180 719-1985 (6) International Standard ISO 719 |RTERNATIONAL ORGANIZATION FOR ET ANDAROIZATIONERAY MAPODWAR OPT ANTHALINANO CTAM/JPTVGAAISONGANSATION ATERWATIONALE D5 NORMALISATION Glass — Hydrolytic resistance of glass grains at 98 °C — Method of test and classification Verre ~ Résistance hydrolytique du verre on grains & 98 °C — Méthode d'essel et elasstcation Second edition — 1985-10-01 COPIA LEGAL AUTORIZADA por convenio con [RAM Instituto Argentino de Normalizaci6n SENTRO DE DOCUMENTACION UDC 666.1: 620.193.4 Ref. No. SO 719-1985 (E) Doseriptors : gloss, teste, boling tomporature tests, determination, hyeralysc resistance, classification, designation. Price based on 5 pagesForeword 1SO {the International Organization for Standardization) is a worldwide federation of national standards bodies {ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committoos. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, govern ‘mental and non-governmental, in fiaison with ISO, also take part in the work. Draft Intemational Standards adopted by the technical committees are circulated to the member bodies for approval before their acceptance as international S-andards by the ISO Council. They are approved in accordance with ISO procedures ‘equiring at least 75 % approval by the member bodies voting. International Standard ISO 719 was prepared by Technical Committee SO/TC 48, Laboratory glassware and related apparatus. 180 719 was first published in 1981. This second edition cancels and replaces the first ‘edition, of which it constitutas a technical revision. Users should note that all International Standards undergo revision from time to time and that any reference made herein to any other International Standard impos its latest edition, unless otherwise stated. © International Organization for Standerdization, 1985 © Printed in SwitzerandINTERNATIONAL STANDARD 1$0 719-1985 (E) Glass — Hydrolytic resistance of glass grains at 98 °C — Method of test and classification 1 Scope and field of application ‘This International Standard specifies ‘}_a method for determining the hydrolytic resistance of ‘lass grains at 98 °C. The resistance is measured and ‘expressed by the volume of acid required for tiation of the alkali extracted from the unit mass of glass, and may also be ‘expressed by the amount of sodium oxide equivalent to this volume of aci b) a classification of glass according to the hydrolytic resistance determined by the method of this International Standard, This International Standard is intended for use on the less resis tant types of glass. For the more resistant glasses, the metho specified in ISO 720 is preferable. NOTE ~ It is emphasized that theres no exect correlation between the ication lad down in this Intemational Standard and that lal jown in ISO. 720, ard it is therefore essential to identity which classification ie being used. 2 References 'S0386/1, Laboratory glassware — Burettes — Part 1: Genera! requirements. 180 385/2, Laboratory glassware — Burettes ~ Part 2: Burettes Tor which no waiting time is specified. 1S0 565, Test sieves — Woven metal wire cloth, perforated plate and electroformed sheet — Nominal sizes of openings. 1S0 648, Laboratory glassware — One-mark pipettes. 1S0 720, Glass — Hydrolytic resistance of glass grains at 121°C — Method of test and classification. 180 1042, Laboratory glassware — One-mark volumetric flasks. ISO 1773, Laboratory glassware — Bolling flasks (narrom- necked). 1S0 3696, Water for lnboratory use — Specifications") 1S0 3819, Laboratory glassware — Beakers. 1) At present at the stage of deaf. 3. Principle ‘The method of test is a test for glass as a material applied on glass grains. Extraction of 2 g of grains, of particle size between 300 and 500 jim, with grade 2 water for 60 min at 98 °C. ‘Measurement of the degree of the hydrolytic attack by analysis of the extraction solutions. 4 Reagents During the test, unless otherwise stated, use only reagents of recognized analytical grade. 4.1 Grade 2 water, which complies with the requirements specified in ISO 3696 and which has been treed from dissolved gases, such as carbon dioxide, by boling for at least 16 min in a bolling flask (6.6) ‘Such water can normaly be stored for 24h in a stoppered flask without change of the pH value. When tested immediately before use the water shall be neutral {to methyl red, ie. it shall produce an orange-red (not a violet- red oF yellow) colour corresponding to pH §,5 + 0,1 when two drops of the methyl red indicator solution (4.4) are added to. 25 mi of the water. NOTE — The water, so coloured, may alo be used a tion {860 caus 7). reforence eolu- 4.2 Hydrochloric acid, e(HCH) = 0,01 moi tandard volumetric solution, 4.3. Hydrochloric acid, solution, c(HCll ~ 1 mol/l 4.4 Methyl red, indicator solution. Dissolve 25 mg of the sodium salt of methy red (CygHy_N3NaO,) in 100 mi of the grade 2 water (4.1) 4.5 Acetone (CH{COCHG).ISO 719-1985 (E) 4.8 Distilled water or water of equivalent purity (grade 3 water complying with the requirements specified in ISO 3696). 5 Apparatus Ordinary laboratory apparatus, and 6.1 Balance, accurate to + 5 mg or better. 5.2 Burettes, having a capacity of 5 ml, 2 ml or 1 ml, com- plying with the requirements specified for class A burettes in 1SO 385/2 (see also general requirements specified in 1SO 385/1) and made of glass of hydrolytic resistance gra class HGA 1 as specified in 1S0 7201) ‘The capacity of the burettes shall be choson according to the expected consumption of hydrochloric acid (4.2) 5.3. Pipette, having a capacity of 25 ml and complying with the requirements specified for class A pipettes in ISO 648. 5.4 One-mark volumetric flasks, having a capacity of 50 mi, complying with the requirements specified for class A. fone-mark volumetric flasks in ISO 1042, made of glass of hydrolytic resistance grain class HGA’ 1 as. specified in 180 7201), and with glass stoppers. NOTE — itis advisable to select flasks with the graduation mark in the lower half of the neck, Before use, each new flask shall be pretreated in the following manner: The flasks shalt be filed to above the graduation mark with hydrochloric acid (4.3) and heated at just above the test temperature for 2 h in the heating bath (5.19). The flasks shall then be rinsed with water (4.6), filled to above the graduation ‘mark with water and heated es above for two periods of 1 h, using fresh watar each time. Notes 1 Flake made from vitreous slica may also be used, in which case protrastment is not required. 2 When flasks havo been used to measure tho akal-roloase from ‘grain of low-esistance glass, it's advisable to pretreat them agein, 95, above, before using them for further test inorder to olminato cross- ‘contamination 5.5 Conical flasks, having a capacity of 100 ml and comply- ing with the requirements of ISO 173. 5.6 Bolling flasks, having @ capacity of 1.000 ml, complying ‘with the requirements of [SO 1773 and made of vitreous silica fr borosilicate glass, Boforo use, each new flask shall be protreated as described in5.4, 5.7. Beakers, having @ capacity of 100 mi and complying with the raquirements of ISO 3819. 5.8 Weighing bottles, having a capacity of about 20 ml 5.9 Desiccator. 5.10 Hammer, having a mass of about 0,5 kg. 5.11 Mortar and pestle, made of hardened magnetic steel, and 2f the design and approximate dimensions shown in the figura 5.12, Magnet. 5.13 Sieves, complying with the requiroments of ISO 885 and comprising a set of 200 mm diameter square-aperture sieves, with stainless stee! mesh, including: = asieve A of 500 jim aperture; = a sieve B of 300 um aperture: —__a sieve O of a convenient aperture botween 600 and 1000 jim, The cover, pan and, especially, the rings shall be of stainlass steel or lacquered wood. NOTE — The use of save 0 Is recommended to retain larger pieces of «lass and to avoid heavy wear on siova A. 5.14 Ball-mill ‘The mill shall be made of agate or stainless steel with a volume ‘of 250 ml. Two balls with 2 diameter of 40 mm or three bails with a diameter of 30 rm are suitable. 6.15 Sieving-machino ‘A mechanical sieve-shakar or sieving-machine may be used to sieve the grains. .16 Ultrasonic cleaner (laboratory type) 5.17 Drying oven, suitable for operation up to 160 °C. 5.18 Thermometer, covering the range from 90 to 110°C, ‘capable of being read to an accuracy of + 0,2 °C. 5.19 Heating bath, gas or electrically heated, ther- ‘mostatically controlled, having capacity sufficient to contain at Teast 1 lite of quid for each flask used in the test and capable ‘of carrying out the heating cycle specified in clause 7. 1) Giass of hydroivtl resistance grain class ISO 719-HGB 1 adequately meets the requirements of class HGA t specified in ISO 720,Approximate dimensions Figure — Mortar and pestle 6 Preparation of sample 6.1 Density of the glass. The density of the glass to be tested should, preferably, be 2,4 + 0,2 g/om3 at 20 °C. 1SO 719-1985 (E) 6.2 Crushing Check that the articles as received have been annealed to @ commercially acceptable quality NOTE — if an atiole is not annealed to a commercially accoptablo quality, this fact should be noted because the results canbe affected. Such articles, if very badly annealed, may also brozk very easily and fextre caro should be taken when handling them. Further anngeling should not be catied out before the tes. Wrap the glass articles, which should, preferably, have a wall thickness greater than 1,5 mm, in clean paper and crush to pleces nat more than 30 mm across. 6.3. Manual preparation Place 20 to 40 g of pieces (see 6.2) between 10 and 30 mm ‘across in the mortar (6.11), insert the pestio (5.11), and strike it sherply, once only, with the hammer (5.10). [NOTE — If more than one hammer blow is used in rushing the gloss, the very fine particles produced may be compacted into aggregates ‘which may of may not be subsequenty broken down and which can thotefore Introduce further variables into tho test. Trensfor the glass from the mortar to the upper sieve O of the assembled set of sieves (6.13), and shake the sat of sieves briefly to separate the finer particles. Return the glass remsin- ing on sieves A and 0 to the mortar. Repeat crushing and siev- ing until only about 10 g of glass remain on sieve O. Discard the ‘lass from siove O and from the receiving pan. Shake the sot of sieves by hand for 5 min. Reserve for the test those grains which pass through sieve A, but which ate retained on sieve B. Atleast 10 g of sample aro required forthe tos. fit is nacessary ‘to crush and sieve more sample, its essential that the sample already obtained should be removed from sieve B and stored in ‘a weighing bottle (5.8). After completion of all crushing and sieving, combine the ‘samples, spread the grains on clean glazed paper and remove any iron particles using the magnet (6.12). Transfer the grains Into a beaker (6.7) for cloaning. 6.4 Mechanic: preparation Transfer about 50 g of the coarsely broken glass (see 6.2) into the mill-beaker (5.14}, add the balls and crush thin-walled glass (wall thickness < 1,5 mm) for 2 min, thick-walled glass (> 1,5 mm) for 5 min, ‘Transfer the grains to the upper sieve O of the assembled set (6.13) of the sievit (6.15), sieve for about 20 s and collect the grains retained on sieve B in the beaker (6.7), which shall be kept in the desiccator (5.9). Transfer the glass from sieves O and A back into the ball-mill and crush again for the time given above. Repeat sleving and crushing until about 10 g of grains have been collected from sieve B, Continue as specified in 6.3, last paragraph. 6.5 Cleaning ‘Add to the grains in each beaker (6.7) 30 mi of the acetone (4.5) and scour the grains by a suitabfe means, such as a rubber- or plastics-coated glass rod.1SO 719-1985 (E) NOTE — The method of scouting involves holding the beaker at an angle of about 30° to 48° firmly against tha banch and pressing fray ‘the covered end of a glass rod of about 10 mm in diameter into the bottom comer and against the sidos, so thatthe grains ate trapped between it and the sides and the bottom of tho beaker as the rod is rotated around the beaker. Contiwe the rotation for about 20 revo After scouring, swirl the greins and decant as much acetone as possible. Add another 30 mi of the acetone, swirl and decant ‘again and add a new portion of the acetone. Fill the bath of the ultrasonic cleaner (5.16) with water at room temperature, then place the beaker in the rack and immerse it until the level of the acetone is at the level of the water; apply the ultrasonics for 1 min, ‘Swirl the beaker and decent the acetone as completely as possible and then repeat the ultrasonic cleaning operation. If a fine turbidity persists, repeat the ultrasonic cleaning and acotona washing until the solution remains clear. Swirl and decant the acetone, then dry the grains, first by putting the beaker with the grains on a warm plato to remove excess acetone and then by heating at 140 °C for 20 min in the drying oven (6.17) ‘Transfar the dried grains from the oven into a weighing bottle (63), insert the stopper and coo! in the desiccator (5.9) 7 Procedure Weigh 2,00 g of the cleaned and dried grains into each of three Of the one-mark volumetric flasks (5.4). Fill the flasks to the ‘mark with the grade 2 water (4,1) and fil two more flasks with the water, one to serve as a reference solution and the other to serve as a temperature control Distribute the glass grains evenly over the flat bases of the ‘sample fasks by gently shaking them, then place all of the flasks, without stoppers, in the heating bath (6.19), so that they are immersed to half-way up the necks (a rack to hold the flasks may be used). Increase the rate of heating such that the specified temperature of 98 + 0,5 °C is achieved in the control flask within 3 min; after a further 2 min, insert the stoppers. Continue heating for 60 + 1 min from the time of immersion, maintaining the temperature at 98 0,5 °C in the flasks. Romove the flasks from the heating bath, take out the stop- pers, coo! the flasks in running water and adjust the contents of each flask to the mark with the grade 2 water. Replace the stoppers and mix the contents of each flask thoroughly, then allow to stand until the grains settle and a clear supematant solution is obtained. Complete the titration within 1 h. By means of the pipette (6.3), transfer 25 ml of the clear sol n from each flask into separate conical flasks (5.5), add to ‘cach of these fiasks two drops of the mathy! red indicator sol tution (4.4), and titrate immediately with the hydrochloric acid solution (4.2), until the colour matches exactly that of the 25 mi of the water of the reference solution plus two drops of the indicator contained in a similar conical flask. 4 & Expression of results 8.1 Calculation Calculate the mean value of the results, in millitres of hydrochloric acid solution (4.2) per gram of sample, and, if required, its equivalent in alkali extracted, calculated as micrograms of sodium oxide (NazO) per gram of glass grains: 1 ml of hydrochloric acid solution [e(HCH = 0,01 moi/ll = 310 41g of sodium oxide If the highest and the lowest obsorved values differ by more ‘than the permissible range given in table 1, repeat the test. Giass shall be classified as shown In table 2, according to the ‘consumption of acid and its equivalent of alkali loxpressod as ‘sodium oxide (NazO}], when tested by the method specified in ‘his International Standard, For convenience of reference to the hydrolytic resistance of class as 2 material complying with the classification of this Ihternational Standard, the use of a designation as follows is recommended: Bxample: ‘Tho designation for 2 glass with a consumption of 0,60 ml of hydrochloric acid solution {e(HC) = 0,01 mol/l per gram of lass grains equivalent to 186 1g of sodium oxide per gram of lass grains (class HGB 3) shall be: Glass, hydrolytic resistance grain class ISO 719 - HGB 3 9 Test report ‘The test report shall include the following information: a) a reference to this International Standard; b) an identification of the sample; )__ the consumption of hydrochloric acid solution Fe(HCt) = 0,01 mol/N, in miliitres per gram of glass grains, mean value; dd) in addition, if required, the equivalent of alkali, in ‘micrograms of sodium oxide per gram of glass grains, mean vvalug; ©) the hydrolytic resistance grain class HGB (designation Of the glass tested); 11 the wall thickness of the articles used for the test if t was < 1,5 mm; 9), tho density ofthe glass if it was outside the range of 24 & 02 glemat20 °C; fh) statement, if appropriate, that the glass article used for the test was not annealed to commercially acceptable quality,1SO 719-1985 (E) Tablo 1 — Permissi lo range of the values obtained “Mean of the values obtained for the consumption of hydrochloric acid solution Te(HCH = 0,01 mol/l (42), Pormi Per gram of glass graine range of the valuos obtained mila Up 10 and Ineuding 0,10 ‘20 % of tho mean from 0,10 up to and including 0,20 20 % af the mean from 0,20 upwards H 10 9 of the mean Table 2 — Limit values in the hydrolytic resistance gr ins test (boiling water tost) (Consumption of hydrochloric cid solution | Equivalent of alkallexprossod Teikch ‘mace of sodium oxi tha,0) toss arom of plans ole | HGB 1 “up to and including 0,10 up to and including 31 G82 | trom 10 ap to ond ncocing 0.20 ftom 3% up toand Incuting 62 ee 3 | fom 0.20 upto ord ncusing 0.88 ftom 62 up to and incdng 264 G84 | fom 0.8 upto and inlcing 20 ftom 264 up to and incudng 20 ves s | tem 2.0” up te and inching 5 from €20 upto and Incling 1 O86 1). “HG” stands for the hydrolytic resistance of gles graine according tothe boling weter test method I | a