US3455654A - Detection of alcohols in gas atmospheres - Google Patents

Detection of alcohols in gas atmospheres Download PDF

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Publication number
US3455654A
US3455654A US460478A US3455654DA US3455654A US 3455654 A US3455654 A US 3455654A US 460478 A US460478 A US 460478A US 3455654D A US3455654D A US 3455654DA US 3455654 A US3455654 A US 3455654A
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United States
Prior art keywords
alcohol
reagent
alcohols
air
color change
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Expired - Lifetime
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US460478A
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English (en)
Inventor
Paul W Mcconnaughey
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MSA Safety Inc
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Mine Safety Appliances Co
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/20—Oxygen containing
    • Y10T436/203332—Hydroxyl containing
    • Y10T436/204165—Ethanol

Definitions

  • United States Patent U.S. Cl. 23-232 4 Claims ABSTRACT OF THE DISCLOSURE A method of detecting alcohols in air in accordance with which the air is passed into contact with a reagent consisting essentially of a soluble hexavalent chromium compound and a pentavalent phosphoric acid supported by an inert carrier.
  • a reagent consisting essentially of a soluble hexavalent chromium compound and a pentavalent phosphoric acid supported by an inert carrier.
  • the reagent undergoes a color change which affords a qualitative determination of the presence of alcohol.
  • Quantitative determination is possible by mounting the reagent in a transparent tube and determining the length over which the color change occurs upon passing a fixed volume of air at a fixed fiow rate through the tube, the length over which the color change occurs being compared with calibrated results.
  • alcohols are used as solvents, in the manufacture of a large number of other compounds, in toilet and other preparations, and for various other purposes. Many of these alcohols are capable of causing determatitis; the vapors of others in air may be hazardous to humans, exhibiting varying toxicity ranging from relatively harmless to definitely hazardous depending on the particular alcohol and the concentration present in the air being breathed. Also some alcohols when present in air present a fire or explosion hazard.
  • a copending application Ser. No. 460,479 filed June 1, 1965, by Charles A. Plantz and David G. Hannan, and assigned to the owner of this application, discloses and claims a reagent for the detection of hydrazine, volatile alkyl hydrazines, red fuming nitric acid, etc., which comprises a composition of a hexavalent chromium compound and an acid of pentavalent phosphorus on an inert carrier which in the presence of moisture undergoes a characteristic and easily observable color change promptly upon contact with the said compounds.
  • the aforesaid reagent is especially adapted to the practice of the method of this invention.
  • the reagent is disposed within a transparent container and the atmosphere to be tested is passed through it.
  • the atmosphere to be tested is passed through it.
  • the reagent changes from its normal yellow color to green. This was unexpected because there is no chemical relationship between the foregoing nitrogen compounds and alcohols.
  • the reagent may be disposed in a glass or other transparent tube of small diameter the ends of which are sealed as described in US. Patent 2,174,349 to John B. Littlefield.
  • the reagent tube is used by breaking the seals and aspirating the atmosphere to be tested through it. Appearance of the color change indicates, of course, the presence of an alcohol.
  • Color standards for comparison with the color change may be provided in the manner known in this general testing field.
  • the hexavalent chromium compound may be supplied as chromium trioxide (CrO or .as a soluble chromate or dichromate, e.g., potassium (or other alkali metal) chromate (K CrO.,,) or dichromate (K Cr O
  • the phosphoric acid may be orthophosphoric acid (H PO or metaphosphoric acid (HPO or other acid of pentavalent hosphorus.
  • the two constituents of the reagents may be used in such proportions as to provide per ml. of silica gel about 0.022 gm. to 24 gms. of pentavalent phosphorus and about 0.0145 gm. to 2.6 gms. of hexavalent chromium.
  • the most vivid color change contrast is to be had by the use of about 0.05 gm. to 3 gms. of chromium trioxide and from about 0.15 gram to 9 gms. of metaphosphoric acid per 100 milliliters of silica gel, most suitably of 8 to 14 mesh size, with the preferred proportions being 0.53 gm. of chromium trioxide and 1.67 gms. of metaphosphoric acid.
  • the reagent may be prepared satisfactorily by addition of the reagents to about 16 milliliters of water and mixing the silica gel with the solution.
  • a relatively coarse silica gel say of about 8 to 14 mesh
  • the introduction of water causes it to break down into particles finer than are desirable for the purposes of the invention. This may be avoided by using silica gel that has been humidified by exposure to humid air.
  • the impregnated silica gel is then vacuum dried until it is free flowing, preferably to a water content of about 10 to 12 percent by weight.
  • the carrier preferably a granular adsorbent, does not enter into the color-producing reaction but serves merely as an inert physical carrier for the reagent, thus avoiding the necessity for liquid reagents with their attendant disadvantages.
  • various carriers that might be used in HCl purified silica gel which, being colorless, insures maximum intensity of the color change.
  • the invention is applicable also to the quantitative determination of a wide variety of alcohols in air, and in many cases to determination of the Threshold Limit Value (T.L.V.) of the ACGIH, i.e., the concentration to which all workers may be exposed repeatedly day after day without ad verse effect.
  • T.L.V. Threshold Limit Value
  • the occurrence of the color change may be used to show the presence of an alcohol.
  • a fixed volume of air at a fixed flow rate supplied, for example, by a pump such as that described in US. Patent 3,166,938 to Weyrauch et al.
  • the length over which the color change occurs as in the tubes referred to above
  • quantitative determination is possible by comparison with calibrated re sults.
  • a pump such as described above delivering 100 ml. of air per stroke iso-amyl alcohol was calibrated as follows.
  • the tubes were 3.011 mm. ID. with a reagent bed depth of 50 mm. i5 mm. held in place by end plugs of fiber glass tape. They were first sealed at one end, dried at 250 C. overnight, filled and the other end sealed.
  • Stain length Stain length, Stain length, Isoamyl alcohol in 5 pump stroke pump stroke air-cone. (p.p.m.) mm.) (mm.)
  • the length over which the stain is produced by a given alcohol will generally be greater as a result of passage of a larger volume of air, as indicated by the foregoing table, thus increasing the sensitivity and utility of the invention.
  • n-Amyl alcohol N.L. 25-2 000 Iso-amyl alcohol. 100 50-1, 000 Sec-amyl alcohol N .L. 25-2, 000 Tert-amyl alcohol N .L. 25-2, 000 n-Butyl alcohoL. 100 50-4, 000 Iso-butyl alcohol N.L. 50-4, 000 Sec-butyl alcohol N .L.
  • Methyl alcohol 2 1 900 Methyl amyl alcohol (methyl isobutyl carbinol) 25 25-1, 00 2-methyl cyclohexanol 100 25-8000 Iso-propyl alcohol 400 100-10, 000 Propyl alcohol N.L- 000 N.L.-No threshold limit value listed in the ACGIH Threshold Limit Values Booklet for 1964.
  • the reagents of the invention may not give fully accurate quantitative results below about. 60 F. (stain length short); below that temperature acceptable results will be had at 40 to 60 P. if the tube is warmed in the hand while testing so that no correction factor will be necessary.
  • the stain may have a light end point when first formed but after about two minutes the stain intensity increases to give a clear end point. Tests have shown that when protected from the atmosphere the reagents of this invention may be expected to have a shelf like of about two years.
  • silica gel as the reagent carrier it will be understood that other substances may be used such as alumina, glass cloth, filter paper, and the like.
  • a method of detecting an alcohol in air consisting of passing air, to be tested for the presence of alcohol, into contact with a reagent consisting essentially of a soluble hexavalent chromium compound and a pentavalent phosphoric acid supported by an inert carrier and providing from 0.0145 gram to 2.6 grams of hexavalent chromium and from 0.022 gram to 24 grams of pentavalent phosphorus per 100 ml. of silica gel, the reagent undergoing a color change in the presence of said alcohol.
  • said reagent consisting essentially of chromium trioxide and metaphosphoric acid supported by silica gel in the proportions of about 0.15 gram to 3 grams of chromium trioxide and from about 0.15 to 9 grams of metaphosphoric acid.
  • the reagent consisting of chromium trioxide and metaphosphoric acid in the proportion of 0.53 gram of the former to 1.67 gram of the latter.

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Molecular Biology (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Biophysics (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
US460478A 1965-06-01 1965-06-01 Detection of alcohols in gas atmospheres Expired - Lifetime US3455654A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US46047865A 1965-06-01 1965-06-01

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US3455654A true US3455654A (en) 1969-07-15

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US (1) US3455654A (enExample)
JP (1) JPS507471B1 (enExample)
GB (1) GB1151595A (enExample)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3951855A (en) * 1971-07-08 1976-04-20 Cand-Aire Industries, Inc. Breath alcohol test medium
US4791065A (en) * 1986-03-13 1988-12-13 Grobel Research Corporation Ethanol sensitive solid
US5403749A (en) * 1992-08-13 1995-04-04 Serguei V. Khartchenko Reagent for the determination of ethanol and method of determination of presence of ethanol in the human body
US5552324A (en) * 1992-06-05 1996-09-03 Supelco, Inc. Method and apparatus for determining the concentration of readily oxidizable organic vapors in gas samples
US12210024B2 (en) 2015-05-12 2025-01-28 Dräger Safety AG & Co. KGaA Fixed-bed reactor, method for preparing a fixed-bed reactor, and use of a fixed-bed reactor

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2939768A (en) * 1956-12-31 1960-06-07 Drager Otto H Alcohol testing reagent
US3223488A (en) * 1962-08-06 1965-12-14 Luckey Lab Inc Device for alcohol determination

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2939768A (en) * 1956-12-31 1960-06-07 Drager Otto H Alcohol testing reagent
US3223488A (en) * 1962-08-06 1965-12-14 Luckey Lab Inc Device for alcohol determination

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3951855A (en) * 1971-07-08 1976-04-20 Cand-Aire Industries, Inc. Breath alcohol test medium
US4791065A (en) * 1986-03-13 1988-12-13 Grobel Research Corporation Ethanol sensitive solid
US5552324A (en) * 1992-06-05 1996-09-03 Supelco, Inc. Method and apparatus for determining the concentration of readily oxidizable organic vapors in gas samples
US5403749A (en) * 1992-08-13 1995-04-04 Serguei V. Khartchenko Reagent for the determination of ethanol and method of determination of presence of ethanol in the human body
US12210024B2 (en) 2015-05-12 2025-01-28 Dräger Safety AG & Co. KGaA Fixed-bed reactor, method for preparing a fixed-bed reactor, and use of a fixed-bed reactor

Also Published As

Publication number Publication date
GB1151595A (en) 1969-05-07
JPS507471B1 (enExample) 1975-03-26

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