IP Library Granted Patent US 9,322,766
Granted Patent B2
US 9,322,766 · App. 14/354,741 · Granted Apr 26, 2016

Rapid test method for evaluating the delamination tendency of glass packaging means

Inventors: Volker Scheumann (Mainz, DE); Michaela Klause (Woerrstadt, DE); Uwe Rothhaar (Birkenheide, DE)
Assignee: SCHOTT AG
G01N21/01G01N21/90G01N21/91
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Quick Facts
Patent No.
US 9,322,766
App. No.
14/354,741
Granted
Apr 26, 2016
Kind
B2
Abstract

A rapid test method for evaluating the delamination in glass packaging is provided. The method includes exposing the glass packaging means to an atmosphere consisting of steam in order to form a corrosion zone; and subsequently carrying out at least one other step. The other step includes: visualizing the corrosion zone using a light microscope; visualizing the corrosion zone by a staining process with a subsequent inspection process; or removing glass components in ultrapure water and quantifying the removed glass components. The rapid test method provides a conclusion about whether a glass packaging exhibits a tendency to delaminate or not in a simple and reliable manner and in a relatively short time span.

Claims (26)

1. A rapid test method for evaluating the delamination tendency of glass packaging, comprising the steps of:

exposing empty glass packaging to an atmosphere of steam to form a corrosion zone; and

subsequently carrying out a further step selected from the group consisting of: visualizing the corrosion zone using a light microscope; visualizing the corrosion zone by staining and subsequent inspection; and dissolving glass components in ultrapure water and quantifying the dissolved glass components.

2. The rapid test method as claimed in claim 1 , wherein the step of exposing the empty glass packaging to the atmosphere of steam is carried out in an autoclave, wherein the empty glass packaging is exposed to steam for at least 30 minutes.

3. The rapid test method as claimed in claim 2 , wherein the empty glass packaging is exposed to steam for 1 to 8 hours.

4. The rapid test method as claimed in claim 1 , wherein the step of exposing the empty glass packaging to the atmosphere of steam is carried out at a temperature in a range of from above 100 degrees Celsius to 180 degrees Celsius.

5. The rapid test method as claimed in claim 1 , wherein the further step comprises visualizing the corrosion zone using a light microscope, and wherein the light microscope comprises a stereomicroscope or a stereomicroscope having grazing illumination.

6. The rapid test method as claimed in claim 1 , wherein the further step comprises visualizing the corrosion zone by staining and subsequent inspection, and wherein the staining is performed using methylene blue, methylene blue in water, or methylene blue alcohol.

7. The rapid test method as claimed in claim 1 , wherein the further step comprises visualizing the corrosion zone by staining and subsequent inspection, wherein the staining comprises charging a solution of methylene blue is into the empty glass packaging and allowing the charged empty glass packaging to stand at room temperature.

8. The rapid test method as claimed in claim 7 , wherein the charged empty glass packaging charged to stand at room temperature for several minutes to several hours.

9. The rapid test method as claimed in claim 7 , wherein the subsequent inspection comprises visual inspection.

10. The rapid test method as claimed in claim 1 , wherein the further step comprises dissolving glass components in ultrapure water and quantifying the dissolved glass components, wherein the step of dissolving glass components in ultrapure water comprises charging the empty glass packaging with the ultrapure water and storing the charged empty glass packaging at an elevated temperature, and wherein the step of quantifying the dissolved glass components comprises determining an amount or concentration of the glass components dissolved in the ultrapure water.

11. The rapid test method as claimed in claim 10 , wherein the elevated temperature is above 50 degrees Celsius.

12. The rapid test method as claimed in claim 1 , wherein the further step comprises dissolving glass components in ultrapure water and quantifying the dissolved glass components, wherein the step of dissolving glass components in ultrapure water comprises charging the empty glass packaging with ultrapure water and autoclaving the charged empty glass packaging at a temperature between 80 degrees Celsius and 150 degrees Celsius for a period from 0.5 to 8 hours, and wherein the step of quantifying the dissolved glass components comprises subsequently determining the amount or concentration of the glass components dissolved in the ultrapure water.

13. The rapid test method as claimed in claim 12 , wherein the period is 2 hours.

14. The rapid test method as claimed in claim 12 , wherein the amount or concentration of the glass components dissolved in the ultrapure water is determined using a method selected from the group consisting of ICP-OES, ICP-MS, and FAAS.

15. The rapid test method as claimed in claim 1 , wherein the empty glass packaging is selected from the group consisting of bottles, vials, phials, ampoules, cartridges, capsules, and syringes.

16. The rapid test method as claimed in claim 1 , further comprising cleaning the empty glass packaging means before and/or after exposing the empty glass packaging to the atmosphere of steam.

17. The rapid test method as claimed in claim 16 , wherein the cleaning comprises multiple rinsing of the empty glass packaging by charging with water, emptying the water from the empty glass packaging, and blowing dry the empty glass packaging means with inert gas.

18. The rapid test method as claimed in claim 16 , wherein the water comprises mains water, demineralized water or ultrapure water.

19. The rapid test method as claimed in claim 16 , wherein a final rinsing operation comprising rinsing with demineralized water or ultrapure water.

20. The rapid test method as claimed in claim 16 , wherein the inert gas is nitrogen.

21. The rapid test method as claimed in claim 16 , wherein the water for rinsing is at room temperature.

22. The rapid test method as claimed in claim 16 , wherein the water for rinsing is preheated to a temperature above room temperature.

23. The rapid test method as claimed in claim 22 , wherein the water for rinsing is preheated to above 50 degrees Celsius.

24. The rapid test method as claimed in claim 1 , wherein the further step comprises dissolving glass components in ultrapure water and quantifying the dissolved glass components, and wherein, before the dissolving step, the empty glass packaging is not rinsed with water.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 21, 2022
From: SCHOTT AG
To: SCHOTT PHARMA AG & CO. KGAA
Reel/Frame 061972/0280 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 8, 2014
From: SCHEUMANN, VOLKER; KLAUSE, MICHAELA; ROTHHAAR, UWE
To: SCHOTT AG
Reel/Frame 033280/0714 →
Priority Claims (1)
DE 10 2011 085 267 · Oct 27, 2011 · national
Continuity (1)
Related Publication 20140240694A1 · Aug 28, 2014