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INTERNATIONAL
STANDARD

ISO
16496
First edition
2016-02-01

Laboratory glassware — Vacuumjacketed vessels for heat insulation
Verrerie de laboratoire — Récipients à double enveloppe à vide pour
isolation thermique

Reference number
ISO 16496:2016(E)
© ISO 2016


ISO 1 6496: 2 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 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47

www.iso.org

ii

© ISO 2016 – All rights reserved


ISO 16496:2016(E)

Contents

Page

Foreword ........................................................................................................................................................................................................................................ iv
1
2

3
4

Scope ................................................................................................................................................................................................................................. 1
Normative references ...................................................................................................................................................................................... 1

Terms and definitions ..................................................................................................................................................................................... 1
Dimensions ................................................................................................................................................................................................................. 2

4. 1

4.2
4.3
5
6
7

Materials ....................................................................................................................................................................................................................... 8
Construction .............................................................................................................................................................................................................. 9
Safety requirements and testing .......................................................................................................................................................... 9

7.1
7.3
7.4

General ........................................................................................................................................................................................................... 9
.............................................................................................................................................................................................. 9
Reaction vessels .................................................................................................................................................................................. 10
Columns ..................................................................................................................................................................................................... 10

8.1

S a fety ins tructio ns

7.2

8

10


D ewar flas ks

Use of vacuum vessels .................................................................................................................................................................................. 10

8.2

9

.............................................................................................................................................................................................. 2
Reaction vessels ..................................................................................................................................................................................... 6
Columns ........................................................................................................................................................................................................ 6
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
1 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 1. 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 2 (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 con 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
1 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 3 . 3 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 1 to 5.
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

do 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

2 Normative references
T he

fol lowi ng

i nd i s p en s able

do c u ments , i n whole or i n p ar t, are normatively re ference d i n th i s do 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 do 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. 3 — Properties
ISO 4803, Laboratory glassware — Borosilicate glass tubing
ISO 4790, Glass-to-glass sealings — Determination of stresses
3 Terms and definitions
For the pu r p o s e s o f th i s do 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 1 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

1


ISO 16496:2016(E)


4 Dimensions

The designs shown in Figures 1 to 5 f
to 5 f
with the scope of this International Standard.
are

are

4

.

1



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 1

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 1 to 3.

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

1
2
3
4
5
6

soft rubber spacer

protective housing
D ewar flas k

plastic foam cushion

glas s b o dy

evacuated space
F

2

i

g

u

r

e



1








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

1 soft rubber spacer
2 protective housing
3
4 plastic foam cushion
D ewar flas k


F

© ISO 2016 – All rights reserved

i

g

u

r

e



2







D

i

s


h

e

d



D

e

w

a

r



f

l

a

s

k


3


ISO 16496:2016(E)

Key

1
2
3
4
5

soft rubber spacer
hard rubber spacer
protective housing
D ewar flas k

plastic foam cushion
Figure 3 — Spherical Dewar flask
Table 1 — Dimensions o f cylindrical Dewar flasks

Nominal
capacity

ml

a


4

200
500
800
1 000
1 000
1 500
1 500
2 000
2 000

Internal diameter

Internal height

d1

h1

Nominal
size
40
57
67
77
100
90
100
90

100

Limit deviations

±3

Dimensions d2 and h 2 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 1 (continued)
Nominal
capacity

ml

a

2 000
2 500
3 000
4 000
7 000
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 2 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 3 — 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
1 280
4 400
8 300

Nominal capacity

Overall
height

Limit deviations

Table 2 — Dimensions o f dished Dewar flasks
Nominal capacity

Housing
diameter

Internal neck diameter

Internal height

d1


±4

1 000
3 000
5 000
10 000

±2
30
60
60
65

Dimensions d2 and h 2 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

5


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



4








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).

6

© ISO 2016 – All rights reserved


ISO 16496:2016(E)

Figure 5 — Column

© ISO 2016 – All rights reserved

7


ISO 16496:2016(E)

Table 4 — 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
0

100
250
500

250
500
1 000
1 000
2 000
2 000
3 000
5 000
10 000
5 000
6 000
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 5 — Dimensions of columns

Packing height
h1


300

500
1 000

Dimensions in millimetres
Internal diameter
d1



30 to 85
30 to 85
30 to 85

NOTE The dimensions are intended as guideline values.
5 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.

8

© ISO 2016 – All rights reserved



ISO 16496:2016(E)

6 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 con form to
ISO 383 and ISO 641 or the respective national standards. Flat flanges should comply with regional

or national standards.

7 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




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 5 . 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 1 and 2 ) 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

9


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.
8 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 1

Dewar flasks are unsuitable for storing or transporting liquefied helium.

NOTE 2

Dewar flasks used to store combustible liquefied gases need to be specifically made for this purpose.

NOTE 3 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 ha 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 1 5 % . 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 ha 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.

9 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 ha l l b e given .

10 Marking
1

0

.

1



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 ha 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 1 6496: 2 01 6(E)

Re ac tion ve s s el s s ha 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 ai 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 0 , 5 m m to 1 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 do 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 1 6496: 2 01 6(E)

ICS  71.040.20

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