Abstract
A glass container is provided having a glass tube with a first end and a second end and a glass bottom closing the second end. The glass tube has a longitudinal axis and has, in a direction from the first to the second end, a top region, a junction region, a neck region, a shoulder region, and a body region. The top region is at the first end and has an outer diameter (d.sub.t), the neck region has an outer diameter (d.sub.n) with d.sub.n<d.sub.t, the body region extends to the second end and has an outer diameter (d.sub.b) with d.sub.b>d.sub.t, and the glass tube in the body region has a thickness (l.sub.b). The outer contour in a transition area between the top and neck regions is defined by a radius of curvature. The glass containers have a neck squeeze test load of at least 1100 N.
Claims
1. A glass container, comprising: a glass tube with a first end, a second end, and a longitudinal axis L.sub.tube therebetween, the glass tube has an outer surface and, in a direction from the first end to the second end, a top region, a junction region, a neck region, a shoulder region, and a body region, wherein the top region is at the first end and has an outer diameter (d.sub.t), the neck region has an outer diameter (d.sub.n) with d.sub.n<d.sub.t, the body region extends to the second end and has an outer diameter (d.sub.b) with d.sub.b>d.sub.t, and the glass tube in the body region has a thickness (l.sub.b); and a glass bottom closing the glass tube at the second end, wherein, when an outer surface of the body region is placed on a plane horizontal substrate, within a cross-section of the glass container that is located in a plane centrically located in the glass container and comprising the longitudinal axis L.sub.tube, f(x) defines a distance between the plane horizontal substrate and the outer surface of the glass tube at a position x and l(x) defines a thickness of the glass tube at the position x, wherein the thickness of the glass tube l(x) is measured for the position x in a direction perpendicular to the longitudinal axis L.sub.tube, wherein k(x)=|f″(x)/[1+f′(x).sup.2].sup.3/2| defines an absolute value of a curvature of f(x) at a given position x; and wherein, in an interval between x=P.sub.1 and x=P.sub.2 for a concave curvature in the interval between x=P.sub.1 and x=P.sub.2, a minimum value for [l(x)/l.sub.b].sup.3/k(x) is at least 0.35 mm, wherein P.sub.2 defines the x-position at which f(x) is ½×d.sub.b−¼×d.sub.t−¼×d.sub.n and P.sub.1 is P.sub.2−d.sub.t/2+d.sub.n/2.
2. The glass container of claim 1, wherein the junction region has another outer surface where the junction region merges into the neck region that is substantially circular arc-shaped, the substantially circular arc-shaped area having an outer radius r.sub.s, wherein the glass tube has a minimum thickness l.sub.n in the neck region, and wherein 2×[l.sub.n/l.sub.b]×r.sub.s≥0.9 mm.
3. The glass container of claim 2, wherein the glass container is a vial having an interior volume of 1 to 8 ml, and d.sub.n≥9.7 mm, and r.sub.s≥0.5 mm.
4. The glass container of claim 3, wherein the vial has a size designation “2R” or “4R” according to DIN EN ISO 8362-1:2016-06.
5. The glass container of claim 2, wherein the glass container is a vial with an interior volume of 8.5 to 22 ml, d.sub.n≥15.5 mm, and r.sub.s≥0.5 mm.
6. The glass container of claim 5, wherein the vial has a size designation “6R”, “8R” or “10R” according to DIN EN ISO 8362-1:2016-06.
7. The glass container of claim 2, wherein the glass container is a vial with an interior volume of 22.5 to 150 ml, d.sub.n≥16.5 mm, and r.sub.s≥0.5 mm.
8. The glass container of claim 7, wherein the vial has a size designation “20R”, “25R”, “30R”, “50R” or “100R” according to DIN EN ISO 8362-1:2016-06.
9. The glass container of claim 2, wherein l.sub.n/l.sub.b≥1.4.
10. The glass container of claim 2, wherein l.sub.n×r.sub.s/l.sub.b≥0.7 mm.
11. The glass container of claim 1, further comprising a pharmaceutical composition in an interior volume of the glass tube and a closure closing the glass tube at the first end.
12. The glass container of claim 1, wherein the shoulder region has a shoulder angle α and wherein the shoulder angle α is in the range from 10° to 70° .
13. A plurality of glass containers, comprising: each glass container having a glass tube with a first end and a second end and having a glass bottom closing the glass tube at the second end, wherein the glass tube has an outer surface, a longitudinal axis L.sub.tube and has, in a direction from the first end to the second end, a top region, a junction region, a neck region, a shoulder region, and a body region, wherein the top region is at the first end and has an outer diameter (d.sub.t), the neck region has an outer diameter (d.sub.n) with d.sub.n<d.sub.t, the body region extends to the second end and has an outer diameter (d.sub.b) with d.sub.b>d.sub.t, and the glass tube in the body region has a thickness (l.sub.b), and wherein at least 75% of the glass containers in the plurality of glass containers fulfil a condition comprising: when an outer surface of the body region is placed on a plane horizontal substrate, within a cross-section of the glass container that is located in a plane centrically located in the glass container and comprising the longitudinal axis L.sub.tube, f(x) defines a distance between the plane horizontal substrate and the outer surface of the glass tube at a position x and l(x) defines a thickness of the glass tube at the position x, wherein the thickness of the glass tube l(x) is measured for the position x in a direction perpendicular to the longitudinal axis L.sub.tube, wherein k(x)=|f″(x)/[1+f′(x).sup.2].sup.3/2| defines an absolute value of a curvature of f(x) at a given position x; and wherein, in an interval between x=P.sub.1 and x=P.sub.2 for a concave curvature in the interval between x=P.sub.1 and x=P.sub.2, a minimum value for [l(x)/l.sub.b].sup.3/k(x) is at least 0.35 mm, wherein P.sub.2 defines the x-position at which f(x) is ½×d.sub.b−¼×d.sub.t−¼×d.sub.n and P.sub.1 is P.sub.2−d.sub.t/2+d.sub.n/2.
14. The plurality of glass containers of claim 13, wherein at least 75% of the glass containers in the plurality of glass containers fulfil a condition comprising: the junction region has another outer surface where the junction region merges into the neck region that is substantially circular arc-shaped, the substantially circular arc-shaped area having an outer radius r.sub.s, wherein the glass tube has a minimum thickness l.sub.n in the neck region, and wherein 2×[l.sub.n/l.sub.b]×r.sub.s≥0.9 mm.
15. The plurality of glass containers of claim 13, wherein each of the glass containers in the plurality of glass containers further comprise a pharmaceutical composition in an interior volume of the glass tube and a closure closing the glass tube at the first end.
Description
BRIEF DESCRIPTION OF THE FIGURES
(1) Unless otherwise specified in the description or the particular figure:
(2) FIG. 1 shows the set-up of a side compression test known from the prior art;
(3) FIG. 2 shows in a cross-sectional view the different regions of a glass container 100 according to the invention;
(4) FIG. 3 shows in an enlarged cross-sectional view the top region 104, the junction region 105, the neck region 106 and the shoulder region 107 of a glass container 100 according to the invention;
(5) FIG. 4A shows in an enlarged cross-sectional view the determination of the outer contour c.sub.outer of the top region 104, the junction region 105, the neck region 106 and the shoulder region 107 of a glass container 100 according to the invention;
(6) FIG. 4B shows the course of the function f(x) within the range from P.sub.1 to P.sub.2 that describes the outer contour c.sub.outer in the transition area between the top region and the neck region;
(7) FIG. 5A shows in a side view the localization of plane 111 that is used to determine the local curvature of function f(x) as well as the glass thickness l(x) within the range from P.sub.1 to P.sub.2;
(8) FIG. 5B shows in a top view the localization of plane 111 that is used to determine the local curvature of function f(x) as well as the glass thickness l(x) within the range from P.sub.1 to P.sub.2;
(9) FIG. 6 shows the determination of r.sub.s;
(10) FIG. 7 is further a cross-sectional view of a glass container 100 according to the invention showing a shoulder angle α;
(11) FIG. 8 illustrates the process 1 according to the invention for the preparation of a glass container;
(12) FIG. 9 shows a flow chart of process 2 according to the invention for packaging a pharmaceutical composition;
(13) FIG. 10 shows the set-up of the neck squeeze test;
(14) FIG. 11A is a schematic side view of the neck squeeze test;
(15) FIG. 11B is a schematic front view of the neck squeeze test.
DETAILED DESCRIPTION
(16) FIG. 1 shows the set-up of a side compression test known from the prior art. As can be seen, the glass container 100 with a glass bottom 109 is placed in a horizontal position sandwiched between two steel plates 117,118 by means of which a compressive force is applied in diametral (radial) direction at two opposing positions of the vial body outer surface geometry. The compressive force is increased at a constant load rate of 1500 N/min until breakage of the container using a universal testing machine. The diametral load is applied by two opposing, uniaxial concave steel surfaces 117, 118, between which the body region 109 of the vial 100 is placed parallel to the axis L.sub.tube. One of the concave surfaces 117 is constructed to be self-adjusting to be able to compensate geometrical irregularities. The radius of the concavity of the two steel surfaces 117,118 is 25% larger than the radius of the outer diameter d.sub.b of the body region, so that the load is applied along two opposing lines. The width of the concave steel surfaces is chosen to be larger than the height of the vial body region 108. As can also be seen in FIG. 1, neither the top region 104 nor the junction region 105 or the neck region 106 come into contact with the clamping jaws 117,118 as d.sub.t (the diameter of the top region 104) and d.sub.n (the diameter of the neck region 106) are smaller than d.sub.b (the diameter of the body region 108).
(17) FIG. 2 shows in a cross-sectional view the different regions of a glass container 100 according to the invention. The glass container 100 comprises as container parts a glass tube 101 with a first end 102 and a further end 103 and a glass bottom 109 that closes the glass tube 101 at the further end 103. The glass tube 101 is characterized by a longitudinal axis L.sub.tube and comprises, in a direction from the top to the bottom, a top region 104 that is located at the first end 102 of the glass tube 101, wherein the outer diameter of the top region is d.sub.t, a junction region 105 that follows the top region 104, a neck region 106 that follows the junction region 105, wherein the outer diameter of the neck region is d.sub.n with d.sub.n<d.sub.t, a shoulder region 107 that follows the neck region 106; and a body region 108 that follows the shoulder region 107 and that extends to the further end 103 of the glass tube 101, wherein the thickness of the glass in the body region is l.sub.b and wherein the outer diameter of the body region is d.sub.b with d.sub.b>d.sub.t. Junction region 105 corresponds to the transition area between the top region 104 and the neck region 106. l.sub.n is the minimum thickness of the glass in the neck region 106. The neck region 106 is defined by a substantially linear and almost horizontal course of the function f(x) defining the outer contour c.sub.couter of the glass container 100 (see FIG. 4B). The beginning and the ending of the neck region 106 are thus defined by those points at which the course of this function f(x) is no longer linear and horizontal. The beginning and the ending of the neck region 106 are indicated as points x.sub.1 and x.sub.2 and FIG. 4B.
(18) FIG. 3 shows in an enlarged cross-sectional view the top region 104, the junction region 105, the neck region 106 and the shoulder region 107 of a glass container 100 according to the invention (the body region 108 that follows the shoulder region 109 is not shown in that figure). In FIG. 3 the junction region 105 has an outer surface that at the end at which the junction region 105 merges with the neck region 106 is substantially circular arc-shaped, the substantially circular arc-shaped area having an outer radius r.sub.s.
(19) FIG. 4A shows in an enlarged cross-sectional view the determination of the outer contour c.sub.outer of the top region 104, the junction region 105, the neck region 106 and the shoulder region 107 of a glass container 100 according to the invention based on images of the glass container 100 as they have been obtained with the methods described herein in the section “Test methods”. These images are positioned in such a way that glass container 100 is placed on a plane horizontal substrate 110 with the outer surface of the body region 108 on it. k(x) and l(x) are then determined between points P.sub.1 and P.sub.2 as also described herein in the section “Test methods”. s corresponds to (d.sub.t−d.sub.n)/2, s/2 corresponds to (d.sub.t−d.sub.n)/4 which means that P.sub.2 is the x-position at which f(x) is (d.sub.b−d.sub.t)/2+s/2=(d.sub.b−d.sub.t)/2+(d.sub.t−d.sub.n)/4=½×d.sub.b−¼×d.sub.t−¼×d.sub.n. P.sub.1 is then the x- position P.sub.2−s=P.sub.2−d.sub.t/2+d.sub.n/2. FIG. 4B shows the course of the function f(x) describing the outer contour c.sub.outer between points P.sub.1 and P.sub.2. Points x.sub.1 and x.sub.2 indicate the beginning and the ending of the neck region 106.
(20) FIGS. 5A and 5B show in a side view and in a top view the localization of plane 111 in the glass container 100 that is used to determine that is used to determine the local curvature of function f(x) as well as the glass thickness l(x) within the range from P.sub.1 to P.sub.2 by means of the approach that is shown in FIGS. 4A and 4B. Plane 111 corresponds to the plane that is centrically located in the glass container and that comprises the longitudinal axis L.sub.tube (see FIG. 2) of the glass container (indicated by the dashed line in FIG. 5A), i. e. the axis that goes perpendicular through the centre of the bottom 109 (see FIG. 5B).
(21) FIG. 6 shows the determination of r.sub.s. For the determination of the outer radius r.sub.s of the substantially circular arc-shaped area at the end of the junction region 105 that merges into the neck region 106 in images of planes 111 obtained by means of the two approaches described herein in the section “Test methods” point A on the outer surface of the junction region 105 is determined at which the slope β of the tangent 112 reaches its maximum value. In case of a linear section in which the slope β of the tangent 112 reaches a maximum value, A is defined at the point which is nearest to the neck region 106. In s second step, line b 113 is defined as the extension of the essentially non-curved outer surface of the neck region 106. Now the largest possible circle 114 is formed, which is adjacent at point A and coincides at gradient (=bevel circle) and which only touches line b 113 (at point B), but does not cross it (see again FIG. 6). The radius of that circle corresponds to r.sub.8.
(22) FIG. 7 shows a cross sectional view of a further glass container 100 according to the invention having a height h.sub.c. h.sub.c corresponds to the length of the body region 108 and h.sub.t-n to the total length of the top region 104, the junction region 105 and the neck region 106. The glass container 100 comprises a shoulder region 107 that connects the body region 108 with the neck region 106, wherein shoulder region 107 is characterized by a shoulder angle α.
(23) FIG. 8 shows a process for the formation of a top region 104, a junction region 105, a neck region 106 and a shoulder region 107 in a container 100 according to the present invention. A glass tube 101 having an outer diameter d.sub.b of 16 mm and a glass thickness (wall thickness) l.sub.b of 1 mm made of borosilicate glass is loaded into the head of a rotary machine. While rotating around its major axis the glass tube 101 is heated at the bottom end to its softening point with flames 116 and the heated end is shaped to form the top region 104, the junction region 105, the neck region 106 and the shoulder region 107. For the formation of the desired shape of these regions in the rotary machine the glass tube 101 is brought in an upward position as indicated in FIG. 8. By using molding rollers 115 having the desired outer shape to ensure that the required maximum curvature is always realized in the transition area between the top region 104 and the neck region 106 the outer contour c.sub.outer in the top region 104, the junction region 105, the neck region 106 and the shoulder region 107 is formed.
(24) FIG. 9 shows a flow chart of a process 200 according to the invention for packaging a pharmaceutical composition. In a process step a) 201, a glass container 100 according to the invention is provided. In a process step b) 202, a pharmaceutical composition is filled into the interior volume V.sub.i of the glass container 100, and in a process step c) 203 the opening 112 of the glass container 100 is closed, thereby obtaining a closed glass container 121.
(25) FIG. 10 shows the test to determine the mechanical resistance of the vial neck region 106 against diametral compression. The resistance is determined by means of a diametral load strength testing adapted from DIN EN ISO 8113 (“Glass containers—Resistance to vertical load—Test methods”), where a compressive force is applied in diametral (radial) direction at two opposing positions of the outer surface of the neck region 106. The compressive force is increased at a constant load rate of 2000 N/min until breakage of the vial 100 using a universal testing machine (breakage can be detected as a sudden drop in the force-time diagram F(t)). The diametral load is applied by two opposing, uniaxial concave steel plates 119,120 between which the neck region 106 of the vial 100 is placed parallel to the axis L.sub.tube. One of the concave steel plates 119 is constructed to be self-adjusting to be able to compensate geometrical irregularities. The radius of the concavity of the two steel surfaces is 25% larger than the radius of the outer diameter d.sub.n of the neck region 106, so that the load is applied along two opposing lines. The width of the concave steel surfaces is chosen to be slightly shorter than the height of the vial neck region 104.
(26) FIGS. 11A and 11B show a schematic side view and a schematic front view of the neck squeeze test.
LIST OF REFERENCE NUMERALS
(27) 100 glass container according to the invention 101 glass tube 102 first end of the glass tube 101 103 further end of the glass tube 101 104 top region 105 junction region 106 neck region 107 shoulder region 108 body region 109 glass bottom 110 planar and horizontal substrate 111 cross-sectional plane in the middle of the glass container 100 112 tangent with maximum slope β 113 extension of the essentially non-curved outer surface of the neck region 105 (line b) 114 largest possible circle 115 molding roller 116 heating element, preferably a flame 117 self-adjusting steel plate 118 rigid steel plate 119 self-adjusting steel plate 120 rigid steel plate 200 process according to the invention for packaging a pharmaceutical composition 201 process step a) 202 process step b) 203 process step c)
