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US3852604A Expired / Lapsed US ⏱️ 0.0 years remaining

Mercury analysis system and method

Assignee: POLLUTION CONTROL Tech I
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Filing: 1972-08-11
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Granted: 1974-12-03
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Expires: 1992-08-11
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Abstract

Abstract The system and method utilize a vessel, such as a test tube, having a predetermined interior side surface area coated with gold. The closed end of the tube is uncoated. Mercury from a fluid sample is adsorbed by the gold coating, such as by passing a gas through the tube or by placing a liquid in the tube and shaking the tube for a short period of time. After mercury from a given amount of sample has been adsorbed by the gold coating, the test tube is placed in an inverted generally upright position with the closed end of the tube above the open end and with the open end vented. Then the tube is rapidly heated to a temperature in excess of 400* centigrade to vaporize the mercury from the gold coating. The mercury vapor will rise in the test tube to the closed end thereof and form a bubble of mercury vapor mixed with hot air. Ultraviolet light in the 2537 angstrom wave length band is passed endwise through the test tube. Some of the ultraviolet light is absorbed by the mercury vapor in the test tube and the transmitted light is detected and measured. Next, the mercury vapor laden air is flushed from the test tube with mercury free air. Ultraviolet light is again passed through the test tube, this time through mercury-free air and the amount of light transmitted through the mercury-free air is detected and measured. The difference between the light transmission measurements is indicative of the concentration of mercury in the fluid sample. In addition to the test tube, the system includes structure for carrying out the method steps described above.

Inventors

  • 👤 W Grengg

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-31 22:04
CPC Classifications
G; G01; G01N; G01N21/00; G01N21/17; G01N21/25; G01N21/31; G01N21/33; G01N30/00; G01N33/00; G01N33/0004; G01N33/0009; G01N33/0027; G01N33/0036; G01N33/0045

Claims Analysis

Total Claims: 35
Claim 1
Independent Claim 213 words
A method for analyzing the concentration of mercury in a fluid including the steps of: placing a given amount of a fluid sample in a vessel having a predetermined interior side surface area coated with a noble metal which has a strong affinity for mercury, such that at least a portion of the mercury in said sample is adsorbed by said noble metal coating; removing said sample from said vessel; positioning said vessel in a generally upright position with a first end of said vessel above a second end of said vessel and with said second end vented; heatinG said vessel to a given temperature to release mercury vapor from said noble metal coating; passing endwise through said vessel an ultraviolet light of a wave length band which is absorbed by mercury vapor; measuring the amount of said light transmitted through the mercury vapor laden air within said vessel; flushing said mercury vapor laden air from said vessel with mercury-free air; passing said ultraviolet light endwise through said vessel having mercury-free air therein; measuring the amount of said light transmitted through said mercury-free air; and comparing the first light transmission measurement with the second light transmission measurement, the difference between said measurements being indicative of the concentration of mercury in said fluid sample.
Claim 2
Independent Claim 213 words
A method for analyzing the concentration of mercury in a fluid including the steps of: placing a given amount of a fluid sample in a vessel having a predetermined interior side surface area coated with a noble metal which has a strong affinity for mercury, such that at least a portion of the mercury in said sample is adsorbed by said noble metal coating; removing said sample from said vessel; positioning said vessel in a generally upright position with a first end of said vessel above a second end of said vessel and with said second end vented; heatinG said vessel to a given temperature to release mercury vapor from said noble metal coating; passing endwise through said vessel an ultraviolet light of a wave length band which is absorbed by mercury vapor; measuring the amount of said light transmitted through the mercury vapor laden air within said vessel; flushing said mercury vapor laden air from said vessel with mercury-free air; passing said ultraviolet light endwise through said vessel having mercury-free air therein; measuring the amount of said light transmitted through said mercury-free air; and comparing the first light transmission measurement with the second light transmission measurement, the difference between said measurements being indicative of the concentration of mercury in said fluid sample.
Claim 3
Dependent Claim 42 words
The method according to claim 1 wherein said fluid is a gas and said steps of placing sample and removing sample from said vessel consists in passing said gas through said vessel at a given flow rate for a given time period.
Claim 4
Dependent Claim 47 words
The method according to claim 2 wherein said gas is injected into said vessel at a point near said first end of said vessel so that said gas flows along and adjacent the interior noble-metal-coated surface of said vessel and out said second end of said vessel.
Claim 5
Dependent Claim 77 words
The method according to claim 2 wherein said gas is injected into said vessel through a pipe which extends into said vessel at said second end and opens into said vessel adjacent said first end and said gas is caused to flow through said pipe into said vessel along and adjacent the interior noble-metal-coated surface of said vessel and out said second end of said vessel by applying a vacuum to said second end of said vessel.
Claim 6
Dependent Claim 25 words
The method according to claim 2 wherein said vessel is positioned in a generally upright position while said gas is being passed through said vessel.
Claim 7
Dependent Claim 74 words
The method according to claim 1 wherein said fluid sample is an aqueous solution and said method includes the steps of adding a reducing agent to the given amount of aqueous solution in said vessel; sealing said vessel; and agitating said aqueous solution and reducing agent for a given period of time to facilitate reduction of mercury compounds to free metal mercury and to facilitate adsorption of said mercury by said noble metal coating.
Claim 8
Dependent Claim 41 words
The method according to claim 6 wherein said aqueous solution sample includes dissolved solids and said method includes the initial steps of; dissolving a solid in an acid and diluting the acid-dissolved solid with water to form the aqueous solution sample.
Claim 9
Dependent Claim 12 words
The method according to claim 7 wherein said solid is a foodstuff.
Claim 10
Dependent Claim 19 words
The method according to claim 6 wherein said step of agitating said solution consists essentially in shaking said vessel.
Claim 11
Dependent Claim 17 words
The method according to claim 6 wherein said aqueous solution is agitated for at least five minutes.
Claim 12
Dependent Claim 20 words
The method according to claim 6 including the steps of rinsing and drying said vessel prior to heating said vessel.
Claim 13
Dependent Claim 38 words
The method according to claim 6 wherein said sample consists essentially of approximately ten cubic centimeters of water and said reducing agent consists essentially of approximately two cubic centimeters of an approximately 1.5 percent hydroxylamine hydrochloride aqueous solution.
Claim 14
Dependent Claim 41 words
The method according to claim 1 wherein said fluid sample is a gas sample including vapors from a thermally decomposed solid and said method includes the initial step of thermally decomposing a solid to obtain vapors which form said fluid sample.
Claim 15
Dependent Claim 12 words
The method according to claim 1 wherein said noble metal is gold.
Claim 16
Dependent Claim 18 words
The method according to claim 1 wherein said vessel is heated to a temperature between 400*C and 1,300*C.
Claim 17
Dependent Claim 14 words
The method according to claim 1 wherein said vessel is heated by infra-red radiation.
Claim 18
Dependent Claim 19 words
The method according to claim 2 including the initial step of filtering said gas to remove undesirable particles therefrom.
Claim 19
Dependent Claim 19 words
The method according to claim 1 wherein Said ultraviolet light is diffused before being passed endwise through said vessel.
Claim 20
Dependent Claim 25 words
The method according to claim 1 including the step of preheating said fluid sample to vaporize mercury in any solid particles carried in said sample.
Claim 21
Dependent Claim 33 words
The method according to claim 1 including the steps of amplifying and logarithmically converting the light measurements to signal values which are directly related to the concentration of mercury in said fluid sample.
Claim 22
Dependent Claim 41 words
The method according to claim 20 including the steps of subtracting said first signal value from said second signal value; multiplying the difference by a predetermined multiplicand to obtain a numerical value in parts per billion; and printing said numerical value.
Claim 23
Dependent Claim 292 words
The method according to claim 1 including the steps of: passing through said mercury vapor laden air ultraviolet light of a second wavelength band which is near to, but which does not include, said mercury absorption band; measuring the amount of said light having said second wave length which is transmitted through said mercury vapor laden air to obtain a light transmission measurement; passing said light having said second wave length band through said mercury-free air; measuring the amount of said light having said second wave length band which is transmitted through said mercury-free air to obtain a light transmission measurement; amplifying and logarithmically converting said light transmission measurements to signal values proportional to the logarithm of said light transmission measurements; subtracting said first signal value derived from the measurement of transmission through said mercury vapor laden air of ultraviolet light of a wavelength band which is absorbed by mercury vapor, from said signal derived from the measurement of transmission through said mercury vapor laden air of ultraviolet light of said second wave length band to obtain a first difference signal; subtracting said signal value derived from the measurement of transmission through said mercury-free air of ultraviolet light of said wave length band which is absorbed by mercury vapor from said signal derived from the measurement of transmission through said mercury-free air of ultraviolet light of said second wave length band to obtain a second difference signal; and subtracting said second difference signal from said first difference signal to obtain a signal value which is related to the concentration of mercury in said fluid sample and which has had subtracted therefrom the undesired effects of ultraviolet light absorption by other vapors which may be in said vessel in addition to mercury vapor.
Claim 24
Dependent Claim 33 words
The method according to claim 22 including the steps of multiplying said last signal value by a given multiplicand to obtain a numerical value in parts per billion; and printing said numerical value.
Claim 25
Dependent Claim 120 words
A mercury analysis system including a vessel having a noble metal coating on an interior side surface thereof and being supported in a generally upright position with an upper end of the vessel above a lower end and with the lower end of the vessel vented, means for vaporizing mercury stored in said noble metal coating, and means for analyzing the mercury vapor, said analyzing means including a source of ultraviolet light of a wave length band which is absorbed by mercury vapor, said source of ultraviolet light being positioned to pass ultraviolet light endwise through the vessel, means for detecting the amount of light transmitted through the vessel, and means for flushing mercury vapor laden air from the vessel.
Claim 26
Dependent Claim 120 words
A mercury analysis system including a vessel having a noble metal coating on an interior side surface thereof and being supported in a generally upright position with an upper end of the vessel above a lower end and with the lower end of the vessel vented, means for vaporizing mercury stored in said noble metal coating, and means for analyzing the mercury vapor, said analyzing means including a source of ultraviolet light of a wave length band which is absorbed by mercury vapor, said source of ultraviolet light being positioned to pass ultraviolet light endwise through the vessel, means for detecting the amount of light transmitted through the vessel, and means for flushing mercury vapor laden air from the vessel.
Claim 27
Dependent Claim 110 words
The system according to claim 24 including an electronic circuit connected to said detecting means, said electronic circuit including means for amplifying signals generated by light detected by said detecting means and for logarithmically converting the generated signals to signal values related to the concentration of mercury in the mercury vapor laden air, means for memorizing a first generated signal related to the light transmitted throUgh mercury-laden-vapor, means for memorizing a second generated signal related to the light transmitted through mercury-free air, and means for subtracting the first signal from the second signal to obtain difference signal directly related to the concentration of mercury in the mercury vapor laden air.
Claim 28
Dependent Claim 45 words
The system according to claim 25 including means for printing the mercury analysis measurement in parts per billion and wherein said electronic circuit includes a multiplying means connected between said subtracting means and said printing means for multiplying the difference signal by a predetermined multiplicand.
Claim 29
Dependent Claim 311 words
The system according to claim 25 including a second source of ultraviolet light of a wavelength band which is near, but which does not include, the mercury vapor absorption band, said second source being positioned to pass ultraviolet light endwise through the vessel at predetermined times, and wherein a memorizing means is operable to memorize a generated signal obtained when ultraviolet light from said second source is passed through the mercury vapor laden air in the vessel; a memory means is operable to memorize a generated signal obtained when ultraviolet light from said second source is passed through mercury-free air in the vessel, said subtracting means being operable to subtract said first signal obtained when ultraviolet light from said first source is passed through the mercury vapor laden air in the vessel from said signal obtained when ultraviolet light from said second source is passed through the mercury vapor laden air in the vessel to obtain a first difference signal, memory means operable to memorize a third signal obtained when ultraviolet light from said first source is passed through mercury-free air in the vessel, memory means operable to memorize a fourth signal obtained when ultraviolet light from said second source is passed through mercury-free air in the vessel, said subtracting means being operable to subtract said third signal from said fourth signal to obtain a second difference signal, and said electronic circuit includes a means for memorizing said first difference signal and a means for memorizing said second difference signal and a second subtracting means for subtracting said second difference signal from said first difference signal to obtain a third difference signal which is directly related to mercury vapor vaporized in the test tube and which has had subtracted therefrom the undesired effects of ultraviolet light absorption by other vapors which may be in the vessel in addition to mercury vapor.
Claim 30
Dependent Claim 66 words
The system according to claim 27 including means for printing the mercury analysis of a fluid sample in parts per billion and wherein said electronic circuit includes multiplying means connected between said second subtracting means and said printing means for multiplying said third difference signal by a predetermined multiplicand to obtain a numerical value in parts per billion of the mercury concentration in the fluid sample.
Claim 31
Dependent Claim 63 words
The system according to claim 24 wherein said flushing means includes a filter for removing mercury vapors from air used as a flushing medium, and a flush nozzle having its outlet orifice arranged to inject flushing air into the lower end of the vessel adjacent one side of the vessel and in a direction generally parallel to the longitudinal axis of the vessel.
Claim 32
Dependent Claim 23 words
The system according to claim 24 including an ultraviolet band pass filter situated between one end of the vessel and said detecting means.
Claim 33
Dependent Claim 14 words
The system according to claim 24 wherein said vaporizing means is an infra-red heater.
Claim 34
Dependent Claim 42 words
The system according to claim 24 wherein said light source is horizontally spaced from the upper end of the vessel and a prism is situated above the upper end of the vessel for reflecting light from said light source downwardly through vessel.
Claim 35
Dependent Claim 24 words
The system according to claim 24 including means interposed between said light source and the vessel for diffusing the light frOm said light source.

References Cited (Backward Citations)

US3173016A Cited
US3178572A Cited
US3544789A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1977-12-02 1978-06-03 1978-12-03 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1981-12-02 1982-06-03 1982-12-03 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1985-12-02 1986-06-03 1986-12-03 $7700.00 Window Closed / Lapsed

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