Measuring and testing – Liquid analysis or analysis of the suspension of solids in a... – Content or effect of a constituent of a liquid mixture
Reexamination Certificate
2001-03-02
2003-12-30
Larkin, Daniel S. (Department: 2856)
Measuring and testing
Liquid analysis or analysis of the suspension of solids in a...
Content or effect of a constituent of a liquid mixture
C073S061530, C073S061550, C073S061560, C073S061580, C210S635000, C210S656000, C210S198200, C422S070000, C436S086000, C436S161000, C436S177000, C436S178000
Reexamination Certificate
active
06668623
ABSTRACT:
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method and an apparatus for analyzing an organic macromolecular component in a solution based on a flow analysis method and to applications thereof. In particular, the present invention relates to an analytical method and an apparatus suitable for quantitatively analyzing very small amounts of glues or gelatins contained in metallic electrolytic solutions, such as copper electrolytic solutions and plating solutions.
2. Description of the Related Art
Various additives are added to electrolytic solutions and plating solutions in accordance with various purposes of improving brightness and smoothness of electrodeposited metal surfaces, hardening plated layers, etc. As the additive, in general, glues are used in electrolytic smelting and gelatins are used in plating. Herein, it is very important in quality control to keep concentrations thereof within specified ranges. For example, although glues are used for improving smoothness of electrodeposited surfaces, when concentrations thereof are too high, polarization is increased to a great degree so that there are problems of deposition of impurities, such as bismuth, contained in the electrolytic solutions, etc.
Therefore, a method for analyzing proteins, such as glues or gelatins, contained in solutions with a high degree of precision has been required. Most of conventional methods for analyzing proteins are performed under from weakly acidic to weakly basic conditions, and there are few analytical methods which can be applied under strongly acidic conditions of pH 1 or less, as in electrolytic solutions, plating solutions, etc. Hitherto, proteins, such as glues or gelatins, contained in electrolytic solutions, plating solutions, etc., have been measured by potentiometric titration, Kjeldahl method, etc., although specific apparatuses and complicated operations have been required in those cases. In the Kjeldahl method, glues are measured after being decomposed into nitrogen in a state of ammonia, although in many cases, nitrogen compounds other than proteins are contained in the electrolytic solutions so as to make precise measurements difficult.
In addition, as a quantitative method for analyzing gelatins and glues in the strongly acidic solution, a method in which those are collected on membrane filters, are bonded with a specific reagent (Amide Black 10B coloring matter), and after excess coloring matters are washed out, the coloring matters are eluted so as to determine gelatins, etc., (Japanese Unexamined Patent Application Publication No. 2-69660), a method in which after gelatins, etc., have been collected on a filter, the resulting filter is dried so as to determine gelatins, etc., based on reflectance (Japanese Unexamined Patent Application Publication No. 6-337247), etc., are reported. Regarding these methods, there are, however, problems that an amount of collected glues is much affected by pore diameters of the filter so as to increase measurement errors, a filtering apparatus for collecting with the filter is required and operations are complicated, and the analytical cost is increased due to disposable filters.
SUMMARY OF THE INVENTION
The present invention has solved the aforementioned problems in conventional analytical methods. It is an object of the present invention to provide a flow analysis method and an apparatus, thereby organic macromolecular components, such as glues and gelatins, in a solution can be promptly and precisely determined even in a strongly acidic solution.
The present invention is due to the completion of a system for measurement with a high degree of reliability and with ease of handling, in which operations of separating organic macromolecular components in a solution by adsorption on a resin, leading these to a gel permeation chromatograph, and analyzing are performed based on the flow analysis.
That is, the present invention relates to the following flow analysis method for separating and analyzing an organic macromolecular component in a sample.
(1) A method for analyzing an organic macromolecular component based on a flow analysis method with a measuring system including a sample introducing section, a preparing section, and a measuring section, composed of steps of supplying a sample with a carrier solution into the measuring system through the introducing section, leading the sample to the preparing section and separating an organic macromolecular component in the sample, and leading the separated organic macromolecular component to the measuring section and analyzing. Herein, the step of separating the organic macromolecular component includes steps of the organic macromolecular component in the sample being adsorbed on a resin and introducing an eluant into the preparing section and eluting the organic macromolecular component adsorbed on the resin.
(2) A method of analysis according to the aforementioned method (1), further composed of the steps of supplying the sample into the measurement system through the introducing section while a pipeline for feeding the sample from the introducing section to the preparing section and a pipeline for discharging a solution from the preparing section out of the measurement system are communicated with the preparing section, leading the sample to the preparing section, the organic macromolecular component in the sample being adsorbed on the resin in the preparing section while leading the solution discharged from the preparing section out of the measurement system, switching pipelines communicating with the preparing section so that a pipeline for supplying the eluant and a pipeline connected to the measuring section communicate with the preparing section, introducing the eluant into the preparing section so as to elute the organic macromolecular component adsorbed on the resin, and leading the resulting solution containing the organic macromolecular component to the measuring section and analyzing.
(3) A method of analysis according to the aforementioned method (1), in which the eluant is used after a buffer solution for preventing the organic macromolecular components from coagulating is added thereto or the buffer solution is added to the solution containing the organic macromolecular component between the preparing section and the measuring section.
(4) A method of analysis according to the aforementioned method (1) or (2), in which gel permeation chromatography is used as an analyzing device so as to fractionate and analyze the organic macromolecular component separated from the sample.
(5) A method of analysis according to the aforementioned method (1) or (2), in which an amount of glues or gelatins separated from the sample or an amount of decomposition products thereof is measured.
(6) A method of analysis according to the aforementioned method (1) or (2), in which gel permeation chromatography is used as an analyzing device so as to fractionate glues or gelatins separated from the sample and to measure the amount thereof or an amount of decomposition products thereof.
(7) A method of analysis according to the aforementioned method (1) or (2), in which an acid-proof and hydrophobic adsorption resin is used as a resin for adsorbing the organic macromolecular component in the sample.
(8) A method of analysis according to the aforementioned method (1) or (2), in which an electrolytic solution taken from a step of metallic electrolysis or a plating solution taken from a step of plating is used as a sample solution.
(9) A method for controlling a step of metallic electrolysis with a method of analysis according to the aforementioned method (1) or (2), in which the method of analysis is further composed of steps of taking a sample solution from an electrolytic solution in the step of metallic electrolysis, measuring an amount of glues or gelatins separated from the sample of the electrolytic solution or an amount of decomposition products thereof, and feeding back the analytical results of the measurement to the step of metallic electrolysis.
(10) A method
Hayashibe Yutaka
Kato Masaaki
Takeya Minoru
Tani Michiko
Larkin Daniel S.
Mitsubishi Materials Corporation
Oblon & Spivak, McClelland, Maier & Neustadt P.C.
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