ASTM E2686-09
(Test Method)Standard Test Method for Volatile Organic Compound (VOC) Solvents Absorbed/Adsorbed By Simulated Soil Impacted by Pesticide Emulsifiable Concentrate (EC) Applications
Standard Test Method for Volatile Organic Compound (VOC) Solvents Absorbed/Adsorbed By Simulated Soil Impacted by Pesticide Emulsifiable Concentrate (EC) Applications
SIGNIFICANCE AND USE
This test method is designed specifically for emulsions of pesticide emulsifiable concentrates.
This test method provides information on the absorption/adsorption of solvents by simulated organic soil and inorganic soil impacted by pesticide EC emulsion applications.
The amount of solvent lost by volatilization at 40ºC as determined by this method is an indirect measure of the atmospheric availability of the solvent to potentially react with nitrogen oxides to form tropospheric ozone, a major air pollutant.
SCOPE
1.1 This test method simulates the application of an emulsion of a pesticide emulsifiable concentrate (EC) to soil with high organic matter (corn cob granules) and to soil with high inorganic matter (clay granules) and determines the amount of solvent retained by the granules, and withheld from the atmosphere, before and after exposure to 40ºC in a vented oven. The granules simulate two extremes of soil composition, and the 40ºC exposure simulates high temperature weathering. Solvent loss from organic substrates other than corn cob may also be determined by repeating the 40°C exposure tests with the chosen substrate replacing corn cob. The results with corn cob, however, are a reference that must be reported with the alternate substrate results. The difference in solvent content of the granules before and after weathering is an indication of the emission of the solvent from soil impacted by emulsions or solutions during pesticide applications using common practices such as spraying and drip irrigating. Analysis of the granules for solvent content is by high pressure liquid chromatography (HPLC), gas chromatography (GC), or other methods tested and proven to be accurate and reproducible.
Note 1—Since it evaluates soil surface sorption, this test method will underestimate soil sorption from pesticide applications made below the soil surface. Sub-soil surface treatments may include, but are not limited to, mechanical soil injection and soil incorporation applications. In these cases, the increased depth of the sub-soil treatments reduce the soil surface exposure and facilitate increased levels of soil sorption.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
General Information
Standards Content (Sample)
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Designation:E2686 −09
StandardTest Method for
Volatile Organic Compound (VOC) Solvents Absorbed/
Adsorbed By Simulated Soil Impacted by Pesticide
Emulsifiable Concentrate (EC) Applications
This standard is issued under the fixed designation E2686; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This test method simulates the application of an emul- 2
2.1 Other Standards:
sion of a pesticide emulsifiable concentrate (EC) to soil with
40 CFR 51.100(s) Protection of Environment—
high organic matter (corn cob granules) and to soil with high
Requirements for Preparation,Adoption, and Submittal of
inorganic matter (clay granules) and determines the amount of
Implentation Plans—Definitions
solvent retained by the granules, and withheld from the
atmosphere, before and after exposure to 40ºC in a vented
3. Terminology
oven.The granules simulate two extremes of soil composition,
3.1 Definitions:
and the 40ºC exposure simulates high temperature weathering.
3.1.1 absorb, v—a process in which one material (the
Solvent loss from organic substrates other than corn cob may
absorbent) takes in, and retains, through its pores and inter-
also be determined by repeating the 40°C exposure tests with
stices the molecules of another material (the absorbate).
the chosen substrate replacing corn cob. The results with corn
cob, however, are a reference that must be reported with the
3.1.2 adsorb, v—a process in which one material (the
alternate substrate results. The difference in solvent content of
adsorbent) attracts to, and retains on, its surface the molecules
the granules before and after weathering is an indication of the
of another material (the adsorbate).
emission of the solvent from soil impacted by emulsions or
3.1.3 emulsifiable concentrate, n—asingle-phaseliquidsys-
solutionsduringpesticideapplicationsusingcommonpractices
tem having the property of forming an emulsion when mixed
such as spraying and drip irrigating. Analysis of the granules
with water.
for solvent content is by high pressure liquid chromatography
3.1.4 emulsifying agent, n—a surfactant that promotes the
(HPLC), gas chromatography (GC), or other methods tested
suspension of one liquid in another.
and proven to be accurate and reproducible.
NOTE 1—Since it evaluates soil surface sorption, this test method will
3.1.5 gas or liquid chromatography, n—a process in which
underestimate soil sorption from pesticide applications made below the
a chemical mixture carried by a mobile liquid or gas is
soil surface. Sub-soil surface treatments may include, but are not limited
separated into components as a result of different affinities of
to, mechanical soil injection and soil incorporation applications. In these
cases,theincreaseddepthofthesub-soiltreatmentsreducethesoilsurface thecomponentsfortheliquidorgasandtheadsorbingmedium
exposure and facilitate increased levels of soil sorption.
through which they pass.
1.2 The values stated in SI units are to be regarded as
3.1.6 inorganic matter, n—substances of mineral origin that
standard. No other units of measurement are included in this
are not characterized by primarily carbon-based structures.
standard.
3.1.7 organic matter, n—in soil, organic matter consists of
1.3 This standard does not purport to address all of the
plant and animal material that is in the process of decompos-
safety concerns, if any, associated with its use. It is the
ing.
responsibility of the user of this standard to establish appro-
3.1.8 tropospheric ozone, n—an air pollutant formed by the
priate safety and health practices and determine the applica-
sunlightcatalyzedreactionbetweenhydrocarbonsandnitrogen
bility of regulatory limitations prior to use.
oxides present in the troposphere, the layer of the atmosphere
closest to the earth’s surface.
This test method is under the jurisdiction of ASTM Committee E35 on
Pesticides and Alternative Control Agents and is the direct responsibility of
Subcommittee E35.22 on Pesticide Formulations and Delivery Systems. AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
Current edition approved April 1, 2009. Published June 2009. DOI: 10.1520/ 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
E2686-09. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2686−09
3.1.9 volatile organic compound (VOC), n—any compound 6.4 Oven, vented, mechanical convection, 40 6 2ºC, 2.0 ft
of carbon, excluding carbon monoxide, carbon dioxide, car- minimum inside capacity, 50 to 90 air exchanges per hour.
bonic acid, metallic carbides or carbonates, and ammonium
6.5 125-mL laboratory media bottles, glass, round, outside
carbonate, which participates in atmospheric photochemical
diameter about 55 mm, height about 123 mm, inside diameter
reactions; excluded is a list of organic compounds which have
opening about 30 mm, with screw-thread caps.An example is
been determined to have negligible photochemical reactivity
Wheaton brand, available from many laboratory supply com-
(40 CFR 51.100(s)).
panies.
3.1.10 volatilize, v—to pass off as vapor; to evaporate.
6.6 Apparatus required by the analytical test method.
4. Summary of Test Method
7. Reagents and Materials
4.1 A pesticide EC (emulsifiable concentrate) is simulated
7.1 Corn cob granules, 20/40 Mesh
with a concentrate consisting only of solvent plus emulsifying
agent(s). The concentrate is then mixed with water, and the 7.2 Montmorillonite clay granules, LVM, 12/24 Mesh.
emulsion is applied to corn cob granules (organic substrate)
7.3 Solvent to be tested.
andmontmorilloniteclaygranules(inorganicsubstrate),which
7.4 Emulsifying agent(s) suitable for emulsifying the sol-
absorb/adsorb the liquid.
vent.
4.2 Other organic substrates, like corn stover, straw, or
7.5 Reagents and materials required by the analytical test
sphagnum peat, for example, may simulate the harvest debris
method.
from some crops better than corn cob, and the test method can
beusedwithanyofthistypesubstratereplacingcorncob.Care
8. Hazards
must be taken to select a substrate appropriate for the crop of
8.1 Before testing, read the precautionary statements on
concern,andtheresultswithcorncobareareferencethatmust
product labels and the Material Safety Data Sheets (MSDS).
be reported with the alternate substrate results. The treated
Take proper precautions to prevent skin contact and inhalation
granules are placed in a vented 40ºC oven in uncapped bottles.
of fumes or dust. Take care to prevent contamination of the
The uncapped bottles allow for loss of the solvent by volatil-
surrounding area. Always wear the appropriate safety equip-
ization. Each bottle is left in the oven for a different, and ever
ment and, where indicated, wear respiratory devices approved
increasing,timeperiod.Thetimeperiodforthefirstbottlemay
by the National Institute of Occupational Safety and Health
be as little as two hours, and that for the last bottle may be as
(NIOSH) for the product being tested.
much as one-hundred twenty hours or longer. After the 40ºC
exposure,thegranulesareanalyzedtodeterminetheamountof
8.2 Store, handle, and dispose of test materials with consid-
solvent still retained. Successive time periods continue until
eration for health and environmental safety, and in accordance
theamountofsolventfoundintwoormoresuccessivesamples
with federal, state, and local regulations.
indicates more exposure time is not expected to cause signifi-
cantly more loss of solvent.Analysis is by high pressure liquid
9. Sampling, Test Specimens, and Test Units
chromatography (HPLC), gas chromatography (GC), or other
9.1 The uniform mixing of the roller system procedure
methods tested and proven to give accurate and reproducible
ensures any size sample taken from the roller system jar is a
results.
representative sample. Do not use riffling to reduce a gross
sampleofthetreatedgranulestoarepresentative,suitablesize.
5. Significance and Use
Significant volatilization of the solvent may occur during
5.1 This test method is designed specifically for emulsions
riffling or any other time the granules are not in a sealed
of pesticide emulsifiable concentrates.
container.
5.2 This test method provides information on the
10. Preparation of Apparatus
absorption/adsorptionofsolventsbysimulatedorganicsoiland
inorganicsoilimpactedbypesticideECemulsionapplications.
10.1 For all apparatus, see the manufacturers’ instructions
for proper operation and maintenance.
5.3 The amount of solvent lost by volatilization at 40ºC as
determined by this method is an indirect measure of the
11. Calibration and Standardization
atmospheric availability of the solvent to potentially react with
nitrogen oxides to form tropospheric ozone, a major air
11.1 See the analytical test method to be used for determin-
pollutant.
ing solvent content for information relative to calibration and
adjustment of the apparatus necessary for the use of the
6. Apparatus
method.
6.1 Balance, sensitivity of 0.01 g.
11.2 See the analytical test method for the standardization
6.2 Roller System, two or more rollers with a drive bed,
and use of reference standards and blanks used in the method.
capable of rotating a glass bottle or jar, about 1 to 4 L in size,
at 20 to 60 r/min. 12. Procedure
6.3 Glass bottle or jar,round,withscrew-threadcap,foruse 12.1 Prepare an emulsifiable concentrate consisting only of
with roller system. Typical size is 1 to 4 L. solvent plus emulsifying agent(s). A typical formula is 90 to
E2686−09
92% solvent and 8 to 10% emulsifying agent(s). Check the 12.9 Use an analytical method tested and proven to give
emulsion performance by adding 1 part concentrate to 14 parts accurateandreproducibleresults.HPLCandGCmethodshave
water. Stir the mixture to form the emulsion. The emulsion been used successfully.
should form easily, remain free of separation for 15 min, and
12.10 Determinebytrialanderrorthenumberofsuccessive
re-emulsifyeasilyaftersitting24h.Iftheconcentratedoesnot
time periods needed for tracking the loss of solvent from the
meet these performance limits, reformulate using a different
granulesbyvolatilizationat40ºCtoaplateauindicatingfurther
emulsifyingagent(s).Keeptheconcentrateandtheemulsionin
loss is not expected to be significant. A minimum of five
closed containers, regardless of the ambient temperature, to
successive time periods is needed to conclude the plateau
prevent loss of solvent by volatilization. Open the containers
occurs; two of those periods must be 0 h and 72 h.Tracking is
only for the time needed to perform a necessary task.
completed when the results from any two of three successive
time periods do not differ from each other by more than the
12.2 Analyze the concentrate for weight % solvent, using
accuracy of the test method. See 15.2 for repeatability and
the same analytical method to be used for the treated granules.
reproducibility standard deviation and the 95% repeatability
Repeat the analysis. The two analyses must not differ more
and reproducibility limits on the difference between test
than 4% from each other. Use the average to calculate the
results.
makeup of the emulsion to be used for treating the granules.
In the rare event it is concluded that a plateau for loss by
12.3 Prepare one batch of emulsion treated corn cob gran-
vaporization will not be seen, the half-life for biodegradation
ules and one batch of emulsion treated clay granules as
of the solvent in soil can be used as a second tier end-point.
described below. These are the primary sampling units. Test
Stop the testing after exposure time at 40°C equals 3× the
unit samples are sub-units taken from these primary units.
biodegradation half-life.The determination of soil biodegrada-
tion half-life, itself, is beyond the scope of this test.
12.4 Keep all treated granules in closed containers, regard-
less of the ambient temperature, to prevent loss of solvent by
12.11 A suggested sequence of successive time periods at
volatilization. Open the containers only for the time needed to
40ºC for starting trial and error tests is: 0 h, 8 h, 24 h, 48 h, 72
perform a necessary task.
h, 96 h, and 120 h.
12.5 Typically,thedesiredweight%solventingranulesfor
12.12 A suggested testing protocol is as follows: Prepare
analysis by HPLC or GC is about 1%%.Asuggested protocol threesetsofseven125-mLmediabottlescontainingthetreated
for the preparation of granules with 1% solvent is as follows:
granules. Trial and error results may reduce or increase the
Prepare a concentrate of 90% solvent plus 10% surfactant(s). number of samples actually needed.
Add 1.1 parts concentrate to 14 parts water.Add the resulting
12.13 Weigh the empty bottle and cap to the nearest 0.01 g.
emulsion to 85 parts granules and mix to uniformity. Deter-
Add a test unit (nominal weight) of granules to the bottle.
mine the initial solvent content of the granules by extracting a
Typically,thenominalweightofgranulesforHPLCanalysisis
sample with a suitable analytical solvent followed by analysis
5 g, and the nominal weight for GC analysis is 5 to 20 g. Use
of the extract. The weight of the sample, or test unit, for 40°C
the nominal weight specified by the analytical method for all
exposure and subsequent analysis is the weight determined to
40ºC exposures and solvent extractions.
be nominal for the analytical method.
12.14 Weigh the bottle and granules and cap to the nearest
12.6 Begin preparation of the two batches of treated gran-
0.01 g. Determine the exact weight of the granules to the
ulesbyaddinguntreatedgranulestotheglassbottleorjartobe
nearest 0.01 g.
rotatedontherollersystem.Thegranulesshouldfillone-fourth
12.15 Foreachsetofsevenbottles,labelbottle#1forWt%
to one-half the container for the best mixing by rotation to
Solvent after0h@ 40ºC, label bottle #2, #3, #4, #5, #6, and
occur.
#7forWt%Solventafter8,24,48,72,96,and120h@40ºC,
12.7 Add the emulsion to the granules in three equal
respectively.
increments using enough total emulsion to give good distribu-
12.16 For each set of seven bottles, remove the caps from
tionoftheliquidbutnotenoughtowetthegranulestothepoint
bottles #2 through #7 and place the uncapped bottles in the
of significantly changing their flow properties. Use a transfer
40ºC oven for the specified time periods. Remove each bottle
pipette to add the emulsion to the inside wall of the container
from the oven at the end of its time period and promp
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