JP2007240216A - Glass test piece for gas analysis, its manufacturing method, and gas analysis method in glass using it - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a glass test piece for gas analysis capable of opening a bubble in glass with high probability, and performing efficient gas analysis in the glass. <P>SOLUTION: This glass test piece 10 for gas analysis is a glass test piece for gas analysis involving the bubble 3, for analyzing a gas which forms the bubble 3, and is a glass test piece for gas analysis wherein at least one notch 2 whose tip part having a V-shaped section toward the bubble 3 is formed up to the periphery of the bubble 3. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a glass test piece for gas analysis used for analyzing a gas forming bubbles contained in a glass article, and a method for producing the same. Furthermore, it is related with the gas analysis method in the glass using the glass test piece for the gas analysis.

  In glass products, gas generated in the manufacturing process may remain as bubbles. A glass product in which bubbles remain may be a defective product depending on the application and the size of the bubbles. In order to reduce such bubbles, it is a common practice to analyze the gas constituting the bubbles, know the components, identify the cause of the bubbles in the glass production process, and take measures.

  In such an analysis, a gas test glass test piece containing bubbles is cut out from a glass product, the test piece is broken and the gas in the foam is taken out, and the gas is analyzed by an analyzer such as a gas chromatograph or a mass spectrometer. The analysis method is generally used.

  Examples of such bubble analysis methods are disclosed in the literature by Feile et al., Japanese Patent Application Laid-Open No. 9-189647 and Utility Model Registration No. 2574714.

  The literature by Feile et al. Discloses general methods for analyzing bubbles in glass.

In Japanese Patent Application Laid-Open No. 9-189647 and Utility Model Registration No. 2574714, a sample subjected to processing for destruction is installed in a destruction device provided with a plurality of sample stands, and needles, screws, etc. are used. And the method of analyzing the gas in a bubble by pressing and destroying a sample under ultra-high vacuum is disclosed.
R. Feile, A. Gotz, FW Kramer,: “Analysis of the Composition and Structure of Glass and Glass Ceramics”, ed. H. Bach and D. Krause, (Springer-Verlag, 1999) pp.451-460 JP-A-9-189647 Utility Model Registration No. 2574714

  A method for preparing a test piece for performing such an analysis is also presented in the literature by Feile et al. And Japanese Patent Laid-Open No. 9-189647. According to these, after cutting out a glass piece containing bubbles from a glass plate and polishing the bubbles so that they are as close to the sample surface as possible, as shown in FIG. In general, it was processed and used as a test piece for gas analysis. In this method, the groove 102 is cut into the glass sample so that the bubble 103 is located in the portion corresponding to the H-shaped horizontal bar, thereby forming the H-shaped glass test piece 101. By pressing the horizontal bar portion of the test piece with the needle 104, the test piece is broken and the gas in the foam is released. By introducing the released gas into the gas analyzer, the pressure, composition and amount can be measured.

  In this case, it is necessary to easily break the test piece by pressing the needle 104. If the test piece is too thick, it cannot be easily broken by pressing the needle. Furthermore, it is desirable that the bubble 103 be positioned in the vicinity of the surface of the glass test piece 101 in order to facilitate the release of the gas in the bubble.

  By the way, since the position where bubbles are generated is arbitrary in the plate thickness direction, the bubbles are not always positioned near the surface of the glass test piece. When bubbles are generated near the center in the thickness direction, the surface of the glass test piece 101 needs to be polished. This polishing step needs to be performed while confirming the position of the bubbles in the thickness direction.

  In addition, the size of the ultra-high vacuum container in the gas analyzer is often limited. In the case of a thick glass plate, even if bubbles are located in the vicinity of the surface of the glass test piece, the back side of the test piece needs to be polished in order to insert the test piece into the ultra-high vacuum container. That is, in the conventional H-shaped processing method, it takes a lot of time and labor to process the gas analysis test piece.

  Moreover, in the test piece for gas analysis disclosed in JP-A-9-189647 and the like, the shape of the tip toward the bubble in the groove is flat. Even if the groove is precisely processed, the shape of the tip is flat, so that the starting position of the crack that occurs when the test piece is broken and the direction in which the crack extends are difficult to determine. As a result, when the bubbles are very small, there are many cases where the gas in the target bubbles cannot be released when the sample is broken. As a result, the target gas analysis cannot be performed, and many precious samples may be wasted.

  The present invention is a glass test piece for gas analysis for analyzing a gas that encloses bubbles and forms bubbles, and at least a slit that has a V-shaped cross section at the tip toward the bubbles is provided at least near the bubbles. One formed glass specimen for gas analysis is provided.

  The present invention also relates to a method of manufacturing a glass test piece for gas analysis for analyzing a gas that forms bubbles by opening bubbles contained in a glass sample. A method for producing a glass test piece for gas analysis is provided, which includes a step of forming at least one notch having a V-shaped cross section at a tip end toward the surface.

  Further, the present invention provides the above glass test piece for gas analysis according to the present invention or the glass test piece for gas analysis obtained by the above method according to the present invention, by extending a crack starting from the notch tip to a bubble, There is provided a gas analysis method in glass for opening a bubble and taking out a gas forming the bubble and analyzing the gas.

  According to the present invention, since it is not necessary to precisely polish the surface of the glass test piece regardless of the bubble generation position and the plate thickness, it takes time to process the glass test piece more than the conventional H-shaped processing method. Time and effort can be reduced, and a large number of glass test pieces can be efficiently produced in a short time. Also, since the cross-section V-shaped tip toward the cut bubble is processed so as to be in the vicinity of the bubble, the gas in the bubble can be taken out with high probability by extending the crack starting from the V-shaped tip. Can do. Therefore, compared with the prior art, even if the contained bubbles are small, efficient gas analysis in glass becomes possible.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings. In the following description, the same members may be denoted by the same reference numerals, and redundant descriptions may be omitted.

  The cross-sectional shape of the glass test piece according to the present invention is shown in FIG. FIG. 1A is a cross-sectional view of a glass test piece 10 in which one notch 2 is formed up to the vicinity of the bubble 3. As in the glass test piece 20 of FIG. 1B, two notches 2 and 2 may be formed at positions facing each other with the bubble 3 interposed therebetween. The glass test pieces 10 and 20 include bubbles 3, and a notch 2 having a tip V-shaped cross section is formed up to the vicinity of the bubbles 3.

  1stly, an example of the manufacturing method of the glass test piece 10 is demonstrated below with reference to FIG. 2 and FIG. 3A-FIG. 3E.

  First, from a glass article containing bubbles, a portion including the bubbles 3 to be analyzed is cut out to an appropriate size to obtain a glass sample 11 before processing. Since it will be processed precisely later, it is preferable to cut out the pre-processed glass sample 11 at a certain size at this stage. As shown in FIG. 2A, this cutting is preferably performed so that the bubbles 3 are located on one side in the glass sample 11 before processing. This is in consideration of ease of handling in a later processing step and fixing the pre-processing glass sample 11 to a processing apparatus.

  Next, as shown in FIG. 2B, it is preferable to place a bubble position mark 6 so that the position where the bubble 3 is present can be grasped. For the marking, an oil-based ink pen, a glass pen, or the like can be used.

  For example, in the production of a glass plate by the float process, a molten glass is stretched in one direction and a continuous glass ribbon is appropriately cut. For this reason, the bubbles generated in the glass plate are often stretched to become an elliptical sphere. Therefore, it is desirable to extend the crack from the direction perpendicular to the long diameter of the bubble in order to reliably destroy the bubble during gas analysis and increase the probability of gas release. Therefore, it is preferable to cut the pre-processed glass sample 11 so that the major axis direction of the bubbles 3 is parallel to the short side direction of the pre-processed glass sample 11 as shown in FIG.

  Next, the cut glass sample 11 before processing is processed. An example of the processing procedure is shown in FIGS. 3A to 3E.

  First, the position of the bubble 3 is grasped from above the cut glass sample 11 before processing using a microscope or the like. For later analysis, measurement of the major axis and minor axis of the bubble 3 may be performed at this stage, and an image of the bubble 3 itself may be left. In that case, it is preferable to use an observation optical system for positioning that has a length measurement function or a photography function.

  First, a rotary table is incorporated in a processing machine, and as shown in FIG. 3A, an alignment XY stage 41 is installed on the rotary table, and the pre-processing glass sample 11 is fixed on the stage by a sample holder 42. . Using the center 43 of the rotary table as a reference point, the XY stage 41 is moved and adjusted so that the bubbles 3 in the glass sample 11 before processing coincide with this reference point. Reference numerals 46 and 47 in FIG. 3A denote the X-ray and Y-line of the XY stage 41, respectively.

  In addition, the bubble 3 has a magnitude | size, The example is demonstrated in detail about the case where this is considered by position alignment of the bubble 3 mentioned above. First, the visual field center of the above-described observation optical system is made to coincide with the center 43 of the rotary table. The XY stage 41 is moved and adjusted so that the bubble 3 comes to the center of the visual field. Further, the focus of the observation optical system may be adjusted to the maximum contour of the bubble 3, and finally the position of the bubble 3 may be finely adjusted so that the contour of the bubble 3 and the X-ray 46 of the XY stage 41 are in contact with each other. With this position as a reference, the pre-processed glass sample 11 may be cut into a predetermined dimension, or a notch with a tip having a V-shaped cross section may be inserted.

  Next, as shown in FIG. 3B, the rotary table is rotated 90 degrees clockwise, and is parallel to the X-ray 46 at a position away from the bubble 3 by a predetermined distance at the free end of the fixed glass sample 11. A certain first cutting line 12 is inserted, and unnecessary portions are cut off. The distance from the bubble 3 to the position of the first cutting line 12 is preferably adjusted according to the size of the bubble 3. The cut surface thus formed becomes the reference surface.

  Next, as shown in FIG. 3C, the rotary table is rotated 90 degrees counterclockwise to return to the positional relationship of FIG. 3A, and the Y line 47 from the cut surface 13 side on both sides away from the bubble 3 by a predetermined distance. First cut lines 14 and 14 that are parallel to each other are made.

  Further, the second cut line 15 is made along the Y line 47 toward the bubble 3 to form a cut having a V-shaped cross section at the tip (hereinafter sometimes referred to as “V-shaped cut”). Here, the V-shaped notch refers to a notch having a substantially V-shaped tip at a predetermined cross section. For example, by repeatedly forming a V-shaped cut, the cutting blade may be worn and the shape of the tip may be rounded. Even in this case, as long as stress concentrates on the front end of the cut and a shape that can be a generation source of a crack is maintained, the shape is substantially regarded as a V shape.

  At this time, the tip of the V-shaped notch is located at a position away from the bubble by a predetermined distance. It is preferable to adjust the distance between the V-shaped cutting tip and the foam according to the size of the foam. In addition, the distance here is the shortest distance between the V-shaped cutting tip and the bubble.

  Finally, as shown in FIG. 3D, the rotary table is rotated 90 degrees clockwise. A glass cutting piece 10 for gas analysis shown in FIG. 3E is obtained by putting a second cutting line 17 parallel to the X-ray 46 into the glass sample 16 in which the notch 2 having a V-shaped cross section at the tip is formed. . At this time, the position where the second cutting line 17 is inserted is a position away from the cutting surface 13 side toward the XY stage 41 by a predetermined distance. The distance from the cut surface 13 to the second cutting line 17 is preferably adjusted according to the size of the bubbles 3. At this time, you may cut off the glass sample after a process used as the glass test piece 10 completely. However, in consideration of ease of handling, a method may be adopted in which the glass test piece 10 is left in a partially attached state and is broken immediately before being installed in the analyzer. In addition, according to this method, corners (one) may remain in the glass test piece 10, but in the present specification, the shape in which the corners remain is substantially regarded as a rectangular parallelepiped as long as it is a rectangular parallelepiped as a whole. . A sectional view of the obtained glass test piece 10 is shown in FIG.

  2ndly, an example of the manufacturing method of the glass test piece 20 shown in FIG.1 (b) is demonstrated below with reference to FIG.2, FIG.5, FIG.6. Similar to FIG. 2 described above, first, a glass sample 21 before processing is obtained by cutting out a portion including the bubble 3 to be analyzed into an appropriate size from the glass article including the bubble 3 (see FIG. 5). In addition, when manufacturing this glass test piece 20, unlike the case of manufacturing the glass test piece 10 shown to Fig.1 (a), the short diameter direction of the bubble 3 is parallel to the short side direction of the glass sample 21 before a process. It is preferable that

  In this case, for fixing the glass sample 21 before processing, the center of the rotary table is used as a reference point, and the center of the bubble 3 in the glass sample 21 before processing is preferably matched with this reference point. First, a reference cut surface is formed at the first cutting line 22. Further, the first cut lines 24 and 24 and the second cut lines 25 and 25 shown in FIG. 5 are inserted while appropriately performing alignment and rotation of the rotary table. Finally, the second cutting line 27 is entered to obtain the glass test piece 20 shown in FIG. The first cut line 24 and the second cut line 25 may be formed in any order.

  As shown in FIG. 6, in the glass test piece 20, the V-shaped cuts 2 and 2 are formed so that the bubble 3 is located substantially at the center of the test piece and is opposed to the bubble 3.

  4 and 6, the distances f1 and f2 between the tip of the V-shaped cut 2 and the inner wall of the bubble 3 closest to the tip are preferably 0.01 to 1 mm. This is to ensure that the crack extending from the tip of the V-shaped notch 2 reaches the bubble 3 and the strength and ease of handling of the glass test pieces 10 and 20 after the V-shaped notch 2 is formed. It ’s something to consider.

  In consideration of performing the subsequent work accurately and easily, it is preferable that the outer shapes of the glass test pieces 10 and 20 are substantially rectangular parallelepipeds or cylinders. In order to cut the outer shape of the test piece into a cylinder, a glass core drill or the like may be used.

  In the processing step, an observation optical system capable of performing alignment or the like, a slicer provided with a rotary table, a dicing saw, or the like can be used.

  In addition, a process process is not restricted to said order. For example, a V-shaped cut 2 may be formed before the step shown in FIG. 3A. That is, the V-shaped cut 2 may be formed before the pre-processed glass sample 11 is cut into a predetermined shape.

  Next, an example of a method for releasing the gas in the bubbles 3 from the glass test piece 10 obtained in the above process and analyzing the gas will be described with reference to FIGS.

  First, as shown to Fig.7 (a), a part P1 of the glass test piece 10 obtained at the said process is fixed to the jig | tool 51 by a cantilever type. At this time, a part P1 of the glass test piece 10 is fixed so that the jig 51 does not hold the portion of the glass test piece 10 containing the bubbles 3. The material and shape of the jig 51 are not limited as long as the glass test piece 10 can be held in a cantilever manner.

  When analysis of residual bubbles in a glass article is performed using an analyzer such as a gas chromatograph or a mass spectrometer, the jig 51 is usually installed in a container that can be maintained in an ultrahigh vacuum. After fixing a part P1 of the glass test piece 10 to the jig 51 in a cantilever manner, the inside of the container is put into an ultrahigh vacuum.

  In this state, the upper surface of the part P2 on the opposite side of the part P1 fixed by the jig 51 is pressed by the push bar 52 in the direction in which the V-shaped cut 2 is inserted. Then, stress concentrates on the tip of the V-shaped cut 2, the crack 53 extends from the tip, and the crack 53 reaches the bubble 3. Thereby, the gas in the bubble 3 is released. A cross-sectional view of the glass test piece 10 at this time is shown in FIG. As shown in the figure, the glass test piece 10 may be completely broken starting from the tip of the V-shaped cut 2.

  In order to release the bubbles, as described above, when the two portions sandwiching the notch of the glass test piece are P1 and P2, respectively, P1 is fixed, a load is applied to P2, and the V-shaped It is preferable to extend the crack starting from the notch tip.

  As shown in FIG. 8, a vacuum vessel 31 containing a glass test piece breaking device having a jig or a push-in bar is connected to a gas analyzer 32, and a vacuum pump 33 is used to form an ultrahigh vacuum inside the vacuum vessel 31. When the gas in the foam is released in the state, the released gas is sent to the gas analyzer 32 and the composition and content thereof can be analyzed. 7A shows an example in which one glass test piece 10 is fixed to one jig. However, a plurality of glass test pieces can be fixed in advance, and the glass test pieces are automatically replaced and broken in order. It is also possible to use such a jig.

  The surface newly generated by the breakage of the glass specimen is physically and chemically active. Therefore, the gas released from the inside of the bubbles may be adsorbed on the newly generated surface of the glass test piece and affect the analysis result. Therefore, the area of the surface of the glass test piece newly generated by breakage should be as small as possible.

  In the conventional H-shape processing, when the bubble diameter to be analyzed is 0.1 to 0.2 mm or less, the probability that the gas in the bubble can be released has been extremely reduced. In fact, when trying to analyze 20 bubbles (bubble diameter is distributed in the range of 0.1 to 0.4 mm) by the H-shaped processing method, there is an example that 10 of them failed. This is because the corner portion of the H-shaped groove becomes the starting point of the crack, and the generated crack extends in a direction completely unrelated to the bubbles. For this reason, in order to generate a crack at an intended location and extend it, a V-shaped notch that intentionally creates a portion where stress is concentrated is preferable.

  Actually, a glass test piece formed with a V-shaped cut was fixed in a cantilever manner, and a cross-section was broken by applying a load to the opposite side across the holding side and the V-shaped cut. The elongation angle of the crack was measured. FIG. 9 shows a conceptual diagram thereof. FIG. 9 shows a cross section set so that the tip of the V-shaped cut 2 has a V-shaped cross section, and the shortest distance f between the tip P of the V-shaped cut 2 and the bubble 3 appears.

  In FIG. 9, a <b> 1 and a <b> 2 are two first tangents and second tangents drawn from the tip P of the V-shaped cut 2 to the bubble 3, respectively. b1 is a crack extension line indicating the extension direction of the generated crack. c is a line obtained by extending the bisector of the angle formed by the V shape in the direction of the bubble 3.

  Here, an angle formed by the first tangent line a1 and the second tangent line a2 is defined as an angle A1. Further, the target line of the crack extension line b1 with the line c as the axis of symmetry is set as b2, and the angle formed between the crack extension line b1 and the target line b2 is set as an angle B1. The angle B1 is an angle twice the angle formed between the crack extension line b1 and the line c, and represents a range in which the crack may be extended.

  The angle A2 is an angle formed by the first tangent line a1 and the line c, and the angle A3 is an angle formed by the second tangent line a2 and the line c. The angle B2 is an angle formed by the crack extension line b1 and the line c, and the angle B3 is an angle formed by the target line b2 and the line c of the crack extension line b1.

  Here, if the angle A1 is set to be equal to or larger than the angle B1 (A1 ≧ B1), the bubbles 3 always exist within a range in which the crack may be extended. This angle A1 is determined by the shortest distance f between the V-shaped cutting tip P and the bubble 3. In order to determine the appropriate angle A1, it is necessary to know the degree of dispersion of the angle B2, which is the crack extension angle.

  Therefore, 77 samples were actually broken and the distribution of the angle B2 was measured. The results are shown in Table 1.

(Table 1)
―――――――――――――――――――――――――――
Crack elongation angle B2 Number ratio (%)
0 ° or more and less than 5 ° 29 37.7
5 ° or more and less than 10 ° 27 35.1
10 ° or more and less than 15 ° 9 11.7
15 ° or more and less than 20 ° 7 9.1
20 ° or more and less than 25 ° 3 3.9
25 ° or more and less than 30 ° 2 2.6
―――――――――――――――――――――――――――
Total 77 100.0
―――――――――――――――――――――――――――

  As can be seen from Table 1, the crack extension angle range was less than 30 ° in all the samples. From this result, if the angles A2 and A3 are both 30 ° or more, the gas in the bubbles 3 can be released with a probability of 100%. Therefore, it is preferable to form the V-shaped cut 2 so that the angles A2 and A3 are both 30 ° or more.

  In addition, it turns out that it is preferable from the above examination that the center of a bubble exists on the notch centerline (the line c which extended the bisector of the angle | corner which a V shape makes) in the direction of a bubble. . At the time of processing, as detailed in the description of FIG. 3A, it is important to match the position of the bubble with the center of the rotary table.

  FIG. 10 shows the relationship between the angle A1 and the shortest distance (f in FIG. 9) between the V-shaped cutting tip P and the bubble 3 with respect to various bubble diameters (g in FIG. 9). The bubble 3 was assumed to be spherical. A1 = A2 + A3. From FIG. 10, if the shortest distance f between the V-shaped cutting tip P and the bubble 3 is set to 50 μm, bubbles with a bubble diameter g of 100 μm or more can release the gas in the bubble with a probability of almost 100%. I understand. Similarly, when f is set to 100 μm, it can be seen that bubbles having a bubble diameter g of 200 μm or more can release the gas in the bubbles with a probability of almost 100%.

  Furthermore, the shortest distance f may be determined in consideration of the probability of releasing the gas in the bubble derived from the relationship between the size g of the bubble 3 and the angle A1, the ease of processing in the glass test piece, and the ease of handling. . In the case of a slicer or dicing saw having normal accuracy, the shortest distance f can be easily set to about 100 μm.

  Regarding the shortest distance f, the probability that the gas in the bubble 3 can be released varies depending on the size of the target bubble 3, but is preferably 500 μm or less, more preferably 240 μm or less, still more preferably 100 μm or less, and 50 μm or less. Most preferably. From the viewpoint of ease of processing and handling in the test piece, 10 μm or more is necessary, 20 μm or more is preferable, and 50 μm or more is more preferable.

  In the above description, the bubble 3 is assumed to be spherical. Actual bubbles are often stretched as described above. Depending on the size of the bubble, if the V-shaped cut 2 is formed so as to be orthogonal to the long diameter of the bubble 3, a good gas release probability is ensured even when the shortest distance f exceeds 500 μm. be able to.

  Thus, by considering the handling and the like as much as possible, by making the shortest distance as small as possible, in the present invention, the analysis efficiency of bubbles can be greatly increased as compared with the conventional H-shaped processing.

  By this invention, it becomes possible to manufacture efficiently the glass test piece for the gas analysis of the bubble in a glass article. In addition, when analyzing the gas in the foam using the glass test piece, the gas in the foam can be taken out with high probability, so that valuable samples can be used effectively and the obtained data is analyzed. Thus, it can be used for improving the bubble quality of the glass article.

It is sectional drawing of the glass test piece for gas analysis by this invention. It is the perspective view and top view of a glass sample before a process. It is a figure which shows the first process in an example of the processing method of the glass sample before a process. It is a figure which shows the process of following FIG. 3A. It is a figure which shows the process of following FIG. 3B. It is a figure which shows the process of following FIG. 3C. It is a figure which shows the glass test piece obtained through the process of FIG. 3A-FIG. 3D. It is sectional drawing of the glass test piece in which only one V-shaped cut was formed. It is a conceptual diagram explaining the process of forming two V-shaped notches in a glass test piece. It is sectional drawing of the glass test piece in which two V-shaped cut | notches were formed in the position which opposes on both sides of the bubble. It is a figure which shows an example of the fracture | rupture method of a glass test piece. It is a figure which shows the gas analysis method. It is a conceptual diagram explaining the relationship between the V-shaped cut | incision, the geometric arrangement | positioning of a bubble, and the range of the elongation angle of a crack. It is the figure which showed the relationship between the shortest distance f and angle A1 with respect to the diameter g of various bubbles. It is a figure which shows the shape (H shape) of the conventional glass test piece for gas analysis.

Explanation of symbols

10: Glass specimen for gas analysis in which only one V-shaped cut is formed 11: Glass sample 12 before processing 12: First cutting line 13: Cut surface 14: First cutting line 15: Second cutting line 16: Glass sample 17 during processing: second cutting line 20: glass specimen for gas analysis in which two V-shaped cuts are formed 21: glass sample 22 before processing 22: first cutting line 24: first cutting line 25: Second cut line 27: Second cut line 2: V-shaped cut 3: Bubble 6: Bubble position mark 31: Vacuum container 32: Gas analyzer 33: Vacuum pump 41: XY stage 42: Sample holder 43: Rotating stage Center 46: XY stage X-ray 47: XY stage Y-line 51: Glass specimen fixing jig 52: Push rod 53: Crack 101: Conventional glass specimen 102: Cut 103: Bubble 104: Needle a : First tangent a2 drawn from the tip of the V-shaped cut to the bubble a2: second tangent b1 drawn from the tip of the V-shaped cut to the bubble b1: crack extension line b2: target line of the crack extension line c: V-shape Lines f, f1, f2 obtained by extending the bisector of the angle formed by the mold in the direction of the bubble: Shortest distance between the tip of the cut and the bubble g: Bubble diameter P: Tip of the V-shaped cut

Claims (15)

A glass specimen for gas analysis for enclosing bubbles and analyzing the gas forming the bubbles,
A glass test piece for gas analysis in which at least one notch having a V-shaped cross section at the tip toward the bubble is formed up to the vicinity of the bubble.   The glass test piece for gas analysis according to claim 1, wherein only one notch is formed.   The glass test piece for gas analysis according to claim 1, wherein two notches are formed at positions facing each other with the bubble interposed therebetween.   The glass test piece for gas analysis according to any one of claims 1 to 3, wherein a distance between the tip of the cut and the bubble is 0.01 to 1 mm.   The glass test piece for gas analysis according to any one of claims 1 to 4, wherein the cut is formed in a glass sample whose outer shape is substantially a rectangular parallelepiped or a cylinder. Assuming two tangent lines drawn from the tip to the bubble in the cross section where the shortest distance between the tip of the cut and the bubble appears, an extension of the bisector of the angle formed by the V-shape in the cross section When drawing a line in the direction of the bubble,
6. The notch is formed so that the extension line exists between the two tangent lines, and the respective angles between the two tangent lines and the extension line are 30 ° or more. The glass test piece for gas analysis of any one of these. A method for producing a glass test piece for gas analysis for analyzing a gas forming a bubble by opening bubbles contained in a glass sample,
A method for producing a glass specimen for gas analysis, comprising the step of forming at least one notch having a V-shaped cross-section at a tip end toward the bubble in the glass sample up to the vicinity of the bubble.   The manufacturing method of the glass test piece for gas analysis of Claim 7 which forms only the said notch | incision.   The manufacturing method of the glass test piece for gas analysis of Claim 7 which forms the said two notches in the position which opposes on both sides of the said bubble.   The method for producing a glass test piece for gas analysis according to any one of claims 7 to 9, wherein the cut is formed such that a distance between the tip of the cut and the bubble is 0.01 to 1 mm. .   The gas analysis according to any one of claims 7 to 10, further comprising a step of identifying bubbles to be analyzed in a glass article containing bubbles and cutting out the glass sample containing the bubbles to be analyzed from the glass article. Method for manufacturing glass test pieces.   The manufacturing method of the glass test piece for gas analysis of Claim 11 which cuts out the said glass sample so that the external shape of the said glass sample may become a rectangular parallelepiped or a cylinder substantially. Assuming two tangent lines drawn from the tip to the bubble in the cross section where the shortest distance between the tip of the cut and the bubble appears, an extension of the bisector of the angle formed by the V-shape in the cross section When drawing a line in the direction of the bubble,
The extension line exists between the two tangent lines, and the notch is formed by setting the shortest distance so that each angle between the two tangent lines and the extension line is 30 ° or more. The manufacturing method of the glass test piece for gas analysis of any one of Claims 7-12 to do. In the glass test piece for gas analysis according to any one of claims 1 to 6, or the glass test piece for gas analysis obtained by the method according to any one of claims 7 to 13,
A method for analyzing gas in glass, in which a crack starting from the tip of the notch is extended to the bubble, the bubble is released to extract a gas forming the bubble, and the gas is analyzed.   15. When two portions of the glass test piece sandwiching the notch are defined as P1 and P2, respectively, the P1 is fixed, a load is applied to the P2, and a crack starting from the tip is extended. The gas analysis method described in 1.

Images