Table Of Contentइंटरनेट मानक
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IS 7918 (2001): Diethylene Glycol [PCD 9: Organic Chemicals
Alcohols and Allied Products and Dye Intermediates]
“!ान $ एक न’ भारत का +नम-ण”
Satyanarayan Gangaram Pitroda
““IInnvveenntt aa NNeeww IInnddiiaa UUssiinngg KKnnoowwlleeddggee””
“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै”
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“Knowledge is such a treasure which cannot be stolen”
IS 7918:2001
Indian Standard
DIETHYLENE GLYCOL — SPECIFICATION
(First Revision)
ICS 71.080.10
0 BIS 2001
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN,9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
Price Group 4
Fet?mly 2001
Organic Chemicals(Misc)SectionalCommittee,PCD9
FOREWORD
This Indian Standard (FirstRevision)wasadoptedbytheBureauofIndian Standards, afterthe draftfinalized by
the Organic Chemicals (Mist) Sectional Committee had been approved bythe Petroleum, Coal and Related
Products Division Council.
This standard wasfirstpublished in 1975.Thecommitteeresponsibleforlhepreparation ofthis standard decided
to revise the same in the light ofthe experience gained over the years soasto align the same with the latest
development intechnology and alsoonthe quality ofrawmaterial presently available.
Diethylene glycol isused as a conditioning agent and lubricant for cotton, rayon and wool fibres to increase
flexibility and improve elasticity. It isalsoused asahumectant for softening and controlling moisture. In the
rubber industry, it isused in compounding to counteract the retarding effectofminetal fillers. Its other uses
include gasdehydration, particularly natural gas,asasoftening agent ingluesandadhesives andinthe extrac-
tion of aromatics. Considerable assistance has been derived from ASTM D2694: 1987in preparation ofthis
standard.
Forthepurpose ofdeciding whether aparticular requirement ofthis standard iscomplied with, thefinal value,
observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with
IS2:1960 ‘Rulesforrounding offnumerical values(revised)’. Thenumber ofsignificant places retained inthe
rounded offvalue should bethe same asthat ofthe specifiedvalue in this standard.
IS 7918 : 2001
Indian Standard
DIETHYLENE GLYCOL — SPECIFICATION
( First Revision)
1SCOPE 3REQUIREMEN’I?3
This standard prescribes the requirements and the 3.1Description
methods ofsampling andtestfordiethylene glycolfor The material ishydroscopic. Itshallbefreefrom sus-
industrial use. pended matter and shall bemiscible with water in all
proportions.
2NORMATWEREFERENCES
Thefollowing Indian Standards arenecessruyadjuncts 3.2 The material shall also comply with the require-
to this standard. The standards contain provisions, ments prescribed inTable 1when tested according to
which through reference in this text constitute provi- thereference givenunder CO14and 5ofTable 1.
sions ofthis standard. Atthe time ofpublication, the
4PRECAUTIONINHANDLJNG
editions indicated werevalid. All standards are sub-
Thematerial shallbekeptwellprotected from atmos-
ject to revision, and parties to agreements based on
pheric humidity as it absorbs water vapour from the
this standard are encouraged to investigate the
atmosphere.
possibility ofapplying the most recent editions ofthe
standards indicated below: 5PACKINGANDMARKING
ISNo. Title 5.1 Packing
1070:1992 Reagent grade water (third revision) Thematerial shallbepackedinwell-closedcontainers
preferablywith replaceable closure.
2362:1993 Determination of water by the Karl
Fischer method (first revision) 5.2 The container shall be closed and shall bear
4905:1968 Methodsforrandom sampling legiblyandindeliblyfollowinginformation:
5298:1983 Method for determination ofdistilla- a) Nameofthemateria~
tionrangeandofdistillationyield@st b) Netmassofthematerial inthecontaine~
revision) c) Nameofthemanufkturerand hisrecognizedtmle
8768:1988 Method of measurement ofcolour in mark, ifany,and
liquidchemicalproductsinHazenunits d) Batch number or lot number, in code or other-
~rst revision) wise.
Table1RequirementsforDiethyleneGlycol
(Clause3.2)
sl NO. Characteristic Requirements Methods of Test, Ref to
I
1Annex IS No!
(I) (2) (3) (4) (5)
i) Colour, Pt-COscale, Max 15 — 8768
ii) Relative density, 27”C127°C 1.l14to 1.117 A —
iii) Distillation range, B —
a) Initial boiling point 240°c
760 mm Hg, Min
b) Dry point 252°C
760 mm Hg, MUX
iv) Water content, percent by mass, Max 0.2 c —
~) Acidity (as acetic acid) percent by mass, Max 0.01 D —
vi) Iron content ppm, Max 1.0 E —
vii) Monoethylene glycol content, percent by mass, Max 0.5 1? —
viii) Triethylene E-.IVGO1content...gercent bv. mass..Max 1.0 F .
1
IS 7918 : 2001
5.2.1 BIS Cert.ij2cation Marking 6 SAMPLING
The container may alsobe marked with the Standard The procedure for sampling and the criteria for
Mark. conformity of the material shall be as prescribed in
AnnexG.
5.2.1.1 The use ofthe Standard Mark isgoverned by
theprovisions ofBureau ofIndian StandardAct, 1986 7QUALITYOFREAGEN’IS
and the Rules and Regulations madethereunder. The
Unless specified otherwise, pure chemicals and dis-
details of conditions under which the licence for the
tilledwater(seeIS1070)shallbeemployedinthetests.
useofthe Standard Mark maybe granted tomanufac-
turers orproducers maybe obtained from the Bureau NOTE — ‘Pure chemicals’ shall mean chemicals that do
ofIndian Standards. not contain impurities, which affect the results of analysis.
ANNEX A
[Table 1,SINO. (ii)]
DETERMINATIONOFRELATIVEDENSITY
A-1OUTLINEOFTHEMETHOD Insertthestopperandimmerseinthewater-bath main-
tained at27.0* 0.2 ‘C. Keepthe entire bulb covered
Inthismethod, mass ofequalvolumes ofthe material
withwaterandholdatthattemperature for30minutes.
andwaterarecompared at27”C.
Carefidly remove any water, which has exuded from
A-2APPARATUS the capilla~ opening. Remove from the bath, wipe
completely, dry and weigh. Again clean and dry the
A-2.1RelativeDensityBottle—25-Inlcapacity.
relative densitybottle. Using the material under test,
A-2.2Thermometer— Anyconvenientthermometer proceed exactlyasin the caseofwater and weigh the
ofasuitablerange with0.1‘CorO.2°Csubdivisions. bottlewiththematerial.
A-2.3 Water-Bath —capable ofbeing maintained at A-4CALCULATION
27.0*0.2°C.
Relativedensityat27°C/270C = fl~~
A-3PROCEDURE
where
Clean and dry the relative density bottle. Weigh and
fillwithrecentlyboiledandcooledwaterat27°C,Fillto A =massing oftherelative densitybottle with
overflowing by holding relative density bottle on its thematerial,
sideinsuchamanner astoprevent entrapment ofair B= massing ofthe relative densitybottle, and
bubbles. C= massing oftherelatie densitybottle with
water.
ANNEX B
[Table 1,SINO. (iii)]
DETERMINATIONOFDISTILLATIONRANGE
B-1PROCEDUXE B-3CORRECTION FORBAROMETRIC
PRESSURE
Determine the distillation range bythe procedure as
prescribedin1S5298applyingfollowingcorrections. Ifthebarometric pressureprevailing during the deter-
mimtion is760mmHg,nocorrection needbeapplied
W2CORRECTION FOR THERMOMETER
tothespecifiedtemperature andthethermometer read-
READING
ing may”beused as such. If however the prevailing
B-2.1ErrorinScale barometricpreasuredeviatesfimn760 mmHg, thespeci-
Inallthethermometer readings, makethecorrections fiedtemperature shall alsobecorrected asfollows:
asindicated onthecalibration certificateoftheinstru- a) Foreve~ 10mmabove760mrnHg,subtract0.5°C
ment. fromthespecifiedtemperatum, and
2
IS 7918: 2001
b) Forevery 10mmbelow760mmHg,add0.5°Cto NOTE — These corrections are valid only for pressure
the specifiedtemperature. above 700 mm Hg.
ANNEX C
[Table 1,S2N0. (iv)]
DETERMINATIONOFWATERCONTENT
C-1GENERAL C-2PROCEDURE
Water content is determined by the Karl Fischer Takeabout20gofthe material, weigh accurately and
method. determine thewater contentbytheprocedure givenin
IS2362.
ANNEX D
[Table 1,S1.No. (v)]
DETERMINATIONOFACIDITYASACE’I’iCACID
D-1OUTLINEOFTHEMETHOD catesthe presence ofalkalinity. Ifthe solution iscol-
orless, titrate with standard sodium hydroxide solu-
Thematerial istitrated with standard sodiumhydrox-
tionuntil apalepink colour persists formore than 15
idesolutiontothephenolphthalein endpointandfrom
seconds.
the volume of standard sodium hydroxide solution .
used, acidity iscalculated asacetic acid. Take100mlofdistilledwaterinanother500-Inl coNcal
flaskandcany outablank test.
D-2REAGENTS
D-4CAKULATION
D-2.1SodiumHydroxide Solution—Approximately
0.1N. (~- J’Jx6x N
Acidity (asacetic acid), =
percent by mass M
D-2.2Phenolphthalein Indicator-O.5 percent(m/m)
in i.~o-propylalcohol and make it faintly pink bythe where
addition ofdilute sodium hydroxide solution.
V,=Volumeinmlofstandardsodiumhydroxide
D-3PROCEDURE solutionusedinthetestwith thematerial,
V~=Volumeinml ofstandardsodimnhydroxide
Weigh accurately about 100 g of the material to the
nearest 0.1gin a500-ml conicalflask.Pourabout 100 solution usedin theblank test,
mloffreshlyboiled andcooleddistilled waterandfew N =Normality ofstandard sodiumhydroxide
dropsofphenolphthalein indicator. Mix-well andnote solution, and
the colour of the solution. A pink coloration indi- M =Massing ofthe material taken forthetest.
IS 7918 : 2001
ANNEX E
[Table 1,SINO. (vi)]
DETERMINATIONOFIRON
El GENERAL each standard, corrected for the blank. Prepare a
calibration curve by plotting the absorbance of the
Two methods for determination ofiron content have
standard iron solutions in 5 cm cells against the
beenprescribed, namely.
milligramsofironper 100mlofsolution.
a) Ortho-phenonthroline method, and
E-2.4.2Analysis ofSample
b) Ammonium thiocyanate method.
Weighabout80gofsamplenearestto0.1gina100ml
E20RTH0-PHENONTHROIJNE METHOD glassstopperedcylinder.Makeup to80mlwithwater.
E-2.10utline oftheMethod Add80mlofwatertoanother glassstopperedcylinder
asblank. Add5mlofhydroxylamine hydrochloride to
The sample is diluted with water and the iron deter-
eachcylinderandmakeupto 100mlmarkwith ortho-
minedphotometrically atapproximately510 nmbythe
phenonthroline solutionand mix.Allowtostand for5
ortho-phenonthroline method without a preliminary
minutes and measure theabsorbance using 5cmcells
ashing. In order to overcome the depression of the
at 510nm corrected forblank. Read mg ofiron from
ferrous-ortho-phenonthroline complex alarge excess
graph.
of hydroxylamine hydrochloride and ortho-
phenonthroline solutions are added. E-2.5Calculation
E-2.2 Apparatus Calculateironpresent inpartspermillion, asfollows:
Iron,ppm=(J?7S’x) 1000
E-2.2. 1 Spectrophotometer — Cdpabieofmeasuring
lightabsorption atapproximately510 nm.
where
E-2.2.2 Absorption Cell— 4-cmlightpath. W= ironfound,mg and
E-2.3 Reagents S= sampleused,g.
E-2.3.1 Hydroxylamine Hydrochloride Solution — E3 AMMONIUMTFIIOCYANATEMETHOD
300@l.
E-3.1OutlineoftheMethod
E-2.3.2 Iron, Standard Solution (1 ml = 0.005 mg
Themlour producedbyaknown quantity ofthemate-
Fe)– Weigh exactly 0.7022 g offerrous ammonium
rial with ammonium thiocyanate iscompared with a
sulfate hexahydrate [FeSOd(NHi)zSOd:6H20]minim-
controlcontaining known quantity ofiron.
um purity 99.5percent, disso lvingin500rrdofwater
containing 20mlofsulphuricacid (l$SOd,Sp.Gr.1.84) E-3.2APPARATUS
anddilutingto 1000 mlwithwater.Dilute50mlofthis
E-3.2.1Nessler Cylinders — 50ml capacity.
solutionto 1000 mlfor0.005mghnl.
E3.3 Reagents
E-2.3.3 Ortho-phenonthroline Solution — 3gll.
E-3.3.1HydrochloricAcid— 1:1(v/v).
Dissolve 0.75 gof 1,10phenonthroline monohydrate
in25mlofiron freeethanol and dilute to250mlwith E-3.3.2 Potassium Permanganate Solution — 0.1 N
water. approximately.
E-2.4 Procedure E-3.3.3 Ammonium Thiocyanate Solution — 60
percent (m/v).
IL-2.4.1Preparation of Calibration Curve
E-3.3.4Mixture ofAmylAlcohol andAmylAcetate —
Prepare aseriesofatleastfivestandards byadding 1.0
1:1(v/v).
mlto12.0mlofstandardironsolution(1ml= 0.005mg
Fe)to 100mlglass-stoppered cylinders.Makeupto80 E-3.4StandardIronSolution
mlwith water. Add 80mlwater toanother glass-stop-
E-3.4.1Standard Iron Solution A
pered cylinder asablank. Add5mlofhydroxylamine
hydrochloride solution, to each flask and makeup to Dissolve 0.7022 g of ferrous ammonium sulphate
100ml with ortho-phenonthroline solution and mix. @?eSO,(NH,),SO,.6~0] inwaterinaone-litmvohrmet-
Allowtostandfor5minutes. Obtain theabsorbanceof ricflask.Add4mlofconcentrated sulphuric acidand
4
IS 7918 : 2001
makeup thevohune tothemarkwithwater.Onemillili- permanganate solutionandmixthoroughly. Add5ml
treofthis solution contains 0.1mgofiron (asFe). ofammonium thiocyanate solution and 10ml ofamyl
alcohol and amyl acetate mixture. Makeup to 50ml,
E-3.4.2 Standard Iron Solution B
shake vigorously and allow the layers to separate.
Take 100ml ofstandard iron solution Aand dilute to Compare the intensity ofany red colour produced in
1000 mlwithwaterinaone-litrevolumetricflask.One
the upper layer with a corttrol test carried out in
millilitre ofthis solution contains 0.01 mg ofiron (as
anotherNesslercylinderinthesamemanner using5ml
Fe).This solution shallbeprepared flesh. ofstandard iron solution Binthe control test.
E-3.4 Procedure
E-3.5INTERPRETATION OF RESULTS
Accurately weigh 50gofthe sample in aplatinum or
silicadish(100mlcapacity). Placeonasand-bath and The limit prescribed in Table 1shall betaken as not
carefully evaporate to dryness. Cool, add 2 ml of having been exceeded if the intensity of colour
hydrochloric acidand25mlofwaterandheattofacili- produced in the test with the material is not greater
tate dissolution and cool. Add one drop ofpotassium than that produced inthe respective control test.
ANNEX F
[Table 1,SINO. (vii) and(viii)]
DETERMINATIONOFMONOETHYLENEANDmniwxm GLYCOL
F-1OUTLINEOFTEEMETEOD Finaltime : 15minutes
Asmallvohnne ofdiethyleneglycolisinjectedintothe Carriergas : Nitrogen
gaschromatograph containing apacked column with FIDhydrogen : 25rnlhninute
Carbowax 20 M as stationary phase on chromosorb Air : 250mlhninnte
GHPassolidsupport.
Samplesize : 3.0microlitrediluted
Quantitativeresultsamobtainexibyusing suitableelec- withiso-propyl alcohol
tronicintegratorandexternalstandardizationtedmique,
NOTE — The above gas chromatographic conditions are
whichgivesdirectconcentrationofeachimpurityalong
only suggestive, bowever, other gas chromatography with
withthechromatogram, are%retention time,etc. different columns may be used provided standardization/
calibrations are done after setting up chromatographic con-
F-2APPARATUS
ditions for the required resolution.
F-2.1Gas Chromatograp—Any instrument havinga F-3REAGENTS
thermal flameionization detectortha t maybe operated
NitrogenChromatographic Grade
atthe conditions given below:
Pure Compound forCalibration — monoethylene
Detector : Ftameionization glycol and
column : Stainless steel triethylene glycol
Isopropyl alcohol
Length : llocm
I.D.10.D. : 2mm/ l/8inch
F4PROCEDURE
Stationary phase : &rbowax20 M
Prepare asyntheticmixture containing knownweight
Solid support : ChromosorbGHP100/ percentageofMEGandTEGinpureDEG.Dilutesyn-
120mesh thetic mixture 1:1 with iso-propyl alcohol. Set the
Injector type : Packedwith glasswool chromatographyandtheelectronicintegratorasrequird,
andinject3microlitre ofdilutedsyntheticmixture. Al-
Temperatures
lowthe chromatogram to develop. At the end ofthe
Injection Port : 250“C
run stoptheintegrator. Calculate factors asfollows:
Detector : 250‘C
Oveninitial : 150°c 0/0MEG obtainedbyGC
FM=
Initialtime : 2minutes Actual‘?4.MEGinsynthetic mixture
Progzunming rate : 5“C/minute 0/0TEG obtainedbyGC
m=
Finaltemperature : 200°c Actual TEG insyntheticmixture
70
5
