must be used, put 3 or 4 small glass beads into the flask. c. Choose an ASTM Low-Distillation Thermometer having a top temperature reading of 580° F., and provided with a tight-fitting cork, d. Choose the proper electric heater, (1) For gasolines and naphthas, use a heater having a hole l£ inches in diameter for the flask to rest. (2) For kerosines, use a heater having a hole if inches in diameter. e. Provide a 100 ml. graduated cylinder having each 10 ml. mark numbered. f. Procure an analysis card, or provide some means of recording data. ACCESSORIES: How to minimize equipment errors. a. Check the room temperature and record it. b. Check the condenser bath temperature to see that it is between 32° and 40° F. c. Using a soft, lint-free cloth attached to a stiff cord, swab the condenser tube to remove any liq uid. d. Prepare a receiver-bath by filling an appropriate glass 3ar with water at 55° to 65° F. e. Recheck flask to make sure It has no cracks. Do this by: (1) Inspecting the flask bottom. (2) Tapping the flask gently on a hard surface to see that it will not crack easily. SAMPLE: How to prepare the product for distil lation. a. Measure 100 ml. of the sample into the grad uated cylinder. (1) Fill the cylinder to a point above the 100 ml. graduation. (2) Take the API gravity. (See Chapter 1.) (3) Check to make sure the sample temperature is between 55° and 65° F. (4) Pour off the excess sample so that exactly 100 ml. remains in the cylinder. b. Transfer the sample to the flask. (1) Pour it carefully so that no sample is spilled. (2) Make sure no sample gets into the vapor tube. c. Insert the thermometer into the flask. (1) The thermometer must be near the middle of the flask neck; under no circumstances touching a flask wall. (2) The lower end of the capillary tube must be just below the vapor tube junction in the flask. (3) The thermometer should be at or near room temperature when inserted. 16 d. Set the flask in position. (1) Place the flask in the heater opening so that it fits snugly with no space between the flask and the support at any point. (2) Adjust the position of the heater so that the vapor delivery tube of the flask ex tends about 1-| inches into the condenser, and runs concentric with it. (3) Fit the cork on the vapor tube snugly into the condenser so that the whole flask is held tightly in position. (4) If the Engier machine is the type having a mirror in back of the flask, set it in position now. e. Set the receiver in position. (1) Use the same cylinder as a receiver as was used to measure the sample. Do hot dry or drain it. (2) Insert the cylinder in the receiver bath. (3) Place cylinder and bath under the lower end of the condenser so that the conden ser tube extends into the cylinder at least an inch. (4) Cover the cylinder top with a piece of blotting paper or thick felt cub* to fit 17 around the condenser tube. DISTILLATION: How to conduct the test. a. Apply heat to the flask. (1) Turn on the switch. (2) Adjust the heating rate such that the first drop will fall from the condenser in not less than 5 nor more than 10 min utes. (Only experience can teach you this step.) b. Read the temperature when the first drop falls, and record this temperature as the initial boiling point (IBP). c. Proceed with the distillation at a rate between 4 and 5 ml. per minute. (1) This may be timed with a stop-watch. (2) After some experience, it may be timed by checking the time between drops. (3) Increase or decrease the heat as necessary to maintain this rate, but: (4) Make no further heating adjustment when the volume remaining in the flask reaches approximately 5 ml. d. Record temperatures corresponding to designated volumes in the receiver. 18. (1) Record the temperature when 5 ml. of liq uid has been distilled into the receiver (5$ point). (2) Record the 10$ point, and each succeeding 10$ point (20$, 30$, etc.). (3) Record*the 95$ point if there is one, otherwise indicate that there is none. (4) Record any other points specifically asked for. (5) Proceed as follows in reading temperatures. (a) As the liquid level in the receiver approaches the designated point, move the receiver so that the drops flow down the side of the cylinder. (b) Read the temperature when the bottom of the meniscus of the liquid level Just reaches the line marking the volume in question. (6) These points may be referred to as "dis tilled" points. e. Record as the end point the maximum temperature reached on the distillation thermometer. (1) This temperature is usually reached after the liquid in the flask has all disappeared. (2) Make.several consecutive temperature read- ings on a separate sheet, and pick the maximum from these readings. (5) Do not discontinue these readings until the thermometer has reached an apparent maximum and then dropped at least ten degrees Fahrenheit. How to record the distillation loss. a. Measure to the nearest 0.1 ml. the volume of liquid collected in the receiver. b. Record this volume as the recovery. c. Pour the cooled residue in the distillation flask, into a small graduated cylinder. d. Record this volume as the residue. e. Add the recovery and residue and subtract this siam from 100. ml. g. Record this volume as the loss. CALCULATION: How to obtain "evaporated" points. a. Note the difference between "distilled" points and "evaporated" points, (1) Distilled points are temperatures corres ponding to certain volumes collected in the receiver. These are the points directly recorded during the distillation. (2) Evaporated points are temperatures corres ponding to certain volumes evaporated from the flask (including the loss). These points must be calculated from the distilled points. b. To find (for example) the 50$ evap. point: (1) Subtract the 40$ dist. point from the 50$ dist. point* This gives the temperature change per 10 ml. near the 50$ point. (2) Divide this difference by 10. This gives the temperature change per ml. near the 50$ point. (3) Multiply this value by the loss. This gives the difference in temperature be tween the dist. and evap. points. (4) Subtract this product from the 50$ dis tilled temperature. This is the 50$ evap. point. d. Proceed in the same manner for any other point except the 10$. In this case: (1) Subtract the 5$ point from the 10$. (2) Divide this difference by 5. (3) Proceed from this point as above. PLOTTING: How to check your distillation. a. Make a graph of your data, plotting temperatures against percent distilled. b. Draw a smooth curve through the points, dis- regarding any values obviously out of line. c. Adjust these points so that they fall on the curve. d. Head from the graph any points missed during the distillation. e. If more than one or two points were missed or are out of line, repeat the distillation. 8. SOURCES FOR THIS CHAPTER: Vfhere to get further assistance. a. ASTM Standards: D 287-39; D 86-46. b. Laboratory manuals and specification lists of the various petroleum refining companies. C. ACTIVITY ASSIGNMENTS: Laboratory work to help you master distillation techniques. 1. GASOLINE: Run preliminary tests on several gasolines and then distill them. Distill more than one gaso line at once. 2. KEROSENE: Run preliminary tests on several kero- sines and then distill them. Distill more than one at a time. 3. PLOTTING: Graph some distillations and compare the types of curves obtained. 22 D. EVALUATION: A best answer test to determine vour know ledge of distillation practices. (Place the number of the best answer in the parentheses.) 1. ( ) To run a distillation, you should select: (1) A new flask. (2) A flask that has been used two or three times. (3) A flask with a well-blackened bottom. 8. ( ) You should place the distillation thermometer: (1) In the boiling liquid. (2) Just above the liquid. (3) Just below the side-arm Junction. (4) With the bulb Just below the base of the cork. 3. ( ) The sample when measured should be: (1) As cold as a salt-ice bath will get it to minimize evaporation loss. (2) 32-40° F. (3) 32-40° C. (4) 55-65° F. 4. ( ) You should maintain the distillation rate such that: (1) the liquid emerges from the conden ser in a continuous but very fine stream. (2) The receiver fills at 4 to 5 ml. per min ute. (3) The drops fall separately from the condenser, but are almost continuous. (4) There is an interval of one second between each drop. 23 CHAPTER 3. VOLATILITY HOW TO OBTAIN THE REID VAPOR PRESSURE A. MOTIVATION; Advantages of learning to perform vapor pressure tests. 1* FIELD TRIPS: The sampling for a vapor pressure test is so important, you will often be asked to witness the sampling before you run the test. 2. MANLY PHYSIQUE: The shaking necessary to the test will develop your arm and shoulder muscles so that you will have that virile look. B. DIRECTIONS: Pointers on determining the Reid vapor pressure of gasolines. 1. APPARATUS: How to assemble the proper equipment, a. Check to make sure that all the following equipment is available and in working order. (1) A Reid vapor pressure bomb including: (a) An air chamber. (b) A gasoline chamber. (2) An accurate pressure gage with a range of 0 to 15 pounds per square inch. (3) A cooling bath to chill sample containers and gasoline chambers. (32° to 40° F.) (4) A vapor pressure bath capable of being maintained at 100° F. plus or minus 0.2°. (5) An air chamber thermometer with a range of 0 to 180° F. (6) A sample transfer connection. b. If the vapor pressure bomb has been used before, make certain all residual gasoline is removed. (1) Direct a small jet of air into the pressure gage for at least five minutes. (2) Rinse the air and gasoline chambers with warm water and allow them to drain. Re peat this at least five times. c. Prepare the apparatus for final assembly. (1) Immerse the corked gasoline chamber in the cooling bath for several minutes. (2) Connect the pressure gage to the air cham ber. (S) Insert a thermometer into the open end of the air chamber. (a) Use a loosely fitting or vented cork to hold it in position. (b) Have the thermometer project for at least 3/4 of its length Into the air chamber. (c) Do not allow the thermometer to touch the walls of the air chamber. SAMPLE: How to prepare the gasoline for the test. As soon as the sample is received, place it in the cooling bath. Do not open the sample until it is thoroughly chilled. Discard any sample whose container shows any evidence of leakage. When the sample has reached the bath temperature, open it and inspect it for liquid level. (1) If less than 70$ of the space is occupied by liquid, discard the sample, (2) If more than 80$ of the space is liquid, pour off some of the sample until the liq uid remaining fills between 70$ and 80$ of the container space. Saturate the sample with air. (1) Shake the closed sample vigorously. (2) Turn the sample upside down and open the container slightly until the inward rush of air subsides. (3) Again shake the sample and vent it as be fore. (4) Continue this process until no more air bubbles enter the container. (5) Replace the sample in the bath, and after a few minutes try again to saturate it. (6) Continue alternately chilling, shaking, and venting until no more air at all will enter the container. TRANSFER: How to get the sample into the gasoline chamber. a. Remove the chilled, air-saturated sample from the bath. b• Open the container -and immediately insert the chilled transfer connection. c. Remove the chilled gasoline chamber from the bath, uncork it, and place over the sample deli very tube of the transfer connection. d. Rapidly invert the system so that the gasoline chamber is in an upright position, and the gasoline flows into it. e. Fill the chamber to overflowing and set aside the sample container and transfer apparatus. VAPOR PRESSURE: How to complete the test, a.. Assemble the air chamber, gasoline chamber and gage into a complete, air-tight unit. (1) Read the temperature shown on the air chamber thermometer, and record this as the initial air temperature. (2) Remove the thermometer and set it aside. (3) Couple the air chamber to the gasoline chamber• (4) Tighten both connections so that the three points are sealed together. (5) Test the seal by immersing the bomb in the 100° bath. (a) The warm water will vaporize some of the gasoline and raise.the pressure within the bomb. (b) If there are any leaks, bubbles will form at the flaw and rise to the bath surface. (6) If there are any leaks, discontinue the test and repeat using another bomb. (7) Complete the gasoline transfer and bomb assembly in as short a time as possible to minimize vapor losses. Assist the system to come to equilibrium. (1) Remove the bomb from the bath, invert it, and shake it vigorously. (2) Right the bomb and replace it in the bath so. that the water level is at least one inch above the top of the air chamber. (5) After five minutes, read the gage and re cord the reading. (4) Remove the bomb, invert, and again shake vigorously. 38 (5) Replace the bomb as before, (6) After two minutes, read and record the pressure. (7) Repeat steps (4) through (6) for a total time of at least 30 minutes until the read ings are constant. (8) Frequently check on the bath temperature to make sure it is maintained at 100° F. (9) if at any time throughout this process a leak develops in the bomb, discontinue the test and repeat it, using another bomb, c. Record the final reading after the system is in equilibrium as the uncorrected vapor pressure. d. Calculate the Reid vapor pressure. (1) If the gage used has a correction, apply this to the uncorrected vapor pressure. (2) Correct this value for the difference be tween the initial air temperature and 100°F. (3) Record this corrected value as the Reid vapor pressure. e. Tear down the apparatus and clean it out for future use. (See section 1-b of this chapter.) 5. SOURCES FOR THIS CHAPTER: Where to get further as sistance. a. ASTM Standard D 323-43. 29 b. Laboratory manuals and lists of specifications of the various oil companies. C. ACTIVITY ASSIGNMENTS: Laboratory work to help you learn vapor pressure techniques. 1. TESTING; Take the vapor pressures of several dif ferent gasolines. 2. SAMPLING; Observe the correct sampling techniques as practiced by a guager~or other experienced worker. S. .CALIBRATION; Check your pressure gages against a mercury column or deadweight tester. Record the gage errors. D. EVALUATION; A rating scale to test your mastery of vapor pressure techniques. (Place an X in the space for which you qualify.) 1. ( ) You assembled all equipment properly. 2. ( ) You checked to see all equipment was clean, 3. ( ) You checked the sample container for any leaks. 4. ( ) You checked the sample for correct liquid-level. 5. ( ) You made sure the sample was thoroughly sat urated with air. 6. ( ) You transferred the sample properly from con tainer to vapor pressure bomb. 7. ( ) You examined the assembled apparatus for leaks. 8. ( ) You shook the sample at 2-minute intervals 9 f 5? • \ 10. ( 11. ( ( 50 while it was coming to equilibrium. ) You applied all necessary gage corrections. ) You recorded the correct value for the vapor pressure. ) You tore down your apparatus and rinsed it out . ) _Total. 31 CHAPTER 4. GUM HOW TO DETECT OXIDATION PRODUCTS A. MOTIVATION: Benefits that may result from learning gum tests. 1. FREE TIME: Since these tests take a long time to ran, you will frequently have extra time to your self to relax. 2. SOCIAL STATUS: Only the best testers enjoy the privilege of working with aviation gasolines. 3. NEW FACES: These tests are usually performed in a separate part of the laboratory, thus you will be able to talk to different people while running these tests. B. DIRECTIONS: Hints on how to perform tests for gum or light oils. 1. OXIDATION STABILITY: How to determine the gum-forming tendency of a gasoline in storage, a. Secure the following apparatus and materials. (1) An oxidation stability bomb including cover and gasket. (2) A source of oxygen having a pressure of at least 100 psi. (3) A recording pressure gage. (4) A water bath maintained at 212° F. (5) A glass sample container and cover. (6) A 50 ml. graduated cylinder, (7) The sample of gasoline to be tested. Prepare the apparatus for use. (1) Clean the glass sample container and cover• (a) Wash container with acetone until free from gum. (b) Immerse container and cover in chromic acid cleaning solution for at least IS hours. (c) Remove them, using steel tongs and handle them only with tongs there after. (d) Wash thoroughly, first with tap water, then with distilled water. (e) Dry in an oven at 500° F. for an hour. (2) Clean the bomb and cover. (a) Drain any gasoline from the bomb. (b) Wipe the inside of the bomb and lid with a clean rag moistened with ace tone. (c) Dry the bomb and cover with another clean rag. Start the test. 35 (1) At room temperature, measure out 50 ml. of gasoline. (2) Place the sample container in the bomb, add the gasoline, and cover with the glass cover. (3) Place the bomb cover in position and screw it on tightly. (4) Connect the side-arm to the oxygen supply and the top to the recording pressure gage. (5) Introduce oxygen up to a pressure of 100 psi. (6) Allow the oxygen to leak out slowly by loosening one of the connections. (This flushes the air out of the bomb.) (7) Tighten all connections, and again intro duce oxygen up to 100 psi. (8) Close the valve and observe for leaks. (a) If leaks are present, as shown by a drop in pressure on the gage, re- tighten all connections and repressure, -(b.) If there are no leaks, proceed with the test. (9) Disconnect the oxygen supply, and immerse the bomb in the water bath. (10) Observe the pressure from time to time, and if any leaks occur, discard the test. d. Continue the test until the break point is reached. This point is one which is: (1) Preceded by a pressure drop of exactly 2 psi. in 15 minutes. (2) Succeeded by a drop of at least 2 psi. in 15 minutes. e. Record the number of minutes from the time the bomb is placed in the bath till the break point and report this as the induction period of the gasoline. f. Release pressure from the bomb slowly, let it open, and clean it in preparation for the next test. ASTM GUM: How to determine the present gum con tent of a gasoline. a. Secure the following apparatus: (1) An ASTM Gum Bath including conical adap tors and a. heated air supply capable of delivering one liter per second of air through each outlet of the machine. (2) At least 2 ASTM Gum Beakers. (3) An analytical balance. (4) A 50 ml. graduated cylinder. (5) The sample to be tested. b. Clean the beakers in exactly the same manner as the oxidation stability sample containers were cleaned. (See section 1-b of this chap ter.) c. Bring the gum bath to approximately 320° F. d. Weigh one of the beakers to the nearest 0.1, mg. Use the other beaker as a tare for the weighing. e. Place both beakers in the bath and start the air flowing. f. Measure out 50 ml. of the sample and add this to the weighed beaker. g. Set the conical adapters in position and center them vertically over the beakers. h. Adjust the air flow to one liter per second. i. Allow the beakers to remain in the bath for 15 minutes after the sample has completely evaporated. j. Remove both beakers using tongs and allow them to cool for at least two hours. k. Weigh the sample beaker, using the other as a tare as before. 1. Report the gum obtained as mg. per 100 ml. of sample. AVIATION GUM: How to determine potential gum in an aviation gasoline. a. Run an oxidation stability test (See section 1 of this chapter) on the sample with the fol lowing changes: (1) Use 100 ml. of sample instead of 50. (2) Instead of running the sample to the break point, run it for 16 hours, (or 'whatever time is specified). b. Inspect the sample after the run for any pre cipitate. (1) To open the bomb, first cool to room tem perature . (2) If a precipitate is present, filter it off through a sintered glass crucible. c. Wash the sample container with two 10 ml. por tions of acetone. d. Divide the sample plus washings into two equal parts. e. Run an ATSM gum on each part, using the whole part for the test. f. Report the results as mg. of gum per 100 ml. of sample after 16 hours induction period. COPPER DISH GUM: How to determine the potential gum in a gasoline. a. Provide the necessary equipment. (1) A copper dish of the type furnished. (S) A copper dish gum bath, properly vented. (3) An. electric oven capable of maintaining a constant even temperature of 212° F. \ (4) An analytical balance. (5) A desiccator. Prepare the copper dish properly. (1) Remove any residue from previous tests by washing with acetone. (2) Polish the dish with clean steel wool until there is no discoloration remaining. (3) Heat it in the oven at 212° for 30 minutes. (4) Transfer the dish to the desiccator to cool. Prepare the sample. (1) Weigh the cooled copper dish to the nearest mg. (2) Place the dish in an opening in the cool steam bath. (3) Measure 100 ml. of the gasoline and trans fer it carefully to the copper dish. Conduct the test. (1) Close the bath, and start the draft. (2) Turn on the steam, slowly at first, then enough to keep the temperature at 212° F. as soon as the initial boiling of the gasoline ceases, (3) Maintain this temperature until the gaso line is completely evaporated, (4) Remove the dish, dry the outside with a clean cloth, and place in the oven at 212°. (5) After 30 minutes, remove to the desiecator and allow to cool to room temperature, (6) Weigh the dish to the nearest milligram. (7) Report the increase in weight as the cop per dish gum content of the gasoline in mg, per 100 ml. 5. SOURCES FOR THIS CHAPTER: Where to go for further assistance, a. ASTM Standards: D 526-46; D 381-46; D 876-43T; D 910-48T; D 439-48T. b. Laboratory manuals and specification lists from the oil companies in the area. C. ACTIVITY ASSIGNMENTS: Laboratory work to help you learn gum analysis. 1. GASOLINE: Perform ASTM and copper dish gums on several gasolines, 2. AVIATION GASOLINE: Run aviation gums on several aviation gasolines. 3. OXIDATION STABILITY: Perform oxidation stability tests on both aviation and regular gasolines. 39 D. EVALUATION; A true-false test to check your knowledge of gum analysis. (Place an X in the proper space for true or false.) T F 1. ( )( ) You should use oxygen at one atmosphere pressure to conduct the oxidation stabil ity test. 2. ( )( ) You should use the ASTM gum test to measure the amount of gum actually present in the gasoline. ( )( ) You should use the copper dish gum test to learn the tendency of the gasoline to form gum. 4. ( )( ) You should expect the oxidation stability of a gasoline to be higher if it contains cracked stock. 5. ( )( ) You should expect the ASTM gum to be higher than the copper dish gum for the same gaso line. 40 PART II. HEAVY OILS HOW TO INSURE QUALITY IN HEAVY PETROLEUM OILS In this part, you will learn further tests, some of a routine nature, some more advanced, hut all of them pecu liar to heavy oils. Just as a house is incomplete without its foundations, so you will be "unprepared for your future work if you cannot perform these tests. The heavy oils are less familiar, but of great importance to the industry, and to you, therefore, as a future member of the industry. They are the first oils you will meet when you come to work. Here you can get acquainted, so it won’t be a "blind date". 41 CHAPTER 5. PRELIMINARIES HOW TO PERFORM ROUTINE TESTS A. MOTIVATION: Advantages of learning to perform routine tests* 1* TRAVEL: You will often be sent to other companyfs laboratories to witness gravity and other tests on crude oils* 2. SECLUSION: Many of these tests are performed in separate rooms away from the scrutiny of the "boss”. 3* VARIETY: Your days will never be monotonous when you can switch from one type of preliminary test to another* B. DIRECTIONS: Pointers to help you perform preliminary tests on heavy oils* 1. GRAVITY: How to determine the density of heavy oils. a. Use the same equipment as used in the case of light oilsv (See Chapter 1.) b. In the case of heavy fuel oils, a gravity bath maintained at 120° F* is used in place of a cylinder to hold the sample. c. Take the gravity at or near room temperature. (The exception is the heavy fuel oil,) (See previous section.) d. Proceed In the same manner as with light oils. e. It is particularly necessary to mix the sample thoroughly before pouring it into the cylinder. f. Where the hydrometer cannot be spun, lower it gently into the liquid, making sure it rests near the center of the cylinder. g. Head the hydrometer where the liquid apparently cuts it, then subtract 0.1° to get the true reading. h. Take the temperature of the sample. I. Correct the gravity observed to gravity at 60° F. BS&M: How to estimate water and sediment by centri fuge. a. Provide the following apparatus. (1) A centrifuge capable of whirling tubes at 1500 rpm. and a 16 inch diameter swing. (g) Conical centrifuge tubes graduated to 100 ml. (3) A heating bath maintained at 120° F. b. Shake the sample In the original container to make sure it is completely mixed. c. Measure 50 ml. of benzene into each of two centrifuge tubes. d. Add 50 ml. of the oil to be tested to each, and stopper the tubes tightly. e. Shake the tubes vigorously until the contents are completely mixed. f. Set the tubes in the water bath for 10 minutes. g. At the end of this time, remove them, and shake them vigorously again. h. Place the tubes in the centrifuge and whirl them at the standard speed for 10 minutes. i. Remove the tubes and note the amount of water and sediment separated out. 3. Replace the tubes in the centrifuge and whirl again for 10 minutes, k. Read the water and sediment again, and recentri fuge, repeating this process until the amount is constant for three consecutive readings. 1. Record the sum of the readings in the two tubes as the water and sediment in the oil. WATER BY DISTILLATION: How to find the amount of water in heavy oils. a. Provide the necessary apparatus and solvent. (1) A round-bottom, 500 ml. flask made of Pyrex. (2) A reflux condenser as furnished. (3) A trap graduated to 10 ml. as furnished. (4) A 100 ml. graduated cylinder with glass stopper. 44 (5) Petroleum naphtha conforming to ASTM speci fications. b. Shake the sample vigorously to make sure the portion used for the test is thoroughly represen tative. c. Measure out 100 ml. of the sample, and transfer it to the flask. d. Rinse the graduate with 100 ml. of naphtha, and transfer this to the flask. (1) First use a rinse of 50 ml. then two rinses of 25 ml. each. (2) Let the cylinder drain thoroughly each time it is rinsed. e. Connect the flask, trap, and condenser by means of tight-fitting corks. f. Adjust the apparatus so that the end of the condenser will dip about 1 mm. below the sur face of the liquid in the trap after equili brium has been established. g. Apply heat to the flask so that distillate falls from the bottom of the condenser at 2 to 5 drops per second. h. Continue the distillation until no water is visible in any part of the apparatus (except at the bottom of the trap). i. Record the volume of condensed water as the percent water by distillations. 5* Discontinue heating the flask and tear down the apparatus when it has cooled. PRECIPITATION NUMBER: How to discover the amount of sediment in lubricating oils. a. Use the same apparatus as for the RS&M test, except that the bath temperature is 90° F. (See section 2 of this chapter.) b. Use ASTM precipitation naphtha as the diluent in this test. c. Measure 10 ml. of the oil to be tested into each of two centrifuge tubes. d. Add to each tube 90 ml. of precipitation naphtha and close each tube with a softened cork. e. Invert the tubes at least twenty times, allow ing the liquid to drain completely from the tapered tip each time. f. Place the tubes in the water bath for 5 minutes. g. Vent the tubes momentarily, and then invert them another twenty times, exactly as before, h. Whirl the tubes in the centrifuge for 10 minutes i. Read the sediment, and recentrifuge for 10 min utes periods until three consecutive, identical readings are obtained. 3. Report the volume of sediment as the ASTM Precipitation Number. CLOSED CUP FLASH: How to check the flash point of oils. a. Use the apparatus provided. (1) A Pensky-Martens flash tester complete with stirring device and flash cup. (2) A heater for the tester. (5) Two thermometers. (a) An ASTM P-M and Tag thermometer. (Range 20° to 230° F.) (b) An ASTM P-M High thermometer. (Range 200° to 700° F.) b. Clean all parts of the cup thoroughly before starting the test. c. Fill the cup up to the mark with the oil to be tested. d. Place the lid on the cup, and insert the ther mometer . (1) If you know that the flash will be above 220° F., use the high range thermometer. (2) If you do not know the flash point, start with the low range thermometer, and change if a temperature of 220° is reached before the oil flashes. e. Light the test flame, and adjust it to the size of the bead on the cover. f. Apply heat to the apparatus, and start the stir rer. g. Adjust the heating rate so that the temperature of the oil rises at 10° per minute. h. Starting about 30° below the probable flash point, apply the test flame at 2° intervals. (1) Lower the flame in 0.5 seconds. (2) Leave it in its lowest position for 1 second. (3) Quickly raise it to its highest position. (4) Stop the stirrer while carrying out this process. 1. If the flash point has not been reached by 220°, apply the flame at 5° intervals until the point is reached. j. Report as the flash point the temperature at which the oil first flashes. {1) There must be a distinct flash in the interior of the cup. (2) Disregard any bluish halo which may form around the test flame, k. Immediately turn off the heat, and tear down the apparatus. 1. Pour out the sample into whatever container is provided. (Be carefull The oil is at its flash point.) m. Wash out the cup with diesel oil, and lay it aside to drain. 6. OPEN CUP FLASH AND FIRE: How to secure the Cleve land flash and fire points. a. Use the apparatus provided. (1) A Cleveland flash cup. (S) A heating plate (3) An ASTM Open Flash Thermometer. (Range 20° to 760° F.) b. Set up the apparatus. U) Set the cup on the heating plate. (2) Suspend the thermometer so that it hangs halfway between the center of the cup and the back, and so that it is | inch above the bottom of the cup. (3) Shield the apparatus on three sides to protect it from drafts. (4) Make sure the location is dark enough so that the flash may be readily seen. c. Fill the cup with the sample so that the top of the meniscus comes exactly to the filling line on the cup. d. Light the test flame and adjust it to approxi- mately 5/52 inch diameter. e. Apply heat to the oil, and adjust the rate of heating. (1) Heat the oil at a rate of 50° per minute until it is within 100° of the probable flash point. (2) Above this temperature, heat the oil at 10° per minute, f. Apply the test flame at 5° intervals. (1) Pass the flame in a straight line across the center of the cup and at right angles to the diameter passing through the ther mometer . (2) Keep the flame in the plane of the upper edge of the cup. (5) Pass the flame across the cup in approxi mately one second. g. Report as the flash point the temperature at which a flash appears at any point on the sur face of the oil. (Do not confuse the true flash with a bluish halo which may form around the test flame.) h. After determining the flash point, continue heating the oil at the same rate. i. Continue to apply the flame at 5° intervals until the fire point is reached, j. Report as the fire point the temperature at which the oil burns for a periof of at least 5 seconds. k. Put out the flame, turn off the heater, and ex tinguish the test flame* 1. Pour out the sample into whatever container is provided, using due care to avoid fire, m. Wash out the cup with diesel oil, and lay it aside to drain. POUR POINT: How to find the temperature at which an oil solidifies. a. Procure the necessary apparatus. (1) A pour point test jar. (2) An ASTM Cloud and Pour Test Thermometer. (Range -36° to 120° F.) (3) A cork to fit the test jar and bored to hold the thermometer. (4) Appropriate baths to hold the test jar. (a) A bath at 118° F. (b) A bath at 32° F. (c) A bath at 0° F. (d) A bath at -30° F. b. Pour between 2 and 2f inches of oil into the test jar. c. Close the jar with the cork and with the thermometer inserted. d. Adjust the thermometer so that it is in the center of the oil with the bulb immersed so that the beginning of the capillary is 1/7 inches below the surface of the oil. e. Heat the oil to 115° in the hot bath. f. Remove the test jar from the bath and let the oil cool to 90° in air. g. Place the test jar in the 32° bath. h. If the pour point has not been reached when the oil temperature reaches 50°, place the test jar in the 0° bath. i. If the pour point has not been reached when the oil temperature reaches 20° place the test jar in the -30° bath. j. Inspect the oil at each multiple of 5° while it is cooling in any of the baths. (1) Begin this inspection about 20° above the expected pour point. (2) Remove the jar from the bath, and tilt it just enough to see if there is any movement of the oil. (3) If there is any movement, replace the jar in the bath as quickly as possible. (4) If the oil does not appear to move, hold it in a horizontal position for exactly 5 seconds. (Use a stop watch.) (a) If there is movement of the oil, quickly replace the test jar in the bath. (b) If there is no movement, discontinue the test. k. Report as the pour point the temperature 5° above the temperature at which the oil was solid. 8. COLOR; How to determine the transparency of a dark oil. a. Procure the following apparatus. (1) An ASTM Union Colorimeter, complete with light source., (2) A glass test jar for use with the colori meter. b. Set up the equipment. (1) Pour about 2 inches of oil into the jar. (2) Set the jar in its place in the colori meter and cover it with the shield. (5) Turn on the light source. c. Determine the color of the sample. (1) Mateh the sample with the color standards as nearly as possible. (2) Find the number of the color standard in the mirror of the left side of the colorimet er. (5) If the colors will not match exactly, re port the color in terms of the darker color. Example: If the color lies between 7 and 8, report as ”8 minus”, d. If the sample is darker than 8 color, proceed as follows: (1) Pour 15 ml. of the sample into a centri fuge tube. (2) Add water-white kerosene up to the 100 ml. mark. (5) Mix thoroughly, pour into a clean test jar, and take the color. (4) Report the color as a number followed by' the designated nDil.n VISCOSITY: How to determine the Saybolt viscosity, a. Provide the following apparatus. (1) A Saybolt viscosity machine equipped with the proper outlet tube. (a) A Saybolt Universal tube may be used for oils of any time of flow above 32 seconds. (b) A Saybolt Furol tube may be used for oils having a time of flow through the Parol tube of more than 25 seconds. (c) For oils of high viscosities, it is more convenient to use the Furol tube. (d) For oils having times of flow below 32 seconds (Universal) this test is not valid. (2) A receiving flask having a graduated volume of 60 ml. (3) Two ASTM Saybolt Viscosity Thermometers of the proper range for the particular test, one for the viscosity machine and one for the sample. (4) A timing device. This may be either (a) A stop watch, or (b) An electric timer which can be started and stopped by means of a switch. (5) A tube for withdrawing excess oil from the viscosity machine. This may be attached to a vacuum line. Set the machine at the proper temperature for the test to be run. (1). Saybolt Universal viscosities are usually run at either 100° or 210° F., but may also be run at 32°, 70°, or-130° F. (2) Saybolt Furol viscosities are usually run at 122°* F. but also may be run at 77°, 100°, or 210° F. (3) Several machines are often maintained at various temperatures, so that you need only select the proper maehine. Clean the oil tube of any residue from past de terminations, (1) Pour gasoline through the tube to wash it out, (2) Remove any excess gasoline from the gallery. (5) Dry the inside of the tube thoroughly using toilet tissue or other absorbent, lint-free material. Strain the sample through a 100-mesh wire strain er. Pour enough of the sample into the tube to wet it thoroughly, and allow the sample to drain out. Discard this used sample. Adjust the sample to the proper temperature for the test. (1) If the test is conducted above room tem perature, heat the oil to a temperature not more than 3° above the test temperature. (2) If the test Is conducted below room tem perature, cool the oil to a temperature not less than 3° below the test temperature. (3) With the stopper in place at the lower end of the outflow tube, pour the sample Into the tube until it Is well above the level of the gallery. (4) Stir constantly with the thermometer, noting the temperature at frequent inter vals. (5) When the temperature remains constant at the required point for one minute, proceed with the test. While the sample has been cooling In the oil tube, perform last minute check-ups on the timing device. (1) See that it will start and stop when the switch is pressed. . (2) See that it is set exactly at zero.- Adjust the level of the sample in the oil tube. (1) When the sample reaches and hold the pro per temperature, withdraw the thermometer. (2) Insert the withdrawal tube to remove ex cess oil. (a) Place the tube at one point in the gallery. 57 (b) Do not let the withdrawal tube touch the overflow rim of the gallery. (c) Never rotate the tube around the gallery. (3) Continue withdrawing excess oil until the level in the gallery is below that of the oil tube proper, i. Set the receiving flask under the outlet tube in such a position that the stream of oil will strike the neck of the flask, j. Conduct the test. (1) Snap the cork from its position. (2) At the same instant, start the timer. (3) Stop the timer when the bottom of the meniscus of the oil reaches the mark on the neck of the flask. (4) As a check on your previous work, allow the oil to continue flowing into the flask until it stops. (a) If this takes an excessive time, the outlet tube is probably partially stopped. (b) If the flask overflows, you forgot to withdraw excess oil from the gal lery. (c) In either ease, re-run the test, k. Report as the Saybolt viscosity the time in seconds as shown on the timer. (1) If the test was run with the Universal Outlet tube, report the.viscosity as "X seconds SSU". (S) If the test was run with the Furol outlet tube, report the viscosity as "X seconds SSF.tt 1. Clean the outlet tube as previously described. 10. SOURCES FOR THIS CHAPTER: Ihere to get further assistance. a. ASTM Standards: D 975-48 T; D 596-48 T; D 887-59; D 96-47 T5 D 95-46; D 91-40; D 93-46; D 97-47; D 155-45 T; D 88-44. b. Laboratory manuals and specification lists of the oil companies. ACTIVITY ASSIGNMENTS: Laboratory work to help you get started testing heavy oils. 1. GAS OIL: -Run routine tests on several gas oils. 2. FUEL OIL: Run routine tests on several fuel oils, 3. LUBRICATING OIL: Run routine tests on several lubricating oils. 4. CRUDE OIL: Run those routine tests which apply to crude oils. 59 5. CLASSIFICATION: List the routine tests that should "be applied to each of the above types of heavy oils. D. .EVALUATION-: A best answer test to evaluate vour mastery of routine tests. (Place the number of the best answer in the parentheses.) 1. ( ) You should use the'BS&M test to obtain a know ledge of the: (1) Sediment in a crude oil. (2) Water in a fuel oil. (3) Sulfur in a gas oil. (4) Water and sediment in any oil. 2. ( ) For heavy oils such as these, you should gene rally take the gravity at a temperature: (1) Higher than that for light oils. (2) Lower than that for light oils. (3) Approximately the same as for light oils. 3. ( ) You should find the amount of water in a sample by using; (1) A hydrometer. (2) A form of distillation. (3) A centrifuge. (4) A chromo meter. 4. ( ) If, on the same oil, you obtained a P-M flash of 180° F. and a Cleveland flash of 230° F. you should: (1) Repeat the tests. (2) Report both as usual. (3) Immediately call the fore man's notice to the results. (4) Check to make sure your thermometers were accurate. 60 5, ( ) You should reject as not meeting specifications a lubricating oil that has a very high; (1) Precipitation number. (2) Flash point (Cleve land). (5 Viscosity index. (4) Initial boiling point. CHAPTER 6. BOILING RANGE HOW TO DISTILL HEAVY OILS \ A. MOTIVATION: Advantages of learning to distill heavy oils, ~ 1. NO FATIGUE: You will only run one distillation for this type at a time, so each test gives you forty- five minutes of rest, 2. NO EXTRA WORK: You cannot perforin other types of tests while running a distillation. 5. HIGHER PAY: Those who run crude distillations of this type often receive more pay than an ordinary inspector. B. DIRECTIONS: Suggestions to help you in distilling heavy oils. 1. GAS OIL: How to distill gas oils, a. Assemble the proper equipment. (1) Use the condenser bath, heater, and shield provided• (2) Choose a 250 ml. distilling flask with a tight-fitting cork stopper on the distilling tube. (a) Select a flask that has been used before. (b) If a new flask must be used, put 5 to 4 small glass beads into the flask. (3) Choose an ASTM High-Distillation Ther mometer having a top temperature reading of 760° F. and provided with a tight-fitting cork. (4) Provide two 250 or 200 ml. graduated cylin ders. (5) Procure an analysis card, or provide some means of recording data. Get the condenser and flask ready for action. (1) Start warm water circulating through the condenser at such a rate that the overflow temperature is between 90 and 100° F. (2) Using a soft, lint-free cloth attached to a stiff cord, swab the condenser tube to remove any liquid. (3) Recheck the flask to make sure it has no cracks. (a) Inspect the bottom of the flask. (b) Tap the bottom of the flask gently on a hard surface to see if it will crack. Prepare the sample for distillation. (1) Measure 2 0 ml. of the sample into the graduated cylinder. (a) Fill the cylinder to a point above the 200 ml. graduation. (b) Take the API gravity unless this has already been done. (See Chapter 5.) (c) Pour off the excess sample so that exactly 200 ml. remains in the cylin der. (2) Transfer the sample to the flask. (a) Pour it carefully so that no sample is spilled. (b) Make sure no sample gets into the vapor tube. (5) Insert the thermometer into the flask. (Follow the same procedure as is given for light oils. See Chapter 2.) (4) Set the flask in position in the same man ner as for light oils. (See Chapter 2.) (5) Set the receiver in position. (a) Use the second cylinder for the re ceiver. (It must be clean and dry.) (b) Place the cylinder under the lower end of the condenser so that the con denser tube extends into the cylinder at least an inch. Conduct the distillation. (1) Apply heat to the flask. Adjust the heating rate such that the first drop falls from the condenser in not less than 10 nor more than 15 minutes. Record the. temperature at which this drop falls as the initial boiling point. (IBP.) Proceed with the distillation at a rate between 8 and 10 ml. per minute. (a) Increase or decrease the heat as necessary to maintain this rate, but: (b) Make no further heating adjustment when the volume of liquid in the re ceiver reaches 180 ml. Record temperatures corresponding to desig nated volumes in the receiver. (a) Record the temperature when 10 ml. of liquid has been distilled into the receiver (5$ point.) (b) Record the 10$ point, and each suc ceeding 10$ point. (20$, 30$, etc.) (c) Record the 95$ point if the distil lation is still being continued at that point. (d) Record any other points specifically asked for. (e) Proceed in reading temperatures in the same manner as for distilling light oils* (See Chapter 2.) When the temperature reaches 500°, raise the temperature of the water in the con denser to 140°, and thereafter maintain it between 140° and 160° F. Terminate the distillation when: (a) The temperature reaches 700°, or (b) The temperature reaches a maximum point and starts decreasing. This may be either a normal end point, or may be due to cracking. If the maximum is due to cracking of the gas oil, so indicate. Cracking can be designated by the following: (a) There will probably be liquid left in the flask when the maximum due to cracking occurs. (At a true maximum, the flask is usually dry.) (b) There will be a sudden increase in the distillation rate (never present at a true maximum.) (c) When you attempt to control the rate, the temperature will drop sharply. (d) The flask may suddenly fill with a greenish or brownish gas. (e) The last part of the distillate will have a typical "cracked" smell. This odor will be quite different from the odor of the original gas oil. (9) Allow a few minutes for _the last of the distillate to drain from the condenser tube into the receiver. e. Record one-half the total volume distilled as the percent recovery. f. Record the difference between 100.0 and the percent recovery as the residue and loss. g. DO not tear down the apparatus until it has cooled for several minutes. SPRAY OIL: How to distill spray oils. a. Use the same equipment as for a gas oil distil lation, except use two 100 ml. graduates instead of 250 ml. (See section 1 of this chapter.) b. Prepare the condenser and flask in the same manner as for a gas oil distillation, except adjust the temperature of the condenser water to 140° F. c. Add the sample to the flask. (1) Measure a 100 ml. sample in a graduated cylinder at 70° to 80° F. (2) Pour the sample into the flask and allow the cylinder to drain for 30 seconds, (3) Place the cylinder in a boiling water bath for about a minute, (4) Again drain the cylinder into the flask for 30 seconds. Bet up the equipment. (1) Insert the thermometer and set the flask in position in the same manner as for gas oils. (See section 1 of this chapter.) (2) Set the receiver in position. (a) Use the second cylinder for the re ceiver. (b) Place the cylinder under the lower end of the condenser so that the con denser tube extends into the cylinder at least an inch, and so that the drops will fall separately without running down the side of the cylinder. Conduct the distillation. (1) Apply heat to the flask. (2) Adjust the heating rate such that the first drop falls from the condenser in not less than 10 nor more than 15 minutes. 68 (3) Record the vapor temperature at which this drop falls as the initial boiling point. (4) Proceed with the distillation at a rate between 4 and 6 ml. per minute, adjusting the heat as necessary to maintain the rate. (5) Record the vapor temperature corresponding to each 5 ml. of distillate received. (6) Terminate the distillation when: (a) The 95^ point has been reached and recorded, or (b) The sample cracks. (For symptoms of crac.king, see section 1 of this chapter.) f. Do not tear down the apparatus until it has cooled for several minutes. 3. CRUDE OILS: How to distill crude oils, a. Assemble the proper equipment. (1) Use the condenser bath, heater, and shield provided. (2) Procure a Hempel flask with jack chain and supporting device. (3) Choose an ASTM Low-Distillation Thermometer provided with a tight-fitting cork. (4) Provide two graduated cylinders. (a) One cylinder capable of holding at least 300 ml. (b) One cylinder with a capacity of 100 ml. and capable of being tightly stoppered. Prepare the condenser and flask in the same manner as for a gas oil distillation, except the condenser bath must be filled with cracked ice to maintain a temperature of 32° to 34° F. Add the sample to the flask. (1) Fill the cylinder to a point above the 300 ml. graduation. (2) Take the API gravity of the sample. (See Chapter 5.) (3) Pour off the excess sample so that exactly 300 ml. remains in the cylinder. (4) Carefully transfer the sample to the flask and allow the cylinder to drain thoroughly Carefully set the supporting device in position Add the jack chain so that it fills the space uniformly and without channels for vapor. Insert the thermometer and set the flask in position in the same manner as for gas oils. (See section 1 of this chapter.) Immerse the receiver graduate in a bath main tained at 32° to 40° F. and place the cylinder under the condenser outlet tube In the usual manner. h. Apply heat vigorously to the flask until the liquid begins to boil* i. Decrease the heat input as the liquid begins to distill. (1) For the first 10 ml. the rate should be 2 to 3 ml. per minute. (2) After this, the rate may be again increased to 4 to 5 ml, per minute. j. Terminate the distillation at the temperature decided upon for the particular test, (usually about 400° F.). k. Stopper the receiving flask and allow the distil late to stand until all water has settled out and the temperature is between 55° and 65° F. 1, Read and record the total volume of liquid in the receiver, m. Read and record the volume of water, if any. n. Calculate the percentage of naphtha in the crude - using the following formula: % - V - W X 100. 300 - W V is the total volume of liquid in the receiver. W is the volume of water in the receiver, o. Repeat the whole procedure, (a through m) enough times so that a total of at least 100 ml. of water-free naphtha is obtained* 71 pw Separate the naphtha from the water, and combine the naphthas. Shake thoroughly, q. Bun an Engler distillation test on the combined distillates. r. Report all results on the appropriate forms. 4. SOURCES FOR THIS CHAPTER: Where to get further assistance. a. ASTM Standards: D 975-48 T; D 596-48 T; D 158-41; D 447-41; D 285-41. b. . Laboratory manuals and specification lists of the various oil companies in the area. C. ACTIVITY ASSIGNMENTS: Laboratory work to help you master distillation techniques. 1. GAS OIL: Distill several gas oils and turn in your data. 2. SPRAY OIL: Distill some spray oils and turn in your recorded points. 3. CRUDE OIL: Distill a crude oil by the Hempel method. Repeat this distillation enough times to obtain at least 100 ml. of naphtha. 4. NAPHTHA: Redistill the naphtha from the crude oil by the appropriate method. Report the end point obtained, and plot the curve for the distillation. 72 D. EVALUATION; A rating scale to test your mastery of distillation techniques. (Place an X in the spaces for which you qualify.) 1. ( ) You selected the proper equipment for the test. 2. ( ) You put beads in the bottom of the flask if it was necessary. 3. ( ) You checked the flask to see that it had no cracks. 4. ( ) You swabbed out the condenser. 5. ( ) You set the temperature in the condenser bath properly. 6. ( ) You measured out the sample correctly. 7. ( ) You poured the sample into the flask carefully and without spilling any. 8. ( ) You set your flask and receiver properly in position. 9. ( ) You brought the first drop of distillate over within the time limits specified. 10. ( ) You recorded the distillation points accurately. 11. ( ) You terminated the distillation at the correct < time . 12. ( ) You reported the recovery and loss accurately. 13. ( ) You disassembled the apparatus after it had cooled. ( ) Total. CHAPTER 7. CONCLUSION HOW TO PERFORM SUPPLEMENTARY TESTS' A. MOTIVATION: Rewards that come from learning these ad vanced tests. i. LEISURE: You will have many free moments while these tests are progressing. •2. LIGHT WORK: There is no manual labor involved in performing these tests. 3. IMPRESSIVE OUTPUT:: You can run several of these tests at once and so have a large quantity of work performed to show for your time. B. DIRECTIONS; Some procedures used in performing sup plementary tests on heavy oils. 1. CARBON RESIDUE: How to determine the carbon forming propensity of an oil. a. Locate the proper equipment. (1) Conradson carbon residue apparatus, which includes the following items: (They will all be assembled under a hood.) (a) A porcelain crucible. Ob) A Skidmore iron crucible. (c) A sheet iron crucible. (d) An iron hood to cover all. (2) A Meker burner. Disassemble the equipment in preparation for the test. (1) Lift off the iron hood. (2) Remove the lid of the sheet iron crucible inside the hood. (3) Remove the lid of the Skidmore crucible which is inside the sheet iron crucible. (4) Set these lids in a convenient place for re-assembly. Weigh out the sample. (1) Select a clean porcelain crucible. (2) Drop in two small glass bead. (3) Weigh this crucible on an analytical balance, and record the weight. (4) While still leaving the crucible on a pan of the balance, add 10 grams of the sample. (5) Weigh crucible and' sample to the nearest 5 mg. Assemble the apparatus. (1) Using tongs, place the porcelain crucible in the center of the Skidmore. (2) Place the lid on the Skidmore. (3) Place the lid on the sheet iron crucible. (4) Place the hood over all. Apply heat with the Meker burner such that the pre-ignition period will be 10 plus or minus 1.5 minutes. When smoke appears in the chimney of the hood, ignite the vapors by using the burner. Adjust the burner flame so that the ignited vapors can be seen burning above the chimney, but do not extend above the wire bridge across the chimney. Keep the vapors burning in this manner for a period of IS plus or minus 1 minute, when they should cease to burn. As soon as the vapors no longer burn, heat the crucible to a cherry red and keep this condition for 7 minutes. (The total time elapsed from the instant of applying heat should be 30 plus or minus 2 minutes.) Turn off the burner and allow the apparatus to cool. Dis-assemble the apparatus, remove the porcelain crucible with heated tongs, and place it in a desiccator to cool. Weigh the cooled crucible, record the weight and the difference between this weight and that of the empty crucible. 76 m. Calculate the percent carbon residue from the formula: % = Weight of carbon in crucible x 100 Weight of sample n. Reassemble the apparatus to keep it all together. 2. ASH: How to find the ash content of oils. a. Secure the necessary apparatus. (1) A wide platinum dish of about 50 ml. capa city. (2) A bunsen burner. b. Prepare the dish. (1) Heat it to redness with the burner. (2) Allow it to cool in a desiccator, e. Weigh out the sample. (1) Weigh the dish accurately on an analytical balance, and record the weight. (2) While the dish is still on the balance pan, add about 20 grams of the sample. (3) Weigh the dish and sample to the nearest 0.1 gram. d. Place dish and sample on a suitable support and start heating gently with the burner. e. When the oil starts to smoke, move the burner to ignite the oil at the surface. f. Remove the burner and allow the oil to burn properly. g. Heat the residue till no further changes can be observed* h. Cool the dish in a desiccator and weigh when cool. i. Record the weight and the difference between this and the first weight of the dish. Calculate the percent ash from the formula; % s r Weight of ash in crucible x 100. Weight of sample k. Place the crucible in the desiccator for re use in determining ash content. (You can consider each determination as the pre-heating for the succeeding one.) SEDIMENT: How to determine the sediment by ex traction. a. Locate the necessary apparatus. (1) The extraction equipment consisting of; (a) A 1-liter Erlenmeyer flask. (b) An Underwriters. » condenser. (c) A heat source (usually an electric hot plate). (2) An alundum thimble. b. . Prepare the thimble for use. (1) Hang..the thimble from the hook on the bottom of the condenser, and hang the condenser in the flask. (2) Check to see that there is about \ inch of benzene in the bottom of the Erlen- meyer flask. (3) Apply heat to the base of the flask. (4) Start a stream of water through the con denser. (5) Extract the thimble for at least one hour in this manner. (6) Dry the thimble for at least an hour in an oven at a temperature of 220° F. (7) Allow the thimble to cool to room tem perature in a desiccator. Weigh out the sample. (X) Weigh the cooled thimble on the analytical balance to 0.0001 gram, and record the weight. (2) Quickly add about 10 grams of the sample. (3) Weigh the thimble and sample as rapidly as possible to nearest 0.01 gram. Again hang the thimble in the extraction ap paratus . Extract the sample with benzene until the sol vent dropping from the thimble is colorless. When the extraction is complete, dry the thimble in the oven for an hour. 79 g. Cool the sample in the desiccator until it reaches room temperature. h. Weigh the thimble to the nearest 0.0001 gram and record this weight and the difference between the original and final weights. i. Calculate the percent sediment from the for mula; % = Weight of sediment in thimble x 10 . Weight of sample 3- Replace the thimble in the desiccator. (You may consider each determination as the pre liminary extraction for the next determination. 4. SOURCES FOR THIS CHAPTER: Where to get further information. a. ASTM Standards: D 975-48 T; D 396-48 T; D 189-46; D 482-46; D 473-48. b. Laboratory manuals and lists of specifications of the oil companies in the vicinity. C. ACTIVITY ASSIGNMENTS: Laboratory work to help you learn analytical techniques. 1. ANALYSIS: Perform the more advanced tests out lined in this chapter on suitable heavy oils. 2. INTERPRETATION: Compare the results obtained on some oils with the State specifications for these oils. Report those which would pass. 80 D. EVALUATION: A true-false test to check your knowledge of procedure in performing advanced tests. (Place an X in the proper space for true or false. T F 1. ( )( ) You should reassemble the carbon residue equipment after performing a test in order to keep it all in order. 2. ( )( ) You should add the glass beads to the crucible after the sample has been added and weighed (carbon residue test). 3. ( )( ) You should time the carbon residue test with a stop-watch. 4. (■)( ) You should notify the foreman immediately if the carbon residue test is more than 0.1$ above the ash test for the same oil. 5. ( )( ) You should perform a preliminary extraction on all thimbles before using them for the sediment by extraction test. 6. ( )( ) When the solvent dripping from the bottom of the thimble is colorless, you should as sume that the test is complete, and place the thimble in the oven to dry. UNIVERSITY OF SOUTHERN CALIFORNIA LIBRARY 81 BIBLIOGRAPHY SPECIAL REFERENCES OF USE TO PETROLEUM TESTERS A. LABORATORY MANUALS: 1* American Society for Testing Materials: ATSM Standards on Petroleum Products and Lubricants. American Society for Testing Materials, Phila delphia, 1949. 2. Englander, Carl J.: Laboratory Manual of Gas. Oil and Fuel Analysis. John Wiley and Sons, Inc., New York, 1951. 5. Institute of Petroleum: Standard Methods for Test ing Petroleum and its Products. Institute of Pet roleum, London, 1943. 4. Universal Oil Products: UOP Laboratory Test Methods for Petroleum and its Products. Universal Oil Products Co., Chicago, 1940. B. TEXTBOOKS: 1. Gruse, William A.: Chemical Technology of Petroleum. McGraw-Hill Co., New York, 1942. 2. Nelson, William L.: Petroleum Refinery Engineering. McGraw-Hill Co., New York, 1941. UNIVERSITY OP SOUTHERN 6AMF§BNfA H H H Y
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