&EPA
United States
Environmental Protection
Agency
Office of Chemical Safety
and Pollution Prevention  , '' ^:"'D
(7101)       January 2012
        Ecological Effects
        Test Guidelines

        OCSPP 850.3200:
        Soil Microbial
        Community Toxicity
        Test

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                                     NOTICE

     This guideline is one of a series of test guidelines established by the United States
Environmental Protection Agency's Office of Chemical Safety and Pollution Prevention
(OCSPP) for use in testing pesticides and chemical substances to develop data for
submission to the Agency under the Toxic Substances Control Act (TSCA) (15 U.S.C. 2601,
et seq.), the Federal Insecticide, Fungicide and Rodenticide Act (FIFRA) (7 U.S.C. 136, et
seq.), and section 408 of the Federal Food, Drug and Cosmetic (FFDCA) (21 U.S.C. 346a).
Prior to April 22, 2010, OCSPP was known as the Office of Prevention, Pesticides and Toxic
Substances (OPPTS). To distinguish these guidelines from guidelines issued by other
organizations, the numbering convention adopted in 1994 specifically included OPPTS as
part of the guideline's  number.  Any test guidelines developed after April 22, 2010 will use
the new acronym (OCSPP)  in their title.

     The OCSPP harmonized test guidelines serve as a compendium of accepted scientific
methodologies and protocols that are intended to provide data to inform regulatory decisions
under TSCA, FIFRA, and/or FFDCA. This document provides guidance for conducting the
test, and is also  used  by EPA, the public, and the companies that are subject to data
submission requirements under TSCA, FIFRA, and/or the FFDCA.  As a guidance
document, these guidelines are not binding on either EPA or any outside parties, and the
EPA may depart from  the guidelines where circumstances warrant and without prior notice.
At places in this  guidance, the Agency uses the word "should."  In this guidance, the use of
"should" with regard to an action means that the action is recommended rather than
mandatory. The procedures contained in this guideline are strongly recommended for
generating the data that are the subject of the guideline,  but EPA recognizes that departures
may be appropriate in specific situations. You may propose alternatives to the
recommendations described in these guidelines, and the Agency will assess them for
appropriateness on a  case-by-case basis.

     For additional information about these test guidelines and to access these guidelines
electronically, please go to http://www.epa.gov/ocspp and select "Test Methods &
Guidelines" on the left side navigation menu.  You may also access the guidelines in
http://www.requlations.qov grouped by Series under Docket ID #s: EPA-HQ-OPPT-2009-
0150 through EPA-HQ-OPPT-2009-0159, and EPA-HQ-OPPT-2009-0576.

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OCSPP 850.3200: Soil microbial community toxicity test.

(a) Scope—
       (1) Applicability. This guideline is intended to be used to help develop data to submit to
       EPA under the Toxic Substances Control Act (TSCA)  (15 U.S.C. 2601,  et seq.), the
       Federal Insecticide, Fungicide, and Rodenticide Act (FIFRA) (7 U.S.C. 136, et seq.), and
       the Federal Food, Drug, and Cosmetic Act (FFDCA) (21 U.S.C. 346a).
       (2) Background.  The source material used in developing this harmonized OCSPP test
       guideline is the OPPT guideline under 40 CFR 797.3700 Soil Microbial Community
       Toxicity Test.  This guideline was formerly Public Draft OCSPP 850.5100 (April, 1996).

(b) Purpose. This guideline is intended for use in developing data on the toxicity of chemical
substances and mixtures ("test chemicals" or "test substances") subject to environmental effects
test regulations.  The guideline prescribes a test using natural soil samples to develop data on the
toxicity of test substances to microbial  populations indigenous to the soil.  The Environmental
Protection Agency will use data from these tests to assess the hazard a test substance may present
in the environment.

(c) Definitions.  The definitions in OCSPP 850.3000  apply to this guideline. The more specific
definitions in this paragraph also apply:

       Ammonification is conversion of organic  nitrogen compounds to ammonia (NHa) or to
       ammonium ion (NH/i) compounds, performed by a variety of microorganisms in soil and
       water.

       Carbon dioxide (CO2) efflux is the evolution of CO2 gas  from substrates mineralized by
       microbial action, indicative of respiration.

       kiloPascal (kPa) is a unit of pressure in the meter-kilogram-second system equivalent to
       one newton per square meter (i.e., 1 Pa x 1,000) used as a measure of water availability in
       soils.

       Mineralization is  the complete  or ultimate degradation  by microorganisms of organic
       material  to  form inorganic end-products,   e.g.,  carbon  dioxide,  water,  chloride,
       ammonium, nitrates, or orthophosphate.

       Nitrification  is the oxidation  of ammonium salts  to nitrites (NO2) and nitrates  (NOs),
       performed by relatively specialized microorganisms.

       Surface soil is that layer of soil representing the top 15 centimeters (cm) of the area to be
       sampled,  excluding the litter horizon.

(d) General considerations—

       (1) Summary  of  the test.  Surface soil is sieved and supplemented with ground, dry
       alfalfa. The test substance, if soluble, is added as a solution to moisten the soil,  or is
       added in  a manner that best simulates its anticipated mode of entry in nature.  All soil
       samples are then incubated in darkness at approximately 22  degrees Celsius (°C).  On

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       days 5 and 28 after introduction of the test substance, samples are analyzed for NHs and
       NOs content to establish ammonification and nitrification values, respectively,  and for
       CC>2 efflux as an indication of microbial respiration.

       (2)  General test guidance.  The general guidance in OCSPP 850.3000 applies to this
       guideline except as specifically noted herein.

       (3)  Range-finding  test.  A range-finding  test  is usually conducted  to  establish if
       definitive testing is necessary and, if so, the concentrations of test substance to be used in
       the  definitive test.   If the maximum concentration of test  substance to which  the soil
       microbial  community is likely to be exposed in  nature can be predicted, soil  samples
       should be treated  with concentrations that  are 0.1,  1,  and 10  times  the  anticipated
       environmental exposure concentration.   Should  reasonable predictions  of  anticipated
       environmental exposure concentrations not be possible, soil samples should be  exposed
       to a series of widely spaced  concentrations of the test  substance (e.g., 1,  10,  100, 1,000,
       10,000 micrograms (jig) test substance per gram (g) of soil).  The test should consist of
       exposing at least two samples of soil from the same source  to each concentration of test
       substance  and  to each control.   Two samples are  the minimum number used  for
       measurement of test endpoints.  The details of the test do not have to be  the same as for
       definitive testing.  Treatment replication is not needed  and nominal concentrations of the
       chemical are acceptable. However, the range-finding test will be more useful the greater
       the  similarity between  the range-finding test and the  definitive test. Report results of
       range-finding tests  along with the results of the definitive test, if range-finding tests are
       conducted.

       (4) Definitive test.  The purpose of the definitive test is to evaluate the toxicity of the test
       substance  to  the community of microorganisms residing  in  a particular  soil  and to
       delineate the concentration-response curve and ECso (with 95 percent (95%)  confidence
       intervals) for each of three variables (CO2 evolution and NHs and NOs soil content) that
       indicate the capacity of the soil microbial community  to  decompose organic  matter and
       release plant  nutrients.   The slopes of the concentration-response curves, associated
       standard  errors, and the 95%  confidence intervals  of the  slopes should  also be
       determined.   For this  determination,  a minimum  of five concentrations of  the test
       chemical,  plus appropriate  controls,  are tested.   For  each  soil  source  tested,  the
       concentration  range should be  selected  to  define,   as  closely  as  possible,  the
       concentration-response  curve between the ECio and ECgo for each variable.  Analytical
       confirmation of the test concentrations is performed as described in OCSPP 850.3000.

(e) Test standards—

       (1)  Test substance.  The substance to be tested should be technical grade, unless the test
       is designed to test a specific  formulation, mixture, or end-use product. OCSPP 850.3000
       lists the type of information that should be known about the  test substance before testing,
       and discusses methods for preparation of test substances.

       (2) Test duration.  The test duration is 28 days after application of the test substance.

       (3)  Test organism.  No particular species of test organisms are recommended for use in
       this test due to  the emphasis placed on maintaining the natural state of the soil  samples
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and their resident populations of microorganisms. The test organisms are those that occur
naturally in the soil; no other test organisms are introduced into the system.  Within a
given test, all soil, including that of the controls is from the same source.

(4) Administration of test substance.   Depending upon the properties  of the  test
substance,  it is  added via  a  stock  solution (aqueous or  solvent vehicle) to the soil,
adsorbed onto the soil, or directly mixed into the soil.

       (i) Preparation methods.

              (A) Reagent water should be used in making stock solutions  of a water-
              soluble test substance.  Sufficient quantities of each concentration should
              be available to minimize storage time and disposal volume.  A constant
              volume of the stock solution should be  added at the beginning of the test
              to  each soil  sample  designed to receive the test  substance.   OCSPP
              850.3000  contains additional  information on the preparation of stock
              solutions.

              (B) A test substance that is insoluble in water, but which can be suspended
              in an aqueous solution by a vehicle, should be added, with the vehicle, to
              those  soil samples designated  to receive the  test substance.  The vehicle
              should be soluble in water, nontoxic to microbial life at the concentration
              applied, and  used in  a minimal  amount to dissolve or  suspend the  test
              substance. There are no preferred vehicles; however, acetone, gum arable,
              ethanol, and others have been used extensively in testing herbicides, plant
              growth regulators, fungicides, and other chemical substances that affect
              plants. Any  such vehicle may be used for this test, providing it neither
              enhances nor inhibits  the activities of the soil microbes.  Vehicle controls
              are included in the experimental design and tested simultaneously with the
              test substance, if a vehicle is used. OCSPP  850.3000 contains additional
              information on preparation of stock solutions using vehicles.

              (C) A water-insoluble test substance for which no nontoxic, water-soluble
              vehicle is available should be dissolved  in an appropriate volatile solvent.
              The solution should be mixed with the ground  alfalfa  soil supplement,
              then placed  in  a  rotary vacuum apparatus and evaporated, leaving  a
              uniform coating of the test substance on the alfalfa.   A  portion of the
              alfalfa is then weighed; the test substance extracted with the same organic
              solvent, and then the test substance is assayed before the alfalfa is mixed
              with the soil  in  the test containers.  Solvent controls (i.e.., alfalfa treated
              only with solvent) should be included  in the experimental  design  and
              tested simultaneously with the test substance.

              (D) If the test substance is not readily soluble in  water or in another
              commonly used vehicle, and  is  known to be applied  or  transported in
              nature directly to  the soil as a previously prepared liquid or powder,  it
              should be mixed, in its liquid  or dry form, directly into the soil samples.
              To ensure equal distribution of  the  test substance throughout each  test
              sample, mix thoroughly.
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       (ii) Test concentrations.  For this  determination, a minimum of five treatment
       levels of the test chemical, plus appropriate controls, are tested.

       (iii) Soil.  To be appropriate for this guideline, a soil should possess a pH of 4 to
       8, organic matter content between 1% and 8%, a cation exchange capacity (CEC)
       greater than 7 milliequivalents per 100 grams, and consist of less than 70% sand.
       Soils  to which fertilizer or pesticide(s)  have been applied within the past  24
       months  should  be  avoided.  Soil collections should be restricted to the surface
       soil. Large objects should be removed manually, and the remaining soil allowed
       to  air-dry until sievable (approximately  12% water content), after which it is
       passed through  a 2-millimeter (mm) mesh screen. For each sample, an amount of
       soil equivalent to approximately 50 grams (g) oven-dry weight should be placed
       in  an inert container.  At least  one of these samples, considered  to provide a
       baseline measurement, should be extracted  immediately to  determine  NHs  and
       NOs content (see paragraph (d)(4) of this  guideline). Alfalfa, dried and ground to
       pass through  a  0.6-mm  mesh screen should be added (0.3 g) to each remaining
       sample and the sample  should be thoroughly mixed.  Water content of the  soil
       should be adjusted  to approximately   10  kPa by adding reagent (distilled,
       deionized or reverse  osmosis) water containing the desired concentration of test
       substance (in vehicle, if necessary).  If insoluble in both water and commonly
       used vehicles, the test substance should be mixed into the soil as a  solid and the
       appropriate amount of water added subsequently.  The test containers may be
       covered with 0.13  jim (0.5 mil) polyethylene to minimize water loss, yet permit
       gas exchange, or left open  and  watered  to  their original weight every 7 days.
       Regardless, the  test substance should be applied only during the original watering.

(5) Controls.

       (i) Every  test includes  a negative control, and  a vehicle (solvent)  control if a
       vehicle  is  used.   Controls consist of  the  same  soil,  soil supplements,  test
       conditions, and  procedures, except that no test substance is added.

       (ii) If an aqueous stock solution was used to prepare test concentrations, controls
       should receive an equal  volume of reagent water without the test substance.  If a
       vehicle was used to dissolve or suspend the test substance, a vehicle control (i.e..,
       solvent in water without the test substance) should also be included. Should the
       test substance be  a  powder that is mixed  directly into soil and  subsequently
       moistened with  distilled  water; the control should receive an equal volume of such
       water only.

(6) Number of replicates. A total  of 10 replicates of each test substance concentration,
control, and vehicle control  (if applicable) are  used.   This  provides two  sets of five
replicates, one set for the  analyses conducted 5 days after test  substance application and
one  set for the  analyses conducted 28  days  after test substance application.   The
assignment of soil containers to  test substance  concentrations should be  random.   In
addition, placement of the  containers in the incubation chamber should be randomized.

(7) Facilities, apparatus and supplies—

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       (i) Environmental chambers or  incubators.   Environmental chambers or
       incubators should  provide  adequate space and controls necessary  to  incubate
       numerous soil samples in total darkness at a constant temperature for prolonged
       periods of time.  Chambers should be designed to prevent escape of internal air
       into the external  environment other than through appropriate filtering material or
       media  to prevent  contamination  of the  external  environment  with  the test
       substance.

       (ii) Test containers.  For each test, at least 60 to 70 soil containers (two series of
       five per concentration of test substance, two series of five for the control, and two
       series of five if a vehicle control is necessary) should be used.  In addition, soil to
       be extracted immediately as the control is most easily  handled  in  an  identical
       container. All containers used in each experiment should be of equal  size and
       volume, posses the same configuration, and should be made of the same inert
       material.  Wide mouth jars (for example, glass canning, 0.5 pint or 110-millilitre
       (mL) capacity) are adequate for this purpose.  Test containers may be covered
       with polyethylene  film (0.13 micrometer (|im); 0.5 mil) to prevent water loss.
       Control containers  should be handled identically to the test containers except that
       none of the test substance is added.

       (iii) Cleaning and sterilization.

             (A) Soil containers and test solution storage containers should be cleaned
             before use.   All equipment should be washed to remove any  residues
             remaining from manufacturing or prior use. A dichromate  solution should
             not be used  for cleaning containers.

             (B) If cleaning  and rinsing of previously used soil containers has been
             thorough, the effects of any microorganisms remaining  on  the interior
             surface of the containers should be insignificant in the presence of the new
             test soil.   Sterilization should  not  be necessary,  but  is  considered an
             acceptable option.

             (C) Soil treated with the test substance and solvent control soil should be
             discarded at the end of the  experiment.  Disposal should  conform to
             applicable regulations.

(8) Environmental  conditions.  Environmental  conditions  should  be maintained as
follows:

       (i) Temperature. The temperature should be 22 °C (or that temperature  to which
       the  microorganisms are most  accustomed  in nature) and  it should  be  constant
       within ± 2°C during the test.

       (ii) Lighting and photoperiod. Total darkness should be used during incubation
       to prevent photosynthesis by algae or the growth of moss.
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(9) Observations-
       (i) Measurement of test substance.  Analytical confirmation of the concentration
       of test substance in the stock solutions and/or in the soil should be performed as
       described in OCSPP 850.3000.  Validated analytical methods are used to measure
       the amount of test substance in a sample before beginning the test, as described in
       OCSPP 850.3000.

       (ii) Environmental conditions—

             (A) Temperature.  Temperature in  the incubation chamber  should be
             monitored continuously.

             (B) Stock solution pH.  The pH of the stock solutions should be measured
             before use.

       (iii) Measures of effect—

             (A) Soil ammonia, nitrate and  nitrogen  content and carbon dioxide
             efflux. Of the soil samples prepared for each test concentration or control,
             one set  of  five  replicate  samples  should be  assayed after  5 days  of
             exposure to  the test substance  for  NHs  and NOs  content,  and  then
             discarded. A second set of  5  replicate samples should be analyzed the
             same day for CO2 evolution and then reincubated (dark, 22 °C). On day
             28  after  exposure to the test substance, all remaining  (reincubated)
             samples  should be assayed first for CO2 efflux and then again for nitrogen
             content.

             (B) Microorganisms.   On days  5 and  28 after introduction  of the test
             substance, the effects of treatment should be assessed  as the CO2 efflux
             rate and  the NOs and NHs concentrations per gram of dry soil in treated
             samples, relative to untreated controls and, if applicable, vehicle controls,
             and to values in freshly sieved (pretreatment) soil.

                    (1) To measure  CO2  efflux, each test container is closed with  a
                    two-hole stopper fitted with Teflon tubes and twistcock  connectors
                    for attachment to the measurement apparatus.  The apparatus (see
                    Figure 1) should deliver a  stream of humid, CO2-free air to the test
                    system, and the effluent air should be dried, diluted,  and delivered
                    for infrared gas analysis (IRGA).  The period of incubation should
                    be adjusted to  match  the CO2  efflux rate with  the  detection
                    capability of the  IRGA,  and may vary from  1 to 77 hours. In lieu
                    of IRGA, CO2 may be trapped in a hydroxide solution and titrated,
                    or measured by  gas  chromatography.   CO2 efflux  rates are
                    expressed in terms of micrograms per gram of dry soil per hour.
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       Figure 1.—Flow Diagram for the IRGA Method of Determining CO2 Evolution from
Soil Samples
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                           (2) Accumulation of inorganic nitrogen is measured by extracting
                           each soil  sample with 80 mL of 1 normal potassium chloride (N
                           KC1) solution.  After adding KC1 and shaking each container by
                           hand to suspend the soil, sample containers should be placed on a
                           rotary  shaker at high speed for 1 hour, then shaken again by hand
                           to resuspend the soil.  Samples should be  filtered (Whatman 42
                           low-nitrate  filter  paper)  and  the  extract  (filtrate)  should  be
                           analyzed for NOs  and NHs.  EPA or ASTM methods should be
                           used  for  these analyses.   NOs  and NH4 concentrations  are
                           expressed in terms of micrograms per gram of dry soil.

(f) Treatment of results—

       (1) Data summary—

             (i)  Environmental conditions.   Temperature data should be  summarized in
             tabular form, showing the mean, standard deviation, and range of temperature
             during the test.

             (ii) Carbon dioxide efflux rates, and  soil nitrate and ammonia content. CC>2
             efflux  rates and  NOs  and NH3  concentrations  in  treated samples and from
             untreated controls, aqueous or solvent vehicle controls (if a vehicle is used), and
             from the freshly sieved,  pretreatment soil  should be summarized in tabular form
             by observation date.  Means and standard deviations should be plotted for each
             treated sample and each control.

       (2) NOEC.  The significance of differences between means may be established using
       analysis  of variance and a multiple  range test such  as Dunnett's.  These hypothesis-
       testing procedures can be used  to determine NOEC and LOEC values based upon  the
       CC>2 efflux, nitrification and ammonification.

       (3) Concentration-response curve, slope, and ECso- The ECso for each of CO2 efflux,
       nitrification and ammonification should be determined.  Appropriate statistical analyses
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       should provide a goodness-of-fit determination for the  concentration-response curves.
       Standard error and 95% confidence intervals for the calculated ECso values are to be
       included.  The slope  of the concentration-response curve, its standard error, and 95%
       confidence interval should also be reported.

       (4)  Statistical  methods.   Statistical procedures  for  modeling  continuous  data  are
       available and  should  be used.  Additional  discussion about endpoints and statistical
       procedures is found in OCSPP 850.3000.

(g) Tabular  summary of test conditions.  Table  1  lists the important conditions that should
prevail  during the  definitive test.   Meeting these test conditions will  greatly  increase  the
likelihood that the completed test will be acceptable  or valid.

       Table 1.—Summary of Test Conditions for Soil Microbial Community Toxicity Test
Test type
Test duration
Substrate
Temperature
Lighting
Test container size
Number of replicate containers per test treatment
Test treatment levels
Test substance application method
Measures of effect (Measurement endpoints)
Spiked natural soil
28 days
Soil, < 70% sand, pH of 4 - 8, organic content 1 -
8%, CEC > 7 meq/100 g; sieved to 2 mm
22 °C (constant during test within ± 2 °C)
Complete darkness at all times
Sufficient to contain 50 g soil (e.g., 0.5 pint jars)
10 (minimum)
Minimum of 5 treatment levels plus appropriate
controls
Via aqueous stock solution, vehicle stock solution,
adsorbed to the alfalfa supplement, or directly
mixed into the soil.
EC50 and NOEC/LOEC based upon CO2 efflux,
ammonification and nitrification at day 5 and 28
(h) Test validity.  This test would be considered to be unacceptable or invalid if one or more of
the conditions in Table 2 occurred. This list should not be misconstrued as limiting the reason(s)
that a test could be found unacceptable or invalid. However, except for the conditions listed in
Table 2 and in OCSPP 850.3000, it is unlikely a study will be rejected when there are slight
variations  from  guideline  environmental conditions  and study  design unless  the  control
organisms are significantly affected, the precision of the test is reduced, the power of a test to
detect differences is reduced, and/or significant biases are introduced in defining the magnitude
of effect on measurement endpoints as  compared to guideline conditions.  Before departing
significantly from this guideline, the investigator should contact the Agency to discuss the reason
for the departure and the effect the change(s) will have on test acceptability. In the test report, all
departures  from the guideline should be identified, reasons for these changes given, and their
effects on test  endpoints noted and discussed.
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       Table 2.—Test validity elements for the soil microbial community toxicity test
1. All test containers were not identical and did not contain the same amount of soil from the same
source.

2. Untreated (negative controls) and appropriate solvent controls were not included in a test.
(i) Reporting—

       (1) Background  information.   Background information  to be  supplied in the report
       consists at a minimum of those background information items listed in paragraph (j)0) of
       OCSPP 850.3000.

       (2) Guideline deviations.  Provide a statement of the guideline or protocol followed.
       Include a description of any deviations from the test guideline or  any occurrences which
       may have influenced the results of the test.

       (3) Test substance.

              (i) Identification of the test  substance: common name, IUPAC and CAS names,
              CAS number, structural  formula, source, lot or batch number,  chemical  state or
              form of the test substance,  and  its purity  (i.e. for pesticides, the identity and
              concentration of active ingredient(s)). If radiolabeled substance was used  provide
              the radio purity and location(s) of the label.

              (ii) Storage conditions of the test chemical  or test substance and stability of the
              test chemical or test  substance under storage conditions if stored prior to use.

              (iii) Methods of  preparation of the  test  substance in  the range-finding and
              definitive test: description of test chemical introduction into the test medium (e.g.,
              directly mixed,  as an aqueous or solvent stock  solution, or adsorbed onto the
              alfalfa supplement),  the mass and volume of soil and test substance used for each
              treatment, how test substance was mixed into the soil.

              (iv) For the definitive test, the number of treatments and nominal concentration at
              test initiation of the test substance per unit  dry weight of test soil when  the test
              substance is introduced as dissolved in water, solubilized with a vehicle, or coated
              on the alfalfa supplement and/or mixed directly into the soil.

              (v) Description of stock solution preparation: the name and source of the vehicle,
              the  nominal  concentration(s) of the test  substance in  the  vehicle, in  stock
              solutions, or mixtures, and the vehicle concentrations used in the treatments and
              controls, pH of test solutions applied to the soil samples.

       (4) Soil microorganisms.

              (i)  Source  of the test soil, the type of ecosystem from which it was removed, its
              chemical  and physical characteristics (mechanical  analysis), and any available
              geological information including soil type (classification).

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       (ii) Collection method, storage, and handling of test soil prior to introduction of
       test substance.

       (iii) Source of alfalfa and amount added to soil.

(5) Test system and conditions.  Description of the test system and conditions used in
the definitive test and any preliminary range-finding tests.

       (i) Description  of the  test  containers:  type, size,  volume, material,  and
       conditioning method.

       (ii) Description of incubation chamber: type and size.

       (iii) Volume and weight of soil used in each test container.

       (iv) Number of replicates per treatment level and control group(s).

       (v) Frequency and methods of adding water to soil containers during the test
       period.

       (vi)  Description  of experimental design  and/or  arrangement of equipment,
       including a diagram, if complex.

       (vii) Methods used to determine the placement of soil containers in the incubation
       chamber and  the  assignment  of  test concentrations to  containers to ensure
       randomization of exposure.

       (viii) Test duration.

       (ix) Methods and frequency of environmental monitoring  performed during the
       definitive test for temperature and humidity.

       (x) Method, type and frequency of observations made on soil  microorganisms
       during the test.

       (xi) For the definitive test, all analytical procedures and  preservation  methods
       should be described.  The accuracy of the method, method detection limit, and
       limit of quantification should be given.

(6) Results.

       (i) Environmental monitoring data results (temperature and humidity) in tabular
       form (provide raw data for measurements not made on  a continuous basis), and
       descriptive  statistics (mean, standard deviation, minimum, maximum).

       (ii) Micrograms of CC>2 evolved per gram of dry soil per hour, and micrograms of
       each of NH3 and NOs present per gram of dry soil, by soil source and treated and
       untreated samples at day 5 and 28 in tabular form (provide raw data).
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              (iii) For the definitive test, report the 5-day and 28-day ECso values, with 95%
              confidence intervals for ammonification, nitrification,  and CC>2 evolution.  The
              slopes of the  concentration-response curves,  associated standard errors, and the
              95% confidence intervals should be reported as well.

              (iv) Description of statistical method(s) used, including  software package, for
              determining ECso,  LOEC and  NOEC, values and the concentration-response
              model parameters and the basis for the choice of method.  Provide results of any
              goodness-of-fit tests and determination of minimum significant differences.

(j) References. The references in this paragraph should be consulted for additional background
material on this test guideline.

       (1) Hammons, A.S. (Ed.), 1981. Methods for ecological toxicology. A  critical review of
       laboratory  multispecies  tests.  ORNL-5708.   EPA-560/11-80-026, Office  of  Toxic
       Substances, U.S. EPA, Washington, DC and Oak Ridge National Laboratory, Oak Ridge,
       TN.
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