Chemical apparatus and process disinfecting – deodorizing – preser – Analyzer – structured indicator – or manipulative laboratory... – Means for analyzing liquid or solid sample
Reexamination Certificate
1998-01-30
2001-01-09
Ludlow, Jan (Department: 1743)
Chemical apparatus and process disinfecting, deodorizing, preser
Analyzer, structured indicator, or manipulative laboratory...
Means for analyzing liquid or solid sample
C422S080000, C436S073000, C436S077000, C436S081000, C436S084000, C436S181000, C436S182000
Reexamination Certificate
active
06171552
ABSTRACT:
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an analytical apparatus that forms and analyzes the hydrides of target components contained in a sample.
2. Description of the Related Art
Atomic absorption and ICP atomic emission analysis techniques are widely used in analytic chemistry laboratories for measuring the concentrations of various elements in a sample. One preferred procedure for performing this analysis is to first decompose the sample into gas phase hydrides then atomize these hydrides in the detecting part of an atomic absorption or ICP atomic emission apparatus, and finally measure the concentrations of selected elements from the sample. Converting the original sample into gas phase hydrides make the target elements much easier to atomize and detect by atomic absorption/emission techniques.
The hydrides are formed preferably by adding acids and reducing agents to the samples. The types and concentrations of acids and reducing agents used to form the hydrides depend upon the elements that are analyzed. Unfortunately, selecting the types and concentrations of the hydride forming agents has, up to now, been a time consuming, manual operation. Every time a new element was measured in a sample, manual adjustments had to be made to the types and concentrations of hydride forming agents.
The concentration of an element from a sample is measured by comparing the spectral intensity of an atomic absorption or emission line with the intensity of that same line from a standard that contains a known concentration of the same element. The intensities of the atomic absorption/emission line are plotted as a function of the concentration of the standard, and the resulting curve of intensity vs. elemental concentration is called the analytical curve.
When the concentration of an element in a sample is too high or too low to fall within the upper and lower concentration limits of the analytical curve, the measurement must be repeated under different hydride formation conditions. Up to now, these adjustments were made by hand by the operator of the apparatus.
Further, conventional apparatuses employ mainly a continuous suction method, a batch addition method and an FIA method (loop injection method) as methods for introducing samples. The continuous suction method requires a lot (at least about 20 ml) of sample liquids, and therefore the concentration rate is restricted, which in turn restricts analysis of trace amounts. The batch addition method makes use of an air segment system, and therefore the sample liquids remain in the tube line to allow the memory to remain. Accordingly, the tube line has to be washed every measurement.
SUMMARY OF THE INVENTION
Accordingly, one object of the present invention is to provide for a hydride formation analytical apparatus that automatically adjusts the type and concentrations of reagents, preferably of hydride forming reagents, when analyzing one or more elements in a sample. Another object of the invention provides for a hydride formation analytical apparatus that automatically introduces a sample into the apparatus, preferably forms hydrides of elements in the sample, and performs an elemental analysis on the hydrides. A further object of the invention provides for a hydride formation analytical apparatus that automatically adjusts the types and concentrations of reagents, preferably hydride forming reagents, to keep the sample element concentration within the upper and low concentration limits of a standard analytical curve.
These and other objects of the present invention have been satisfied by the development of a hydride formation analytical apparatus.
The apparatus of the present invention reduces the concentration of residual sample materials preferably below a detectable level, by transporting a sample liquid, preferably with a carrier liquid instead of an air segment. The apparatus also preferably uses an amount of sample liquid small enough to permit measurements at elevated concentrations of the sample. The amount of sample liquid used by the apparatus for a measurement is preferably less than 5 ml, more preferably less than 1 ml. The apparatus of the present invention also preferably provides a means capable of controlling an acid concentration and a reducing agent concentration in an acid-feeding part and a reducing agent-feeding part that form part of a sample-introducing part to permit the control of these concentrations based on the kinds of samples analyzed. The apparatus preferably further comprises a control circuit for controlling integrally the respective parts to permit the automation of a series of operations extending from the introduction of the sample liquid through the analysis thereof.
The present invention preferably provides for a hydride formation analytical apparatus preferably comprising a sample-introducing part, a reagent-introducing part, a reaction part, a gas-liquid separating part and a detecting part which are continuously connected via tube lines. A sample liquid holding part, preferably a loop, is located in the sample-introducing part to introduce the sample liquid into the reaction part via the tube line preferably by the aid of a carrier. The reagent-introducing part is connected to the reaction part. An acid-feeding part and a reducing agent-feeding part are preferably components of the reagent-introducing part. The hydride gases formed from target elements in the sample are made by reacting the acid and reducing agents with the sample liquid, preferably in the reaction part. The mixture of the sample liquid and hydride gases are introduced into the gas-liquid separating part preferably from the reaction part, to separate the gases from the liquid. Preferably, inert gas is also introduced into the above gas-liquid separating part to aid in the hydride gas separation process. The separated hydride gases are preferably introduced into the detecting part where they are analyzed.
The analytical apparatus of the present invention preferably includes a preliminary reducing agent-introducing part as well as the acid-feeding part and the reducing agent-feeding part located in the reagent-introducing part. The acid and the reducing agent are preferably fed after the preliminary reagent is fed to the sample liquid in the reaction part.
The analytical apparatus of the present invention preferably further comprises a means capable of selecting the concentrations of the acid and the reducing agent. Preferably this includes an analytical apparatus in which the acids having different concentrations are held in the acid-feeding part, and the concentrations of the acids are selected based on the type of sample liquid. Preferably, this also includes an analytical apparatus in which the reducing agents having different concentrations are held in the reducing agent-feeding part, and the concentrations of the reducing agents are selected based on the type of sample liquid. The analytical apparatus of the present invention preferably includes a feeding means for the acid and diluting water located in the acid-feeding part, wherein the acid concentration is controlled by the relative portions of acid and diluting water fed into the reaction part. Likewise, an analytical apparatus of the present invention preferably provides for a feeding means for the reducing agent and diluting water, wherein the reducing agent concentration is controlled by the relative portions of reducing agent and diluting water fed into the reaction part.
The analytical apparatus of the present invention also preferably comprises a plurality of preliminary reducing agents held in the preliminary reducing agent-introducing part, and selected based on the types of sample liquids analyzed. The apparatus also preferably includes a control circuit for controlling integrally the actions of the sample-introducing part, the reagent-introducing part, the reaction part, the gas-liquid separating part and the detecting part. This control circuit permits the automation of operations extending from the introduction of th
Hayashibe Yutaka
Shimura Kazutoshi
Takeya Minoru
Ludlow Jan
Mitsubishi Materials Corporation
Oblon & Spivak, McClelland, Maier & Neustadt P.C.
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