EPA-600/2-77-233
November 1977
Environmental  Protection Technology Series
            FIELD  MEASUREMENT OF  DENITRIFICATION

                                    Robert S. Kerr Environmental Research Laboratory
                                              Office of Research and Development
                                             U.S. Environmental Protection Agency
                                                       Ada, Oklahoma  74820

-------
                RESEARCH REPORTING SERIES

Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology.  Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:

      1.  Environmental Health Effects Research
      2.  Environmental Protection Technology
      3.  Ecological Research
      4.  Environmental Monitoring
      5.  Socioeconomic Environmental Studies
      6.  Scientific and Technical Assessment Reports (STAR)
      7.  Interagency Energy-Environment Research and Development
      8.  "Special" Reports
      9.  Miscellaneous Reports

 This report has been assigned to the ENVIRONMENTAL PROTECTION TECH-
 NOLOGY series. This series describes research performed to develop and dem-
 onstrate instrumentation, equipment, and methodology to repair or prevent en-
 vironmental degradation from point and non-point sources of pollution. This work
 provides the new or improved technology required for the control and treatment
 of pollution sources to  meet environmental quality standards.
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia  22161.

-------
                                              EPA-600/2-77-233
                                              November 1977
      FIELD MEASUREMENT OF DENITRIFICATION
                       by

                Dennis E. Rolston
              Francis E. Broadbent
          Land, Air and Water Resources
            University of California
            Davis, California 95616
                Grant No. R804259
                 Project Officer

                Arthur G. Hornsby
            Source Management Branch
Robert S. Kerr Environmental Research Laboratory
               Ada, Oklahoma 74820
ROBERT S. KERR ENVIRONMENTAL RESEARCH LABORATORY
       OFFICE OF RESEARCH AND DEVELOPMENT
      U.S. ENVIRONMENTAL PROTECTION AGENCY
               ADA, OKLAHOMA 74820

-------
                                  DISCLAIMER

     This report has been reviewed by the Robert S. Kerr Environmental
Research Laboratory, U.S. Environmental Protection Agency, and approved for
publication.  Approval does not signify that the contents necessarily reflect
the views and policies of the U.S. Environmental Protection Agency, nor does
mention of trade, names or commercial products constitute endorsement or
recommendation for use.
                                      ii

-------
                                   FOREWORD

     The Environmental Protection Agency was established to coordinate
administration of the major Federal programs designed to protect the quality
of our environment.

     An important part of the Agency's effort involves the search for infor-
mation about environmental problems, management techniques and new technolo-
gies through which optimum use of the Nation's land and water resources can
be assured and the threat pollution poses to the welfare of the American
people can be minimized.

     EPA's Office of Research and Development conducts this search through a
nationwide network of research facilities.

     As one of these facilities, the Robert S. Kerr Environmental Research
Laboratory is responsible for the management of programs to:  (a) investigate
the nature, transport, fate and management of pollutants in groundwater;
(b) develop and demonstrate methods for treating  wastewaters with soil and
other natural systems; (c) develop and demonstrate pollution control technolo-
gies for irrigation return flows; (d) develop and demonstrate pollution
control technologies for animal production wastes; (e) develop and demonstrate
technologies to prevent, control or abate pollution from the petroleum refin-
ing and petrochemical industries; and (f) develop and demonstrate technolo-
gies to manage pollution resulting from combinations of industrial wastewaters
or industrial/municipal wastewaters.

     This report contributes to the knowledge essential if the EPA is to meet
the requirements of environmental laws that it establish and enforce pollu-
tion control standards which are reasonable, cost effective and provide
adequate protection for the American public.
                                      William C. Galegar
                                      Director
                                      Robert S. Kerr Environmental
                                        Research Laboratory
                                      iii

-------
                                  ABSTRACT

     The amount of NO- in irrigation return flow waters is dependent upon
each of the components of the N cycle in soils.  One of those components for
which absolute amounts and rates are not well known is denitrification.
Volatile denitrification products, primarily NJD and N», are evolved whenever
anoxic sites develop within the soil and when sufficient carbon is available.
Absolute amounts and rates of denitrification from a Yolo loam field profile
at Davis, California, were studied in relation to the influence of soil-water
content, organic carbon source, and soil temperature.  Field plots were inten-
sely instrumented with soil atmosphere samplers, soil solution samplers, and
tensiometers.  Soil-water pressure heads (h) in the upper 15 cm of soil were
maintained constant at -15 and -70 cm of water and at -8 and -50 cm of water
for the soil temperature treatments (5 cm depth) of 23 and 8°C, respectively.
Plots cropped with ryegrass, uncropped plots, and plots to which manure was
mixed in the top 10 cm of soil were used to establish three different carbon
levels.  Fertilizer was applied at the rate of 300 kg N ha~  as KNO, enriched
with 20 and 40% 15N for the h = -15 or -8 and h = -70 or -50 cm treatments,
respectively.  The flux of volatile gases at the soil surface was measured
from the accumulation of N«0 and •'•%- beneath an air-tight cover placed over
the soil surface for 1 or 2 hours per day and from measured soil gaseous dif-
fusion coefficients and concentration gradients.  Denitrification from gas
fluxes occurred for the high-temperature experiment in order of decreasing
magnitude in manure (h = -15 cm), manure (h = -70 cm), cropped (h = -15 cm),
cropped (h = -70 cm), uncropped (h = -15 cm), and uncropped (h = -70 cm)
plots.  Approximately 70% of the fertilizer N was denitrified for the manure
(h = -15 cm) treatment.  Approximately 1% of the added fertilizer was deni-
trified in the uncropped (h = -70 cm)  treatment.  Denitrification from gas
fluxes for the low-temperature experiment occurred in the same order as that
of the high-temperature experiment except that the rate and absolute magni-
tude were much smaller.  Approximately 11% of the fertilizer N was denitri-
fied for the manure (h = -8 cm), and no measureable denitrification occurred
in the uncropped (h = -50 cm)  treatment.  The amount of N_ produced was much
greater than N»0.  The N-0 flux at the soil surface varied between 5 and 26%
of total denitrification.

     Denitrification measured from gas fluxes compared reasonably with that
determined by difference of all other components of the N cycle for the
wettest water treatments.   For the drier treatments, denitrification measured
directly was smaller than that determined by difference due to the inability
to measure very small fluxes of   N« over relatively long time periods,
inability to continuously monitor gas fluxes, and uncertainty in measuring
denitrification by difference.  Determining denitrification by difference
was highly uncertain due primarily to variability of the water flux and NO.,
concentrations within the soil.
                                      iv

-------
     Since nearly all denitrification occurred in the upper 30-60 cm of soil,
the amount of N07 leaching below the root zone was strongly dependent upon
the soil-water treatment and the amount of carbon for denitrification.  Nit-
rate was completely leached from the 180 cm profile after approximately 7
months in the h = -15 and -8 cm treatments, whereas nearly all NO^ remained
in the upper 60 cm of soil for the h = -70 and -50 cm treatments.

     The proportion of volatile products and rates of denitrification as
influenced by field-soil environmental conditions can only be ascertained by
measuring the flux of the gases produced.  A thorough, quantitative evaluation
of the rate and magnitude of denitrification, leaching, and plant uptake
provides a means for making management decisions to control irrigation return
flow water quality.

     This report was submitted in fulfillment of Grant No. R-804259 by
University of California, Davis, under the sponsorship of the U.S. Environ-
mental Protection Agency.  This report covers a period from December 1, 1975,
to July 31, 1977, and work was completed as  of August  8, 1977.

-------
                                   CONTENTS

Foreword	ill
Abstract	iv
Figures	viii
Tables	xi
Abbreviations and Symbols 	 xiii
Acknowledgments	xv

   1.  Introduction	1
   2.  Conclusions	3
   3.  Recommendations	6
   4.  Experimental Procedures	8
            Field installation	8
            Experimental procedures - field 	 13
            Analytical techniques 	 16
   5.  Results and Discussion	18
            High-temperature experiment 	 18
               Plot characteristics	18
               Soil gases	22
               Gas fluxes	28
               Plant uptake	37
               Leaching	38
               Residual soil N	40
               Mass balance	43
            Low-temperature experiment	45
               Plot characteristics	45
               Soil gases	51
               Gas fluxes	56
               Plant uptake	63
               Leaching	65
               Residual soil N	68
               Mass balance	69

References	72
Publications	74
                                     vii

-------
                                   FIGURES

Number                                                                   Page

  1   Schematic of plot layout and treatments	8

  2   Bulk density as a function of soil depth for experimental area. . . 10

  3   Organic carbon as a function of soil depth for the uncropped and
        manure plots of the  summer and winter experiments	11

  4   Soil-water content as  a function of the soil-water pressure
        head for surface soil within plots	12

  5   Soil-water content as  a function of soil-water pressure head for
        several soil depths	13

  6   Mean soil temperature  of two probes at the 5-cm soil depth of
        six plots as a function of time after fertilizer was applied
        to the plots of the  summer experiment.  The arrows give the
        fertilizer application for each plot with the symbols given
        in Table 2	18

  7   Mean soil-water pressure head of three tensiometers in each
        plot at the 5- and 15-cm soil depth  as a function of time
        after fertilizer application to the  two water treatments of
        the summer experiment.  The arrows give the fertilizer
        application for each plot with the symbols given in Table 2  ... 19

  8   Mean soil-water pressure head as a function of soil depth for
        the three plots of each water treatment of the summer
        experiment	20

  9   Mean soil-water content as a function  of soil depth for the
        three plots of each  water treatment  of the summer
        experiment	21

 10   Mean soil-air content  as a function of soil depth for the
        three plots of each  water treatment  of the summer
        experiment	.....22

 11   Oxygen concentration as a function of  soil depth in the plots
        of the summer experiment.  Symbols are given in Table 2	23

 12   Nitrous oxide concentration with depth on one day in the
        h = -15 cm treatment of the summer experiment	25

                                    viii

-------
Number                                                                  Page

13   Nitrous oxide concentration with depth on one day in the
       h = -70 cm treatment of the summer experiment	26

14   Concentration of   ^ with depth on one day in the h = -15 cm
       treatment of the summer experiment	27

15   Concentration of   N£ with depth on one day in the h = -70 cm
       treatment of the summer experiment  	 28

16   Flux of N20 calculated from measurements beneath cover with
       time for the manure and cropped plots of the summer
       experiment	29

17   Flux of N£O calculated from measurements beneath cover with
       time for the uncropped plots of the summer experiment	30

18   Flux of   N£ calculated from measurements beneath cover with
       time for the manure and cropped plots of the summer experiment. . 31

19   Flux of   N2 calculated from measurements beneath cover with
       time for the uncropped plots of the summer experiment	32

20   Plant uptake of fertilizer N with time of the summer experiment . . 38

21   Concentration of fertilizer derived NO, in the soil solution as
       a function of soil depth for the h = -15 cm treatments of the
       summer experiment 	 39

22   Soil extractable N from fertilizer as a function of soil depth,
       5.5 months after fertilizer application, of the summer
       experiment	42

23   Soil digestible N from fertilizer as a function of soil depth,
       5.5 months after fertilizer application of the summer
       experiment	43

24   Mean soil temperature at the 5-cm soil depth as a function of
       time after fertilizer was applied to the plots of the winter
       experiment.  The arrows give the fertilizer application for
       each plot with the symbols given in Table 2	46

25   Mean soil-water pressure head at the 5- and 15-cm soil depth as
       a function of time after fertilizer application to the two
       water treatments of the winter experiment.  The arrows give
       the fertilizer application for each plot	47

26   Mean soil-water pressure head as a function of soil depth for
       the two water treatments of the winter experiment	48
                                     ix

-------
Number                                                                  Page

27   Mean soil-water content as a function of soil depth for the
       two water treatments of the winter experiment .......... 49

28   Mean soil-air content as a function of soil depth for the two
       water  treatments of the winter experiment ............ 50

29   Oxygen concentration as a function of soil depth in the plots
       of the winter experiment.  The symbols are given in Table 2 ... 51

30   Nitrous  oxide concentration with depth on one day in the
       h = -8 cm treatment of the winter experiment  .......... 53

31   Nitrous  oxide concentration with depth on one day in the
       h = -50  cm treatment of the winter experiment .......... 54

32   Concentration of  -"N^ with depth on one day in the h = -8 cm
       treatment of  the winter experiment   ........... ....55

33   Concentration of   N? with depth on one day in the h = -50 cm
       treatment of  the winter experiment   ............... 56

34   Flux of  N£0 calculated from measurements beneath a cover with
       time  for the  manure and cropped plots of the winter
       experiment   ........................... 57
 35   Flux of N£0 calculated from measurements  beneath  a  cover with
        time for the uncropped plots of the winter  experiment  ...... 58

 36   Flux of   N2 calculated from measurements beneath a cover with
        time for the manure and cropped plots of the winter  experiment.  . 59

 37   Plant uptake of fertilizer N with time during the winter experiment 64

 38   Concentration of fertilizer derived NO- in the soil solution as
        a function of soil depth for the h = -8 cm  treatments of  the
        winter experiment ........................ 65

 39   Soil extractable N from fertilizer as a function  of soil depth,
        4 months after fertilizer application in the winter  experiment.  . 68

 40   Soil digestible N from fertilizer as a function of  soil depth,
        4 months after fertilizer application in the winter  experiment.  . 69

-------
                                   TABLES

Number                                                                   Page

  1   Texture With Soil Depth	10

  2   Fertilizer Application and  % Enrichment of Each Treatment .... 14

  3   Concentration  (ppmv) of N20 Within Profiles Before Application
        of Fertilizer of the Summer Experiment.  Ambient Concentration
        of N20 in Air is Approximately 0.30 ppm	24

  4   Denitrification as N20, N2, and Total for the Summer Experiment
        as Determined From Measurements Beneath a Cover Placed Over
        the Soil	33

  5   Ratios of N2 to N20 Produced from Denitrification in the Plots
        of the Summer Experiment from Measurements Beneath a Cover
        Placed Over  the Soil	34

  6   Soil Gaseous Diffusion Coefficients Determined by the C02 Flux
        Method for the Summer Experiment  	 35

  7   Soil Gaseous Diffusion Coefficients Determined by the Transient-
        State Method for the Summer Experiment	36

  8   Percentage Recovery of Fertilizer N Leached in the h = -15 cm
        Plots of the Summer Experiment Calculated by Various Ways of
        Determining  the Soil-Water Velocity, vs.  The Mean Recovery
        of all Depths for Each Plot is Given in Parentheses	41

  9   Mass Balance of Fertilizer N for the Summer Experiment	44

 10   Concentration  of N20 (ppmv) Within Profiles Before Application
        of Fertilizer of the Winter Experiment.  Ambient Concentration
        of N20 in Air is Approximately 0.30 ppmv	52

 11   Denitrification as N20, N-, and Total for the Winter Experiment
      .  as Determined from Measurements Beneath a Cover Placed Over
        the Soil	60

 12   Ratios of N2 to N20 Produced from Denitrification in the Plots
        of the Winter Experiment from Measurements Beneath a Cover
        Placed Over  the Soil	61

 13   Soil-Gas Diffusion Coefficients for the Winter Experiment  	 62

                                     xi

-------
Number                                                                   Page

 14   Percentage Recovery of Fertilizer N Leached in the h = -8 cm
        Plots of the Winter Experiment Calculated by Various Ways
        of Determining the Soil-Water Velocity.  The Mean Recovery
        of all Depths for Each Plot is Given in Parentheses	67

 15   Mass Balance of Fertilizer N for the Winter Experiment.  The
        Numbers in Parentheses Were Obtained by Calculating Leaching
        from Concentration Versus Soil Depth.  The Minus Sign
        Indicates Greater Recovery Than Fertilizer Applied  	 70
                                     xii

-------
                      LIST OF ABBREVIATIONS AND SYMBOLS
ABBREVIATIONS
cm
m
ml
°C
kg ha
mg
ppm
ppmv
cm^
g
Ug
-1
— centimeter
— meter
— milliliter
— degrees Centigrade
— kilograms (10^ grams) per hectare
— milligram (10   grams)
— parts per million on a weight basis
— parts per million on a volume basis
— cubic centimeters
— gram
— micro grams (10~  grams)
SYMBOLS
N
NH+
NO-
NO"
NH3
N20
N2
15N
C02
02
f
DP
c
x
h
        Nitrogen
        Ammonium
        Nitrite
        Nitrate
        Ammonia
        Nitrous Oxide gas
        Nitrogen gas
        Nitrogen isotope of mass 15
        Carbon dioxide gas
        Oxygen gas
        gas flux (mg cm   day~l)
        soil gaseous diffusion coefficient  (cnr day"-'-)
                                — o
        gas concentration (mg cm  )
        distance (cm)
        soil-water pressure head (cm)
                                    xiii

-------
SYMBOLS (continued)



                                   3   —3
6         — soil-water content (cm  cm  )

                                 3   —3
e         — soil-air content  (cm  cm  )


vs        — soil-water velocity (cm day  )
                                      xiv

-------
                               ACKNOWLEDGMENTS

     The authors gratefully acknowledge additional financial support for this
research from the National Science Foundation - RANN (Grant No. G134733X),
the Kearney Foundation of Soil Science, and the University of California
Agricultural Experiment Station.  The laboratories and mass spectrometer
facilities of the Department of Land, Air and Water Resources provided strong
support for this research.

     The authors gratefully acknowledge the able assistance, ingenuity, and
dedication of the three technicians primarily responsible for the establish-
ment, operation, and analytical procedures of this research, David L. Hoffman,
David A. Goldhamer, and Dianne W. Toy.  Several students including
Paul Brooks, Nora H. Monette, and Brian D. Brown assisted in analyses, and
their help is greatly appreciated..  The assistance of Tyler Nakashima and
James Burgess, in mass spectrometer maintenance is greatly appreciated.  The
use of the gas chromatograph under the control of Professor C. C. Delwiche
was indispensable and is gratefully acknowledged.
                                      xv

-------
                                  SECTION 1

                                INTRODUCTION
     The amount of N07 reaching the ground water of irrigated lands is
dependent upon each or the components of the N cycle in soils.  The amount
of fertilizer N applied and crop uptake of N are easily measured parameters
of the total balance.  The other components of the N balance, however, are
not as easily measured or determined.  The leaching component of the N balance
has been a subject of much study and is the primary concern in terms of NOo
in ground water.  The natural spatial variability of the leaching component
has been demonstrated to be large (Biggar and Nielsen, 1976).  The other
components such as residual soil N, denitrification, and NH^ volatilization
losses are also not easily measured.  The residual soil N is difficult to
measure due to the large organic N pool of most soils and complicated by the
natural spatial variability of that pool (Rolston, 1977).  The transient
processes of immobilization and mineralization within the large organic N
pool also contribute to the complexity of the measurement.  Volatilization
loss of fertilizer as NHo occurs to varying degrees in calcareous soils.
This component can generally be minimized by incorporating NH^ fertilizer
below the soil surface.  Another loss of N from the soil system for which
absolute amounts and rates are not well known is denitrification.  Volatile
denitrification products, primarily ^0 and N£, are evolved whenever anoxic
sites develop within the soil and when sufficient carbon as supplied by soil
organic matter, plant materials, and manure is available.

     Simulation models of the N balance in soil systems attempt to predict
the amount and concentration of NOT in irrigation return flow water as a
function of irrigation and cropping practices (Mehran and Tanji,  1974;
Donigian and Crawford, 1976; Shaffer et al., 1976;  Tanji  and  Gupta, 1977;  and
van Veen, 1977).  In general, the denitrification component of the various
mathematical models has not had adequate input data especially for the rates
of denitrification.  Total denitrification of applied fertilizer is used
quite frequently such as 10-15% of the fertilizer N applied (Fried et al.,
1976).

     Very few experiments have evaluated the absolute amounts and rates of
denitrification in the field.  Rolston et al. (1976) demonstrated that the
volatile gases from denitrification could be measured in a field profile.
Total denitrification from gas fluxes compared reasonably with denitrifica-
tion determined by difference for a small, intensely-instrumented, field plot.
Total denitrification was determined by integrating with time the flux of the
gaseous denitrification products as determined from measured soil gaseous
diffusion coefficients and concentration gradients.  However, these studies
only evaluated the amount of denitrification under one cropping or carbon

-------
input system and one soil-water content near saturation.

     The objectives of the research reported here were:

     a.   To measure denitrification in a field soil directly from the fluxes
          of N£ and ^0 at the soil surface.

     b.   To compare denitrification obtained from N« and ^0 gas fluxes with
          denitrification obtained by difference.

     c.   To measure the amount of denitrification from an applied inorganic
          fertilizer source as affected by an actively growing crop or manure
          amendment, soil-water content, and temperature of a field soil.
                                       o
The research was conducted on small 1-nr field plots because of the large .. _
cost of NOg fertilizer tagged with high enrichments of the stable isotope   TJ.
The use of •*--% tagged NOo is presently the only positive means of measuring
N£ gas resulting from denitrification in the field.  The experiments were
conducted at a high and low soil  temperature, at two water contents near
saturation, and at three levels of carbon input  (cropped, uncropped, and
manure).

-------
                                  SECTION 2

                                 CONCLUSIONS

     The results of this research demonstrate that denitrification can occur
at very large rates with the largest rates occurring soon after application
of N07 fertilizer to soil maintained constantly wet.  The rate of denitrifi-
cation generally decreases rapidly after the initially large rate due to a
decrease in NOT concentration and to the movement of the N03 pulse out of the
zone of high carbon content and low oxygen concentrations.  For soils in
which the profile development is such that large bulk densities occur near
the surface, denitrification is limited to the top 30 to 60 cm of the soil
profile inasmuch as that is the zone where water content is greatest, soil-
air content is smallest, and biological activity is greatest due to generally
high carbon values.  Thus, denitrification would be greatest in the surface
zone.  This is not an uncommon situation for many alluvial, irrigated soils
of the West.

     Denitrification occurs over a very narrow range of soil-water content on
Yolo loam soil.  Very little denitrification occurred in plots at which the
soil-water pressure head was maintained at -70 cm of water.  This soil-water
pressure head corresponds to a soil-air content of 9-10%.  It would be expec-
ted that for alluvial, loam soils such as Yolo, that very little denitrifica-
tion would occur if soil-water pressures were maintained smaller than
approximately -100 cm of water.

     The presence of the crop root system has a large influence on denitrifi-
cation.  For the Yolo loam soil, very little denitrification occurred even at
the water content nearest water saturation if a crop was not growing on the
soil.  The influence of the root system in providing carbon and consuming Q£
results in anoxic development and provides the carbon necessary for denitri-
fication.  As expected, the addition of manure to the soil greatly increased
denitrification over that of the cropped plots.  It would be  expected that
the addition of other organic materials such as crop residues  along with the
NOg fertilizer would also have the effect of substantially  increasing deni-
trification.  With manure added to the soil and water contents  maintained
very close to saturation, approximately 73% of the fertilizer was lost by
denitrification at 23°C.  Only 14% of the fertilizer was lost in the cropped,
wet treatment of the summer experiment.  Only 3% of the NO^ was lost for the
wet treatment of the summer- experiment without a crop growing on the soil.

     At a soil temperature of between 8 and 10°C, very little denitrification
occurred.  This was primarily due to limited microbial activity as reflected
in relatively constant Q£ concentrations with soil depth.  The largest deni-
trification loss at the low soil temperature occurred in the wet, manure
treatment with 11% of the fertilizer denitrified.  The uncropped plots lost

-------
very little NO^ at the low soil temperatures.

     The predominant gas evolved was ^ with total amounts being at least 6
times greater than that for ^0, and in some cases 20 times more N2 than N20
was produced under very anoxic conditions.  The N2 to ^0 ratios were general-
ly small (1 to 5) early in the denitrification process and then became much
larger as denitrification proceeded.

     Measurement of denitrification from the gaseous components was slightly
smaller than that measured by difference.  This failure to account for the
total amount of N apparently denitrified was most likely due to the inability
to continuously monitor gas fluxes,to very small rates of denitrification
over an extended time period after the initially large rates had decreased,
and to errors in the difference method.  The sensitivity of the instrumenta-
tion was not sufficient to measure denitrification rates less than approxi-
mately 1 kg N ha"-'- day"*- over many days or weeks.  Although denitrification
measured from gas fluxes was less than that determined by difference due
primarily to the lack of sensitivity in measuring small denitrification rates,
measuring N£ and ^0 is the only means that the rates and position of denitri-
fication in the profile can be ascertained.  The sensitivity for measuring
small gas fluxes can be increased by increasing the "N enrichment of the
added fertilizer and by increasing the time that covers are left in place at
the risk of changing the normal soil condition.

     Calculations of the denitrification gas flux from the soil gaseous dif-
fusion coefficient and gas concentration gradients measured within the soil
compared reasonably with measured fluxes of N£ and N£0 as determined by
taking gas samples from beneath the cover placed over the soil surface for
1- or 2-hour time intervals on each sampling day.  This statement is valid
only if the diffusion coefficient is measured immediately before and after
an experiment is conducted, since the values of the diffusion coefficient
were very much dependent upon surface soil conditions.  Since   No concentra-
tions within the soil were greater than those under a cover, increased sensi-
tivity should be possible if concentration gradients and diffusion coeffi-
cients can be accurately measured.

     All NO^ had been leached from the profile of the wet treatments by 7
months after application of the fertilizer.  In the dry plots, most of the
NO^ was still in the upper 60 cm of the soil profile after 5 months.  There-
fore, the amount of water applied and the soil-water velocity has an enormous
effect on the amount of N0~ leaching and the position of the NO, within the
soil profile.

     Determination of the leaching component was highly uncertain due to
errors in determining the soil-water flux and variability in Ng^ concentra-
tions.  For the low-temperature experiment, it was impossible to obtain a
mass balance inasmuch as N leaching was greater than N applied as fertilizer.
This discrepancy was attributed primarily to an overestimation of the soil-
water flux resulting from spatial variability, flux changes with time, and
anion exclusion or immobile water.  Errors are also possible in measuring the
residual soil N.  Thus, the determination of denitrification by difference is
highly uncertain.

-------
     Both cropped plots of the wet and dry treatments took up fertilizer N
at approximately the same rate until the NO^ was either denitrified or leached
from the upper part of the profile.  The rate of uptake for the wet treatments
decreased to near zero after the NO^ had been leached from the upper 60 to 90
cm of the profile, whereas uptake continued in the dry treatments where the
NOo was still in the upper portion of the profile and being taken up by the
grass.

     It would be expected that considerable fertilizer N would be immobilized
as live and dead roots in the cropped plots.  However, there was also consid-
erable immobilization of fertilizer N in the manure and uncropped plots.
This immobilization most likely occurred as microbial biomass and the roots
of a few weeds and moss which were difficult to keep from the plots.

-------
                                  SECTION 3

                               RECOMMENDATIONS

     These results demonstrate that the addition of manure with the fertilizer
greatly increased denitrification of the fertilizer NO^.  Thus, it is recom-
mended that manure not be applied with fertilizer.  Manure applications should
be timed such that the NO^ from fertilizer does not occur at the same position
within the profile as does the carbon from manure.  It also becomes important
that water management be controlled even more carefully when manure is applied
than with inorganic fertilizers in order to prevent anoxic development and
denitrification.  There is most likely some loss of N which is mineralized
from the manure added to soil due to anoxic development during periods of
high water content.  Thus, the N in manure may not be as effective as an equal
amount of N from inorganic fertilizers due to the inclusion of considerable
carbon in the manure to increase denitrification.

     Irrigation management practices directed at minimizing N loss from deni-
trification should be designed with the idea of maintaining soil-water
pressure or water content within a range that anoxic conditions will most
likely not develop for that part of the profile with the largest amount of
carbon.  For loam soil similar to Yolo, very little denitrification should
occur if soil-water pressures are maintained smaller than -100 cm (-10 centi-
bars) or tensions greater than 10 centibars.  This limit of tension would be
larger for a clay soil and smaller for a sandy soil.  The degree of soil
aggregation would also influence these limits.

     Another management recommendation which may be made is that if water
contents or pressures cannot be maintained outside the range where denitrifi-
cation will occur, it may be possible to time fertilizer application so that
NOo will not occur in the zone along with the carbon at a time when water
contents will be close to saturation.  It may be possible, for instance, to
apply NHj fertilizer immediately before a large irrigation for wetting a
profile at the beginning of the irrigation season.  The next irrigation would
be timed and managed such that the NOg would be moved out of the zone where
most of the carbon occurs, yet remain within the zone where roots could obtain
the N.  This management approach would minimize the potential for denitrifi-
cation in soils similar to the profile described in this report.
                                                               t
     Field research should be conducted to determine such factors as the rate
that microbial populations increase after irrigating an initially dry soil.
Along with the population increase, the irrigation frequency and water con-
tents maintained between irrigations should have an enormous influence on
denitrification during normal irrigation cycles.  Management decisions to
maximize fertilizer use efficiency and minimize NO^ leaching to ground water

-------
can be made only after the dynamics of microbial population growth,
leaching, and denitrification rates in field sites are ascertained.

-------
                                  SECTION  4


                           EXPERIMENTAL PROCEDURES
FIELD INSTALLATION


     Twelve, 1-m2 field plots were  established  on Yolo  loam soil  (Typic
Xerorthents) at Davis, California.  The Yolo  loam soil  is  a deep, well-
drained, alluvial soil in  the Sacramento Valley.  The soil is  a prominent
agricultural soil of  the area and is  similar  to other soils of extensive
acreage.  A schematic diagram of the  experimental location and the  treatment
layout is given in Figure  1.  Each  of the  1-m2  plots was established with  a
                      MANURE
UNCROPPED

CROPPED
                                 DRY TREATMENT
                                HIGH
                            TEMPERATURE
                            EXPERIMENT
   LOW
TEMPERATURE
EXPERIMENT
UNCROPPED

CROPPED
                                  WET TREATMENT
Figure 1.  Schematic of plot  layout  and  treatments.

-------
60-cm deep redwood barrier around the outside edges of each undisturbed block
of soil.  The redwood barriers were installed by digging a trench around the
l-m2 area, slipping the redwood over the undisturbed block of soil, and back-
filling the trench on the outside of the redwood.  The space between the
redwood barrier and the soil on the inside was sealed by pouring melted
paraffin into the small crack between the soil and the wood.  Each of the
twelve plots was instrumented with tensiometers, soil solution samplers, soil
atmosphere samplers, and thermocouples.  Five soil atmosphere samplers were
installed at the 2-, 5-, 10-, and 15-cm depths; three soil atmosphere samplers
were installed at the 20-, 30-, 60-, 90-, and 120-cm soil depths.  Triplicate
samplers, designed to function as tensiometers or solution extractors, were
installed at the 60-, 90-, 120-, 150-, and 180-cm depths of the soil profile.
Triplicate tensiometers were also installed at the 5- and 15-cm depths.  Du-
plicate thermocouples were installed at the 5-cm depth.  Soil solution sam-
plers consisted of porous cups glued to polyvinyl chloride tubing.  All of
the deeper solution samplers and gas samplers were installed on an angle begin-
ning on the outside of the 1-m^ plot with the cup or the tip of the gas sam-
pler ending up in the center of the l-m^ area of the plot.  Soil atmosphere
samplers consisted of 0.1 cm inside diameter nylon tubing glued into a 5-cm
long perforated acrylic plastic tube.  For the deeper soil depths the small
diameter nylon tubing was placed inside a 1.3-cm diameter polyvinyl chloride
tube and the nylon tubing glued into a milled plastic tip.  For all samplers,
the volume of the sampling tubes was very small.  Soil solution samples  were
obtained by evacuating bottles connected to samplers.  Soil atmosphere sam-
ples were obtained by withdrawing 1-ml increments of gas with plastic, dispos-
able syringes.  All gas samples were analyzed within a few hours after
sampling.

     Six plots were constantly maintained at a soil-water pressure head (h)
very close to water saturation and six plots were maintained drier than near
saturation but wetter than field capacity.  The soil was maintained at a
constant water content or pressure with a spray irrigation system which
consisted of spray nozzles on a traveling boom.  The system was activated by
a timer so that plots could be irrigated on as frequent an interval as neces-
sary to maintain constant soil-water content conditions.

     In order to establish different carbon treatments within each of the two
water regimes, two plots were cropped with perennial ryegrass (Lolium Perenne)
for approximately 4 months prior to the experiment.  Two plots remained un-
cropped, and manure at a rate of 3.4 x 10  kg ha    was mixed in the top 10cm
of soil of four plots approximately two weeks before fertilizer was applied.

     The two water content treatments and the three carbon treatments were
also conducted at two times of the year in order to evaluate the effect of
soil temperature on denitrification.  One experiment was conducted in July
when the average soil temperature at the 5-cm depth was approximately 23°C
during the experimental period.  Another experiment was conducted in January
when the average soil temperature at the 5-cm depth was approximately 8°C
during the experimental period.  The entire experimental area was covered
with plastic sheeting in order to prevent rain from changing the constant
soil-water content conditions while experiments were being conducted.

-------
     The particle size analysis  as a function of soil depth for the Yolo loam
soil is given in Table 1 and the average bulk density at the field site is
given as a function of depth in Figure 2.   The bulk density is greatest near

                      TABLE 1.   TEXTURE WITH SOIL DEPTH
Depth
0
15
30
60
90
120
150
- 15
- 30
- 60
- 90
- 120
- 150
- 180
Sand (%)
41
40
42
38
38
32
25
Silt (%)
37
37
38
42
42
46
51
Clay (%)
22
23
20
20
22
24

Loam
Loam
Loam
Loam
Loam
Silt Loam
Silt Loam
                               BULK DENSITY (g cm"3)
                             1.20 .     1.30        L.40
                                        o WINTER
                                          SUMMER
1.50
Figure 2.  Bulk density as a function of soil depth for  experimental area.

                                      10

-------
the soil surface with a minimum at the 120-cm depth.  Bulk density was deter-
mined on 7.6 cm long, 7.6 cm diameter undisturbed soil cores.

     The percentage of organic carbon as  a function of soil depth for the
uncropped and manure plots of the summer  and winter experiments  is given by
Figure 3.  Organic carbon was determined  on soil samples taken after experi-
  O
  UJ
  Q
  o
  c/)
  0

 20

 40

 60

 80

100

120
                          ORGANIC CARBON (%)
         0    0.2   0.4   0.6   0.8    1.0    1.2
                                                       .6   1.8
   ° Uncropped
— • Manure - Summer
   * Manure- Winter
Figure 3.   Organic carbon as a function of soil depth for the uncropped and
           manure plots of the summer and x/inter experiments.


ments were conducted, so several months had elapsed after manure application.
The soil for  organic carbon determination was ground to pass a 2mm sieve or
finer.  A subsample was then thoroughly ground with a pica mill to pass a 60
mesh sieve.   Approximately 0.2 grams of the soil sample were placed in a
crucible to which a small amount of iron and tin accelerator was added.  The
sample was covered with a single hole lid and placed into an induction furna:e.
The (X>2 produced was collected in a Nesbit tower containing ascarite.  The
tower was  weighed before and after the burn to determine the amount of carbon
dioxide trapped.  There was no difference in the % carbon between a soil
                                    11

-------
sample that had been  extracted with KC1 and a sample that had not been
extracted.

     Figures 4 and 5  gives soil-water characteristic curves (soil-water  con-
tent versus soil-water pressure) at several depths of the experimental site.
The data points are the means of at least three  7.6-cm diameter,  7.6-cm  long
undisturbed soil cores.  Figure 4 gives curves from surface cores obtained
within the l-m^ plots of the wet (South) and dry (North) water treatments
after the denitrification experiments were completed.  Figure 5 gives curves
for cores obtained at various depths outside the 1-m2 plots.
                 0.48
             •?   0.46
              E
              o
              o
             O
             O
                 0.42
                 O.4O
                 0.38
             ^ 0.36
             .J
             O
             w 0.34
                 0.32
      SURFACE CORES
                                    INSIDE SOUTH SUMMER
       INSIDE NORTH SUMMER
INSIDE
NORTH WINTER
                                 I
      I
I
I
                     0   -20   -40  -60  -80  -100  -120  -140
                    SOIL-WATER PRESSURE HEAD h (cm H20)
Figure 4.   Soil-water content as a function of the soil-water  pressure head
           for  surface soil within plots.
                                    12

-------
       0.30
            0   -20   -40   -60   -80   -100  -120  -140  -160  -180 -200
                     SOIL-WATER PRESSURE HEAD h (cm H20)
Figure 5.  Soil-water content as  a.  function of soil-water pressure head  for
           several soil depths.
EXPERIMENTAL PROCEDURES - FIELD

     After constant,  steady-state water content conditions were achieved  in
the plots, N03 solution equivalent to 300 kg N ha   was uniformly applied to
the plots by applying approximately 3 ml of solution to each of 400  points at
the soil surface.   The 15N enrichment of the added fertilizer was 20 and  40%
excess 1% for the wet and dry treatments, respectively.  The actual amounts
and enrichments applied to each plot are given in Table 2.

     Within 6 hours after applying the fertilizer solution, an airtight cover
was placed over the plots.  The cover consisted of a thick sheet of  acrylic
plastic with rubber tubing on the lower edge to make an airtight seal with
the top of the redwood border.  Samples of the atmosphere beneath the cover
were taken after one  or two hours with the lid in place and analyzed for  15N2
and 15N20.  Soil atmosphere samples from within the soil profile were also
taken soon after applying the fertilizer.  Soil atmosphere samples were taken

                                    13

-------
    TABLE 2.  FERTILIZER APPLICATION AND 15N ENRICHMENT OF EACH TREATMENT
High-Temperature
Experiment
Cropped, h
Manure, h
Uncropped,
Cropped, h
Manure, h
Uncropped ,
= -15 cm
= -15 cm
h = -15 cm
= -70 cm
= -70 cm
h = -70 cm
Plot
#
IS
2S
3S
IN
2N
3N
% 15N Excess
19.4
19.3
19.2
38.3
39.2
38.4
Fertilizer
Rate (kg N ha"1)
296.0
300.6
304.9
297.4
298.4
292.8
    Low-Temperature
      Experiment
Cropped, h
Manure, h =
Uncropped ,
Cropped, h
Manure, h =
Uncropped,
= -8 cm
-8 cm
h = -8 cm
= -50 cm
-50 cm
h = -50 cm
4S
5S
6S
4N
5N
6N
19.8
19.8
19.4
39.9
40.0
39.6
299.9
294.3
294.0
296.5
297.6
294.2
in 1-ml aliquots and N20, C02, 02, and N2 analyzed by gas chromotography in
the laboratory.  Another 0.5 to 1 ml of gas was taken to determine 15N2 with
a mass spectrometer.  All soil samples to be analyzed by mass spectrometry
were pulled through ascarite, dehydrite (magnesium perchlorate), and a com-
mercial 02 scrubber.  Gas samples from the profile and samples from beneath
the cover were taken daily for a few days after the fertilizer was applied
and then at less frequent intervals until ^^N2 and  %20 could no longer be
detected above background.

     Soil solution samples were taken at weekly intervals.  Thg grass of the
cropped plots was cut periodically, and the total clippings dried for analysis.
After the NO^ had been completely leached through the 180-cm depth of the wet
treatments, both the wet and dry plots were allowed to dry and soil samples
taken in 15-cm increments down to 120 cm.  The samples consisted of eight
separate holes taken with a Veihmeyer tube within the 1-m2 plot.  On some
plots, each of these samples was run individually.  On others, the eight
                                      14

-------
samples from each depth were combined into  two samples  at  each  depth.

     Soil gas-diffusion coefficients were determined for the plots by the CC>2
flux method.  This method measures the CC>2  trapped in a NaOH solution from an
air stream flowing over the top edge of the plot.  The C02 concentration gra-
dients within the soil were measured several times during the CC^-trapping
process.  The C02 concentration gradient and CC>2 flux were used in calculat-
ing the diffusion coefficient of CC^ from
                                f = -Dp(3C/3x)                          (1)

where f is the gas flux (mg cm   day "•'•) , D  is the soil gas-diffusion
coefficient (cm2 day"-'-) , C is the gas concentration (mg cm~3) t and x is dis-
tance (cm) .  The diffusion coefficient for ^0 is about equal to that for C02.
The diffusion coefficient for No is calculated by multiplying the diffusion
coefficient for CC>2 by 1.25, which is the ratio of the diffusion coefficient
of N2 to the diffusion coefficient of C02 in air at 0°C.  The basic assump-
tion in the CC^ flux method is that there is no production or consumption of
CC>2 within the zone over which the gradient is measured or beneath the cover
and that steady-state conditions exist throughout the sampling period.  Thus,
the method is not applicable to the cropped plots.

     Soil gas-diffusion coefficients were also determined for the plots by a
transient-state method.  The one-dimensional, transient-state equation for
diffusion of a non-reactive gas in soil is

                                            ?C                           (2)
                                  3te  9x2
                                                                       o
where C is concentration of the gas with reference to the gas phase  (cm  gas
cm" 3 soil air) , t is time  (hours) , D  is the soil gaseous diffusion  coeffi-
cient (CTB~ hour~^) , e is the soil-air content  (car air cm~3 soil) , and x is
soil depth (cm) .  Values of D  and e are assumed to be constant with respect
to x and t.  Equation (2) was solved analytically using a time-dependent
upper boundary  condition.  Such a condition could be easily achieved experi-
mentally by feeding gas at a constant rate into an enclosed chamber  above  the
soil with ports for the mixed gas to leave the chamber.  If N2 is  the gas  of
interest, the N~ concentration within a chamber above the soil could be
decreased with  time by feeding gas of zero N2 concentration into  the chamber
with the mixed  gas leaving the chamber through exit ports.  The N£ concentra-
tion at the soil surface would decrease as some function of time.  For the
general case where the concentration at the soil surface varies with time  by
a smooth function, the surface condition may be described by a step  function
given by
                                      15

-------
                       C(0,t) = SQ       t0 < t
                                S
                                S2       t2 < fc - t3
                                Sk
                                Sn       tn < *                         (3)

where Sfc is the surface concentration within any time interval k.  The solu-
tion of Eq. (2) using Eq.  (3) and

                C = S0                x > 0         t = 0               (4a)
is
                       L
         C(x,t) = SQ + Z   (Sk - 5^}) erfc {x/ [2/Dm(t-tk) ] }             (5)
                      k=l
where L = {k:t > tk>, that is, k is the largest integer such that tfc is less
than t, Dm = Dp/e, and k is a dummy variable.  The only assumptions inherent
in the use of Eq. (5) for determining the diffusion coefficient are that Dm
is constant with respect to x and t and that diffusion is not allowed to
proceed so long that concentrations markedly change at the bottom of a field
box.

     The general procedure for determining the diffusion coefficient D  was to
fit Eq. (5) to concentration profiles measured in the field at several times,
using values of S^ and  t obtained from interpolation of measured values at
the surface and at t = 0, and various values of Dm.  The least absolute dif-
ference was used to evaluate the best fit of the predicted to the measured
profiles.  The use of the absolute difference gave a more clearly defined
minimum (best fit) than did least squares.

ANALYTICAL TECHNIQUES

     Oxygen, N£, CO^, and N-0 were analyzed by gas chromotography with a
thermal conductivity detector.  The concentration of N-0 in the gas samples
was determined by chromatography with a helium ionization detector according
to the procedure described by Delwiche and Rolston (1976).
                                      16

-------
     The isotopic composition of N in gas samples was determined on samples
scrubbed for 02> CC^, and l^O by direct injection into the mass spectrometer.
An independent experiment was conducted in which manure was added to soil in
order to determine if gaseous compounds were being evolved from the manure
and soil mixture which would interfere with the -*--%2 analyses.  These experi-
ments showed that no such evolution occurred to any significant degree.

     Soil samples were analyzed for extractable and digestible nitrogen and
soil solution samples were analyzed for NET, NO^, and N07.  The soil sample
was extracted with 1.0 N KC1 and the solution analyzed by MgO-Devarda alloy
reduction technique.  The extraction procedure removed solution NHT, NO^,
NO^, and exchangeable NH^.  The NHj~ and NO^ concentrations in all soil and
soil solution samples were negligible.  The Kjeldahl method was used to
determine the total digestible N in the soil and plant samples.  Two-g samples
of soil were digested with 36N H2SO^ and salts (KoSO^, CuSO,, and selenium)
for approximately 17 hours to convert the N to NHT.  The same procedure was
used for the plant digests except that 0.25 g of plant material was used, and
digestion time was 6 hours.  The N in the digests was determined by titration
of the NH+ liberated by distillation of the digest with 40% NaOH.  Detailed
procedures for determination of N in soil, plant, and soil solution samples
are given by Bremner (1965).
                                     17

-------
                                 SECTION 5

                          RESULTS AND DISCUSSION


HIGH-TEMPERATURE EXPERIMENT

Plot Characteristics

     Temperature at the 5-cm soil depth as a function of time after the ferti-
lizer was applied  to the plots of the summer experiment is  given by Figure 6.
         0
10     20
30     40     50    60    70     80
   TIME (days)
Figure 6.  Mean soil  temperature of two probes at the 5-cm soil depth of six
           plots as a function of time after fertilizer was applied to the
           plots of the summer experiment.  The arrows give the fertilizer
           application for each plot with the symbols given in Table 2.
                                    18

-------
The arrows give the time that fertilizer was  applied  to particular plots.
The average soil temperature during most of the denitrification  activity was
approximately 23°C.  There was a slight increase in soil  temperature begin-
ning about two weeks after the fertilizer was applied to  the  first plot.  The
increase in soil temperature occurred at the  time fertilizer  was applied to
the cropped and uncropped plots of the dry  treatment.

     The increase in soil temperature at two  weeks after  fertilizer was
applied to the first plot coincided with a  decrease in the  soil-water pressure
of the dry plots.  The soil-water pressure  head, h, for the 5- and 15-cm
depths as a function of time after fertilizer application for the summer ex-
periment is given by Figure 7.  For the h = -15 cm and h  =  -70 cm soil-water
   -160
                                                SUMMER
                                                 •  5cm depth
                                                 o  15cm
                                          30
                                     TIME (days)
Figure 7.  Mean soil-water pressure head of three tensiometers in each plot
           at the 5- and 15-cm soil depth as a function of time after ferti-
           lizer application to the two water treatments of the summer experi-
           ment.  The arrows give the fertilizer application for each plot
           with the symbols given in Table 2.
pressure treatment, the soil-water pressure head for the h = -15 cm treatment
was relatively constant throughout the denitrificafeion period,  whereas the

                                      19

-------
soil-water pressure for  the h = -70 cm treatment varied due to changing tem-
perature and radiation conditions.  Soil-water pressure values were main-
tained by reading tensiometers daily and making changes in number of passes of
the irrigation system in order to correct any increases or decreases in the
soil-water pressure head from the desired values.  It was sometimes difficult
to maintain constant water content in the h = -70 cm plots during rapid
changes in air temperature.  Values of the soil-water pressure head as a
function of depth are given by Figure 8 for the h = -15 and -70 cm treatments.
          SOIL-WATER  PRESSURE HEAD  h(cmH20)
                     -40   -80   -120  -160 -200
                                           SUMMER     _
  Figure 8.  Mean soil-water pressure head as a function of soil depth for the
            three plots of each water treatment of the summer experiment.
  The soil-water pressure head values are average numbers of the three plots of
  each soil-water treatment.  In a similar manner the soil-water content, 0, as
  a function of depth for the two water treatments is given in Figure 9.  It is
  obvious from Figures 8 and 9 that soil-water content, and soil-water pressure
  both decrease with depth.  This is due primarily to the fact that the soil
  surface tended to seal with time resulting in lower infiltration rates in the
  surface than in the remainder of the profile. This characteristic of decreas-
  ing water contents and pressures with depth results in the possibility of

                                    20

-------
                       SOIL-WATER  CONTENT 6 (cm3 cm'3)
                  0.30
0.33
0.36
0.39
0.42
0.45
Figure 9.  Mean soil-water content as  a function  of soil depth for the three
           plots of each water treatment of  the summer experiment.
limited denitrification occurring  in  the lower part of the profile. From soil-
water content and soil bulk density,  the soil-air  content, e, as a function
of depth can be calculated and is  plotted  in Figure 10 for the two soil-water
treatments.  These values of e are average values  for the three plots of each
water treatment.  The'h = -15 cm and  h = -70 cm  treatments result in only
very small differences between the soil-air content in the surface soil.
However, as will be shown later, this small difference is sufficient to make
a very large difference in the denitrification rate and magnitude.

                                     21

-------
                           SOIL-AIR CONTENT e(cm3cm~3)
                                0.08
0.16
0.24
Figure 10.  Mean soil-air content as a function of soil depth for the three
            plots of each water treatment of the summer experiment.
Soil Gases

     The amount of 02 in the soil and the diffusion rate of 02 within the
soil profile is one of the very important factors determining whether denitri-
fication will occur or not.  Figure 11 gives 02 concentrations within five
plots of the summer experiments as a function of soil depth.  Although mea-
surements were not made on the uncropped, h = -15 cm treatment, the 02 concen-
tration would be expected to be no smaller than 10%.  The oxygen concentra-
tions were measured during the time of the denitrification experiments.

     For the three plots at h = -70 cm, 02 values decreased to no less than
approximately 16% and that occurred in the plot to which manure had been added.
For the plots maintained at a soil-water pressure head of -15 cm, 02 values
became as small as 9% at the 20-cm depth of the cropped plot and as low as
approximately 3% at the 10-cm depth in the plot to which manure had been added.
In all cases, the smallest concentration of 02 occurred at the 10-to 20-cm
                                      22

-------
                                 02 CONCENTRATION (%)
                          10
                         20
                      - 30
                      ^j
                      I
                      ^~~ 40
                      0-
                      5  50
                      CO
                         60
                         70
                         80
                         90
                                      10
15
20
25
                             SUMMER
Figure 11.  Oxygen concentration as a function of soil depth in the plots of
            the summer experiment.  Symbols are given in Table 2.
depth in the profile with higher concentrations toward the soil surface and
also higher concentrations deeper with depth in the profile.  This phenomenon
has also been observed by Rolston et al. (1976) where G£ levels were smallest
near the soil surface and increased with depth due to smaller soil-water
pressures, smaller water contents, and more diffusion of 62 from the deeper
depths of the soil profile.  Since these samples were determined by extract-
ing a volume of gas with a syringe, the concentrations reported here are most
likely those concentrations in the large, continuous pores of the soil profile.
Thus, the G£ concentrations only give a qualitative estimate of the anoxic
conditions within the profiles.
     Table 3 gives initial concentration of N£0 within the six plots of the
summer experiment before application of NO^ fertilizer.  This gives an idea
of the degree of reducing conditions within the profiles and the denitrifica-
tion of native nitrogen.  These data indicate that the ^0 concentration
before fertilizer application was dependent upon the reducing conditions of
                                      23

-------
TABLE 3.  CONCENTRATION (PPMV) of NO WITHIN PROFILES BEFORE APPLICATION OF
          FERTILIZER OF THE SUMMER EXPERIMENT.  AMBIENT CONCENTRATION OF N~C
          IN AIR IS APPROXIMATELY 0.30 PPM
Soil
Depth (cm)
2
5
10
15
20
30
60
90

Cropped
0.08
0.09
0.09

0.19
0.37
0.29
1.25
h = -15 cm
Manure
4.0
2.6
6.8
32.4
26.3
38.4

9.2

Uncropped
2.6
3.1
3.3
3.3
3.0
3.5



Cropped
0.81
0.46
0.23

0.78
0.96
1.2

h = -70 cm
Manure
32
39
40

37
41
30
16

Uncropped
1.33
0.71
1.19

1.06
1.52
4.31

the profile and the amount of soil nitrogen available.  The concentrations in
the cropped plots were initially near ambient.  This was most likely due to
the grass using nitrogen which was slowly mineralized from soil organic matter
and to the reducing conditions within the root zone caused by root and micro-
bial respiration with the overall result of reduction of any N20 to N2.
Almost all samples from the h = -15 cm, cropped plot were below ambient indi-
cating very little production of N20 or reduction of N20 to N2.  The manure
plots initially had N20 concentrations ranging from 2 to 41 ppm.  Apparently
there was some denitrification of nitrogen mineralized from the manure.  The
h = -70 cm manure treatment had generally higher N20 concentrations than did
that of the h = -15 cm, manure treatment.  Nitrous oxide concentrations in
the uncropped plots ranged from . 7 to 4 ppm.  Apparently there was some miner-
alization of soil organic matter in the uncropped plots resulting in a small
amount of N which could be denitrified forming N20.  However, conditions were
apparently not anoxic enough that the N20 was further reduced to N2.

     Representative N20 concentration profiles from denitrification of the
added fertilizer as a function of soil depth for two days after fertilizer
application for the h = -15 cm treatments are given by Figure 12.  The concen-
tration profiles demonstrate the enormous differences in N20 production among
the cropped, manure, and uncropped plots.  It appears that the greatest
denitrification in the manure plot was occurring in the upper 1$ cm of soil,
whereas denitrification in the cropped plot appeared to be occurring slightly
deeper.  Similar data for the plots of the h = -70 cm treatment for two days
after application of fertilizer are shown by Figure 13.  There was much less
production of N20 in the h = -70 cm treatments than in the h = -15 cm treat-
ments.  Since N20 concentrations did not become great enough to measure 15N
without concentrating the N20 sample, N20 concentrations greater than initial
values were considered to be derived from the fertilizer.
                                      24

-------
                    N.O CONCENTRATION (ppm v)
I
I-
o.
     0
    10
   20
   30
                  200
                                  400
600
800
O
to  40
   50
   60
                                            SUMMER
                                            Day I
                                            h = -!5cm
                                            CROPPED
                                            MANURE
                                            UNCROPPED
Figure 12.  Nitrous oxide concentration with depth on one day in the h
          cm treatment of the summer experiment.
                                                          = -15
                             25

-------
                 0
                 I
               10
              20
           x
           t-
              30
           o
           co 40
              50
              60
N20 CONCENTRATION  (ppm v)
     100           200
300
                  SUMMER
                  Day 2
                  h = - 70 cm
                • CROPPED
                o MANURE
                A UNCROPPED
Figure 13.  Nitrous oxide concentration with depth on one day in the h = -70
           cm treatment of the summer experiment.

                                                          t
     Similar representative N£ profiles derived from the fertilizer for two
days after  application of the fertilizer are given in Figures 14 and 15 for
the h = -15 and h = -70 cm treatments, respectively.  The concentration
profiles for   No gas follow the same pattern as do those of the ^0, with
considerable differences in  N2 production among the cropped, manure, and
uncropped plots.
                                   26

-------
             ISL FROM FERTILIZER (mg N liter"1 soil air)
                                             SUMMER
                                             Day 2
                                             h = -15 cm
                                            • CROPPED
                                            o MANURE
                                            A UNCROPPED
Figure 14.  Concentration of 15N2 with depth on one day in the h
           treatment of the summer experiment.
= -15 cm
                                  27

-------
     X
     I-
     Q_
     UJ
     O
     O
     If)
              N2 FROM  FERTILIZER (mg N liter'1 soil air)
          ,0             0.2            0.4            0.6
        10
        20
    * 30
       40
        50
       60
                                                                    0.8
  SUMMER
  Day 2
  h =- 70 cm
• CROPPED
o MANURE
AUNCROPPED

Figure 15.  Concentration of   N2
                                       depth on one day in the h = -70 cm
            treatment of the summer experiment.
Gas Fluxes

     Flux of ^0 derived from the fertilizer as a function of time for the
manure and cropped plots is given by Figure 16.  These fluxes were determined
from the accumulation of N£0 beneath a cover placed over the soil surface for
1- or 2-hour intervals.  The time interval that the covers remained on the
plots was calculated from the air volume of the cover above the soil, the
enrichment of the fertilizer, the minimum detectable limit of 1%2 by
spectrometer, and the criterion that an N£ flux of at least 1.0 kg N
was measurable.  The numbers below each of the soil-water pressure head treat-
ments are total N£0 produced as determined from the area bene%th each of the
flux versus time curves.  The flux calculated from the concentration increase
beneath the cover was corrected for the decrease in the concentration gradient
with time as the gases accumulated.  The decrease in the concentration gra-
dient with time would result in an underestimation of the diffusive flux as
measured fromconcentration changes beneath the cover.  A simple correction
for this underestimation of the flux can be made based upon the steady-state
                                     28

-------
             o»
             cr
             LU
                 8.0
                 6.0
             >\
             -g  4.0
                 2.0
£   o
n  0.8
                 0.6
                 0.4
              CJ
                 0.2
                      "I—I—\
              .4 kg N ha'
                                                  MANURE
                                                 CROPPED
                                        = -!5cm
                                      _4.3 kg N ha"
                          1.8 kg N ha"
          l   I   l   I   I  I   l  I  I   I   I   I   I
                   0
                     5              10
                      TIME (days)
15
Figure 16.  Flux of NnO calculated from measurements beneath  cover with time
            for the manure and cropped plots of  the summer  experiment.
diffusion equation,
                                f = -Dp(dC/dx)
                                                            (6)
where f is the gaseous flux, D  is the soil gaseous diffusion coefficient,  C
is gas concentration, and x is soil depth.  If  it  is assumed  that  the concen-
tration at the soil surface is equal  to  the concentration beneath  the cover
and that the concentration at the shallowest  sampling depth (2 cm)  does  not
change with time, the following boundary conditions apply:
                                           x =  0  cm

                                           x =  2  cm
                 C = C2

                 and  (7]

              Dp = -(VL)(Atr1to[(C2-C0)/C2]
The solution to Equations  (6) and  (7) rearranged  to  solve  for  D   is
          (7a)

          (7b)



          (8)
                                      29

-------
where V is the volume of the chamber placed over the soil surface, L is the
depth of soil for which measurements are taken  (2 cm), A is the cross-
sectional area of the soil covered with the chamber, t is the time after
covering the soil at which the concentration beneath the lid (Co) was measured,
and An is the natural logarithm.  The value of Dp was determined from Equation
(8) for the 0 to 2-cm depth interval from the change in concentration (Co) of
N20 over a 1- or 2-hour time period and the measured concentration at the 2-cm
depth (C2).  The calculated Dp and the measured concentration gradient (dC/dx)
at t = 0 (assumed to be linear for 0 to 2 cm) were used to calculate the
corrected flux from Equation (6).  This corrected flux was the best estimate
of the gaseous flux of N20 if the cover had not been placed over the soil
surface.  Measurements of concentration at the  2-cm depth both before and
after the cover had been in place for 2 hours demonstrated that Condition (7)
was valid for a 2-hour period.   The greatest correction in the calculated flux
was for the cropped  (h = -15 cm) treatment.  Corrections for all other plots
were less than 5% of the total denitrification.

     Similar data for the flux of N20 from the  fertilizer as a function of
time for the uncropped plots are given by Figure 17.  The scale of the
         0.48
    CSJ
                                     TIME  (days)
Figure  17.   Flux of  N20 calculated  from measurements, beneath cover with time
             for  the  uncropped  plots of the  summer experiment.
                                      30

-------
ordinate is considerably smaller than that for the cropped and manure plots.
Both Figures 16 and 17 show that ^0 could not be detected beneath the lid
after approximately 20 days.

     Similar data for the flux of N£ derived from the fertilizer as a function
of time for the manure and cropped plots are given by Figure 18.  These fluxes
                                    10         20
                                      TIME (DAYS)
30
Figure 18.  Flux of   N2 calculated from measurements beneath cover with time
            for the manure and cropped plots of the summer experiment.


were also determined from the accumulation of N£ beneath a cover placed over
the soil surface and corrected for the decrease in the concentration gradient
as N£ accumulated.  The numbers below each of the soil-water pressure head
treatments are total No produced.

     The increase in the N2 flux at 1.4 days of the h = -15 cm, manure treat-
ment (Figure 18) was from a sample taken in the afternoon of a fairly hot day.
Thus, the fluxes may be slightly underestimated for a few days after applica-
tion due to increased denitrification as surface soil temperature increased
in the afternoon.  The increase in the N£ flux for the h = -15 cm, cropped
                                      31

-------
treatment at approximately 3  days after the fertilizer was  applied coincided
with the increase in temperature  (Figure 6).  The N2 flux from  the uncropped,
h = -70 cm treatment would also be expected to increase due to  the temperature
increase.  There appeared to  be a slight increase in flux although the total
flux was small and any increase would have a small effect.   Data for the flux
of N£ from the fertilizer as  a function of time for the uncropped plots are
given by Figure 19.  The scale of Figure 19 is considerably different than
  O>
  -  3
  tr
  UJ
  N

  ^  2
  tr
  LJ
  O
  DC
  U_
    CM
                                            I    I
                                                  UNCROPPED
hs-15cm
5.7 kg N ha
-i
                       h = -70cm
                       3.6 kg N ha'1
                              5                     10
                                   TIME (DAYS)
 Figure 19.  Flux of   N£ calculated from measurements beneath cover with time
            for the uncropped plots of  the summer experiment.
 that of Figure 18.  The very high initial N£ denitrification rate and rapid
 decrease in the rate are similar to the behavior of the ^0 flux.  In all
 cases, the amount of N£ produced was much greater than N20.  f

     The data given in Table 4 are the total amount of denitrification con-
 sisting of both N£ and N20 for the six treatments of the summer experiment as
 determined from measurements beneath a cover placed on the soil surface over
 the time period for which N2 and ^0 were measureable.  The amount of denitri-
 fication ranged from 1% for uncropped, h = -70 cm treatment to 69% for the
                                     32

-------
     TABLE 4.  DENITRIFICATION AS N20, N2, AND TOTAL FOR THE SUMMER
               EXPERIMENT AS DETERMINED FROM MEASUREMENTS BENEATH A
               COVER PLACED OVER THE SOIL
                                                          Total
Treatment
                   N20
(kg N ha"1)     (kg N ha"1)     (kg N ha'1)     (% of  fertilizer)
Manure,
h = -15 cm
Manure,
h = -70 cm
Cropped,
h = -15 cm
Cropped,
h = -70 cm
Uncropped,
h = -15 cm
Uncropped,
h = -70 cm

9.9

5.4

4.3

1.8

2.1

0.6

198

42

30

7

5.7

3.6

208

47

34

9

8

4

69

16

11

3

3

1
manure, h = -15 cm treatment.  It is obvious that water content and carbon
level had an enormous influence on the total denitrification.

     The N2 to N20 ratio as a function of time after application of the NOT
to each of the plots is given in Table 5.  The average ratio calculated on
the basis of total amount of each gas produced is also given.  The largest
ratio of 20.0 occurred for the manure treatment at the soil-water pressure
head of -15 cm.  All other treatments gave N2 to N20 ratios of between approx-
imately 2.7 and 8.0.  The ratio of 6.0 for the uncropped, h = -70 cm treat-
ment is most likely not real due to the error in measuring very small fluxes.
For very anoxic conditions it would be expected that the ratio would be large
as is demonstrated by the large ratio of the manure plot compared to the
other treatments.  Without manure added to the plots the data show that there
is still considerably more N2 produced than N20.

     Some N2 and N20 may have diffused below the 60 cm deep barrier of each
plot and lost.  The amount of gas lost in this manner was calculated from the
N2 and N20 concentration gradient between the 30-and 60-cm depths and from
the average gaseous diffusion coefficient between the two depths.  Using a
diffusion coefficient of 5 cm^ hr"1 corresponding to a soil-air content of
0.12 (Rolston and Brown, 1977) the amount of N2 and N20 diffusion below the
60 cm depth was calculated to be 10, 5.5, and 2.5 kg N ha'1 for the manure,
cropped, and uncropped plots, respectively, of the h = -15 cm water treatment.
                                     33

-------
              TABLE 5.  RATIOS OF N2 TO N20 PRODUCED FROM DENITRIFICATION IN THE PLOTS OF THE
                        SUMMER EXPERIMENT FROM MEASUREMENTS BENEATH A COVER PLACED OVER THE SOIL
10
Treatment N2/N20 ratio
Days after NO^ application
0.25 1 2 34 56 78 10 13
Manure ,
h = -15 cm 8.8 8.3 16.4 	 	 22.5 	 	 	 	 	
Manure,
v. — _7f) pm 9 Q A7 9 Q An A 	 	 	 	 	 	 	
Cropped ,
h = -15 cm 2.8 4.3 1.9 2.2 	 	 7.0 	 8.9 14.6 17.7
Cropped ,
h = -70 cm 	 0.5 	 5.0 	 	 6.0 	 	 	 	
Uncropped,
h = -15 cm 	 8.2 3.7 	 2.8 	 	 14.3 	 	 	
Uncropped,
h - -7fl r-m 1 _ 5 1 V 1 	 	 	 	 	 Q A 	 	 	
Average
N2/N20 ratio


20.0
7 ft
7.0
3.9
2.7
A n

-------
The concentration gradients for the 30-to 60-cm depth in the plots of the
h = -70 cm treatment were very near zero so the loss of gas below the barrier
was negligible.

     Soil gaseous diffusion coefficients, determined by the C02 flux method,
are given for four plots of the high-temperature experiment in Table 6.  The
               TABLE 6.  SOIL GASEOUS DIFFUSION COEFFICIENTS
                         DETERMINED BY THE C02 FLUX METHOD FOR
                         THE SUMMER. EXPERIMENT

               Treatment          Date          D  (cm2 hr"1)
Manure,
h = -15 cm
Manure ,
h = -70 cm
Uncropped,
h = -15 cm
Uncropped,
h = -70 cm
8/26
9/16
9/22
10/6
10/7
10/14
9/3
9/21
10/11
10/5
11/11
0.09
0.009
0.02
0.05
1.02
0.84
0.10
0.07
4.07
1.70
2.14
diffusion coefficient of the cropped plots could not be determined using the
C02 flux method because of the sink for C02 in photosynthesis.  Each value in
the table is the individually determined value for several different days.
The diffusion coefficients for any plot tended to decrease with time indica-
ting that the soil surface was becoming less permeable to the diffusion of
gas as more irrigation water was applied.  Determinations of diffusion coef-
ficients were made more than one month after denitrification experiments were
conducted.  Thus, it may be expected that the measured diffusion coefficients
would have been smaller than those during the denitrification experiment.
These measured diffusion coefficients were generally an order of magnitude
smaller than those required to approximate the measured flux as determined
from a cover placed over the soil surface.  These results demonstrate the very
dynamic nature of the soil-gas duffusion coefficient and the importance of the
soil surface condition on the transport of water and gas across the soil-
atmosphere boundary.

     Soil gaseous diffusion coefficients determined by the transient-state
method (Equation 5) are given by Table 7.  Values of D  determined by the
transient-state method are at least an order of magnitude larger than those
determined by the steady-state method.  The soil-air content, e, is required
to convert fitted values of Dm from the transient-state method to values of
Dp.  If only a portion of the total air space of the soil was contributing to
diffusion as would occur with trapped air isolated by water films, the effec-
tive e for diffusion would be much less than the total air space.  Apparently,

                                      35

-------
TABLE 7.  SOIL GASEOUS DIFFUSION COEFFICIENTS DETERMINED BY THE TRANSIENT-
          STATE METHOD FOR THE SUMMER EXPERIMENT
treatment
Manure, h = -15 cm
Manure, h = -70 cm

Cropped, h = -15 cm

Cropped, h = -70 cm

Uncropped, h = -15 cm

Uncropped, h = -70 cm



Date ]
9/15
10/6
10/15
9/16
9/21
9/28
10/12
6/28
9/14
10/7
10/14
11/9
11/10
DmCcrn2 hr-1)
90
120
110
220
200
100
60
60
80
225
240
200
280
e(cm3 cm 3) Dp (cm2 hr"1)
0.078 7.0
0.119 14.3
13.1
0.008 1.8
1.6
0.023 2.3
1.4
0.071 4.3
5.7
0.086 19.4
20.6
17.2
24.1
 the  effective e must be less than 10% of  the actually measured values of e at
 the  water  contents maintained in the field plots.
      Gas  sampling within the soil profiles demonstrated  that  considerable
was  produced from denitrification of 15N03 fertilizer.   Similar profiles were
also measured for N20.   For all plots except the manure  plot  at h = -15 cm,
the  1%2  concentrations were nearly constant with  depth  or  decreased  gradually
near the  surface.  For  the manure (h = -15 cm)  treatment, however, the great-
est  concentrations of ^-%2 an
-------
     The addition of manure to the soil greatly increased the rate and total
denitrification.  The addition of crop residues would also increase the deni-
trification potential.  The presence of living plants greatly increased the
amount of denitrification as shown by the differences in N2 and N£0 flux at
the soil surface of the cropped and uncropped plots.  The consumption of (^
through respiration of grass roots and addition of carbon to the system from
sloughed roots increased denitrification by approximately three to four times
over that of the uncropped plots at equal soil-water pressures.  For the un-
cropped plot maintained at a soil-water pressure head of -15 cm, only 8 kg of
N ha"^- were lost as N£ and N20.  Thus, it appears that very little denitrifi-
cation of added NOo will occur from uncropped Yolo loam even under the most
adverse soil-water conditions.  The maximum rate of denitrification in the
cropped plot maintained at h = -15 cm was considerably less than that reported
by Rolston et al. (1976).  The field plot used by Rolston et al. (1976) had
been cropped with perennial ryegrass for approximately two years before appli-
cation of NO^, and the soil may have been slightly wetter than that of this
study since water was occasionally pulled into the soil atmosphere samplers.
It appears that long-term cropping with grass may substantially increase the
available carbon of the soil and the denitrification potential.

     The soil-water pressure also has a large effect on denitrification.  By
decreasing the soil-water pressure head from -15 to -70 cm, denitrification
in the manure plots was decreased from 208 kg N ha~-*- to 47 kg N ha"-*-.  De-
creasing the soil-water.pressure head from -15 to -70 cm for the cropped plots
decreased total denitrification from 34 to 9 kg N ha  .  Decreasing soil-
water pressure in the uncropped plots decreased denitrification from 8 to 4
kg N ha""l.  The very narrow range of soil-water pressure for which denitrifi-
cation occurs for this particular soil  indicates that slight manipulation of
soil-water content may be achieved to either increase or decrease denitrifi-
cation depending upon particular objectives.

Plant Uptake

     Figure 20 gives the cumulative N uptake by the grass as a function of
time after the fertilizer was applied to the two cropped plots of the high-
temperature experiment.  The grass of the h = -70 cm treatment took up 20% of
the applied fertilizer as compared to 11% uptake by the grass of the h = -15
cm treatment.  This difference in uptake was due to the greater N loss through
denitrification and the greater rate of N movement through the root zone of
the h = -15 cm treatment.  The rate of N uptake for both treatments was very
large soon after the fertilizer was applied.  The rate of N uptake in the h =
-70 cm treatment also increased drastically at approximately 50 days after
fertilizer was applied.  This increase in N uptake was primarily due to in-
creased dry matter production most likely due to decreasing air and soil tem-
perature..  The N uptake of the h = -15 cm treatment, however, did not increase
at 50 days as did that of the h = -70 cm treatment since the fertilizer NO^
had been either denitrified or leached from the root zone by that time.  Both
plots had approximately the same rate of N uptake for the first 50 days.
                                      37

-------
                                       60
                                    TIME (days)
80
100
120
Figure 20.  Plant uptake of fertilizer N with time of the summer experiment.
Leaching

     Figure 21 gives soil solution NO, concentrations derived from the
fertilizer as a function of soil depth at approximately 125 days after appli-
cation of the fertilizer to the h = -15 cm treatments.  The large differences
in denitrification among the cropped, manure, and uncropped plots of the h =
-15 cm treatment also resulted in large differences in the concentration of
fertilizer N0~ in the soil solution of the profile.  As expected, the manure
plot with the largest amount of denitrification resulted in the smallest N0~
concentrations in the soil solution.  Denitrification in the uncropped plot
of only 3% resulted in the largest NOg concentration in the soil solution.
The peak of the NO" pulse for all three plots of the h = -15 cm treatment was
at approximately 140 cm for 120 days after fertilizer application.  On the
other hand, for the h = -70 cm treatments, most of the NO^ was still in the
upper 60 cm of the soil profile.  An estimate of evapotranspiration was
obtained from the water application rate for the h = -15 cm treatments, the
volumetric water content of the soil profile, and the rate of movement of NO^
through the soil profile.  Inasmuch as the profiles were kept constantly wet,

                                      38

-------
                          SOIL SOLUTION FERTILIZER N (ppm)
                              20    40   60    80   100
                                         I      i     I
                                      SUMMER
                                      h =-!5cm
                                      CROPPED, day 120
                                      MANURE, day 133
                                      UNCROPPED, day 127
 Figure 21.  Concentration of fertilizer derived N07 in the soil solution as
             a function of soil depth for the h = -15 cm treatments of  the
             summer experiment.


it would be expected that evapotranspiration would be similar for all plots.
Applying this estimated evapotranspiration to the h = -70 cm treatments gave
a pore-water velocity, vs, for theh = -70 cm treatments of approximately 0.5
cm day""1 as compared to 1.1 cm day~  for the h = -15 cm treatments.  From
these estimates of pore-water velocity, the peak of the NO^ pulse should have
been at about 55 cm at 110 days for the h = -70 cm treatment.  Soil solution
samples taken at 110 days show a slight increase in NO^ concentration at the
60 cm depth of the h = -70 cm treatments.  The position of the NOo pulse in
the h = -70 cm treatments can be ascertained from the soil samples taken ap-
proximately 5.5 months after the NO^ was applied.  The residual soil N  will
be presented in a later section.

     The total leaching of NO^ from the h = -15 cm treatments was determined
from the flux of water and the NOj concentration at each of the 15 soil solu-
tion samplers as NOj moved through the soil profile.  The soil-water flux was
                                      39

-------
determined from the time of arrival of the NO^ peak at each sampler and the
average water content above that sampler.  The soil-water flux used in calcu-
lating NOg recovery was determined from the pore-water velocity at each sam-
pler, the mean pore-water velocity from the 9 samplers (3 plots) at each
depth, the mean pore-water velocity from the 15 samplers of all depths of one
plot, and the mean pore-water velocity from the 43 (2 samplers not functional)
samplers of all depths of three plots.  The results of determining NOg re-
covery by these methods are given in Table 8.  In calculating the NC>3 leach-
ing component, the mean recovery was calculated from all depths of each plot
using the mean pore-water velocity of the 9 samplers at each depth (second
row of Table 8).  The pore-water velocity of the 9 samplers at each depth
was considered the best estimate of the velocity at that depth inasmuch as
velocity would change with depth due to changing water content with depth.
Although this method was selected due to the above mentioned reason, the
recovery percentages of any of the other methods of determining pore-water
velocity are similar.  However, the data indicate  that the recovery percent-
ages  are too large for the shallow depths and too small for the deep depths.
This discrepancy is believed to be due to the inability to accurately deter-
mine the water content at all depths and time from soil-water characteristic
curves, limited soil-water pressure head data for the deeper depths, and
nonuniform displacement of the NO^ pulse through the soil.  These data demon-
strate the difficulty and uncertainty in determining the leaching of NO^ in
a field soil even in small, well-instrumented plots.

Residual Soil N

     The extractable soil N derived from the fertilizer as a function of soil
depth for the h = -70 cm treatments of the high-temperature experiment is
given in Figure 22.  Extractable N for the h = -15 cm treatments was very
small.  Extractable soil N includes NflJ, NO^, and NO- in solution and NtiJ on
the exchange sites of the soil.  The concentration of Nfll" was determined
separately and found to be less than 1 ppm  (usually smaller than 0.6 ppm in
top 15-cm and much less below).  The data points are mean concentrations
within 15-cm depth increments from eight samples.  The extractable N in the
h = -70 cm treatments was large in the upper 60 cm of soil due primarily to
NOg which had not yet been leached out of the upper part of the profile.

     The digestible soil N derived from the fertilizer as a function of soil
depth for the six plots of the high-temperature experiment is given in Figure
23.  Digestible soil N is that portion of the soil N existing as live or dead
plant roots, microbial biomass, and fixed NfiJ.  Fixed NHj is expected to be
small for Yolo loam soil.  The data points are mean concentrations within
15-cm depth increments from eight samples.  Digestible soil N was greatest
near the surface due to plant roots and microorganisms.  The cropped and
manure plots resulted in the greatest digestible N, although  the uncropped
plots also had digestible N in the upper part of the profile. "Digestible N
in the manure and uncropped plots was due in part to microbial immobilization,
although  it was difficult to keep small weeds and moss from growing on the
manure and uncropped plots which would immobilize N in roots.  Although the
manure plots had very little plant growth, considerable N was immobilized.
                                      40

-------
   TABLE 8.   PERCENTAGE RECOVERY OF FERTILIZER N LEACHED IN THE h = -15 CM PLOTS OF THE SUMMER EXPERIMENT
             CALCULATED BY VARIOUS WAYS OF DETERMINING THE SOIL-WATER VELOCITY, v .  THE MEAN RECOVERY OF
             ALL DEPTHS FOR EACH PLOT IS GIVEN IN PARENTHESES                    S
   Method of determining
   pore-water velocity
                                         Cropped
 60  90  120  150  180
                                  % Recovery
                                   Manure
60  90  120  150  180
                                 Uncropped
 60  90  120  150  180
   From v  of each
•o  sampler
132  57   68   61   44
        (72.4)
11  14   12   11   10     104 121   78   66   56
       (11.6)                     (85.0)
   From mean v  of all
              S
   samplers at each depth
   (9 samples)
   From mean v  of all
              O
   depths of one plot
   (15 samples)
   From mean v  of all
   depths of 3 plots
   (43 samples)
 75  55   64   57   44
        (59.0)
 86  64   68   57   44
        (63.8)
 80  60   63   53   41
        (59.4)
14  14   12   12   10     100 114   76   66   57
       (12.4)                     (82.6)
13  14   11   10
       (11.4)
14  15   12   11
       (12.2)
110 129   77   65   55
        (87.2)
108 122   76   62   54
        (84.4)

-------
                  SOIL  EXTRACTABLE  FERTILIZER N (JJLQ N g" soil)
                  .0      10     20    30    40     50    60
                               T
                                                 \
                                       Summer
                                       h = -70cm
                                      • Cropped
                                      o Manure
                                      * Uncropped
Figure 22.   Soil extractable N from fertilizer as a function of soil depth,
            5.5 months after fertilizer application, of the summer experiment,
                                   42

-------
                                                         -I
            SOIL DIGESTIBLE  FERTILIZER  N (/tgNg  soil)
          0     10    20 0     10    20   30    40   50   60
                                          Summer
                                          • Cropped
                                          ° Manure
                                            Uncropped
                                              h=-70cm
IOOT-h = -l5cm
Figure 23.  Soil digestible N from fertilizer as a function of soil depth,
           5.5 months after fertilizer application of the summer experiment.
Mass Balance

    Table 9 gives the N balance for each of the components of the N cycle.
Denitrification was determined by difference from fertilizer application,
plant uptake, leaching, and residual soil N.  Denitrification as determined
                                 43

-------
                  TABLE 9.   MASS BALANCE OF FERTILIZER N FOR THE SUMMER EXPERIMENT
                                                                     Residual
                                                             	in soil	Denitrification
                              Gaseous loss             Plant
                       N£     below 60 cm  Leaching   Uptake  Extractable Digestible   Direct  Difference
Treatment (kg N/ha) (kg N/ha)  (kg N/ha)  (kg N/ha) (kg N/ha)   (kg N/ha)  (kg N/ha)    (kg N/ha)   (kg N/ha)


Manure,
h = -15 cm    9.9     198         10          37       —          1         25          218        237

Manure,
h = -75 cm    5.4      42          0          —       —        157         62           47         79

Cropped,
h = -15 cm    4.3      30          5.5       175       34          0         52           40         35

Cropped,
h = -75 cm    1.8       7          0          —       62         64        132            9         39

Uncropped,
h = -15 cm    2.1       5.7        2.5       252       —          1         27           10         25

Uncropped,
h = -75 cm    0.6       3.6        0          —       —        254         23            4         16

-------
by difference is compared with denitrification determined from the flux of N£
and N£0 at the soil surface and any gaseous loss below the 60-cm barrier.
The amount of fertilizer applied to each plot is given by Table 2.

     The direct method for determining denitrification compares reasonably
well with the difference method.  The direct method gave 19 kg N ha~  less
denitrification than did the difference method for the manure, h = -15 cm
treatment.  A difference of only 19 kg N ha"-*- could easily be accounted for
by an underestimation of the gaseous flux on hot afternoons since measurements
were generally taken mid-morning, by small denitrification rates below the
detection limits for   N£ over several weeks, and errors in measuring leach-
ing and residual soil N.  Denitrification calculated directly was slightly
greater (5 kg N ha~l) than that of the difference method for the cropped, h =
-15 cm treatment.  This difference may be explained by an overestimation of
the leaching component since all samplers, including those at the 60-cm depth,
were used in determining NO^ leaching.  It would be expected that plant roots
could take up some additional N below 60 cm and thus, result in an overestima-
tion of the leaching.

     For all other plots, denitrification as determined directly was between
12 and 30 kg N ha~l less than that determined by difference.  The substantial
differences between the two methods for the h = -70 cm treatments may be
explained by small rates of gaseous loss below  the minimum detection limits
over several weeks and elevated rates on hot afternoons which were not mea-
sured.  These speculations seem especially reasonable since the NO, pulse
remained in the upper 60 cm of the profile for several months.  There may
also be some error in the residual soil N component of the difference method.
The sensitivity of the direct method may be increased by increasing the ^N
enrichment; of the added fertilizer, increasing the time that covers remain over
the soil surface, decreasing the volume of the chamber placed over the soil
surface, or by calculating gas flux from diffusion coefficients and concentra-
tion gradients within the soil. Although larger concentrations are possible
from soil air samples, the latter method is plagued with uncertainty in
measuring both the diffusion coefficient and the concentration gradient
(Rolston, 1977).

LOW-TEMPERATURE EXPERIMENT

Plot Characteristics

     Temperature at the 5-cm soil depth as a function of time after fertilizer
was applied to the plots of the winter experiment is given by Figure 24.  The
average soil temperature during most of the denitrification activity was
approximately 8-10°C.  There was a gradual increase in soil temperature ap-
proximately two weeks after the fertilizer was applied to the first plot.
The labeled arrows in the figure give the fertilizer applications to each of
the six plots.  The fertilizer was applied to plots at a temperature of 8-10°
C except for the cropped plot of the dry treatment at which the temperature
was 10-13°C.

     The soil-water pressure head, h, for the 5- and 15-cm depths as a function
of time after fertilizer application for the winter experiment is given by

                                      45

-------
      o
      o
      LU
      a:
      ID
      a:
      Ld
      o_
      2
      LU
              0
10
20     30     40
  TIME  (days)
50    60
Figure 24.  Mean soil temperature at the 5-cm soil depth as  a function of
            time after fertilizer was applied to the plots of the winter
            experiment.   The  arrows give the fertilizer application for each
            plot with the symbols given in Table 2.


Figure 25.  The soil-water pressures during the fertilizer application were
approximately -6 to -8 cm for the wet treatment, and approximately -50 cm for
the dry treatment.  The arrows in the figure give the times  that the  fertili-
zer was applied to each plot.  The pressure heads are mean values of  the
three plots of each soil-water treatment.  Values of the soil-water pressure
head as a function of depth are given by Figure 26.  As with ,the summer ex-
periments, the soil-water pressure heads became smaller with depth.   In a
similar manner, the soil-water content data as a function of depth for the
two water treatments are given in Figure 27.  These data were>obtained from
neutron moisture probe data,  and the data points are mean values for  the three
plots of each water treatment.  Water contents determined from neutron meter
data compare closely with those from tensiometers and soil-water characteris-
tic curves.  The soil-air content, e, as a function of depth can be calculated
and is plotted in Figure 28 for the two soil-water treatments.  These values
                                     46

-------

     -120
  <  -100 h
	1	1—
  WINTER
—•— 5cm depth
 -°- 15cm depth
                    10
         20
      30
TIME  (days)
40
50
Figure 25.  Mean soil-water pressure head  at  the 5- and 15-cm soil depth as
           a function of time after fertilizer application to the two water
           treatments of the winter experiment.  The arrows give the fertili-
           zer application for each plot.
                                    47

-------
       SOIL-WATER PRESSURE HEAD h (cm H20)
         0
^  30
    S  60
a.  90
UJ
Q
  , 120
       150


       180
          0   -40   -80   -120  -160 -200
           h-\
       -  \
                 »

                 \WET
                 i
                 A
                              WINTER
                               DRY
Figure 26. Mean soil-water pressure head as a function of soil depth for the
        two water treatments of the winter experiment.
                         48

-------
                       SOIL-WATER CONTENT 6 (cm3 cm'3)

                0.30  0.32  0.34 0.36  0.38 0.40  0.42  0.44 0.46
                0
Figure 27.  Mean soil-water content as a function of soil depth for the two
           water treatments of the winter  experiment.
                                    49

-------
                      SOIL-AIR CONTENT € (cm3 cm"3)
                ff.O  0.04  0.08  0.12   0.16  0.20  0.24  0.28
               160 -
               180
Figure 28.  Mean soil-air content as a function of soil depth for the two
           water treatments  of the winter experiment.
                                   50

-------
of e are average values for the three plots of each water treatment.  The h =
-8 cm and h = -50 cm treatments result in only very small differences of soil-
air content in the surface soil.

Soil Gases

     The amount of 02 in the soil as a function of soil depth for the six
plots of the winter experiment is given by Figure 29.  The Q£ concentrations
                        10
12
                                02 CONCENTRATION (%)
14
Figure 29.  Oxygen concentration as a function of soil depth in the plots of
            the winter experiment.  The symbols are given in Table 2.

were measured during the time that the denitrification experiments were con-
ducted.  Because of decreased biological activity at low temperature, all
plots exhibited relatively uniform Q£ concentrations with depth.  The only
major deviation among plots was the manure, h = -8 cm treatment.  The minimum
value attained in that particular plot was approximately 13% at the 5-cm
depth.  All other plots had Q£ values between 18 and 21%.  Although Q£ concen-
tration within the profile gave only a qualitative estimate of anoxic develop-
ment, it is obvious from Figure 29 that anoxic development in the profiles was
smaller than those of the summer experiment.
                                      51

-------
     The initial concentration of N20 within the six plots of the winter
experiment before application of NO^ fertilizer is given by Table 10.  The


TABLE 10.  CONCENTRATION OF N20  (PPMV) WITHIN PROFILES BEFORE APPLICATION OF
           FERTILIZER OF THE WINTER EXPERIMENT.  AMBIENT CONCENTRATION OF
           N20 IN AIR IS APPROXIMATELY 0.30 PPMV
Soil
Depth (cm)
2
5
10
15
20
30
60
90
h
Cropped
0.6
0.6
0.6

0.8
0.7
2.1

= -8 cm
Manure
11.0
12.8
15.1
15.6
8.5
6.9
2.2
1.4

Uncropped
0.7
0.7
0.6
0.8
1.1
0.7
0.7
0.8
h = -50 cm
Cropped Manure Uncropped
0.5 19.0 0.5
0.5 0.5
18.0 0.5
0.6 0.5
11.8 0.6
1.0 8.0 0.7
0.8
0.8
N£O concentrations in all plots were above ambient  (0.3 ppm) indicating that
conditions were not reduced enough to cause the small amount of ^0 produced
to be further reduced  to N2.  This observation is  entirely different from
that of the  cropped plots of  the  summer experiments where the small amount of
N£O produced was reduced to N£ resulting in N£0 concentrations below ambient.
The manure plots of the winter experiments had initial concentrations of N£0
as large as  20 ppm.  All other plots were slightly above the ambient concen-
tration with very little difference between plots.

     Representative N20 concentration profiles from denitrification of added
fertilizer as a function of soil  depth at 7 days after fertilizer application
for the h =  -8 cm treatments  are  given by Figure 30.  The concentration pro-
files demonstrate that considerable differences in ^0 production occurred
among the cropped, manure, and uncropped plots, although the differences are
not nearly as great as those  observed during the summer experiments.  Also,
the N20 concentration  profiles were generally much smoother and uniform with
depth than were those  of the  summer experiment.  Similar data for the plots
of the h = -50 cm treatment at 7  days after application of the fertilizer are
shown by Figure 31.  There was much less production of N£0 in the h = -50 cm
treatments than in the h = -8 cm  treatments, and the concentration profiles

                                      52

-------
                     N.O CONCENTRATION (ppm v)
    0
    10
Q_
liJ
O
O
CO
   20
   30
                  50
                                   100
150
               WINTER
200
                                             Day 7
                                             h =-8cm
                                             • CROPPED
                                             o MANURE
                                             * UNCROPPED
                                                 I      I
Figure 30.  Nitrous oxide concentration with depth on one day in the h
          cm treatment of the winter experiment.
                                                         = -8
                            53

-------
                       N.O  CONCENTRATION (ppm v)
               0
                               10
 20
30
               10
           a.
           UJ
           Q
           O
           cn  20
               30 •-*
                       WINTER
Day 7
h= -50cm
• CROPPED
° MANURE
* UNCROPPED
Figure 31.   Nitrous oxide concentration with depth on one day in the h = -50
            cm treatment of the winter experiment.
were fairly uniform with depth.   The  largest N£0 production occurred in both
the h = -8 and -50 cm water treatments of plots to which manure had been
added in the top 10 cm of soil.                             *

     Similar representative N£ profiles derived from the fertilizer at 7 days
after application of the fertilizer are given in Figures 32 and 33.  Concen-
tration profiles for ^%2 8as follow  the same pattern as that of N£0 with
differences in N£ production among the cropped, manure, and uncropped plots.
However, substantial denitrification  occurred only in the manure plots.
                                    54

-------
                               N,
                                          -i
             FROM  FERTILIZER (mg N liter" soil air)

                0    0.2   0.4   0.6  0.8   1.0
                                            I
                      WINTER

                      Day 7
 h=-8cm
• CROPPED
o MANURE   ~
* UNCROPPED
Figure 32. Concentration of 15N2 with depth on one day in the h = -8 cm
         treatment of the winter experiment.
                             55

-------
               FROM  FERTILIZER  (mg N liter   soil air)

                ^ 0      0.05    0.10     0.15    0.20
           E
           o
           a.
           UJ
           a
           en
               10
               30
                                                    I
                      WINTER
                      Day 7
  h=-50cm
• CROPPED
o MANURE
A UNCROPPED
 	I
Figure  33.   Concentration of  N£ with depth on one day in the h = -50 cm
             treatment of the winter experiment.
Gas Fluxes

     Flux of N£0 derived from the fertilizer as a  function of time  for the
manure and cropped plots is given by Figure 34. These fluxes were  determined
from the accumulation of ^0 beneath the cover placed over the soil surface
for 1- or 2-hour intervals.  The numbers below each of the soil-water pressure
head treatments are total ^0 produced as determined from the area  beneath
each of the flux versus time curves.  All data were corrected for the concen-
tration increase beneath the cover using Equations (6), (7), and (8).
                                                           4
     As with the NoO flux data of the summer experiments, the flux  of gases
from denitrification occurred immediately after addition of the fertilizer.
However, the ^0 flux increased at a much smaller  rate than that of the
summer experiments.  In all cases the total amount of denitrification which
occurred as N£0 was very small. Similar data from the flux of ^0  from the
fertilizer as a function of time for the uncropped plots are given  by Figure
                                    56

-------
             o
            •O
            IT
            LJ
            N
            tr
            UJ
            U_

            2
            O
            
-------
       0.03
    o
    TJ
       Q02
    o:
    UJ
    N

    o
    cr
    o
     eg
        0.01
                  1	1	T

                   UNCROPPED
                     h = -8cm
-i
                                          1
           0
10
         20
    TIME (days)
30
40
Figure 35.  Flux of ^0 calculated from measurements beneath a cover with
            time for the uncropped plots of the winter experiment.
35.  Again, very little denitrification as N£0 occurred in the uncropped plots
with the total amount being  only slightly different than that which occurred
in the cropped plots.  Denitrification occurred for a much longer time period
than for the summer experiments, although concentrations and fluxes were
small.
                                                                        \
     Data for the flux of  N2 derived from the fertilizer as a function of
time for the manure and cropped plots are given by Figure 36.  These fluxes
                                     58

-------
             o
             •o
             z
             o>
             N
             oc
             LJ
             O
             o:
             u.
                3.0
            -r-  2.0
 1.0
 0


0.8


0.6


0.4


0.2


 0
                                                        T
                                                 MANURE
h=-8cm
                                                 CROPPED
                                           20
                                     TIME (days)
                                       30
Figure 36.  Flux of   N2 calculated from measurements beneath a cover with
            time for the manure and cropped plots of the winter experiment.
were determined from the accumulation of N2 beneath the cover placed over the
soil surface and corrected for the decrease in the concentration gradient as
N£ accumulated.  The numbers below each of the soil-water pressure head treat-
ments are total N£ produced.  Denitrification was largest soon after applica-
tion of the fertilizer and decreased to relatively small values by approxi-
mately 20 days.  As determined by the criterion used for measuring the N2
beneath the cover over the soil, the minimum value which we considered signi-
ficantly different than background or machine noise was approximately 1 kg N
ha"1 day"1.  Thus, all of the N2 fluxes given in Figure 36 except for the
manure, h = -8 cm treatment were either at or below what is considered as the
minimal detectable limit.  Thus, the uncertainty of the denitrification in
this very small flux range is quite large.  There was very little difference
in denitrification in the manure plots of the h = -8 and -50 cm treatments,
although there was considerable uncertainty in the fluxes at these small
                                     59

-------
rates of denitrification.  Data for the N2 flux of the uncropped plots are
not given inasmuch as all fluxes were so near zero that no denitrification
was considered to have occurred as N2.

     The data given in Table 11 are the total amounts of denitrification
     TABLE 11.  DENITRIFICATION AS N20, N2, AND TOTAL FOR THE WINTER
                EXPERIMENT AS DETERMINED FROM MEASUREMENTS BENEATH A
                COVER PLACED OVER THE  SOIL
                                                          Total
                  N20            N2
Treatment      (kg N ha'1)     (kg N ha~l)     (kg N ha'1)     (% of fertilizer)
Manure,
h = -8 cm
Manure,
h = -50 cm
Cropped,
h = -8 cm
Cropped,
h = -50 cm
Uncropped ,
h = -8 cm
Uncropped,
h = -50 cm
4.2
3.8
0.7
0.1
0.4
0.2
27.1
26.4
17.6
1.9
0.0
0.0
31.3
30.2
18.3
2.0
0.4
0.4
11
10
6
1
* 0
= 0
 consisting of both N2 and N20 for the six treatments  of the winter  experiment.
 The amount of denitrification ranged from zero for the uncropped plots to 11%
 of  the total fertilizer added for the manure,  h = -8  cm treatment.  The water
 content or carbon level had very little influence on  the total amount of
 denitrification at these low temperatures.

      The N2 to N20 ratio as a function of time after  application of the NO,
 to  each of the plots  is given in Table 12.  The average ratio^calculated on
 the basis of total amount of each gas produced is also given. *The  largest
 ratios of 25 and 19 occurred for the cropped treatments at h = -8 and -50 cm,
 respectively.  These ratios may be somewhat  uncertain inasmuch as the flux of
 N2  was below that flux considered to be significant.

      Soil gaseous diffusion coefficients, determined  by the C02 flux method,
 are given for four plots of the winter experiment in  Table 13.  Diffusion
                                      60

-------
     TABLE 12.  RATIOS OF N2 TO N20 PRODUCED FROM DENITRIFICATION IN THE
                PLOTS OF THE WINTER EXPERIMENT FROM MEASUREMENTS BENEATH
                A COVER PLACED OVER THE SOIL
  Treatment                      N2/N20 ratio

                          Days after NO^ application

             0.25   12456      78      9

Manure,
h = -8 cm    6.2   2.5   3.8   	   4.3   7.5   11.9   	   12.7

Manure,
h = -50 cm   3.8   6.9   8.2  12.9   	   	    4.0   	   10.0

Cropped,
h = -8 cm    	  30.9  20.0   	   	  11.3    	  12.2

Cropped,
h = -50 cm  25     	   	   	  20     	   48.6   	   31.4
     TABLE 12 (continued)


                                                                    Average
  Treatment                      N2/N20 ratio                     N2/N20 ratio

                          Days after NO^ application

              12    13    14    15    16    20     21    28

Manure,
h = -8 cm    15.8   	  15.0   	  18.8   	    	   	           6.5

Manure,
h = -50 cm    	   	   	   6.8   	   	    4.8   4.8           6.9

Cropped,
h = -8 cm    13.3   	   	  51.5   	  34.5    	   	          25.1

Cropped,
h = -50 cm    	  16.2   	   	   	   	    	   	          19.0
                                      61

-------
    TABLE 13.  SOIL-GAS DIFFUSION COEFFICIENTS FOR THE WINTER  EXPERIMENT
Treatment
Date
Dp(cm2 hr"1)
                                                        Date of Fertilizer
                                                           Application
Manure
h = -8 cm



Manure
h = -50 cm

Uncropped
h = -8 cm




Uncropped
h = -50 cm



2/2
4/5
4/14
4/15
4/28
3/10
4/7
4/12
12/10
12/15
12/17
2/3
5/16
5/17
11/9
11/10
12/1
12/13
12/14
0.84
0.40
0.24
0.10
0.25
2.43
3.29
2.55
2.79
1.59
1.56
0.44
0.30
0.41
5.40
7.06
3.53
2.84
1.77
1/12



1/17

1/10




1/12



coefficients for N2 are approximately 1.25 times larger than those of C02.
Each value in the table was determined on different days.  Diffusion coeffi-
cients generally decreased with time in a similar manner to those of the
summer experiments due to changing soil surface conditions.  Diffusion coef-
ficients were used in conjunction with measured N2 and N20 concentration
gradients (five samplers at each depth) to calculate the denitrification flux
from Equation (1).  Values of the diffusion coefficients required in Equation
(1) in order to result in the same amount of denitrification as determined
                                      62

-------
from beneath the cover were approximately equal to measured values of the
h = -50 cm treatments (Table 13).  For instance, a value of Dp equal to 4
cm2 hr   for the h = -50 cm treatments resulted in the calculated flux to be
equal to the measured gas flux.  Values of Dp required in order that the
calculated flux for the h = -8 cm treatments be equal to the measured flux
were larger than those measured (Table 13) .  For instance, a value of Dp equal
to approximately 2.7 cm2 hr"1 for the h = -8 cm treatments resulted in the
calculated flux to be equal to the measured flux from gas accumulation beneath
covers.  The underestimation of denitrification flux from Equation (1) was
due primarily to the general decrease in diffusion coefficients with time and
the resultant uncertainty in knowing the value of Dp during denitrification.
However, additional gaseous transport mechanisms such as mass flow due to
pressure fluctuations of a barometric and wind turbulence source cannot be
absolutely neglected.  The very dynamic nature of diffusion coefficients,
strongly dependent upon surface soil conditions, requires that the measure-
ment of Dp be made several times as close as possible to the time period of
denitrification.  Although the temporal variability of the gaseous diffusion
coefficient results in some uncertainty in calculating flux of gases from
denitrification, Equation (1) can be used to determine denitrification if
accurate measurements of diffusion coefficients and concentration gradients
are made.  The advantage of calculating flux from Equation (1) over measur-
ing flux from accumulation of gas beneath a cover is the increased sensitiv-
ity due to larger concentrations of ^%2 within the soil than that from
accumulation beneath a cover.
     Measurements of  -   an(* ^0 within the soil profiles and beneath the
lids placed over the soil surface demonstrated that very little denitrifica-
tion of added NOg occurred at the low temperatures of approximately 8-10°C.
However, there was some denitrification in the manure and cropped plots with
rates being very small.  The addition of manure to the soil greatly increased
denitrification over that of the cropped plots.  Low amounts of denitrifica-
tion were due to low microbial activity which was reflected in relatively
constant and high values of D£ within the soil profile.  Differences in deni-
trification due to soil- water treatment were not great due to the overall
small rates of denitrification and uncertainty in the measured fluxes at
small denitrification rates.

Plant Uptake

     Figure 37 gives the cumulative N uptake by the grass as a function of
time after the fertilizer was applied to the two cropped plots of the winter
experiment.  The grass of the h = -50 cm treatment took up 47% of the applied
fertilizer at 115 days after application compared to 35% for the h = -8 cm
treatment.  The rate of N uptake was similar for both treatments until approx-
imately 50 days after application, at which time the NO^j pulse was being
leached below the major root zone in the h = -8 cm treatment.  The N uptake
was much greater for the grass of the winter experiment than that of the
summer experiment.  The difference in uptake was due to a much greater dry
matter production during the winter than in the summer because of more favor-
able growing conditions.
                                      63

-------
  0»
  LU
  CL
                20    40     60    80    100    120    140
                              TIME (days)
Figure 37.  Plant uptake of fertilizer N with time during the winter
          experiment.
                               64

-------
Leaching

     Figure 38 gives soil solution NO^ concentrations derived  from the ferti-
 Or



20 if-



4O
                           SOIL SOLUTION FERTILIZER N (ppm)
                             40   80    120   160  200   240
                             T
T
T
T
                                          WINTER
                                          h=-8cm
                                        • CROPPED (DAY 79) -
                                        o MANURE (DAY 79)
                                          UNCROPPED (DAY 81)
Figure 38.  Concentration of fertilizer derived NO^  in the soil solution as
            a function of soil depth for the h = -8  cm treatments of the
            winter experiment.
lizer as a function of soil depth at approximately  80  days  after application
of the fertilizer to the h = -8 cm treatments.   Since  denitrification was
small for all three plots, the greatest difference  in  the leaching component
was due to the large plant uptake.  Thus,  the NO^ concentrations in the
cropped plot were much less than in either the manure  or  the uncropped plots.
The NOg pulse moved faster through the plots of  the winter  experiment than
through those of the summer experiment.

     The total leaching of NO^ from the h  = -8 cm treatments was determined
from the flux of water and the NOo concentration at each  of the 15 soil solu-
tion samples of each plot using the same approach as described for the summer
                                      65

-------
experiments.  The recovery percentages using various ways of averaging the
soil-water velocity are given in Table 14.  The NO^ leaching component was
calculated using the mean soil-water velocity of the 9 samplers at each depth
since the soil-water velocity tended to change slightly with depth.  All
approaches for averaging the soil-water velocity resulted in recovery of much
more fertilizer N than was applied for the manure and uncropped treatments
and more than is reasonable for the cropped plot.  The mean recovery deter-
mined from all depths using the mean soil-water velocity of the 9 samplers at
each depth was 56, 138, and 182% for the cropped, manure, and uncropped plots,
respectively.  The greater recovery as leaching than that applied as fertili-
zer may be explained by an overestimation of the soil-water velocity or flux
of water in the field profiles.  The average soil-water flux (vs 0) was cal-
culated from values of vg determined by the time the NO^ peak reached a par-
ticular depth.  Values of the flux for the 60-, 90-, 120-, 150-, and 180-cm
depths were 0.54, 0.58, 0.55, 0.52, and 0.49 cm day"1, respectively.  The
water applied by the sprinkler was 0.51 cm day"1 for the first 3 months after
fertilizer application and 0.56 cm day"1 for the next 2 months.  Thus, for
the shallower depths, the calculated water flux within the profiles was
greater than the application rate.  For the deeper depths and longer leaching
time, the water flux within the profile was less than that applied due to
increasing temperatures and greater evaporation.  The overestimation of the
water flux within the profile would result in an overestimation of the NOg
leaching also.

     One explanation for the overestimation of the water flux within the soil
is an overestimation of the soil-water velocity due to anion-exclusion or
immobile water. Rolston and Marino  (1976) determined for packed soil columns
of Yolo soil with a similar water flux that approximately 8% of the water was
not contributing to NO^ transport.  However, if anion exclusion or Immobile
water was the reason for the overestimation of the water flux, a much larger
portion of the water must not be contributing to NOo transport in the field
soil than that of laboratory columns in order to decrease the water flux suf-
ficiently.  The variability of NO^ concentrations at triplicate samplers of
each depth also contributed to the uncertainty in determining the NO^ leach-
ing component  from flux of water and concentration of N07.

     The recovery percentages of fertilizer N determined from concentration
versus depth  (Figure 38) was 50, 120, and 109% for the cropped, manure, and
uncropped treatments, respectively.  This approach more reasonably  estimated
leaching loss for these experiments than did estimations of water flux and
concentration.  Although this approach is not dependent upon knowledge of the
water flux, it is plagued with averaging concentrations across any particular
depth.  Thus, it seems that anion exclusion, immobile water, or other unknown
mechanisms may indeed be causing a  considerable overestimation of the water
flux and the resulting overestimation of  the NO^ leaching in t^ie field
 profiles.

     Potential error in the leaching component from lateral movement of NO^
below the 60-cm deep barrier around each plot exists and would reduce NO^
recovery.  This possible error was  minimized by placing soil-solution samplers
near the center of  each 1-m2 plot.  This  error does not appear to be very
large in relation to the uncertainties in determining  the water flux and the

                                      66

-------
TABLE 14.  PERCENTAGE  RECOVERY  OF FERTILIZER N LEACHED IN THE h = -8 CM PLOTS OF THE WINTER EXPERIMENT
           CALCULATED  BY VARIOUS  WAYS  OF DETERMINING THE SOIL-WATER VELOCITY.  THE MEAN RECOVERY OF ALL
           DEPTHS FOR  EACH  PLOT IS GIVEN IN PARENTHESES
Method of determining
pore-water velocity
                                    Cropped
                                 Recovery

                                 Manure
60  90  120  150  180     60  90  120  150  180
       Uncropped
 60  90  120  150  180
en   From vs of each
    sampler

    From mean vs of all
    samplers at each depth
    (9 samples)

    From mean vs of all
    depths of one plot
    (15 samples)

    From mean vg of all
    depths of 3 plots
    (45 samples)
                            49  97   66   50   50     78 124  133  152  155     113 165  165  206  185
                                     (62)                      (128)                      (167)
                            44  98   61   44   32     89 137  143  148  172     114 150  167   233   246
                                     (56)                      (138)                      (182)
                            50 103   67   51   40
                                     (62)
                            44  91   59   45   36
                                     (55)
                          83 120  131  142  176
                                  (130)
                          89 129  141  153  190
                                  (140)
107 132  154  225  253
        (174)
113 140  163  238  268
        (184)

-------
variability in NO^ concentrations at any particular depth.

Residual Soil N

     The extractable soil N derived from the fertilizer as  a function of soil
depth for the h = -50 cm treatments of the low-temperature  experiment is
given in Figure 39.  Extractable N for the h = -8 cm treatment was negligible.
                                                         -I
              SOIL  EXTRACTABLE FERTILIZER N (>*gNg  soil)
                    0    20   40   60   80   100   120
                120
                                      WINTER
                                      h=-50cm
                                     • Cropped
                                     o Manure
                                     * Uncropped
Figure 39.  Soil extractable N from fertilizer as a function of  soil depth,
            4 months after fertilizer application in the winter  experiment.


The data points are mean concentrations within 15-cm depth increments from
eight samples.  The extractable N  in the h = -50 cm treatments j/as large in
the upper 60 cm of soil due primarily to NO^ not yet leached from the upper
portion of the profile.

     The digestible soil N derived from the fertilizer as a function of soil
depth for the six plots is given in Figure 40.  As with the summer experi-
ments, digestible soil N was greatest near the soil surface due  to plant roots
                                     68

-------
                                                          -I
                  SOIL DIGESTIBLE FERTILIZER N Ug N g  soil)
                 0    20   40    0    20   40   60   80    100
           E
           o
gj 60
a
_j
o
                            T
              90
             ieo
                  _    h=-8cm
   WINTER

  • Cropped
  o Manure
  * Uncropped

h=-50cm
Figure 40.  Soil digestible N from fertilizer  as a function of soil depth,  4
            months  after fertilizer application in the winter experiment.
and microorganisms.  The manure and uncropped plots had negligible plant
growth, so the digestible N was primarily due to microbial immobilization of
fertilizer NO^.

Mass Balance

     Table 15 gives  the N balance for each of the components of the N cycle.
Denitrification was  determined by difference from fertilizer application,
plant uptake, leaching and residual soil N.  Denitrification was determined
directly from N£  and ^0 gas flux at the soil surface and any gaseous loss
below the 60-cm barrier.  The amount of fertilizer applied to each plot is
given by Table 2.

     The total denitrification as determined by the direct method was sub-
stantially less than that determined by difference in the h = -50 cm treat-
ments.  The direct method resulted in 41 to 64 kg N ha"1 less than that
                                     69

-------
TABLE 15.  MASS BALANCE OF FERTILIZER N FOR THE WINTER EXPERIMENT.  THE NUMBERS  IN PARENTHESES WERE
           OBTAINED BY CALCULATING LEACHING FROM CONCENTRATION VERSUS SOIL DEPTH.  THE MINUS  SIGN
           INDICATES GREATER RECOVERY THAN FERTILIZER APPLIED
                                                                       Residual
                                                                       in soil
                                                                          Denitrification
                                 Gaseous loss            Plant
               .N20        N£     below 60 cm Leaching   Uptake  Extractable Digestible Direct Difference
Treatment   (kg N/ha)  (kg N/ha)  (kg N/ha) (kg N/ha) (kg N/ha)  (kg N/ha) (kg N/ha)  (kg N/ha)  (kg N/ha)
Manure,
h = -8 cm
4.2
Manure,
h = -50 cm     3.8
Cropped,
h = -8 cm

Cropped,
h = -50 cm
0.7


0.1
Uncropped,
h = -8 cm   %  0.4

Uncropped,
h = -50 cm     0.2
27.1


26.4


17.6


 1.9


 0.0


 0.0
1.5
                      1.3
0.5
 406
(353)
 168
(150)
118
                    137
                                535
                               (320)
                              186
                      22
 3


39


70


71
                                                    209
                                         37
33      (-62)


32        73


19      (-38)


 2        66


 0      (-28)


 0        48

-------
determined by difference after approximately 4 months.  These differences are
consistent with those measured in the summer experiment for the dry treatment
and are explained by small rates of gaseous loss below the minimum detection
limits for 15N2-  After 4 months, most of the NO^ remained in the upper 45 cm
of soil in the h = -50 cm treatments.  Temperatures gradually increased over
the 4-month period.  Thus, denitrification may have occurred at small rates
since NO, remained in the portion of the profile most conducive to anoxic
development.  The difference in denitrification between the direct and differ-
ence methods for the manure and cropped plots seems consistent with the
difference observed in the summer experiment over comparable time periods of
4 to 5 months.  However, the amount of denitrification as calculated by
difference in the uncropped treatment is much greater than that determined in
either of the uncropped plots of the summer experiment.

     Although total denitrification of 48 kg N ha"-'- in an uncropped plot
maintained at h = -50 cm seems unrealistic compared with the results of the
summer experiment, it has been shown that small changes in soil-air content,
carbon level, and diffusion of oxygen through the soil surface can drastically
change denitrification rates.  A small change in the rate of denitrification
occurring over several weeks can greatly increase total denitrification.

     These results for the h = -50 cm treatments suggest that the sensitivity
of the direct method of measuring the volatile denitrification products should
be increased in order to measure small fluxes over long time periods.  However,
small fluxes over  a long  time may not be as  important  during normal irrigation
or rainfall events due to generally rapid wetting and drying of the upper
soil profile where most of the denitrification occurs.  Research on rates of
denitrification during and after irrigation cycles should provide further
insight into the many interacting factors resulting in denitrification in
field soils.

     The comparison of denitrification by the direct and difference methods
for the h = -8 cm treatments of the winter experiment was difficult due to
recovery of much greater than 100% of the fertilizer by the difference method.
This discrepancy was attributed to the inability to accurately measure leach-
ing losses of NOg from the soil profile.  In addition to considerable vari-
ability in NOg concentrations at individual depths, the determination of the
soil-water flux was. not sufficiently accurate to determine realistic amounts
of leaching in any plot.  Sampling variability of the residual soil N may
also have attributed to failure in obtaining a mass balance.  The most realis-
tic method of determining the leaching component for the winter experiment
was from concentration versus soil depth.  Although this approach does not
depend upon an accurate value for the soil-water flux, it does depend upon
average concentrations at particular depths which may also be quite uncertain
due to enormous spatial variability.

     These results demonstrate the difficulty and potential uncertainty in
determining denitrification by difference.  Although uncertainties also exist
for the direct determination of N20 and ^%2 fl"* from the soil surface,
especially at small fluxes, rates and total denitrification are consistent and
easily measured using "N fertilizer.  The direct method is the only way that
rates of denitrification  from applied fertilizer can be practically measured.

                                      71

-------
                                  REFERENCES

 1.   Biggar, J. W., and D. R. Nielsen.  Spatial variability of the leaching
     characteristics of a field soil.  Water Resources Research, 12:78-84,
     1976.

 2.   Bremner, J. M.  Inorganic forms of nitrogen.  In:  Methods of soil
     analysis.  Part 2., C. A. Black (ed.).  Agronomy 9:1179-1237, 1965.

 3.   Delwiche, C. C., and D. E. Rolston.  Measurement of small nitrous oxide
     concentrations by gas chromatography.  Soil Sci. Soc. Am. J., 40:324-327,
     1976.

 4.   Donigian,Jr., A. S., and N. H. Crawford.  Modeling pesticides and nutri-
     ents in agricultural lands.  EPA-600/2-76-043.  U.S. Environmental
     Protection Agency, Athens, Georgia, 1976.  318 pp.

 5.   Fried, M., K. K. Tanji, and R. M. Van De Pol.  Simplified long term
     concept for  evaluating leaching of nitrogen from agricultural land.  J.
     Environ.  Quality, 5:197-200, 1976.

 6.   Mehran, M.,  and K. K. Tanji.  Computer modeling of nitrogen transforma-
     tions in  soils.  J. Environ.  Quality, 3:391-396, 1974.

 7.   Rolston, D.  E.  Application of gaseous-diffusion theory to measurement
     of denitrification.  In:  Nitrogen and the Environment, D. R. Nielsen
     and J. G. Mac Donald, eds.  Academic Press, New York, N.Y., 1977-
     (in press)

 8.   Rolston, D.  E., M. Fried, and D. A. Goldhamer.  Denitrification measured
     directly  from nitrogen and nitrous oxide gas fluxes.  Soil Sci. Soc. Am.
     J., 40:259-266, 1976.

 9.   Rolston, D.  E., and M. A. Marino.  Simultaneous transport of nitrate and
     gaseous denitrification products in soil.  Soil Sci. Soc. Am. J., 40:860-
     865, 1976.

10.   Rolston, D.  E., and B. D. Brown.  Measurement of soil gaseous diffusion
     coefficients by a transient-state method with a time dependent surface
     condition.   Soil Sci. Soc. Am. J., 41:499-505, 1977.      *

11.   Shaffer, M.  J., R. W. Ribbens, and C. W. Huntley.  Detailed return flow
     salinity and nutrient simulation model, Vol. V. of Prediction of mineral
     quality of irrigation return flow.  Draft rept. to U.S. Environmental
     Protection Agency, Ada, Oklahoma, 1976.  242 pp.


                                      72

-------
12.  Tanji, K. K., and S. K. Gupta.  Computer simulation modeling for nitrogen
     in irrigated croplands.  In:  Nitrogen and the Environment, D. R. Nielsen
     and J. G. Mac Donald, eds.  Academic Press, New York, N.Y., 1977.
     (in press)

13.  van Veen, H.  Behavior  of nitrogen in soil.  A computer simulation
     model.  Ph.D. Thesis, Wageningen, The Netherlands, 1977.
                                      73

-------
                                 PUBLICATIONS

Rolston, D. E., and B. D. Brown.  Measurement of soil gaseous diffusion
    coefficients by a transient-state method with a time dependent surface
    condition.  Soil Sci. Soc. Am. J., 41:499-505, 1977.

Rolston, D. E.  Application of gaseous-diffusion theory to measurement of
    denitrification.     In:  Nitrogen and the environment, D. R. Nielsen and
    J. G. Mac Donald, eds.  Academic Press, New York, N.Y., 1977  (in press)

Rolston, D. E., D. A. Goldhamer, D. L. Hoffman, and D. W. Toy.  Field measured
    flux of volatile denitrification products as influenced by soil-water
    content and organic carbon source.  In:  Proceedings of National Conference
    on Irrigation Return Flow Quality Management, Fort Collins, Colorado,
    1977.  pp. 55-61.
                                       74

-------
                                   TECHNICAL REPORT DATA
                            (Please read Instructions on the reverse before completing)
1. REPORT NO.
  EPA-600/2-77-233
                              2.
                                                           3. RECIPIENT'S ACCESSION NO.
 , TITLE AND SUBTITLE

  Field Measurement of Denitrification
              5. REPORT DATF
                November 1977 issuing  rlate
                                                           6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)

  Dennis E.  Rolston and Francis E.  Broadbent
                                                           8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
  University of California
  Davis,  California 95616
                                                           10. PROGRAM ELEMENT NO.

                                                              1HB617
               11. CONTRACT/GRANT NO.
                 R804259
 12. SPONSORING AGENCY NAME AND ADDRESS
  Robert S. Kerr  Environmental Research Lab.  - Ada, OK
  Office of Research and Development
  U.S. Environmental Protection Agency
  Ada, Oklahoma   74820
               13. TYPE OF REPORT AND PERIOD COVERED
               Final  12/1/75  - 7/31/77
               14. SPONSORING AGENCY CODE
               EPA/600/15
15. SUPPLEMENTARY NOTES
16. ABSTRACT
        Denitrification from a Yolo loam field profile was studied in relation to the
   influence of soil-water  content, organic carbon  source, and temperature.   Field plots
   were intensely instrumented with soil atmosphere samplers, soil solution  samplers,
   and tensiometers.  The two soil-water pressure treatments were -0.01 and  -0.05 bars
   in the topsoil.  Three levels of soil carbon were studied by evaluating plots cropped
   with ryegrass, uncropped plots, and plots amended with manure.  Experiments were
   conducted at soil temperatures of 8 and 23°C.  Fertilizer was applied as  KN03 en-
   riched with 1%.  The flux of volatile gases at  the soil surface was measured from
   the accumulation of N20  and 15N2 beneath an air-tight cover placed over the soil
   surface for 1 or 2 hours per day.  Denitrification at 23°C ranged from 73% of the
   fertilizer N for the manure treatment at -0.01 bar to 1% for the uncropped treatment
   at -0.05 bar.  At 8°C, denitrification ranged from 11% for the manure treatment at
   -0.01 bar to zero for the uncropped plots.  The  N20 flux at the soil surface varied
   between 5 and 26% of total denitrification.
17.
                                KEY WORDS AND DOCUMENT ANALYSIS
                  DESCRIPTORS
                                              b.lDENTIFIERS/OPEN ENDED TERMS
                            c.  COSATI Field/Group
   Nitrogen cycle
   Nitrogen isotopes
   Nitrogen oxide  (N20)
   Soil water
   Fertilizer
   Irrigation
  Denitrification
  Irrigation Return Flow
  Nitrate Leaching
  Gas Fluxes
    02/A,C
18. DISTRIBUTION STATEMENT

    RELEASE TO PUBLIC
 19. SECURITY CLASS (ThisReport)
   Unclassified
21. NO. OF PAGES
    91
                                              20. SECURITY. CLASS (This page!
                                               Unclassified
                                                                         22. PRICE
EPA Form 2220-1 (9-73)
75
                                                                     ft U.S. GOVBtHMEHTPRHraiG OFFICE 1978— 757-140/6628

-------