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‘This international standard was develop in acordane with internationally recognized principles on sandardationetablshed inthe Deon on Principe for the
Bevcopnent af international Standards, ods nd Recommendations ied fy the Word Trade Organization Techs! Barker to Trade BT) Camm,
Designation: D7066 - 04 (Reapproved 2017)
Standard Test Method for
dimer/trimer of chlorotrifluoroethylene (S-316) Recoverable
Oil and Grease and Nonpolar Material by Infrared
Determination’
‘This snd is sean he fed! designation 7065; the numer immed folowing the designation iia the year of
vial ation on the ese of eis, he year of lt revison.A umber in pretheses nde te ear fst approval. A
‘Siperscipe epsilon e) ndats an etal hung since he ast evson or eappona
1. Scope
LLL This test method covers the determination of oil and
grease and nonpolar material in water and wastewater by an
infrared (IR) determination of dimer/trimer of chlorotrifluoro-
ethylene (S-316)* extractable substances from an acidified
sample, Included in this estimation of oil and grease are any
other compounds soluble in the solvent
1.2 This test method is applicable to measurement of the
light fuel although loss of some light ends during extraction
can be expected.
1.3 This test method defines oil and grease in water and
wastewater as that which is extractable in the test method a
measured by IR absorption at 2930 cnr! or 3.4 microns,
‘Similarly, this test method defines nonpolar material in water
and wastewater as that oil and grease which is not adsorbed by
silica gel in the test method and measured by IR absorption at
2930 cm"
1.4 This test method covers the range of 5 to 100 mg/L and
‘may be extended to a lower or higher level by extraction of a
larger or smaller sample volume collected separately.
LS The values stated in ST units are to be regarded as
standard, No other units of measurement are included in this
standard,
1.6 This standard does not purport 10 address all of the
safery concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
‘mine (Guide D3856) the applicability of regulatory limitations
rior 10 use.
andi the dct responsi of Subcom D910 on Meo for Anyi for
Organic Substances in Wate
‘Cura! citon apeoved Sept, 2017. Published September 2017. Oxiinaly
DOI: 10,15200 70656-04817, - 7
2 The soe sure of spp ofthe material S-316 known othe commie this
lime is Hort Instant, Iva, CA If you ae aware af alematve supe,
nents wl ceive cart consideration at « meting ofthe esnnbe fecha
ennmite." which you may tend
1.7 This international standard was developed in accor.
dance with internationally recognized principles on standard
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
‘mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Commitee.
2, Referenced Documents
2.1 ASTM Standards:*
D1129 Terminology Relating to Water
1D1193 Specification for Reagent Water
1D3370 Practices for Sampling Water from Closed Conduits
3856 Guide for Management Systems in Laboratories
Engaged in Analysis of Water
12777 Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water
S847 Practice for Writing Quality Control Specifications
for Standard Test Methods for Water Analysis
E168 Practices for General Techniques of Infrared Quanti-
tative Analysis,
E178 Practice for Dealing With Outlying Observations
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in
‘Terminology D1129 and Practices E168.
3.2 Definitions of Terms Specific to This Standard:
‘nonpolar material, n—the oil and grease remaining in
solution after contact with silica gel and measured by this test
method.
3.2.2 oil and grease, n—the organic matter extracted from
water or wastewater and measured by this test method.
3.2.3 solvent, n—dimeritrimer of chlorotrifluoroethylene (S-
316).
is Standard, refer to
>For refrenced ASTM standard, visi the ASTM website, ww amorg, oF
‘contact ASTM Canomer Service sericea or Anal Book of ASTH
Sondant ome information retro the sands DotmentSommary p86 09
ihe ASTM wot
Ceo © ASTM earn 10 Ba Ht Dr, PO Box C70, el Corekchocen, PASE 20, a Se(fl o7066 - 04 (2017)
4, Summary of Test Method
4.1 An acidified 250-mL sample of water or wastewater is
extracted serially with three 15-mL. volumes of dimerftrimer of
chlorotrfluoroethylene (S-316). The extract is diluted to 50 mL
and a portion is examined by infrared spectroscopy (IR) for an
oil and grease measurement.* A portion of the extract is
contacted with silica gel 1o remove polar substances, thereby
producing a solution containing nonpolar material. The non-
polar material is measured by infrared spectroscopy.
5. Significance and Use
5.1 The presence and concentration of oil and grease in
domestic and industrial wastewater is of concern to the public
because of its deleterious aesthetic effect and its impact on
aquatic life.
Regulations and standards have been established that
require monitoring of oil and grease in water and wastewater
6, Interferences
6.1 Soaps, detergents, surfactants, and other materials may
form emulsions that may reduce the amount of oil and grease
extracted from a sample. This test method contains procedures
that can assist the analyst in breaking such emulsions.
6.2 Organic compounds and other materials not considered
as oil and grease on the basis of chemical structure may be
extracted and measured as oil and grease. Of those measured,
certain ones may be adsorbed by silica gel while others may
not. Those not adsorbed are measured a nonpolar material
7. Apparatus
7.1. Al glassware that will come in contact with the sample
must be rinsed with dimerftimer of ehlorovrifluoroethylene
(S316) prior to beginning this procedure.
7.2 Celi(s), quartz, 10-mm path length (lower concentra-
tions. may requite a longer pathlength), two required for
double-beam operation, one required for single-beam
operation, or built-in or drop-in cell for infrared filtometer
analyzer operation.
7.23 Filter paper, ashless, quantitative, general-purpose, 11-
em, Whatman #40 or equivalent.
74 Glass fuel
75 Glass wide mouth sample bottle, minimum 250-mL,
with serew cap having a fluoropolymer liner.
7.6 Glass graduated cylinder, 100-mL.
1.7 Infrared spectrometer, double-beam dispersive, single-
beam dispersive, Fourier transform, filtometers or other ca-
pable of making measurements at 2930 cm’
7.8 Magnetic stirrer, with small TFE-fluorocarbon stirring
bar,
7.9 Glass separatory-funnel, S00mL, with fluoropolymer
stopcock and stopper
“Consult the manafctae's operation manual for the specie instructions
rele the iniared spectrometer or atalyzer be wed
7.10 Volumetric flasks, glass, various (10, 25, 50, 100, and
200-mL),
7.1 TFE-fluorocarbon spritz bottle, one-piece wash bottle
for rinsing
7.12 Repeating pipetter, glass, 15-mL, (optional.
7.13 Volumetric pipettes, glass, various (0.50, 1.00, 5.00,
10.0 and 25.0-mL, including a 1,00 serological pipet graduated
in 0.01-mL increments and a 5.00-mL. serological pipet gradu-
ated in .I-mL inerements, or equivalent),
7.14 Benchtop shaker, (optional).
TAS Glass stirring rod, (optional).
7.16 Analytical balance.
7.17 Syringes, 50 and $00 mL.
8, Reagents,
8.1. Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, i is intended that
all reagents shall conform to the specification of the Committee
‘on Analytical Reagents of the American Chemical Society,
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
accuracy of the determination
82 Purity of Water—Unless otherwise indicated, references
to Taboratory or reagent water shall be understood to mean
reagent water conforming to Specification D1193, Type Il.
83 Isooctane (2,2,4-1rimethylpentane) 98 % minimum
purity, for use in calibration
84 Octanoic Acid 98 % minimum purity, for use in calibra-
tion,
85 Silica Gel, Anhydrous, 75-150 micrometres, Davisil
Grade 923 (Supelco 21447-7A, or equivalent). Dry at
200-250°C for 24 hour minimum and store in a desiccator or
tightly sealed container. Determine the dimer/rimer of chloro-
uifluoroethylene (S-316) soluble material content of the silica
gel by extracting 10 g of silica gel with 25 mL of dimer/trimer
of chlorotrifuoroethylene (S-316) and collect the elute in a
flask, Filter and fill a quartz cell for analysis by IR. The