GB/T 4548-1995 Test method and classification of water erosion resistance of inner surface of glass containers
Some standard content:
1Cs81.040.30
National Standard of the People's Republic of China
GB/T45481995
tqs04802-1.1988
Test niethod and classification for hydrolytic resistanceof the interior surfaces of glass containers1995-12-08Promulgated
State Bureau of Technical Supervision
Implementation on 1996-08-01
GB/I4548-1995
This standard is formulated according to national standard 1S046021.1988Test method for hydrolytic resistance of the interior surfaces of glass containersPart 1: Determination and classification by titration> and is equivalent to the international standard in terms of technology. [504802-1] The test method for the water corrosion resistance of glass bottles is developed by scientists in many countries around the world after years of work. The qualitative method used in my country is no longer suitable for the production and production of glass bottles and jars. The test results are not comparable internationally. Therefore, a new technical standard was formulated using ISO4802-1 to keep pace with the international standards. Since many laboratory equipment in my country do not adopt international standards, they cannot be equivalent to ISO4802-1 in related items. This standard is equivalent to the implementation from August 1, 1996. From the date of effectiveness, this standard replaces GB4543-84. This standard is issued by the Ministry of Software Industry of the People's Republic of China. This standard is under the responsibility of the National Standardization Administration of China and the Glass Industry Research Institute of the Ministry of Light Industry. The main organizers of this standard are Yin Man and Zhang Guoxiu. GL/E4548—1995
ISO Preface
This part of ISO4602 is based on the test method for the hydrolysis resistance of the inner surface of the penetrator approved by the Second Technical Committee of the International Commission for Glass (ICG) (Analysis of Chemically Stabilized Wires). The European Pharmacopoeia Commission has adopted the principle of disease-specific testing and formulated the classification of penetrators for injectable preparations, which is included in this part of the standard.
Based on the test results of many international laboratories, this standard stipulates more stringent test conditions than the European Codex in order to improve the reproducibility of the test results.
1 Scope
National Standard of the People's Republic of China
Test ruethod and elassification far hydralytic resistanceof the interior aurfaces of glass rontainers
Performance test method and classification
Test ruethod and elassification far hydralytic resistanceof the interior aurfaces of glass rontainers This standard stipulates:
GB/T 4548—1995
cqv1$O4802-1:1988
Generation 4548-84
:) Determination method of the water resistance of glass containers when the inner surface is subjected to 1211× water erosion for 60±1min. The water resistance is obtained by measuring the prepared water with a certain resistance using a viscoelastic solution. At this time, the resistance of the container is inversely proportional to the amount of water consumed. H) Classification of glass containers. This classification is determined according to the method for determining the water resistance of the inner surface of glass containers specified in the standard. The water resistance of the glass container determined by the standard method is HC level and IIC level according to the ISO4D2-2 carbon code. The individual test results of the two methods are not the same. This standard is applicable to a total of bottles, small glass bottles, flasks and beakers. These glass containers are made of sodium-calcium glass that has been treated with a surface treatment and is made of carbonate neutral adsorption. This standard does not apply to double-ban containers.
2 Referenced standards
The provisions contained in the following standards are referenced in this standard and are marked as relevant texts. At the time of publication of this standard, the versions indicated are valid. All standards are reviewed and all parties using this standard should consider the possibility of using the latest version of the following standards. G8/T6582-86 Test method for water resistance of carbon dioxide at 93°C and GB1211%.2-90 Test method for water resistance of glass particles at 121°C GH12803.91 Laboratory glass burette GB22803-91 Laboratory glass instrument single line volume 2HN644I01-27 Laboratory instrument beaker ZRN6410287
3 Definition
Laboratory instrument narrow-necked bottle
This standard adopts the following definitions.
3.1 Container: Any product made of phosphate glass, neutral glass or polyurethane, such as general-purpose glass bottles, small glass bottles and ampoules, etc., as well as glass products for laboratory or pharmaceutical use that can be filled with phosphate. 3.2 Phosphate-free phosphate glass, emulsified phosphate glass with a content of 5% to 13%, which has high heat resistance and excellent water resistance due to its chemical composition.
This type of container made of borosilicate glass meets the HC1 water resistance requirements specified in this standard. 3.3, silicate glass containing a certain amount of oxides (mainly 5% to 13%), metal oxides and/or metal oxides: this kind of glass has extremely high water resistance due to its chemical composition, and various containers made of this kind meet the grade 1 water resistance requirements specified in this standard. GH/T4548-1995 3.4 Sodium Calcium Silicate Glass: silicate glass containing about 15% of pure metal oxides (mainly calcium hydroxide) and about 15% of pure metal oxides (mainly sodium oxide).
This kind of calcium glass container has good water resistance due to its chemical properties and meets the requirements of IC:3 grade water resistance or HCD grade water resistance. After surface treatment (see 3.5), the sodium calcium glass container with C3 grade water resistance will be solidified and have high water resistance, meeting the requirements of HC2 grade water resistance. 3.5 Surface treatment: Treat the surface of the sodium calcium container with reagents to obtain a good surface, significantly reduce the concentration of metal ions, and the concentration of metal ions.
3.6 Fill the container, when water is poured into a hole placed on a horizontal surface. Until the surface just touches the liquid contact plate (see 6.7), the volume of water medicine is
3.7 Filling container: The volume of water medicine in the container. ~ Stock plate monument bottle, small glass plate and right mouth ball end through the container, the water filling volume is specified as SC% of the full mouth. For the safety statement, the basic requirement is that the inner surface of the bottle is lowered and the bottle has a high container tray (see Figure 2). 3.8 Generally, glass bottles are made of flat glass containers with this shape. This glass container is thick and its capacity is generally more than 5nL. The cross-section of the filled bottle can be shaped like another shape or other shapes. Note: Generally, glass bottles are usually made of non-glass materials for sealing without flame sealing. 3.9 Small glass bottle. Tube bottle: A small flat-bottomed glass container formed by a glass tube or mold. The glass container is thick enough and its capacity is about within 100L. Small glass bottles usually need to be made of non-glass materials for sealing without flame sealing. 3.10 Anguan: A flat-bottomed glass container usually made of thin tube and with necks of different shapes. The one that is sealed with flame after blasting is called Anguan. Its capacity is less than 25L. Its types are divided into open-mouth Anguan and sealed Anguan (see 1). at
Figure 1 Typical drug oral test, b)
4 Li
This method is a surface test method, generally applicable to glass containers delivered for use, Figure 2 Plated capacity
(to point A)
Pour the specified water into the test container to the "specified container plate", and heat the unsealed container under specified conditions. The degree of water erosion on the container is measured by titration. 2
5 Test
G/T 4548-1995
Unless otherwise specified, only approved reagents of pure purity shall be used in the test. 5.1 Test water:
Does not contain heavy metal ions (especially copper), and can be tested by sulfur chamber test method when necessary. Its conductivity does not exceed 0.1ms/m at 25℃.
It is prepared by boiling water in a non-glass or ionized flask for more than 15min. It does not contain decomposable gases such as carbon dioxide. Before the next use, it shall be treated once according to the provisions in 2. The test water should be neutral to formaldehyde. That is, before the test, add tetramethyl red to the test water (see 5.5) should be: a red color (not red or pale color) equivalent to pH 5.5 ± 0.1 Note: the test water selected according to the above requirements can also be used as a reference (see 9.3). This test water can usually be kept in a bottle for 24 hours without changing its pH value.
5.2 Hydrochloric acid standard solution (HCl)-C.01mol/L53 Quick roll (CI) = HCl/
5.4 Hydrogen hydroxide (HF) + 22ol/L 400IF/L Filter), 5.5 Methyl red indicator.
2mg sodium salt of methyl red can be used5.6 Water, purified or equivalent:
6 Apparatus
General laboratory apparatus and test equipment.
6.1 Pressure or pressure relief apparatus capable of withstanding a pressure of at least 2.×10\N/m*1 and capable of being subjected to the heating cycles specified in 8.2. Preferably, it should be equipped with a regulator or other device capable of maintaining the temperature at 121 ± 1 °C. The reservoir should have an internal diameter of at least 3 mm and should be equipped with a heating device, a thermometer or a calibrated thermocouple, a pressure gauge, a pressure relief safety device, a plug and a support for the sample. The auxiliary control of the high pressure should be thoroughly cleaned before use. 5.2 The filter tube should have appropriate capacity such as 50L, 25ml, 70ml and 2ml, which should meet the requirements of Class A titration in GB12895 and be made by the water resistance test of the 1-year paste method in GB12416.2. The capacity of the tube should be based on the expected use rate (see 5.2). 6.3 The conical flask should have 100mL and 25mL capacity, which should meet the requirements of GBNG002. Each new conical flask should be pre-conditioned in high temperature according to 8.2 before use. 6.4 The filter should have appropriate capacity, especially the requirements of Class A in GB12809. 6.5 The water scale should be able to heat to about 80℃, and 6.6 The beaker should have appropriate capacity and meet the requirements of GB12416.2. Each new beaker should be pre-conditioned in high temperature according to B.2 before use.
67 The contact plate (the time-limited plate for measuring the pressure drop of the bottle and the small glass bottle) is made of a rigid and flexible material, with a suitable shape and a central hole with a diameter of 5m. The size of this contact plate should match and completely correspond to the sealing surface of the port to be measured.
7 Test specimens
7.1 Test specimen rate
1) 2. 5×10N/t*=0. 2: MP%=2. 5 ha2>GB6021 longitudinal glass meets the requirements of GB12416.1 medium-term 1-level installation, a
GB/4548-.1995
The average number of containers to be added depends on the maximum number of containers, the volume of the sample liquid required for one titration and the results of the determination, etc. It should be calculated according to the requirements given in Table 1. The titration method is too individual. 1.2.1 ... At this time, it should be ensured that there are no bubbles on the interface between the filter water and the filter. Then, the evaporation volume is obtained from the filter. The filtration should be accurate to the decimal point. This value is the micro-permeability of the amine separation zone. Calculate 90% of the average value of the filling volume of each glass container, calculate the correct decimal point, and the obtained value is the filling volume of this particular sample group. 7.2-2 Half-bottom effect containers with a capacity of less than or equal to 30mL are randomly selected from a batch of test pads. 6 full-bottom containers (capacity less than or equal to 100mL) or 9 glass replacement containers (capacity less than 105ml.). Move these glass containers to remove all dirt and packaging debris. Let these glass containers reach a resistance of 22±2°C. Cover each glass container with an appropriate contact plate (must be 7), and The air permeation of the touch plate is continued until the value reaches 0.1 g. Remove the touch plate and adjust the water (1.6 g) to 22°C. Place the container at the desired position, then put the touch plate back on and make the small hole of the plate approximately at the center of the container according to 7.2.1. Use a burette (see 6.2) to inject 22±2°C water into the glass container through the small hole in the melt plate. Weigh the glass container filled with distilled water and its liquid plate together until the value reaches 0.1 g. Calculate the mass of water in the center of the glass container in units of nL. Calculate the average value of the test results of the 5 glass containers. The calculated value can be expressed in nL of water. This calculated value is the average filling capacity of the glass container. Calculate the value of 9 of this average filling capacity to obtain nL of water. 7.2.3 Two glass containers (except for plastic)
Select 4 glass containers (capacity 10DL or more) or 3 glass containers (volume greater than 100m>) from a batch of samples. Remove all waste and filling debris from these glass containers. Allow these dry containers to drain to 22 ± 2. Fix each glass container vertically in an appropriate environment and measure the filling volume according to the provisions of 7.2.1 or 7.2.2. Calculate the average filling volume of 90% of the value, accurate to a low decimal point, and the individual containers are the filling volumes of the specific test group. 7.24 Confirm glass container
Place plastic glue on the glass container in reverse order to prevent it from leaking. The plastic container should be flush with the opening of the container. The fertilizer filter plate should be installed (see 6.7) and then weighed without removing the contact plate. 7.2.5 Place at least ten dry containers at a temperature of 22 ± 2 ° C on a flat horizontal surface and use a burette (see 6.2) to add sample temperature water (see .6) until the steam reaches point A, which is the middle of the bottle (see Figure 2). Take a small amount of each container and calculate the average value. The measured value is accurate to the decimal point, which is the melt volume and should be added to all other containers selected for the fertilizer test. 8 Test steps This test process should be completed within one working hour. 8.1 Cleaning of the specimens
The cleaning process should be completed within 20-25 min from the first cleaning. All open specimens should be free of any packaging debris or dirt that may have occurred during storage and transportation. Rinse each specimen at least twice with room temperature distilled water (see 6.6) and then fill with distilled water. Before the test, empty the specimen and rinse it with water as required. Then rinse it once more with test water (see 5.1) and drain it completely.
Closed specimens should be placed in a water bath or incubator at about 6.4°C for 2 min before being opened. They should not be rinsed before the test. 8.2 Filling and filling
With the aid of appropriate containers, fill each glass container selected in accordance with 7.1 and 8.1 with test water (see 5.1) to the specified filling volume.
Each glassware, including the beaker, shall be capped with a non-determined cap of a material such as a beaker ring (see 6.6) of similar size, i.e. the beaker is placed with the top of the beaker down over the edge of the sample. For the beaker, a clear pin may be used for the capping.
Note: The aluminum should not be allowed to enter the test water. The samples should be placed on a pressure-sensitive test stand (see 6.1) with room temperature distilled water (see (.6)); and it should be ensured that the samples are above the required liquid level in the tester. The lid or door of the high-pressure vehicle is opened and the screw is turned off. , heat the system at a constant speed, after 2 minutes, let the steam escape through the exhaust, and continue to let the steam escape through the exhaust for 10 minutes. Close the exhaust gas, raise the temperature to 121℃ at a rate of 1℃/min. From the time the temperature is reached, maintain it at 121±1℃ for 60±1min. After storage, cool the temperature to 10G℃ at a rate of 5.5℃/min to prevent air from leaking.
Transfer: Experience has shown that the temperature of 121℃ is kept at a limit of 121.1℃ and the cooling ratio cannot reach the specified value, which may cause undesirable results, and even reach this side effect. Some drill stations are not recommended. Take the hot samples from the press and place them in a water bath with 8DC (see 6, 3), then cool the water bath. The cooling water should be passed through the water bath at a rate that allows the sample to cool to room temperature as quickly as possible, but to avoid damage caused by heat shock. Considering the rate, the amount of sample, the thickness and the type of polymer used to make the sample, the cooling time should not exceed 30mm. After the sample has cooled, the measurement should be started immediately.
Warning: Note that the cooling water should not contact the loose pin foil, which is dangerous. Especially for small bottles, please note 8.3 Analysis of the Extracted Liquid || tt || Apply the extract in the following solution (see column 3 in Table 1). To avoid the risk of carbon (C()) being neutralized when evacuating the low frequency anhydrous anhydrous, temporarily turn the anhydrous anhydrous anhydrous and heat the anhydrous anhydrous slowly with a low flame. When the mixed sample is taken from a container less than or equal to 31 mL, pipette 25 mL of the sample (see column 3 in Table 1) into a 100 mL conical flask (see 6.3). When the mixed sample is taken from a container of 8 to 30 mL or 39 to 100 mL (see column 1 in Table 1), pipette 50 mL and 100 mL of the sample (see column 3 in Table 1) into two separate 250 mL conical flasks (see 6.3). In the case where the test volume is greater than 100 mL (see column 1 in Table 1), pipette 150 mL of the sample from each sample into a 250 mL conical flask (see 6.3) containing only oil. The reference sample may be prepared by the following method: pipette the test effluent (equivalent to the sample from the sample) into a 100 mL conical flask (see 6.3). The maximum (see small.1> is sucked into the same conical flask (see 5.3) as the one containing the test sample. For every 2% ml. test water, add 2% methyl red indicator solution (see 5.5). For each plate, every 25 mL of liquid should be filled with 2% methyl red indicator solution (see.5.5), and drip with hydrochloric acid (see 5.2). It is 5
GB/T4548-1995
until the color that appears is completely consistent with the color of the reference solution. The titration value less than 1.0 should be expressed to two decimal places, and the titration value of 1.Cml. should be expressed to the center of the heart. 8.4 Test to determine whether the glass container has been treated with a surface 8.4.1 Small glass bottles and through glass bottles
Note that the small glass bottles made of calcium glass are relatively separated from the plate during manufacturing. During the process, the inner surface is treated, and the resistance of the inner surface can be obtained. The results must determine whether a container has been treated: if a tested sample is used for comparison, a mixture of 1 part hydrofluoric acid (see 5.4) and 9 parts hydrochloric acid (see 5.3) is injected into the sample until it is full: the filled test column is placed in the chamber for 10 minutes, and then the test column is carefully emptied. Rinse the sample with distilled water (see 5.5) 3 times, and then rinse the sample with water (see 5.1) twice at a high rate. Then test the test column according to the provisions of 8.2 and 5.3. If the test result is significantly lower than the test result of the initial surface (about 5 to 10 times higher), it should be considered that the surface has been treated. B.4.2 Required surface |Note: The surface treatment of the glass tubes is not required because they have a hydrophobic effect. The chemical composition (see 3) is determined here.
If it is necessary to determine whether the glass tube has been treated, a comparison shall be made with a sample that has been tested. The sample shall be tested in accordance with the requirements of 6.4.1, with a surface treatment and in accordance with the requirements of 9.2 and 9.3. If the glass tube has not been treated, the test value obtained shall be lower than the test value obtained previously. 9.1 The half-mean value of the titration of the sample shall be expressed as the number of liters of hydrochloric acid solution (see 5.2) per 100 nl of the sample. The test result may also be expressed as the number of micrograms of sodium hydroxide (Na2O3) per 100 mL of the sample. 1 mL of a hydrochloric acid solution with a concentration of 0.ulmol/L is equivalent to 310 g of the sample. 9.2 Classification
Glass containers shall be classified according to the consumption pressure of the scale liquid (see 6.2) when tested in accordance with 8.3 and calculated in accordance with 9.1. As shown in Table 2.
9.3 The difference between the water resistance of the container HC1 and HC2 shall be determined according to the provisions of 1. The glass of HC1 grade shall meet the requirements of water resistance of glass of HC1 and HC2 given in Table 2.
After the immersion and repeated tests in accordance with 8.4, the test results given by the water resistance container of HC1 grade IC2 will fall within the values given in the second column of Table 2. These test values will be very close to the values measured for the glass of HC1 grade IC2 in Table 2. 9.4 Expression method
According to this standard, the water resistance of the inner surface of the glass container shall be expressed as follows: number
9mL capacity glass container, every 100ml. The amount of 1.6mL hydrochloric acid solution [e(HCl) 0.nlmul/L] is expressed as, glass container water resistance GB4548-HCB grade
>20,5G
>2c,560
10 test report
CB/T4548--1995
Table 2 Glass container inner surface water resistance test (titration method) maximum slope value stop nmm]. Take according to the amount of slightly soluble C(Hl)=0.G1mol!/1 mml
HC| grade HC2| |tt||The test report shall include the following:
8) According to CR4548 standard;
1.) Marking of the sample:
) Average full capacity of the sample (except ampoules);
d) Filling capacity of the sample;
e) Number of samples used at one time:
}) Average value of the dry drops:
R) HC grade of water resistance of the container (see S.4);
HCD grade
h) For HC2 grade of water resistance, it should be stated whether the surface has been tested (see 8.4) and the test results obtained:
1) Whether the closed ampoules have passed the test.
) Any abnormal phenomenon recorded during the test.1 mL of hydrochloric acid solution with a concentration of 0.ulmol/L is equivalent to 310 g of HCl. 9.2 Classification
When glass containers are tested according to 8.3 and calculated according to 9.1, these glass containers shall be classified according to the consumption pressure of the scale liquid (see 6.2). This is shown in Table 2.
9.3 The difference between the water resistance of containers of grade HC1 and HC2 shall be determined according to the provisions of 1. The glass of grade HC1 shall meet the requirements of the water resistance of glass of grade HC1 and HC2 given in Table 2 for oil immersion and repeated tests.
After the immersion and repeated tests according to 8.4, the test results given by the water resistance of grade 1IC2 containers will fall within the values given in the second column of Table 2. These test values will be very close to the values measured for the glass of grade 1IC3 in Table 2. 9.4 Expression method
According to this standard, the water resistance of the inner surface of the glass container shall be expressed as follows: number
9mL capacity glass container, every 100ml. The amount of 1.6mL hydrochloric acid solution [e(HCl) 0.nlmul/L] is expressed as, glass container water resistance GB4548-HCB grade
>20,5G
>2c,560
10 test report
CB/T4548--1995
Table 2 Glass container inner surface water resistance test (titration method) maximum slope value stop nmm]. Take according to the amount of slightly soluble C(Hl)=0.G1mol!/1 mml
HC| grade HC2| |tt||The test report shall include the following:
8) According to CR4548 standard;
1.) Marking of the sample:
) Average full capacity of the sample (except ampoules);
d) Filling capacity of the sample;
e) Number of samples used at one time:
}) Average value of the dry drops:
R) HC grade of water resistance of the container (see S.4);
HCD grade
h) For HC2 grade of water resistance, it should be stated whether the surface has been tested (see 8.4) and the test results obtained:
1) Whether the closed ampoules have passed the test.
) Any abnormal phenomenon recorded during the test.1 mL of hydrochloric acid solution with a concentration of 0.ulmol/L is equivalent to 310 g of HCl. 9.2 Classification
When glass containers are tested according to 8.3 and calculated according to 9.1, these glass containers shall be classified according to the consumption pressure of the scale liquid (see 6.2). This is shown in Table 2.
9.3 The difference between the water resistance of containers of grade HC1 and HC2 shall be determined according to the provisions of 1. The glass of grade HC1 shall meet the requirements of the water resistance of glass of grade HC1 and HC2 given in Table 2 for oil immersion and repeated tests.
After the immersion and repeated tests according to 8.4, the test results given by the water resistance of grade 1IC2 containers will fall within the values given in the second column of Table 2. These test values will be very close to the values measured for the glass of grade 1IC3 in Table 2. 9.4 Expression method
According to this standard, the water resistance of the inner surface of the glass container shall be expressed as follows: number
9mL capacity glass container, every 100ml. The amount of 1.6mL hydrochloric acid solution [e(HCl) 0.nlmul/L] is expressed as, glass container water resistance GB4548-HCB grade
>20,5G
>2c,560
10 test report
CB/T4548--1995
Table 2 Glass container inner surface water resistance test (titration method) maximum slope value stop nmm]. Take according to the amount of slightly soluble C(Hl)=0.G1mol!/1 mml
HC| grade HC2| |tt||The test report shall include the following:
8) According to CR4548 standard; bzxz.net
1.) Marking of the sample:
) Average full capacity of the sample (except ampoules);
d) Filling capacity of the sample;
e) Number of samples used at one time:
}) Average value of the dry drops:
R) HC grade of water resistance of the container (see S.4);
HCD grade
h) For HC2 grade of water resistance, it should be stated whether the surface has been tested (see 8.4) and the test results obtained:
1) Whether the closed ampoules have passed the test.
) Any abnormal phenomenon recorded during the test.
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