NASA/TMm2000-209891, Vol. 233

Technical Report Series on the

Boreal Ecosystem-Atmosphere Study (BOREAS)

Forrest G. Hall and Sara K. Conrad, Editors

Volume 233

BOREAS TGB-6 Soil Methane

Oxidation and Production from

NSA BP and Fen Sites

Bruce Deck and Martin Wahlen

UCSD , Scripps Institute of Oceanography, LaJolla

National Aeronautics and

Space Administration

Goddard Space Flight Center

Greenbelt, Maryland 20771

November 2000

https://ntrs.nasa.gov/search.jsp?R=20010022986 2018-05-14T19:03:18+00:00Z
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NASA/TMm2000-209891, Vol. 233

Technical Report Series on the

Boreal Ecosystem-Atmosphere Study (BOREAS)

Forrest G. Hall and Sara K. Conrad, Editors

Volume 233

BOREAS TGB-6 Soil Methane

Oxidation and Production from

NSA BP and Fen Sites

Bruce Deck and Martin Wahlen

UCSD , Scripps Institute of Oceanography, LaJolla

National Aeronautics and

Space Administration

Goddard Space Flight Center

Greenbelt, Maryland 20771

November 2000
NASA Center for AeroSpace Information

7121 Standard Drive

Hanover, MD 21076-1320

Price Code: A17

Available from:

National Technical Information Service

5285 Port Royal Road

Springfield, VA 22161

Price Code: A10
BOREAS TGB-6 Soil Methane Oxidation and Production from NSA BP

and Fen Sites

Bruce Deck, Martin Wahlen

Summary

The BOREAS TGB-6 team collected soil methane measurements at several sites in the SSA and NSA.

This data set contains soil methane consumption (bacterial CH4 oxidation) and associated 13C

fractionation effects in samples that were collected at various sites in 1994 and 1996 from enclosures

(chambers). Methane 13C data in soil gas samples from the NSA YJP and OJP sites for 1994 and 1996

are also given. Additional data on the isotopic composition of methane (carbon and hydrogen isotopes)

produced in the NSA beaver ponds and fen bog in 1993 and 1994 are given as well. The data are

stored in tabular ASCII files.

Table of Contents

1) Data Set Overview

2) Investigator(s)

3) Theory of Measurements

4) Equipment

5) Data Acquisition Methods

6) Observations

7) Data Description

8) Data Organization

9) Data Manipulations

10) Errors

11) Notes

12) Application of the Data Set

13) Future Modifications and Plans

14) Software

15) Data Access

16) Output Products and Availability

17) References

18) Glossary of Terms

19) List of Acronyms

20) Document Information

1. Data Set Overview

1.1 Data Set Identification

BOREAS TGB-06 Soil Methane Oxidation and Production from NSA BP and Fen Sites

1.2 Data Set Introduction

Destruction of methane in the troposphere by chemical reaction with OH- is the primary sink for

this gas. As much as 10% (Born et al., 1990) of the total destruction of atmospheric methane may be

due, however, to bacterial oxidation on relatively dry soils. In determining the global isotopic budget

for methane, the isotopic fractionation and enrichment due to soil oxidation must be considered in

comparison to that resulting from the reaction with the OH- in the troposphere. Boreal forest soils have

a large aerial extent, and adequate measures of the fractionation occurring in the methane oxidation

process must be determined for inclusion in any global budget.

Page 1
Methaneemissionsfrom pondsandfensareasignificantsourcein themethanebudgetof the

borealregion.An initial studyontheisotopiccompositionof thismethanesourceandtheisotopic

compositionin relationto oxidationof methaneatthesedimentsurfaceof thepondsorfenwas

conducted.Informationontheisotopiccompositionof themethaneis importantin bothunderstanding

thebiogeochemistryof thesystemanddeterminingtheregionalandglobalmethaneisotopebudget.

Soilmethaneoxidationis anetconsumptionof methanefrom theoverlyingatmosphereby bacterial

processesin aerobicsoils,with anaccompanyingisotopefractionation.Theflux will beafunctionof

themicrobiologicalactivityof themethanotrophs,andin dependentonthemicrobiology,soil

character,temperature,andmoisturecontent.

Theisotopiccompositionof methaneemittedby saturatedanoxicsedimentisdependentonthe

sedimentcompositionandgeochemistry,butit isinfluencedby oxidation,whichis inpartafunction

of rootedplantactivity.Thedependenceof theisotopiccompositiononrootedplantactivitiesisnot

well knownandwill dependontheplanttype,sedimentemperature,andnumerousothervariables.

Air samplesindicatingmethaneconsumptionwereobtainedfrom sealedenclosuresplacedoversoil

sitesfor severalhours.Soil gassamplestakenby subsurfaceprobeswereanalyzedfortheisotopic

carboncompositionin methane.Gassamplesof varyingmethaneconcentrationfrombubblesand

equilibratedwatersamplestakenfrom beaverpondsandfenswereanalyzedfor thecarbonand

hydrogenisotopecomposition.

1.3 Objective/Purpose

The objective of this study was to determine the isotopic composition of methane released from the

BOReal Ecosystem-Atmosphere Study (BOREAS) Northern Study Area (NSA) Beaver Pond and Fen

sites.

1.4 Summary of Parameters and Variables

The main variables measured in this study were soil depth, CH4 concentration, 13C isotope

concentration, and H isotope concentration.

1.5 Discussion

Dislodged bubbles from anoxic sediments from five beaver ponds were sampled in 1993, and

bubble and sediment/water samples from the NSA Tower Beaver Pond (TBP) were taken in 1994 to

determine the carbon and hydrogen isotope values of methane emitted from these sites.

Gas samples from flux enclosures (chambers) over the soil and subsurface soil gas samples were

taken and returned to the lab for analysis. Data were collected once in 1994 and at four time periods in

1996 from two sites near the towers at the Old Jack Pine (OJP) and Young Jack Pine (YJP) sites in the

NSA. A set of chamber measurements from the Southern Study Area (SSA) OJP and YJP sites along

with soil gas samples was obtained in 1994. While some concentration measurements were made in

the field in conjunction with other investigators, these data sets consist of methane concentration and

carbon isotope (13C/12 C) ratios for each analyzed sample.

The sites sampled in 1996 duplicated the NSA sites that were sampled in 1994. At OJP, the Crill

(Trace Gas Biogeochemistry [TGB]-01) Lichen chamber #4 and the TGB-01 Moss chamber #7 were

sampled. For the YJP, Moore (TGB-05) chambers #4 and #6 were sampled. Two-liter samples were

taken from each of the chambers, drawn over a 1-min sampling period, at times of 0.75 to 7 hr

depending on estimated methane uptake. The chambers at the OJP were approximately 20 m apart,

while those of the YJP were within 5 m of each other. Soil probe samples were taken at shallow

depths in the immediate (1 m) vicinity of the chambers. Samples were drawn slowly (5 min for 2

liters) to avoid contamination from gas sucked in from intermediate levels. A summary description of

the data collection is given in Section 6.2.

1.6 Related Data Sets

BOREAS TGB-01 Soil CH4 and CO2 Profile Data from NSA Tower Sites

BOREAS TGB-01 CH4 and CO2 Chamber Flux Data

BOREAS TGB-01 CH4 Concentration and Flux Data from NSA Tower Sites

BOREAS TGB-03 CH4 and CO2 Chamber Flux Data over NSA Upland Sites

BOREAS TGB-03 Soil CO2 and CH4 Profile Data over the NSA

Page 2
2. Investigator(s)

2.1 Investigator(s) Name and Title

Dr. Martin Wahlen

Professor of Physics, PI

Dr. Bruce Deck

Research Specialist, Assoc. PI

2.2 Title of Investigation

Isotopic Composition of Methane Produced and Consumed in Boreal Ecosystems

2.3 Contact Information

Contact 1:

Bruce Deck

UCSD, Scripps Institution of Oceanography

La Jolla, CA, 92093-0220,

(619) 534-6248

(619) 534-0967 (fax)

bdeck@ UCSD.edu

Contact 2:

Jeffrey A. Newcomer

Raytheon ITSS

Code 923

NASA GSFC

Greenbelt, MD 20771

(301) 286-7858

(301) 286-0239 (fax)

Jeffrey.Newcomer@ gsfc.nasa.gov

3. Theory of Measurements

In order to determine the effect the land surface has on the overlying atmospheric concentration, the

flux of any gas through the various pathways into or out of the soil sediment or biota must be

determined. In the case of methane in boreal forests, the interaction between the atmosphere and forest

soils is direct and not mediated to any major extent by trees or woody plants. Thus, the flux of

methane into or out of the soil can be determined, and the isotopic fractionation examined, by placing

closed chambers on the surface for a period of time. In addition, samples of soil gas taken below the

soil surface will provide information on the rate of methane consumption and the isotopic fractionation.

In the case of ponds or bogs, funnels at the water surface or monitoring of the overlying water can be

used to determine sediment gas exchange. In either situation, changes in concentration and isotopic

composition of methane over time will indicate the effect the soil or sediment will have on the

overlying atmosphere (source/sink).

The basic problem with this sampling approach is to avoid having chamber placement cause

perturbations of the naturally occurring gas exchange either through biological or physical changes in

the system. To this end, the temperature, humidity, air circulation, light, and other parameters inside

the chamber can be controlled to mimic those outside the chamber. In many cases, controls on chamber

parameters are not adequate for extended periods of time and the best sampling strategy is to leave the

chambers enclosed for the minimum consumption of methane to ensure the necessary accuracy in the

determinations. For concentration changes in methane, the high degree of precision attainable allows

Page 3
for short(0.3-1hr)maximumenclosuretimes.In thedeterminationof isotopicmethanecomposition,

thetimesnecessaryfor measurablechangesto bedeterminedwithreasonableprecisionin theanalysis

areafactorof 2to 4 longer.In addition,caremustbetakenatall timesto ensurethatthesamplingand

storageproceduresdonot introduceadditionalerrors.Finally, it mustberealizedthatchamber,soil

probesamples,and/oranydiscreetmeasurementsat afinite numberof sitescanonly approximatethe

estimatesof actualaveragesoil-atmosphereinteractionatanyonesite.

Samplestakenfrompondsandfensshowanetflux of methaneintotheatmosphere.The

investigationsstartedherewerenotmeanttoquantifythenetflux, butto allowadeterminationof the

isotopiccompositionof theemittedmethane.

Becauseof thelargeamountof timerequiredfor theprocessingof theisotopesamples,alimit on

thenumberof samplestakenin anyfield seasonwasnecessary.Thefewerthenumberof samplesor

thegreaterthevariabilityin sitecharacteristics,thepoorerthedataapproximation.Thelimitationson

thenumberof samplestakenimposedby isotopicanalysisproceduresaresignificantin thisstudy,but

arebalancedin partby theuniformity in microbialbiochemistry,whichdrivesthemethaneproduction

andconsumptionin all areas.

4. Equipment

4.1 Sensor/Instrument Description

• Chambers (funnels)/Soil Probes

• Sampling Flasks/Manifold

• Gas Chromatography Analysis

• Separation Chromatography/Combustion

• Mass Spectrometric Analysis

4.1.1 Collection Environment

Samples were taken at specific sampling periods, the majority from sites at tower locations. Sites

for 1993 were chosen to determine (preliminary) methane production and included the NSA Fen site

and several beaver ponds. It was proposed that 1994 data be taken at different times to cover a

seasonal cycle, but only samples from late August-September were collected. These included chamber

gas and soil gas sampling at the SSA YJP and OJP sites 04-Aug and NSA YJP and OJP sites

23-24-Aug. Sets of methane production samples from the TBP site were taken 25-26-Aug, 31-Aug,

and 09-Sep-1994. Samples for 1996 were taken in the NSA only from the YJP and OJP sites at four

sampling times, 03-Jun, 26-Jun, 02-03 Aug, and 08-11-Sep. Most samples were taken in good

weather. Samples taken on 03-Jun-1996 were made following several days of rain and while the

ground was frozen below approximately 10 to 15 cm. Also, the final samples on 11-Sep-1996, from

the NSA OJP were made following a heavy cold rain period.

4.1.2 Source/Platform

Samples from the wet production areas were taken from the shore or walkways. Soil flux

measurements were made utilizing fixed collars left in the soil from year to year. Tube and sample

probes were inserted into the soils for each soil gas collection.

4.1.3 Source/Platform Mission Objectives

The purpose of the collars was to support the chamber and allow measurements to be made.

4.1.4 Key Variables

Isotopic composition of methane (carbon, 13CH4 and hydrogen, CH3D isotopes) in samples from

sediment production, and carbon isotope fractio nation in the methane consumption by bacteria in

soils.

Page 4
4.1.5 Principles of Operation

Samples were taken in the field and returned to Scripps Institute of Oceanography (SIO) for

methane concentration analysis, after which the methane was quantitatively separated from the bulk air

sample. Following combustion with pure oxygen, the methane sample was separated into fractions for

carbon and (if possible) hydrogen isotope analysis on a high-precision duel inlet isotope ratio mass

spectrometer (VG Prism II).

4.1.6 Sensor/Instrument Measurement Geometry

Discrete sample sites was selected; there were no field sensors as such. The actual nature of the soil

surface or pond sites, with relationship to rock, litter cover, and vegetation, was of importance in

determining sampling sites, and soil depth in conjunction with soil probe measurements. Samples were

analyzed with a GOW-MAC flame ionization gas chromatograph (GC) and a VG Prism II isotope ratio

mass spectrometer.

4.1.7 Manufacturer of Sensor/Instrument

Chambers as made by Crill TGB-01, Moore TGB-03. Concentration analysis GOW-MAC flame

ionization GC (GOW-MAC Inst. Co. Lehigh Valley, PA 18002). Separation and methane combustion

on custom high vacuum lines (M. Wahlen). Mass spectrometric determinations on a VG Prism II

isotope ratio mass spectrometer (Micro Mass, Beverly, MA 01915).

4.2 Calibration

4.2.1 Specifications

Calibrations were performed using methane standard concentration determinations and isotopic

analysis conducted at SIO during the lab analysis. Methane determination on field samples was made

with a manometric manifold inlet loop on a flame ionization GC system with a 2-meter, 1/8-inch i.d.,

60/80 mesh Poropack Q column, using nitrogen carrier gas. Calibration was performed with a set of

five working standards covering the range of 0.8 to 2.8 ppm previously calibrated against

SIO/Commonwealth Scientific and Industrial Research Organization (CSIRO) international standards

(R. Weiss) to better than 0.2%. Overall precision and accuracy of the system in this range was

approximately 0.5%. Calibration against the BOREAS working methane standards (0.9 and 2.0 ppbv)

also showed this agreement within experimental errors. Samples with higher than 3-ppm methane

concentration were diluted and/or injected at reduced pressure and calibrated against volumetric

standards up to 10% methane. Uncertainty for these samples was approximately 5%.

For the 2-liter soil chamber and probe sample runs on the extraction line, pure nitrogen blank

determinations, synthetic air standards, and calibrated isotopic methane standards passed through the

lines and combustion systems during development provided the calibration of the system. For

calibration during normal run, clean SIO air was used as a standard, with 12/13C methane values of

-47.2 permil Pee Dee Belemnite (PDB). Approximately 1 standard per 4 samples was run. Based on

replicate SIO air standards (2 liters) and replicate 2-liter samples taken in the field, the uncertainty in

analysis was found to be primarily dependent on the uncertainty introduced in the separation

procedure. This was determined to be approximately +/- 1 permil. The mass spectrometric

determination error was far smaller than this value and is included in the +/- 1 permil value. Actual

runs of the mass spectrometer using the working standard (-43.40 +/- 0.05 permil), measured in the

size range of the samples, yielded a running precision of better than +/- 0.1 permil.

For samples of higher methane concentration from production sites, the variability for the sample

size processed again limited the error to approximately +/- 2 permil (PDB) for carbon and +/- 5 permil

Standard Measure Ocean Water (SMOW) for hydrogen isotopic composition.

4.2.1.1 Tolerance

Samples with a methane concentration less than 0.75 pl methane/sample were not reliable for

carbon isotopes measurements. Samples with less then 250 pl methane/sample did not produce reliable

hydrogen isotope results.

Page 5
4.2.2 Frequency of Calibration

Individual GC systems and the mass spectrometer were calibrated daily using additional standards

in the middle of the GC runs. Separation and combustion procedures were calibrated biweekly or more

often if necessary.

4.2.3 Other Calibration Information

The mass spectrometric standards are directly traceable to the National Institute of Standards

Technology (NIST) primary isotope standards: National Bureau of Standards (NBS)-19, NBS-16,

and NBS-17 for 13C, SMOW, Standard Light Antarctic Precipitation (SLAP), Greenland Ice Sheet

Precipitation (GISP) for D. Methane concentrations were measured against SIO/CSIRO (R. Weiss)

substandards.

5. Data Acquisition Methods

Soil gas exchange at the NSA was measured using either aluminum enclosures at OJP or plastic

enclosures at YJP of 0.4 m2 and 0.075 m3 or 0.05 m2 and 0.018 m3, respectively. The chambers

rested on skirts permanently placed 10 cm deep in the soil in 1993 or 1994 and were equipped with a

water seal to prevent air leakage. Once the chambers were in place, the air was mixed approximately

every 5 minutes either with a fan or by rapidly drawing and returning 50 cc of air several times with a

syringe. After a suitable time period (0.75 to 2 hr, in most cases), air samples were withdrawn through

a restricting manifold, to prevent a sudden vacuum in the chamber, into 2-liter evacuated glass flasks

with high vacuum valves. After the sampling manifold was attached to the sample flask, it was

evacuated to remove extra air and to check for leaks, before the sample was taken. Subsurface gas

samples were taken using a pointed 3/8-inch steel probe inside of which was a 1/8-inch tube connected

to a nose chamber open to the soil through several small holes. This probe was pushed into the soil to

the desired sampling depth, the manifold was attached and evacuated, and the sample flask (as above)

was filled. For the subsurface samples, the manifold was set to allow approximately 3 minutes for the

flask to fill. For a few of the 1994 soil gas samples, horizontal 1/8-inch sample tubes (TGB-03)

previously placed at several depths in the soil were used following the same procedures.

Samples taken for methane production from submerged sediments were primarily obtained by

capturing bubbles that had either been released over time or were dislodged by motion from the surface

of the sediment. The gas from these samples (20 to 100 cc) was transferred to evacuated serum bottles

with rubber septum caps. Several sets of samples equilibrated with helium gas from water samples

above the sediments or piezometers in the sediments were also collected.

Methane concentration analyses were performed with a flame ionization GC equipped with a 2-m,

1/8-inch Porapack Q (60-80 mesh) column using nitrogen as a carrier gas. Replicate peak height

measurements from a chart recorder were used to quantify the results. The inlet line to the sample loop

was equipped with a precision pressure gauge calibrated to 0.5%. Standards at 959, 1649, and 2722

ppb were run at several pressures, several times during sample analyses, to allow correction for any

deviation in linearity as a function of pressure or concentration.

Separation and combustion of the methane in the chamber and soil gas samples to CO2 for the

mass spectrometric analysis was performed on an extraction line specifically designed for this type of

sample. The 2-liter (air) sample was passed at 50 cc/min or less through two liquid nitrogen

(LNz)-cooled traps to remove water, CO2, and other condensable gases, and then through a trap

containing several grams of 10 mesh activated charcoal. This charcoal column retains 500-800 cc of air

(N2, O2) at any time, with methane and other trace components totally retained. After the entire sample

was processed (down to <10 torr) and pumped at vacuum for 15 minutes, the charcoal was warmed

from LN2 temperature to approximately -150 °C over a period of 5 minutes. During this time, the

majority of the air retained on the charcoal was allowed to bleed off at a carefully controlled rate, while

the methane was retained. Then the charcoal column was immersed in a -90 °C acetone bath and the air

allowed to continue to bleed off at a controlled rate, again retaining the methane. A low flow of helium

is passed through the column for 1 min to dislodge additional air. The gas on the charcoal was then

Page 6
transferredto a smallercharcoalcolumn(approx.1g)in LN2by first warmingit toroomtemperature

for 10minutesandthenheatingit 240°Cfor 10minutes.

In asimilarmanner,thesecondcharcoalcolumnwaswarmedandagainanyremainingexcessair

wasremoved.Helium waspassedthroughthefirst columnontothesecondto maximizethetransfer.

At thisstage,1to 2cc of totalgascontainingapproximately3.7microliters(orless)of methane

(correspondingto themethanein 2 liters atambientair)remained.This samplewastransferredto an

inlet loopof athermalconductivityGCfittedwith aspecialow flow MS5acolumnusinghelium

carriergas.Thecolumnanddetectorweremodifiedsothatanearlycompleteseparationof methane

from nitrogencouldbeobtainedwith anelutiontimeof 25minutesatroomtemperature.Themethane

elutingfrom thecolumnwascapturedona shortMS5acolumnandtransferred,following removalof

theresidualhelium,with anMS5afingerto thecombustionsystem.Thecombustionof themethane

wasdoneby condensingthemethanesampleat LN2temperatureontotwo aluminumoxidepellets

coatedwith platinum(Alfa #89106),andthencondensingatenfoldexcessof pureoxygenontothe

pellets,followedby acombustionof themixtureat 650°C for 1hour.TheCO2wasthenseparated

from thewaterproducedin atrapat-70°Candsealedin a6-mmglassbreaktubeforlatermass

spectrometricanalysis.Extensiveworkwasnecessaryto initially cleanthepellets,andthenkeepthem

clean,resultingin alow CO2blankfor thisstep.Sampleswith methaneconcentrationhigherthan10

ppmrequiredproportionatelysmallerthan2-liter air samplestobeanalyzed.Samplesin thepercent

methanerangewereableto beprocessedusingsimilarGCstepsandcombustion;however,when

morethen250]al of water were generated, the water was saved for D isotope analysis.

6. Observations

6.1 Data Notes

None given.

6.2 Field Notes

Sampling NSA 1993

24-Aug-93 Bubbles from dislodgment Fen Tower walkways i, 2, and 3.

25-Aug-93 Bubbles, Gilliam Rd. beaver pond (14.5 km N of 391) west shore.

26-Aug-93 Bubbles, OBS beaver ponds #3, 4, and i, TBP, south shore. All samples

from near shore,water depths 10-50 cm, various degrees of plants and

algal growth.

Sampling SSA 1994

4-Aug-94 YJP Tower Flux (TF)-04 chambers A, B, and D soil probes A/B 15 cm,

cm. OJP TF-4chambers G, H, and J probes G/H 15 cm, 20 cm. Samples

taken by R. Strieglis TF-04group, chamber times long (12+ hr) .

2O

Sampling NSA 1994

24-Aug-94 OJP, three chambers at TGB-01 lichen site, no collars, three soil gas

probes. YJP,three chambers TGB-03 with collars #4, 5, and 6, five

soil probes 1-2 meters southof TBG-03 soil tubes.

25-Aug-94 TBP samples from funnels, piezometers, water profile. BOREAS AES

2-ppm and 0.9-ppmstandards sampled.

26-Aug-94 YJP TGB-03 soil tubes site ic and 3a sampled at 20 and 40 cm depth.

Ambient air sampledeach day.

31-Aug-94 TBP samples, gross bubbles, funnel, piezometer, and water samples.

through Taken by A. DoveTGB-03.

13-Sep-94

Page 7
Sampling NSA 1996

29-May-96 Ground frozen below 15 cm, surface soil <10 °C with a high

to degree of watersaturation. One sample taken at each chamber OJP 4 and

3-Jun-96 7, YJP 4 and 6, OJP at approximately4.5-hr sampling time, YJP at

approximately 6 hr. No soil probe samples.

28 and One sample collected from each chamber (above) over 1.5 to 2 hr. No

29-Jun-96 soil gas samples.

l-Aug-96 General surface temperatures approximately 25 °C, weather good

to and dry. Duplicatesamples at 45 and 90 min for both OJP chambers,

4-Aug-96 four soil probe samples, two neareach chamber at approximately 20 cm

depth. Sampling the YJP site chambers was identicalexcept for

collection times of 1 and 2 hr.

8-Sep-96 OJP sampled 8-Sep, light showers two days prior, chamber samples

to collected in duplicateat 1 and 2 hr. Soil samples, two near each

12-Sep-96 chamber at approximately 15-cm depth.Cold heavy rain for two days.

OJP samples taken on ll-Sep, temperature ⁢9 °C.Single samples

at 1 hr, duplicate samples collected each chamber 1 and 2 hr. Twosoil

probe samples taken 15 and 17-cm depth. Two ambient air samples

collected.

7. Data Description

7.1 Spatial Characteristics

7.1.1 Spatial Coverage

The data for 1993 were sampled as a preliminary examination of production from the available

pond and fen locations. This set of analyses (dislodged bubbles) was not repeated in subsequent years.

The data for 1994 and 1996 were collected from specific soil sites at the tower locations in the NSA

and SSA, OJP and YJP, and the NSA. The North American Datum of 1983 (NAD83) coordinates for

the sites are:

NSA Tower Fen (55.91481N, 98.42072W)

NSA Beaver Pond Gillam Road 14.5-km N of Highway 391 on Gillam Road

NSA OBS Beaver ponds (55.88007N, 98.48139W)

NSA TBP (55 84225N, 98.02747W)

NSA OJP (55 92847N, 98.62396W)

NSA YJP (55 89575N, 98.28706W)

NSA TBP (55 84225N, 98.02747W)

SSA OJP (53 91634N, I04.69203W)

SSA YJP (53 87581N, I04.64529W)

7.1.2 Spatial Coverage Map

Not available.

7.1.3 Spatial Resolution

These data represent point measurements from the 2-m x 2-m sample areas.

7.1.4 Projection

Not applicable.

7.1.5 Grid Description

Not applicable.

7.2 Temporal Characteristics

Page 8
7.2.1 Temporal Coverage

Data were collected over the SSA sites in August 1994 only. Data were collected over the NSA

sites at various times in 1993, 1994, and 1996.

7.2.2 Temporal Coverage Map

Site Name Date

NSA Tower Fen

NSA Beaver Pond

Gillam Road

NSA-TBP

SSA-OJP

SSA-YJP

NSA-OJP

NSA YJP

24-Aug-93

25-Aug-93

26-Aug-93

31-Aug-94

13-Aug-94

25-Aug-94

4-Aug-94

4-Aug-94

23-Aug-94

30-May-96

2-Aug-96

ll-Sep-96

28-Jun-96

24-Aug-94

26-Aug-94

3-Jun-96

3-Aug-96

8-Sep-96

28-Jun-96

7.2.3 Temporal Resolution

Individual samples were taken over several hours of field time at each site. Production samples

from funnels and piezometers represent collection or equilibration over several days.

7.3 Data Characteristics

7.3.1 Parameter/Variable

The parameters contained in the data files on the CD-ROM are:

Column Name

SITE NAME

SUB SITE

DATE OBS

SAMPLE TYPE

SAMPLE LOCN

MEASUREMENT DURATION

SOIL DEPTH

CH4 CONC

ISOTOPE 13C

ISOTOPE H

CRTFCN CODE

REVISION DATE

Page 9
7.3.2 Variable Description/Definition

The descriptions of the parameters contained in the data files on the CD-ROM are:

Column Name Description

SITE NAME

SUB SITE

DATE OBS

SAMPLE TYPE

SAMPLE LOCN

MEASUREMENT DURATION

SOIL DEPTH

CH4 CONC

ISOTOPE 13C

ISOTOPE H

CRTFCN CODE

REVISION DATE

The identifier assigned to the site by BOREAS, in

the format SSS-TTT-CCCCC, where SSS identifies

the portion of the study area: NSA, SSA, REG,

TRN, and TTT identifies the cover type for the

site, 999 if unknown, and CCCCC is the identifier

for site, exactly what it means will vary with

site type.

The identifier assigned to the sub-site by

BOREAS, in the format GGGGG-IIIII, where GGGGG is

the group associated with the sub-site

instrument, e.g. HYD06 or STAFF, and IIIII is the

identifier for sub-site, often this will refer to

an instrument.

The date on which the data were collected.

Type of medium for the sample.

Specific location where the sample was measured.

Length of time for the measurement.

The depth below the soil surface at which the

measurement was taken.

CH4 concentration.

Carbon 13/12 isotope ratio.

Hydrogen D/H isotope value of methane.

The BOREAS certification level of the data.

Examples are CPI (Checked by PI), CGR (Certified

by Group), PRE (Preliminary), and CPI-??? (CPI

but questionable).

The most recent date when the information in the

referenced data base table record was revised.

7.3.3 Unit of Measurement

The measurement units for the parameters contained in the data files on the CD-ROM are:

Column Name Units

SITE NAME [none]

SUB SITE [none]

DATE OBS [DD-MON-YY]

SAMPLE TYPE [none]

SAMPLE LOCN [none]

MEASUREMENT DURATION [minutes]

SOIL DEPTH [millimeters]

CH4 CONC [parts per million]

ISOTOPE 13C [permil]

ISOTOPE H [permil]

CRTFCN CODE [none]

REVISION DATE [DD-MON-YY]

Page 10
7.3.4 Data Source

The sources of the parameter values contained in the data files on the CD-ROM are:

Column Name Data Source

SITE NAME Investigator

SUB SITE Investigator

DATE OBS Investigator

SAMPLE TYPE Investigator

SAMPLE LOCN Investigator

MEASUREMENT DURATION Investigator

SOIL DEPTH Investigator

CH4 CONC gas chromatograph

ISOTOPE 13C VG Prism II

ISOTOPE H VG Prism II

CRTFCN CODE Assigned by BORIS

REVISION DATE Assigned by BORIS

7.3.5 Data Range

The following table gives information about the parameter values found in the data files on the

CD-ROM.

Minimum Maximum Missng Unrel Below Data

Data Data Data Data Detect Not

Column Name Value Value Value Value Limit Cllctd

SITE NAME NSA-999-T06GR

SUB SITE TGB06-CON01

DATE OBS 24-AUG-93

SAMPLE TYPE N/A

SAMPLE LOCN N/A

MEASUREMENT DURATION 0

m

SOIL DEPTH 0

CH4 CONC -197.98

ISOTOPE 13C -68.3

ISOTOPE H -384

CRTFCN CODE CPI

REVISION DATE 12-JUN-97

SSA-YJP-FLXTR None None None None

TGB06-CON01 None None None None

II-SEP-96 None None None None

N/A None None None None

N/A None None None None

960 None None None None

i0000 None None None None

3.3 None None None None

-30.8 -999 None None None

-224 -999 None None Blank

CPI None None None None

12-JUN-97 None None None None

Minimum Data Value -- The minimum value found in the column.

Maximum Data Value -- The maximum value found in the column.

Missng Data Value -- The value that indicates missing data. This is used to

indicate that an attempt was made to determine the

parameter value, but the attempt was unsuccessful.

Unrel Data Value -- The value that indicates unreliable data. This is used

to indicate an attempt was made to determine the

parameter value, but the value was deemed to be

unreliable by the analysis personnel.

Below Detect Limit -- The value that indicates parameter values below the

instruments detection limits. This is used to

indicate that an attempt was made to determine the

parameter value, but the analysis personnel determined

that the parameter value was below the detection

limit of the instrumentation.

Data Not Cllctd -- This value indicates that no attempt was made to

Page 11
determine the parameter value. This usually

indicates that BORIS combined several similar but

not identical data sets into the same data base table

measure that parameter.

Blank -- Indicates that blank spaces are used to denote that type of value.

N/A -- Indicates that the value is not applicable to the respective column.

None -- Indicates that no values of that sort were found in the column.

7.4 Sample Data Record

The following are wrapped versions of sample data records from a selected file on the CD-ROM:

SITE NAME,SUB SITE,DATE OBS,SAMPLE TYPE,SAMPLE LOCN,MEASUREMENT DURATION,

SOIL DEPTH,CH4 CONC, ISOTOPE 13C, ISOTOPE H,CRTFCN CODE,REVISION DATE

'NSA-OJP-FLXTR', 'TGBO6-CONOI',24-AUG-94, 'chamber flux', 'OJP 4-1',82,0.0,1.838,

-46.1,, 'CPI',I2-JUN-97

'NSA-OJP-FLXTR', 'TGBO6-CONOI',24-AUG-94, 'chamber flux', 'OJP 4-1',147,0.0,1.798,

-46.7,, 'CPI',I2-JUN-97

8. Data Organization

8.1 Data Granularity

The smallest unit of data tracked by the BOREAS Information System (BORIS) is the

measurements made for a given site on a given day.

8.2 Data Format(s)

The Compact Disk-Read-Only Memory (CD-ROM) files contain American Standard Code for

Information Interchange (ASCII) numerical and character fields of varying length separated by

commas. The character fields are enclosed with single apostrophe marks. There are no spaces between

the fields.

Each data file on the CD-ROM has four header lines of Hyper-Text Markup Language (HTML)

code at the top. When viewed with a Web browser, this code displays header information (data set

title, location, date, acknowledgments, etc.) and a series of HTML links to associated data files and

related data sets. Line 5 of each data file is a list of the column names, and line 6 and following lines

contain the actual data.

9. Data Manipulations

9.1 Formulae

None.

9.1.1 Derivation Techniques and Algorithms

None.

9.2 Data Processing Sequence

The data, after calibration of the measurement, were not modified, except for the Craig correction

applied by the mass spectrometer data calculation of d 13C.

9.2.1 Processing Steps

None.

Page 12
9.2.2 Processing Changes

None.

9.3 Calculations

9.3.1 Special Corrections/Adjustments

None.

9.3.2 Calculated Variables

None.

9.4 Graphs and Plots

None.

10. Errors

10.1 Sources of Error

Data quality appears to be high for most of the data set, although the chambers from the 1994 SSA

and May/June 1996 were left closed far longer than the normal 2 hours. Low consumption of methane

in the soils resulted in final concentrations of methane in the chambers somewhat higher than desired.

The 1994 OJP samples were not tightly sealed to the ground and probably exchanged with the outside

air, resulting in low apparent consumption. The duplicate samples in 1996 were used to determine the

analytical error. Soil methane flux measurements using these data are lower than the values determined

by other groups that sampled for shorter periods of time.

Errors in these data are a combination of sample transport, storage, processing, and analyses. The

greatest uncertainty in any of the data results from the synoptic nature of the discrete sampling.

Samples taken in proximity to one another varied widely in their data values, often with results

differing by more than any combination of experimental errors would allow. In this study, sample

storage, processing, and analysis procedures were checked before and during the field work using

standards and blank determinations, and the associated error was determined. Errors introduced during

sampling could be inferred from several conditions, such as lack of good seals on chambers or long

chamber deployments, which did not reproduce the normal planned conditions of sampling. Where

there are indications that this happened, it has been noted. Analysis of some of the data, such as the

methane production samples, shows an enormous range of values, in part because they were sampled

in several different ways at many different sites. Also, questions such as dislodged bubbles

representing the release of methane are not considered. Lacking a more complete data set describing

many additional parameters influencing methane production/consumption, analysis of even the error

from this type of sample is difficult.

10.2 Quality Assessment

10.2.1 Data Validation by Source

Prior studies and controls introduced during this work show that the sample storage, concentration

analysis, and the mass spectrometric determinations introduced relatively small errors into the

determinations. The separation and combustion procedure were the most important steps in the error

determination and accounted for the majority of error in the analysis.

10.2.2 Confidence Level/Accuracy Judgment

For all the production samples, the error in analysis is +/- 2 permil vs. PDB for d 13C in carbon

and +/- 5 permil in dD in hydrogen, based on replicates and standards. No estimate of the errors

introduced by the sampling procedure is made.

Page 13
Forthechamberandsoilgassamples,theerrorin carbonisotopedeterminationis +/- 1permil

from thetotal analysisprocedure,over80%of whichisrelatedto theseparationstep.Sampling

"errors"for chambersampleswereprobablyminimal for enclosuretimeslessthan2hr.,butthisis

only acomparisonto anondisturbedsystem.Soil gassampleshadarealerrorassociatedwith the

sampledepthdetermination,+/- 5 cm,becauseof thesoilcharacter.

10.2.3 Measurement Error for Parameters

Production samples, 2 permil (PDB) carbon, 5 permil (SMOW) hydrogen. Chamber and soil gas

samples, 1 permil (PDB) carbon; except samples with concentrations below 500 ppbv, 2 permil (PDB)

d 13C in carbon. Soil depth for probe +/- 5 cm.

10.2.4 Additional Quality Assessments

None given.

10.2.5 Data Verification by Data Center

Data were examined for general consistency and clarity.

11. Notes

11.1 Limitations of the Data

The data as presented are not correlated with many of the other parameters necessary for

evaluation. These parameters were collected by other investigators and must be processed and included

with these data. The synoptic nature of the data must be understood. Only the chamber and soil gas

data in 1996 cover any part of the seasonal cycle.

11.2 Known Problems with the Data

The production data from 1993 do not have much supporting data from other investigators, and

several of the sites were not sampled at later times. Almost all of the prodded/dislodged bubble

samples were taken near the shore, where plant root activity would be a major variable, but a

quantification of this variable has not been made. The samples from the SSA 1994 chambers were left

down far longer than would have been desired, and the results were most probably influenced by this.

The May 1996 chambers were sampled when the ground was still frozen and saturated with water, and

were in place longer than desired. This may have resulted in unusual conditions.

11.3 Usage Guidance

None given.

11.4 Other Relevant Information

In a large project like this, the number of sites that needed to be covered was greater than the

group's ability and funding. Promised help in field sampling was good at times and lacking in other

cases. Coordination of this effort, which required primarily lab time, with those of the other

investigators, who worked primarily in the field, proved difficult.

12. Application of the Data Set

The data, while still under analysis, demonstrate the methane fractionation occurring with soil

oxidation/consumption. When the approximate methane consumption flux is calculated for the

representative soil types, the effect on the atmospheric methane isotope composition can be

determined. The probability of a concurrent methane production occurring with methane consumption

in the soils is suggested by some of the data.

Page 14
13. Future Modifications and Plans

The data presented here need to be combined with other available parameters that were measured by

other investigators.

14.1 Software Description

Not applicable.

14.2 Software Access

Not applicable.

14. Software

15. Data Access

The TGB-06 soil methane data are available from the Earth Observing System Data and Information

System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center

(DAAC).

15.1 Contact Information

For BOREAS data and documentation please contact:

ORNL DAAC User Services

Oak Ridge National Laboratory

P.O. Box 2008 MS-6407

Oak Ridge, TN 37831-6407

Phone: (423) 241-3952

Fax: (423) 574-4665

E-mail: ornldaac@ornl.gov or ornl@eos.nasa.gov

15.2 Data Center Identification

Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory

(ORNL) Distributed Active Archive Center (DAAC) for Biogeochemical Dynamics

http://www-eosdis.ornl.gov.

15.3 Procedures for Obtaining Data

Users may obtain data directly through the ORNL DAAC online search and order system

[http://www-eosdis.ornl.gov/] and the anonymous FTP site [ftp://www-eosdis.ornl.gov/data/] or by

contacting User Services by electronic mail, telephone, fax, letter, or personal visit using the contact

information in Section 15.1.

15.4 Data Center Status/Plans

The ORNL DAAC is the primary source for BOREAS field measurement, image, GIS, and

hardcopy data products. The BOREAS CD-ROM and data referenced or listed in inventories on the

CD-ROM are available from the ORNL DAAC.

Page 15
16. Output Products and Availability

16.1 Tape Products

None.

16.2 Film Products

None.

16.3 Other Products

These data are available on the BOREAS CD-ROM series.

17. References

17.1 Platform/Sensor/Instrument/Data Processing Documentation

Instrument manual, VG Prism II, Micro Mass, Beverly, MA.

17.2 Journal Articles and Study Reports

Born M., H. Doerr, and I. Levin. 1990. Methane consumption in aerated soils of the temperate zone,

Tellus, 42B, 2-8.

Deck, B., M. Wahlen, P. Hodder, K. Bananal, J. Fessenden, and S. Rosengreen. 1993. Methane

consumption and CO2 exchange in dry soils. Trans. Am. Geo. Union, 74, 43, pg. 121.

Newcomer, J., D. Landis, S. Conrad, S. Curd, K. Huemmrich, D. Knapp, A. Morrell, J. Nickeson,

A. Papagno, D. Rinker, R. Strub, T. Twine, F. Hall, and P. Sellers, eds. 2000. Collected Data of The

Boreal Ecosystem-Atmosphere Study. NASA. CD-ROM.

Sellers, P. and F. Hall. 1994. Boreal Ecosystem-Atmosphere Study: Experiment Plan. Version

1994-3.0, NASA BOREAS Report (EXPLAN 94).

Sellers, P. and F. Hall. 1996. Boreal Ecosystem-Atmosphere Study: Experiment Plan. Version

1996-2.0, NASA BOREAS Report (EXPLAN 96).

Sellers, P., F. Hall, and K.F. Huemmrich. 1996. Boreal Ecosystem-Atmosphere Study: 1994

Operations. NASA BOREAS Report (OPS DOC 94).

Sellers, P., F. Hall, and K.F. Huemmrich. 1997. Boreal Ecosystem-Atmosphere Study: 1996

Operations. NASA BOREAS Report (OPS DOC 96).

Sellers, P., F. Hall, H. Margolis, B. Kelly, D. Baldocchi, G. den Hartog, J. Cihlar, M.G. Ryan, B.

Goodison, P. Crill, K.J. Ranson, D. Lettenmaier, and D.E. Wickland. 1995. The boreal

ecosystem-atmosphere study (BOREAS): an overview and early results from the 1994 field year.

Bulletin of the American Meteorological Society. 76(9): 1549-1577.

Sellers, P.J., F.G. Hall, R.D. Kelly, A. Black, D. Baldocchi, J. Berry, M. Ryan, K.J. Ranson, P.M.

Crill, D.P. Lettenmaier, H. Margolis, J. Cihlar, J. Newcomer, D. Fitzjarrald, P.G. Jarvis, S.T.

Gower, D. Halliwell, D. Williams, B. Goodison, D.E. Wickland, and F.E. Guertin. 1997. BOREAS

in 1997: Experiment Overview, Scientific Results and Future Directions. Journal of Geophysical

Research 102(D24): 28,731-28,770.

Wahlen, M., N. Tanaka, B. Deck, and R. Henry. 1990. dD in Methane; Additional constraints of a

global CH4 Budget. Trans. Am. Geo. Union 71, 43, pg. 1249.

Page 16
Wahlen,M., N. Tanaka,R. Henry,B. Deck,J.Zeglen,J.S.Vogel, J.Southon,A. Shemesh,R.

Fairbanks,andW. Broecker.1989.Carbon-14in methanesourcesandin atmosphericmethane:The

contributionfrom fossil carbon.Science,245,286-290.

17.3 Archive/DBMS Usage Documentation

None.

18. Glossary of Terms

Chamber/Enclosure - A sealed space in contact with the soil. Usually mounted on a skirt dug

into the soil.

LN2 - Liquid nitrogen.

NBS 19, NBS 16, NBS 17 - Reference standards for d 13C in carbon provided by NIST,

formerly known as NBS.

PDB - The reference standard for 13C isotope of carbon. 0 permil.

Permil - Description of the isotopic composition of a sample relative to a standard.

SMOW, SLAP, GISP - Reference standards for dD in hydrogen provided by NIST.

Soil probe - A metal tube pushed to depth in the soil allowing soil gas samples to be taken.

19. List of Acronyms

AES - Atmospheric and Environment Service

ASCII - American Standard Code for Information Interchange

BOREAS - BOReal Ecosystem-Atmosphere Study

BORIS - BOREAS Information System

CD-ROM - Compact Disk-Read-Only Memory

CSIRO - Commonwealth Scientific and Industrial Research Organization

(Division of Atmospheric Research, Australia)

DAAC - Distributed Active Archive Center

EOS - Earth Observing System

EOSDIS - EOS Data and Information System

GC - Gas Chromatograph

GIS - Geographic Information System

GISP - Greenland Ice Sheet Precipitation

GSFC - Goddard Space Flight Center

HTML - HyperText Markup Language

NAD83 - North American Datum of 1983

NASA - National Aeronautics and Space Administration

NBS - National Bureau of Standards (now NIST)

NIST - National Institute for Standards and Technology

NSA - Northern Study Area

OA - Old Aspen

OBS - Old Black Spruce

OJP - Old Jack Pine

ORNL - Oak Ridge National Laboratory

PANP - Prince Albert National park

PDP - Pee Dee Belemnite

SIO - Scripps Institution of Oceanography

SLAP - Standard Light Antarctic Precipitation

SMOW - Standard Measure Ocean Water

SSA - Southern Study Area

Page 17
TBP

TF

TFEN

TGB

UCSD

URL

YJP

- Tower Beaver Pond (NSA)

- Tower Flux

- Tower Fen (NSA)

- Trace Gas Biogeochemistry

- University of California,

- Uniform Resource Locator

- Young Jack Pine

San Diego

20. Document Information

20.1 Document Revision Date

Written: 22-May- 1996

Last Updated: 29-Jul- 1999

20.2 Document Review Date(s)

BORIS Review: 06-Oct- 1997

Science Review:

20.3 Document ID

20.4 Citation

When using these data, please include the following acknowledgment as well as citations of

relevant papers in Section 17.2:

M. Wahlen and B. Deck, Scripps Institution of Oceanography, University of California San

Diego, La Jolla CA 92093-0220

If using data from the BOREAS CD-ROM series, also reference the data as:

Wahlen, M. and B. Deck, "Isotopic Composition of Methane Produced and Consumed in Boreal

Ecosystems." In Collected Data of The Boreal Ecosystem-Atmosphere Study. Eds. J. Newcomer, D.

Landis, S. Conrad, S. Curd, K. Huemmrich, D. Knapp, A. Morrell, J. Nickeson, A. Papagno, D.

Rinker, R. Strub, T. Twine, F. Hall, and P. Sellers. CD-ROM. NASA, 2000.

Also, cite the BOREAS CD-ROM set as:

Newcomer, J., D. Landis, S. Conrad, S. Curd, K. Huemmrich, D. Knapp, A. Morrell, J.

Nickeson, A. Papagno, D. Rinker, R. Strub, T. Twine, F. Hall, and P. Sellers, eds. Collected Data of

The Boreal Ecosystem-Atmosphere Study. NASA. CD-ROM. NASA, 2000.

20.5 Document Curator

20.6 Document URL

Page 18
REPORT DOCUMENTATION PAGE FormApproved

OMB No. 0704-0188

Public reporting burden for this collection of informationis estimated to average 1 hour per response, including the time for reviewing instructions, searching existing data sources,

gathering and maintaining the data needed, and completing and reviewing the collection of information. Send comments regarding this burden estimate or any other aspect of this

collection of information, including suggestions for reducing this burden, to Washington Headquarters Services, Directorate for Information Operations and Reports, 1215 Jefferson

Davis Highway, Suite 1204, Arlington, VA 22202-4302, and to the Office of Management and Budget, Paperwork Reduction Project (0704-0188), Washington, DC 20503.

1. AGENCY USE ONLY (Leave blank) 2. REPORT DATE 3. REPORT TYPE AND DATES COVERED

November 2000 Technical Memorandum

4. TITLE AND SUBTITLE 5. FUNDING NUMBERS

Technical Report Series on the Boreal Ecosystem-Atmosphere Study (BOREAS)

BOREAS TGB-6 Soil Methane Oxidation and Production from NSA BP

923 and Fen Sites

6. AUTHOR(S) RTOP: 923-462-33-01

Bruce Deck and Martin Wahlen

Forrest G. Hall and Sara K. Conrad, Editors

7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS (ES)

Goddard Space Flight Center

Greenbelt, Maryland 20771

9. SPONSORING / MONITORING AGENCY NAME(S) AND ADDRESS (ES)

National Aeronautics and Space Administration

Washington, DC 20546-0001

8. PEFORMING ORGANIZATION

REPORT NUMBER

2000-03136-0

10. SPONSORING / MONITORING

AGENCY REPORT NUMBER

TM--2000-209891

Vol. 233

11. SUPPLEMENTARY NOTES

B. Deck and M. Wahlen: UCSD, Scripps Institute of Oceanography, La Jolla;

S.K. Conrad: Raytheon ITSS

12a. DISTRIBUTION / AVAILABILITY STATEMENT

Unclassifie_Unlimited

Subject Category: 43

Report available from the NASA Center for AeroSpace Information,

7121 Standard Drive, Hanover, MD 21076-1320. (301) 621-0390.

12b. DISTRIBUTION CODE

13. ABSTRACT (Maximum 200 words)

The BOREAS TGB-6 team collected soil methane measurements at several sites in the SSA and NSA.

This data set contains soil methane consumption (bacterial CH 4 oxidation) and associated t3C fractionation effects in samples that were collected at various sites in 1994 and 1996 from enclosures (chambers). Methane t3C data in soil gas samples from the NSAYJP and OJP sites for 1994 and 1996 are

also given. Additional data on the isotopic composition of methane (carbon and hydrogen isotopes)

produced in the NSA beaver ponds and fen bog in 1993 and 1994 are given as well. The data are

stored in tabular ASCII files.

14. SUBJECT TERMS

BOREAS, trace gas biogeochemistry.

17. SECURITY CLASSIFICATION

OF REPORT

Unclassified

NSN 7540-01-280-5500

18. SECURITY CLASSIFICATION

OF THIS PAGE

Unclassified

19. SECURITY CLASSIFICATION

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Unclassified

15. NUMBER OF PAGES

18

16. PRICE CODE

20. LIMITATION OF ABSTRACT

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