© ISO 2016 Laboratory glassware — Vacuum jacketed vessels for heat insulation Verrerie de laboratoire — Récipients à double enveloppe à vide pour isolation thermique INTERNATIONAL STANDARD ISO 16496 F[.]
INTERNATIONAL STANDARD ISO 16496 First edition 2016-02-01 Laboratory glassware — Vacuumjacketed vessels for heat insulation Verrerie de laboratoire — Récipients double enveloppe vide pour isolation thermique Reference number ISO 16496:2016(E) © ISO 2016 ISO 6496: 01 6(E) COPYRIGHT PROTECTED DOCUMENT © ISO 2016, Published in Switzerland All rights reserved Unless otherwise specified, no part o f this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission Permission can be requested from either ISO at the address below or ISO’s member body in the country o f the requester ISO copyright o ffice Ch de Blandonnet • CP 401 CH-1214 Vernier, Geneva, Switzerland Tel +41 22 749 01 11 Fax +41 22 749 09 47 copyright@iso.org www.iso.org ii © ISO 2016 – All rights reserved ISO 16496:2016(E) Contents Page Foreword iv Scope Normative references Terms and definitions Dimensions 4.2 4.3 Materials Construction Safety requirements and testing 7.1 7.3 7.4 General Reaction vessels 10 Columns 10 8.1 S a fety ins tructio ns 7.2 10 D ewar flas ks Use of vacuum vessels 10 8.2 Reaction vessels Columns D ewar flas ks 10 Functional requirements 10 User information 11 Marking 11 11 10.2 Reaction vessels and columns 11 Annex A (normative) Testing glass for residual strain (bifilar method) 13 0.1 D ewar flas ks Bibliography 14 © ISO 2016 – All rights reserved iii ISO 16496:2016(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies) The work o f preparing International Standards is normally carried out through ISO technical committees 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, governmental and non-governmental, in liaison with ISO, also take part in the work ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters o f electrotechnical standardization The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part In particular the different approval criteria needed for the di fferent types o f ISO documents should be noted This document was dra fted in accordance with the editorial rules of the ISO/IEC Directives, Part (see www.iso.org/directives) Attention is drawn to the possibility that some o f the elements o f this document may be the subject o f patent rights ISO shall not be held responsible for identi fying any or all such patent rights Details o f any patent rights identified during the development o f the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents) Any trade name used in this document is in formation given for the convenience o f users and does not constitute an endorsement For an explanation on the meaning o f ISO specific terms and expressions related to formity assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary in formation The committee responsible for this document is ISO/TC 48, Laboratory equipment iv © ISO 2016 – All rights reserved INTERNATIONAL STANDARD ISO 16496:2016(E) Laboratory glassware — Vacuum-jacketed vessels for heat insulation Scope T h i s I nternationa l Stand ard re com mend s d i men s ion s a nd s p e ci fie s re qu i rements and te s t me tho d s for lab orator y gl as s ware manu fac tu re d for from b oro s i l ic ate gl as s and provide d with a vac uu m j acke t therma l i n s u lation I t covers D ewa r ve s s el s , vac uu m-j acke te d re ac tion ve s s el s and vac uu m-j acke te d for colu m n s i ntende d in Tables to This I nternationa l lab orator y u s e and lab orator y rel ate d appl ic ation s Typic a l d i men s ion s are given Stand ard e s no t apply to la rge s c a le pro duc tion operated with pressures of more than 0,1 bar above atmospheric pressure e qu ipment and e qu ipment Normative references T he fol lowi ng i nd i s p en s able c u ments , i n whole or i n p ar t, are normatively re ference d i n th i s c u ment a nd are for its appl ic ation For date d re ference s , on ly the e d ition cite d appl ie s For u ndate d re ference s , the late s t e d ition o f the re ference d c u ment (i nclud i ng any amend ments) appl ie s ISO 383, Laboratory glassware — Interchangeable conical ground joints ISO 641, Laboratory glassware — Interchangeable spherical ground joints ISO 718, Laboratory glassware — Thermal shock and thermal shock endurance — Test methods ISO 3585, Borosilicate glass 3 — Properties ISO 4803, Laboratory glassware — Borosilicate glass tubing ISO 4790, Glass-to-glass sealings — Determination of stresses Terms and definitions For the pu r p o s e s o f th i s c u ment, the fol lowi ng term s and defi n ition s apply 3.1 Dewar flask gla s s ve s s el with vac uu m j acke t for therma l i n s u l ation, de s igne d temperature within a range from -200 °C to +200 °C N o te to entr y: S e e for ke epi ng s ub s tance s at a control le d 8.1 f o r re s tr ic tion s o n the u s e o f D ewa r fl a s ks 3.2 cryo vessel vac uu m j acke te d ve s s el made o f materi a l s o ther th an gla s s 3.3 column c yl i nd ric a l ve s s el for the therma l s ep a ration o f s ub s tance s i n a lab orator y or pi lo t plant © ISO 2016 – All rights reserved ISO 16496:2016(E) Dimensions The designs shown in Figures to f to f with the scope of this International Standard are are D e or i l lu s trative pu rp o s e s on ly T he d i men s ion s given i n Tables or gu idance, o ther d i men s ion s b ei ng p erm i s s ible, provide d the re s u lti ng c ap acitie s comply w a r f l a s k s D ewa r flas ks may have a c yl i nd ric a l, s pheric a l or d i she d sh ap e, a s s hown exempla ri ly i n Figures to O ther flas k de s ign s are p erm itte d , e g flas ks with flat b o ttom or rol le d- on or i ntegra l fla nge Key soft rubber spacer protective housing D ewar flas k plastic foam cushion glas s b o dy evacuated space F i g u r e — C y l i n d r i c a l D e w a r f l a s k © ISO 2016 – All rights reserved ISO 16496:2016(E) Key soft rubber spacer protective housing plastic foam cushion D ewar flas k F © ISO 2016 – All rights reserved i g u r e — D i s h e d D e w a r f l a s k ISO 16496:2016(E) Key soft rubber spacer hard rubber spacer protective housing D ewar flas k plastic foam cushion Figure — Spherical Dewar flask Table — Dimensions o f cylindrical Dewar flasks Nominal capacity ml a 200 500 800 000 000 500 500 000 000 Internal diameter Internal height d1 h1 Nominal size 40 57 67 77 100 90 100 90 100 Limit deviations ±3 Dimensions d2 and h are intended as guideline values Nominal size 170 210 240 235 150 245 240 340 290 Limit deviations ±3 Dimensions in millimetres Housing diameter Overall height d2 a h2 a ≈ ≈ 66 82 90 106 128 125 130 125 130 220 265 300 300 190 305 300 395 350 © ISO 2016 – All rights reserved ISO 16496:2016(E) Table (continued) Nominal capacity ml a 000 500 000 000 000 10 000 14 000 21 000 28 000 40 000 Internal diameter Internal height d1 h1 Nominal size 138 110 138 138 200 200 200 250 250 290 Limit deviations ±4 ±5 ±6 Dimensions d2 and h are intended as guideline values Nominal size 170 290 230 310 270 360 500 480 625 650 ml 168 140 170 170 240 240 240 295 295 340 220 350 285 365 375 465 600 580 720 745 ±4 ±5 ±6 ≈ Dimensions in millimetres Housing diameter Overall height d1 h1 d2 h2 ≈ ≈ ≈ ≈ 100 110 138 170 200 250 65 70 80 110 140 170 130 138 170 215 250 300 Table — Dimensions o f spherical Dewar flasks a h2 a ≈ Internal height NOTE All dimensions are intended as guideline values ml d2 a Internal diameter 260 390 680 280 400 300 Nominal capacity Overall height Limit deviations Table — Dimensions o f dished Dewar flasks Nominal capacity Housing diameter Internal neck diameter Internal height d1 ±4 000 000 000 10 000 ±2 30 60 60 65 Dimensions d2 and h are intended as guideline values © ISO 2016 – All rights reserved h1 230 305 350 380 110 115 125 145 190 220 Dimensions in millimetres Housing diameter Overall height ≈ ≈ 175 225 260 330 295 375 425 475 d2 a h2 a ISO 16496:2016(E) 4.2 Reaction vessels O p tiona l fe atu re s o f re ac tion ve s s el s i nclude an outle t s top co ck at the ve s s el’s b o ttom, a he ati ng/co ol i ng j acke t a nd a fl at flange at the ve s s el’s top F i g u r e — E x a m p l e f o r a r e a c t i o n v e s s e l w i t f 4.3 h l a o n u g t l e t s t o p c o c k , h e a t i n g / c o o l i n g j a c k e t a n d f l a t e Columns C olu m n s may b e de s igne d to b e op erate d with or without an add itiona l he ati ng j acke t T he de s ign o f column inlet and outlet connections is at the manufacturer’s discretion (see 6.6) © ISO 2016 – All rights reserved ISO 16496:2016(E) Figure — Column © ISO 2016 – All rights reserved ISO 16496:2016(E) Table — Dimensions of reaction vessels Nominal capacity ml Nominal size DN Internal height Installation height h1 h2 d1 a d2 a d3 a 160 215 305 170 200 265 250 340 280 325 450 735 350 380 505 70 70 700 105 105 105 130 130 160 160 160 160 215 215 215 100 100 100 125 125 125 160 160 190 190 190 190 250 250 250 130 130 130 150 150 150 190 190 225 225 225 225 300 300 300 +5 100 250 500 250 500 000 000 000 000 000 000 10 000 000 000 10 000 60 60 60 100 100 100 120 120 150 150 150 150 200 200 200 Dimensions in millimetres 115 170 260 130 160 225 205 295 235 290 405 690 290 320 445 Diameters ±5 a Tolerances on d1 , d2 and d3 are as specified in ISO 4803 or in national standards Alternatively, commercial tubing made o f borosilicate glass 3.3 may be used Table — Dimensions of columns Packing height h1 ≈ 300 500 000 Dimensions in millimetres Internal diameter d1 ≈ 30 to 85 30 to 85 30 to 85 NOTE The dimensions are intended as guideline values Materials The glass parts o f vacuum-jacketed vessels shall be o f borosilicate glass 3.3 as specified in ISO 3585, and shall be free o f residual strain and de fects likely to impair the vessel’s appearance, service li fe and strength The protective housing o f Dewar flasks shall be made o f sheet metal, stainless steel sheet, aluminium or plastics © ISO 2016 – All rights reserved ISO 16496:2016(E) Construction 6.1 The glass used for the vessel and the glass-to-glass seals shall be free from residual strain likely to impair the strength o f the vacuum jacket Testing shall be performed by examination under polarized light When glass-to-glass seals include borosilicate glass 3.3 of different origins, e.g where alterations 6.2 are made to the vessels or in the case o f repairs, any residual strain should be determined in accordance with ISO 4790 or as specified in Annex A 6.3 The vacuum jacket (i.e all walls that enclose the vacuum) shall have a minimum wall thickness conforming to that calculated in accordance with acknowledged methods given in expert literature Some examples are listed in the Bibliography The wall thickness specification does not apply to bellows-type expansion joints o f columns The actual wall thickness shall be determined using an ultrasonic method 6.4 The outer glass surface o f vacuum-jacketed vessels may be coated with plastics for protection 6.5 Reaction vessel ports and connections should pre ferably be equipped with flat flanges in against mechanical damage during handling, transport and in the event of implosion accordance with regional or national standards Other ports and connections are acceptable The design o f connections to the heating or cooling jacket is at the manufacturer’s discretion In the case of columns, the design of connections at the column inlets and outlets is at the 6.6 manu facturer’s discretion I f conical or spherical ground joints are used, they shall form to ISO 383 and ISO 641 or the respective national standards Flat flanges should comply with regional or national standards Safety requirements and testing 7.1 General 7.1.1 The walls o f glass parts shall have no de fects likely to impair their strength, e g stones, bubbles, knots, cords, cracks, scratches Testing shall be performed by visual inspection 7.1.2 Glass tubing used to fabricate vacuum vessels shall conform to ISO 4803 or to national standards 7.1.3 Glass-to-glass seals between the inner and outer part o f vacuum jackets shall be homogeneous and free from stones, bubbles and sharp edges Glass-to-glass seals and sealed-off parts shall have a clean and rounded finish Testing shall be performed by visual inspection 7.2.1 D e w a r f l a s k s Dewar flasks supplied for end-use in the laboratory shall have a rigid protective housing made of a material in accordance with Clause Alternatively, the Dewar flask may be coated with plastics, as specified in 6.4 The glass part and protective housing shall stand upright on a flat horizontal sur face without rocking or rotating The glass body shall be protected against damage, e g by a cushioning between the glass body o f the vessel and the protective housing The cushion (see Figures and ) shall provide su fficient support so that the tip o f the sealed evacuation nozzle does not contact the protective housing when the flask is used as intended 7.2.2 The glass vessel shall have thermal shock endurance © ISO 2016 – All rights reserved ISO 16496:2016(E) a) of at least 100 °C in the temperature range from +20 °C to +200 °C or b) of at least 180 °C in the temperature range from +20 °C to -200 °C Test for both temperature ranges, as specified in ISO 718, with the Dewar flasks being filled with the liquid to 30 mm below the top rim, instead of being immersed in the liquid 7.2.3 Dewar flasks shall not have any gastight closure mechanisms, such as expansion closures or locking closures Lids shall be designed to ensure equilibration o f pressure with the atmosphere I f applicable, Dewar flasks which are specifically designed to store combustible liquefied gases 7.2.4 shall conform to the stipulations of national regulations for these substances 7.3 Reaction vessels The sealed evacuation nozzle of reaction vessels shall be protected from mechanical damage, assuming the intended use o f the vessel Plastic protective caps may be use ful for this purpose The fused shoulder shall be rounded without sharp edges Testing shall be per formed by visual inspection 7.4 Columns The jacket tubes of columns shall be fitted with internal bellows-type expansion joints The number of expansion bellows will depend on the length of the column and the intended operating temperature range NOTE When columns are used with temperatures >200 °C, it might be use ful to employ an additional heating jacket to avoid thermal stresses The sealed evacuation nozzle of columns shall be protected from mechanical damage, assuming intended use o f the vessel Plastic protective caps may be use ful for this purpose Testing shall be per formed by visual inspection Use of vacuum vessels 8.1 Safety instructions When working with vacuum-jacketed vessels, applicable national sa fety regulations for the work with vacuum shall be observed Be fore use, the vessels shall be visually inspected to ensure that there are no de fects, such as chipping, cracks and scratches Damaged glass parts shall not be used A replacement o f the glass body o f Dewar flasks should be per formed by the manu facturer or by qualified personnel New glass bodies shall not be installed into corroded or deformed protective housings Loose lids or stoppers for closure on Dewar flasks shall be designed to ensure pressure equilibration with the atmosphere NOTE Dewar flasks are unsuitable for storing or transporting liquefied helium NOTE Dewar flasks used to store combustible liquefied gases need to be specifically made for this purpose NOTE There are national sa fety regulations in some countries prohibiting the use o f liquefied air or liquefied oxygen for low temperature cooling 8.2 Functional requirements Every three to five years, the user should check vacuum jackets o f laboratory equipment for the insulation ability Reaction vessels and columns shall be checked following consultation with the manufacturer 10 © ISO 2016 – All rights reserved ISO 16496:2016(E) When te s ti ng D ewar fl as ks a s de s c rib e d b elow, the le a kage rate me as u re d b y the u s er s l l no t exce e d the va lue s given b y the manu fac tu rer i n the u s er i n formation b y more tha n % I f the va lue s a re h igher, the us er s hou ld h ave the flas k re - eva luate d by the ma nu fac turer I n the te s t, the fla s k s l l b e fi l le d to its nom i na l cap acity with l iqu id n itro gen or d r y ice (fol lowi ng the manu fac tu rer ’s i n s truc tion s) and place d on a b a lance T he le a kage rate i s the weight lo s s , i n gra m s p er day, up to the ti me at wh ich the ve s s el contents have evap orate d comple tely User information E ach vac uu m- j acke te d ve s s e l s h a l l b e acco mp a n ie d b y a u s er i n fo r m atio n , wh ich s h a l l co mp r i s e o f the following: a re ference to the appropri ate s a fe ty i n s tr uc tion s i n nationa l regu lation s; a) b) operating parameters: — m i n i mu m and ma xi mum op erati ng temp eratu re s; — p erm i s s ible pre s s u re i n the e ffe c tive volu me; — with reaction vessels and columns, the minimum permissible heating and cooling times in the s p e c i fie d temp erature range; — with D ewar flas ks , le a kage rate and re s tric tion s on u s e, e g regard i ng l iqu id hel ium and l iquefie d combu s tible gas e s With reaction vessels and columns intended to be assembled to form a more complex apparatus, i n formation on a s s emb ly s l l b e given 10 Marking D e w a r f l a s k s D ewar fla s ks sha l l b e p ermanently ma rke d at an appropriate pl ace with the a) the name and/or tradema rk o f manu fac tu rer and/or s uppl ier; b) the gla s s typ e or bra nd; c) the nom i na l c ap acity or typ e; fol lowi ng de tai l s: d) the number of this International Standard, i.e ISO 16496 10.2 Reaction vessels and columns T he gla s s b o dy o f ve s s el s a nd colu m n s sh a l l b e marke d i n a s p erma nent a man ner a s p o s s ible, a s a) the name and/or tradema rk o f manu fac tu rer and/or s uppl ier; b) the gla s s typ e or bra nd; c) the typ e or i nd ividua l comp onent numb er; d) the ma xi mum op erati ng temp eratu re; fol lows: e) the number of this International Standard, i.e ISO 16496 T ho s e colu m n s wh ich have b e en i nd ividua l ly te s te d s l l a l s o b e marke d with the te s t temp eratu re a nd date of testing © ISO 2016 – All rights reserved 11 ISO 6496: 01 6(E) Re ac tion ve s s el s s l l add itiona l ly b e marke d with thei r nom i na l c ap acity and ye ar o f manu fac tu re 12 © ISO 2016 – All rights reserved ISO 16496:2016(E) Annex A (normative) T e s t i n g g l a s s f o r r e s i d u a l s t r a i n ( b i f i l a r Fu s e the gla s s s p e ci men u nder te s t to a gl as s ro d a nd s quas h it with flat m e t h forcep s o d ) P rep are a re ference s p e ci men i n the s ame man ner T hen, he at the two s p e c i men s with a ho t r blower u nti l they s o ften, pre s s them agai n s t one ano ther latera l ly and d raw out the p oi nt where they overlap to form a fi la ment ab out , m m to m m th ick O n co ol i ng , the bi fi l ar pie ce c u r ve s toward the s ide o f the gl as s havi ng the h igher contrac tion, i e the gla s s havi ng the h igher exp a n s ion i s on the i n s ide o f the c u r ve I f the fi la ment e s no t b end, the two glasses have the same expansion and are thus free from residual strain © ISO 2016 – All rights reserved 13 ISO 16496:2016(E) Bibliography [1] AD 2000-Merkblatt B 0, Design of pressure vessels [2] AD 2000-Merkblatt B 1, Cylindrical and spherical shells subjected to internal overpressure [3] AD 2000-Merkblatt B 2, Conical shells subjected to internal and external overpressure [4] AD 2000-Merkblatt B 3, Domed ends subjected to internal or external pressure) [5] AD 2000-Merkblatt B 4, Dished heads [6] AD 2000-Merkblatt B 5, Unstayed and stayed flat ends and plates [7] AD 2000-Merkblatt B 6, Cylindrical shells subjected to external overpressure [8] AD 2000-Merkblatt N 4, Pressure vessels made of glass [9] AD 2000-Merkblatt N 4, Anhang 1, Assessment of defects in walls of pressure vessels made of glass 14 © ISO 2016 – All rights reserved [10] Source for all AD-guidelines in English language: www.beuth.de/en ISO 6496: 01 6(E) ICS 71.040.20 Price based on 14 pages © ISO 2016 – All rights reserved