US3323050A - Method for determination of combined oxygen in liquid alkali metals - Google Patents

Method for determination of combined oxygen in liquid alkali metals Download PDF

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US3323050A
US3323050A US199953A US19995362A US3323050A US 3323050 A US3323050 A US 3323050A US 199953 A US199953 A US 199953A US 19995362 A US19995362 A US 19995362A US 3323050 A US3323050 A US 3323050A
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oxygen
electrode
metal
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liquid alkali
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Mausteller John Wilson
Sheridan J Rodgers
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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
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/06—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a liquid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/20—Metals
    • G01N33/202—Constituents thereof
    • G01N33/2022—Non-metallic constituents
    • G01N33/2025—Gaseous constituents

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  • This invention relates to the quantitative determination of oxygen in liquid alkali metals, and more particularly to its determination indirectly by measuring the electrical resistance of an oxygen gathering metal surface exposed to the liquid alkali metal.
  • Liquid alkali metals have been used for a great variety of purposes and are widely used as heat transfer media in closed loop heat transfer systems.
  • the determination of oxygen content is necessary to assess the corrosion potential and determine dissolution rates of structural materials.
  • a number of methods of determining oxygen are known, but they require the removal of a sample of liquid metal for subsequent chemical manipulation. Such methods are cumbersome and time consuming, require a high degree of skill, and because the liquid alkali metals are pyrophoric, are not Without hazard.
  • This invention is based on the fact that alkali metal oxides will react with a second metal to form an oxide of the second metal if the free energy of formation of the oxide of the second metal is .greater than that of the alkali metal oxide.
  • a second metal and electrodes formed therefrom are herein referred to as oxygen gathering metals or oxygen gathering electrodes.
  • an oxygen gathering electrode is immersed in a body of liquid alkali metal to be tested for oxygen content and the electrode-liquid alkali metal interface is included in a resistance measuring circuit.
  • the oxygen gathering electrode reacts with the oxygen contained in the liquid metal a film of oxygen gathering metal oxide forms thereon increasing the electrical resistance between the electrode and the liquid alkali metal since the metal oxides are much poorer conductors of electricity than the metals.
  • the electrical resistance increases linearly at a rate proportional to the oxygen concentration in the liquid alkali metal until the entire immersed surface of the electrode is coated with an oxide film. At this point the rate of resistance change decreases markedly, the rate apparently being dependent on the rate of diffusion of oxygen gathering metal oxide into the body of oxygen gathering metal.
  • This break point is readily determinable in use because it is indicated by an abrupt change of slope in a plot of resistance against time, such as can be provided by conventional recording apparatus. Such plots may be used to predetermine the break point, or oxygen gathering capacity, for an electrode of any given metal and configuration.
  • the initial linear rate of resistance increase is a measure of oxygen content and is readily determined by periodic measurement of the resistance and calculation of the rate of change from two or more of such measurements. It will be apparent to those skilled in the art that the rate may be recorded or read out directly with suitable recorders and simple calculators.
  • the rate of resistance change for a given oxygen concentration will be different for each different combination of oxygen gathering metal and liquid alkali metal to be analyzed, so calibration for the particular combination used is necessary.
  • the analyzer is calibrated by determining the rate of resistance change with a given electrode and a given liquid alkali metal by comparison with chemical analysis of the liquid metal containing varying amounts of oxygen. This data is conveniently correlated in a table or family of curves with parameters of oxygen concentration and rate of resistance change.
  • the accompanying drawing is a schematic representation of an oxygen analyzer embodying this invention.
  • Liquid alkali metal 2 is contained by metal vessel 4, which is conveniently an integral part of the system in which the liquid metal is being used.
  • An oxygen gathering electrode 6 is immersed in the liquid metal and is supported by electrical conducting rod 8 which is insulated from the vessel by a gas tight insulating sleeve 10.
  • a DC. current source 12 and ohmmeter 14 are electrically connected to rod 8 and the vessel 4 completing a circuit including the vessel, the liquid metal and the electrode 6.
  • As the oxide film forms on the electrode imposing a high resistance in the circuit between the electrode and the liquid alkali metal the resistance is indicated by the ohmmeter.
  • the rate of resistance change is determined from periodic resistance measurements to indicate oxygen concentration as heretofore described.
  • rod 8 is slideably engaged by insulating sleeve 10.
  • the sleeve is mounted in a detachable tubular section 16, separated from the system by valve 18, suitably a gate valve, which when closed isolates the liquid metal system and when opened can pass the electrode.
  • valve 18 suitably a gate valve, which when closed isolates the liquid metal system and when opened can pass the electrode.
  • rod 8 is positioned so that the electrode is within the tubular section 16.
  • the tubular section is attached to the system at valve 18 forming an air lock which is flushed with inert gas through conduits 20 and 22 to prevent atmospheric contamination of the liquid metal system.
  • the valve is then opened and the electrode is lowered into the liquid metal.
  • the circuit may be completed through a second electrode immersed in the liquid metal rather than by connection to the vessel.
  • the resistance of the oxide film is thus imposed in the circuit at both electrode surfaces.
  • two electrodes When two electrodes are used they may be formed of the same or different oxygen gathering metals.
  • the resistance of the circuit will vary if the area of electrode surface in contact with the liquid metal changes, so it is necessary for precise measurements to maintain a constant level of electrode immersion.
  • the electrode may be raised or lowered in coordination with the level changes.
  • the electrode is totally immersed in the liquid alkali metal below the lowest anticipated liquid metal level so that adjustment for level changes is not necessary; similarly totally immersed electrodes may be used for analyzing flowing stream in pipes or conduits.
  • the conducting electrode support rod When the electrode is totally immersed, the conducting electrode support rod must be insulated from the liquid alkali metal, as by coating with an insulating refractory.
  • the electrode support may be formed from an oxygen gathering metal which has been inactivated by preforming an oxide coating on it.
  • the rate of resistance increase is also dependent on temperature. Although it is preferred to carry out the analysis at a substantially constant temperature, generally satisfactory precision is obtained when temperature variation cannot be avoided by considering the analysis to be made at an average temperature and averaging fluctuation of rate of resistance change over the period of analysis.
  • Table 1 lists the free energies of formation of oxide of metals which can be used as electrodes and the alkali metals. The listing is arranged with the most stable oxide at the top, progressing to the least stable oxide at the bottom.
  • a metal whose oxide is more stable than a given alkali metal oxide is an oxygen .gathering metal in that system and is suitable for use as an electrode material.
  • the relative stability of oxides in some cases changes with temperature, according to well known thermodynamics principle, so some oxygen gathering metals are operative only over limited temperature ranges for determining oxygen in a given alkali metal.
  • beryllium is not suitable for determining oxygen in lithium at low temperatures, such as 300 K., because beryllium oxide is less stable than lithium oxide, it is suitable at higher temperatures, e.g. 750 K.
  • thorium, magnesium and beryllium are suitable electrode materials for use in analyzing lithium for oxygen.
  • These three metals as well as yttrium, aluminum, hafnium, cerium, zirconium, titanium and niobium can be used to analyze sodium. All the foregoing plus chromium and zinc can be used to analyze potassium.
  • Preferred electrode materials for analyzing alkali metals other than lithium are the high melting zirconium and hafnium. Aluminum, because of its cheapness and availability, is especially preferred for analysis of alkali metals other than lithium at temperatures below about 1000 F.
  • a method of determining the concentration of combined oxygen in liquid alkali metals comprising contacting the liquid alkali metal to be tested with an electrode of a metal that forms an oxide more stable than the oxide of the alkali metal and measuring the substantially linear rate of electrical resistance increase of said electrode occurring responsive to the presence of combined oxygen in the liquid alkali metal.

Description

y 30, 1957 J. w MAUSTELLER ETAL METHOD FOR DETERMINATION OF COMBINED OXYGEN IN LIQUID ALKALI METALS Filed June 4, 1962 INEIZ'I' GAS METER LIQUID ALKALI METAL CONTAINING COMBINED OXYGEN LIQUID METAL INVENTORS. qb/m Wnsozv Maw-ream,
JWLemA/v J. P000525.
their a 7- roea/s Y2 United States Patent 3,323,950 METHOD FOR DETERMINATION OF COMBINED OXYGEN IN LIQUID ALKALI METALS John Wilson Maustellcr, Evans City, and Sheridan J.
Rodgers, Ellwood City, Pa., assignors, by mesne assignments, to Mine Safety Appliances Company, Pittsburgh,
Pa, a corporation of Pennsylvania Filed June 4. 1962. Ser. No. 199,953 5 Claims. (Cl. 324-65) This invention relates to the quantitative determination of oxygen in liquid alkali metals, and more particularly to its determination indirectly by measuring the electrical resistance of an oxygen gathering metal surface exposed to the liquid alkali metal.
Liquid alkali metals have been used for a great variety of purposes and are widely used as heat transfer media in closed loop heat transfer systems. The determination of oxygen content, the oxygen being present in combined oxide form with the liquid alkali metal, is necessary to assess the corrosion potential and determine dissolution rates of structural materials. A number of methods of determining oxygen are known, but they require the removal of a sample of liquid metal for subsequent chemical manipulation. Such methods are cumbersome and time consuming, require a high degree of skill, and because the liquid alkali metals are pyrophoric, are not Without hazard.
It is therefore an object of this invention to provide a method of determining the oxygen concentration in liquid alkali metals in situ. Another object is to provide such a method that is simple, easily performed, and utilizes an easily measurable electrical quantity. Yet another object is to provide simple and inexpensive apparatus for performing the method of the foregoing objects.
Other objects will appear from the following description. I
This invention is based on the fact that alkali metal oxides will react with a second metal to form an oxide of the second metal if the free energy of formation of the oxide of the second metal is .greater than that of the alkali metal oxide. Such a second metal and electrodes formed therefrom are herein referred to as oxygen gathering metals or oxygen gathering electrodes. We have discovered that the electrical resistance of an oxygen gathering electrode contacted with a liquid alkali metal increases linearly with a rate of increase proportional to the oxygen content of the liquid metal, and that the electrical resistance can simply and conveniently be measured to indicate the oxygen content of a liquid alkali metal.
In the practice of this invention, an oxygen gathering electrode is immersed in a body of liquid alkali metal to be tested for oxygen content and the electrode-liquid alkali metal interface is included in a resistance measuring circuit. As the oxygen gathering electrode reacts with the oxygen contained in the liquid metal a film of oxygen gathering metal oxide forms thereon increasing the electrical resistance between the electrode and the liquid alkali metal since the metal oxides are much poorer conductors of electricity than the metals. The electrical resistance increases linearly at a rate proportional to the oxygen concentration in the liquid alkali metal until the entire immersed surface of the electrode is coated with an oxide film. At this point the rate of resistance change decreases markedly, the rate apparently being dependent on the rate of diffusion of oxygen gathering metal oxide into the body of oxygen gathering metal. This break point is readily determinable in use because it is indicated by an abrupt change of slope in a plot of resistance against time, such as can be provided by conventional recording apparatus. Such plots may be used to predetermine the break point, or oxygen gathering capacity, for an electrode of any given metal and configuration. The initial linear rate of resistance increase is a measure of oxygen content and is readily determined by periodic measurement of the resistance and calculation of the rate of change from two or more of such measurements. It will be apparent to those skilled in the art that the rate may be recorded or read out directly with suitable recorders and simple calculators.
The rate of resistance change for a given oxygen concentration will be different for each different combination of oxygen gathering metal and liquid alkali metal to be analyzed, so calibration for the particular combination used is necessary. Suitably, the analyzer is calibrated by determining the rate of resistance change with a given electrode and a given liquid alkali metal by comparison with chemical analysis of the liquid metal containing varying amounts of oxygen. This data is conveniently correlated in a table or family of curves with parameters of oxygen concentration and rate of resistance change.
The accompanying drawing is a schematic representation of an oxygen analyzer embodying this invention. Liquid alkali metal 2 is contained by metal vessel 4, which is conveniently an integral part of the system in which the liquid metal is being used. An oxygen gathering electrode 6 is immersed in the liquid metal and is supported by electrical conducting rod 8 which is insulated from the vessel by a gas tight insulating sleeve 10. A DC. current source 12 and ohmmeter 14 are electrically connected to rod 8 and the vessel 4 completing a circuit including the vessel, the liquid metal and the electrode 6. As the oxide film forms on the electrode, imposing a high resistance in the circuit between the electrode and the liquid alkali metal the resistance is indicated by the ohmmeter. The rate of resistance change is determined from periodic resistance measurements to indicate oxygen concentration as heretofore described.
To provide for adjustment and removal and replacement of the electrode, rod 8 is slideably engaged by insulating sleeve 10. The sleeve is mounted in a detachable tubular section 16, separated from the system by valve 18, suitably a gate valve, which when closed isolates the liquid metal system and when opened can pass the electrode. To introduce the electrode, rod 8 is positioned so that the electrode is within the tubular section 16. The tubular section is attached to the system at valve 18 forming an air lock which is flushed with inert gas through conduits 20 and 22 to prevent atmospheric contamination of the liquid metal system. The valve is then opened and the electrode is lowered into the liquid metal.
When increased sensitivity is required, that is, a larger resistance change for a given concentration of oxygen, the circuit may be completed through a second electrode immersed in the liquid metal rather than by connection to the vessel. The resistance of the oxide film is thus imposed in the circuit at both electrode surfaces. When two electrodes are used they may be formed of the same or different oxygen gathering metals.
The resistance of the circuit will vary if the area of electrode surface in contact with the liquid metal changes, so it is necessary for precise measurements to maintain a constant level of electrode immersion. In vessels wherein the liquid metal level changes substantially, the electrode may be raised or lowered in coordination with the level changes. Preferably, the electrode is totally immersed in the liquid alkali metal below the lowest anticipated liquid metal level so that adjustment for level changes is not necessary; similarly totally immersed electrodes may be used for analyzing flowing stream in pipes or conduits. When the electrode is totally immersed, the conducting electrode support rod must be insulated from the liquid alkali metal, as by coating with an insulating refractory. Conveniently, the electrode support may be formed from an oxygen gathering metal which has been inactivated by preforming an oxide coating on it.
Since the analysis is dependent on a chemical reaction, the rate of resistance increase is also dependent on temperature. Although it is preferred to carry out the analysis at a substantially constant temperature, generally satisfactory precision is obtained when temperature variation cannot be avoided by considering the analysis to be made at an average temperature and averaging fluctuation of rate of resistance change over the period of analysis.
Table 1 lists the free energies of formation of oxide of metals which can be used as electrodes and the alkali metals. The listing is arranged with the most stable oxide at the top, progressing to the least stable oxide at the bottom.
A metal whose oxide is more stable than a given alkali metal oxide is an oxygen .gathering metal in that system and is suitable for use as an electrode material. The relative stability of oxides in some cases changes with temperature, according to well known thermodynamics principle, so some oxygen gathering metals are operative only over limited temperature ranges for determining oxygen in a given alkali metal. For example, although beryllium is not suitable for determining oxygen in lithium at low temperatures, such as 300 K., because beryllium oxide is less stable than lithium oxide, it is suitable at higher temperatures, e.g. 750 K.
From the table for example, it can be seen that at 750 K. only thorium, magnesium and beryllium are suitable electrode materials for use in analyzing lithium for oxygen. These three metals as well as yttrium, aluminum, hafnium, cerium, zirconium, titanium and niobium can be used to analyze sodium. All the foregoing plus chromium and zinc can be used to analyze potassium.
must be higher than the liquid metal temperature, so that the oxide film can form on the solid state electrode.
Preferred electrode materials for analyzing alkali metals other than lithium are the high melting zirconium and hafnium. Aluminum, because of its cheapness and availability, is especially preferred for analysis of alkali metals other than lithium at temperatures below about 1000 F.
The following example of analysis performed using a two active electrode circuit illustrates this invention. Two zirconium electrodes, supported by insulated rods, Were partially immersed in liquid sodium containing 0.005% oxygen at 600 F., as determined by chemical analysis. The resistance increased linearly for about 2 hours at a rate of 1.6 ohms per hour, at which time the rate of resistance increase decreased sharply showing the effective measuring capacity of the electrode had been used. Two zirconium electrodes of the same size were immersed to the same depth in liquid sodium containing 0.35% oxygen at 600 F. as determined by chemical analysis. The resistance increased linearly for about one hour at a rate of 3.7 ohms per hour.
Although in the foregoing description and examples the electrical resistance increase has been measured directly, it will be apparent to the artisan that it can be measured indirectly equally as well, as, for example, by measuring the change in voltage with a constant current.
According to the patent statutes we have explained the principle of our invention and have illustrated and described what we now believe to be its best embodiments. However, we desire to have it understood that, within the scope of the appended claims, the invention may be practiced otherwise than as specifically described.
We claim:
1. A method of determining the concentration of combined oxygen in liquid alkali metals comprising contacting the liquid alkali metal to be tested with an electrode of a metal that forms an oxide more stable than the oxide of the alkali metal and measuring the substantially linear rate of electrical resistance increase of said electrode occurring responsive to the presence of combined oxygen in the liquid alkali metal.
2. A method according to claim 1 in which aconstant temperature is maintained.
3. A method according to claim 1 in which the electrode is zirconium.
4. A method according to claim 1 in which the electrode is hafnium.
5. A method according to claim 1 in which the electrode is aluminum.
References Cited UNITED STATES PATENTS 2,374,088 4/1945 Fontana et al. 3243O 2,525,754 10/1950 Albrecht 32430 2,593,878 4/1952 Haines et al. 32430 RUDOLPH V. ROLINEC, Primary Examiner.
WALTER L. CARLSON, Examiner.
C. A. S. HAMRICK, C. F. ROBERTS,
Assistant Examiners.

Claims (1)

1. A METHOD OF DETERMINING THE CONCENTRATION OF COMBINED OXYGEN IN LIQUID ALKALI METALS COMPRISING CONTACTING THE LIQUID ALKALI METAL TO BE TESTED WITH AN ELECTRODE OF A METAL THAT FORMS AN OXIDE MORE STABLE THAN THE OXIDE OF THE ALKALI METAL AND MEASURING THE SUBSTANTIALLY LINEAR RATE OF ELECTRICAL RESISTANCE INCREASE OF SAID ELEC-
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3652427A (en) * 1969-12-22 1972-03-28 Little Inc A Method for monitoring the oxygen and carbon contents in a molten metal
FR2558260A1 (en) * 1983-12-29 1985-07-19 Inst Geokhimii Analitichesko Determining the gas content of metallic samples

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2374088A (en) * 1941-01-28 1945-04-17 Du Pont Corrosion recorder
US2525754A (en) * 1948-09-29 1950-10-17 Hall Lab Inc Conductivity cell
US2593878A (en) * 1945-02-26 1952-04-22 Fmc Corp Detection and quantitative determination of halogenated hydrocarbons in atmosphere

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2374088A (en) * 1941-01-28 1945-04-17 Du Pont Corrosion recorder
US2593878A (en) * 1945-02-26 1952-04-22 Fmc Corp Detection and quantitative determination of halogenated hydrocarbons in atmosphere
US2525754A (en) * 1948-09-29 1950-10-17 Hall Lab Inc Conductivity cell

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3652427A (en) * 1969-12-22 1972-03-28 Little Inc A Method for monitoring the oxygen and carbon contents in a molten metal
FR2558260A1 (en) * 1983-12-29 1985-07-19 Inst Geokhimii Analitichesko Determining the gas content of metallic samples

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