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GB/T 7962.21-2019: Test method of colourless optical glass -- Part 21: Resistance to attack by aqueous alkaline solutions
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Test method of colourless optical glass -- Part 21: Resistance to attack by aqueous alkaline solutions
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GB/T 7962.21-2019
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| GB/T 7962.21-1987 | English | 199 |
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Colourless optical glass test methods--Knoop hardness
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Basic data | Standard ID | GB/T 7962.21-2019 (GB/T7962.21-2019) | | Description (Translated English) | Test method of colourless optical glass -- Part 21: Resistance to attack by aqueous alkaline solutions | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | L50 | | Classification of International Standard | 81.040.01 | | Word Count Estimation | 14,185 | | Date of Issue | 2019-08-30 | | Date of Implementation | 2020-03-01 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 7962.21-2019: Test method of colourless optical glass -- Part 21: Resistance to attack by aqueous alkaline solutions
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Test method of colourless optical glass - Part 21.Resistance to attack by aqueous alkaline solutions
ICS 81.040.01
L50
National Standards of People's Republic of China
Colorless optical glass test method
Part 21.Alkali resistance stability
2019-08-30 released
2020-03-01 Implementation
State Administration for Market Regulation
Issued by China National Standardization Administration
Table of contents
Preface Ⅲ
1 Scope 1
2 Normative references 1
3 Principle 1
4 Reagent 1
5 Instrument 2
6 Preparation of the tested sample 3
7 Test Step 4
8 Calculation of results 6
9 Classification and judgment 7
10 Test report 7
Appendix A (informative appendix) Structure changes of this part compared with ISO 10629.1996 9
Foreword
GB/T 7962 "Test Method for Colorless Optical Glass" is divided into the following 23 parts.
---Part 1.Refractive index and dispersion coefficient;
---Part 2.Fizeau Plane Interferometry for Optical Uniformity;
---Part 3.Optical uniformity holographic interferometry;
---Part 4.Temperature coefficient of refractive index;
---Part 5.Stress birefringence;
---Part 6.Young's modulus, shear modulus and Poisson's ratio;
---Part 7.Streakness;
---Part 8.Bubble degree;
---Part 9.Light absorption coefficient;
---Part 10.X-ray resistance;
---Part 11.Precision test of visible refractive index;
---Part 12.Intraspectral transmittance;
---Part 13.Thermal conductivity;
---Part 14.Acid resistance stability;
---Part 15.Moisture resistance stability;
---Part 16.Linear expansion coefficient, transition temperature and sag temperature;
---Part 17.Ultraviolet and infrared refractive index;
---Part 18.Kjeldahl hardness;
---Part 19.Abrasion;
---Part 20.Density;
---Part 21.Alkali resistance stability;
---Part 22.Phosphoric acid resistance stability;
---Part 23.Weather resistance stability.
This part is Part 21 of GB/T 7962.
This section was drafted in accordance with the rules given in GB/T 1.1-2009.
This part uses the redrafting method to amend and adopt ISO 10629.1996 "Test of the alkali resistance stability of optical glass blanks in alkaline solution at 50℃"
Test method and classification.
Compared with ISO 10629.1996, this part has many adjustments in structure. Appendix A lists this part and ISO 10629.1996.
A list of changes in chapter numbers.
The technical differences between this part and ISO 10629.1996 and the reasons are as follows.
---Regarding normative reference documents, this section has made technically different adjustments to adapt to my country's technical conditions and adjustments.
The situation is collectively reflected in Chapter 2 "Normative Reference Documents", and the specific adjustments are as follows.
● Replace ISO 2768-1.1989 with GB/T 1804-2000, which is equivalent to the international standard;
● Replace ISO 3696.1987 with GB/T 6682-2008 which is modified to adopt international standards;
● Deleted ISO 3585.1991;
● Added reference to GB/T 903 and GB/T 1185-2006.
---Unify "2-propanol" as "isopropanol" (according to its molecular formula and function, the two are the same substance, and the name is unified according to Chinese custom).
---Chapter 6 adds 6.1 material requirements (to reduce the difference in test results caused by material differences).
--- Change the 6.1 polishing and fine grinding process requirements of ISO 10629.1996 to the quality requirements of this part 6.2 (conducive to the implementation of the standard).
--- Modify the measurement accuracy of 6.3 size (reduce the difference in surface area of the tested sample).
---The content of Chapter 7 shall be re-divided and modified according to the test requirements and test steps, and the tolerances have been increased (conducive to the implementation of the standard).
---The grade of optical glass alkali resistance stability is tabulated after the decimal point, and the test report format is added.
This section has made the following editorial changes.
--- Amend the standard name to "Colorless Optical Glass Test Method Part 21.Alkali Resistance Stability";
---Informative Appendix A has been added.
Please note that certain contents of this document may involve patents. The issuing agency of this document is not responsible for identifying these patents.
This part was proposed by China Machinery Industry Federation.
This part is under the jurisdiction of the National Optical and Photonics Standardization Technical Committee (SAC/TC103).
Drafting organizations of this section. Chengdu Guangming Optoelectronics Co., Ltd., China Ordnance Industry Standardization Institute, Shanghai Optics, Chinese Academy of Sciences
Institute of Precision Machinery.
The main drafters of this section. Zhou Huimin, Zhou Quanquan, Liu Xiaodong, Su Yong, Li Weina, Hu Junjiang.
Colorless optical glass test method
Part 21.Alkali resistance stability
1 Scope
This part of GB/T 7962 specifies the principle, test procedure, data processing and classification of the alkali resistance stability test method of colorless optical glass.
This section applies to colorless optical glass, other types of glass can be used as reference.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated references, the latest version (including all amendments) applies to this document.
GB/T 903 colorless optical glass
GB/T 1185-2006 Surface defects of optical parts
GB/T 1804-2000 General Tolerances Tolerances of linear and angular dimensions without tolerances (eqvISO 2768-1.1989)
GB/T 6682-2008 Analytical laboratory water specifications and test methods (ISO 3696.1987, MOD)
3 Principle
Put the polished test sample into a sodium hydroxide test solution with a temperature of 50°C and a concentration of 0.01mol/L to etch for a specified time,
Weighing measures the mass loss of the tested sample, and calculates the erosion depth based on the glass density. According to the time t0.1 and the invasion depth required to reach 0.1μm
The change of the surface of the tested sample after the completion of the etching determines the alkali resistance stability level of the tested glass.
4 reagent
4.1 General
During the test, unless otherwise specified, chemical reagents should be used.
4.2 Water
It shall meet the requirements of secondary water specified in GB/T 6682-2008.
4.3 Test solution
Dilute the sodium hydroxide solution with water to control and adjust the pH value so that the pH value = 12 ± 0.1.
4.4 Nitric acid (HNO3)
Dilute with analytical grade to pH 4.5±0.1.
4.5 Sodium hydroxide solution
Concentration cNaOH≈0.1mol/L.
4.6 Isopropanol (C3H7OH)
There is no residue after distillation.
5 Instruments
5.1 Stirrer
The stirrer is made of stainless steel or polytetrafluoroethylene (PTFE). The length of the stirrer rod of the stainless steel stirrer is (350.0±2.5) mm and the diameter is
(10.0±1.0)mm; polytetrafluoroethylene (PTFE) material agitator stirring rod length (350.0±2.5)mm, diameter (15.0±1.0)mm; horizontal blade
The vertical height of the section is (15.0±1.0)mm and the width is (58.0±1.0)mm, as shown in Figure 1.
5.2 Reaction tank
A flat-bottomed cylindrical barrel with a closed lid is made of stainless steel. Its inner diameter is (150.0±2.5)mm, and the height is (200.0±2.5)mm.
Connect the screw and the barrel with the nut, as shown in Figure 2.The lid is made of a wide neck, and there are two hooks at the bottom for hanging the tested sample; the neck
There is a plug with a hole at the mouth to insert the agitator; the allowable deviation of the size without tolerance should meet the minimum requirements specified in Table 1 of GB/T 1804-2000
Rough v grade. The stopper is made of a suitable inert material and should be boiled in sodium hydroxide solution for about 60 minutes.
5.3 Platinum wire or silver wire
Wrap the tested sample with platinum wire or silver wire with a diameter of less than 0.1mm or make a sample frame to support and hold the tested sample.
5.4 Constant temperature bath
The volume is 30L~40L; the thermostatic control is (50.0±0.2)℃.
5.5 Analytical balance
Minimum graduation value. 0.1mg.
5.6 Drying dish
Use silane mixture (absorbing water) and soda lime (a mixture of CaO and Na2O, absorbing CO2) as desiccants.
5.7 Fixture
It is made of a material that does not scratch the smooth surface of the tested sample, for example, plastic.
5.8 Vernier calipers
Minimum graduation value. 0.02mm.
5.9 Ultrasonic equipment
The cleaning tank is filled with water and can be heated to 50°C.
5.10 Beaker
The capacity is 100mL~500mL.
5.11 pH meter
Minimum graduation value. 0.05.
6 Preparation of the tested sample
6.1 Material requirements
The sample to be tested should have no visible stripes or inclusions. The stress birefringence of the rough glass of the tested sample should meet the requirements of GB/T 903.
The central stress birefringence is less than or equal to 6nm/cm.
6.2 Processing quality and quantity
All surfaces of the tested sample are polished, the size is (30.0±0.1)mm×(30.0±0.1)mm×(2.00±0.05)mm, and the surface roughness reaches
Ra=0.012μm, the surface defects reach B/2×0.63 specified in B.1 of GB/T 1185-2006, and the polished chamfer C0.2.Number of tested samples. 6 pieces.
6.3 Calculation of the total surface area
Before cleaning the sample to be tested, perform all size measurements, take three different test positions, and measure the distance and thickness between the two parallel sides.
Degree, whichever is the average value. The measurement accuracy is 0.02mm, and the calculation accuracy of the actual full surface area is 2%. Record the measured value.
6.4 Cleaning pretreatment
The cleaning pretreatment requirements are as follows.
a) The tested sample should be cleaned as soon as possible after polishing. Place three 100mL beakers in an ultrasonic water bath to heat and keep the water
At (45±3)℃. Each beaker should keep enough isopropanol to make it immersed in the cleaned test sample. Wash throughout
During the process, the sample under test should be clamped and moved by the fixture. To avoid contamination of its surface, such as fingerprints.
b) Immerse the test sample in the first beaker and clean it with ultrasonic for about 1 min; then use tissue paper and soft cloth soaked in isopropyl alcohol
Gently wipe the tested sample; then immerse the tested sample in the second and third beakers, and clean them for about 1 min.
c) Isopropanol should be replaced every time a test sample is cleaned in the first beaker. The isopropanol in the second and third beakers should be cleaned.
Test samples should be less than 10, if any contamination of isopropanol is found, it should be replaced immediately.
d) Place the cleaned tested sample in the air to dry naturally or at (115±5)℃ for about 30min.
e) Before the test, the tested sample should be placed in a dry dish.
7 Test steps
7.1 Routine test
7.1.1 The prepared sample to be tested should be used only once. At least two tested samples should be measured at the same time under the same conditions.
7.1.2 Put the reaction tank with 2L test solution into the constant temperature tank, adjust the stirrer to (15±1) mm above the bottom of the reaction tank, and
And keep the temperature at (50.0±0.2)°C.
7.1.3 Use a clamp to clamp the clean tested sample out of the drying dish, put it into an analytical balance and weigh it, and record the mass as m1.
7.1.4 Wrap the tested sample with platinum wire or silver wire in a cross shape or put the tested sample into the sample frame, hang it on the stirrer and react.
The middle of the tank wall. The bottom surface of the tested sample is (50±1.5) mm from the bottom of the reaction tank, as shown in Figure 2.The allowable deviation of the dimension without tolerance in Figure 2
The difference should comply with the roughest v level specified in Table 1 of GB/T 1804-2000.The sample to be tested should not touch the wall of the reaction vessel.
7.1.5 The stirring speed of the stirrer is (100 ± 2) r/min, and the reaction time is calculated according to the immersion time of the tested sample.
7.1.6 After the test is completed, take the tested sample out of the reaction tank, and clean the tested sample according to the following steps, without stopping between steps. in
A set of 250mL beakers are each filled with.200mL of water, nitric acid, isopropanol and other liquids, and each test sample is immersed in the following cycle sequence for about 1s.
a) Dip into the beaker filled with water 5 times, and the water temperature is (50±0.2)℃. Change the water when cleaning the next sample to be tested.
b) Dip in nitric acid once at room temperature.
c) Immerse again in water at room temperature.
d) Immerse in isopropanol 3 times at room temperature.
7.1.7 Clamp the tested sample with a clamp, untie the platinum wire or silver wire or take out the tested sample from the sample frame. Immerse the test sample in isopropanol
It is about 1s, then take it out to dry in the air, and then transfer the clean tested sample to a drying dish to cool to room temperature. Weigh and record immediately
The mass is m2.Calculate the time required for the erosion depth of 0.1μm according to the formula in Chapter 8.Under natural light,
Observe the changes on the surface of the tested sample from a direction close to 45° or under a microscope.
7.2 Unknown test time tested sample test
In order to determine the time required for erosion, the six tested samples prepared as specified in Chapter 6 were initially tested in the order given in Figure 3.
a) Immerse a test sample in the test solution for 1h, and calculate the alkali resistance stability level according to the mass loss or continue to the next step of erosion time (4h or 0.25h).
b) After 1h of erosion, the mass loss of the tested sample is between 1mg/block~4mg/block, and the alkali resistance stability grade can be calculated and judged.
c) After 1h of erosion, if the mass loss of the tested sample is more than 4mg/block, the erosion time of the tested sample is adjusted to 0.25h; if the mass loss of the tested sample is less than 1mg/block, the erosion time is adjusted to 4h.
d) After corrosion for 0.25h or 4h, the mass loss of the tested sample is >1mg/piece, and the alkali resistance stability level can be calculated and determined;
After 0.25h, if the mass loss of the tested sample is less than 1mg/piece, the data after 1h of erosion is directly used to calculate the alkali resistance stability, etc.
Grade; after 4h of erosion, the mass loss of the tested sample is less than 1mg/block, and further erosion is required for 16h.
e) After initially determining the test time according to the above steps, follow 7.3.
7.3 Test of the tested sample with known test time
If the integer level of the alkali resistance stability of the optical glass is known or the corrosion time has been determined according to 7.2, the following steps should be used.
a) Immerse two test samples in the same test solution for a specified time (for example, 0.25h, 1h or 4h, etc.). If it is corroded after 4h,
If the weight loss of the tested sample is less than 1mg/block, it will be further eroded for 16h; if the mass loss of the tested sample is still less than 1mg/block after the erosion, the alkali resistance stability level is calculated and judged.
b) If the mass loss of the tested sample is more than 4mg/piece after 1h of erosion, the erosion time needs to be shortened, as shown in Figure 3.
c) If the mass loss of the tested sample is between 1mg/block~4mg/block after 1h of erosion, calculate the alkali resistance stability grade.
d) Either the mass loss of the tested sample after 1h or 4h is greater than 1mg/piece, or the alkali resistance stability grade is calculated and judged according to the test result of 16h erosion.
8 Result calculation
According to the measured average value of the mass loss (m1-m2) of the two tested samples, according to the provisions of 7.3, the time required to erode the surface layer of the tested sample to 0.1 μm is calculated according to the following formula t0.1(h).
9 Classification and judgment
9.1 Integer grade of alkali resistance stability
According to the time t0.1 required to corrode the 0.1μm surface layer of the tested sample, the integer grade of the alkali resistance stability of the optical glass is judged according to Table 1.
9.2 Alkali resistance stability
The measurement of level m2 after the decimal point is in Chapter 7, and the calculation is in Chapter 8.
Use the naked eye to qualitatively determine the surface change of the tested sample, and determine the grade after the decimal point of the alkali resistance stability of the optical glass according to Table 2.
10 Test report
10.1 The test report should include the following information.
a) The standard number of this part.
b) Glass density (g/cm3).
c) The surface area of the tested sample (cm2).
d) The time (h) required for the test sample to be eroded to a depth of 0.1μm, calculate and determine the integer level of the alkali resistance stability of the glass; and observe the changes on the surface of the test sample,
Determine the decimal point level of the alkali resistance stability of the tested sample.
e) Determine the alkali resistance stability class AR.
f) Record any abnormal characteristics during the test.
10.2 See Table 3 for the format of the alkali resistance stability test report.
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