US2950958A - Determination of minute traces of water by use of methylene blue - Google Patents

Determination of minute traces of water by use of methylene blue Download PDF

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US2950958A
US2950958A US611796A US61179656A US2950958A US 2950958 A US2950958 A US 2950958A US 611796 A US611796 A US 611796A US 61179656 A US61179656 A US 61179656A US 2950958 A US2950958 A US 2950958A
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water
methylene blue
carbon tetrachloride
determination
blue
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Nesh Florence
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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
    • G01N31/222—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 for investigating moisture content
    • 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
    • Y10T436/25—Chemistry: analytical and immunological testing including sample preparation
    • Y10T436/25375—Liberation or purification of sample or separation of material from a sample [e.g., filtering, centrifuging, etc.]
    • Y10T436/255—Liberation or purification of sample or separation of material from a sample [e.g., filtering, centrifuging, etc.] including use of a solid sorbent, semipermeable membrane, or liquid extraction

Definitions

  • the present invention concerns a composition and method for determination of minute traces of water in materials that contain no water molecules or potential water molecules as a basic part of its structure.
  • the invention relates to a composition and method for determination of minute traces of water in materials such as jet fuel by use of an indicator such as methylene blue.
  • An object of the invention is to provide a simple and sensitive composition and method for determination of minute traces of water in materials in cases where drying methods cannot be used.
  • Another object is to provide a composition and method for determination of minute traces of water in material such as jet fuel by use of an indicator such as methylene blue.
  • Another object is to provide an indicator composition for detecting minute traces of water in a methylene blue inert material such as jet fuel in which the composition comprises a methylene-blue-inert solvent that forms a solution in which the water is less soluble than in the material alone, and the composition further comprises an admixture of methylene blue.
  • Another object is to provide a method for determination of minute traces of water in a methylene-blue-inert material such as jet fuel which comprises releasing the water by dissolving a sample of the material in a methylene-blue-inert solvent to form a solution in which the water has decreased solubility and whereby the water coagulates in globules, and then exposing the released water to methylene blue indicator.
  • a methylene-blue-inert material such as jet fuel which comprises releasing the water by dissolving a sample of the material in a methylene-blue-inert solvent to form a solution in which the water has decreased solubility and whereby the water coagulates in globules, and then exposing the released water to methylene blue indicator.
  • the determination may be made, for example, by dissolving one volume of sample material such as jet fuel in two volumes of solvent such as carbon tetrachloride and a small quantity of methylene blue.
  • solvent such as carbon tetrachloride and a small quantity of methylene blue.
  • a preferable solvent with jet fuel and hexachlorethane is carbon tetrachloride, although other solvents such as acetone and benzol can be used provided that they do not react with the indicator being used and they do not react with the material being tested and furthermore that with jet fuels and hexachlorethane they form a solution with the material in which the water is less soluble than it is with the material alone.
  • the indicator used is preferably methylene blue because of its extreme solubility in water and because of the fact that it does not react on materials such as jet fuel and hexachlorethane and furthermore it does not react with solvents such as carbon tetrachloride, acetone 'and benzol.
  • Indicators other than methylene blue can be used so long as they are extremely soluble in water and have a high sensitivity thereto, and provided that they furthermore do not react with the material being tested and do not react with the solvent used.
  • the indicator For example jet fuel is dissolved in carbon tetrachloride and methylene blue is added. Water present in the sample tends to be released due to decreased solubility of the water in the mixture of jet fuel with carbon tetrachloride. Upon release the water coagulates in globules. If the indicator is methylene blue, it is a dry, water soluble, reddish-brown powder in the carbon tetrachloride before formation of water globules and it turns a deep blue upon formation of the globules thus indicating the presence of water.
  • Example 1 One volume of jet fuel, Navy Grade IP-S or heavy end fuel HEAF is dissolved in two volumes of carbon tetrachloride and a small quantity such as 10 mg. of dry methylene blue, water soluble, technical, Fisher Cat. No. A-766 is added. Water present in the sample tends to be released due to decreased solubility in the mixture of jet :fuel and carbon tetrachloride and the water coalesces in globules. The methylene blue which remains as a reddish-brown powder in the carbon tetrachloride will turn a deep blue as globules form indicating the presence of water. The saturation point of the jet fuel used in this example had been carefully studied and determined to be about at 0.011% water.
  • Example 2 One volume of turbine oil is dissolved in two volumes of carbon tetrachloride and a small quantity such as 10 mg. of dry methylene blue, water, soluble, technical, Fisher Catalogue No. A-76 6 is added. Water present in the sample tends to be released due to decreased solubility in the mixture of turbine oil and carbon tetrachloride and the water coagulates in globules. The methylene blue which remains as a reddish-brown powder in the carbon tetrachloride will turn a deep blue as globules form indicating the presence of water. Various samples of turbine oil containing different quantities of water were tested and as little as 0.03 mg. of water was detected. The dry turbine oil when dissolved in the carbon tetrachloride showed no reaction with the methylene blue.
  • Example 3 One volume of the sample of hexachlorethane which mately mg. of dry methylene blue, water soluble,
  • Fisher Cat. No. A-766 was added. Water present in the sample tends to be released due to de creased solubility in the mixture ofhexachlorethaneand carbon tetrachloride, and coagulates in globules.- The methylene blue which remains as a reddish-brown powder in the carbon tetrachloride will turn a deep blue as globules form indicating the presence of water. This indication will appear with as little as 0.03 mg. of Water.

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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)
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  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Description

iinited States Patent W DETERMINATION OF MINUTE TRACES (3F WATER BY USE OF METHYL-ENE BLUE Florence Nesh, 164 Hart St., Brooklyn 6, NY. No Drawing. Filed Sept. 24, 1956, Ser. No. 511,796
4 Claims. (Cl. 23-230) (Granted under Title 35, US. Code (1952), sec. 266) The invention described herein may be manufactured and used by or for the Government of the United States of America for governmental purposes without the payment of any royalties thereon or therefor.
The present invention concerns a composition and method for determination of minute traces of water in materials that contain no water molecules or potential water molecules as a basic part of its structure. In particular the invention relates to a composition and method for determination of minute traces of water in materials such as jet fuel by use of an indicator such as methylene blue.
An object of the invention is to provide a simple and sensitive composition and method for determination of minute traces of water in materials in cases where drying methods cannot be used.
Another object is to provide a composition and method for determination of minute traces of water in material such as jet fuel by use of an indicator such as methylene blue.
Another object is to provide an indicator composition for detecting minute traces of water in a methylene blue inert material such as jet fuel in which the composition comprises a methylene-blue-inert solvent that forms a solution in which the water is less soluble than in the material alone, and the composition further comprises an admixture of methylene blue.
Another object is to provide a method for determination of minute traces of water in a methylene-blue-inert material such as jet fuel which comprises releasing the water by dissolving a sample of the material in a methylene-blue-inert solvent to form a solution in which the water has decreased solubility and whereby the water coagulates in globules, and then exposing the released water to methylene blue indicator.
Other objects and many of the attendant advantages of this invention will be readily appreciated as the same becomes better understood by reference to the following detailed description.
The determination of minute traces of water, especially in cases where drying methods cannot be used, has been :difiicult in the past and has involved the use of long procedures and complicated and unwieldly apparatus. These difiiculties are overcome by the present invention which provides a simple and very sensitive composition and method making use of an indicator such as methylene blue that has extreme solubility in water.
The determination may be made, for example, by dissolving one volume of sample material such as jet fuel in two volumes of solvent such as carbon tetrachloride and a small quantity of methylene blue. Water present Patented Aug. 30, 1960 materials. A preferable solvent with jet fuel and hexachlorethane is carbon tetrachloride, although other solvents such as acetone and benzol can be used provided that they do not react with the indicator being used and they do not react with the material being tested and furthermore that with jet fuels and hexachlorethane they form a solution with the material in which the water is less soluble than it is with the material alone. The indicator used is preferably methylene blue because of its extreme solubility in water and because of the fact that it does not react on materials such as jet fuel and hexachlorethane and furthermore it does not react with solvents such as carbon tetrachloride, acetone 'and benzol. Indicators other than methylene blue can be used so long as they are extremely soluble in water and have a high sensitivity thereto, and provided that they furthermore do not react with the material being tested and do not react with the solvent used.
In application of the invention to materials such as petroleums and hexachlorethane a determination is made by dissolving a sample of the material to be tested in a suitable solvent and adding the indicator. For example jet fuel is dissolved in carbon tetrachloride and methylene blue is added. Water present in the sample tends to be released due to decreased solubility of the water in the mixture of jet fuel with carbon tetrachloride. Upon release the water coagulates in globules. If the indicator is methylene blue, it is a dry, water soluble, reddish-brown powder in the carbon tetrachloride before formation of water globules and it turns a deep blue upon formation of the globules thus indicating the presence of water.
Example 1 One volume of jet fuel, Navy Grade IP-S or heavy end fuel HEAF is dissolved in two volumes of carbon tetrachloride and a small quantity such as 10 mg. of dry methylene blue, water soluble, technical, Fisher Cat. No. A-766 is added. Water present in the sample tends to be released due to decreased solubility in the mixture of jet :fuel and carbon tetrachloride and the water coalesces in globules. The methylene blue which remains as a reddish-brown powder in the carbon tetrachloride will turn a deep blue as globules form indicating the presence of water. The saturation point of the jet fuel used in this example had been carefully studied and determined to be about at 0.011% water. Various volumes of this water-saturated jet fuel were dissolved in carbon tetrachloride and methylene blue added. As little as 0.08 mg. of water, representing 0.000016% on the basis of a 500 gm. sample were indicated by the methylene blue. The dry jet fuel when dissolved in the carbon tetrachloride showed no reaction with methylene blue.
Example 2 One volume of turbine oil is dissolved in two volumes of carbon tetrachloride and a small quantity such as 10 mg. of dry methylene blue, water, soluble, technical, Fisher Catalogue No. A-76 6 is added. Water present in the sample tends to be released due to decreased solubility in the mixture of turbine oil and carbon tetrachloride and the water coagulates in globules. The methylene blue which remains as a reddish-brown powder in the carbon tetrachloride will turn a deep blue as globules form indicating the presence of water. Various samples of turbine oil containing different quantities of water were tested and as little as 0.03 mg. of water was detected. The dry turbine oil when dissolved in the carbon tetrachloride showed no reaction with the methylene blue.
Example 3 One volume of the sample of hexachlorethane which mately mg. of dry methylene blue, water soluble,
technical, Fisher Cat. No. A-766 was added. Water present in the sample tends to be released due to de creased solubility in the mixture ofhexachlorethaneand carbon tetrachloride, and coagulates in globules.- The methylene blue which remains as a reddish-brown powder in the carbon tetrachloride will turn a deep blue as globules form indicating the presence of water. This indication will appear with as little as 0.03 mg. of Water.
Obviously many modifications and variations of the present invention are possible in the light of the above teachings. the scope of the appended claims the invention may be practiced otherwise than as specifically described.
I claim:
1. A method for determining the presence of trace amounts of water in a liquid material to be examined and that contains no water molecules and no potential water molecules as a basic part of its structure, which comprises adding to said material anhydrous carbon tetrachloride in a quantity sufiicient to free any water that is incorporated in said liquid material, agitating this mixture to free any water incorporated therein, and then adding to the mixture a small quantity of dry, water soluble, methylene blue,- whereby any water released from said liquid material will dissolve said methylene blue and change its color to a deep blue.
2. A method for determining the presenceof trace amounts of chemically uncombined but physically entrapped water in a material to be examined and that a quantity sufficient torelease any water that is physi cally entrapped in said material, and a small quantity of- It is therefore to be understood that within dry, water soluble, methylene blue, whereby any water released from its physical entrapment in said material will dissolve said methylene blue and change its color to blue.
3. A method for determining the presence of trace amounts of water in a liquid petroleum compound that contains no water molecules and no potential water molecules as a basic partof its structure, which comprises bringing saidpetroleum into intimate contact with carbon tetrachloride in an amount suflicient to free any water incorporated in said petroleum, and a small quantity of dry, water soluble methylene blue, whereby the water released from said petroleum by said carbon tetrachloride will dissolve said methylene blue and change its color to its deep blue.
4. The method according to claim 2 wherein the contacfofthe material with the methylene blue occurs after the contact of the material with the carbon tetrachloride.
References Citedin thefile of this patent i UNITED STATES PATENTS 270,489
, OTHER REFERENCES Weber: Kiiltetechnik, October 1954, Iahrg. 6, pp. 267 to 269.
v Allenetal.: Methods for the Determination of Water in, Petroleum and its Products, Bureau of Mines Pe-- troleum Technilogy 1, Technical Paper 25 (1912), page 5.
'Ofiicial and Tentative Methods of Analysis of the Assoc. of OfiicialAgricultural- Chemists, 6th ed. (1945), published .by the Assoc. of Official Agricultural Chemists, Washington, D. C. Sec. 39.60(a) pages 683, 684.

Claims (1)

1. A METHOD FOR DETERMINING THE PRESENCE OF TRACE AMOUNTS OF WATER IN A LIQUID MATERIAL TO BE EXAMINED AND THAT CONTAINS NO WATER MOLECULES AND NO POTENTIAL WATER MOLECULES AS A BASIC PARTS OF ITS STRUCTURE, WHICH COMPRISES ADDING TO SAID MATERIAL ANHYDROUS CARBON TETRACHLORIDE IN A QUANTITY SUFFICIENT TO FREE ANY WATER THAT IS INCORPORATED IN SAID LIQUID MATERIAL, AGITATING THIS MIXTURE TO FREE ANY WATER INCORPORATED THEREIN, AND THEN ADDING TO THE MIXTURE A SMALL QUANTITY OF DRY, WATER SOLUBLE, METHYLENE BLUE, WHEREBY ANY WATER RELEASED FROM SAID LIQUID MATERIAL WILL DISSOLVE SAID METHYLENE BLUE AND CHANGE ITS COLOR TO A DEEP BLUE.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3216802A (en) * 1962-01-24 1965-11-09 West Virginia Pulp & Paper Co Method and reagent for determining moisture content of paper
WO1986000711A1 (en) * 1984-07-12 1986-01-30 Olsson Bozena Reagent test for determining the water content of a product
US4962039A (en) * 1988-06-30 1990-10-09 2V Industries, Inc. Simple and rapid method for detecting the presence of water in various organic fluids
US5229295A (en) * 1992-04-02 1993-07-20 Travis Basil B Method for testing gasoline for water and alcohol in the presence or absence of the other
US20220355948A1 (en) * 2021-05-04 2022-11-10 The Boeing Company Computation of aircraft airspeed by inclusion of static air temperature

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US270489A (en) * 1883-01-09 Process of testing oils
GB563182A (en) * 1942-11-11 1944-08-02 Harold Jacob Stern Means for detecting water in fuel, lubricating oils and the like
US2515232A (en) * 1946-12-31 1950-07-18 Morris S Kantrowitz Water-detecting paper and a water-detecting coating composition therefor
US2780601A (en) * 1952-12-09 1957-02-05 Pharmacia Ab Improved chemical reagent for the quantitative determination of water

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US270489A (en) * 1883-01-09 Process of testing oils
GB563182A (en) * 1942-11-11 1944-08-02 Harold Jacob Stern Means for detecting water in fuel, lubricating oils and the like
US2515232A (en) * 1946-12-31 1950-07-18 Morris S Kantrowitz Water-detecting paper and a water-detecting coating composition therefor
US2780601A (en) * 1952-12-09 1957-02-05 Pharmacia Ab Improved chemical reagent for the quantitative determination of water

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3216802A (en) * 1962-01-24 1965-11-09 West Virginia Pulp & Paper Co Method and reagent for determining moisture content of paper
WO1986000711A1 (en) * 1984-07-12 1986-01-30 Olsson Bozena Reagent test for determining the water content of a product
US4962039A (en) * 1988-06-30 1990-10-09 2V Industries, Inc. Simple and rapid method for detecting the presence of water in various organic fluids
US5229295A (en) * 1992-04-02 1993-07-20 Travis Basil B Method for testing gasoline for water and alcohol in the presence or absence of the other
US20220355948A1 (en) * 2021-05-04 2022-11-10 The Boeing Company Computation of aircraft airspeed by inclusion of static air temperature

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