AD-A269 720

*Z Development of an Improved

Confirmation Separation Suitable

for Use With SW846 Method 8330

Thomas F. Jenkins and Susan M. Golden June 1993

a- OTIC_

ELECTE SEP231993

£~~I= ubUczi'

a 93-22077

S22 0O4-
Abstract

An improved RP-HPLC confirmation separation was developed that is suitable

for use with EPA SW846 Method 8330. This separation provides adequate

resolution of the analytes most commonly found in explosives-contaminated

waters and soils. The separation is achieved on an LC-CN (cyanopropyl)

column eluted with an eluent composed of water (65%), methanol (12%) and

acetonitrile (23%) at 1.2 m~lmin. Analysis of field-contaminated soil and

groundwater samples indicate that this comfirmation separation is an improvement over the confirmation separation currently recommended in SW846

Method 8330.

For conversion of SI metric units to U.S./British customary units of measurement

consult ASTM Standard E380-89a, Standard Proctice for Use of the Internotionol

System of Units, published by the American Society for Testing and Materials,

1916 Race St., Philadelphia, Pa. 19103.

This report is printed on paper that contains a minimum of 50% recycled

material.
Special Report 93-14

US Army Corps

of Engineers

Cold Regions Research &

Engineering Laboratory

Development of an Improved

Confirmation Separation Suitable

for Use With SW846 Method 8330

Thomas F. Jenkins and Susan M. Golden June 1993

Accesion For

NTIS CRA&l

DTIC TAB

Unannounced 0)

Justification

B y .......... ......... .... . ..... .........

Distribution I

Availability Codes

Avail and I or

Dist Special

Z-fc

Prepared for

U.S. ARMY ENVIRONMENTAL CENTER

CETHA-TS-CR-93048

Approved for pubic release; dlstribution is unlimited
PREFACE

This report was prepared by Dr. Thomas F. Jenkins, Research Chemist, Geological

Sciences Branch, Research Division, U.S. Army Cold Regions Research and Engineering

Laboratory (CRREL) and Susan M. Golden, Chemist, Science and Technology Corporation.

Funding was provided by the U.S. Army Environmental Center (formerly the U.S. Army

Toxic and Hazardous Materials Agency), Aberdeen Proving Ground, Maryland, Martin H.

Stutz, Project Monitor.

The authors gratefully acknowledge Marianne E. Walsh and Louise V. Parker, CRREL, for

their technical review of this manuscript. Patricia Schumacher is acknowledged for careful

preparation of individual analyte stock standards. The authors would also like to thank

Karen Myers of the U.S. Army Engineer Waterways Experiment Station, Vicksburg, Mississippi, for providing groundwater samples from the Rockeye Site, Naval Surface Warfare

Center, Crane, Indiana.

This publication reflects the personal views of the authors and does not suggest or reflect

the policy, practices, programs, or doctrine of the U.S. Army or Government of the United

States. The contents of this report are not to be used for advertising or promotional purposes.

Citation of brand names does not constitute an official endorsement or approval of the use

of such commercial products.
CONTENTS

Page

P reface ................................................................................................................................. ii

In trod uction ........................................................................................................................ 1

Experim ental ....................................................................................................................... 2

C h em icals ....................................................................................................................... 2

Instrum entation ............................................................................................................. 2

Sep arations ..................................................................................................................... 2

Field-contaminated soil and groundwater samples ................................................. 2

Preparation of stock standards ..................................... 2

Results and discussion ....................................................................................................... 2

C onclusions ................................................................................................................... 8

Literature cited ................................................................................................................ . 8

A bstract ................................................................................................................................ 11

ILUSTRATIONS

Figure

1. Retention times of target analytes on LC-CN column as a function of the

percentage of acetonitrile and methanol in the eluent ................................ 4

2. LC-CN chromatogram for the eight primary target analytes with an eluent

composition of 65:12:23 (V/V/V) water/MeOH/ACN at 1.2 mL/min ... 5

3. LC-CN chromatogram for 15 target analytes at an eluent composition of

65:12:23 (V/V/V) water/MeOH/ACN at 1.2 mL/min .............................. 6

4. LC-CN chromatogram for soil extract from Hastings East

Industrial A rea ................................................................................................... 6

5. LC-CN chromatogram for soil extract from Hawthorne AAP .......................... 7

6. LC-CN chromatogram of soil extract from Nebraska Ordnance Works .......... 7

7. LC-CN chromatogram of groundwater sample from Hastings East

Industrial A rea ......................................................................................................... 8

8. LC-CN chromatogram from groundwater sample from the Rockeye site,

Naval Surface Warfare Center ................................................................................ 8

TABLES

Table

1. Retention times for target analytes in EPA SW846 Method 8330 on

LC -C N colum n .................................................................................................. 1

2. Retention times of target nitroaromatic and nitramine analytes on LC-CN

column with various eluents .......................................................................... 3

3. Most frequently observed analytes in explosives-contaminated soils

and waters from ammunition plants, arsenals and depots ................................ 4

4. Retention times for target analytes on LC-CN column eluted with

65/12/23 (V/V/V) water/MeOH/ACN at 1.2 mL/min ........................... 5

u!,i
Development of an

Improved Confirmation Separation

Suitable for Use With SW846 Method 8330

THOMAS F. JENKINS AND SUSAN M. GOLDEN

INTRODUCTION mation was based on the different mechanisms of

separation found for the LC-18 and LC-CN (Jenkins

Several years ago CRREL developed a method 1989) and the ability to separate these compounds

for the determination of residues of nitroaromatics thought to occur most frequently in explosivesand nitramines in explosives-contaminated soils, contaminated soil and water.

based on reversed-phase high performance liquid Over the past several years, this analytical

chromatography (RP-HPLC) (Jenkins et al. 1989). method has been used extensively at CRREL, at

This method was collaboratively tested through other Corps of Engineers Division Laboratories,

the Association of Official Analytical Chemists and at severalcontract laboratories working for the

(AOAC) (Bauer et al. 1990) and was subsequently Army and the EPA. Recently an assessment of this

adopted by the AOAC (1990), the American Soci- method's ability to satisfy Army needs was conety for Testing and Materials (1991) and the U.S. ducted by examining the large data base of water

Environmental Protection Agency (1992) as the and soil analyses accumulated at CRREL and the

standard method for this analysis.

For this method air-dried soils are extracted with acetonitrile (ACN) in a tem- Table 1. Retention times for target analytes in EPA SW846

perature controlled ultrasonic (201C) bath Method 8330 on LC-CN column* (Jenkins et al. 1989).

for 18 hours. The soil is allowed to settle and

an aliquot of the ACN extract is mixed with Tor Rettntion tine

anequal volumeof an aqueous calcium chlo- get analyte (16)

ride solution and filtered. The resulting ex- nitrobenzene (NB) 3.81

tract is •analyzed by RP-HPLC on a LC-18 1,3,5-trinitrobenzene (TNB) 4.05

1,3-dinitrobenene (DNB) 4.18

column using an eluent composed of 1:1 o-nitrotoluene (2NT) 4.37

methanol/water. If the chromatogram con- p-nitrotoluene (4NT) 4.41

tains peaks corresponding to the Iarget m-nitrotoluene (3NT) 4.45

analytes (Table 1), the presence of those cern- 2,6-dinitrotoluene (2,6-DNT) 4.61

pounds is confirmed by RP-HPLC analysis 2,4-dinitrotoluene (2,4-DNT) 4.87

2,4,6-trinitrotoluene (TNT) 5.00 on a second column. The confirmation col- 4-amino-2,6-dinitrotoluene (4-Am-DNI) 5.10

umn is an LC-CN (cyanopropyl) column 2-amino-4,6-dinitrotoluene (2-Am-DNT) 5.15

eluted with 1:1 methanol/water at 1.5 mL/ hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) 6.15

min. Retention times for the LC-CN separa- methyl-2,4,6-trinitro-phenylnitramine (Tetryl) 7.36

tion and a summary of the abbreviations for octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) 8.35

thetargetanalytes for Method8330 are shown * Eluent 1:1 methanol/water at 1.5 mL/min

in Table 1. The selection of LC-CN for confir- Column 25 cm x 4,6 mm (5 pm) (Supelco)
Missouri River Division Laboratory (Walsh et al., 3. Hewlett-Packard model HP 3393A digital inte1993). Two major conclusions of this study were 1) grator equipped with a Hewlett-Packard Model

the target analyte list should be modified to include HP911B disk drive.

3,5-dinitroaniline (DNA) and four current target 4. Linear Model 500 strip chart recorder.

compounds, nitrobenzene and the three isomers of

nitrotoluene, should be dropped, and 2) an im- Separations

proved confirmation separation should be devel- All separations were obtained on a Supelco LCoped that provides a better separation for 2,4- CN column (25 cm x 4.6 mm, 5 pm) using either

dinitrotoluene (2,4-DNT) and 2,4,6-trinitrotoluene binary or ternary eluents composed of water, metha-

(TNT). A large TNT concentration, often several nol and acetonitrile.

orders of magnitude higher than that of 2,4-DNT,

interferes with confirmation of 2,4-DNT using the Field-contaminated soil and

current confirmation separation. groundwater samples

The objective of this study is to develop an im- Air-dried soil from Department of Defense instalproved confirmation separation that provides ade- lations including Hawthorne Army Ammunition

quate resolution of the target analytes of Method Plant (Hawthorne, Nevada), Nebraska Ordnance

8330, even when TNT or RDX is present in large Works (Mead, Nebraska) and Hastings East Indusconcentrations, a common occurrence for explosives- trial Area (Hastings, Nebraska), and contaminated

contaminated soils. groundwater from Hastings and the Rockeye Site,

Naval Surface Warfare Center, Crane, Indiana were

used to test various eluents. Soil extracts were obEXPERIMENTAL tained as described by Jenkins et al. (1989).

Preparation of stock standards

Chemicals All individual analyte stock standards were preStock standards for the target analytes for pared by weighing out approximately 100 mg of

Method 8330 (Table 2) were prepared from Stan- dried standard material to the nearest 0.1 mg, transdard Analytical Reference Materials (SARM) ob- ferring it to individual 100-mL volumetric flasks

tained from the U.S. Army Environmental Center, and diluting to volume with acetonitrile. StopAberdeenProving Ground, Maryland.In addition, pered joints were wrapped with Parafilm to retard

a stock standard for 3,5-dinitroaniline (DNA) was evaporation and solutions were stored at 4°C in the

prepared from material obtained from Aldrich, dark. Combined analyte test solutions were preand its identity was confirmed by GC/MS. Water pared by combining appropriate volumes of these

used in the preparation of the aqueous calcium stock standards and diluting to volume with

chloride (CaCl2 ) solution and in the preparation of acetonitrile.

HPLC eluent was reagent grade water from a MilliQ Type I Reagent Grade Water System (Millipore

Corp.). Methanol used in the preparation of eluent RESULTS AND DISCUSSION

was Ailtech HPLC grade. AcetonirTile used for soil

extraction and for preparation of eluent was Baker Initial experiments were conducted using the

Analyzed HPLC grade. Eluent was prepared daily LC-CN column with different eluents than used in

by combining the appropriate volumes of water, the standard method (50/50 V/V water/methaacetonitrile and methanol and vacuum filtering nol). The first eluent tested was composed of 65/35

through a nylon-66 membrane (0.45 gm) to degas (V/V) water/methanol (MeOH) at a flow rate of

and remove particulate matter. 1.2 mL/min; this eluent is used at the Corps of

Engineers Missouri River Division Laboratory.*

Instrumentation Retention times of the 15 analytes of interest using

RP-HPLC retention time data were obtained on this separation are shown in Table 2. This separaa modular system composed of the following: tion is inadequate, however, in several respects.

1. Spectra PhysicsModel8800 ternary HPLC pump.

2. Spectra Physics Spectra 100 variable wavelength

UV detector set at 254 nm with a cell path length of * P.S. Schnitker, Missouri River Division Laboratory,

0.6 cm. personal communication, 1992.

2
Table 2. Retention times of target nitroaromatic and nitramine analytes on LC-CN column with

various eluents (1.2 mUmin).

% Water/% Methanolf% Acetonitrile (V/V/IV)

65/3510 65/30/5 65/25/10 65/20/15 65/15/20 15/10/25 65/5/30 65/0/35

Nitrate ion 2.1 2.1 2.1 2.1 2.1 2.1 2.1 2.1

NB 6.2 - - 6.1 - - - -

TNB 6.4 6.8 6.8 7.1 7.3 7.4 7.6 8.0

DNB 6.8 6,9 6.8 6.8 6.8 6.6 6.7 6.8

2-NT 8,3 8.1 7.8 7.8 7.5 7.3 7.4 7.5

4-NT 8.4 8.1 7.7 7.7 7.6 7.3 7.4 7.5

3-NT 8.6 8.3 7.9 7.9 7.7 7.5 7.5 7.1

TNT 9.1 9.6 9.7 10.1 10.3 10.2 10.7 11.1

2,4-DNT 9.3 9.2 8.9 8.9 8.7 8.3 8.4 8.5

2,6-DNT 9.3 9.2 9.1 9.1 8.8 8.5 8.6 8.7

DNA 9.9 - - 8.9 8.3 7.7 7.6 7.5

4-Am-DNT 12.3 11.9 11.0 10.6 9.9 9.0 8.8 8.7

RDX 12.7 11.6 10.2 9.4 8.5 7.7 7.4 7.2

2-Am-DNT 12.9 12.1 11.1 10.6 9.9 9.0 8.8 8.6

Tetryl 19.5 18.8 17.2 16.5 15.7 14.8 14.5 14.3

HMX 22.0 19.1 16.3 14.4 12.7 10.9 10.2 9.5

The resolution between TNT and 2,4-DNT is only The effect of ACN incorporation was dramatic

0.2 min. When TNT is present in n~uch higher for HMX and RDX. Retention times for these two

concentration, as is often the case, the ability to analytes were reduced from 22.0 and 12.7 minutes

confirm the presence of a much smaller concentra- in water/methanol to 9.5 and 7.2 minutes, respection of 2,4-DNT is poor. Thnadequate separation of tively, in water/ACN. Retention times for tetryl, 4-

2,4-DNT and TNT was the major problem with the Am-DNT, and 2-Am-DNT and DNA, were also

standard confirmatory separation. An additional reduced significantly ad smaller decreases were

problem is the very late elution of HMX, which observed for the three isomers of NT and the two

reduces the sensitivity for that analyte and sub- isomers of DNT. Retention times for TNT and TNB,

stantially increases analytical run times. Neverthe- interestingly, increased as the percentage of ACN

less, this separation proved to be a useful starting was increased.

point for this evaluation. Recently, Walsh et al. (1993), summarized the

Since ACN has been found to have a special results obtained from analysis of hundreds oi soil

affinity for HMX and RDX (Jenkins 1989), we felt and watersamplesfrom Army ammunitionplants,

that incorporatingACNinthe eluent would reduce arsenals and depots. The eight nitroaromatic and

the retention time for HMX. In addition, changing nitramine explosives, impurities and degradation

from MeOH to ACN on some columns reverses the products most commonly found in soils and waters

retention order of TNT and 2,4-DNT, and hence from these sites are listed in Table 3, along with

incorporation of ACN in the eluent could have a their frequency of occurrence. A plot of the retenpositive effect on the TNT/2,4-DNT separation as tion times for these eight compounds, as a function

well. of the percentage of acetonitrile in the eluent, is

To pursue this possibility, a series of experi- shown in Figure 1. It should be emphasized, howments were conducted in which the aqueous por- ever, that the total organic content of this eluent is

tion of the eluent was maintained constant at 65% maintained at 35% for this plot, the difference

(by volume), but the 35% organic portion was between 35% and the percentage of ACN being

varied between pure MeOH and pure ACN in 5% MeOH.

increments. Retention times of the 15 analytes of Clearly, the separation using the binary eluents

interest were obtained at each composition (Table (water/MeOH or water/ACN) is inadequate. For

2). The retention times for nitrate (an unretained water/MeOH, the resolution between TNT and

species) was also obtained to facilitate calculation 2,4-DNT is poor, as is that for RDX and 2-Am-DNT.

of capacity factors (Table 2). For water/ACN, the separation between 2,4-DNT

3
Percent MeOH in Eluent

30 20 10 0

20

is8 Optimum

Separation

16

'E

12d 2-Am-DNT i ndqae tsvrltray totm oH~n erl hcwudrsli

10

X ho r aFigure 1. Retention times of target

61DN8 analytes on LC-CN column as afunc0 020 30 tion of the percentage of acetonitrile

Percent ACN in Eluent (W535, water/organic) and methanol in the eluent.

and 2-Am-DNT is inadequate. At several ternary tion time for HMX and tetryl, which would result in

eluents, however, adequate separation for all eight the inability to confirm the presence of these analytes

analytes appears to be achieved. Two eluents in at very low concentration due to peak broadening.

particularlook dLive. One is !L,. zluent com, In addition,2,4-T)NT cannotbe adequately resolved

posed of 65/20/15 (V/V/V) water/MeOH/ACN. from either DNA or2,6-DNT, and the three isomers

The only obvious problem is the fairly long reten- of NT are not resolved. A second useful separation

appears to be possible between 20 and 25% ACN. In

Table 3. Most frequently observed this region, HMX elutes much earlier, reducing the

ana!lytes in explosives contaminated problem with detection capability. DNA, however,

soils and waters from ammunition elutes near RDX (Tahbl 1) and thus the ability to

plants, arsenals and depots (Walsh et confirm the presence of DNA would be poor for

aL., 1993) soils containing RDX.

Freqiiency of occnj'ence The best separation was achieved using an eluent of 65/12/23 (V/V/V) water/MeOH/ACN at

Analyte Soil Water 1.2 mL/min. (Table 4). These results are also shown

on the plot in Figure 1. Chromatograms for a stanTNT 44 28 dard containing the eight primary target analytes

RDX 35 61 (Walsh et al., 1993) is shown in Figure 2. A chro2,4-DNT 28 21 matogram showing the separation for all 15 target

DNB 22 13 analytes is shown in Figure 3. The only significant

2-Am-DNT 18 23 problem demonstrated is the inability to separate

HMX 14 14 RDX from DNA. Although the three isomers of NT

Tetryl 12 13 are not adequately separated from TNB, these iso4
Table 4. Retention times for target mers are not commonly found in these samples

analytes on LC-CN columneluted with (Walsh et al., 1993) and hence this does not seem to

water 65n12/23 (V/VN) water/MeOH/ be a major problem. It is interesting that the two

ACN at 1.2 mL/min. isomers of DNTare separated sufficiently to be able

Retention time to confirm if one or both are present. Since they

Analyte (min) elute almost 2 minutes before TNT, they should be

Nitrate ion 210 easily confirmed even when the concentrations of

NB 5.96 TNT is orders of magnitude higher than either

DNB 6.69 DNT isomer.

TNB 7.32 Tests of this separation were conducted using

2-NT 7.41 soil extracts from Hastings East Industrial Area 4-NT 7.41 3-NT 7.61 (Fig. 4), Hawthorne Army Ammunition Plant (Fig.

DNA 8.03 5) and Nebraska Ordnance Works (Fig. 6). The

RDX 8.07 separation achieved in all cases was adequate for

2,4-DNT 8.51 confirmation of the analyte present. Groundwater

2,6-DNT 8.69 samples from Hastings (Fig. 7) and the Rockeye 2-Am-DNT 9.43 4-Am-DNT 9.44 Site, Naval Surface Warfare Center (Fig. 8) were

TNT 10.36 also analyzed using this separation. Again the sepaHMX 11.66 ration achieved was adequate to confirm the presTetryl 15.07 ence of the analytes present in these samples.

z

4

ci

X

co 0

a: -

z

Z

a-.

1-

CV

Figure 2. LC-CN chromatograinfor the

8 primary targetanalytes with an eluent

I I I I I I I I I composition of65:12:23 (V/V/V) water/

0 4 8 12 16

Retention Time (min) MeOH/ACN at 1.2 mLnin.

5
XbH

INI .LNO-9 'Z SIN(3c-W'V

VNG PUB XaG -'a,'

0

a: ~~

INIJ

___________________________________ -1J -(e- ;

ING-9*

VNG Pu X(3o

(0
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iNCO-9 Z SMINOWJV

GNI 6 NO

'NN

C)

0

SNI

CL.r
z -

Q z

X

0-

cc

z r

z

I I I. a- , .. I 

CY

co a

z a:

0 4 8 12 0 4 8 12

Retention lime (rain) Retention Time (ran)

Figure 7. LC-CN chromatogram of groundwater Figure 8. LC-CN chromatogram from grao -idwater

samplefrom Hastings East Industrial Area (65:12:23 samplefrom the Rockeye site, Naval Surfiace Warfare

water/MeOH/ACN at 1.2 mL/min). Center (65:22:23 V/V/V water/MeOH/ACN at 1.2

mL/min).

CONCLUSIONS contaminated soil and groundwater samples indicates that this confirmatory separation is an imAn improved RP-HPLC confinmation repara- provement over the confirmatory separation curtion was developed that is suitable for use with rently recommended in SW846 Method 8330.

EPA SW846 Method 8330. This separation provides adequate resolution of the analytes most

commonly found in explosives-contaminated wa- LITERATURE CITED

ters and soils. The separation is achieved on an LCCN (cyanopropyl) column eluted with an eluent Association of Official Analytical Chemists (1990)

composed of water (65%), methanol (12%) and Munition residues in soil, liquid chromatographic

acetonitrile (23%) at 1.2 mL/min. Analysis of field- method. Official First Action, September, 1990.

8
Method 991.09, Second Supplement to the 15th method for the determination of extractable

Edition of Official Methods of Analysis, pp. 78-80. nitroaromatics and nitramines in soils. Ph.D, disAssociation of Official Analytical Chemists. sertation, University of New Hampshire (unpubAmerican Society for Testing and Materials (1991) lished).

Method for analysis of nitroaromatic and nitramine Jenkins, T.F., M.E. Walsh, P.W. Schumacher, P.H.

explosives in soil by high performance liquid chro- Miyares, C.F. Bauer and C.L. Grant (1989) Liquid

matography. Method D5143-90. chomatographic method for the determination of

Bauer, C.F., S.M. Koza and T.F. Jenkins (1990) extractable nitroaromatic and nitramine residues

Collaborative test results for a liquid chromato- in soil. Journal of t-: Association of Official Analytical

graphic method for the determination of explosive Chemists, 72: 890 - -9

residues in soil. Journal of the Association of Official Walsh, M.E., T.F. Jenkins, P.H. Miyares, P.S.

Analytical Chemists, 73: 541-552. Schnitker, J.W. Elwell and M.H. Stutz (1993).

Environmental Protection Agency (1992) Evaluation of analytical requirements associated

Nitroaromatics and nitramines by HPLC. Second with sites potentially contaminated with residues

Update SW846 Method 8330. of high explosives. USA Cold Regions Research

Jenkins, T.F. (1989) Development of an analytical and Engineering Laboratory, CRREL Report 93-5.

9
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4. TITLE AND SUBTITLE 5 FUNDING NUMBERS

Development of an Improved Confirmation Separation Suitable for

Use With SW846 Method 8330

6. AUTHORS

Thomas F. Jenkins and Susan M. Golden

7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES) 8. PERFORMING ORGANIZATION

REPORT NUMBER

U.S. Army Cold Regions Research and Engineering Laboratory

72 Lyme Road Special Report 93-14

Hanover, New Hampshire 03755-1290

9. SPONSORING/MONITORING AGENCY NAME(S) AND ADDRESS(ES) 10. SPONSORING/MONITORING

AGENCY REPORT NUMBER

U.S. Army Environmental Center

Aberdeen Proving Ground, Maryland 21010 CETHA-TS-CR-93048

11. SUPPLEMENTARY NOTES

12a. DISTRIBUTiON/AVAILABILITY STATEMENT 12b. DISTRIBUTION CODE

Approved for public release; distribution is unlimited.

Available from NTIS, Springfield, Virginia 22161

13. ABSTRACT (Maximum 200 words)

An improved RP-HPLC confirmation separation was developed that is suitable for use with EPA SW846 Method 8330. This

separation provides adequate resolution of the analytes most commonly found in explosives-contaminated waters and soils.

The separation is achieved on an LC-CN (cyanopropyl) column eluted with an eluent composed of water (65%), methanol

(12%) and acetonitrile (23%) at 1.2 mL/min. Analysis of field-contaminated soil and groundwater samples indicate that this

comfirmation separation is an improvement over the confirmation separation currently recommended in SW846 Method

8330.

14. SUBJECT TERMS 15. NUMBER OF PAGES

Chemical analysis RDX TNT 14

Explosives Soil contamination Water contamination 16. PRICE CODE

Munition residues

17. SECURITY CLASSIFICATION 18. SECURITY CLASSIFICATION 19. SECURITY CLASSIFICATION 20. LIMITATION OF ABSTRACT

OF REPORT OF THIS PAGE OF ABSTRACT

UNCLASSIFIED UNCLASSIFIED UNCLASSIFIED UL

NSN 7540-01-280-5500 Standard Form 298 (Rev. 2-89) Prescnbed by ANSI Std Z39-8

298-102