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: 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 safe analytical technique for determining the concentration amount of dibutyl and monobutyl phosphate degradation products in the TBP-dodecane solvent used in solvent extraction processes. This method of chemical analysis eliminates the use of diazomethane, which is toxic and explosive, thereby providing a safer laboratory technique for routine analyses required to monitor production solvent extraction processes. The solvent sample to be analyzed is spiked with mass labelled, deuterated dibutyl and monobutyl phosphates, which act as internal standards. After adding a silylating agent, bistrimethylsilyltrifluoracetamide, the sample is injected into a gas chromatograph/mass spectrometer, which measures the ratio between the labelled internal standard and the naturally occurring material to obtain a quantitative result.

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: An improved internal standard for use in determining the concentration of decomposition products of tributyl phosphate in solvent used for solvent extraction. The improved internal standard includes deuterated variants of the decomposition products to be measured, e.g., deuterated dibutyl and monobutyl phosphoric acids. The use of deuterated dibutyl and monobutyl phosphoric acids eliminates the use of diazomethane, which is toxic and explosive, thereby providing a safer laboratory technique for routine analyses required to monitor production solvent extraction processes.

Abstract: An apparatus and a method providing an open-split interface between a gas chromatograph and a mass spectrometer for delivering a substantially solvent free sample material from the gas chromatograph to the mass spectrometer. The apparatus has a junction having an inlet to receive a gas chromatograph effluent. An inert auxiliary fluid such as helium supplied through a port is used to scavenge the solvent rich effluent to atmosphere. A transfer member disposed partially within the junction is initially positioned at a first position to accomplish the aforementioned scavenging action. The transfer member is then repositioned to a second position to direct the substantially solvent free sample to the mass spectrometer for a qualitative and a quantitative analysis.

Abstract: An apparatus and method for combining a liquid chromatograph and a magnetic sector mass spectrometer is described. The liquid chromatograph elution solvent is removed and sample particles relatively free of solvent are transported, without producing an electrical glow discharge, to the magnetic sector mass spectrometer having a chemical ionization source therein.

Abstract: A switching device for a high resolution multidimensional gas chromatograph and a method of supplying a constituent from a component of a sample in a gas chromatograph effluent to a mass spectrometer. A series of open-split interfaces are interposed between a series of gas chromatographs having gas chromatographic columns with different liquid phases. An inert auxiliary fluid such as helium is supplied to the interfaces for carrying the effluent through the various stages of the device. A transfer member of the first interface is initially positioned to a first position to divert the inert fluid and the effluent to atmosphere until the desired component starts eluting from the first gas chromatograph. The transfer member of the first interface is then repositioned to a second position to direct the component and the inert fluid to the second gas chromatograph.

Abstract: An apparatus for combining a liquid chromatograph and a mass spectrometer is described. The liquid chromatograph elution solvent is removed and sample particles are carried to the mass spectrometer relatively free of solvent.

Abstract: Sets of certain halogenated aromatic organic compounds, for example, N-alkyl tetrahalophthalimides, have been found useful as chemical tags when employed in a thermal particulating organic resin. Improved tagging performance has been achieved over extended use periods at temperatures up to 140.degree. C., if the tags are microencapsulated prior to incorporation into the particulating organic resin.

Abstract: A system for detecting thermal breakdown of organic resin coatings is described which can be used for locating failure occurring in electrical apparatus based on the use of a minor amount of a chemical tagging material. The chemical tag can be readily extracted from particulate generated by the thermal breakdown of the organic resin coating by extracting the particulate with an organic solvent and analyzing the extract in a gas chromatograph using an electron capture detector. Useful results have been found when employing certain halogenated aromatic organic compounds, such as N-alkyl tetrahalophthalimides, which can be employed in the particulating resin at concentrations of as little as 0.01% by weight.

Abstract: This mass spectrometer field desorption device has a field anode in the form of a directionally solidified alloy eutectic wire of relatively large active surface and includes electrical resistance heating element to heat the field anode and thereby improve field desorption performance.

Abstract: Delivery of a test specimen vapor--carrier gas mixture into a gas chromatograph is accomplished by means of an apparatus including a barrel to receive a probe which serves to maintain the test specimen in contact with carrier gas within the barrel, a heating coil disposed around portions of the barrel housing the sample, and a compression seal releasably bearing against a portion of the probe to prevent air flow into and gas flow from the open end of the barrel.