Granted Patent B2

US 10,384,972 · App. 14/174,439 · Granted Aug 20, 2019

Abstract

Claims (42)

1. A method of forming an article comprising high purity fused silica comprising:

(a) heating a raw material comprising SiO 2 to form a fused quartz melt;

(b) forming a quartz glass tube from the fused quartz melt;

(c) treating the quartz glass tube from (b) with a composition comprising an acid followed by a water rinse to remove the acid from the glass tube;

(d) heat treating the quartz glass tube from (c) at a temperature of from about 900° C. to about 1250° C.; and

(e) converting the quartz glass tube into a pharmaceutical package via thermal processing, wherein the article has a surface glass test result equal to or less than 0.10 ml of 0.01M HCl per 100 ml of test solution according to the USP<660> surface glass test.

2. The method of claim 1 , wherein the acid comprises an acid chosen from hydrofluoric acid, hydrochloric acid, hydrogen bifluoride, ammonium bifluoride, nitric acid, phosphoric acid, or a combination of two or more thereof.

3. The method of claim 1 , wherein treating with the composition comprising the acid is conducted at a temperature of from about 10° C. to about 100° C.

4. The method of claim 1 , wherein the treating operation (c) comprises agitating the acid composition and/or the quartz glass tube.

5. The method of claim 1 , wherein the treating operation (c) is conducted two or more times with or without other process steps in between, and the quartz glass tube is washed with water subsequent to each treating operation (c).

6. The method of claim 1 , wherein step (e) further comprises:

cutting the quartz glass tube subsequent to operation (d) to form cut quartz glass sections; and

washing the cut quartz glass sections with an acid composition followed by a water rinse.

7. The method of claim 6 , wherein the acid composition comprises an acid chosen from hydrofluoric acid, hydrochloric acid, hydrogen bifluoride, ammonium bifluoride, nitric acid, phosphoric acid, or a combination of two or more thereof.

8. The method of claim 1 , wherein the article has a SiO 2 concentration of about 99% or greater.

9. The method of claim 1 , wherein the surface glass test result is equal to or less than 0.025 of 0.01 M HCl per 100 ml of test solution.

10. A method of forming a pharmaceutical package comprising:

(A) providing quartz glass tube having a SiO 2 concentration of about 99% or greater, the quartz glass tube being produced by a process comprising:

(i) heating a raw material comprising SiO 2 to form a fused quartz melt;

(ii) forming a quartz glass tube from the fused quartz melt;

(iii) treating the quartz glass tube from (A)(ii) with a composition comprising an acid followed by a water rinse to remove the acid, and

(iv) heat treating the quartz glass tube following (A)(iii);

(v) cutting the quartz glass tube to desired lengths suited for pharmaceutical packaging; and

(B) converting the quartz glass tube into a pharmaceutical package via thermal processing, wherein the package has a surface glass test result equal to or less than 0.10 ml of 0.01M HCl per 100 ml of test solution according to the USP<660> surface glass test.

11. The method of claim 10 , wherein converting the quartz glass tube into a pharmaceutical package comprises converting the tube into a package in the form of a vial, an ampoule, or a syringe.

12. The method of claim 10 , wherein the treating operation (iii) is conducted at a temperature of from about 10° C. to about 100° C.

13. The method of claim 10 , wherein the treating operation (iii) comprises agitating the composition comprising the acid and/or the quartz glass tube.

14. The method of claim 10 , wherein the treating operation (iii) is conducted two or more times, with or without other process steps in between, and the quartz glass tube is washed with water subsequent to each treating operation.

15. The method of claim 10 , wherein the heat treating operation (iv) comprises heating at a temperature of from about 900° C. to about 1250° C. at a pressure of about 10 torr or less.

16. A method forming a pharmaceutical package from an article comprising a high purity silica, the method comprising;

(a) heating a SiO 2 raw material having a SiO 2 concentration of about 99% or greater at a temperature of from about 2000° C. to about 3000° C. to form a fused quartz material;

(b) drawing the fused quartz material to form a quartz tube;

(c) treating the quartz tube from (b) with an acid composition at a temperature of from about 10° C. to about 100° C.;

(d) washing the quartz tube treated in (c) with water to remove the acid from (c);

(e) heating the quartz tube from (d) at a temperature of from about 900° C. to about 1250° C. and a pressure of 10 torr or less; and

(f) converting the quartz tube into a pharmaceutical package via thermal processing, wherein the article has a surface glass test result equal to or less than 0.10 ml of 0.01M HCl per 100 ml of test solution according to the USP<660> surface glass test.

17. The method of claim 16 , wherein the acid composition comprises an acid chosen from hydrofluoric acid, hydrochloric acid, nitric acid, hydrogen bifluoride, ammonium bifluoride, phosphoric acid, or a combination of two or more thereof.

18. The method of claim 16 , further comprising:

(f) cutting the quartz tube subsequent to operation (e) to form cut quartz glass sections; and

(g) washing the cut quartz glass sections with an acid composition followed by a water rinse.

19. The method of claim 16 , wherein the treating operation comprises agitating the acid composition and/or quartz tube.

20. The method of claim 16 , comprising drying the quartz tube following the washing operation (d).

Assignments (14)