Process for material preparation, apparatus therefor and...

Chemistry: analytical and immunological testing – Including sample preparation – Stabilizing or preserving

Reexamination Certificate

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C083S015000, C083S452000, C422S091000, C422S105000, C422S105000, C436S174000

Reexamination Certificate

active

06537826

ABSTRACT:

FIELD OF THE INVENTION
The present invention relates to a process and apparatus for material preparation and to a method for analysis therewith, by processing a material by forming a cut face and/or a rift therein, in particular, for preparing a sample which serves advantageously for analysis, observation, record or the like (in the following, denoted sometimes as analysis etc.). More particularly, the present invention relates to a process and apparatus for material preparation adapted especially to deal with materials which are subject to deformation, destruction and denaturing, including biological objects, organic and inorganic substances, chemical products and so on, as well as to a method for analysis therewith.
BACKGROUND OF THE INVENTION
For subjecting a material, especially among those, for example, biological bodies, such as plant seeds, and others, as a sample to a spectroanalysis, it is necessary to prepare a mirror-finished cut face of the material. On the other hand, for examining a sample by mass spectrometry by penetrating through the sample with a laser beam, the sample should be cut to form a slice of a specific thickness. For the device for preparing such a mirror-finished face of a sample by forming therein a cut face and/or a rift, a sliding cutter or a rotary cutter is used.
A sliding cutter operates by sliding a sharp blade and is adapted for slicing, for example, an animal tissue, such as liver, embedded in a soft substance, such as paraffin. However, the sliced tissue is apt to be deformed or destroyed by the pressure of the cutter blade. In particular, in the case of slicing a tissue, such as a stalk or a leaf, of a plant, which contains silica components, such as plant opal, the steel knife may be nicked by such silica and scars, such as knife marks, may be left on the resulting sliced sample.
A rotary cutter operates with a rotary cutting element, such as a diamond saw, which may encounter a similar disadvantage of deformation and destruction of the tissue by the cutter pressure as in the sliding cutter mentioned above, with a further defect that the cut sample is apt to suffer from denaturing due to the frictional heat upon cutting. For evading such a defect, cutting oil is used for the purpose of cooling and prevention of oxidation. In the case of a biological sample, cutting oil is absorbed in the cut sample easily and is detected upon the spectroanalysis as a contaminant component, reducing the analysis accuracy.
In both cutter arrangements, the material to be cut is fixedly held by embedding it in, for example, a paraffin wax or a resin, in order to immobilize the material upon cutting, which may cause also a decrease in the accuracy of the analysis by a possible interminglement of such holding material into the cut sample upon cutting.
A first object of the present invention is to provide a process for material preparation in which a material can be processed by forming a cut face and/or a rift therein while preventing deformation, destruction and denaturing of the material in a simple way using an apparatus of simple construction.
A second object of the present invention is to provide a process for material preparation in which a material can be processed by forming a cut face and/or a rift therein and preparing an examination surface at a predetermined position and at a definite angle of inclination while preventing deformation, destruction and denaturing thereof in a simple way, so as to obtain a sample to be examined by analysis, observation, recording or the like at a high accuracy, using an apparatus of simple construction.
A third object of the present invention is to provide a material preparing apparatus adapted for realizing such a material preparation as above.
DISCLOSURE OF THE INVENTION
The present invention resides in the following process and apparatus for performing the material preparation:
(1) A process for effecting preparation of a material, comprising
fixing the material on a holding unit,
freezing the material with dry ice, while replacing the gas-phase with the evolved carbon dioxide gas and
cutting the material by a cutter so as to form a cut face and/or a cut rift.
(2) The process as defined in the above (1), wherein the material is embedded in a filler filled in the holding unit and the filler is frozen in this state by dry ice to solidify, before the material is cut by the cutter.
(3) The process as defined in the above (1) or (2), wherein the cut surface, resulting after the cut face and/or the cut rift is formed by the cutter, is polished by the cutter to attain a mirror surface finishing.
(4) The process as defined in any one of the above (1) to (3), wherein the material is a sample for analysis, observation or recording.
(5) A material prepared by the process as defined in any one of the above (1) to (4).
(6) An apparatus for effecting material preparation comprising
a holding unit having one or more holders,
a settling means for settling the material held in the holder,
dry ice wells disposed so as to effect freezing of the material held in the holding unit and to effect a gas phase replacement and
a cutting space for permitting the cutting of the material by a cutter in a state frozen by dry ice with a gas phase replacement to form a cut face and/or a cut rift.
(7) The apparatus as defined in the above (6), wherein a plurality of the holders are arranged in a row.
(8) The apparatus as defined in the above (6) or (7), wherein it further comprises a mount which has a support for supporting the protruding portion of the material protruding from the holding unit and which is disposed on the holding unit disengageably.
(9) The apparatus as defined in the above (8), wherein the mount has an affixing means for affixing the cut off protruding portion.
(10) A method for effecting analysis, in which the material as defined in the above (5) is used as the sample.
The material to be subjected to the material preparation according to the present invention is processed by forming a cut face and/or a cut rift therein. For such a material, every one subject to deformation, destruction and denaturing may be mentioned, wherefor especially materials for samples for analyses etc. are particularly adapted.
Such a material may be those of biological, organic and chemical origins. Specific examples thereof include seeds, stalks, leaves and roots of plants and tissues of plants and animals including human beings. They may be those for use in applications other than a sample. Materials other than the above include, for example, materials for slicing a wafer from a silicon crystal, easily deformable textiles and others.
Such analysis, observation and others using a sample obtained by the material preparation may comprise every practice of analysis, observation, recording and so on to be carried out on the cut face or on the cut rift of the sample, including those in which mathematical processing is employed, such as for example, spectroanalyses using electromagnetic wave (including IR spectroscopy, Raman spectroscopy, X-ray fluorometry and chromatic differential spectrophotometry) and mass spectrometry, and further, those in which observation, determination and recording of an image is included, such as for example, microscopy (including electromicroscopy), TV-image analysis, photography, visual inspection and so on.
According to the present invention, such a material subject to deformation, destruction or denaturing is held on a holding unit and the material is frozen substantially instantaneously by dry ice while replacing the ambient atmosphere by carbon dioxide gas, whereupon the material is cut to form a cut face and/or a cut rift to effect the material preparation. Dry ice is a solid product of carbon dioxide produced by cooling and compressing carbon dioxide gas, for which a product having a grain size of 0.1-5 mm, preferably 0.1-2 mm, may be employed. It is enough to place dry ice at a portion capable of cooling and freezing the material and replacing the ambient atmosphere with carbon dioxide gas, while it is preferable to pla

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