Abstract: An air contamination monitor includes a sample heater connectable to an air source such as an aircraft engine bleed air port. The heater causes any oil and other hydrocarbons in the sample air to decompose into CO.sub.2 and H.sub.2 O. A vacuum pump draws the heated air sample from the heater to a carbon dioxide analyzer. The response of the analyzer is recorded by means of a strip chart or paperless recorder.

Abstract: A flame based method for analyzing a sample by introducing the sample into a combustible gas mixture, igniting the combustible gas mixture to produce a flame, and detecting a characteristic of the resulting flame to determine the identity and/or concentration of one or more chemical substances in the sample, wherein the combustible gas mixture is generated by water electrolysis. The same method is also utilizable for determining the identity and/or concentration of one or more chemical compounds in the sample. A flame based detector apparatus for analyzing a sample is also described.

Abstract: A gas analyzer system for providing a spectroscopic analysis of the sample gas. This analysis is accomplished by first introducing the sample gas into the inlet of the system and transporting it to a spectral analyzer. The sample gas is then spectrally analyzed and the analyzer outputs a signal indicative of a radiation intensity spectrum associated with the analyzed sample gas. A processing unit uses the analyzer signal to detect the presence of one or more prescribed gases and to determine the concentration of each of the prescribed gases in the sample gas. Next, the reacting agent is supplied to the sample gas to convert one or more gases whose presence in the sample gas cannot be detected via spectral analysis due to the masking effects other gases present in the sample gas. The masked gases are converted to secondary gases at least one of which is readily detectable via spectral analysis.

Abstract: A method for the synthesis of complex organic compounds at high temperatures and internal pressures in a closed system, where autocatalytic activity is present.

Abstract: This invention is directed to an improved total sulfur chemiluminescence detection system that uses a dual burner to generate the SO speckles for contact with ozone.

Abstract: This invention provides a process for determining the nitrogen content of a sample involving (a) combusting the sample in a combustion reactor in the presence of oxygen, which oxygen is introduced into the combustion reactor in pulse form; (b) reducing the resulting combustion gases by flowing them in a flow of helium or other noble carrier gas through a Cu-containing reduction reactor; (c) performing the steps of (i) making anhydrous in a water trap the reduced gases, (ii) flowing the reduced gases through a gas-chromatographic column in order to carry out a gas-chromatographic separation of N.sub.2 from CH.sub.4 possibly present within the reduced gases, and (iii) removing CO.sub.2 from the reduced gases using a CO.sub.2 trap, with the proviso that step (i) immediately precedes step (ii); and (d) analyzing the resulting gases by detecting thermal conductivity.

Abstract: By heating a wire and positioning the wire against a specimen, the specimen may be pyrolyzed to release a pyrolysate therefrom. The pyrolysate is collected in a hood and carried to a membrane separator from which the pyrolysate may be spectrochemically analyzed. The heated wire may be repeatedly indexed for replacing the adulterated portion of the wire with a clean portion of the wire for each subsequent pyrolysis and spectrochemical analysis of the pyrolysate therefrom. A pyrolysis instrument includes a movable probe supporting the heated wire with the probe being preferably joined to a remote membrane separator flexibly joined thereto.

Abstract: Methods of assessing the destruction and removal efficiency (DRE) of a thermal combustion device having a gaseous effluent according to the formulaDRE=100.times.(W.sub.in -W.sub.out)/W.sub.inwhere:W.sub.in =mass feed rate of an organic compound into the device, andW.sub.out =the mass emission rate of the organic compound in the gaseous effluent. An apparatus for determining the destruction and removal efficiency of a thermal combustion device is also described. The methods and apparatus are capable of assessing the DRE in real time and are particularly useful in thermal combustion devices regulated by the U.S. Environmental Protection Agency that combust or burn hazardous materials containing organics.

Abstract: An apparatus which mounts a sample in a vacuum chamber, heats the sample, and analyzes the gas generated from the sample. A loading lock mechanism, enables the vacuum chamber to be maintained at a vacuum even when a measurement is not conducted, and even when a sample is introduced/discharged in/from the chamber, thereby minimizing the background noises and increasing detection performance.

Abstract: A method and apparatus for detecting the presence of a vapor of an alkyl ester of phosphoric acid, particularly tributylphosphate, in ambient air. A sample of ambient air is heated to convert any alkyl ester of phosphoric acid to an alkene. The heated sample of air is then passed to a sample loop. Carrier air periodically carries a fixed volume of sample from the sample loop through a chromatographic column to a photoionization detector which detects the presence and amount of the alkene in the sample.

Abstract: A system and method for minimizing the effects of background signals in masking signals indicating the presence of substances to be detected such as contaminants in materials moving rapidly along a conveyor. The contaminants detected may include nitrogen containing compounds and hydrocarbons. The system and method minimize, during detection of the presence or absence of such substances, the number of falsely positive indications of the presence of such substances due to background signals and changes in background signals. The substances detected are divided into first and second sample portions and the respective portions are heated. The first heated portion is mixed with ozone to cause a chemical action therewith in order to generate radiation by chemiluminescence having characteristic wavelengths related to substances in the first portion.

Abstract: This invention relates to a method and apparatus for detecting and identifying a non-volatile chemical substance, in which the chemical substance (when in a sample) is pyrolyzed into its gaseous components and then the gaseous components are monitored to determine whether or not specific gaseous components are present.

Abstract: Non-toxic combustion decomposition accelerators and processes for their production for elemental analysis. The non-toxic accelerators may be either single component or multicomponent. The single component non-toxic accelerators are glass frit, niobium pentoxide, and inorganic phosphate compounds. The multicomponent accelerators are formed from a combination of the foregoing, and most preferably from (a) one or more of niobium pentoxide, tungsten oxide and mixtures thereof, and (b) one or more of glass frit, inorganic phosphate compounds, and mixtures thereof.

Abstract: An electrochemical detection cell (320), which is usable either for potentiometric or electrolytic conductivity detection, has a capillary (305), which controls electrolyte flow. A gas stream containing detectable substances is input through a non-wettable plastic capillary (306). A reaction zone (310) through which both gas and liquid flow is internally wettable. Reference electrode (309) and either electrode (311) or (312) may be used for potentiometric detection. Sensor electrodes (311) and (312), both in the reaction zone, are used for conductivity detection. The electrolyte is fed through the capillary (305) gravimetrically from a reservoir, and the gas stream is supplied by a pyrolysis furnace. The mechanism of ionization in the gas phase ionization detector (GPELCD) is described.

Abstract: A method for evaluating a degree of dispersion of an inorganic material in a composite material comprising an organic material having dispersed therein the inorganic material, the method comprising the steps of: forming a block sample of the composite material; dividing the block sample into a plurality of unit volume pieces; incinerating each of the unit volume pieces under an oxidative atmosphere; quantitatively determining the ash content of each of the unit volume pieces; and calculating the scatter of the inorganic material content within the plurality of unit volume pieces.

Abstract: By heating a wire and positioning the wire against a specimen, the specimen may be pyrolyzed to release a pyrolysate therefrom. The pyrolysate is collected in a hood and carried to a membrane separator from which the pyrolysate may be spectrochemically analyzed. The heated wire may be repeatedly indexed for replacing the adulterated portion of the wire with a clean portion of the wire for each subsequent pyrolysis and spectrochemical analysis of the pyrolysate therefrom. A pyrolysis instrument includes a movable probe supporting the heated wire with the probe being preferably joined to a remote membrane separator flexibly joined thereto.

Abstract: A sample autoloader loads a sample into a furnace and removes a sample from the furnace. The sample autoloader includes a sealing plate for sealing the furnace. The sample autoloader also includes a mechanism for pushing a sample into the furnace and removing a sample from the furnace. The sample autoloader may include a hotel which stores sample containers for automatic loading and a container which receives spent sample containers.

Abstract: Apparatus for preconcentrating trace amounts of organic vapors in a sample of air for subsequent detection, comprising a metallic substrate; a thin film of fullerenes deposited on the metallic substrate for adsorbing the organic vapors on the thin film of fullerenes, thereby preconcentrating the organic vapors; and apparatus for heating the metallic substrate to a predetermined optimum temperature for desorbing the vapors from the thin film of fullerenes to form desorbed organic vapors for subsequent detection.

Abstract: A method of separating strontium from a sample of biomass potentially contaminated with various radionuclides. After the sample is reduced, dissociated, and carried on a first precipitate of actinides, the first precipitate is removed to leave a supernate. Next, oxalic acid is added to the supernate to cause a second precipitate of strontium and calcium. Then, after separating the second precipitate, nitric acid is added to the second precipitate to cause a third precipitate of strontium. The calcium remains in solution and is discarded to leave essentially the precipitate of strontium.

Abstract: A highly preferred container for ashable material, which material is to be ashed by heat in an ashing furnace, while it is in such container, especially when such container is to be heated by microwave radiation onto microwave absorptive elements of the furnace, which thereby heat the container, is a heat resistant, walled container which is light weight, microwave transmissive, porous and air transmissive, which is of quartz microfibers that are held in desired walled container form, preferably in substantially flat cylindrical form. Such a container may be made by shaping a heat resistant, light weight, microwave transmissive and porous non-woven sheet of quartz microfibers to container form and heating and curing such sheet in such form, preferably after moistening it with water, whereby a form-retaining container results that can be successfully employed to hold ashable samples to be ashed for analysis during microwave powered ashings of such samples.

Abstract: An on-line multidimensional system which includes a liquid chromatograph having an on-line connection to a pyrolysis probe, which in turn has on-line connection to a gas chromatograph. Preferred applications use a size-exclusion chromatograph coupled to a pyrolysis probe coupled to a gas chromatograph to simultaneously produce composition as a function of molecular weight/size information for polymeric materials.

Abstract: A ventable container for materials to be heated (preferably digested) by microwave radiation includes a movable rupture diaphragm in a venting passageway in a closure or cover for such container. Such diaphragm is tightenable into place so that the container is sealed and in such sealed state is protected by the rupture diaphragm against pressures that could develop in the container that are higher than that for which it was designed. An important feature of the invention is that the rupture diaphragm is controllably movable, when desired, to open positions to vent the container during heating and afterward, and is resealable after venting. Because of the chemical reactivity of the reagents utilized in digestions an inner chemically resistant liner is desirably employed in conjunction with a physically stronger outer body, with the outer body giving the liner enough strength to withstand pressures developed during the heating.

Abstract: An optical microscope supports a housing having a closed chamber in which a particle to be pyrolyzed is disposed and is exposable to a targeting laser beam for precisely positioning the particle and a power laser beam for heating and pyrolyzing the selected particle. The pyrolysis chamber housing is supported on a heater disposed on the microscope stage for movement into the focal plane of the objective lens and into the beam path of the targeting and power lasers. The lasers are mounted together and, in combination with multiple reflecting mirrors, direct their beams along a common beam path. The lasers are mounted on an adjustable support base for adjusting the position of the beam path along three mutually perpendicular axes.

Abstract: A method for detecting the presence of a vapor of an alkyl ester of phosphoric acid, particularly tributylphosphate, in ambient air. A sample of ambient air is heated to convert any alkyl ester of phosphoric acid to an alkene. The heated sample of air is then passed to a sample loop. Carrier air periodically carries a fixed volume of sample from the sample loop through a chromatographic column to a photoionization detector which detects the presence and amount of the alkene in the sample.

Abstract: A device for trapping reaction products and especially for generating and trapping decomposition products from thermal decomposition processes, including combustion, is described. Decomposition products of a solid sample are formed at the top end of an externally heated vertical decomposition tube and are channeled downward through a region of decreased diameter in which a trapping device is positioned. The trapping device consists of two vertical concentric tubes of which the top end of the inner tube is slightly lower than that of the outer tube. Water flows upward between the two concentric tubes, traps the decomposition products at the top, and drops down through the inner concentric tube. Products contained in the water are collected externally from the lower end of the trapping device for analysis. The insoluble gaseous products are collected by an external vacuum system after passing through the stream of water.

Abstract: A resistively-heated furnace such as a graphite furnace is employed to atomize a sample for electron ionization and mass spectrometric analysis. Wide-ranging sample types such as biological tissue, semi-solid and nonhomogeneous materials, as well as bulk organic and inorganic chemicals, can be effectively and accurately analyzed with the instrument and instrumental method with little if any sample preparation.

Abstract: A sample autoloader loads a sample into a furnace and removes a sample from the furnace. The sample autoloader includes a sealing plate for sealing the furnace. The sample autoloader also includes a mechanism for pushing a sample into the furnace and removing a sample from the furnace. The sample autoloader may include a hotel which stores sample containers for automatic loading and a container which receives spent sample containers.

Abstract: A method of determining the binder content of bituminous building material including a mixture of a mineralic constituent, a bituminous binder and moisture comprises the steps of: preparing a sample of the material, heating the sample to a temperature between 300.degree. to 550.degree. C.

Abstract: A system for introducing a sample to an analyzing device, such as a spectrometer, wherein the flow rate of gas to the analyzing device is maintained substantially constant and uncontaminated during sample changeover. The system includes a flow controller and flow control paths arranged to avoid having any flow diverting valves or direction change in the analyte flow path.

Abstract: A method for flow injection analysis of total inorganic phosphate contained in an aqueous system such a cooling tower or boiler is described which uses a reducing agent and preservative composition therefore as the carrier for the sample to be analyzed, thereby creating a facile process which permits conversion of the various polyphosphates to orthophosphate and development of the molybdenum blue complex color reaction at 60.degree.-95.degree. C. and under 2-10 psi. This method has less stringent pressure and temperature requirements than those employed heretofore, thus permitting the use of more reliable and economic devices for measuring total inorganic phosphate in the field.

Abstract: An analytical furnace includes a pair of generally vertically extending coaxially mounted spaced furnace tubes mounted to a support. The inner tube is made of a material which does not react with the specimen during pyrolysis to produce intereferring byproducts. An analytical sample crucible is supported above the support by a carbonaceous material which in the preferred embodiment comprises a combination of a carbon-felt packing material resting on the support and granular carbon black on which the crucible is placed. The material is selected to position the crucible in the hot zone of the furnace which includes a heater for heating an analytical sample for pyrolysis. The analytical furnace further includes a lance tube extending over and in coaxial alignment with the inner and outer furnace tubes for directing a sample and a carrier gas into the open mouth of the cup-shaped crucible.

Abstract: A furnace with two hot zones holds multiple analysis tubes. Each tube has a separable sample-packing section positioned in the first hot zone and a catalyst-packing section positioned in the second hot zone. A mass flow controller is connected to an inlet of each sample tube, and gas is supplied to the mass flow controller. Oxygen is supplied through a mass flow controller to each tube to either or both of an inlet of the first tube and an intermediate portion between the tube sections to intermingle with and oxidize the entrained gases evolved from the sample. Oxidation of those gases is completed in the catalyst in each second tube section. A thermocouple within a sample reduces furnace temperature when an exothermic condition is sensed within the sample. Oxidized gases flow from outlets of the tubes to individual gas cells. The cells are sequentially aligned with an infrared detector, which senses the composition and quantities of the gas components.

Abstract: This invention relates to the apparatus, for sequencing natural or recombinant DNA and other polynucleotides. In particular, this invention relates to a method for sequencing polynucleotides based on mass spectrometry to determine which of the four bases (adenine, guanine, cytosine or thymine) is a component of the terminal nucleotide. In particular, the present invention relates to identifying the individual nucleotides by the mass of stable nuclide markers contained within either the dideoxynucleotides, the DNA primer, or the deoxynucleotide added to the primer. This invention is particularly useful in identifying specific DNA sequences in very small quantities in biological products produced by fermentation or other genetic engineering techniques. The invention is therefore useful in evaluating safety and other health concerns related to the presence of DNA in products resulting from genetic engineering techniques.

Abstract: A method of detecting and analyzing impurities wherein a substrate is cleaned by heating it under vacuum, a liquid sample is dropped on a surface of the substrate under vacuum which vacuum is less than that of the previous step, the liquid sample which has thus been dropped on the substrate is dried by reducing the pressure of the atmosphere surrounding the substrate, and impurities contained in the liquid sample are detected and analyzed by examining the surface of the substrate. Thus, this method is adapted to minimize the risk of any foreign matter becoming mixed with the sample liquid, to thus ensure a high level of precision in the detection and analysis of impurities.

Abstract: A method and an apparatus for measuring and controlling the efficiency of a combustion whereby, ash samples are drawn at predetermined time intervals from a region of a combustion plant, each drawn sample is set in an exhausted reaction cell, combustion reaction gas is introduced under controlled pressure, a superficial layer of the sample is heated to the carbon combustion temperature by a CO.sub.2 laser beam, the reaction gas is drawn from the cell and the amount of carbon dioxide produced by the carbon combustion is measured in a calibrated detector. The amount of unburnt carbon contained in the ashes is determined based on a preceding calibration carried out on ashes of known carbon content.

Abstract: A heating and targeting laser beam and microscope apparatus optically senses, heats to generate a effluent fluid and chemically analyzes the thermal extract fluid or fluid pyrolyzates from a microscopic particle within a heterogeneous composite sample. A transparent duct-like chamber having a bottom opening is attached to a microscope. A contact surface of the sample is raised to abut against the bottom opening, which encloses the space around the particle and also brings the particle into the common focal plane of the microscope and the converging laser beam(s). This single step avoids the complex separate focusing and sealing steps required by present day techniques.

Abstract: Oxygen in carbonaceous materials is converted to carbon monoxide (CO) by pyrolyzing the material in a stream of oxygen-free helium. The CO is reacted with Ni.sup.63, a readioactive isotope of nickel, to form nickel tetracarbonyl (Ni.sup.63 (CO).sub.4) which is carried by the helium stream into a flow-through gas proportional counter. The quantity of Ni(CO).sub.4 is determined by the radioactivity of the gas as measured by the gas proportional counter. After exiting the flow through counter the Ni.sup.63 (CO).sub.4 is destroyed by exposing it to high temperatures. The Ni.sup.63 is retained within the apparatus while the CO is flushed from the system after being oxidized to carbon dioxide (CO.sub.2). The detection limit is estimated to be less than 1 part per billion oxygen for a 10 mg sample.

Abstract: A matrix modifier of finely-divided metallic palladium dispersed to contact a metal constituent to improve analysis of the constituent during graphite furnace atomic absorption spectroscopy. The palladium interacts with a variety of metals in a sample to increase the vaporization temperatures of the metals. One way of contacting palladium with the metal analyte is to introduce it as a salt in solution with the sample into the graphite furnace along with a surfactant. A finely-divided metallic palladium having high surface area is produced in the furnace by introduction of hydrogen gas, which acts as a reducing agent, to reduce and maintain palladium in its metallic form at an early point in the temperature program, prior to evaporation of the surfactant.

Abstract: An improved sample-holding platform for a stabilized temperature platform furnace in atomic absorption spectroscopy is provided having a recessed base and elevated sidewalls to retain an organic liquid sample and concentrate the atomized elements in a confined area for analysis after vaporization.

Abstract: The binder content of bituminous building materials, especially asphalts is determined. To enable samples of relatively great mass to be analyzed within comparatively little time, the binder is removed from the sample by thermal degradation. The binder content is then calculated from the weight loss which the sample undergoes due to the thermal decomposition.

Abstract: For the analysis of a sample in a method capable of wide application, the sample is reacted in a combustion reaction with elementary pure fluorine in a multiple molar excess in relation to the sample in a reactor of pure nickel so that the products of fluorination may be analyzed by spectrometry. A line spectrum can be produced in this manner, for example, from a silicon carbide sample combusted or reacted with elementary fluorine.

Abstract: A container for an ashable material, to be ashed by heat in an ashing furnace, especially one heated by microwave radiation onto microwave absorptive elements thereof, comprises a heat resistant, walled container which is light weight, microwave transmissive and porous, and which is of quartz microfibers that are held in desired walled container form, preferably in substantially flat cylindrical form. Such a container is made by shaping a heat resistant, light weight, microwave transmissive and porous non-woven sheet of quartz microfibers to container form and heating and curing such sheet in such form, preferably after moistening it with water, whereby a form-retaining container results that can be successfully employed to hold ashable analytic samples during ashings thereof.

Abstract: A method capable of detecting low concentrations of a pollutant or other component in air or other gas, utilizing a combination of a heating filament having a catalytic surface of a noble metal for exposure to the gas and producing a derivative chemical product from the component, and an electrochemical sensor responsive to the derivative chemical product for providing a signal indicative of the product. At concentrations in the order of about 1-100 ppm of tetrachloroethylene, neither the heating filament nor the electrochemical sensor is individually capable of sensing the pollutant. In the combination, the heating filament converts the benzyl chloride to one or more derivative chemical products which may be detected by the electrochemical sensor.

Abstract: For analyzing solid substances on mercury by measuring the atomic absorption, the substance is heated in order to expel the mercury. The generated mercury vapor is conveyed with a carrier gas flow over a body having a large surface made of an amalgam-generating material, so that the mercury vapor bonds and is accumulated as amalgam on the surface of this body. Subsequently, the body is heated in order to set the mercury accumulated as amalgam free again, and is conveyed by a carrier gas flow into a measuring vessel of an atomic absorption spectrometer. The solid substance which is to be analyzed is enclosed within a vessel having a closure which is destroyed during the heating of the solid substance. For this purpose, a cover is sealingly placed onto the vessel above the destructable closure through which cover a carrier gas flow can be supplied and be carried off.

Abstract: An improvement in an apparatus for carrying out chemical reactions is disclosed. The apparatus includes a housing defining a vacuum chamber, with a reactor located within the vacuum chamber. The improvement comprises a device disposed within the housing having a high-pressure outlet tube for engagement with the reactor, a bypass for placing the high-pressure outlet tube in fluid communication with the outside of the vacuum chamber, an orifice for placing the high-pressure outlet tube in fluid communication with the vacuum chamber and at least one valve for selectively opening or closing the bypass and the orifice. The device may be engaged and disengaged with the reactor by a manual shaft and gear arrangement for operating the reactor at higher pressures relative to the normal vacuum operation.

Abstract: An industrial process oxygen analyzer, and method of using same, incorporates an automotive oxygen sensor to minimize the criticalness of controlling heater temperature during operation. Higher sensor heater temperature, required to accommodate the automotive oxygen sensor, is achieved by application of higher supply voltage to the sensor heater. Current limiting of the heater supply circuit reduces stress on the sensor heater, even at the higher operating temperature.

Abstract: A detector system (10) especially suited for detecting a halogen containing component in a gas stream includes a gas chromatograph (12), which is connected by gas line (13) to pyrolysis chamber (14). Sources (16) of additional gas streams are connected by a gas line (18) to the pyrolysis chamber (14). The detector electrodes in the pyrolysis chamber (14) are electrically connected to detector electronics (20) by line (22). A temperature control circuit (24) is electrically connected to heater (26) by line (28). Heater (26) is thermally coupled to the pyrolysis chamber (b 14) at (30). The pyrolysis chamber (14) is thermally coupled to thermocouple (32) at (34). The thermocouple (32) is electrically connected to the temperature control circuit (24) by line (36). The heater (26) is independent of the detector electrodes and maintains a temperature between about 700 degrees and 1000 degrees Centigrade. The detector electrodes are substantially alkali metal free.

Abstract: A heat treatment device for the conversion of gaseous test samples into constituents determinable by a detector provides the possibility of obtaining the desired pyrolysis products even during the sampling, then feeding them directly to the detector. The device has a small structural shape, and is able to be carried and used easily and operated independently of an external energy supply. The heat treatment device is connectable to a number of different detectors. A container 1 through which the test gas can flow is provided with a chemical filler 5, 7, 8 capable of an exothermic reaction, and with a starter 4 initiating the reaction.

Abstract: A flame detector comprising a ceramic flame jet for use in a high temperature gas chromatography system is disclosed. The interior volume of the flame jet is fabricated of a highly inert ceramic material so that sample eluting from the end of a gas chromatography column located within the interior volume of the flame jet does not contact any metallic surface en route to the flame. By avoiding sample contact with metallic surfaces, interferences which are prone to occur at high temperature, such as peak tailing, are avoided. In a further aspect the flame detector is treated with a silylating reagent to further passivate the surfaces which may affect the sample.

Abstract: A closed inductively coupled plasma cell generates a relatively high power, low noise plasma for use in spectroscopic studies. A variety of gases can be selected to form the plasma to minimize spectroscopic interference and to provide a electron density and temperature range for the sample to be analyzed. Grounded conductors are placed at the tube ends and axially displaced from the inductive coil, whereby the resulting electromagnetic field acts to elongate the plasma in the tube. Sample materials can be injected in the plasma to be excited for spectroscopy.