&EPA
             United States
             Environmental Protection
             Municipal Environmental Research  EPA-600/2-79-038
             Laboratory          July 1979
             Cincinnati OH 45268       >»  t
             Research and Development
Liner Materials
Exposed to
Municipal  Solid
Waste Leachate
            Third Interim Report

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                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.


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                                                    EPA-600/2-79-038
                                                    July  1979
LINER MATERIALS EXPOSED TO MUNICIPAL SOLID WASTE LEACHATE

                   Third Interim Report
                             by

                    Henry E. Haxo, Jr.
                      Robert S. Haxo
                    Thomas F. Kellogg
                      Matrecon, Inc.
                Oakland, California 94623
                  Contract No. 68-03-2134
                     Project Officer

                     Robert Landreth
       Solid and Hazardous Waste Research Division
       Municipal Environmental Research Laboratory
                 Cincinnati, Ohio 45268
       MUNICIPAL ENVIRONMENTAL RESEARCH LABORATORY
           OFFICE OF RESEARCH AND DEVELOPMENT
          U.S. ENVIRONMENTAL PROTECTION AGENCY
                 CINCINNATI, OHIO 45268
            U.S. Environmental Protection Agency
            Region V,  Library
            230 South Dearborn  Street
            Chicago, Illinois  60604

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                                 DISCLAIMER
     This report has been reviewed by the Municipal Environmental Research
Laboratory, U.S. Environmental Protection Agency, and approved for publica-
tion.  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 rec-
ommendation for use.
                    U,S. Environmental Protection Agency
                                     11

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                                  FOREWORD
     The Environmental Protection Agency was created because of increasing
public and government concern about the dangers of pollution to the health
and welfare of the American people.  Noxious air, foul water, and spoiled
land are tragic testimony to the deterioration of our natural environment.
The complexity of that environment and the interplay between its components
require a concentrated and integrated attack on the problem.

     Research and development is that necessary first step in problem solu-
tion and it involves defining the problem, measuring its impact, and search-
ing for solutions.  The Municipal Environmental Research Laboratory develops
new and improved technology and systems for the prevention, treatment, and
management of wastewater and solid and hazardous waste pollutant discharges
from municipal and community sources, for the preservation and treatment of
public drinking water supplies, and to minimize the adverse economic, social,
health, and aesthetic effects of pollution.  This publication is one of the
products of that research; a most vital communications link between the re-
searcher and the user community.

     Although the information contained herein is preliminary,  it will pro-
vide a guide and insight to the effects that happen after limited exposure.
This information and data could be useful for design purposes if not taken
out of context.
                                      Francis T.  Mayo,  Director
                                      Municipal Environmental Research
                                      Laboratory
                                    111

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                                  ABSTRACT
     This report is the third interim report of a project that aims to assess
the effects upon various liner materials of extended contact with leachate
from simulated sanitary landfills.   In this part of the study, the primary
exposure tests of liner specimens at the bottom of simulated landfills were
supplemented by immersion of 28 different polymeric materials in sanitary
landfill leachate.  Immersed membranes were tested for changes in physical
properties, permeability, and water absorption.  The polymeric materials
tested included butyl rubber, chlorinated polyethylene, chlorosulfonated
polyethylene, elasticized polyolefin, ethylene propylene rubber, neoprene,
polybutylene, polyester elastomer,  low-density polyethylene, plasticized
polyvinyl chloride, and polyvinyl chloride plus pitch.

     The results of the immersion tests generally confirm the earlier results
for membrane liner materials exposed for one year in simulated landfills.
Specimens of chlorinated polyethylene, chlorosulfonated polyethylene,
ethylene propylene rubber, and neoprene liners showed the greatest swell and
loss of properties, although specimens of some ethylene propylene rubber and
neoprene liners showed low swelling and little loss of properties.

     Also reported are results of the water vapor permeability testing of
28 membrane liners, the water absorption of a series of membranes at room
temperature and at 70°C, and the retrieval and testing of samples of a 6-
year old membrane liner from a demonstration landfill.  The monitoring of the
simulated landfills during 180 months of operation is described and the
analyses of the leachates produced during the period of operation are
summarized.

     A simple bag test for assessing permeability and physical properties of
membrane liners for landfills is described and test results are presented.

     This report was submitted in partial fulfillment of Contract 68-03-2134
by Matrecon, Inc., under the sponsorship of The U. S. Environmental Protec-
tion Agency.  It  covers work performed during the period January 1, 1976
to May 31, 1978.
                                      IV

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                                  CONTENTS
Foreword
Abstract
List of Figures  .......................................... _ _ f              v^
List of Tables [[[     vi^
List of Abbreviations and Metric Conversion Table .....................  viii
Acknowledgements . . ....................                                    j „
                                         *******"*"*•**••"•••«•••»•••••    JLj£

   1 .  Introduction .........................................               ^
   2 .  Summary .............. „ ......... , ..................                  *
   3 .  Future Work  ...........................................              g
   4 .  Experimental Work ..... . ......................................       8
             Immersion of Membrane Liners in Leachate .................     8
             Water Vapor Permeability of Polymeric Membrane Lining
                Materials ...........................................      ±Q
             Bag Test for Assessing Membrane Liner Materials ..........    24
             Water Absorption of Membrane Liner Materials .............    31
             Monitoring the Leachate Generators .......................    34
             Recovery and Testing of Samples of a Polyvinyl Chloride
                Liner from a Demonstration Landfill ...................    43

References ................. . ....................                           4fi
Appendices [[[     ' '    47
   A.   Properties of Unexposed Polymeric Membranes in Project ...... ...    47

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                             LIST OF FIGURES








Number                                                                Page




   1.  Individual polyethylene immersion tank ............   10




   2.  Immersion system set up with gravity feed of leachates ....   11




   3.  Immersion system set up with pump and gas relief valves. ...   12




   4.  Leachate pH during the immersion test .............   I5




   5.  E96 water vapor permeability cup and auxiliary equipment ...   19




   6.  Constant-air-velocity cabinet for holding E96 permeability cups  22





   7.  Schematic of osmosis bag assembly ...............   26




   8.  Osmosis bag and auxiliary equipment for monitoring ......   27




   9.  Leachate collection bag with water seal and vent  .......   36




   10.  Average solids content of leachate produced in generators.  .  .   37




   11.  Average pH of leachate produced  in the generators .......   38




   12.  Average total volatile acids of  leachate produced in  the
                                                                        ->Q

          generators  .........................   J:y
   13.   Average chemical  oxygen  demand of  leachate produced  in the

                                                                        40
          generators .........................
   14.   Average refuse consolidation in the 12  generators.
                                                                        41
                                     VI

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                               LIST OF TABLES

Number

   1  Analysis of Leachate used in the Immersion System 	   14

   2  Summary of Effects of Immersion of Polymeric Membrane Liners in
      Leachate for 8 months	   17

   3  Effects of Test Conditions on Water Vapor Permeability of  Polymeric
      Membrane Liners	   20

   4  Water Vapor Permeability of Polymeric Membrane Liners 	   23

   5  Effect of Test Time on Water Vapor Permeability	   24

   6  Characteristics of Leachate in Bags	   25

   7  Tests of Membrane Liner Bags Filled with Leachate 	   29

   8  Tests of Bags Containing Leachate  	   28

   9  Tests of Membrane Liner Bags Filled with 5%  NaCl  Solution  	   30

  10  Test of Bags Containing 5%  Salt  Solution	   31

  11  Water Absorption of Selected Membrane Liner  Materials  	   33

  12  Order of Increased Swelling in Water	   32

  13  Comparison  of the Swelling  of Membrane Lining Materials  	   34

  14  Cumulative  Collection  of  Leachate Below  Liners	   42

  15  Analyses of Polyvinyl  Chloride Liner  from Demonstration Landfill .   44

  16  Properties  of Polyvinyl Chloride Liner from Demonstration Landfill.   45
                                    VII

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                            LIST OF  ABBREVIATIONS

                    cm            — centimetres
                   COD            — chemical oxygen demand
                     h            — hour
                    Hg            — mercury
                   ipm            — inches per minute
                   MPa            — megapascals
                  ymho            — micro-mho
                    ml            — millilitres
                    mm            — millimetres
                    pH            — hydrogen ion concentration
                   ppi            — pounds per inch
                   ppm            — parts per million
                   psi            — pounds per square inch
                   TVA            — total volatile acids

                          METRIC CONVERSION TABLE

FACTORS FOR CONVERTING DATA IN U. S. CUSTOMARY UNITS TO SI METRIC UNITS
Inches to centimetres (cm)                                     x 2.54
Feet to metres                                                 x 0.3048   _3
Mils to centimetres  (cm)                                       x 2.54 x 10_2
Mils to millimetres  (mm)                                       x 2.54 x 10 _3
Pounds per square inch  (psi) to megapascals  (MPa)              x 6.895 x 10_1
Pounds per inch  (ppi) to kilo Newtons per metre  (kN/m)         x 1.751 x 10
Pound  (force) to Newtons                                       x 4.448
Some U. S. Customary units are used in this report as they are commercially
used in the United States in the solid wastes industry as well as the liner
production and installation industries.
                                    viii

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                              ACKNOWLEDGEMENTS
     The authors wish to thank Robert E. Landreth for his support and guid-
ance in this project.  They also wish to acknowledge the guidance of Dr.
Clarence Golueke and Stephen Klein of the Sanitary Engineering Research
Laboratory, University of California, Berkeley, California, who were
responsible for the analyses and characterization of the wastes.

     The following companies contributed to this project by supplying
samples, information, and technical assistance:

               Burke Industries, Inc.
               Carlisle Tire and Rubber Company
               Cooley, Inc.
               Dow Chemical Company
               E. I. du Pont de Nemours and Company
               Exxon Chemical Company
               Firestone Tire and Rubber Company
               Gaco Western, Inc.
               B. F. Goodrich Company
               Goodyear Tire and Rubber Company
               Pantasote Company
               Phillips Petroleum Company
               Plymouth Rubber Company
               Polysar Corporation
               Quarry Products, Inc.
               Ransome Company
               Reeves Bros., Inc.
               Ruberoid Building Products,  Ltd.
               Staff Industries
               Union Carbide Company
               Watersaver Company
               Witco Chemical Corporation

     We also gratefully acknowledge the cooperation of The Asphalt Institute
and The Portland Cement Association.
                                     IX

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                                   SECTION I

                                  INTRODUCTION


      The lining of sanitary landfills with impervious materials has been
 found to be a feasible method of intercepting and controlling leachate that
 may be generated in a landfill and preventing it from entering and polluting
 surface and ground waters.   A wide variety of materials were potentially
 useful for lining sanitary  landfills  but this application and information
 regarding the effects of leachate contact were almost nonexistent when this
 study was initiated.   A technology that had been developed to impound and
 control water in canals, ponds,  etc.,  appeared to be  applicable to the
 lining of sanitary landfills,  but the effects of prolonged contact.of liner
 materials with leachate were not known.   The development of this type of
 information was needed to insure the  choice of adequate materials for lining
 sanitary landfills.   This study  was undertaken to develop such information
 in terms that could be readily understood by engineers,  designers,  and users.

 OBJECTIVES

      The primary objectives  of the project as  a whole   are  as  follows:

      1.   To determine the effects of exposure  to leachate from compacted,
          municipal  refuse on the physical  properties of  12  selected  liner
          materials  (excluding  soils and  clays)  that were  believed to  be
          potentially  useful  for  the lining of  sanitary  landfills.

      2.   To determine  the durability of  these  liner materials  and to  estimate
          their  effective  lives when exposed to  leachate  for prolonged periods
          under  conditions comparable to  those  encountered in a sanitary  land-
          fill.

      3.  To  develop accelerated testing procedures for evaluating new
         materials that may have potential  application to lining  landfills.

      4.  To  analyze the costs of sanitary  landfill liner materials,
         including installation costs and the benefits of greater durability.


BACKGROUND

     The primary effort in this project has been to assess the effects of
landfill leachate on a wide  range of potential liner materials (except soils
and clays) under conditions  that simulate real-life exposure.  In taking this
approach, which would develop information that would be directly translatable

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into use in field application, we constructed 24 simulated landfills,  each
containing about one cubic yard of shredded municipal refuse.   Specimens,
two ft in diameter, of 12 different lining materials, six polymeric mem-
branes and six admixes, were sealed in the bases (1-4).   Leachate was  pro-
duced in each generator by saturating the refuse and adding one in. of tap
water on a biweekly basis to equal 26 in. of water per year.  Leachate was
allowed to pond on the liner specimens to a depth of one ft to supply  an
hydraulic head and thus a driving force for the leachate to seep through the
liner specimen.

    The exposure tests of the primary membrane liners were supplemented by
simultaneously exposing two sets of small specimens of 42 polymeric membrane
materials.  These were buried in the sand above the primary liners.

    The permeabilities of the primary liners are being assessed by measuring
the amount of leachate that seeps through the liners.  The effects of
leachate upon the properties of liners are determined by recovering and
testing the liner specimens at two time intervals, initially planned for
12 and 14 months, but now planned for 12 and 55 months.

    In November 1975, after a year of exposure, the first of the two sets
of samples was recovered, and properties of the leachate exposed materials
were measured.  Results were presented in the Second Interim Report (2).
One year of exposure to landfill leachate had only relatively minor effects
upon all the liner materials under test.  All materials appeared to have
maintained their original permeabilities.  The admix materials became some-
what more impermeable.

    Losses were measured in the compressive strength of the admix materials
and in the physical properties of some of the polymeric membranes.  Most
membranes swelled; the chlorinated polyethylene and the chlorosulfonated
polyethylene were affected the most, and the polyolefins, polyethylene,
polypropylene, and polybutylene, the least.

    The limited effects of the one year of exposure on the  liner materials,
even in leachate that was considered to be relatively concentrated, made
long-term extrapolations to liner service life very tenuous.  Consequently,
the exposure period was extended and the dismantling and testing of the
liner materials was postponed, first to June 1978, and later to July  1979.
In addition, the scope of the project was expanded to include immersion
studies, analyses of liner materials, additional permeability studies,  and
efforts to develop simpler testing procedures  for evaluating liner materials
for sanitary landfills.

      Progress  in this  project is being  presented  in  a  series of  interim
reports.  The  First Interim Report  (1)  describes  the overall technical
approach, the  construction of  the  leachate generators, the  selection  of
liner materials, the loading  of the  cells with ground refuse, and  the
bringing of  the  cells  to field capacity.  In that report, various  liner
materials, are  discussed, and  the bases  for selecting the  12 primary materials
are presented.   The original  properties  of unexposed liner  materials  were
determined so  that the effects of  the various  exposures could be measured

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from these values.  Cost data for the various materials used to line ponds,
lagoons, pits, etc., are also examined.

    The Second Interim Report (2) presents the results of exposing liner
materials to leachate for one year.  The monitoring of the generators is
described, and the analyses of leachate generated over the one-year period
are reported.  Also described are the overall operation of the leachate
generators and the performance of the materials employed in fabricating the
apparatus used in this project.   Permeability of the various materials to
water and leachate is discussed.  The report also includes Appendixes of
test data taken from the First Interim Report (1).

    This report, the Third Interim Report, covers the period January 1976
through May 1978, and concentrates on the membrane liner materials.
Discussed are the testing of liner materials by immersion in leachate;
water vapor permeability, leachate, and water absorption of polymeric
membranes; permeability of thermoplastic, heat-sealable membranes to
leachate by osmosis; the continued monitoring of the leachate generators,
and the recovery and testing of  a sample of polyvinyl chloride liner taken
from a demonstration landfill.  The design, construction, and operation of
the immersion system are also described.

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                                 SECTION 2

                                  SUMMARY
IMMERSION TESTS

    Three sets of 28 different polymeric membrane liner specimens  were
immersed in a series of tanks containing a blend of leachates  produced in
the 12 generators.  This system was designed to maintain anaerobic condi-
tions and to allow the leachate to flow slowly through the tanks.   After
8 months of immersion, one set of the 28 lining specimens was  removed and
tested.

    The eight months of immersion in leachate appears to be approximately
equivalent to one year of one-sided exposure of the primary specimens of
the same materials in the bases of the generators.  This immersion condition
duplicated the effects on the buried specimens of the same liners  placed in
the sand.  In the case of the other lining materials which are not being
exposed in the generators, the effects were not large.  The liners based
upon chlorinated polyethylene, chlorosulfonated polyethylene,  and neoprene
tended to swell and soften more than the other lining materials.  On the
other hand, the polyolefins, such as polyethylene, polybutylene, elasticized
polyolefin, and polyester elastomer, all of which are partially crystalline,
swelled and softened the least.  The polyvinyl chloride membranes approxi-
mated the latter materials in swelling and changes of properties.

WATER VAPOR PERMEABILITY

    Permeability testing of the various membrane liner materials has been
continued, using several test methods.  Results of water vapor permeability,
by ASTM E-96, Method BW  (5), are reported for 27 different liner materials,
including butyl rubber, chlorinated polyethylene, chlorosulfonated poly-
ethylene, elasticized polyolefin, ethylene propylene rubber, neoprene,
polyester, and polyvinyl chloride.  As a group, the polyvinyl chloride liner
materials have the highest permeability to water vapor and the butyl rubber
and elasticized polyolefin the lowest.  Permeability appears to increase
with test time, probably because of swelling of the membranes by water.

OSMOTIC BAG TEST

    A laboratory test method now being developed appears feasible for
assessing membrane materials for lining sanitary landfills and the contain-
ment of hazardous wastes.  In this test, leachate or other waste fluid is
sealed in a small bag fabricated of the material under test.  The bag is
then placed in a somewhat larger bag  containing deionized water.  The

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 permeability of the membrane is assessed by measuring weight increase of the
 inner bag and pH and conductivity of the deionized water.   After the perme-
 ability test is completed,  the physical properties of the  bag material can
 be measured to determine the effects of exposure to the leachate.   Data are
 presented for bags  made of  six different polymeric membranes in which
 leachate and 5% salt solution were sealed.   During immersion in the deion-
 ized water, the bags increased in weight and the deionized water changed in
 pH and conductivity, depending on the membrane.

 WATER ABSORPTION TESTS  OF SELECTED MEMBRANE LINERS

     Two series of water swelling tests,  run for  100 weeks  at room temper-
 ature and at 70°C,  indicate that membrane liners of neoprene,  chlorosulfon-
 ated polyethylene,  and  chlorinated polyethylene  continually swell  in water,
 whereas the polyethylene, polybutylene,  polyester, and elasticized poly-
 olefin reach a plateau  in the swell,  as  does polyvinyl chloride.   At least
 one of the polyvinyl chloride liners  tended to harden on long-term exposure,
 indicating loss of  plasticizer.

 MONITORING OF THE LEACHATE  GENERATORS

     The 12 simulated landfills in which  12  different liner materials are
 being exposed to leachate continue to be operated.  No leachate has been
 collected below the liners  of seven of these generators after  43 months of
 operation.   Two of  the  generators with butyl rubber and polyethylene
 membrane liners appear  to have failed at the epoxy resin seals  between the
 liners  and the bases of the generators.   Two admix liners,  soil asphalt and
 soil cement,  have allowed minor  amounts  of  leachate to seep into the bases.
 The current schedule calls  for the operation of  the 12 generators  to be
 continued until July 1979,  when  they  will be disassembled  and  the  liners
 will be retrieved and tested.

     The leachate  that is being produced  in  the 12  generators is  gradually
 becoming more  dilute in solids content,  chemical oxygen demand,  and
 volatile acids.   Also,  the  average pH has now risen from approximately 5 to
 6.5,  with leachate  from several  generators  over  7.0.

     The refuse  in the cells  continues  to consolidate  linearly with  time.
 After 43 months,  the  average  consolidation  of shredded refuse in the  12
 remaining generators  is  16%.

 RECOVERY AND TESTING OF MEMBRANE  LINER FROM A LANDFILL

     Samples of  a polyvinyl  chloride liner were retrieved from a demon-
 stration  landfill and tested.  This liner had good properties and probably
 changed  little during the six-year  exposure  period.  Because of an
 impermeable clay  cover on the membrane,  leachate probably did not directly
 contact  the liner;  furthermore, the leachate  appeared  to be quite dilute.
 There were no data available on the properties of  the  liner before  exposure
with which to make a comparison.

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                                 SECTION  3

                                FUTURE WORK
    The period covered by this  project has been  extended through  November
1979,  during which time the following tasks  will be  performed:

       Exposure of the primary  liners in the bases of  the~leachate
       generators  will be continued through  June 1979, when  they  will have
       been exposed for 56 months.   The exposure of  the  small supplemental
       specimens buried in the  sand above the primary  liners will also be
       continued.

       The immersion and osmosis bag tests now underway  will be continued.

    -   The second  set of 28 specimens will be recovered  in June 1978  and
       tested after 19 months of immersion in leachate and the third  and
       final set will be removed and tested  in June  1979 after 30 months of
       immersion in leachate.   At  the end of the project the membrane
       osmosis bags will be cut and the membranes tested.

       The small specimens buried  in the sand above  the  primary liners in
       the two leachate generators  containing the asphaltic  membranes will
       be recovered and tested  in  June 1978  to assess  the effects of  43
       months of exposure to leachate.  These two primary liners  will be
       inspected and one will be sampled and a repair  made.  New  small
       membrane samples will be placed in the sand and the generators will
       be returned to operation for the remainder of the project.

    -   Permeability studies will be expanded as  follows:

       a.  Additional bags will be  prepared  to assess  the permeability of
           membrane liner materials to water and to  dissolved constituents
           of the  leachate.

       b.  A newly-designed top-pressure permeameter will be used to
           determine the permeability of membrane liners to  leachate.

       c.  Additional tests will be made of  water vapor  permeability  using
           ASTM E-96, Method BW.

       d.  The permeability of  membrane liners to gases, such as  methane,
           carbon  dioxide, and  air, will be  determined.

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The various methods of joining dissimiliar lining materials will be
investigated and, if necessary, experimental work will be performed
to develop adequate methods for limited combinations.

The analysis of membrane liners will be completed for possible use
in specifications.

The specifications now being followed by manufacturers, suppliers,
and installers of various liner materials will be reviewed.

An investigation of soil-membrane liner composites will be carried
out to determine the effect of a soil cover on the rate of deteri-
oration of the membrane liner.

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                                 SECTION 4

                             EXPERIMENTAL WORK


IMMERSION OF MEMBRANE LINERS IN LEACHATE

    Assessing liner materials for lining sanitary landfills by exposing to
leachate at the bottom of simulated landfills, such as is being done in this
project, is time-consuming and expensive.  Simpler methods are needed to
evaluate a liner material for this application.  The results obtained in
this project should form a basis for the development of simpler procedures
which will correlate with the results obtained and with actual landfill
experience.

    An obvious simplification of the simulated landfill method is to im-
merse specimens of various liner materials in the leachate from municipal
refuse and determine the changes in properties during the exposure.  The
availability of leachate from the simultated landfills presents the oppor-
tunity for obtaining a direct correlation between these two procedures for
use in developing a laboratory evaluation test.  The same materials can be
tested by the two methods in essentially the same leachate.

    Membrane liners are amenable to immersion testing but admix materials
pose many experimental problems in such types of tests.  The study which
was undertaken of the effects of immersion in leachate was, therefore,
restricted to membrane liners.

    Our basic plan was to immerse liner specimens of sufficient size to be
able to obtain data on volume arid area swell and on the same physical
properties as were measured on the primary liners.  The leachate  from the
generators would be used and allowed to  flow slowly past the specimens.
The liner materials selected would include some of the materials
being exposed in the simulated landfills  as well as new materials which
have subsequently become available either commercially or on a developmental
basis.  In order to obtain sufficient data with which to make projections
of  service life, it was planned to immerse three sets of liner specimens
and to withdraw them at three time intervals.  Originally it was  planned  to
immerse the  specimens  for six months, 12  months and 18 months, but  the  times
were later changed to  eight months,  19 months  and  30 months.

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 Design and Construction of  the Immersion System


     We originally planned to attach small cells or bags containing the
 liner specimens directly to the individual leachate generators and allow
 the leachate to flow by the specimens as it was continuously being
 collected.  Such a design would maintain the anaerobic condition that
 existed in the generator where the primary liners were being exposed.
 However, the leachates being produced were varying in composition from one
 generator to another which would make comparison between liners difficult.
 Furthermore, the number of containers would be large and monitoring of
 the 12 generators with the attached containers posed a variety of problems
 and additional effort.
     This design was replaced with one in which blended leachate from the
 12 generators slowly flowed through a series of polyethylene tanks in which
 the membrane specimens could be hung.  We felt this arrangement would be
 acceptable because only small changes in composition of the leachate were
 observed when it was stored in polyethylene containers at room temperature
 over a period of one month.  Furthermore, this design allowed easy exposure
 of more specimens, exposures of all specimens to the same leachate, and
 required considerably less time to construct and monitor.


     After considering a wide variety of containers  for use as immersion
 cells,  we selected heavy-duty high-density polyethylene tanks (Nalgene),
 14 x 10 x 10 in.  in dimensions, each with a 6-gal capacity.   These tanks,
 which were placed on a 3.5 ft wooden platform,  are  of heavy-gauge  con-
 struction with  flat lids from which the specimens were hung on stainless
 steel hooks.  Inlets and outlets  were installed,  and the  lids with the
 specimens were  welded to the tanks  (Figure 1).   The flow  of the  leachate
 through the tanks was  by gravity  feed from a drum containing leachate
 placed  above  the  tanks as  shown in  Figure 2.  Problems were  encountered
 with this arrangement  due  to plugging of  the  system by precipitation of
 solids  in the leachate.
    A Masterflex pump was, therefore, installed that delivered leachate
at the rate of 14 ml per minute through the tanks, recirculating the
supply of leachate in about 12 days  (Figure 3).
Exposure Specimens


    Twenty-eight different membranes of 11 different polymeric materials
were selected for immersion testing:

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         COVER DETAIL
SPECIMENS ATTACH
TO HOOKS
                                                  CROSS SECTION

                                    LEACHATE IN -^              ^- LEACHATE OUT
      LEACHATE IN
                                          LEACHATE OUT
                                                 14  SPECIMENS
                                                    NOTE:
                                                    PLASTIC WELD  SEALS
                                                    COVER TO CONTAINER
                                                        POLYETHYLENE  TANK
      Figure  1.  Individual polyethylene immersion tank,  showing method of
                holding specimens and the inlet and outlet for the  leachatfe.

-------
Figure 2.   Immersion system set up with gravity feed of leachates through
           the tanks.   Leachate generators are in the rear.

-------
DO
                  Figure  3.   Immersion system set up with pump and gas  relief valves  on
                              individual tanks.  The pump is  in the center  of the  upper
                              shelf; leachate generators are  in the rear.

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                                                Number of different
          Type of Material	     liners immersed

          Butyl rubber	   1
          Chlorinated polyethylene (CPE)  	   3
          Chlorosulfonated polyethylene (CSPE)  ....   3
          Elasticized polyolefin 	   1
          Ethylene propylene rubber  	   5
          Neoprene	   4
          Polybutylene (PB)   	   1
          Polyester elastomer  	   1
          Polyethylene (PE)   	   1
          Polyvinyl chloride (PVC)  	   7
          PVC and pitch	   1

               Total	28

 Three specimens  of each  membrane were  immersed in the leachate in sets of
 the 28 so that they could be removed from the  system after three exposure
 periods.

     The 8 x 10 in. size of the test specimens was  sufficient to make all of
 the tests required.   The specimens were hung vertically 0.92 in.  apart in
 the tanks (Figure 1).

     The tests  which were performed on  the  lining  materials  before exposure
 and at three subsequent  intervals  are:

          Weight,  before  and after  exposure.
          Dimensions, before and  after  exposure.
          Tensile  strength,  in machine  and  transverse  direction, ASTM D412.
          Hardness, ASTM  D2240.
          Tear  strength in machine  and  in transverse direction,
            ASTM D264, Die C.
          Puncture  resistance, FTM  101B, Method 2065.
          Volatiles at 105°C, ASTM  D297.
          Specific  gravity,  ASTM  D297.

    The physical properties of the unexposed lining materials  that were
immersed  are presented in Appendix A.

Operation of Immersion System

    Approximately 48 gallons of  leachate obtained by blending the output
of the 12 generators, was introduced into the system every 4 weeks and a
similar amount of the used leachate was drawn off.  The new leachate was
the accumulation of the two previous collections of 24 gallons each from
the generators.  Samples  of both the new and used leachate were tested at
each addition for:  pn, chemical oxygen demand (COD), total solids  (TS),
total volatile solids (TVS), and total  volatile acids (TVA).
                                    13

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    The differences in the composition of the leachate added and of that
removed were small, indicating the air-tight, anaerobic character of the
system.  During the initial operation of the system, the analytical results
 (Table 1) were close to the calculated averages of the leachates from the
generators  (see below, "Monitoring the Leachate Generators").  In later
months, however, differences developed between the two that may have been
caused by biological contamination of the blended leachate.  The pH of the
leachate from the generators (Figure 4) is increasing at a regular rate
 (see below, "Monitoring the Leachate Generators"); however, the pH of the
blended leachates in the system became substantially higher in October-
November 1977 and has remained high.
         TABLE  1.  ANALYSIS OF LEACHATE USED  IN THE IMMERSION SYSTEMa
                                     Leachate added     Leachate removed
              Property                   to  system         from  system
PH
Chemical oxygen demand, g/1
Total volatile acids, g/1
Total solids, %
Total volatile solids, %
5.27
32.6
11.3
1.70
0.94
5.27
29.0
11.3
1.80
1.00

     Samples were taken on January  31,  1977.
    Some gas was generated in the tanks, which necessitated the addition of
relief valves to prevent pressure buildup.  During the course of the
operation there were two leaks in the welds that required repairs.

Results of Exposure to Leachate

    After eight months of immersion, two tanks containing one set of test
specimens were removed from the system and the exposed specimens were
recovered and tested to assess the effects of exposure to leachate.
Retrieval consisted of bypassing the cells to be removed, disconnecting
them, flushing them with water, and then cutting open the cells.  Exposed
liner samples were stored in polyethylene bags to retain moisture until
testing could be completed.  The results of analyses and measurements of
physical properties of the exposed specimens are presented in Appendix B.
                                    14

-------
Ul
         7.5
         7.0
     " 6.5
        6.0
        5.5
UJ
fe
i
        5.0
       4.5
              O pH OF LEACHATE ADDED TO SYSTEM
              • pH OF LEACHAT€ REMOVED FROM SYSTEM
                                            1977
                                                      r
                                                      i
                                                      i
                                                     FIRST SET OF IMMERSION SAMPLES REMOVED
                                                                                      -1978-
                            100                20)                300
                                            ELAPSED TIME,  DAYS

                                  Figure 4.  Leachate pH during the Jjwiersion test.
                                                                              400
                                                                                                500

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    Table 2, based upon selected data from Appendixes A and B,  summarizes
the effects of eight months of immersion of the 28 liner materials in
leachate, compares the 11 different types of material, and shows the
ranges of leachate absorption and the retention of physical properties for
each type of material.

    The materials tested fell into three groups with regard to  swelling or
leachate absorption during the eight months:

    1.  Those with the greatest leachate absorption, which included the
        chlorosulfonated polyethylene and the chlorinated polyethylene
        liners (13% to 19% and 8% to 10%, respectively).   Neoprene and
        ethylene propylene rubber ranged from low to high absorption (1%
        to 19% and 1% to 13.5%, respectively).

    2.  Those with low leachate absorption, which included the  polyolefins,
        plasticized polyolefin, and polybutylene (all with 0.1% absorption),
        and polyethylene (with 0.6% absorption).

    3.  Those with relatively low leachate absorption, which included
        polyvinyl chloride (1% to 3%), polyester (2%), and butyl rubber
         (1% to 2%).

    The membrane liner of polyvinyl chloride plus pitch swelled 6%.

    Changes in physical properties generally followed swelling.  Those
specimens that swelled little changed relatively little in physical
properties.  The materials that exhibited significant drops in tensile
strength during the exposure period were neoprene, chlorinated polyethylene,
and chlorosulfonated polyethylene.  They were the materials that swelled
the most.  The polyolefins showed little loss, as did the polyvinyl chloride
liners.  In elongation at break, there was a similar effect, except that one
of the ethylene propylene rubber materials exhibited a significant loss when
tested in the transverse direction.  This material appeared to have cured
or crystallized during exposure, resulting in a substantial increase in
modulus.

    A general decrease in hardness and modulus of the liners occurred
during exposure, but  there were some increases, i.e., the ethylene
propylene rubber  discussed above and some specimens  of chlorinated poly-
ethylene and  chlorosulfonated polyethylene.

    Overall,  the  polyolefins and polyvinyl chloride  materials  changed  the
least during  the  immersion period.  As groups of materials, the polyvinyl
chloride membranes varied  the  least  during this time period and neoprene
and ethylene  propylene rubber varied the most.
                                     16

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    TABLE 2.
SUMMARY OF THE EFFECTS OF IMMERSION OF POLYMERIC MEMBRANE LINERS IN LEACHATE FOR 8 MONTHS
Polymer
Butyl rubber
Chlorinated
polyethylene
Chlorosulfonated
polyethylene
Elasticized polyolefin
Ethylene propylene
rubber
Neoprene
Polybutylene
Polyester elastomer
Polyethylene
Polyvinyl chloride
Polyvinyl chloride
+ pitch
a
No. of
liners
in test
1

3

3
1

5
4
1
1
1
7

1
Absorption
of leachate,
%
1-2

8-10

13-19
0.1

1-13.5
1-19
0.1
2.0
0.6
1-3

6.0
% Original value
Tensile strength
90-97

80-115

82-124
86-94

90-91
69-100a
96-99
99-115
110-180
91-110

92
for unexposed
Elongation
104-106

64-135

97-107
91-92

76-138
82-103a
96-97
101-108
96-181
98-129

109-133
membrane
S-200
85-86

84-123

47-113
102-106

98-220
79-102a
99-103
95-110
100-116
76-102

93-108b
Change in
hardness ,
points
0

-5 to -1

-20 to -4
0

-1 to +2
-11 to +5
-3
-4
— 7
-2 to +1

-2
^     on fabric-reinforced neoprene liner #42 were not included.
 S-100 - unexposed specimen broke at 150% elongation.

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    As indicated above, there were considerable variations among the speci-
mens of a given polymer type, as shown in Table 2 and Appendix B.  These
variations within a single polymer group point out the importance of other
factors in addition to the polymer that determine the properties of a given
liner composition.  For example, swelling would be greatly affected by
crosslinking, percent of crystallinity, and the type and amount of fillers
used.  Minor amounts of other constituents, such as soaps and occluded salts
from the preparation of the polymer can also affect swell.

    Two additional sets of the same 28 polymeric liner materials remain in
the immersion tanks.  These will be retrieved and tested after immersion
periods of 19 and 30 months.

WATER VAPOR PERMEABILITY OF POLYMERIC MEMBRANE LINING MATERIALS

    The very low permeabilities of polymer membrane liners, compared with
those of soils and admix liner materials, have made it difficult to obtain
compatible permeability data for all these materials.  Polymeric membrane
liners are nonporous.  Therefore, the rate of transmission of a liquid,
such as water, depends upon its solubility in the liner and the rate of
diffusion of the molecules of the liquid  through the liner.  Permeameters
normally used for soils are not applicable for measuring the permeability
of membranes.  Consequently, the polymeric membrane liner industry has been
using water vapor transmission as a measure of the permeability of polymeric
liners.  This type of  test was used to determine the permeability of the six
polymeric membranes  that are being exposed as the primary liners sealed in
the bottoms of the leachate generators  (2).

Test Method

    The test method  used in  our initial  measurements basically  followed
ASTM E-96, "Water Vapor Transmission of  Materials in Sheet Form,"  Method
BW  (5).   In this  test  a small water cup  with  a membrane  specimen cover is
inverted  to wet the  specimen  (Figure 5).   The cup in the  inverted position
is  placed in  a box having  controlled temperature, humidity, and air  stream,
and its  loss  in weight is  observed as  a  function of time.  This test is
intended  for  those  applications in which one  side is wetted under  conditions
where  the hydraulic  head is  relatively  unimportant and  the moisture  transfer
 is  governed by  capillary and water vapor diffusion forces.  The driving
 force  is  supplied by the difference in the vapor pressure on  the two sides
 of  the membrane.

     The conditions  under which  these  tests were  initially performed were
 at  variance  with  those specified  in the ASTM Test Method E-96,  leading to
high absolute values of vapor transmission.   In  particular,  the relative
 humidity on  the outside  of the  cups was significantly  less  than 50% and
 the air velocity  was substantially higher than that  called  for in  the
 method.  The relative values,  however, are valid (Table 3).
                                     18

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              CUP IN  INVERTED
                 POSITION
      COP
            TEST  SPECIMEN
            SEALED  IN CUP
                                                          WAX FOR SEALING
                                                           LINER IN CUP
                                                            HOT PLATE FOR
                                                             HEATING  WAX
                                                         MOLD FOR MAKING
                                                           RING SEAL
                             TEST SPECIMEN
Figure 5.  E96 water vapor permeability cup and auxiliary equipment.

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           TABLE 3.  EFFECTS OF TEST CONDITIONS ON WATER VAPOR PERMEABILITY  OF POLYMERIC MEMBRANE LINERS
ro
o
Rate of Water vapor Water vapor
•water vapor permeance, permeability,
transmission, 10~2 g/d-m2-mmHg 10"^ g/d-m2-mmHg-cm
g/d-m2 (metric perm) (metric perm-cm)
Liner Thickness Test conditions Test conditions Test conditions
Polymer
Chlorinated
polyethylene
Chlorosulfonated
polyethylene
Polyvinyl chloride
No. mils cm ASTMa Ref.2D ASTMa Ref.2D ASTMa

12 33.3 0.085 0.264 0.610 2.10 4.60 1.76

6 37.0 0.094 0.422 0.825 4.21 6.20 3.79
17 20.0 0.051 2.97 3.69 24.4 27.7 12.0
Ref . 2"

3.70

5.70
15.0
     aResults of  tests  made  under  conditions  specified in ASTM E96 (data from Table 4).

     bResults of  tests  made  in low relative humidity and high air flow (data from Ref.  2).

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    To comply with the test conditions of the ASTM method, we constructed
a small cabinet  (Figure 6), to hold the cups.  The cabinet has a built-in
controlled air flow and is operated in a constant-temperature and humidity
room controlled at 72 - 1°C and 50 - 2% relative humidity.  The effect of
the change in test conditions on the water vapor transmission values is
shown in Table 3.  The values for water vapor transmission and permeability
are significantly lower when the tests are run under the ASTM conditions,
than under the conditions  existing in the previous tests, (2). This probably
reflects the higher relative humidity and lower air velocity of the ASTM
conditions.  The driving force for transmission increases with increasing
difference in humidity on  each side of the membrane.

Results
    The water vapor permeability of 27 membrane liners, including three
previously tested, were then determined and the results are presented in
Table 4.

    The polyester liner, which was the thinnest membrane in the series with
a thickness of eight mils, had the highest rate of water vapor transmission.
However, its water vapor permeability, which corrects for thickness and is
a property of the liner polymer, is in the same range as that of polyvinyl
chloride compositions, some of which are considerably more permeable.  There
is a threefold variation from the lowest permeability to the highest in the
case of polyvinyl chloride liners.  As a group the polyvinyl chloride liners
are the most permeable, confirming the results given in the Second Interim
Report  (2).  The most impermeable materials in this test series are
elasticized polyolefin or butyl rubber, both of which have less than one-
tenth of the water vapor permeability of polyvinyl chloride.  There is a
considerable spread in the values for butyl rubber (Table 4) indicating
compound differences.  The other liner materials are intermediate in water
vapor permeability,  with a possible twofold variation among them.

    Swelling of polymeric compositions, such as that anticipated for
polymeric liners exposed to leachate for long periods, generally increases
permeability.   Consequently,  running the permeability tests for long periods
should result in some swelling of the test specimens and higher permeability.
Table 5    presents  such results for 11 liner specimens.  Permeability
values obtained from the 35th to the 63rd day are compared with those
obtained before the  35th day.  In all cases, values determined in the 35th
to 63rd day interval are higher than those that were determined in the
7-to 28-day interval.  Furthermore,  the increases tend to follow the
respective tendencies of the  liner specimens to swell in water.  Additional
testing of the effect of swelling on permeability is planned with pre-
swollen specimens.
                                    21

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to
                  Figure 6.   Constant-air-velocity  cabinet for holding  E96  permeability cups.
                             The cabinet is operated in a constant-humidity room having a
                             temperature of 73 F and a relative humidity of 50%.

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           TABLE 4.   WATER VAPOR PERMEABILITY OF POLYMERIC MEMBRANE LINERS,  ASTM E-96,  METHOD
Polymer
Butyl rubber

Chlorinated poly-
ethylene



Chlorosulfonated
polyethylene


Elasticized
polyolefin
E thyle ne-propyle ne
rubber




Neoprene



Polyester elastomer
Polyvinyl chloride






Liner
No.
22
57

12
38
77
86

3
6b
55

36

8
18
26
41
83
9
42
43
82
75
11
17
19
40
59
88
89
Thickness
mils
73.?
33.5

33.3
32.3
31.0
21.0

31.0
37.0
35.0

28.3

67.0
48.5
38.0
20.0
37.0
61.0
20.0
31.5
61.2
8.0
30.0
20.0
21.0
32.5
33.0
20.5
11.0
cm
0.185
0.085

0.085
0.082
0.079
0.053

0.079
0.094
0.089

0.072

0.170
0.123
0.097
0.051
0.094
0.159
0.051
0.080
0.155
0.020
0.076
0.051
0.054
0.083
0.084
0.052
0.028
Test
time,
days
49
21

28
21
21
28

32
40
42

28

28
28
28
21
28
21
42
28
63
21
28
35
42
42
21
35
35
Rate of
water vapor
tr ansmis s ion ,
g/d-m2
0.097
0.020

0 . 264
0.361
0.320
0.643

0.634
0.422
0.438

0.142

0.172
0.314
0.327
0.270
0.190
0.237
0.304
0.448
0.240
10.50
1.85
2.97
2.78
4.17
4.20
2.94
4.42
Water vapor
permeance,
10~2 g/d-m2. mmHg
(metric perm)
0.75
0.17

2.10
2.90
2.80
5.10

5.00
4.21
3.47

1.20

1.40
2.49
2.80
2.15
1.50
1.90
24.1
3.90
2.00
91.0
16.0
24.0
22.0
33.0
36.0
23.0
35.0
Water vapor
permeability,
10" • g/d-m -nrnHg-cm
(metric perm-cm)
1.39
0.15

1.76
2.35
2.10
2.72

3.97
3.79
3.09

0.85

2.52
3.07
2.72
1.09
1.42
2.89
1.22
3.12
3.11
18.2
12.2
12.0
11.8
27.3
30.2
12.1
9.77
faAverage temperature, 72°F; average relative humidity, 42%.
 Fabric-reinforced.

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TABLE 5.  EFFECT OF TEST TIME ON WATER VAPOR PERMEABILITY OF MEMBRANES IN
                               E96-BW TEST
Polymer
Butyl rubber
Chlorinated polyethylene
Chlorosulfonated
polyethylene
Elasticized polyolefin
Ethylene propylene rubber
Neoprene
Polyester elastomer
Polyvinyl chloride
Liner
no.
57
77
6°
36
8
26
43
82
75
11
59
Permeability
metric perm- sec x 10".
7-28 daysa
0.18
2.63
2.07
1.09
2.87
3.40
3.90
1.61
1.14
15.25
38.21
35-63 days0
0.22
2.87
2.57
1.18
3.11
3.68
5.14
38.5
1.18
17.09
40.98
% Increase
22
9
24
8
8
8
32
139
3
12
7
 aTemperature,  72°F; relative humidity, 54%, AP, 9.23.
  Temperature,  74°F; relative humidity, 55%; AP, 9.65.
 °Fabric  reinforced.
BAG TEST FOR ASSESSING MEMBRANE LINER MATERIALS

    As the permeability of membrane liners to water and to other leachate
components under landfill conditions is not necessarily reflected by the
water vapor permeability as determined by E-96, other methods of assessing
the permeability of liner materials are, therefore, being investigated:

    1.  Sealing leachate into bags fabricated from the liner membranes and
        immersing these bags in deionized water.  The permeation of
        dissolved leachate components into the deionized water can be
        observed through pH and conductivity measurements and changes in
        weight of the filled bags.

    2.  Testing liner specimens in a top-pressure permeameter in which air
        pressure of one or more atmospheres can be placed on a layer of
        water or leachate covering a liner material.

    3.  Determining the permeabilities of membrane liners after swelling
        specimens in water at room temperature and at 70°C to simulate
        long exposure to leachate.
                                     24

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    The  first of these methods is discussed and results are presented.

    Initial experiments carried out with various heat-sealable liner
materials demonstrated the feasibility of the test procedure.  Two series
of bags were then fabricated of heat-sealable lining materials.  One set
was filled with leachate and the second set with 5% sodium chloride.  The
liner materials in these tests include the following polymers:  chlorinated
polyethylene, chlorosulfonated polyethylene, elasticized polyolefin,
polyester elastomer and polyvinyl chloride  (3 different membranes).

    Figure 7 shows a schematic of the bag assembly and Figure 8 is a
photograph of the bags and the necessary testing equipment.

    The individual bags for the leachate were 20 x 14 cm, which gave an
exposable surface of approximately 560 cm2.   For the sodium chloride
solution the bags were 17 x 12 cm, which yielded an exposable surface of
approximately 400 cm2.

    Each bag was constructed with a neck through which the test fluid is
introduced.   After the bag is filled,  the neck is  heat sealed.  Leachate,
(100 ml), of the composition shown in  Table  6, and 305-490 ml of 5% salt
solution were added to the respective  bags.
              TABLE 6.  CHARACTERISTICS OF LEACHATE IN BAGSa
                        Property                      Value

              Total solids, %                           2.0

              Total volatile solids,  %                  1.1

              Chemical oxygen demand,  g/1              35.7

              Total volatile acids,  g/1                15.2

              PH                                       5.15b
              Conductivity, Umho                     11,500

              a
               Amount of leachate in  each bag is 100 ml.
               Samples were taken from the blend of leachates
               collected on November  8,  1976.
               Average value for the  leachates taken from the
               12 generators.
   The following tests were performed during the exposure of these bags:

   1.  The deionized water was tested periodically for pH, conductivity,
       and for the odor of butyric acid, in the case of the inner bags
       containing leachate.
                                   25

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                                                       INNER BAG
                                                       MEMBRANE  UNDER TEST
                                                            LEACHATE OR
                                                            NaCI SOLUTION
                                                            (INSIDE INNER BAG)

                                                            DEIONIZED WATER
OUTER BAG
POLYBUTYLENE
 Figure  7.   Schematic of osmosis bag assembly,  showing  inner bag made of
            membrane material  under test.  The inner  bag  is filled with
            leachate or 5% salt solution and sealed at  the neck.  The
            outer polybutylene bag, which can be easily opened, is filled
            with deionized water.  The water in the outer bag is monitored
            for pH and conductivity; the inner bag is monitored for weight
            change.
                                   26

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Figure 8.  Osmosis bag and auxiliary equipment for monitoring.
                           27

-------
     2.  The bags  containing the test  fluid were removed periodically  from
        the water and weighed.

 Results of the  tests after extended exposures are given in Tables  7-10.

     In the case of the bags containing  leachate, after 500 days  of exposure
 it was apparent that there was movement through the  liner by both  the water
 and  the dissolved ingredients of  the  leachate  (Table 7).  An increase in
 electrical conductivity  occurred,  indicating the permeation of some ions
 from the  leachate into the deionized  water.  Also, there was an  increase in
 the  weight of the bags containing the leachate, indicating permeation of
 water into the  bags containing leachate.  In.this series, the elasticized
 polyolefin yielded the lowest transmission of water  and of dissolved
 components and  the chlorinated polyethylene appears  to be the most
 permeable.  The order of the liner materials is shown in Table 8 for
 increasing conductivity  of the deionized water and for the increase in
 the  weight of the bags -shown in Table 8.


      TABLE 8.   TESTS  OF  BAGS  CONTAINING LEACHATE  - ORDER OF LINERS BY
        INCREASING BAG WEIGHT  AND BY CONDUCTIVITY  OF  DEIONIZED WATER


Order of          Conductivity of
increase          deionized water                      Weight  of  bag

    1     Elasticized polyolefin  (#36)    Elasticized polyolefin  (#36)

    2     Polyvinyl chloride (#59)        Polyvinyl chloride (#11)

    3     Polyvinyl chloride (#11)        Polyvinyl chloride (#59)
    4     Polyester elastomer (#75)       Polyvinyl chloride (#17)

    5     Chlorinated polyethylene (#77)  Polyester elastomer (#75)

    6     Polyvinyl chloride (#17)        Chlorinated polyethylene  (#77)
     Somewhat similar results  were obtained when the inner bags were filled
 with 5% sodium chloride solution (Table 9).  Again, the elasticized poly-
 olefin was the most impermeable of the liners and one of the polyvinyl
 chloride membranes (#11)  was  the second most impermeable.  The order
 for the liners in this set is shown in Table 10 for increasing conductivity
 of the deionized water and increasing weight in the bags.
                                     28

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to
                            TABLE 7.  TESTS OF MEMBRANE LINER BAGS FILLED WITH LEACHATE - PERMEABILITY
                                           OF MEMBRANES TO WATER AND TO IONS DUE TO OSMOSIS
Original values Values at 70 days Values at 500 davs
Conduc- Weight of Conduc- Weight Conduc-
Liner w tivityb, filled bag, tivity*1, increase0, tivitA
Polymer no. pH* ymho g pHb umho g pHb pmho
Chlorinated
polyethylene 77 5.7 5.2 170.91 5.8 29.7 1.68 6.5 124.0
Elasticized
polyolefin 36 5.1 4.3 142.63 5.0 9.82 -0.07 4.5 17.8
Polyester
elastomer 75 4.0 20.5 112.25 3.5 73.0 0.58 6.4 50.0
Polyvinyl
chloride 11 5.8 6.0 166.88 4.4 30.9 0.41 6.0 32.0
Polyvinyl
chloride 17 5.0 13.3 138.28 2.9 310.1 0.33 2.8 325.0
Polyvinyl
chloride 59 5.7 5.9 170.14 3.8 61.5 0.97 6.3 23.2
Blank " 5'5 1-33 - 5.7 1.75 - 4.3 11.6
Weight
increase ,
g

4.74

0.22

2.95

1.12

1.37

1.21
—
a 	 ^ — ~ 	 •• 	 — 	 — — — — 	
       bArea of each bag exposed to test fluid is 560 cm.
       CPH and conductivity of deionized water outside the bags  containing  leachate.
        Weight increase of bags containing leachate.

-------
CO
o
                   TABLE 9.   TESTS OF MEMBRANE LINER BAGS  FILLED WITH 5% NaCl SOLUTION -

                              PERMEABILITY OF LINERS  TO WATER AND TO IONS DUE TO OSMOSIS
Polymer
Chlorinated
polyethylene
Chlorosulfonated
polyethylene
Elasticized
polyolefin
Polyester elastomer
Polyvinyl chloride
Polyvinyl chloride
Blank
Line;
no.
77
6
36
75
11
59
—
Original
Conduc-
tivity13,
ymho
1.92
3.48
1.51
1.62
1.67
1.77
0.63
values
Weight of
filled bag,
g
370.91
391.02
329.50
424.35
479.81
537.80
—
Values at
Conduc -
tivityb,
ymho
23.3
86.0
9.5
22.9
13.7
19.5
7.8
113 days
Weight
c
xncrease ,
g
1.01
1.36
-0.02
2.61
0.26
1.07
"•" ""
Values at
Conduc-
tivity13,
Vimho
31.2
113.0
10.9
30.0
15.3
21.5
6.6
200 days
Weight
increase0 ,
g
+1.56
+2.20
+0.06
+5.30
+0.69
+1.86
"
        *Area of bag exposed to test fluid was 480 cm .

        ""conductivity of deionized water outside the test bags.

        'Weight increase of bags.

-------
   TABLE 10.  TEST OF BAGS CONTAINING 5% SALT SOLUTION - ORDER OF LINERS BY
              INCREASING BAG WEIGHT AND BY CONDUCTIVITY OF DEIONIZED WATER

Order of          Conductivity of
increase          deionized water                       Weight of bag

    1      Elasticized polyolefin (#36)a       Elasticized polyolefin (#36)

    2      Polyvinyl chloride (#11)             Polyvinyl chloride (#11)

    3      Polyvinyl chloride (#59)             Chlorinated polyethylene (#77)
    4      Polyester elastomer (#75)            Polyvinyl chloride (#59)

    5      Chlorinated polyethylene (#77)       Chlorosulfonated polyethylene
                                                 (#6)

    6      Chlorosulfonated polyethylene (#6)   Polyester elastomer (#75)
_^                                                         .  ___         .
 Membrane liner identification number.


     After the completion of individual tests, the bags will be cut,
 physical properties of the liner materials will be determined, and the
 leachate will be analyzed.

     This may be a good laboratory test for assessing membrane liner
 materials.  It is planned to extend this work to include additional membrane
 liners, including rubber membranes which must be cemented.  A similar series
 of tests is now underway on various hazardous wastes.

 WATER ABSORPTION OF MEMBRANE LINER MATERIALS

     The swelling of a rubber or plastic membrane liner generally results
 in a reduction of desired physical  properties as well as an increase in
 permeability.   Severe  swelling over a long period of time could ultimately
 cause the failure and  non-performance of a polymeric liner material.  When
 materials are  evaluated for specific liner applications their swelling
 should be studied under various conditions.

     During the first year  of exposure in  the  simulated landfills,  some  of
 the specimens  showed significant absorption of leachate.   A concurrent  test
 run in the laboratory  of some of the same  liner materials in water showed
 similar absorption,  although the order of  increasing swell was  not the
 same.   These data were presented in  the Second Interim Report (2),  along
 with absorption  data run at 100°C.   Raising the test temperature during
 immersion accelerated  the  rate  of water absorption.   It was hoped  that a
 short-term test  of two hours would indicate the swelling  characteristics
 of a liner material, but the results did not  correlate  with either the room
 temperature data or  with the cell exposure.
                                     31

-------
    The  temperature used was  felt to be  too high.  Consequently,  another
 series of  swell  tests was  run,  in accordance with ASTM  D570,  at room
 temperature  and  at 70°C.   The results  of swelling up  to 100 weeks are  shown
 in Table 11.   Generally, the  immersion at room temperature and at 70°C
 resulted in  essentially the same order of increasing  swelling; the cor-
 relation was significantly better than immersion at 100°C, as shown in
 Table 12.
            TABLE 12.  ORDER OF INCREASED SWELLING IN WATER
                         AT ROOM TEMPERATURE AND AT 70°Ca
Order of
increased
swelling
At room temperature
                                     At 70°C
    1       Polyvinyl chloride  (#11)

    2       Polyester elastomer (#75)

    3       Ethylene propylene rubber  (#8)

    4       Ethylene propylene rubber  (#26)

    5       Polyvinyl chloride  (#59)

    6       Elasticized polyolefin  (#36)

    7       Butyl rubber  (#57)
    8       Chlorinated polyethylene  (#77)

    9       Chlorosulfonated polyethylene
              (#6)
                             Polyester  elastomer  (#75)
                             Elasticized  polyolefin (#36)

                             Ethylene propylene rubber  (#26)

                             Ethylene propylene rubber  (#8)

                             Polyvinyl  chloride (#59)

                             Polyvinyl  chloride (#11)

                             Butyl rubber (#57)
                             Chlorinated  polyethylene (#77)

                             Neoprene (#82)
10
11
Neoprene (#43)
Neoprene (#82)
Chlorosulronatea poxyetnyj-ene
(#6)
Neoprene (#43)
  ASTM D570.
     One of the major differences in the results obtained at the two tem-
 peratures was in one of the polyvinyl chloride liners which at room
 temperature yielded the lowest swelling, but at 70°C was sixth in swelling.
 The materials that had the lowest swell were polyvinyl chloride, elasticized
 polyolefin, and ethylene propylene rubber.  Those swelling the most were
 neoprene, chlorosulfonated polyethylene, and chlorinated polyethylene.
 These exposures are being continued and will be supplemented by limited
 physical testing of the highly swollen materials to determine the relation-
 ship of physical properties to the degree of swelling.
                                     32

-------
        TABLE 11.  WATER ABSORPTION OF SELECTED MEMBRANE  LINER  MATERIALS AT ROOM TEMPERATURE AND AT 70
                                                                                                       o_a
to
Co

Water absorbed. %
At room temperature
Polymer
Butyl rubber
Chlorinated polyethylene
Chlorosulfonated poly-
ethylene
Elasticized polyolefin
Ethylene propylene rubber
Neoprene
Polyester elastomer
Polyvinyl chloride
Liner
No.
57
77
6
36
8
26
43
82
75
11
59
1
week
0.82
1.63
3.44
0.39
0.50
1.20
3.80
2.43
1.07
1.29
1.59
11
weeks
3.22
5.53
6.97
0.52
1.30
1.84
13.62
8.29
1.05
1.10
2.34
44
weeks
4.50
10.2
10.9
0.0
1.56
1.49
37.8
18.5
0.67
0.70
2.43
100
weeks
6.4
12.5
16.3
4.5
2.25
2.56
75.1
32.1
1.31
1.25
2.98
1
day
2
3
5
0
0
0
3
2
1
1
2
.04
.04
.68
.24
.42
.74
.89
.49
.18
.51
.09
by weiaht

1
week
4.62
15.9
22.1
0.36
1.11
1.44
14.1
8.11
1.28
5.59
4.87
At 70°C
11
weeks
17.54
58.4
131.0
0.45
3.55
4.52
107.0
47.4
1.10
12.13
8.25

44
weeks
53.9
140.0
245.6
0.57
10.8
11.20
240.0
191.4
0.72
39.2
24.0

100
weeks
103.2
179.3
370.5
8.7
17.8
17.4
(b)
295.0
0.22
87.4
25. 5C

     OL  ___
      ASTM D570-63 specimens 1x2 in. in deionized water.

      Specimens began to disintegrate between 44th and 69th weeks.

      Specimens have become hard, indicating loss of plasticizer.

-------
    The immersion tests described earlier also furnish information for com-
parison with these swelling data.  In Table 13, for example, liners that
have been swollen in both water and leachate are compared.  The liner
materials immersed in the leachate swelled significantly more in 32 weeks
than did the same materials immersed in deionized water for 44 weeks.  This
difference is probably due to the organic content of the leachate.
      TABLE 13.  COMPARISON OF THE SWELLING OF MEMBRANE LINING MATERIALS
                      IMMERSED IN WATER AND IN LEACHATE

Polymer
Chlorosulfonated polyethylene
Elasticized polyolefin
Ethylene propylene rubber
Polyester elastomer
Polyvinyl chloride
Liner
no.
6
36
8
75
11
Swelling,
In water
for 44 weeks
10.9
0
1.6
0.67
0.70
%
In leachate
for 32 weeks
13.3
0.1
6.0
2.0
2.9

    Extended exposures at 70 C were run to determine whether there is a
tendency on the part of liner materials to reach a plateau of swelling with
respect to time.  Chlorinated polyethylene and ethylene propylene rubber
appeared to have essentially plateaued.  One of the polyvinyl chloride
liners appeared to have come to a maximum value; however, it hardened,
presumably from loss of plasticizer.  The neoprene and chlorosulfonated
polyethylene specimens appeared to continue to swell.  The elasticized
polyolefin absorbed little during the first 400 days; after that, it began
to swell.  This swelling test of the liners is being continued.  Also, one
of the three specimens of each of the polyvinyl chloride liners will be
analyzed for loss of plasticizer.

MONITORING THE LEAChATE GENERATORS

    In November 1975, after one year of operation. 12 of the 24 original
leachate generators - liner exposure cells were disassembled and the
exposed liner specimens were recovered and tested  (2, 4).  Monitoring of
the 12 remaining generators has continued:

    1.  Every two weeks, 2 gal tap water were added to simulate 1 in.
        rainfall.  Over the year, this is equivalent to 26 in. of rain
        entering the landfill, a condition which exists in the Pacific
        northwest.
                                     34

-------
      2.   Records were made of leachate output,  ambient temperature,
          temperature within two generators,  and level of refuse and
          cover within the generators.

      3.   The leachate was analyzed approximately once a month for percent
          total solids,  percent volatile solids,  total volatile acids,
          chemical oxygen  demand,  and pH.

      4.   The seepage of the  leachate through  the liner was measured.

  Collection  of Leachate

      The  leachate  is  collected continuously in bags prepared  from polybuty-
  lene.  These  bags replaced  the polyethylene bags that failed at  the heat-
  sealed seams.  A  constant head of  1 ft of leachate was maintained by
  allowing the  leachate to pass through an inverted U-tube placed  in the out-
  flow line at  1 ft above the lining.  During recent months, gas was generated
  in the bases  and bags causing the bags to inflate.  To prevent a buildup of
  excess pressure and  failure of the  bags, relief valves were  installed, as
  shown in Figure 9.  Since the installation of these valves there has been
  no leakage of the bags.

  Leachate Characteristics

     The leachate has been analyzed on approximately a monthly basis  since
 the cells reached "field capacity" in November 1974.   Average analytical
 results for solids,  pH, volatile acids, and chemical  oxygen damand are
 presented in Figures 10 through 13, respectively.  During the first  year
 of operation, the characteristics of the leachate remained constant  except
 the volatiles acid content,  which increased.   Since that time, there has
 been a reduction in  the solids,  total  volatile  acids, and chemical oxygen
 demand,  and a rise in pH.   The early leachate contained a relative high
 concentration of butyric  acid, which seems  to be essentially  absent  in the
 more  recent  leachate.

 Consolidation of Refuse

    During the course of  the operation  of the generators,  considerable
 consolidation of  the shredded  refuse has occurred within  the  generators,  as
 shown in  Figure  14.   This  consolidation has been essentially  linear with
 time, although there  are indications that this consolidation  is slowing
 down.  At the  end  of  180 weeks of leachate production,  the consolidation
 averages  about 16% for the refuse in the 12 generators.

 Seepage of Leachate

    One of the primary design features of the leachate generator - exposure
 cells is the capability of their functioning as  large permeameters.  The
 liner specimens were sealed in the bases of the generators to prevent by-
passing of the liners.
                                    35

-------
VENTED TO ATMOSPHERE f
                                                                                   1 FOOT ABOVE LINING
                                                                                   MOUNTED IN CELL
                                                                                  LEACHATE FROM
                                                                                  GENERATOR
                                                                 POLYBUTYLENE COLLECTION BAG
     Figure  9.  Leachate collection bag with water  seal and vent to prevent excessive gas  pressure build-
               up in the bag.  The seal prevents air from entering the bag and oxidizing  the leachate.

-------
LJ

O
O
V)
to
            NON-VOLATILE SOLIDS
                                                   1976
                                                 ELAPSED
                                          1978
TIME
      Figure  10.  Average solids contents of the leachate produced in the generators, November 1974 - May 1978
                 The data for November  1974 - November 1975 are the averages  for  the leachate from 24 generators
                 Twelve generators were disassembled in November 1975 and,  consequently, the data for December
                 1975 - May 1978 are  the averages for the leachates from the  12 remaining generators

-------
w    5.5--|
oo
4.5
                                                     1976
                                                  ELAPSED  TIME
                                                                                 1977
                                                                                                         1978
         Figure 11.   Average pH of the leachate produced  in the generators, November 1974  -  May  1978.  The data
                     from November 1974 - November  1975 are the averages for the leachates from  24 generators.  The
                     data for December 1975 to May  1978 are the averages for the leachate  from 12 generators.

-------
|1974|
Figure 12.
    1975
 1976
ELAPSED  TIME
1978
Average total  volatile acids content (TVA),  as acetic acid,  of  the leachate produced in the gen-
erators, November  1974 - May 1978.  The data for November  1974  - November 1975 are the averages
for the leachates  from 24 generators.  The data for December 1975 - May 1978 are the averages
for the leachates  from 12 generators.

-------
60
                                                                            1977
1978
   Figure 13.
                                 1976            |
                               ELAPSED TIME
Chemical oxygen demand (COD) of the  leachate produced in the generators,  November 1974 - May 1975.
The data for November 1974 - November 1975 are the averages for the leachates  from 24 generators.
The date for December 1975 through May 1978 are the averages for the leachates from 12 generators.

-------
0
                                              ELAPSED  TIME

 Figure 14.   The average refuse consolidation  in the leachate generators, November 1974 - May 1978.  The data
             for November 1974 - November  1975 are averages for the refuse in the 24 generators.  The data  for
             December 1975 and later are the averages for the consolidation in  12 generators.

-------
     A constant head of one ft of leachate is maintained above the liner to
 supply a driving force for the fluids through the liner specimens.   Perme-
 ability of the liner can, therefore, be determined by collecting the
 leachate below it.

     The results of the cumulative collection of the leachate below the
 liner specimen is reported in Table 14.  The seals in two of the generators,
 #1 and #3, in which polyethylene and butyl rubber are being exposed
 respectively, appear to have failed.  The epoxy resin that was used to make
 the seal probably disintegrated in much the same fashion as occurred in two
 of the first 12 generators that were previously dismantled.  The mercaptan
 epoxy resin that was used to achieve rapid set does not have high chemical
 resistance and is sensitive to off-ratios between the resin and hardener.
 Although the leachate is being collected from drains below these liners,
 it is still being ponded on the liners to keep them immersed in leachate.
 The remaining cells appear to be functioning properly with only three
 showing seepage; i.e., polyvinyl chloride, soil cement, and soil asphalt.
            TABLE 14.   CUMULATIVE COLLECTION OF LEACHATE BELOW
                       LINERS MOUNTED IN BASES OF GENERATORS3

Generator
no.
1
2
3
4
5
6
7
8
9
10
11
12
Liner Material
Polyethylene (#21)b
Polyvinyl chloride (#17)
Butyl rubber (#7)
Chlorosulfonated polyethylene (#6)
Ethyl ene propylene rubber (#18)
Chlorinated polyethylene (#12)
Paving asphalt concrete (2 in. thick)
Hydraulic asphalt concrete (2 in. thick)
Soil cement (4.5 in. thick)
Soil asphalt (4 in. thick)
"Cat" blown asphalt membrane (0.25 in. thick)
Emulsion asphalt on fabric (0.25 in. thick)
Amount of leachate
collected, kg.
(c)
1.27
(c)
0
0
0
0
0
0.23
1.33
0
0

^From November 21, 1974, to May 31, 1978.
 Membrane liner identification number.
 Leachate appears to be by-passing the liners and is being collected from
 drains below the liners.
                                      42

-------
     At the conclusion of the exposure  (now planned for June 1979) , it will
 be possible to determine whether there has been any failure in the liners
 or if, in fact, the epoxy resin seal disintegrated.

 RECOVERY AND TESTING OF SAMPLES OP A POLYVINYL CHLORIDE LINER FROM A
   DEMONSTRATION LANDFILL

     Information from the field regarding the performance of artificial
 lining materials on long exposure to sanitary landfill leachate has been
 very limited.   First, such use for these liners, particularly the polymeric
 membranes, is  relatively new, dating from the early 1970's.  Second,
 effective and economic methods of retrieving specimens and repairing
 linings at the bottoms of landfills have not been developed.

     A demonstration landfill in Crawford County, Ohio, placed in the spring
 of 1971,  was  lined with a polyvinyl chloride liner.   The liner from this
 landfill  was  relatively accessible  as the total fill  contained one lift of
 8 ft of refuse and was about 12 ft deep,  including the cover.   This
 demonstration  landfill had been designed to compare  conventionally processed
 solid waste with rough and compacted wastes.   The  various  types of refuse
 had been  placed in essentially waterproof cells lined with plastic membranes.
 The effect of  water content on consolidation and decomposition of the  refuse
 was to be determined.   However,  all of  the cells were  flooded  with water in
 a heavy rainfall just before the fill was closed.  Thus, the original
 objectives could not be  met and the project  was terminated.

     In view of the relative accessibility of  the liner,  the  landfill was
 opened in May  1977,  after  six  years,  and  the  membrane  liner  was recovered.
 The cells appeared to have  retained the water.   The condition  of  -the refuse
 did not appear to  be  typical of  sanitary  landfills.  The odor  was  mild,  and
 the refuse showed  little deterioration.   The  samples of  liners  recovered
 from the  cells  appeared  to be  in excellent condition with  little  difference
 apparent  between samples taken from the top of  the cell, above  the refuse,
 and those taken  from the bottom, below the refuse.  The top  liner  had been
 under  3 ft of  clay  cover, and the bottom  liner had been under  about 2 ft of
 clay and  was on top of pea gravel.  Both  liners had taken  the  shape of soil
 and gravel without breaking.  The depressions were as much as 6 in. deep
 in a 1 ft area in the exposed top liner.

    These samples were analyzed along with a sample of polyvinyl chloride
 sheeting that was thought to have been in the same lot as the material used
 for lining the cells.  However, the results,  (Table 15) show that  the two
 specimens taken from the fill were very similar and considerably different
 in composition from the unexposed sample, indicating that it was not a
 control for the liner.  As Table 16 and Appendix B show, the amount of
swelling and the decrease in properties of the lining were  within the spread
of values  observed in the leachate immersion test for seven polyvinyl
chloride materials.  The specimen taken from the bottom was probably not in
                                    43

-------
        TABLE 15.   ANALYSES OF POLYVINYL CHLORIDE LINER  RECOVERED
                   FROM DEMONSTRATION LANDFILL IN CRAWFORD COUNTY, OHIO

Property
Volatiles (2 h at 105°C) , %
Specific gravity (dry basis)
Ash (dry basis), ASTM D297, %
Extractables, ASTM D3421b, %
Pyrolysisc:
Polymer and organic
content, %
Polymer content, %
Carbon black, %
Ash, %

Unexposeda
liner
(#95)
0.10
1.379
10.26
7.54

80.6
73.1
8.6
10.9
Composition
Liner from
top of fill
(#96)
0.41
1.260
6.14
34.10

87.0
52.9
6.7
6.4

Liner from
bottom of fill
(#97A)
1.33
1.265
6.01
34.43

89.0
54.6
4.4
6.8
     Shelf, indefinite exposure in shop.
     Modified: 20 h refluxing with mixed solvent of carbon tetrachloride
     (CC1 ):methyl alcohol (CT^OH), 2:1.
    f-»
     Test method: Reference 6.

direct contact with the leachate in the fill during the 6 years it was in
place.  The 2 ft soil layer above the liner was a highly impermeable clay
having a permeability coefficient of 1.4 x 10~7 cm/sec.  The clay layer
and the weak leachate created a situation that was not typical of what
might be anticipated for a liner in a fullscale landfill.
                                     44

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Ui
                        TABLE 16.  PROPERTIES OF POLYVINYL CHLORIDE LINER  RECOVERED FROM A
                                   DEMONSTRATION LANDFILL IN CRAWFORD COUNTY, OHIO
Property
Thickness, mils
Tensile strength, psi
Elongation at break, %
Set at break, %
S-100, psi
S-200, psi
S-300, psi
Tear strength, ppi
Hardness (Duro A) , instant
Puncture resistance, Ib

Elongation, in.
Seam strength (shear) , ppi
Locus of failure
Test
method
—
ASTM D412
ASTM D412
ASTM D412
ASTM D412
ASTM D412
ASTM D412
ASTM D624
ASTM D2240
Fed Std 101
-B-2065

ASTM D413

Liner from
top of fill
(#96)
Machine
30
2665
340
66
1290
1830
2245
374
77

41.4
0.66
49.5
SEa
Transverse
—
2600
360
79
1245
1750
2300
370
—

—
—
—
—
Liner from
bottom of fill
(#97A)
Machine
28
2550
325
55
1185
1785
2400
343
78

37.3
0.65
45.5
BRKb
Transverse
__
2475
350
70
1085
1605
2205
341
— —

	
__
— —
	

              Break at seam.
              Break in tab.

-------
                                 REFERENCES
1.  Haxo, H. E.,  and R. M.  White.   First Interim Report:  Evaluation of Liner
    Materials Exposed to Leachate.  EPA Contract 68-03-2134,  unpublished,  1974.

2.  Haxo, H. E.,  and R. M.  White.   Second Interim Report: Evaluation of Liner
    Materials Exposed to Leachate.  EPA-600/2-76-255,  U.  S. Environmental Pro-
    tection Agency, Cincinnati,  Ohio, 1976.   NTIS No.:  PB259-913.

3.  Haxo, H. E. Assessing Synthetic and Admixed Materials for Lining Land-
    fills.  In:  Gas and Leachate from Landfills: Formulation, Collection and
    Treatment. EPA 600/9-76-004, U. S. Environmental  Protection Agency,
    Cincinnati, Ohio, 1976. NTIS No.: PB251-161.

4.  Haxo,H.E. Compatibility of Liners with Leachate.   In:  Management of Gas
    and Leachate in Landfills, Proceedings of the Third Annual Municipal
    Solid Waste Research Symposium, EPA-600/9-77-026, U.  S.  Environmental
    Protection Agency, Cincinnati,  Ohio, 1977. NTIS No.:  PB272-595.

5.  ASTM E96-66 (1972).  Tests for Water Vapor Transmission of Materials in
    Sheet Form. Parts 18, 20, 35,  and 41. American Society for Testing and
    Materials, Philadelphia, PA, 1977.

6.  Wake, W. C.  The Analysis of Rubber and Rubber-like Polymers.   Wiley In-
    terscience, New York, N.Y.,  2nd Edition, 1968.
                                      46

-------
             APPENDIX A.   PROPERTIES OF UNEXPOSED POLYMERIC MEMBRANES IN PROJECT
Item
b
Liner No.
Thickness, mils
Tensile strength, psi

Elongation at break, %

Set at break, %

S-100, psi

S-200, psi

S-300, psi

Tear strength, ppi

Hardness, Duro A:
Instant reading
10-sec. reading
Puncture resistance, Ib
Elongation, in.
Specific gravity
Ash (dry basis) , %
Volatiles, %
Exposure tests
Direction
of test

-
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse

_
-
-
-
-
-
-
Chlorinated
12
31
2460
2080
300
520
199
230
1220
520
1820
840
2460
1200
270
240

85
77
47.0
1.04
1.360
14.40
0.10
P,S,I
38
32
2190
2000
340
505
192
201
1345
565
1640
770
2005
1065
252
213

82
76
47.8
0.86
1.336
11.83
0.24
I
polyethylene
77
29
2055
2340
325
480
140
160
1240
560
1540
820
1955
1205
273
239

87
80
43.9
0.94
1.362
12.56
(d)
L,N
86
22
1845
1510
355
595
208
235
870
275
1210
405
1575
605
187
178

76
67
20.9
0.91
1.377
17.37
O'.OS
I
Chlorosulfonated
polyethylene
3C
31
1710
1430
580
640
370
380
670
520
850
620
1030
760
290
270

86
83
25.4
1.16
1.433
33.45
0.84
S,I
6C
32
1770
1610
240
225
78
79
990
895
1715
1445
-
-
317
287

79
75
34.4
0.57
1.343
3.35
0.29
P,S,I,N
85
33
2345
2055
260
325
167
192
1150
750
2130
1410
-
2020
308
277

83
79
47.8
0.86
1.311
4.02
0.92
I
See footnotes at end of table.
                                            47

-------
    APPENDIX A (Continued).   PROPERTIES OF UNEXPOSED POLYMERIC MEMBRANES IN PROJECT

a
Item
Liner No.
Thickness, mils
Tensile strength, psi

Elongation at break, %

Set at break, %

S-100, psi

S-200, psi

S-300, psi

Tear strength, ppi

Hardness, Duro A:
Instant reading
10-sec. reading
Puncture resistance, Ib
Elongation, in.
Specific gravity
Ash (dry basis) , %
Volatiles, %
Exposure tests
Direction
of test
_
-
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse

-
-
-
-
-
-
-
Ethylene propylene rubber
8
62
1635
1550
520
500
14
11
350
320
800
740
1170
1110
206
111

62
58
51.8
1.36
1.173
6.78
0.38
S,I
18
49
1510
1440
420
400
13
9
350
350
760
760
1120
1120
181
181

57
54
39.4
1.44
1.122
5.42
0.50
P,S,I
83°
39
1066
870
20
240
59
51
-
630
-
845
-
-
303
276

73
70
33.6
0.61
1.199
0.32
0.31
I
91
37
1790
1865
500
475
10
11
300
375
795
915
1220
1370
196
195

55
52
29.2
1.17
1.160
7.33
0.34
I
41
20
3290
2720
700
650
495
438
950
920
1060
1020
1230
1180
429
417

84
81
25.1
0.96
0.938
0.93
0.16
I
Butyl
rubber
44
62
1625
1570
415
470
18
18
335
280
750
615
1210
1020
201
221

59
54
39.5
1.17
1.176
4.28
0.46
I
See footnotes at end of table.
                                         48

-------
 APPENDIX A (Continued).   PROPERTIES OF UNEXPOSED POLYMERIC MEMBRANES IN PROJECT
a
Item
Liner No.b
Thickness, mils
Tensile strength, psi

Elongation at break, %

Set at break, %

S-100, psi

S-200, psi

S-300, psi

Tear strength, ppi

Hardness, Duro A:
Instant reading
10-sec. reading
Puncture resistance, Ib
Elongation, in.
Specific gravity
Ash (dry basis) , %
Volatiles , %
Exposure tests
Direction
of test
-
-
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse

-
-
-
-
-
-
-
Neoprene
9
60
2320
2090
340
340
11
13
640
560
1320
1150
2060
1830
220
210

71
66
58.7
1.16
1.500
12.98
0.76
S,I
37
73
2400
2330
265
290
2
3
765
570
1800
1470
-
2400
221
199

69
67
80.4
1.02
1.451
3.31
0.64
I
42°
19
17420
9580
25
25
2
2
-
-
-
-
-
-
1545
1802

74
73
124.6
0.37
1.302
27.70
0.86
I
90
37
2185
2010
415
415
26
25
565
550
1450
1225
1895
1700
207
196

68
61
44.9
1.01
1.388
4.67
0.37
I
See footnotes at end of table.
                                      49

-------
       APPENDIX A  (Continued).  PROPERTIES OF UNEXPOSED POLYMERIC MEMBRANES  IN PROJECT

a
Item
Liner No.
Thickness, mils
Tensile strength, psi

Elongation at break, %

Set at break, %

S-100, psi

S-200, psi

S-300, psi

Tear strength, ppi

Hardness, Duro A:
Instant reading
10-sec. reading
Puncture resistance, Ib
Elongation, in.
Specific gravity
Ash (dry basis) , %
Volatiles, %
e
Exposure tests

Direction
of test
_
-
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse

_
-
-
-
-
-
-

Polyvinyl
11
30
2800
2550
350
350
90
103
1355
1205
1980
1740
2585
2255
374
370

85
79
37.4
0.63
1.275
6.20
0.11
S,I,L,
N
17
20
2640
2520
270
290
68
77
1260
1130
2080
1850
-
-
353
317

81
76
25.8
0.69
1.264
5.81
0.09
P,S,
I,L
19
22
2780
2260
330
340
97
105
1150
1060
1890
1590
2620
2170
295
275

80
72
24.0
0.71
1.231
3.65
0.05
S,I

40
33
2935
2640
385
400
62
71
1235
1115
1825
1610
2445
2150
350
316

81
74
43.1
0.72
1.289
8.09
0.21
I

chloride
59
33
2505
2365
370
400
45
60
1020
895
1570
1355
2160
1860
306
287

80
71
37.3
0.78
1.280
6.94
0.31
L,N

67
22
3020
2765
385
415
192
207
1250
1110
1820
1585
2430
2135
340
297

81
75
27.8
0.68
1.245
6.70
0.03
I

88
20
3395
2910
325
335
102
101
1870
1600
2610
2190
3230
2770
463
470

85
80
28.6
0.56
1.255
2.80
0.17
I

89
11
3715
3085
315
325
196
205
1845
1530
2715
2195
3520
2880
408
391

87
82
17.0
0.48
1.308
5.67
0.03
I

See footnotes at end of table.
                                             50

-------
     APPENDIX A (Continued).  PROPERTIES OF UNEXPOSED POLYMERIC MEMBRANES IN PROJECT
a
Item
Liner No.
Thickness, mils
Tensile strength, psi

Elongation at break, %

Set at break, %

S-100, psi

S-200, psi

S-300, psi

Tear strength, ppi

Hardness, Duro A:
Instant reading
10-sec. reading
Puncture resistance, Ib
Elongation, in.
Specific gravity
Ash (dry basis) , %
Vola tiles, %
Exposure tests6

Direction
of test
-
-
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse

-
-
-
-
Poly-
ethylene
21
11
1700
2590
320
690
177
667
1270
1030
1470
1050
1680
1120
415
360

97
97
13.9
0.76
PVC +
pitch
52
80
1185
1005
150
175
36
18
1175
860
-
-
-
-
292
208

75
69
62.3
0.49
0.931 1.294
-
-
-

0.00
0.36
P,S,I,
C,G
9.46
0.39
I

a ~~
Tests performed were tensile, elongation, modulus and
tear strength, ASTM D624;
puncture ,
bASTMD297; vola tiles (weight loss in
cContractor ' s liner number
^Fabric-reinf orced .
.

FM 101B, No.
2 h at 105°C)


2065;
.


Elasticized
polyolefin
36
23
2645
2540
675
650
460
430
880
865
975
960
1145
1150
388
369

90
87
26.3
0.97
0.938
0.90
0.15
I,L,N

set, ASTM D412;
Polyester
elastomer
75
7
6770
6765
560
590
340
370
2715
2455
2880
2585
3610
3315
911
782

93
93
29.9
1.30
1.236
0.38
0.26
I,L,N

Duro A, ASTM
specific gravity, ASTM D297






Poly-
butylene
98
8
5625
5580
390
375
346
331
2330
2360
3035
3200
4405
4610
355
380

94
93.7
13.9
0.66
0.915
0.08
0.12
I,C

D2240;
; ash ,



C, leachate collection bags; G, used as liner of all generators; I, in immersion test;
L, leachate osmosis bag; N, NaCl osmosis bag,- P, primary test specimens; S, secondary
test (specimens buried in sand).
                                           51

-------
      APPENDIX B.   PROPERTIES OF MEMBRANE LINER MATERIALS AFTER 8 MONTHS IN LEACHATE
                   FROM SIMULATED MUNICIPAL SANITARY LANDFILLS.

Item
b
Liner No.
Thickness, mils
Leachate absorption, %
Increase in area, %
Volatiles, %
Tensile strength, psi

Elongation at break, %

Set at break, %

S-100, psi

S-200, psi

S-300, psi

Tear strength, ppi

Hardness, Duro A:
Instant reading
10-sec. reading
Puncture resistance, Ib
Elongation, in.
Specific gravity, dried
Ash (dry basis) , %
Direction
of test
-
-
-
-
-
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse

-
-
-
-
-
Chlorinated polyethylene
12
36.0
9.5
3.3
7.9
2190
1660
340
460
195
195
1115
480
1525
735
1960
1065
210
200

81
72
50.7
1.00
1.354
14.52
38
36.0
10.2
3.0
8.3
1940
1860
340
480
185
165
1170
455
1465
680
1825
1025
185
170

82
75
50.1
0.99
1.335
12.06
86
23.0
8.5
3.0
7.5
1850
1740
480
380
130
140
760
320
1080
500
1460
800
150
145

74
66
27.1
1.06
1.389
18.08
Chlorosulfonated
polyethylene
3°
34.0
19.2
7.0
18.6
1790
1700
580
620
250
265
365
250
500
290
665
375
170
160

67
63
38.5
1.86
1.393
33.88
6C
33.5
13.3
4.6
1.21
2190
1920
230
240
75
75
940
775
1930
1620
-
-
250
210

74
71
48.7
0.76
1.325
2.10
85
35.0
14.4
8.8
12.6
1980
1680
250
320
60
90
875
485
1690
1030
-
1600
220
205

77
73
54.5
0.96
1.294
2.63
See footnotes at end of table.
                                           52

-------
    APPENDIX B (Continued).   PROPERTIES OF MEMBRANE LINER MATERIALS AFTER 8 MONTHS
                             IN LEACHATE FROM SIMULATED MUNICIPAL SANITARY LANDFILLS.
a
Item
Liner No.
Thickness, mils
Leachate absorption, %
Increase in area, %
Vo la tiles, %
Tensile strength, psi

Elongation at break, %

Set at break, %

S-100, psi

S-200, psi

S-300, psi

Tear strength, ppi

Hardness, Duro A:
Instant reading
10-sec. reading
Puncture resistance', Ib
Elongation, in.
Specific gravity, dried
Ash (dry basis) r %
Direction
of test
-
-
-
-
-
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse

-
-
-
-
-
Ethylene propylene rubber
8
66.0
6.0
3.6
2.9
1700
1660
480
510
18
18
415
355
925
820
1305
1200
195
195

64
60
55.1
1.26
1.168
6.35
18
50.0
8.4
4.8
6.0
1360
1460
350
380
9
9
385
360
865
815
1235
1195
125
135

56
53
43.1
1.18
1.113
5.36
83C
36.0
2.8
1.2
3.0
990
920
240
330
50
75
930
665
960
845
-
890
285
280

74
70
27.8
0.51
1.194
0.30
91
36.0
20.9
13.5
12.7
3410
2380
460
360
20
15
730
330
1750
1355
2565
2085
160
165

58
54
27.5
1.12
1.110
6.38
41
19.5
0.5
-0.1
0.3
3080
2480
700
640
485
435
940
930
1070
1000
1225
1140
375
345

85
82
25.2
0.84
0.935
0.98
Butyl
rubber
44
67.5
1.8
0.3
1.4
1470
1520
440
490
20
25
295
240
635
540
1055
910
185
195

59
54
37.9
1.13
1.172
4.29
See footnotes at end of table.
                                         53

-------
APPENDIX B (Continued).   PROPERTIES OF MEMBRANE LINER MATERIALS AFTER 8 MONTHS
                         IN LEACHATE FROM SIMULATED MUNICIPAL SANITARY LANDFILLS

a
Item
b
Liner No.
Thickness, mils
Leachate absorption, %
Increase in area, %
Vo la tiles, %
Tensile strength, psi

Elongation at break, %

Set at break, %

S-100, psi

S-200, psi

S-300, psi

Tear strength, ppi

Hardness, Duro A:
Instant reading
10-sec . reading
Puncture resistance, Ib.
Elongation, in.
Specific gravity, dried
Ash (dry basis) , %
Direction
of test
-
-
-
-
-
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse

_
-
-
-
-
Neoprene
9
70.5
19.3
14.4
9.0
1720
1450
300
280
9
8
400
310
1060
890
1690
1470
105
95

59
55
63.9
1.21
1.436
10.58
37
72.5
1.2
0.4
2.1
2380
2340
260
300
3
4
770
580
1765
1500
-
2335
215
220

74
72
90.6
1.11
1.459
5.33
42C
20.5
13.2
0.8
13.3
13510
2800
20
50
1
5
-
-
-
-
-
-
1245
1285

73
71
82.5
0.35
1.275
26.31
90
37.5
7.1
4.5
7.2
2130
1890
400
390
25
25
310
405
1380
1110
1890
1625
170
155

68
60
49.6
1.05
1.388
4.51
See footnotes at end of table.
                                       54

-------
       APPENDIX B (Continued).  PROPERTIES OF MEMBRANE  LINER MATERIALS AFTER 8 MONTHS
                                IN LEACHATE FROM SIMULATED  MUNICIPAL SANITARY LANDFILLS.
Item3
Liner No.
Thickness, mils
Leachate absorption, %
Increase in area, %
Volatiles, %
Tensile strength, psi

Elongation at break, %

Set at break, %

S-100, psi

S-200, psi

S-300, psi

Tear strength, ppi

Hardness, Duro A:
Instant reading
10-sec . reading
Puncture resistance, Ib
Elongation, in.
Specific gravity, dried
Ash (dry basis) , %
Direction
of test
-
-
-
-
-
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse

-
-
-
-
-
Polyvinyl chloride
11
31.0
2.9
2.4
2.4
2940
2700
360
380
95
100
1330
1255
1915
1770
2505
2345
360
350

85
80
43.6
0.69
1.277
6.45
17
21.5
2.3
1.9
2.3
2560
2320
340
350
60
65
1150
990
1695
1440
2335
2000
300
305

79
74
32.5
0.78
1.268
5.39
19
21.5
1.6
1.9
0.9
2720
2490
380
440
80
105
1145
970
1680
1410
2170
1865
290
265

77
72
24.8
0.64
1.231
3.64
40
32.5
1.2
1.4
1.4
2670
2430
390
390
65
75
1105
980
1650
1470
2200
1955
315
275

82
75
45.5
0.80
1.287
6.63
67
22.0
1.6
0.4
1.4
2850
2660
380
440
85
110
1125
1010
1685
1460
2280
2000
285
285

80
74
29.8
0.73
1.246
5.39
88
20.0
1.0
0.5
2.4
3220
2660
340
360
90
100
1460
1140
2130
1665
2840
2275
345
330

84
79
28.7
0.60
1.251
2.81
89
11.0
2.5
1.1
2.3
3560
3160
310
350
90
110
1710
1455
2570
2165
3420
2870
340
320

87
83
20.1
0.70
1.288
5.59
See footnotes at end of table.
                                              55

-------
APPENDIX B (Continued).  PROPERTIES OF MEMBRANE LINER MATERIALS AFTER  8 MONTHS
                         IN LEACHATE FROM SIMULATED MUNICIPAL SANITARY LANDFILLS.
Itema
b
Liner No.
Thickness, mils
Leachate absorption, %
Increase in area, %
Volatiles, %
Tensile strength, psi

Elongation at break, %

Set at break, %

S-100, psi

S-200, psi

S-300, psi

Tear strength, ppi

Hardness, Duro A:
Instant reading
10-sec . reading
Puncture resistance, Ib
Elongation, in.
Specific gravity, dried
Ash (dry basis) , %
Direction
of test
-
-
-
-
-
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse
Machine
Transverse

_
-
-
-

Poly-
ethylene
21
12.5
0.6
-0.2
0.0
3090
2880
580
660
455
520
1370
• 1175
1465
1220
1685
1255
405
360

90
90
15.9
0.99
0.928
0.03
PVC +
pitch
52
83.5
5.8
4.0
6.1
1090
920
200
190
40
15
990
745
1090
930
-
-
225
175

73
67
53.6
0.51
1.290
9.65
Elasticized
polyolefin
36
23.0
0.1
0.6
0.4
2480
2180
620
590
430
385
940
895
1030
975
1195
1130
390
380

89
87
28.5
1.02
0.938
0.93
Polyester
elastomer
75
6.0
2.0
1.3
1.4
6720
7760
580
640
360
345
2455
2665
2745
2835
3010
3665
740
625

89
89
19.6
1.11
1.232
0.33
Poly-
butylene
98
8
0.1
0.4
-0.2
5420
5500
380
360
230
210
2395
2420
3015
3305
4375
4735
410
400

92
91
20.2
0.74
0.904
0.01
 Tests performed were tensile, elongation, modulus  and  set, ASTM D412;  Duro  A,  ASTM D2240;
 tear strength, ASTM D624; puncture, FM 101B, No. 2065;  specific gravity,  ASTM D297;  ash,
 ASTM D297; volatiles (loss to constant weight at room temperature,  plus loss in weight in
b2 h at 1Q5°C).
 Contractor's  liner number.
 Fabric reinforced.
                                              56

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                                    TECHNICAL REPORT DATA
                             (Please read Instructions on the reverse before completing)
 1. REPORT NO.
 EPA-600/2-79-038
                             2.
                                                           3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
 LINER MATERIALS EXPOSED TO MUNICIPAL SOLID
 WASTE LEACHATE
 Third Interim Report
                                                            5. REPORT DATE
                                                            July 1979 (Issuing Date)
                                                            6. PERFORMING ORGANIZATION CODE
 7. AUTHOR(S)
 Henry  E.  Haxo, Jr., Robert S. Haxo,  Thomas F. Kellogg.
                                                           8. PERFORMING ORGANIZATION REPORT NO.
 9. PERFORMING ORGANIZATION NAME AND ADDRESS
 Matrecon,  Inc.
 P. 0. Box  24075
 Oakland, CA  94623
                                                           10. PROGRAM ELEMENT NO.

                                                           1DC818,  SOS  1,  Task 20
                                                           11. CONTRACT/GRANT NO.

                                                           68-03-2134
 12. SPONSORING AGENCY NAME AND ADDRESS
 Municipal  Environmental Research Laboratory—Gin,  OH
 Office of  Research and Development
 U.S. Environmental Protection Agency
 Cincinnati, Ohio 45268
                                                           13. TYPE OF REPORT AND PERIOD COVERED
                                                           Interim 1/1/76  to 5/31/78	
                                                           14. SPONSORING AGENCY CODE

                                                                     EPA/600/14
 15. SUPPLEMENTARY NOTES
 See also "Evaluation of Liner Materials  Exposed to Leachate", EPA  600/2-76-255
 September 1976.   NTIS PB-259913    Project Officer:  Robert Landreth  (513)684-7871
   ABSTRACT
      This report  is  the third interim report  of a project that aims  to  assess the
 effects upon various liner materials of extended contact with leachate  from simulated
 sanitary landfills.   In this part of the  study, the primary exposure  tests of liner
 specimens at the  bottom of simulated landfills  were supplemented by  immersion of 28
 different polymeric  materials in sanitary landfill leachate.  Immersed  membranes were
 tested for changes in physical properties, permeability, and water absorption.

      The results  of  the immersion tests generally confirm the earlier results for
 membrane liner materials exposed for one  year in simulated landfills.

      Also reported are results of the water vapor permeability testing  of  28 membrane
 liners, the water absorption of a series  of membranes  at room temperature  and at 70°C,
 and the retrieval and testing of samples  of a 6-year old membrane liner from a demon-'
 stration landfill.   The monitoring of the simulated landfills during 180 months of
 operation is described and the analyses of the  leachates produced during the period
 of operation are  summarized.

      A simple bag test for assessing permeability and  physical properties  of membrane
 liners for landfills  is  described and test results  are presented.	
 7.
                                KEY WORDS AND DOCUMENT ANALYSIS
                  DESCRIPTORS
 Inings,  Leaching, Refuse Disposal,
 Pollution,  Decomposition Reactions,
 lastics
                                              b.lDENTIFIERS/OPEN ENDED TERMS
                                                Solid Waste  Management
                                                                         c.  COSATI Field/Group
  13B
  DISTRIBUTION STATEMENT
RELEASE TO PUBLIC
                                             19. SECURITY CLASS (ThisReport)
                                             UNCLASSIFIED
21. NO. OF PAGES
       67
                                              20. SECURITY CLASS (Thispage)

                                              UNCLASSIFIED
                                                                        22. PRICE
EPA Form 2220-1 (Rev. 4-77)
                                             57
                                                                     4 U.S. GOVERNMENT PRINTING OFFICE: 1979-657-060/5339

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