Overview of Glass Durability Tests

Acid resistance tests

Chemical durability of glasses is a property that has been measured by a large number of variations of several methods. For the purpose of comparing results obtained in different laboratories, every technologically developed country has issued its own standards and norms regulating all essential details of each widely used method of chemical durability measurements. Quite often the authors, when presenting the results of their measurements, simply refer to the corresponding standard without describing of the details of the measurements.

Below, the most widely used standards of acid resistance tests are presented.

ACS. Method No.1

Grains with particle size 295-417 \(\mu\)m. Mass 10 g. Attack agent 0.02 N H2SO4. Temperature 90\(^{\circ}\)C\(\pm\)0.5. Test duration 4 h. Solution volume 50 ml. After testing, a flask is cooled quickly in running water, and a phenol red indicator is added. Then 0.02 N NaOH (free from CO₂) until in about 1 ml excess is added. The solution is titrated with 0.02 N H₂SO₄ until the color changes from red to yellow. The Calculation is done according to the formula:

Wt.% Na₂O = (ml 0.02 N H₂SO₄ used - ml 0.02 N NaOH used)*0.00062*100/10

Note

Information was taken from (Report of the committee on the chemical durability of glass, 1935) [see References].

CSN 70 0532

Similar to DIN 12116 (I), GOST 10134.2-82, and TGL 14801.

DIN 12116

Pruefung von Glas: Griessverfahren zur Pruefung der Saurebestandigkeit (gravimetrisches Verfahren) und Einteilung der Glaeser in Saureklassen.

Similar to CSN 70 0532, GOST 10134.2-82, and TGL 14801.

Bulk samples with surface area ~200 cm². Attack agent 6 N HCl. Temperature 108\(^{\circ}\)C. Test duration 3 h. Solution volume 550-600 ml. The results are expressed as weight loss, mg/dm² of glass.

Acid class	Weight loss, mg/dm2
1	To 0.7
2	Above 0.7 to 1.5
3	Above 1.5 to 20

Note

Information was taken from (Steklo, 1973) [see References]. This version of the standard was valid through May 1976.

Pruefung von Glas: Griessverfahren zur Pruefung der Saurebestandigkeit (gravimetrisches Verfahren) und Einteilung der Glaeser in Saureklassen.

Bulk samples with surface area ~300 cm². Attack agent boiling 6 N HCl. Test duration 6 h. Solution volume ~600 ml. The results are expressed as half of weight loss, mg/dm² of glass.

Acid class	Designation	Half of surface weight loss after 6 hours, mg/dm2
1	Acid-resistant	To 0.7
2	Weakly acid-soluble	Above 0.7 to 1.5
3	Moderately acid-soluble	Above 1.5 to 15
4	Strongly acid soluble	Above 15

Note

Information was taken from (Scholze, 1991) [see References]. This version of the standard was valid through May 1976.

GOST 9111-59

Steklo Khimiko-Laboratornoe. Tekhnicheskie Trebovaniya. Metody Ispytaniya.
[Laboratory Glass Ware. Technical Conditions. Methods of Tests]. Acid resistance.

Samples in the form of rods, initially annealed. Surface area 100-200 cm². Boiling in 1 N H₂SO₄ The level of the acid should be 1 cm above the upper ends of samples. Test duration 2 h. The results are expressed as weight loss in mg per 100 cm² of glass surface.

Types of glasses	Weight losses, mg/100 cm2
Chemically durable, 1 class (KhU-1)	Not greater than 0.5
Chemically durable, 2 class (KhU-2)	Greater than 0.5 but not greater than 1.0
Thermally durable (TU)	Not greater than 0.5

GOST 10134-62

Steklo Neorganicheskoe i Steklokristallicheskie Materialy. Metod Opredeleniya Khimicheskoi Stoikosti.
[Inorganic Glass and Glass-Crystal Materials. Method for the Determination of Chemical Resistance]

Grains with particle size 500-800 \(\mu\)m. Mass ~10 g. Solution volume 100 ml. Boiling in 1N HCl. Test duration 3 h. The results are expressed as weight losses in percent.

GOST 10134.2-82

Steklo Neorganicheskoe i Steklokristallicheskie Materialy. Metod Opredeleniya Khimicheskoi Stoikosti.
[Inorganic Glass and Glass-Crystal Materials. Method for the Determination of Chemical Resistance]

Similar to CSN 70 0532, DIN 12116 (I), and TGL 14801.

Samples are in the form of plates or other forms permitting the precise determination of sample surface (with an error not higher than 2%). Surface area 2.0-4.0 dm². Solution volume 500-600 ml. Boiling in 6N HCl. Test duration 3 h.

The results are expressed as weight losses in mg/dm².

Class of acid resistance	Weight loss, mg/dm2
1	Not greater than 0.7
2	Greater than 0.7 but not greater than 1.5
3	Greater than 1.5

GOST 21400-75

Steklo Khimiko-Laboratornoe. Tekhnicheskie Trebovaniya. Metody Ispytaniya.
[Laboratory Glass Ware. Technical Conditions. Methods of Tests]. Acid resistance.

Bulk samples with surface area ~400 cm². Boiling in 20.4% HCl for 6 h. Solution volume 500-600 ml.

The results are expressed as a half-weight loss in mg/cm².

Groups of acid resistance	Weight loss, mg/dm2
KhS1	Not greater than 0.004
KhS2	Not greater than 0.005
KhS3	Not greater than 0.006

TGL 14801

Similar to CSN 70 0532, DIN 12116 (I), and GOST 10134.2-82.

Alkali resistance tests

Chemical durability of glasses is a property that has been measured using a large number of variations of several methods. For the purpose of comparing results obtained in different laboratories, every technologically developed country has issued its own standards and norms regulating all essential details of each widely used method of chemical durability measurements. Quite often the authors, when presenting the results of their measurements, simply refer to the corresponding standard without describing the details of the measurements.

Below, the most widely used standards of alkali resistance tests are presented.

CSN 70 0533

Glass - Determination of Resistance to Attack by a Boiling Aqueous Solution of Mixed Alkali. Method of Test.

Similar to DIN 12122, DIN 52322, GOST 10134.3-82, GOST 19810-85, GOST 21400-75, ISO 695, and TGL 14802.

Sample pieces with surface area 10-15 cm². A boiling solution of mixed alkali - 1:1 mixture of 1N NaOH and 1 N Na₂CO₃. Solution volume 800 ml. Test duration 3 h. Silver or silver alloy vessel. The results are expressed as weight loss of glass mg per dm².

Alkali class	Weight loss, mg/dm2
A 1	To 75
A 2	Above 75 to 175
A 3	Above 175

DIN 12122

Similar to CSN 70 0533, DIN 52322, GOST 10134.3-82, GOST 19810-85, GOST 21400-75, ISO 695, and TGL 14802.

DIN 52322

Similar to CSN 70 0533, DIN 12122, GOST 10134.3-82, GOST 19810-85, GOST 21400-75, ISO 695, and TGL 14802.

GOST 111-41

Steklo listovoe okonnoe mashinnoy vyrabotki
[plate window glass]

Samples in the form of plates, 10x5 cm² (for a test, several samples should be used). Boiling in 1N solution of Na₂CO₃. Solution volume 600 ml. Test duration 3 h. The results are expressed as weight loss in mg/dm². The quality of glass is considered as acceptable if the weight loss does not surpass 38 mg/dm².

GOST 111-54

Steklo listovoe okonnoe mashinnoy vyrabotki
[plate window glass]

Samples in the form of plates, 10x5 cm² (for a test, several samples should be used). Boiling in 1N solution of Na₂CO₃. Solution volume 600 ml. Test duration 3 h. The results are expressed as weight loss in mg/dm². The quality of glass is considered as acceptable if the weight loss does not surpass 32 mg/dm².

GOST 9111-59

Steklo Khimiko-Laboratornoe. Tekhnicheskie Trebovaniya. Metody Ispytaniya.
[Laboratory Glass Ware. Technical Conditions. Methods of Tests]. Alkali resistance.

Samples in the form of rods, initially annealed. Surface area 100-200 cm². Boiling in 2N solution of NaOH. The level of the solution should be 1 cm above the upper ends of samples. Test duration 2 h. The results are expressed as weight loss in mg per 100 cm² of glass surface.

Types of glasses	Weight losses, mg/100 cm2
Chemically durable, 1 class (KhU-1)	Not greater than 60
Chemically durable, 2 class (KhU-2)	Greater than 60 but not greater than 70
Thermally durable (TU)	Not greater than 90

GOST 10134-62

Steklo Neorganicheskoe i Steklokristallicheskie Materialy. Metod Opredeleniya Khimicheskoi Stoikosti.
[Inorganic Glass and Glass-Crystal Materials. Method for the Determination of Chemical Resistance]

Grains with particle size 500-800 \(\mu\)m. Mass ~10 g. Solution volume 100 ml. Boiling in 1 N solution of NaOH. Test duration 3 h. The results are expressed as weight losses in percent.

GOST 10134.3-82

Steklo Neorganicheskoe i Steklokristallicheskie Materialy. Metod Opredeleniya Khimicheskoi Stoikosti.
[Inorganic Glass and Glass-Crystal Materials. Method for the Determination of Chemical Resistance]

Similar to CSN 70 0533, DIN 12122, DIN 52322, GOST 19810-85, GOST 21400-75, ISO 695, and TGL 14802.

GOST 19810-85

Steklo Meditsinskoe. Metod Opredeleniya Shchelochestoikosti.
[Medical Glass. Method for the Determination of Alkali Resistance] Similar to CSN 70 0533, DIN 12122, DIN 52322, GOST 19810-85, GOST 10134.3-82, GOST 21400-75, ISO 695, and TGL 14802.

GOST 21400-75

Steklo Khimiko-Laboratornoe. Tekhnicheskie Trebovaniya. Metody Ispytaniya.
[Laboratory Glass Ware. Technical Conditions. Methods of Tests]. Alkali resistance. Similar to CSN 70 0533, DIN 12122, DIN 52322, GOST 19810-85, GOST 10134.3-82, ISO 695, and TGL 14802.

ISO 695

Glass - Determination of Resistance to Attack by a Boiling Aqueous Solution of Mixed Alkali. Method of Test.

Similar to CSN 70 0533, DIN 12122, DIN 52322, GOST 19810-85, GOST 10134.3-82, GOST 21400-75, and TGL 14802.

Chemical durability of nuclear waste glasses

ASTM Standard C 1285-97 (the same C 1285-94)

The Product Consistency Test (PCT) (method described the behavior of the glass in concentrated solutions)

Method PCT-A
The method was developed to test the chemical durability of radioactive waste glasses during production. The glass does not need to be annealed prior to testing. Grains with particle size 74-149 mm, mass >= 1 g are placed in a stainless steel vessel. An amount of ASTM Type I water - equal to 10 cc/g of sample mass is added and the vessel is sealed. Test duration 7 days \(\pm\)3.4 h under static conditions. Temperature 90\(\pm\)2\(^{\circ}\)C. SA/V=2000 -2400 m^-1.

The leachate is filtered and analyzed for boron, silicon and all alkali elements in the glass at > 1 wt.%. All tests for each glass should be carried out at least in triplicate. The results are expressed as the concentration of the elements in solution, and as the concentration of the elements in solution is normalized by the weight fraction of that element present in the glass.

Method PCT-B.
The method cannot be used as a consistency test for production of high-level radioactive waste glass. Procedure is the same as procedure of the PCT-A Method.

1. Test vessel - stainless steel or PFA TFE - fluorocarbon.

2. Leachant - specific distilled water or other solutions.

3. Test duration 7 days \(pm\) 3.4 h or varying times.

4. Particle size-74-149 \(\mu\)m or < 420 \(\mu\)m.

5. Leachant volume - 10 cc/g of sample mass or variable volume/sample mass.

6. Temperature 90 \(\pm\)2\(^{\circ}\)C or other.

ASTM Type I water
Purified water with a maximum total matter content including soluble silica of 0.1 g/m³, a maximum electrical conductivity of 0.056 \(\mu\)Ohm/cm at 25\(^{\circ}\)C.

ASTM Standard C 1220-92

Standard Test Method for Static Leaching of Monolithic Waste Forms for Disposal of Radioactive Waste (MCC-1, MCC-2, MCC-3).

MCC-1 test

The size or shape of the samples is not critical, but a surface area of about 400 mm² is recommended (Method excludes study of powdered materials).

Three leachants are used:

1. High purity (ASTM Type I or II) water.

2. Silicate/bicarbonate water prepared by dissolving 0.179 g NaHCO3 and 0.058 g SiO2 as silicic acid in sufficient water to make about 900 ml of solution. Adjusting the pH to within 0.1 of 7.5 with 0.01 N HCl. Adding water to make 1.0 l of solution.

3. Brine prepared by dissolving 48.2 g KCl, 90 g NaCl and 116 g MgCl₂ (247.9 g MgCl₂·6H₂O).

Both aerated and deaerated solutions may be used.

Deaerated conditions and argon atmosphere for highly radioactive specimens are used. Testing under static conditions. Polytetrafluoroethylene (PTFE) vessels at low radiation levels, <10⁴ rad are used. Stainless steel or fused silica vessels at radiation levels <10⁴ rad are used. The surface area to volume ratio (SA/V) is held constant within 0.5 of 10.0 m^-1. Three temperatures (40, 70 and 90\(^{\circ}\)C) and a number of specific time periods (3, 7, 14, 28, 56, 91, 182 or 364 days) can be used for different purposes.

Five test materials are used that vary from short quality control testing to long duration tests to establish the mechanisms of leaching:

Matrix A

Leachant - water.

Temperature - 90\(^{\circ}\)C.

Test duration - 7 days.

Preparing and testing one blank for 7 days for each group of samples tested simultaneously in the same environmental test chamber.

Matrix B

Leachants water, silicate water or brine.

Temperature - 90\(^{\circ}\)C.

Test duration - 28 days.

Using the following matrix giving the number of specimens:

Test period, days	Number of specimens
3	1
7	1
14	1
28	3

Preparing and testing two blanks of each leachant for 28 days under identical test conditions but excluding a specimen.

Matrix C

The required test temperature is 90\(^{\circ}\)C. Also use 40\(^{\circ}\)C or 70\(^{\circ}\)C, or both. The procedure is otherwise identical to Matrix B.

Matrix D

Leachants - water, silicate water or brine.

Temperature - 90\(^{\circ}\)C.

Using all or selected portions of the following matrix ("Selected portions" means, for instance, that only one leachant may be used.) Also, the test may be terminated at 56 days or at any longer duration shown in the matrix. Suitable blanks must be carried through to the end of the test.

Test period, days	Number of specimens
7	1
14	1
28	1
56	3
91	1
182	3
364	1
Optional 12-month intervals	3

Preparing and testing two blanks at 28, 91, and 364 days (and yearly thereafter to the culmination of the test when it extends beyond 364 days) in each leachant under identical test conditions but excluding a specimen.

Matrix E

The same as matrix D, but temperatures 40\(^{\circ}\)C, 70\(^{\circ}\)C and 90\(^{\circ}\)C are used.

MCC-2 test
This test is performed at temperatures >100\(^{\circ}\)C but <200\(^{\circ}\)C. The reference temperatures are 100, 150 and 190\(^{\circ}\)C. Five test matrixes similar to those in MCC-1 are used.

MCC-3 test This is the only test using powdered specimens. Constant agitation is used, but in other respects the test matrices are the same as MCC-2.

METHOD 1311
Toxicity characteristic leaching procedure (TCLP)

Grains with particle size <=9.5 mm in diameter. Mass ~100 g as minimum. Two leaching solutions may be used. Determing the appropriate fluid for testing as follows:

1. 5 g grains with particle size ~1 mm or less in diameter are placed in 96.5 ml of ASTM Type II water. Stirring for 5 minutes using a magnetic stirrer. If the pH is <5, fluid Nl - sodium acetate/acetic acid buffer solution with pH 4.93\(\pm\)05 is used.

2. If the pH from section 1 is >5, is added 3.5 ml 1N HCI and heated at 50\(^{\circ}\)C for 10 minutes. If the pH (after cooling to room temperature) is <5, fluid Nl is used. If the pH>5, fluid N₂ - CH₃COOH solution with pH 2.88\(\pm\)0.05 is used.

Solution mass is equal to 20 times the mass of the grains. Testing is produced in agitation apparatus that rotates the extraction vessel in an end-over-end fashion at 30\(\pm\)2 rpm for 18\(\pm\)2 hours at temperature 23\(\pm\)2\(^{\circ}\)C.

TCLP extracts should be analyzed as soon as possible following extraction. The results are expressed as the leachates concentrations in ppm.

Note

Information was taken from (Strachan, Turcotle, Barnes, 1982), and from: (Johnston, Daniel, 1982): [see References].

Acid Resistance Test. ASTM Standard C-225

Resistance of glass containers to chemical attack

Method B-A. Resistance of bottles to attack by dilute acid

Filling the containers, at room temperature, to 90% of overflow capacity with 0.0005 N H₂SO₄ (If the bottles to be tested neutralize less than the equivalent of 0.80 ml of 0.020 N H₂SO₄, use 0.0002 N H₂SO₄ as attacking medium). Maintaining the temperature at 121\(\pm\)0.5\(^{\circ}\)C (250\(\pm\)0.9\(^{\circ}\)F) for 1 h in autoclave, counting from the time when the holding temperature is reached. The results are expressed as milliliters of 0.020 N H₂SO₄ consumed in the test, calculated as follows:

ml of 0.02 N H₂SO₄ consumed = V - 0.98B,

where:

V - ml of 0.020 N NaOH solution equivalent to 100 ml of the attacking medium,

B - ml of 0.020 N NaOH solution used in the titration of 100 ml of bottle extract, and

0.98 - factor applied to the titration of the bottle extract for loss of attacking medium during cooling of the autoclave.

Dimming resistance tests

Chemical durability of glasses is a property that has been measured by a large number of variations of several methods. For the purpose of comparing results obtained in different laboratories, every technologically developed country has issued its own standards and norms regulating all essential details of each widely used method of chemical durability measurements. Quite often the authors, when presenting the results of their measurements, simply refer to the corresponding standard without describing of the details of the measurements.

Below, the most widely used standards of dimming resistance tests are presented. The dimming resistance test is one of the characteristics of weathering resistance.

GOST 3514-57

Steklo Opticheskoe Bestsvetnoe. Technicheskie Usloviya.
[Optical Colorless Glass. Technical Norms].

Test of resistance of optical glass to humid atmosphere. Freshly well-polished glass is kept in the atmosphere with 85% controlled relative humidity at 50\(^{\circ}\)C for 5-20 h. Examination under a microscope. Magnification 80x. The glass is then classified according to the number of hours necessary for a visible haze appearance.

Dimming test group	Time, h
A	Above 20
P	Above 5 to 20
V	Less than 5

Note

The haze on the glass surface results from the formation of tiny droplets due to the hygroscopicity of the glass.

GOST 13917-68

Steklo Opticheskoe.Metody Opredeleniya Khimicheskoi Ustoichivosti.
[Optical Glass. Methods of Determination of Chemical Durability].

a. Silicate glasses

Test of resistance of optical glass to humid atmosphere. Freshly well-polished glass is kept in air atmosphere with 73% controlled relative humidity at 50\(^{\circ}\)C for 5-20 h. Examination under a microscope. Magnification 80x. The glass is then classified according to the results of inspection of the glass surface.

Group of resistance to humid atmosphere	Time of keeping in humid atmosphere, h	Characteristics of glass surface
A - stable	20	No changes
B - intermediate stability	5 - 20	Haze
V - unstable	5	Haze

Note

The haze on the glass surface results from the formation of tiny droplets due to the hygroscopicity of the glass.

b. Nonsilicate glasses (glasses containing less than 30 mol.% of SiO2)

Test of resistance of optical glass to humid atmosphere. Freshly well-polished glass is kept in air atmosphere with 73% controlled relative humidity at 80\(^{\circ}\)C for 10 h. Examination under a microscope. Magnification 80x. The glass is then classified according to results of examinations.

Group of resistance to humid atmosphere	Characteristics of glass surface
a - stable	No changes
u - intermediate stability	Surface corrosion is seen by microscope but does not be seen by eye in a reflected light
d - unstable	Surface corrosion is seen by eye in a reflected light

GOST 13917-82

Steklo Opticheskoe.Metody Opredeleniya Khimicheskoi Ustoichivosti. [Optical Glass. Methods of Determination of Chemical Durability].

Test of resistance of optical glass to humid atmosphere. Freshly well-polished glass is kept in the atmosphere with 85% controlled relative humidity at 50\(^{\circ}\)C for 5-20 h. Examination under a microscope. Magnification 25-80x. The glass is then classified according to the number of hours necessary for a visible haze appearance.

Group of resistance to humid atmosphere	Time, h	Characteristic of polished surface
A	20	No degradation
B	20	Uniform haze
V	5	Uniform haze
G	2	Uniform haze

Note

The haze on the glass surface results from the formation of tiny droplets due to the hygroscopicity of the glass.

Staining resistance tests

Chemical durability of glasses is a property that has been measured by a large number of variations of several methods. For the purpose of comparing results obtained in different laboratories, every technologically developed country has issued its own standards and norms regulating all essential details of each widely used method of chemical durability measurements. Quite often the authors, when presenting the results of their measurements, simply refer to the corresponding standard without describing of the details of the measurements.

Below, the most widely used standards of staining resistance tests are presented. Staining resistance tests are one of the characteristics of weathering resistance.

GOST 13917-68

Steklo Opticheskoe.Metody Opredeleniya Khimicheskoi Ustoichivosti.
[Optical Glass. Methods of Determination of Chemical Durability].

Determination of resistance to leaching by observation of an interference effect. Freshly well-polished glass is kept in 0.1N CH₃COOH solution or in distilled H₂O at 50\(^{\circ}\)C for 1-5 h. The glass is then classified according to a number of hours of leaching necessary to observe a violet color of a light reflected from the surface of the sample, which is indicative of certain thickness of the layer with lower refractive index.

Stain test group	Acid consumption of 0.01 N HCl, ml	Base equivalent as Na2O, \(\mu\)g/g
I	CH3COOH	5
II	CH3COOH	from 5 to 1
III	CH3COOH	1
IV	Distilled H2O	1

GOST 13917-82

Steklo Opticheskoe.Metody Opredeleniya Khimicheskoi Ustoichivosti.
[Optical Glass. Methods of Determination of Chemical Durability].

Freshly well polished glass samples 20x20x10 mm are kept in 0.1N CH₃COOH solution or in distilled water at 50\(^{\circ}\)C for 15-300 min. It is assumed that formation of a leached layer with a thickness greater than 0.1 \(\mu\)m leads to a decrease in the coefficient of reflection greater than 0.004. The time of leaching required for a given decrease in reflection coefficient (\(\Delta R_{v}\)) is a basis for determination of the group of acid resistances.

Group of acid resistance	Leaching time, min	Reagent	\(\Delta R_{v}\)
1	300	CH3COOH	less than 0.004
2	>60 up to 300	CH3COOH	0.004 or greater
3	>15 up to 60	CH3COOH	0.004 or greater
4	>15 up to 60	Distilled H2O	less than 0.004
5	>15 up to 60	Distilled H2O	0.004 or greater0.004 or greater
6	15 or less	Distilled H2O	0.004 or greater

Water resistance tests

Chemical durability of glasses is a property that has been measured by a large number of variations of several methods. For the purpose of comparing results obtained in different laboratories, every technologically developed country has issued its own standards and norms regulating all essential details of each widely used method of chemical durability measurements.

Quite often the authors, when presenting the results of their measurements, simply refer to the corresponding standard without describing of the details of the measurements. Below, the most widely used standards of water resistance tests are presented.

ASTM STANDARD C 225-54

Test Method B-W. Resistance of bottles to attack by distilled water.
Similar to CSN 70 0529 and SIS 711032.

Selection of either three bottles (if their capacity is equal of higher than 6 oz) or a sufficient number of bottles so that the contents can be combined to form three sets to give 100 ml per set. Rinsing each container with two portions of the special distilled water. Filling the containers, at room temperature, to 90% of overflow capacity with the same kind of water. Maintaining the temperature at 121\(\pm\)0.5\(^{\circ}\)C (250\(\pm\)0.9 \(^{\circ}\)F) for 1 h in autoclave, counting from the time when the holding temperature is reached. The results are expressed as milliliters of 0.02 N H₂SO₄ used for titration of 100 ml bottle extract, less the titration of the blank.

Test Method P-W. Resistance of powdered sample to attack by distilled water.
Grains with particle size 297-420 \(\mu m\). Mass 10 g. Addition of 50 ml of special distilled water to the sample. Maintaining the temperature at 121\(\pm\)0.5 \(^{\circ}\)C (250\(\pm\)0.9 \(^{\circ}\)F) for 30 min, counting from the time when the holding temperature is reached. As the measure of water resistance, the number of ml of 0.02 N H₂SO₄ used to neutralize the extract from 10 g of glass less the titration of the blank is taken.

CSN 70 0529

Similar to ASTM STANDARD C 225-54 [Test Method B-W] and SIS 711032.

CSN 70 0531

The Testing of Glass - Determination of Resistance to Water (Grain Titration Method)
Similar to DIN 12111, GOST 10134.1-82: METHOD A, GOST 21400-75, ISO 719, and TGL 14809.

Grains with particle size 315-500 \(\mu m\). Mass 2 g. Solution volume 50 ml. Special distilled water. Temperature 98\(^{\circ}\)C. Test duration 1 h. Titration of 25 ml of the extract solution with 0.01 N HCl against methylene red. The consumption of acid less the titration of the blank serves to characterize the hydrolytic class:

Hydrolytic class	Acid consumption of 0.01 N HCl, ml	Base equivalent as Na2O, \(\mu\)g/g
1	To 0.1	To 31
2	Above 0.1 to 0.2	Above 31 to 62
3	Above 0.2 to 0.85	Above 62 to 264
4	Above 0.85 to 2.0	Above 264 to 620
5	Above 2.0 to 3.5	Above 620 to 1085

DGG METHOD

Standard test for total substance leached out of powdered glass.

Similar to SIS 136321.

Grains with particle size 300-490 \(\mu m\). Mass 10 g. Solution volume 100 ml. Boiling Special distilled water. Test duration 5 h. It is then filtered through a 7 cm quantitative filter with a black band. As a measure of water resistance the amount of residue in mg, obtained by the evaporation of 75 ml liquid at 150\(^{\circ}\)C to a constant weight is taken.

The amount of residue substance serves to characterize the hydrolytic class:

Hydrolytic class	Acid consumption of 0.01 N HCl, ml
I	0 - 10
II	10 - 15
III	15 - 25
IV	25 - 50
V	Over 50

Note

Information was taken from (Volf, 1961) [see References].

DIN 12111

Pruefung von Glas: Griessverfahren zur Pruefung der Wasserbestandigkeit von Glas als Werkstoff bei 98\(^{\circ}\)C und Einteilung der Glaeser in hydrolytische classen

Similar to CSN 700 531, GOST 10134.1-82: METHOD A, GOST 21400-75, ISO 719, and TGL 14809.

Note

Information was taken from (Scholze, 1991) [see References].

GOST 9111-59

Steklo Khimiko-Laboratornoe. Tekhnicheskie Trebovaniya. Metody Ispytaniya.
[Laboratory Glass Ware. Technical Conditions. Methods of Tests]. Water resistance.

Samples in the form of rods, initially annealed. Surface area 100-200 cm². Boiling in distilled water. The level of the solution should be 1 cm above the upper ends of samples. Test duration 5 h. The results are expressed as weight loss in mg per 100 cm² of glass surface.

Types of glasses	Weight losses, mg/100 cm2
Chemically durable, 1 class (KhU-1)	Not greater than 2.0
Chemically durable, 2 class (KhU-2)	Not greater than 2.0
Thermally durable (TU)	Not greater than 1.7

GOST 10134-62

Steklo Neorganicheskoe i Steklokristallicheskie Materialy. Metod Opredeleniya Khimicheskoi Stoikosti.
[Inorganic Glass and Glass-Crystal Materials. Method for the Determination of Chemical Resistance]

Grains with particle size 500-800 \(\mu m\). Mass ~10 g. Solution volume 100 ml. Boiling special distilled water. Test duration 5 h. The results are expressed as weight losses in percents.

According to the additional official document (OST 11027.035-79), the data can be used for characterization of hydrolytic classes:

Hydrolytic class	Weight loss, %
I	To 0.08
II	Above 0.08 to 0.12
III	Above 0.12 to 0.22
IV	Above 0.22 to 0.44
V	Above 0.44

GOST 10134.1-82: METHOD A

Steklo Neorganicheskoe i Steklokristallicheskie Materialy. Metod Opredeleniya Vodostoikosti.
[Inorganic Glass and Glass-Crystal Materials. Method for the Determination of Water Resistance]. Method A: for glasses containing R₂O.

Similar to CSN 70 0531, DIN 12111, GOST 21400-75, ISO 719, and TGL 14809.

GOST 13905-78

Tara Steklyannaya. Metod Opredeleniya Vodostoikosti Vnutrennei Poverkhnosti.
[Glass Containers. Method of Determination of Water Resistance of Inner Surface.]

Not less than ¾ of a container is filled by freshly prepared distilled water. The container with water is placed in a vessel with water which should be heated until boiling for not longer than 15 min. Time of boiling 1 h. From each container a probe of 50 cm³ is taken. Water resistance is expressed by the amount of 0.01 N HCl (in cm³) needed for titration of 50 cm³ of the probe less the titration of the blank.

GOST 19809-85

Steklo Meditsinskoe. Metod Opredeleniya Vodostoikosti.
[Medical Glass. Determination of Water Resistance].

Grains with particle size 300-425 m. Mass 10 g. Solution volume 50 ml. Special distilled water. Treatment in an autoclave at 121\(\pm\)0.5 \(^{\circ}\)C for 30 min counting from the time when the holding temperature is reached. As a measure of hydrolytic resistance, the number of milliliters of 0.02 N HCl used to neutralize the extract form 10 g of glass less the titration of the blank is taken. The consumption of acid is converted to an equivalent amount of Na₂O. The results are related to 1 g of glass.

Hydrolytic class	ml 0.02 N HCl/1 g glass	\(\mu\)g Na2O /g glass
HGA 1	To 0.1	To 62
HGA 2	Above 0.1 to 0.85	Above 62 to 527
HGA 3	Above 0.85 to 1.5	Above 527 to 930

Similar to ISO 720.

GOST 21400-75

Steklo Khimiko-Laboratornoe. Tekhnicheskie Trebovaniya. Metody Ispytaniya.
[Laboratory Glass Ware. Technical Conditions. Methods of Tests]. Water resistance.

Similar to CSN 70 0531, DIN 12111, GOST 10134.1-82: METHOD A, ISO 719, and TGL 14809.

ISO-719

Glass-Hydrolytic Resistance of Glass Grains at 98\(^{\circ}\)C. Method of Test and Classification.

Similar to CSN 70 0531, DIN 12111, GOST 10134.1-82: METHOD A, GOST 21400-75, and TGL 14809.

ISO-720

Glass-Hydrolytic Resistance of Glass Grains at 121\(^{\circ}\)C. Method of Test and Classification.

Similar to GOST 19809-85.

JIS R-3502

Grains with particle size 250-420 \(\mu\)m. Mass 2 g. Solution volume 50 ml. Boiling distilled water. Test duration 1 h. Water resistance is expressed in wt. percent of dissolved alkali.

Note

The description of the standard was taken from (Ikeda, Kaite, and Ikuma, 1983): [see References].

SIS 136321

Similar to DGG METHOD.

SIS 711032

Similar to ASTM STANDARD C 225-54 [Test Method B-W] and CSN 70 0529.

TGL 14809

Similar to CSN 70 0531, GOST 10134.1-82: METHOD A, GOST 21400-75, DIN 12111, and ISO 719.

Weathering test

The Mylius iodeosine method.

Test of chemical durability under the influence of a highly-humid atmosphere (Mylius,1923): see References. Aging a freshly fractured glass surface in a saturated water vapor atmosphere at 18\(^{\circ}\)C for 7 days. A subsequent immersion in an ether solution of iodeosine for 1 min. The alkali on the glass surface forms an alkali salt of iodeosine which is then dissolved in water and determined colorimetrically. The results are expressed as mass (in mg) of iodeosine per m² of glass (the weathering alkalinity).

Hydrolytic class	mg/m2
I	0-5
II	5-10
III	10-20
IV	20-40
V	Above 40