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An AmrlcanN&na, St&(ffi

D 2269- 93

StandardTest Methodfor
Evaluation of White Mineral Oils b-yUltraviolet Absorptionl
thc year of
immcdiatcly foltowinr the designation indicatcs
This standard is issued under rhe fixed designation D2269;thenumbcr
year of ltrst rcapgoval' A
tbc
indicatcs
parenthcscs
in
outt"t
ge
hst r"ti-r;;n
original adoption o., in thc Caseof revision,-rhc V*,
rcapproval.
ipuilon 1.; indicares an editorial change since the last revision or
,uil,*ript

A = log,e(l/f) = -log,oT

test method describesa procedurefor the examevaluation of NF and USP gradewhite mineral
rcst method is not applicableto oils containing
in dimethyl sulfoxide that exhibit fluoresorescencequenchilg ProPerties'
""lu"t in Si units are regardedas the standard'
in mesh are for information only' -- stated
-itandard
does not purport to address all of the

(l)

where Iis the transmittanceas definedin 3'2'l'


by the
3.2.2 absorptivity, a, n-the absorbancedivided
symbols:
In
r:oncentration'
ptoau& of sanpte pathlen$h and
Q)
a = A/bc
whereA is the absorbanceasdefinedin3.2.2,b is the sample
p"Of"tgtn as Aeflrneain 3.2.3,anrl c is the concentrationas
in'3.2.4.
defined
ex3.2.3 concentration, c, n-the quantity of sample

ns, if any, assoiiatid with its use. It is the


of tie user of this standard to establishapp.ro'

aia neaUnpiacticesand determinethe applica'


ulatorv limitationsprior to use. Fot specific
see7.1.1,7.1.2,and'7.1.3.
statiments,
Documcnts
Standards:

t Method for NaphthaleneHydrocarbonsin


Turbine Fuels by Ultraviolet SpectrophotoRelating to Molecular Spectroscopy3
foibescribing and MeasuringPerformance
g Visible, and Near Infrared Spectropho-

from vrhich it is emergent


sPecimen
-g.Z.S transnfittance, T, n-the ratio of the radiant power
oil extract in its cell to the radiant
by the *i"".t
t-or-itt"a
solvent control in its cell' Exthe
bv
d
;;;d;.itt
pressedby,
(3)
T =p$,.
oil
where P" is thdl;diant power transmitted by the mineral
solvept
the
by
power
transmitted
"*to"t J"a P" is the radiant
control.

(USP Xll)/National FormularY (NF

energy, fl-energy

transmitted as electro-

power, P, n-the

rate at which energy is

in a beam ofradiant energy.


'iption of Terms Specilic to This Stgnd3rd:
i, ,5.,,-th" togaritnm to the base l0 of
of the transmittance,T. In sYmbols:
Committee D2 on
wrhod is under the jurisdiaion of ASTM
of Subcomresponsibility
the
direct
is
and
ana Lubricants
t
m Hydrocarbon AnalYsis.
Nov. tj, tee:. Publi$*^ j:nu::v lee4' originallv
il;p;;;;

iOi'- A+T. L:st prcviouseditionD 2269 88'

ofASTM Standards,Vol 05'01ifASTM


'Uni,"a Standards'Vol 14'01'
States Pharmacopeial Convention, Inc'' 12601
t"
MD 20852. Library of congress Catalog card
io"ttiire,
fr"v,

5. Significance and Use


oils is
5.1 The ultrzwiolet absorptiorl of white mineral
and
drug'
food'
in
use
for
oseJto aetermi"" tha.toit"Uility
aPPlications.
cosmetic
--i.i
fn"'O-S- Pharmacopeiaandlhe National Formulary
ntt -ioltuf oil require the measwement of
,pJanotio*
ultraviolet absorption.

I nm or less.
testing spectrophotometers
Norr I -For recomminded methcds of.
E 275'
to L-ot"A in this test method refer to Praaicc

path lengthsof 1'00


6.2 Fused Quartz Cells, two, having
doesnot
centimetres
in
* O.OOS
cm, & better' The dist:'nce

743

(fl}lo zzss
include the ihicknes of the cell in vrhich the sample is
contained.
6.3 Separatory Funnels, giass-stoppered, 125-mL capacity, equipped with TFE fluorocarborr stopcocks or other
iuitable stopcocks that will not contaminate the solvents
used.
7. Reagcntsand Materials
'
7.1 Solvents:
7.1.1 Normal Hexane-Pure grade, having an ultraviolet
light absorbanc not e>:ceeding0.02 down to 260 nm rvhen
measuredin a l-cm cell (Warning-See Note 2.) The purity
shall be such that the solvent control as defined in 8'3 shall
have an absorbance curve compared tr: water showing no
extraneous impurity perks and no absorllance exceeding that
of dimethyl sulfoxide compared to lA'aterat any wavelength
in the range 260 to 35(t nm, inclusive.
Norr 2: Warning-Normal hexane is extremely flammable'
barmfulif inhaled.May prtducenervecell dantage.
7.1.2 Spectroscopic 2.2.4-Trimetlrylltentane (Isooctane)
(Warning-See Note 3.).
NorE 3: warning-Isooctaneis extremel)rllammable,harmful if
inhaled.
Norn 4-For a suitableisooctaneand a procedurefor preparing
solventsfronr commerciallyavailablestocks,see Test
spectroscopic
MethodD 1840.
7.1.3 Dimethyl Sulfcxide-For use as spectroscopicsolvent (Note 5) (Warning-See Note 6.) Pure grade, clear,
water white, 99.9 Vodimethyl sulfoxide, tn.p. I8.5'C, with an
absorbance curve coml)ared to water not exceeding 1.0 at
264 nm and showing rro extraneous impurity peaks in the
wavelength range up to 350 nm when lneasured through a
path lenglh of I cm.
Nore 5-This solventcan be purified by percolationthrough a
1.2-mcolumnof typeCAL 1.68by 0.420mm (l2 by 40 mesh)activated
The cotumnis !.5 mm in diameter'drawn to 6.4 mm in
charcoal.5
diameterat thebonomandhasa reservoirat thc top for containingthe
liquid.Glasswoolis placedin the bottomof ttrecolumn,and about 13
mm of 0.707to 0.074(25t(, 200mesh)or 0.0149to 0.074(100to 200
mesh)silicagelis placedon top of it. The colunrnis filled with activated
solvent poured into the rescrvoirand
charcoaland thp spectroscopic
allowedto percolatcthrougt tbe charcoalat atnrosphericpressurc'The
purified sotventis collectedat the bottom ol'the column and storcdiD
glass-stoppred.bottles
as it is very hygroscopicand reactswith some
mctal containersin the prescnceof air.
Nore 6: \l'arning-Dimethyl sulfoxide is rnrnbustible.Also it is
tbrougbskin.SeeAnnexA1.3)'
rapidlyabsorbed
99 * o/o.
7.2 N aphthalene-hrfi-puity,
7.3 Standard Reference Solution-A solution containing
7.0 mg of naphthalene pr litre of purified lsooctane.
absorbance
7.4 Standard Reference Spectrogram-The
solution
reference
the
standard
scanuing
curve obtained by
in the range from 260 to 350 nm against lsooctane of the
same spectral purity as that used to prepare the standard.

(6.21
at
Absorbance-Theabsorbance
7.5 StandardReference
(6.2)
spectrogam.
reference
275nm of the standard
5 Availablc from Pitsburgh Cokc and Chcmical Gr''
PittsburSi, PA.

1970 Grant Bldg.,

Nore 7-This

absorbancewill be approximatcly

8. Procedure
8.1 Transfer 25 mL of the mineral oil
hexane to a separatoryfunnel and mirdimethyl sulfoxideand shakethe mixturt v{
least I min. Allow to standuntil the lo\rer
8.2 Transferthe lower laYerto a
mL of hexane and shake the mixture vi

standuntil the lower layeris clear.Draw off


designated as mineral oil extract, into a I
8.3 Add 5.0 mL of dimethyl sulfoxidctct
in a separatory funnel. Shake vigorously fnr

and allow to standuntil the lowerlayeris


layer, designated as solvent control, inta a
8.4 Determine the absorbance of the
compared to the solvent control throug!

'',i,

350 nm ihclusive.
9. Correctionfor Inhibitor Content6
dt&
9.1 A correctionfor the absorbance
if
a
below
as
described
be made
same inhibitor containedin the samdc
sample are available to prepare a blend"
additional inhibitor to be added to th8
should be equal to the conccntration
inhibited sample.
Nore 8-The inhibitorcontentis usually

thousand barrels. Pound per thousand barrck x


litre. For example,3 lb/1000 banels x 0.002S5'*

9.2 Weigh a minimum of 50 mg


volumetricflask,hll to volumewith i
mix thoroughly. Make furthcr diluti

to obtain thc
sample,as necessary,
addedinhibitor.
9:3 Run the originalinhibitedsamplc
Test Method D 2269and label it Run &llli
9.4 Run the blend containingknqw,
inhibitor in accordancewith Tcst
it Run B.
9.5 Calculate the difference rn

and Run A at correspondingspectratr


M:

Ao- Ao

where:
at a
M :difference in absorbance
,4a = absorbanceof Run B at the
and
lo = absorbanceof Run A at the
9.5.1 Conect the absorbanceat
follows:
A": Ao- 5'4

where:
: c;onected absorbanceat each I
A"-9.6
Mark the points of inflection
Run A at wavelengths lower and
were increased.

6 Clorrcction lbr inhibitor con(cn( llils llul *tr*

(fi1[
ozzes
11. Precisionand Bias
ll.l The precision of this test method as obtained by
stadJcar examination of interlaboratory test results is as
the absorbanca,Aa,along the baselineat each
'AaandA.ateacbposition.Ifl"islessthan . follows:
lt'l'l Repeatabilitlt-Thedifferencehtween su@essrve
rue samg operator with the sapg
ur the
irUta;neaby
results (JuBu'us{r
-r^-e ^d.L^ ^i;-;r
test rssurls
rEst
rtedthat the inhibitor content of the origindl'
operating conditions on identical
constant
;;;*
Pgder
than the amount added.
would in the long-run'.in-the "o"P"I119
iff -"i*"t,
,,!-L---r- :- -^^.^- .^
a baselinetangentto the curve connectingthe

,{awhicheveris-greater,-toilftfr-'-oJi"ti.'n
theabsorbaneA"or
of the test meihod, exceed0.014
,thesolventcontrolthroughtherange260to 3)U absorbance
unitsonlyin onecasein twenty.

the differencebetweenthe absorbanceof the


r-^r ar
wavelength
the.'-.,arana+h
at .La
thesolventcontrol

extractand

I l.
single
tolT r
rial,
opera
only in-oqg casein twenty'
ti.t3 tnese preqisiondatawereobtainedon absorbances

t" iiJ#j;rh

ili"i

zi

" rri0 ;-.

I1.2 Ar.as_this procecurehas no bias becausethe value


'ofabsorbancecanuaenneaonlyintermsofatestmethod.

culationscan be found in U.S, Pharmacopcia(USP


FormularyNF XVII).'

12' KeYwords

mineral oil
12.1 ultraviolet spectroscopy,rvhite

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