I NTERNATI ONAL STAN DARD I S0 1 065 Secon d edi ti on 1 991 09 01 Non i oni c surface acti ve agents obtai ned from ethyl ene oxi de and mi xed non i oni c surface acti ve agents Determi nati on of c[.]
INTERNATIONAL STANDARD IS0 065 Second edition 991 -09-01 Non-ionic surface-active agents obtained from ethylene oxide and mixed non-ionic surface-active agents - Determination of cloud point Agents de surface non ioniques obtenus B par-fir de I’oxyde d’&hy/&ne et mixtes - DBtermination de /a tempdratwe de trouble (point de trouble) Reference number IS0 065:1 991 (E) IS0 065:1 99j(E) Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies) The work of preparing International Standards is normally carried out through IS0 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 IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization Draft International Standards adopted by the technical committees are circulated to the member bodies for voting Publication as an International Standard requires approval by at least 75% of the member bodies casting a vote International Standard IS0 065 was prepared by Technical Committee ISO/TC 91, Surface active agents This second edition cancels and replaces the first edition (IS0 065:1 975), to which two new methods (D and E) have been added in order to extend the scope to cover mixed non-ionic surface-active agents IS0 991 All rights reserved I\io part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permlsslon in writing from the publisher international Organization for Standardization Case Postale 56 l CH-1 21 Genbve 20 l Switzerland Printed in Switzerland ii I S0 065: 991 (E) I ntroducti on Aqu eou s sol uti ons ethyl ene oxi de rai sed, becau se above Thi s whi ch of of the thi s of creases fal l s The cal l ed Th e occurs system becomes at agents temperature - of i s referred oxi de the cl ari fi cati on is often the the becomes is poi nt as the product i n- temperature h omog eneou s defi ned (defi ni ti on cl oud i ncreases in wh en as from Th e temperature whi ch system deri ved temperature to as the combi ned cl ari fi cati on” Vocabul ary thei r phases h omogen eou s whi ch of l i qui d temperature ethyl ene “temperature acti ve a agents wh en of two occ\J rs at of temperature the Surface formati on mol ecul es Th e surface-acti ve heterogeneous ph en omen on ph en omen on nu mber non-i oni c become in I S0 is 862: 984, No 0) determi ned as the “cl oud poi nt” Th e knowl edge cati ons, as of the the cl oud poi nt snrface-acti ve is of great properti es vary i mportance in very around rapi dl y al l appl i thi s temperature Th e determi nati on and preci se meth od assessi ng the of of the quanti ty mol ecul e However, poi nt the an d extent of thi s a l ong chai n Th e cl oud above and the l eads cri ti cal to the ethoxyl ated tures Methods mari l y Other di ffi cul t pearance further nati on C are and of the in separates wh en Thi s a rapi d meth od gi ven rel ati ng base cl oud asymptote; of is a wi th separati on; two phases, the temperature determi ne as products i nto property to a for temperature esters not i s rai sed speci fi c cl oud to tempera- oxi de to e g have Su ch over by deal non-i oni c pri - surface- condensati on fatty ami nes, wi th fatty ac- oxi de/propyl ene properti es properti es very therefore materi al s, ethyl ene a temperature or three E) are of such of aci ds poi nts of two Standard poi nt al cohol s, agents, cl oudi ng (D and poi nt I nternati onal cl oud fatty kn own cl oud exi stence methods as of fatty are thei r thi s the ethyl ene surface-acti ve cl oud an preci se cri ti cal possi bl e of su ch copol ymers, the to curve sol uti on sol uti on from mol ecul es of a progressi ve and towards i s l ess phases it is C speci fi ed to determi ne degrees, the determi nati on non-i oni c bl ock the two and deri ved base l ower the is qui ckest bonded that tends product i t i s the of deri vati ve and al kyl phenol s oxi de Two B agents l i pophi l i c i ds, types the a of these of a non-i oni c oxi de of checki ng is cl oudi ng A, wi th acti ve ethoxyl ati on deri vati ves for other ethyl ene temperature, appearance of be remembered method temperature thi s poi nt I n manufacture, of i t mu st consequence, ethoxyl cl oud of control range di sti nct speci fi ed for whi ch whi ch make i ncl ude cl oud for the methods the it ap- of several poi nts determi A, B and nnsui tabl e 111 INTERNATIONAL STANDARD IS0 065:1 991 (E) Non-ionic surface-active agents obtained from ethylene oxide and mixed non-ionic surface-active agents - Determination of cloud point Scope This International Standard specifies five methods for the measurement of the cloud point of non-ionic surface-active agents Methods A, B and C are applicable to non-ionic surface-active agents derived from ethylene oxide by condensation with a lipophilic compound which has no oxypropylene groups The selection of the method (A, B or C) depends on the temperature at which the aqueous solution of the product being tested becomes cloudy Methods D and E are intended for use, after agreement between the parties concerned, with products for which methods A, B and C prove unsatisfactory Such products include mixed non-ionic surfaceactive agents such as those derived from ethylene oxide/propylene oxide block copolymers The selection of the method (D or E) depends on the temperature at which the acid aqueous solution of the product being tested becomes cloudy Method E is not applicable, however, to products derived from fatty acids or fatty-acid esters NOTE The cloud point of products derived from fatty repeatability of the determination is verified acids or fatty-acid esters can only be determined if the Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard At the time of publication, the editions indicated were valid All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards in- dicated below Members of IEC and IS0 maintain registers of currently valid International Standards IS0 607:1 980, Surface active agents and detergents - Methods of sample division IS0 773: 976, Laboratory glassware - Boiling flasks (narrow-necked) IS0 21 74:1 990, Surface active agents - Preparation of water with known calcium hardness Selection of method NOTE It may be impossible to measure the cloud temperature of certain very pure derivatives of ethylene oxide if dissolved in distilled water of very low conductivity In such cases, the solution does not become heterogeneous at a definite temperature; instead, only a slight loss of clarity is observed However, replacement of the distilled water by an aqueous solution of sodium chloride (234 mgll) enables the cloud temperature to be measured 3.1 Method A If the aqueous solution of the non-ionic surfaceactive agent becomes cloudy at a temperature between “C and 90 “C, carry out the measurement in distilled water (see 8.1) 3.2 Method B If the aqueous solution of the non-ionic surfaceactive agent becomes cloudy at a temperature lower than OC, or if the product is not sufficiently soluble in water, carry out the measurement in an aqueous 25 % (m/m) solution of n-butyldiglycol (see 8.2) However, this method is not applicable to certain products with low ethylene oxide contents and which are insoluble in the aqueous 25 % (m/m) solution of n-butyldiglycol IS0 065:1 991 (E) 3.3 Method C If the aqueous solution of the non-ionic surfaceactive agent becomes cloudy at a temperature higher than 90 ‘C, carry out the measurement in a sealed ampoule (see 8.3), which makes it possible, by operating under pressure, to reach temperatures higher than the boiling point of the solution at atmospheric pressure NOTE It is also possible, if agreed between the parties concerned, to determine the cloud point in salt solution but this technioue is not so sensitive and there is no simple correlation ‘between the.results obtained in salt solution and those obtained with the sealed-ampoule method 3.4 Method If the acid surface-active temperature measurement acid solution, aqueous solution of the non-ionic agent tested becomes cloudy at a between “C and 90 “C, carry out the in standard volumetric hydrochloric c(HCI) = I,0 mol/l (see 8.4) If the acid aqueous solution of the non-ionic surface-active agent tested becomes cloudy at a temperature higher than 90 “C, carry out the measurement in water of calcium hardness 40 mg Ca*+ ions per litre and containing % (m/m) of butan-1 -01 (see 8.5) Principle The product under test is heated in solution at the required concentration until the liquid is completely opaque It is then cooled, with constant stirring The temperature at which the opacity disappears is observed Apparatus apparatus and: 6.1 Conical flask, capacity 250 ml, complying with IS0 773 6.2 Thermometer, graduated in 0,l “C, with a range appropriate to the temperature to be measured capacity 00 ml 6.4 Beaker, capacity 000 ml, containing a trans- parent heat-transfer fhlid (ethylene glycol, for example) 6.5 Test tube, capacity 20 ml 6.6 Ampoule, made of safety glass covered with wire gauze, outside diameter mm, inside diameter mm, height 20 mm 6.7 Analytical 6.8 Conventional balance heating appliance 6.9 Magnetic stirrer with heater Reagents Durina the analvsis unless otherwise stated, use only Reagents of recognized analytical grade and only distilled water or water of equivalent purity [2-(2-butoxyethoxy)-ethanol], 25 % (m/m) solution, for method B The n-butyldiglycol [C4H,0(CH,),0(CH,),0H] have the following characteristics: - density, ~20 = 0,954 g/ml + 0,002 g/ml; - refractive index, np = 432 + 0,OO1; sol- 5.3 Butan-l-01 , % (1 72/m) solution in water of calcium hardness 40 mg Ca*+ ions per litre, prepared in accordance with IS0 21 74, for method E 6.3 Graduated cylinder, E 5.1 n-Butyldiglycol 5.2 Hydrochloric acid, standard volumetric ution, c(HCI) = I,0 mol/l, for method D Ordinary laboratory D 3.5 Method - water content less than 0,l % (m/m) NOTE Even with the given specification, variable amounts of impurities in the n-butyldiglycol will influence the cloud point to a certain extent shall Sampling The laboratory sample of surface-active agent shall be prepared and stored in accordance with the instructions given in IS0 807 Procedure IMPORTANT - The cloud point is related to the number of ethylene oxide units bonded to the base molecule, but it also depends on the concentration of the solution It is therefore essential to operate the test at a clearly defined concentration I S0 Met h od at ( Use A a temperatu re Test Wei g h tory wh en cl oudi ness between “C Proceed appears an d porti on ou t, to sampl e the n earest ( see 0, Ol cl au se g, 0, g of th e as secon d 90 “C) Determi n ati on Pl ace th e 00 ml ated of porti on di sti l l ed cyl i nder di ssol ved Pl ace or 15 ml of th e th ermometer beaker it is no by water, thi s th e opaci ty th e th an th e th e sol u ti on the (6 ) wi th th e test Ad d tu be h as pl ace th e wi th the th ermometer opaci ty an d of the to cool at in sol uti on at At exceed the sti rri ng opaqu e ban d s di sappear pen di n g on puri ty the of cl au se l i qui d th e n ote Carry ou t di fferent cl ear more or non- i oni c u sed for opal escent, produ cts thei r de- an d preparati on th e ( see of materi al s) temperatu re porti ons n ot th e puri ty several by of stay materi al s on test feri ng may n atu re raw at Meth od B a temperatu re product unti l th an is ( Use wh en bel ow i nsol ubl e Test Pl ace 00 tory out, sampl e Pl ace 45 test to measu remen ts at l east ‘C are two on resu l ts di f- test of th e ( see pou l e th e a in “C, or wh en g of th e porti on test n- bu tyl di gl ycol is di ssol ved appears 90 “C) the to in g, th e water, 0, g of coni cal the fl ask measu red Sti r tai ni ng the As a unti l l abora- (6 ) wi th the th e test Ad d gradu - porti on th e h as Pl ace th e th ermometer sti rrer l i qui d (6 9) in to cool the i n th e whi l e th e the i ndi cated for - en d of a pro- ) fl ui d an d th e may fi gu re heati n g th e h eati n g becomes n ext mag wh en cl ou dy heat- transfer wh i ch th e met h od th e pl asti c ampou l e h eater at i t wi th (6 4) beaker ( see stop sti rri ng Seal pl ace th e ampou l e temperatu re as in th e operati on; tai n ed n ote Set am- mm transparen t seal ed (6 2) ampou l e the gl ass, or gl ass cover u pper from si n ce wel l 40 beaker Th e fl yi ng been th e an d th e gl ass apparatu s n ot to fl ame in sl i ghtl y safety h as seal ed a it agai n st of if it th e of fl ui d proj ect screen of sol u ti on approxi matel y Pu t bu rst to of heat- transfer shal l front thi s mean s gau ze precau ti on tecti ve in of a depth by wi re di sappears, 01 g, g of th e A fl ui d cl ou di n ess ( see 2) ou t by not N OTE If poi nt i n a seal ed th e coni cal sol u ti on fl ask (5 ) (6 ) Sti r several test temperatu re porti ons more unti l th an 0, at “C measu remen t s l east are two on resul ts di f- obtai n ed l abora- 7) in 0, Ol 7) water) n earest porti on porti on (6 3) ampou l e di fferent cl au se n earest qu anti ty (6 6) , coarse an d Determi n ati on th e th e di ssol ved Tran sfer Al l ow appears porti on to cl oudi ness than cl au se di sti l l ed cyl i nder neti c obtai ned cl oudi ness th e ( see compl etel y cl ou d 2 out, th e ml feri ng Wei g h at Determi n ati on Carry porti on sampl e th e wh en hi gher Test ampou l e Th e begi n n i n g the wh i ch whi l e th e tory ated unti l coal esce sl owl y wh i ch in appl i an ce appears th en Pu t tu be heati n g temperatu re Al l ow (6 5) th e temperatu re th e test tu be, ( Th e temperatu re N OTE 2, gradu - porti on wi th thi cken “C appears ) Read in wh i ch shal l more fl ask th e in h eat opaqu e ban d s ti me unti l sol uti on an d compl etel y of coni cal measu red Sti r (6 2) (6 4) sti rri ng forrn th e di spersed th e (6 8) , in (6 3) ( see 7) Wei g h test A C ( Use a temperatu re 8 met h od ( E) paragraph ) Met h od at l abora- in 065: 991 unti l Ad d th e ag reed can tech n i qu e th e su rface- acti ve 00 ml the parti es i n sal t cern ed, sol u ti on rather the th an ampou l e Th e aq u eou s bet ween be determi n ed is 50 g/l of di sti l l ed an al og ou s agen t sol u ti on to that bei n g of of met h od di ssol ved sodi u m in chl ori de A ( see 00 ml i n stead ) , of of an in water I S0 065: 991 ( E) ,, ; ,’ ;.: ; : ‘ ; y, ; ‘ : : , ; , ” ,, : :, : I , : , , , , ; ; ‘ : Q .j ; ;’ ‘ ’ “ , : - Safety screen - Th ermometer : , y: : , ’ ,., j , ‘, I : , : , ::, , : ; _ , , ;‘ : ‘, ‘L: : , , ; , , .;; :, : : _ , : : - Seal ed ampou l e - Test - Heat-transfer T sol u ti on fl u i d Sti rrer - Fi gu re at Met h od ( Use D a temperature wh en cl oudi ness between “C - Apparatu s no appears and for ti me by 90 “C) met h od opaci ty Test Wei g h tory porti on out, (see th e nearest cl ause 0, Ol g, g of the l abora- N OTE pen di n g 7) puri ty the Al l ow of th e sol u ti on temperatu re to temperatu re Th e on l i qui d the of th e cl au se temperatu re “C at cool at sl owl y wh i ch whi l e th e exceed wh i ch th e sti rri ng opaq u e ban ds di sappear to the sampl e the th an appears ) Read C shal l more Heater raw 3, n ote may n atu re of stay the materi al s cl ear or n on- i on i c u sed for opal escent, produ cts thei r de- an d preparati on the ( see 2) Determi n ati on Carry Pl ace 50 ml ured the of test the wi th test porti on porti on coni cal hydrochl ori c aci d graduated cyl i nder the hydrochl ori c i n the has di ssol ved aci d sol uti on or fl ask sol uti on (6 ) (5 2) , (6 3) Sti r di spersed, (5 2) to gi ve Ad d meas- unti l then a fi nal ou t di fferent feri ng several test by temperatu re porti ons not more unti l th an 0, measu remen t s at “C l east are two on resu l ts di f- obtai ned the add vol u me of 00 ml in Met h od meth od E ( Use D at wh en cl oudi ness a temperature appears hi gher than 90 “C) Pl ace ml of thi s the thermometer the beaker (6 8) , sti rri ng of (6 2) (6 4) the i t i s compl etel y form bands sol uti on and i n the heat sol uti on opaque whi ch i n the tube, test tube pl ace (6 5) the wi th the heati ng wi th the th ermometer ( The thi cken opaci ty and tube in appl i ance appears then Pu t 51 Test porti on unti l i n the coal esce At Wei g h tory ou t, sampl e to the ( see n earest cl au se 0, Ol 7) g, g of the l abora- I S0 Determi nati on Pl ace 00 th e ml test of porti on th e measu red th e in th e i cal fl ask cal ci u m/bu tan - - 01 wi th test 10 th e porti on g rad u ated h as (6 ) Ad d sol u ti on cyl i n der compl etel y (6 3) (5 3) , Sti r unti l or di s- di ssol ved persed Proceed secon d as in meth od D ( see 2, beg i n n i n g at th e 1 Repeatabi l i ty Th e di fferen ce n ati on s carri ed cessi on , on operator, shal l two as th e resu l ts I n di cate, of resu l t wh i ch to peratu re th e at resul ts th e fi rst deci mal by more pl ace, th e of at th an th e of became an d was mean sol u ti on ag en t measu remen t di ffer th e ag n Th e ari thmeti c n ot wh i ch su rface- acti ve opal escen t ei th er med i u m 0, mean th e in l east ‘C ou t th e th e resu l ts si mu l tan eou sl y, same n ot sampl e exceed 0, of two or in an d determi rapi d by th e su csame ‘C tem- Cl ou d cl ear or wh i ch th e at g/l poi n t poi n t Cl ou d Cl ou d n ess 11 at Th e poi nt in 00 g/l at sol u ti on : poi n t di sti l l ed g /kg water: in th e b) 40 mg bu tan - l - 01 : of th e obtai n ed same by sampl e two di f- shal l n ot “C report test report al l presen ce in seal ed g/l in of shal l i n cl u de th e fol l owi n g parti cu - mol /l h ydroch l ori c d) g/l , Ca* + in i on s water per l i tre of cal ci u m i n th e h ard- requ i red th e th e for compl ete i denti fi cati on of sampl e; a referen ce ri ed ampou l e: I,0 detai l s meth od to u sed, med i u m in thi s I ntern ati on al e g “I S0 wh i ch 065, th e Stan d ard meth od an d th e A”; measu remen t was car- ou t: resu l ts an d th e u ni ts in wh i ch th ey h ave been expressed: _ at resu l ts on l ars: c) at Test th e poi n t between l aboratori es exceed a) Cl ou d aci d di fferen ce feren t mad e n-bu tyl di gl ycol : Cl ou d Reprodu ci bi l i ty n on - i on i c EXAMPLES of between parag raph ) Expressi on Take (E) Preci si on 065: 991 e) an y u n u su al featu res n oted du ri n g th e determi - in I n ternati on al n ati on : presen ce f) an y operati on Stan dard, or n ot i n cl u ded reg ard ed as thi s opti onal - I I S0 065: 991 (E) _- _-_ - U DC _- _ 661 I 65543 Descri ptors: surfactants, Pri ce on pages based non-l onl c surfactants, - ethyl ene oxi de, tests, cl oud -m===_e - : - - poi nt determi nati on -. - _ =