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
2001-03-30
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
C073S061550, C073S061560, C073S061580, C422S068100, C422S070000, C436S086000, C436S161000, C436S178000
Reexamination Certificate
active
06668624
ABSTRACT:
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method and an apparatus for analyzing organic macromolecular components in a solution based on a flow analysis method, and relates 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. Discussion of the Background
Additives are added to electrolytic solutions and plating solutions for various purposes, such as improving brightness and smoothness of electrodeposited metal surfaces, hardening plated layers, etc. Generally, glue additives are used in electrolytic smelting, and gelatins are used in plating. Herein, for quality control, it is very important to keep concentrations thereof within specified ranges. For example, although glues are used for improving the smoothness of electrodeposited surfaces, when concentrations thereof are too high polarization is increased to such a great degree that there are problems with 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 the conventional methods for analyzing proteins are performed under conditions being from weakly acidic to weakly basic, and there are few analytical methods which can be applied under strongly acidic conditions of a 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 a potentiometric titration, the Kjeldahl method, etc., although specific apparatuses and complicated operations have been required in those cases. In the Kjeldahl method, glues are measured after the nitrogen in the glues is converted into 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 a strongly acidic solution, a method in which gelatins and glues 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); and a method in which after gelatins, etc., are 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 in that the amount of collected glues is greatly affected by pore diameters of the filter so as to increase measurement errors. A filtering apparatus for collecting with a filter and complicated operations therefor are required, and the analytical cost is increased due to the disposable filters.
SUMMARY OF THE INVENTION
The present invention has solved the aforementioned problems in the conventional analytical methods. Accordingly, the present invention provides a flow analysis method and an apparatus by which organic macromolecular components such as glues and gelatins in solutions can be promptly and precisely quantified even in strongly acidic solutions.
The present invention resides in the completion of a measurement system with a high degree of reliability and with handling ease, in which the operations of separating an organic macromolecular component in a solution by adsorption on a resin, leading this to a gel permeation chromatograph, and analysis are performed based on the flow analysis.
That is, the present invention relates to the following flow analysis methods for separating and analyzing an organic macromolecular component in a sample.
According to a first aspect of the present invention, a method for analyzing an organic macromolecular component based on a flow analysis method with a measurement system including a sample introduction section, a preparation section, and a measuring section, includes the steps of supplying a sample together with a carrier solution into the measurement system through the introduction section, leading the sample to the preparation section and separating the organic macromolecular component in the sample, and leading the separated organic macromolecular component to the measuring section for analysis. Herein, the step of separating the organic macromolecular component includes the steps of adsorbing the organic macromolecular component in the sample on a resin and introducing an eluant solution into the preparation section and eluting the organic macromolecular component adsorbed on the resin.
Preferably, the method of analysis may further include the steps of supplying the sample into the measurement system through the introduction section while a pipeline for feeding the sample running from the introduction section to the preparation section and a pipeline for discharging the solution running from the preparation section to the outside of the measurement system are connected to the preparation section; and leading the sample to the preparation section, where the organic macromolecular component in the sample is adsorbed on the resin in the preparation section, and leading the discharged solution from the preparation section to the outside of the measurement system. Switchable pipelines are connected to the preparation section so that a pipeline for supplying the eluant solution and a pipeline connected to the measuring section are connected to the preparation section, introducing the eluant solution into the preparation 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 for analysis.
Preferably, the method of analysis may further include the steps in which the eluant solution is used after a buffer solution to prevent 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 preparation section and the measuring section.
Preferably, the method of analysis may further include the step in which a gel permeation chromatography is used as an analyzing device so as to fractionate and analyze the organic macromolecular component separated from the sample.
Preferably, the method of analysis may further include the step in which an amount of glues or gelatins is separated from the sample, or amounts of decomposition products thereof are measured.
Preferably, the method of analysis may further include the step in which a gel permeation chromatography is used as an analyzing device in the measuring section so as to fractionate glues or gelatins separated from the sample and to measure the amount thereof or the amounts of decomposition products thereof.
Preferably, the method of analysis may further include the step in which an acid-proof and hydrophobic adsorption resin is used as a resin for adsorbing the organic macromolecular component in the sample.
Preferably, the method of analysis may further include the step 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.
Preferably, the method for controlling a metallic electrolysis process with the method of analysis may further include the steps of taking a sample solution from an electrolytic solution in the step of metallic electrolysis, measuring the amount of glues or gelatins separated from the sample of the electrolytic solution or amounts of decomposition products thereof, and feeding the results of the measurement back to the step of m
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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