US2718493A - Distillation test apparatus - Google Patents

Distillation test apparatus Download PDF

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US2718493A
US2718493A US350620A US35062053A US2718493A US 2718493 A US2718493 A US 2718493A US 350620 A US350620 A US 350620A US 35062053 A US35062053 A US 35062053A US 2718493 A US2718493 A US 2718493A
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distillation
flask
condenser
bath
tube
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US350620A
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Jr Paul Lawler
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/14Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S203/00Distillation: processes, separatory
    • Y10S203/23Methanol

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  • ASTM test D86 The standard method of test for distillation of gasoline, naphtha, kerosine and similar petroleum products, designated as ASTM test D86, is a single sample unit involving a distillation flask with thermometer, shielded heating unit therefor, metal condenser tube in a metalwalled water bath, and a graduated cylinder disposed under the condenser tube outlets for receiving the condensed distillate.
  • the present invention involves a compact unit for multiple sample distillation wherein the operator can readily and easily watch as many as four determinations at one time. without any loss in efficiency. It also provides for cooling of the receiver unit, illumination of the receiver zone, uniform cooling of the condenser tube as well as receiver, etc.
  • Figure 1 depicts a front view
  • Figure 2 illustrates a cross-sectional side view taken along 22 of Figure 1.
  • a cross-sectional side view taken along 33 of Figure 1 is shown in Figure 3.
  • Figure 4 is a cross-sectional top view taken along 44 of Figure 2
  • Figure 5 is a partial cross-sectional front view taken along 55 of Figure 6.
  • a top or plan View of the apparatus is depicted in Figure 6. Similar numerals refer to similar parts in the various figures.
  • flask housing 11 Attached to side wall 10 of condenser bath 1 is flask housing 11 comprising a rectangular metal shield 12 and bottom 13, provided with metal separator 14, whereby there are formed two compartments in which are mounted front distillation flask 15 and rear flask 16 on electrical heaters 17 and 18 respectively.
  • a similar flask housing 19 having rectangular metal shield 20, bottom 21 and separator 22 which likewise forms two compartments in which are installed front distillation flask 23 and rear flask 24 set on electric heaters 25 and 26 respectively.
  • the two left flasks 15 and 16 have their vapor outlet tubes 27 and 28 respectively directed to the right, inserted in stoppers fit in inlets 29 and 30, respectively, of condenser tubes 6 and 4, respectively.
  • vapor outlet tubes 31 and 32 of flasks 23 and 24, respectively are directed to the left and fitted into inlets 33 and 34 (via stoppers) of condenser tubes 7 and 5, respectively.
  • receiver unit 45 Disposed in front of refrigerator compartment 35 .is receiver unit 45 comprising .a trough having metal base 46 and metalsidewalls 47 and 48 into which arecemented front glass panel 49 .and rear glass ,panel ;50 ,( Figures .2 and 4).
  • This trough is filled with cooling liquid 51 (usually water) into which are inserted glass graduates 52 serving as receivers for distillate dropping from condenser tube outlets 3.
  • Cooling liquid 51 is maintained at proper temperature by means of circulating pump 53 driven by shaft 54 of motor 41.
  • Liquid from receiver unit 45 is drawn up through tube 55, into condenser bath 1 (through grommet 56 in front wall 2), where it is cooled. Then it is fed into pump 53, and out through line 57, and is discharged into the right section of receiver unit 45.
  • Fluorescent lamp 44 having electrical leads 58 may be attached to base 46 or the rear portion of the walls 47 and 48 of the trough and serves to illuminate the interior of the trough to facilitate reading of the graduations on cylinders or graduates 52.
  • Thermometers 60 serve to indicate the vapor temperatures in flasks 15, 16, etc. during the distillation operation.
  • the samples to be distilled are placed in flasks 15, 16, 23 and 24.
  • the proper cooling liquids 8 and 51 already are at proper constant operating temperature through use of thermostatically controlled cooling coil 39 (thermostat not being shown), and pump 41. Then heat is applied at electric heaters 17, 18, 25 and 26 and the rate of heating maintained via controls on panel 42 so that the prescribed distillation rate is obtained. It will be apparent that, with the present arrangement, one person can readily read the thermometers while at the same time watch the distillation rate and make readings of the distillate dropping into graduated cylinders 52 from condenser tube outlets 3. Readings of graduations on cylinders 52 is facilitated considerably by use of lamp 44. The unit is very compact and can be moved readily with out much effort.
  • distillation tubes 6 and 7 may be straight lengths rather than coiled tubes, in which case, tube 7 would terminate at outlet 39 and tube 6 at outlet 3 in Figure 6.
  • grommets 9 may be substituted by a soldered joint.
  • bath 8 in Figure 2 could be lowered so that pump 53 is below the level of liquid 51 in trough 45 to allow for better suction.
  • the upper instruments 62 on panel 42 are wattmeters connected with each of the electric resistance heating coils in heaters 17, 18, etc. whereby much better control is obtained during the distillation than by use of ammeters according to conventional practice.

Description

Sept. 1955 P. LAWLER, JR
DISTILLATION TEST APPARATUS 5 Sheets-Sheet 1 Filed April 25, 1953 gmiaw/emzz p 20, 9 P. LAWLER, JR 2,718,493
DISTILLATION TEST APPARATUS Filed April 25, 1953 3 Sheets-Sheet 2 Sept. 20, 1955 P LAWLER, JR 2,718,493
DISTILLATION TEST APPARATUS Filed April 25, 1953 3 Sheets-Sheet S 1/1, Z zzqya'.
United States Patent DISTILLATION TESTAPPARATUS Paul Lawler, 'Jr., Bayonne, N. J.
Application .April 23, 1953, Serial No. 350,620
1 Claim. (Cl. 202-.172)
This invention deals with a multiple sample distillation testing apparatus for distillation testing of liquid products.
The standard method of test for distillation of gasoline, naphtha, kerosine and similar petroleum products, designated as ASTM test D86, is a single sample unit involving a distillation flask with thermometer, shielded heating unit therefor, metal condenser tube in a metalwalled water bath, and a graduated cylinder disposed under the condenser tube outlets for receiving the condensed distillate.
The present invention involves a compact unit for multiple sample distillation wherein the operator can readily and easily watch as many as four determinations at one time. without any loss in efficiency. It also provides for cooling of the receiver unit, illumination of the receiver zone, uniform cooling of the condenser tube as well as receiver, etc.
The invention may be more readily understood by reference to the accompanying drawings showing a preferred embodiment. Figure 1 depicts a front view, while Figure 2 illustrates a cross-sectional side view taken along 22 of Figure 1. A cross-sectional side view taken along 33 of Figure 1 is shown in Figure 3. Figure 4 is a cross-sectional top view taken along 44 of Figure 2, while Figure 5 is a partial cross-sectional front view taken along 55 of Figure 6. A top or plan View of the apparatus is depicted in Figure 6. Similar numerals refer to similar parts in the various figures.
Referring again to the drawings, numeral 1 represents a metal condenser bath having four side walls and a bottom, the front wall 1 of which serves to hold forwardly projecting outlet ends 3 of condenser tubes 4, 5, 6, and 7 immersed in liquid 8, usually water, serving as the cooling medium for the condenser tubes, all of which have the same length. Outlets 3 are sealed by rubber grommets 9 so as to prevent leakage of liquid 8.
Attached to side wall 10 of condenser bath 1 is flask housing 11 comprising a rectangular metal shield 12 and bottom 13, provided with metal separator 14, whereby there are formed two compartments in which are mounted front distillation flask 15 and rear flask 16 on electrical heaters 17 and 18 respectively. Likewise, attached to the opposite condenser bath sidewall 59 is a similar flask housing 19 having rectangular metal shield 20, bottom 21 and separator 22 which likewise forms two compartments in which are installed front distillation flask 23 and rear flask 24 set on electric heaters 25 and 26 respectively. The two left flasks 15 and 16 have their vapor outlet tubes 27 and 28 respectively directed to the right, inserted in stoppers fit in inlets 29 and 30, respectively, of condenser tubes 6 and 4, respectively. Likewise, vapor outlet tubes 31 and 32 of flasks 23 and 24, respectively, are directed to the left and fitted into inlets 33 and 34 (via stoppers) of condenser tubes 7 and 5, respectively.
Disposed beneath condenser bath 1 in metal compartment 35 (Figure 2) is hermetically sealed refrigerating unit 36 into which vaporized refrigerant is fed through 5 insures a uniform temperature.
-line 37, and from which liquefied refrigerant .is vaporized ihroughline .38 and into refrigerating coil39 which serves to cool liquid '8 .in .bath 1. .Stirrer 40, driven by motor 41 facilitates .circulation .of liquid .8 .in bath 1.and thus Panel 42 mounted on back wall 43 of bath 1 holds the instruments and-controls for heaters 17, 18, 25 and 26, .as well .as stirrer motor 41, light 44, refrigerator unit 36, etc.
Disposed in front of refrigerator compartment 35 .is receiver unit 45 comprising .a trough having metal base 46 and metalsidewalls 47 and 48 into which arecemented front glass panel 49 .and rear glass ,panel ;50 ,(Figures .2 and 4). This trough is filled with cooling liquid 51 (usually water) into which are inserted glass graduates 52 serving as receivers for distillate dropping from condenser tube outlets 3. Cooling liquid 51 is maintained at proper temperature by means of circulating pump 53 driven by shaft 54 of motor 41. Liquid from receiver unit 45 is drawn up through tube 55, into condenser bath 1 (through grommet 56 in front wall 2), where it is cooled. Then it is fed into pump 53, and out through line 57, and is discharged into the right section of receiver unit 45.
Fluorescent lamp 44 having electrical leads 58 (which are connected to a switch, not shown, in panel 42), may be attached to base 46 or the rear portion of the walls 47 and 48 of the trough and serves to illuminate the interior of the trough to facilitate reading of the graduations on cylinders or graduates 52.
Thermometers 60 serve to indicate the vapor temperatures in flasks 15, 16, etc. during the distillation operation.
When the unit is to be used for testing, the samples to be distilled are placed in flasks 15, 16, 23 and 24. The proper cooling liquids 8 and 51 already are at proper constant operating temperature through use of thermostatically controlled cooling coil 39 (thermostat not being shown), and pump 41. Then heat is applied at electric heaters 17, 18, 25 and 26 and the rate of heating maintained via controls on panel 42 so that the prescribed distillation rate is obtained. It will be apparent that, with the present arrangement, one person can readily read the thermometers while at the same time watch the distillation rate and make readings of the distillate dropping into graduated cylinders 52 from condenser tube outlets 3. Readings of graduations on cylinders 52 is facilitated considerably by use of lamp 44. The unit is very compact and can be moved readily with out much effort.
It is to be understood that variations apparent to those skilled in the art may be made and are within the scope of this disclosure. For example, distillation tubes 6 and 7 may be straight lengths rather than coiled tubes, in which case, tube 7 would terminate at outlet 39 and tube 6 at outlet 3 in Figure 6. Also, grommets 9 may be substituted by a soldered joint. Furthermore, bath 8 in Figure 2 could be lowered so that pump 53 is below the level of liquid 51 in trough 45 to allow for better suction.
The upper instruments 62 on panel 42 (Figure 1) are wattmeters connected with each of the electric resistance heating coils in heaters 17, 18, etc. whereby much better control is obtained during the distillation than by use of ammeters according to conventional practice.
I claim:
In a multiple-flask distillation test unit employing distillation flasks, each flask being disposed in a shield housing with its vapor outlet tube leading to an inlet of a condenser tube immersed in an elevated cooled bath container to allow flow of distillate therefrom into a receiver disposed thereunder, the improvement comprising at least one flask shield housing mounted on each side of said bath container so that the vapor outlet tube of the flask therein may be directed to the side wall of the container, the condenser tube inlet being directed through said side wall of the container andadjacent flask shield for connection with the flask tube, a wall separating each flask shield housing to form a front flask compartment and a rear flask compartment, a separate condenser tube inlet leading into each of said compartments for delivery of distillate from separate outlet tubes emerging from the front of the bath container, a receiver trough disposed under said condenser tube outlets, a suction tube leading from within one end of said trough and into the bath container, a circulating pump disposed within said bath container and fed by said suction tube, a discharge tube leading from said pump, through the wall of said 15 References Cited in the file of this patent UNITED STATES PATENTS 192,635 Clark July 3, 1877 1,516,314 Sebald Nov. 18, 1924 1,648,547 Goodfellow Nov. 8, 1927 2,222,464 Newman Nov. 19, 1940 2,342,366 Podbielniak Feb. 22, 1944 2,413,374 Phillips et al. Dec. 31, 1946 2,608,387 Randall Aug. 26, 1952
US350620A 1953-04-23 1953-04-23 Distillation test apparatus Expired - Lifetime US2718493A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2894881A (en) * 1955-11-29 1959-07-14 American Oil Co Laboratory distillation testing apparatus
US3496068A (en) * 1966-09-08 1970-02-17 Kontes Glass Co Sweep distillation apparatus
US3852159A (en) * 1973-07-24 1974-12-03 Koppers Co Inc Coke quenching car alignment indicating system

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US192635A (en) * 1877-07-03 Improvement in apparatus for refining and aging alcoholic liquors
US1516314A (en) * 1921-01-27 1924-11-18 Griscom Russell Co Flash evaporator
US1648547A (en) * 1921-05-14 1927-11-08 Walter V Goodfellow Method for producing an anaesthetic
US2222464A (en) * 1939-07-27 1940-11-19 Prec Scient Company Distillation testing apparatus
US2342366A (en) * 1939-11-08 1944-02-22 Benjamin B Schneider Low-temperature apparatus for analyzing fluids
US2413374A (en) * 1944-03-15 1946-12-31 American Smelting Refining Process for producing elemental selenium
US2608387A (en) * 1947-02-19 1952-08-26 Randall David Geoffrey Fractional distillation apparatus

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US192635A (en) * 1877-07-03 Improvement in apparatus for refining and aging alcoholic liquors
US1516314A (en) * 1921-01-27 1924-11-18 Griscom Russell Co Flash evaporator
US1648547A (en) * 1921-05-14 1927-11-08 Walter V Goodfellow Method for producing an anaesthetic
US2222464A (en) * 1939-07-27 1940-11-19 Prec Scient Company Distillation testing apparatus
US2342366A (en) * 1939-11-08 1944-02-22 Benjamin B Schneider Low-temperature apparatus for analyzing fluids
US2413374A (en) * 1944-03-15 1946-12-31 American Smelting Refining Process for producing elemental selenium
US2608387A (en) * 1947-02-19 1952-08-26 Randall David Geoffrey Fractional distillation apparatus

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2894881A (en) * 1955-11-29 1959-07-14 American Oil Co Laboratory distillation testing apparatus
US3496068A (en) * 1966-09-08 1970-02-17 Kontes Glass Co Sweep distillation apparatus
US3852159A (en) * 1973-07-24 1974-12-03 Koppers Co Inc Coke quenching car alignment indicating system

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