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US1594593A - Apparatus for analyzing by heat of reaction - Google Patents

Apparatus for analyzing by heat of reaction Download PDF

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Publication number
US1594593A
US1594593A US696301A US69630124A US1594593A US 1594593 A US1594593 A US 1594593A US 696301 A US696301 A US 696301A US 69630124 A US69630124 A US 69630124A US 1594593 A US1594593 A US 1594593A
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receptacles
heat
reagent
chemical
reaction
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US696301A
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John C Boertlein
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Grasselli Chemical Co
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Grasselli Chemical Co
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Priority to US696301A priority Critical patent/US1594593A/en
Priority to DEG67267D priority patent/DE468912C/en
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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
    • G01N25/20Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
    • G01N25/48Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation

Definitions

  • Said apparatus comprises reservoirs for the chemical product and the reagent with overflows for maintaining constant levels therein, dippers mounted to rotate and dip into the reservoirs and deliver measured quantities of the two liquids into receptacles in which the average temperature of the two liquids is measured, and means for mixing the two liquids and measuring the temperature of the mixture.
  • the difference between the equalizing temperature of the two liquids land the temperature of the mixture is a measure of the heat of reaction, as is apparent from the publication referred to-and as is explained in the application referred to, by the use of resistance thermometers and a galvanometer and a suitably calibrated scale may be made to indicate the composition of the chemical product directly.
  • the present invention relates to a modified form of apparatus capable of performing the same functions.
  • the single figure is a vertical elevational view with parts in section of the apparatus.
  • 1 is a basin having a suitable base or legs and provided on its upper'edge with a groove containing a cushion or gasket 2 upon which rests the tubular'case 3.
  • the plate 4 closes the upper end of the case, both the plate 4 and the case 3 being held in place upon the basin 1 by means of bolts 5.
  • a sta-nd or supporting structure 6 Within the case 3 and resting also upon the upper edge of the basin 1 is a sta-nd or supporting structure 6.
  • A.Dewar flask is supported in thebasin 1 in any suitableimanner, for instance in a nestnot illustrated.
  • the stand -6 supports two cylindrical receptacles 8 and '97' provided ⁇ with Asurrotmding channels 10 and'll having sp'outs 12 and 13 for catching liquid overflowing therefrom and delivering the same into the funnel 14 which in turn empties into the basin 1 from which liquid flows through the pipe 15 to waste.
  • orifices 16 and 17 In the bottoms of the receptacles and 9 are orifices 16 and 17 surrounded by -up wardly extending peripheral walls 18 and 19 and downwardly extending peripheral walls 20 and 21.
  • the walls 16 and 17 provide sediment traps in the bottoms 0f the receptacles, while. the walls 20 and 21 extend through openings in the stand 6 ⁇ into the two branches 22 and 23 of a Y-shaped tube, the third branch 24 of which extends into the Dewar flask 7.
  • a thermometer 25 is supported by the plate 4, extending therethrough into the Dewar flask 7.
  • the plate 4 also supports the supply pipes 26 and 27 which deliver into the receptacles 8 and,9,
  • thermometers 32 ,a'nd 33 which extend downwardly through the supply pipes 26 and 27 into the receptacles 8 and
  • the apparatus operatcsas follows, assuming for convenience that the chemical product to be analyzed is oleumtand the reagent is sulfuric acid solution, hereafter called. test acid, containing sufficient free water to hy- Idrate the free S103 in the oleum.-
  • the oleum and testacid are supplied to the receptacles 8 and 9 at rates sufficient to maintain them full to overflowing,
  • thermometers 32 ⁇ and 33 the thermometer 25 may be made to indicate the analysis of the oleum.
  • the apparatus may be made of any suitable materials, for instance, if oleum is to be tested, the basin 1 and cover plate 4 may be made of cast iron or steel and th res is expensive construction and is free of moving parts.
  • Apparatus for the continuous analysis of chemical 1products comprising a receptacle for aA c emical product and a second receptacle forI a reagent capable of reacting with said chemical product to produce a sensible heat change, means for measuring the equalizing temperature of the chemical product and the reagent in said receptacles, means for continuously delivering constant flows of said chemical product and said reagent from said receptacles into a third receptacle, and means for measuring the temperature of the resulting mixture in said third receptacle.
  • Apparatus for the continuous analysis of chemical roducts comprising two receptacles provi ed with overflows, means for supplying said receptacles with a chemical product and a reagent respectively, orifices in said receptacles, means for delivering the chemical roduct and 3.
  • Apparatus for the continuous analysis of chemical products comprising two receptacles each provided with an overflow at the top and an' orifice at the bottom, means for delivering a chemical product and a reagent into said two receptacles respectivelly, a Y- sha ed tube positioned to receive c emical pro uct and reagent delivered by said perennials andto deliver the same into a third receptacle, and means Afor measuring the tem.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)

Description

' J. C. BOERTLEIN BY HEAT OF REACTION' APPARATUS FOR ANALYZING 4Filed March l, 1924 @Tlf ///////////////////ll/ll//l//////////// atto: mz 13A.
Patented Aug. 3, 1926.
` v d 1,594,593 I UNITED STATES PATENT OFFICE."
JOHN C. BOERTLEIN, OF CLEVELAND, OHIO, ASSIGNOR TO THE GRASSELLI CHEMICAL COMPANY, OIE CLEVELAND, OHIO, A CORPORATION OF OHIO.
APPARATUS FOR ANALYZING B Y HEAT OF lREACTION.
Application filed March 1,1924. Serial No. 696,301.
In an article published in the Journal of the Society of Chemical Industry, volume 29, 1910, page 3l and following, there is described a method for the quantitative analysis of chemical products, such as sulfuric acid or oleum, by causing the same to react with some other material or reagent, such as' water or dilute sulfuric acid, measuring the resulting heat of reaction and determining therefrom the composition of the chemical product.
An apparatus capable of carrying out analyses of this type is disclosed in an ap` plication in the name of Henry Howard, filed March 1, 1924, Ser. No. 696,274. Said apparatus comprises reservoirs for the chemical product and the reagent with overflows for maintaining constant levels therein, dippers mounted to rotate and dip into the reservoirs and deliver measured quantities of the two liquids into receptacles in which the average temperature of the two liquids is measured, and means for mixing the two liquids and measuring the temperature of the mixture. The difference between the equalizing temperature of the two liquids land the temperature of the mixtureis a measure of the heat of reaction, as is apparent from the publication referred to-and as is explained in the application referred to, by the use of resistance thermometers and a galvanometer and a suitably calibrated scale may be made to indicate the composition of the chemical product directly.
The present invention relates to a modified form of apparatus capable of performing the same functions.
In the drawing the single figure is a vertical elevational view with parts in section of the apparatus. Referring to the drawing, 1 is a basin having a suitable base or legs and provided on its upper'edge with a groove containing a cushion or gasket 2 upon which rests the tubular'case 3. The plate 4 closes the upper end of the case, both the plate 4 and the case 3 being held in place upon the basin 1 by means of bolts 5. Within the case 3 and resting also upon the upper edge of the basin 1 is a sta-nd or supporting structure 6. A.Dewar flask is supported in thebasin 1 in any suitableimanner, for instance in a nestnot illustrated. The stand -6 supports two cylindrical receptacles 8 and '97' provided `with Asurrotmding channels 10 and'll having sp'outs 12 and 13 for catching liquid overflowing therefrom and delivering the same into the funnel 14 which in turn empties into the basin 1 from which liquid flows through the pipe 15 to waste.
In the bottoms of the receptacles and 9 are orifices 16 and 17 surrounded by -up wardly extending peripheral walls 18 and 19 and downwardly extending peripheral walls 20 and 21. The walls 16 and 17 provide sediment traps in the bottoms 0f the receptacles, while. the walls 20 and 21 extend through openings in the stand 6 `into the two branches 22 and 23 of a Y-shaped tube, the third branch 24 of which extends into the Dewar flask 7. A thermometer 25 is supported by the plate 4, extending therethrough into the Dewar flask 7. The plate 4 also supports the supply pipes 26 and 27 which deliver into the receptacles 8 and,9,
respectively. Atthg,` upper ends of the sup ply 4pipes 26 and 27 are T-connections 28 and 29 into the lateral openings of which are connected the feed pipes 30 and 31 and in the upper openings of which are supported.
in any suitable manner, not illustrated, the thermometers 32 ,a'nd 33 which extend downwardly through the supply pipes 26 and 27 into the receptacles 8 and The apparatus operatcsas follows, assuming for convenience that the chemical product to be analyzed is oleumtand the reagent is sulfuric acid solution, hereafter called. test acid, containing sufficient free water to hy- Idrate the free S103 in the oleum.-
oleum and test acid in the receptacles 8.
and 9. The oleum and testacid are supplied to the receptacles 8 and 9 at rates suficient to maintain them full to overflowing,
thus maintaining constant heads of the liquids on the orifices 16 and 17, asa result of which substantially constant amounts of the oleum and testacid are delivered throu h the orificesand branches 22 and 23 of t e V' i Y-shaped tube into the branch 24 in 'which the two liquids vmix. The mixture flows through the branch 24 into the Dewar flask `7 in which the temperature of the mixtureis measured by thermometer 25. The overflow from the Dewar flask as well as the vmainder of the apparatus of glass. evident the apparatus is orv simple andinoverlow from lthe-.receptacles 8 and 9 is collected in the basin 1 and flows to waste' ence indicated by the two thermometers 32` and 33 and the thermometer 25 may be made to indicate the analysis of the oleum.
The apparatus may be made of any suitable materials, for instance, if oleum is to be tested, the basin 1 and cover plate 4 may be made of cast iron or steel and th res is expensive construction and is free of moving parts.
1. Apparatus for the continuous analysis of chemical 1products comprising a receptacle for aA c emical product and a second receptacle forI a reagent capable of reacting with said chemical product to produce a sensible heat change, means for measuring the equalizing temperature of the chemical product and the reagent in said receptacles, means for continuously delivering constant flows of said chemical product and said reagent from said receptacles into a third receptacle, and means for measuring the temperature of the resulting mixture in said third receptacle.
2. Apparatus for the continuous analysis of chemical roducts comprising two receptacles provi ed with overflows, means for supplying said receptacles with a chemical product and a reagent respectively, orifices in said receptacles, means for delivering the chemical roduct and 3. Apparatus for the continuous analysis of chemical products as defined in claim 2 in which a thermometer is positioned ineach y of said receptacles.
4. Apparatus for the continuous analysis of chemical products comprising two receptacles each provided with an overflow at the top and an' orifice at the bottom, means for delivering a chemical product and a reagent into said two receptacles respectivelly, a Y- sha ed tube positioned to receive c emical pro uct and reagent delivered by said orices andto deliver the same into a third receptacle, and means Afor measuring the tem.
peratures in said receptacles.
In testimony whereof, I alix my signature.
JOHN C. BOERTLEIN.v
reagent lowing through said orifices into a third receptacle.
US696301A 1924-03-01 1924-03-01 Apparatus for analyzing by heat of reaction Expired - Lifetime US1594593A (en)

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US696301A US1594593A (en) 1924-03-01 1924-03-01 Apparatus for analyzing by heat of reaction
DEG67267D DE468912C (en) 1924-03-01 1926-05-13 Device for continuous analysis of a liquid chemical product

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3273968A (en) * 1960-03-23 1966-09-20 Theodor H Benzinger Heat-burst microcalorimeter
US3436190A (en) * 1964-01-17 1969-04-01 Eastman Kodak Co Device for the determination of the concentration of a chemical compound in a liquid
US3440013A (en) * 1964-12-01 1969-04-22 Gulf Research Development Co Apparatus and process for direct measurement of heat of reaction
US3467501A (en) * 1964-06-04 1969-09-16 Microscal Ltd Calorimeter for the determination of heats of reaction
FR2427596A1 (en) * 1978-05-31 1979-12-28 Zellweger Uster Ag METHOD FOR THE DETERMINATION OF NITRIC ACID OR NITRATE
US20050036536A1 (en) * 2001-09-18 2005-02-17 Lewis Edwin A. High throughout energy array

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3273968A (en) * 1960-03-23 1966-09-20 Theodor H Benzinger Heat-burst microcalorimeter
US3436190A (en) * 1964-01-17 1969-04-01 Eastman Kodak Co Device for the determination of the concentration of a chemical compound in a liquid
US3467501A (en) * 1964-06-04 1969-09-16 Microscal Ltd Calorimeter for the determination of heats of reaction
US3440013A (en) * 1964-12-01 1969-04-22 Gulf Research Development Co Apparatus and process for direct measurement of heat of reaction
FR2427596A1 (en) * 1978-05-31 1979-12-28 Zellweger Uster Ag METHOD FOR THE DETERMINATION OF NITRIC ACID OR NITRATE
US20050036536A1 (en) * 2001-09-18 2005-02-17 Lewis Edwin A. High throughout energy array

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