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([f[ o""'snation: D 226e - s3 An Amedcan Nahal SlsrxH

Standard Test Method for


Evaluation of White Mineral Oils b'y UltraViolet Abs6rptionl
designation indicatcs thc 1ar of
This sandard is issued under rhe fued designation D 2269; rhe numbcr immediatcly followin-grhe
oq in the ofrevision,-the year oftast rcvision. ,t number in parentheges indicates the year ofltst rcappmval' A
original adoption case
suierscript ipsilon (r) indicat€s an editorial chan'e since the last revision or reapprovd.

A = lo9,6 (l/t) = -log,oT (1)


l. Scope
l. t This test method describes a procedure for the orilrD: where 7is the transmittance as defined in 3'2'l'
ination and evaluation of NF and USP grade white mineral 3.2.2 absorpti"ity, a, n-the absorbance divided by the
oils. product of pathlength and r:oncentration' In symbols:
"ample
1.2 This test method is not applicable to oils containing a: Albc Q)
additives soluble in dimethyl sulfoxide that exhibit fluores-
where A is the absorbance as delined in 3.2'2, b is the sample
cence or fluorescence quenching properties.
1.3 The values in SI units are regarded as the standard'
p"tnf*gtl as defined in 3.2.3, and c is the concentration as
defined in3.2.4.
The values stated in mesh are for information only.
3.2.3 concmfiation, c, n-the quantity of sample ex-
1.4 This standard does not purport to address all of the
in grams Per litre.
safery problems, d any, associated with its use. It is the
pressed
' i-i.q simpte iathtensth, b, n-the distance in centi-
risponsibility ofthe user ofthis standard to establish appro-
health practices and determine the applica' metres, mers,rt"ci in the airection of propagation of the beam llly
priate safety aid
'bility
oi r'egulatory limitations prior to use. For specific of oai-t energy, between the surfaces of the specimen on tllp
,tlfr
which tUe raaiint energy is incident and the surface of the
precautionary statements, see 7.1.1, 7.l.2,and7.l-3. . specimen
-- from vrhich it is emergent ,tl}
2. Refcrcnced Documents 3.2.5 transnittance, T, n-lhe ratio of the radiant poriler
toos-itr.a by the mineral oil extmct in its cell to the radiant
2.1 ASTM Standards: poor"r t astiittua by the solvent control in its cell' Ex-
D 1840 Test Method for Naphthatene Hydrocarbons in pressed by,
Aviation Turbine Fuels by Ultraviolet Spectrophoto- PJt'"T : (3) l,,h
metry2
E l3l 'ierminology Relating to Molecular Spectroscopy3 where f" is tnettadiant power trasmitted by the mineral oil lltr

E 275 Practice for Describing and Measuring Performance extract ioa f" isthe radiant powertransmitted by the solvept
1ii,
of Ultravioleg Visible, and Near Infrared Spectropho- control.
tometers3
Other Standard: 4. Sumn4ry of Test Method
U.S. Pharmacopeia (USP Xl[)A'{ational Formulary (NF 4.1 Asample of oil is extracted with dimethyl sulfoxi-d.e
xvlDo andtheultravioletabsorbanceoftheextractisdeterminedin
tn" *og" from 260 to 350 nm. The absortance is compared lllN

3. Terminology with that of a naphthalene standard'


IttP
3.1 DeJinitions:
3.1.1 For definitions of terms and symbols relating to
5. Significance and Use 'il|)

absorption spectroscopy see Terminology E 131. Terms of 5.1 The ultr:rviolet absorption of white mineral oils is
particular significance are the following: *"a to determiae their suitability for use in food, drug, and
3.l.l.l ridiant enerfn), n-energy transmitted as electro' cosmetic aPplications.
magnetic waves. 5.2 The-U.S. Pharmacopeia and the National Formulary 4h
i.t.t.Z radiant power, P, n-the rate at which energy is tp""inotio* for mineral-oil require the measurement of tlllt

transported in a beam ofradiant energy. ultraviolet absorPtion. rlif,

3.i Description of Tcrms SpeciJic to This Standard: iltr

3.2.1 absorbanci, ,1., n-the logarithm to tle base 10 of 6. Apparatus liliif

the reciprocal of the transmittance, T. In symbols: 6.1 Spearophotometer,equiprred to handle liquid samples
i"l-*--p"tn Gn4n cels.-The in-sttomeot shall be capable of +l'0.%'ot
-*oti"g absoibance with a repeatability of
rThis test method is under the jurisdiction of ASTM Committee D2 on betterfrom an average at the 0'4 absorbance level in the
petroleum Products and Lubricants and is the direct responsibility of subcom- of
rp""t*f region od290 nm with a nominal band width
miaee D02.04 on Hydrocarbon Analysis. -ot
Current edition approved Nov. 15, 1993. Published January 1994' Originally 1 nm or less.
published as D 2269 - 64 T. Lrst previous edition D 2269 - 88'
2 Annual Book ofASTM Standards, Vol 05.01'
Ncrrrl_Forrecommendedmethcdsoftestilgspectrophotometers
1 Annual Book of ASTM Standards, Vol 14'01 ' to be use<l in this test method refer to PncticeE2T5'
.C 1989 The United States Pharmacopeial Convention, Inc', 12601 6.2 Fused Quartz Cells,tvto, having path lengths of l'00
Twinbrook Parkway, Rockville, MD 20852-, Library of Congress Catalog Card + 0.005 c-, & better. The distz.nce in centimetres does not
Number 83-640O88.

743

,'i
filb o zzsg
Nore 7-This absorbance will be approximately 0'30'
cell in which the sample is
8. Procedure '

8.1 Transfer 25 mL of the mineral oil and


25 mL oi
funnel and, mix' Add 5'0 mL ot
hexane to a separatory
ai*"ttwi ."ffo*iae ,na shake the mixture vigorously for at
used.
leastl.rnin.Allowtostanduntilthelowerlayerisclear.-
-- add I
Reagcnts and Materials
g.Z- the lower layer to a separatory funnel'
io"tfer
-r, 7.
tire mixture vigorously. Allorv to
' 7.1 Solvents:
,,,1 of fr"iune and'shake
it lower layer is clear. Draw off the lower la1er.
7.1.1 Normal Hexane-Pure grade, having an ullraviolet
,t "J
""iii
e;sign;t"a "mineral oil extract, into a l-cm cell'
light ;t;;"nc€ not exceeding 0'02 down to 260 nm'wften --i.T n'aa as5.0 mL of dimethyl sulfoxide to-25 mL of
hexanc
rieasured in a l-cm cell (Warning-See Note 2')The-p"."t{ for at least I min
shall be such that the solvent control as defrned in
8'3 shall i"""'t"p"t*ty n on"f. Shake vigorously clear' Draw offthis
haveanabsorbancecurvecomparedtrtwatershowingno ;;J"6; to stand until the loweilayer is
as solvent control, into a l-cm cell'
ot*o"out impurity perks and no absorllance exceeding that '-'8; desienated
laver.
r;#;t* the absorbance of the mineral oil extraci
oiOi-"itVf .rffo*iOi compared to.u'ater at any wavelength *ilqJ to in" .otueot control through the range 260 tt'
in the range 260 to 35(' nm, inclusive'
350 nm iirclusive.
Norr 2: Warning-Normal hexane is extremely flammable,
harmful if inhaled. Mayprrduce nerve cell dalnge'
9. Correction for Inhibitor Contenf
(Isooctane)
7.1.2 Spectroscopic 2.2.4-Trimethylltentane 9.1 A correction for the absorbance due to inhibitor
mat

be-;ade as described below if a suffrcient amount of


(Warning-See Note 3.). tht

Norr 3: lVarning-Isooctane is extremely flammable' harmful if il; trhtbttoi containea in the sample and the inhibited

--Noi,
iuhaled. ;;;;;;;=iluute to prepare a b]end' The.concentration oi
4_For a suiUble r.sooctane and a procedure for preparing u]aitio"rr inhibitor to be added to the inhibited samplc
,p"aior"opi" sottens fronr commercially available stocks' see
Test
itroufa be equal to the concentration contained
in tht
Method D 1840.
inhibited samPle.
7.1.3 Dimethyt Sulfcxide-For use as spectroscopic sol-
Nore 8-The inhibitor @ntent is usually expressed in:'8rams
pounds pc
,.rri-(Nott 5) (warning-See Note- 6') Pure grade; clear'
tfro"*.aLtt ls. Pound per thousand barrg!-x 0'00285 0c
*ui.r'*tit., ig.g y"dimethyl sulfoxide, tn'p' l8'5"C, Tq iii.". io. lb/ldm barrets x 0.00285 : 0.00855 e/litre.
"1 example, 3
absorbance curve comp:ued to water not exceeding l'0 -"t
,eirrr and showing no extraneous impurity peaks in the 9.2 Weigh a minimum of 50 mg of. inhibitor in a
wavelength range up-to 350 nm when tneasured through a fill to volume with inhibite{ *ry919.3ni
path length of I cm. -ii if,otoughty. Make further dilutions with inhibited
"offi"iti"-nask,
sample, as neoessarJ' to obtain the desired concentration
oi
NoreS_Thissolventcanbepurifiedbypercolationthrougha
f -Z-- cof"o" ottype CAL 1.68 by Q:420
mnr (12 by 40 mesh) activatcd --g,i inhibitor.original inhibited sample in accordance uith
added
iidthl
drawn to 6'4 mm in
;i;;iTh. *iu-o is 25 mm in diameter, for containing the Test Method D 2269 and label it Run A'
diameter at the bottom and has a reservoir at thr: top -
fiq-JCG**f is ptacea in the bottom of the column' and aboul!] t.4 fu" the blend containins known amoyry "f *9{
latti
or 0'0149 to-0'074 (l0O to 200
i]"-"f O:zOz to 0.074 (25 t(, 200 mesh) Method D 2269 and
iot iUito, in accordance with Teit
placed on top of it' The columu. is hled with activated
-*nj tni* g"iis itrtq the reservoir and
it Run B.
'-
Ail"l aod Ue-sp"cttoscopic solvent Poo*l pressure' The e.3-.e"i"ofut" the difference in absorbance between
Run B
;ll.ofi to p.r*t"rc Orougl'tUe charcoal at.atmosPheric and Run A at corresponding spectral positions as follows:
the: column and stored in
,"k; *iti"rit couectfat thq bottom of
M:At- Ao {'l
gfq*.t"pp.*d.bottles as it is very hygroscopic and reacts with rcme
ietal coutainers inrthe presence of air,
where:
,' 'Nore 6: lVarning-Dmethyl sulfoxide ji rpmbustible' Also it is
a7-: Oiff.r.t . in absorbance at a given spectral position'
rapidly absorbedlGough skin. See Annex Al'3)'
; :;;;6;; of Run B at the same spectral position'
.2 Naphthalene-htfi-pttity, 99 +
o/o'
1
and
i.l stiiioia Referdce' Soliion--A solution containing ,4- : absortance
-"q.S.i"C-"-r."t
of Run A at the same spectral position'
per litre of-purified lsooctane' thi absorbance at each spectral position c
' mg of naphthalene
7.0
t.q"Sta"aird Referince Spectfogram-The absorbance follows:
A": Ao- M lj
curve obtained by scanning th", stindatd reference solution
ir tn.i-i" from zOO to lsO nm"against liooctane of the where:
*t*-tp"d.a purity as that used to pre'pare the standard' A- : gtriected absorbance at each spectral position' fror
(6.21 ""q.0'ft;ki[" poi"i* orinflection on the spectrogram
'--i.S Snnaard Reference Absorbance'-The absorbance at whict
Run A at waveftngths lower and higher than those
275 nmof the standard reference spectrogram' (6'2) were increased'

JAvailablefromPil6bu8hCokeandClremicalc().'19?0CrantBldg.' 6Corrcctionlbrinhibitorcontcntlritsn()lbccoc(x\,erativclylcsllal.
Pittsburgh, PA.

7M

rm,
I

I
t
(fff[ o ezos

I I
9.6. Draw a baseline tangent to the curve connecting the 11. Precision and Bias
tl.l The precision of this test methodtest as obtained by
two points.
rt f,tti*f of interlaboratory results is as
| 9.6.2 Rcad the absorbance, A7, along the baseline at each
spectral position.
follows: "*imination
9.7 Compare Aa and A" at each position. If l" is less than
ll.l.l Repeatability-The
-by difference between successrve
test-results irUtuir.a the sam3 operator with the same
/a,it is indicated that the inhibitor content of the origindl under constant operating conditions on identical
sample is less than the amount added. "pp*iot
tii *ii"riA, would in the long-run, in the normal0'014 and
9.8 Use the absorban c* A, or.4a whichever is greater, to op"iuti.,n of the test method, exceed
compare to the solvent control throtrlh the range 260 to 350 "orrect
absorbance units only in one case in twenty'
nm, inclusive. ll.l.2 Reproducibility-The differerce -betweenopera- two
single and independent resuls obtained by different
iori working in-<tifferent laboratories on identical test mate-
rial, would-in the .long run, in th9 ^oglq'l and correct
10. Report the testmeiho4lxceed 0'044 absorbance units
"E*ti", "f
--f in one case in twentY.
onlv
10. I
Report the difference between the absorbance of the f .i.g These precision data were obtained on absorbances
mineral oii extract and the solvent control at the wavelength in the wavelength region 275 to 280 'nm'
desired. - i.Z .ai^-lt it procedure has no bias because the value
of ca! be defined only in terms of a test method
Norr 8-€alculations can be found in U.S. Pharmacopeia (USP "i*iU*o
12. Kelvords '
XXII)/National Formulary (NF X\III).1
l2.l ultraviolet spectroscopg,white mineral oil

The funerican Soiety ,ot Testing atd Matedals takfn tto rxlJltbt tqpeditng
the uaild!-l q
any Dd(e,il tlgfts ssse,t€|ol connectlon

pi-ii,tia.Users
n ot thb staidiJ rlr.-i[U*rh ldl'r:r,rd inat oaqA'atn d ttEvailcfity'nol anv such
wtth any ftom mentionad
prr*r;bh, ine rrcx.& Wihgenant d s,tch ttghts, arc stkdy thdt orn responslbilltt'
"tn
rr,is standard is suqFci to twtston at any th/, by the rcpotffie tl''',/|tr,,!
@,,,mttt,f aill ttu,ll b
.ft,view.i, avery five.yoa,r- and

wtthcldwn. Varr-r;orn rpntsi-ffii *u tn relttston d lhb 5ra"dad q lq acdittonal stadards


It not revtslg, eitlw rllrpruvecl or
and sho.rtdbo addrossod to *sru i*ewrtn". v*, ffi iru-t@Na carolut c,,1rjtr,etr/rfii a a fi|,ff,/.ilto d tl?€ ta6,po/tslble
tehnicdt cot,rntilee, whtch you mdy ,11teg. tl you leel tna yui-;;,,,,fr t*,. not *"e6 a 1afi Mq yat slutld m*e yanr
vitrl,,1. known to tt"
rcru c*riii. @ gand:ads, rslO R;co St', Phfladetphla' PA l9'0:l'
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