GB 4771-1984 Test method for alkali dissolution of pharmaceutical glass and its glass containers

This standard is applicable to the determination of alkali dissolution of pharmaceutical glass and pharmaceutical glass containers. This standard is equivalent to the United States Pharmacopoeia (USP) 20th Edition (1980). GB 4771-1984 Test method for alkali dissolution of pharmaceutical glass and its glass containers GB4771-1984 standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Pharmaceutical Glass and Glass Containers
Alkali Dissolution Test Method
Released Alkali Tests of Glass and Glass Containers for Pharmaceutical PreparationsThis standard applies to the determination of alkali dissolution of pharmaceutical glasses and pharmaceutical glass containers. This standard is equivalent to the 20th edition (1980) of the United States Pharmacopoeia (US.P). 1 Definition
UDC 666.11.01
GB 4771-84bzxz.net
Glass powder or glass container is subjected to distilled water under hot pressure to partially leach the alkali metal ions in the glass or glass container. The amount of alkali dissolved by the leaching is expressed by the consumption of 0.020N sulfuric acid solution. 2 Test conditions
2.1 Sample: a predetermined amount of glass or glass container that has not been used and has not been subjected to any chemical test. 2.2 Instruments and Equipment
2.2.1 High-pressure sterilizer: The temperature should be 121±1℃ or the corresponding pressure. 2.2.2 Mortar and pestle: The mortar and pestle are made of 45# steel according to the provisions of Appendix A and are hardened. 2.2.3 Sieve: A set of 20cm diameter sieves are made of stainless steel, including sieves with square mesh sizes of 710μm, 420μm and 300μm, as well as a bottom plate and a lid.
2.2.4 Glassware
2.2.4.1 Conical flask: The chemical stability meets the requirements of QB519-66 "Beakers and Flasks". Several 250ml conical flasks are required for the test. Newly purchased conical flasks should be leached (aged) in a 90℃ water bath with distilled water for at least 24h or leached (aged) in a high-pressure sterilizer at 121℃ for 1h before use.
2.2.4.2 Volumetric flask: The allowable error of capacity shall comply with the requirements of QB701-80 "Volume Flask" Class A. One 50ml and one 100ml volumetric flask are required for the test.
2.2.4.3 Burette: The allowable error of capacity shall comply with the requirements of QB702-80 "Burette" Class A. A 1ml or 2ml microburette is required for the test. The minimum graduation value is 0.01ml. 2.2.4.4 Beaker: The chemical stability shall comply with QB519-66. Several 100ml beakers are required for the test and shall be subjected to the same aging treatment as the conical flask.
2.2.5 Tools: One hammer weighing 900g, one permanent magnet, and one dryer. 2.3 Reagents and solutions
2.3.1 Sulfuric acid solution: Prepare 0.020N sulfuric acid solution with analytical grade sulfuric acid (GB625-77). 2.3.2 Anhydrous ethanol (GB678-78): analytical grade. 2.3.3 Sodium hydroxide solution: Prepare 0.05N sodium hydroxide solution with analytical grade sodium hydroxide (GB629-77). 2.3.4 Hydrofluoric acid solution: Prepare 4% (volume percentage) hydrofluoric acid solution with analytical grade hydrofluoric acid (GB620-77). 2.3.5 Distilled water: It should comply with the provisions of distilled water on page 662 of Part II of the Pharmacopoeia of the People's Republic of China (1977 edition). Issued by the National Bureau of Standards on November 30, 1984
Implementation on January 1, 1986
GB 4771--84
2.3.6 Methyl red indicator solution: Methyl red should comply with the standard HG3-958--76 "Methyl Red". Weigh 0.1g, add 7.4ml of 0.05N sodium chloride solution to dissolve it, and then dilute it to 200ml with water. 3 Test method
3.1 Powder glass test
3.1.1 Determination method
Take 100±5g of well-annealed glass bottles or glass, rinse them thoroughly with distilled water, and place them in a clean oven at a temperature of 110-120℃ for drying. After coarse crushing, place them in a special mortar in batches, insert the pestle, and hit them three to four times with a hammer. Then crush the glass that passes the 710μm sieve and does not pass the 420μm sieve. Take the glass powder that passes through the 420um sieve and does not pass through the 300μm sieve, shake for 10 minutes, remove the particles that do not meet the requirements, carefully absorb the iron with a magnet, place it in a conical flask, rotate and wash with 30ml ethanol for 30s, carefully pour off the ethanol, repeat the above operation 5 times, put it in an oven at 110~120℃ to dry for 20min, move it to a dryer to cool to room temperature, and use it within 48h. Weigh 10.00g of the above sample in a conical flask, accurately add 50.0ml of distilled water, cover the beaker and place it in a high-pressure sterilizer, close the sterilizer, open the exhaust cock, heat until steam violently ejects from the exhaust cock, continue for 10min, close the exhaust cock, continue heating, and make the temperature reach 121℃ within 19~23min. Start timing from the time when this temperature is reached, keep warm at 121±2℃ for 30min, turn off the heat source, exhaust slowly, and exhaust is completed in 38~46min. After taking out the conical flask, immediately cool it to room temperature with running water, carefully pour the leaching solution into another clean conical flask, wash the remaining sample four times with 50.0ml distilled water, combine the washing solution into the above overflow solution, add 2-3 drops of methyl red solution, quickly titrate with 0.020N sulfuric acid solution until it turns slightly red, which is the end point, and correct it with a blank test. 3.1.2 Calculation formula
(VV)>
Alkali dissolution amount:
Where: V
The number of milliliters of sulfuric acid solution consumed by the sample,
The number of milliliters of sulfuric acid solution consumed by distilled water with the same volume as the test solution and subjected to the same test conditions as the sample; The equivalent concentration of sulfuric acid solution;
-The equivalent concentration of sulfuric acid specified in this standard;
G—sample weight, g,
Alkali dissolution amount--The number of milliliters of 0.020N sulfuric acid solution consumed by 10g sample. 3.1.3 Quality judgment
Use the calculated value in 3.1.2 to judge according to the numerical value listed in Table B1 of Appendix B. 3.2 Test of complete glass container
3.2.1 Determination method
Rinse the inner wall of each container of the number of containers to be tested according to Table B2 of Appendix B at least twice with distilled water. Fill each medicine bottle with distilled water to 90% of the full capacity, and seal the mouth with a suitable bottle cap lined with tin foil that has been rinsed twice with ethanol in advance. The powder glass test 3.1.1 is carried out according to the law from "Put in the high pressure sterilizer" to "Immediately cool to room temperature with running water", except that the hot pressing time is changed to 60 minutes. Pour all the leachate in the inspected containers into a clean, dry glass beaker of appropriate capacity, then accurately measure 100 ml of the leachate from the beaker into a 250 ml conical flask, add 2 to 3 drops of methyl red solution, and titrate with 0.020 N sulfuric acid solution until a slightly reddish color is reached, which is the end point, and correct with blank distilled water. 3.2.2 Calculation formula
(VV)×
Alkali dissolution amount:
0.020-×100
Wherein: V is the number of milliliters of sulfuric acid solution consumed by the test solution; V,--the number of milliliters of sulfuric acid solution consumed by blank distilled water with the same volume as the test solution; (2)
N--the equivalent concentration of sulfuric acid solution
Alkali dissolution amount
GB4771-84
The equivalent concentration of sulfuric acid specified in this standard;
Test solution volume, m,
The number of milliliters of 0.020N sulfuric acid solution consumed by 100ml of test solution. 3.2.3 Quality judgment
Use the calculated value in 3.2.2 to judge according to the numerical value listed in Table B3 of Appendix B. If it is necessary to understand the chemical nature of the glass container or to further distinguish between Class I and Class II glass, in addition to proceeding according to 3.1, the following method can also be used: rinse the inner wall of each container of the number of containers to be tested according to Table B2 of Appendix B at least twice with distilled water, fill it completely with 4% (volume percentage) nitric acid solution, and keep it at room temperature for 10 minutes, empty the container, rinse it with water 5 times, and then proceed according to 3.2.1. If the result value is almost equal to the provisions of Table B3 of Appendix B for Class I or Class II glass, the container is Class I glass. If the result value is close to the provisions for Class III glass, the container is Class II glass. Note: 3.2.3 of this standard and Tables B2 and B3 of Appendix B are formulated with reference to the British Pharmacopoeia (B.P) (1980). 38
GB4771-84
Appendix A
Special mortar and pestle for crushing glass
(Supplement)
Special mortar and pestle for crushing glass are made as shown in the figure below: e25.4
Scale, 1.2.5
Unit: mm
Material: 45 steel hardened
.1 Quality judgment of powdered glass method See Table B1 GB 4771-84
Quality judgment table of pharmaceutical glass
(reference)
Table B1 Glass types and test limits
Test method
Highly corrosion-resistant borosilicate glass②
Soda-lime glass③
General-purpose soda-lime glass④
Powdered glass method
Powdered glass method
Powdered glass method
Note: ①This classification applies to containers of this type of glass that are generally available. Test
All capacities
All capacities
All capacities
②Class I borosilicate glass containers are generally used to contain acidic, neutral and alkaline injection pharmaceutical preparations. Limit
0.020N sulfuric acid
③Class III soda-lime glass containers are not usually used to contain injectable pharmaceutical preparations, unless there is appropriate stability test data to show that the Class III glass is suitable for the injectable pharmaceutical preparations contained. Generally used for non-aqueous liquid preparations or injectable powders, and should only be used once. ④[Class V glass containers are usually used to contain enteral pharmaceutical preparations, i.e. oral preparations or topical preparations. See Table B2 for the number of containers tested.
Nominal capacity of the container
5 or less than 5
greater than 5~30
days more than 30
number of containers used
B.3 Quality judgment of the complete glass container method is shown in Table B3. 40
Volume of test solution used for titration
Capacity of the container
(equivalent to 90% of the average overflow capacity)
not more than 1||tt ||Greater than 1, but not greater than 2
Greater than 2, but not greater than 5
Greater than 5, but not greater than 10
Greater than 10, not greater than 20
Greater than 20, but not greater than 50
Greater than 50, but not greater than 100
Greater than 100, but not greater than 200
Greater than 200, but not greater than 500
Greater than 500
GB 4771-84
The volume of 0.020N sulfuric acid solution consumed per 100ml of test solution, ml
Type I or Type II glass
Type III glass
Note: ①Type II glass (i.e., soda-lime glass that has been appropriately dealkalized) containers are generally used to hold acidic and neutral pharmaceutical preparations for injection. If the stability test data can prove its applicability, it can be used to contain alkaline injection drug preparations and should only be used once. ②, Class III shall be classified according to the same category in Table B1.
Additional Notes:
This standard was proposed by the State Drug Administration and is under the jurisdiction of the Glass Pond Porcelain Industrial Science Research Institute of the Ministry of Light Industry. This standard was drafted by Shanghai Glass Factory, Shenyang Pharmaceutical Glass Factory, and Baoji Pharmaceutical Glass Factory. 41
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