United States
Environmental Protection
Agency	
Hazardous Waste Engineering
Research Laboratory
Cincinnati OH 45268
Research and Development
EPA/600/S2-88/017   Mar.1988
 Project Summary
 Factors  in  Assessing  the
 Compatibility of  FMLs and
 Waste  Liquids

 Henry E. Haxo, Jr., Thomas P. Lahey, and Mark L. Rosenberg
  This experimental research project
studied various  factors in  the
compatibility  of flexible  membrane
liners (FMLs) with waste  liquids and
other hazardous  substances that
may be  encountered  in waste
storage and disposal facilities. This
work was conducted  in three basic
areas:
 1.  Swelling of FMLs  and  other
    FML-related compositions in
    organics, and  calculation  of the
    solubility parameters of  these
    compositions.
 2.  Distribution  of organics between
    aqueous solutions, such  as
    leachates, and FMLs.
 3.  Variables in EPA  Method 9090
    compatibility testing of FMLs and
    waste liquids.
  Equilibrium swelling of  28 FML-
related polymeric compositions  was
determined  in 30 organics and
deionized water. These 28 polymeric
materials  included thermoplastic
crosslinked  and  semicrystalline
compositions,  of  which  22 were
commercial FMLs  or  sheetings  and
six   were known compositions
prepared  in the laboratory for  this
study. Basic polymer and compound
variations (e.g.,  differences  in
polymer type, level of crystallinity,
crosslink density,  filler  level,  and
amount and type of plasticizer) were
assessed.
  Crystallinity of the base polymer
appears to be the dominant factor in
reducing the  swelling of an FML or
an FML-related composition in all of
the  organics and to override both the
solubility  parameters and cross-
 linking. Among compositions  based
 on amorphous  polymers, the
 proximity of the component solubility
 parameters to those of the organics
 could be used in  most cases  to
 indicate  the  swelling and the
 probability of changes in properties.
 Nevertheless,  empirically  derived
 data are still necessary for untested
 combinations of organics and FMLs.
    This  Project Summary was
 developed by EPA's Hazardous  Waste
 Engineering Research  Laboratory,
 Cincinnati, OH,  to announce key
 findings of the research project  that is
 fully documented in a separate  report
 of the same title (see Project Report
 ordering information at back).

 Introduction
   The  compatibility of a proposed
 polymeric membrane liner with the waste
 to be contained is a principal requirement
 of the  Resource  Conservation and
 Recovery  Act permitting process  for the
 construction of  a  waste storage and
 disposal facility. The other principal
 requirements are low permeability and
 durability.  Thus,  a  liner material must
 have  low permeability to  all the
 constituents of a waste liquid and must
 maintain  its physical integrity,  including
 seams,  to contain  the particular  waste
 effectively for the required  length of time.
   In assessing the suitability  of  a
 polymeric product designed to  be in
 contact with liquids and chemicals, it is
 common  practice  in the rubber and
 plastics  industries to  use solubility
 parameters to  select  the polymer
 compound and ultimately  to expose the
 composition to the liquid with which it is

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to be  in contact. The  effects of the
exposure upon the physical properties of
the compositions are measured  as a
function  of time.  The  swelling  and
dimensional changes that take place and
the changes  in  mechanical  properties,
such as  tensile  strength, elongation  at
break,  tear strength  and modulus are
normally  measured.   For  many
applications service  life is estimated as
the time of  a percentage  change  in
property  relevant to its performance  or
one  that has  been  correlated  with
performance.  In the  case  of FMLs used
in lining  waste  storage  and disposal
facilities,  specific criteria for an allowable
magnitude  of  change  in  specific
properties beyond which an FML "fails"
have not been developed.
   The technology involving  the use  of
polymeric membranes for lining  storage
and disposal facilities is relatively new. At
present, information in the open literature
regarding the  compatibility of FMLs and
waste liquids based on actual experience
continues to  be  limited.  On the  other
hand, considerable information regarding
the compatibility  of  specific polymeric
materials with  specific  organics  and
liquids  is available which the engineer
and designer can use to assess potential
compatibility  of given materials with
given  waste  liquids.  Because  waste
liquids  can be complex mixtures with the
possibility of  detrimental effects due  to
the combination  of  components, the
compatibility of a lining material with a
specific  waste  liquid  needs  to  be
determined. Reliable test protocols are
needed so that correct assessment of the
liner-waste  compatibility  can  be made
by the permit writer when  reviewing a
permit  application.
   Among properties that appear to be
related to FML performance, the swelling
or loss in weight  in service is one of the
most  useful   tools  in assessing  its
compatibility  with wastes.  Associated
with these  changes  in weight are
changes  in   most  of  the  physical
properties, such as tensile strength, tear
strength,  modulus,  hardness, permea-
bility, puncture resistance,  and  fatigue
resistance.
   Matching the  solubility  parameter
values  of an FML with those  of a specific
waste  liquid  and its  constituents has
been suggested as a means  of predicting
the swelling that might take place  in an
FML on exposure. Determination of the
applicability of the  solubility parameter
values  to estimate the compatibility  of
FMLs  and  specific  wastes and  to
estimate  the service lives of FMLs was
one  of the principal objectives of this
project.
   In  addition  to  the possible use  of
solubility parameters  for  predicting
compatibility and  service lives of  FMLs
as liners in specific  waste  storage and
disposal facilities, there are several other
factors which can affect the magnitude of
swelling and  possibly  the  ultimate
service  life.  The  compositional factors
include:
•  Degrees of  crystallinity  of the
   polymer.
•  Level of crosslinking of the polymer.
•  Amount  of  filler  in  the  compound
   formulation.
•  Amount  of  plasticizer  in  the
   compound.
•  Amount of waste soluble constituents
   in the compound.
   The environmental factors include:
•  Concentration of the organics and the
   partitioning of an organic dissolved in
   the waste liquid with a polymeric liner.
•  The effect of strain or  stress on a liner
   in service.
   This  project   was  undertaken  to
investigate and  quantify  the  various
factors that contribute to the performance
of FMLs and  their  compatibility  with
waste liquids  in   waste storage  and
disposal facilities and  to  investigate
factors involved in predicting long-term
compatibility and service life.


Objectives
   The four principal  objectives of this
project were:
•  To develop  a  methodology that can
   be used to predict the compatibility of
   FMLs with specific waste  liquids and
   to estimate their service lives for lining
   waste storage and disposal facilities.
•  To  determine   the  solubility
   parameters of polymeric FMLs and to
   explore their use for  determining the
   compatibility  of FMLs  with waste
   liquids of different types.
•  To assess the  different  factors that
   affect the magnitude of swelling of an
   FML in contact  with waste liquids.
•  To determine  the effects  of  swelling
   on mechanical and permeability
   characteristics of FMLs in service.
   In  addition to  the above,  this project
had the following secondary objectives:
•  To assess the  effects on polymeric
   FMLs of organics in  dilute solutions
   and  determine  whether  threshold
   levels for organic species  in  waste
   liquids can be set.
•  To assess the  effects on polymeric
   FMLs of exposure to waste liquids,
   such as in the testing of environment!
   stress-cracking resistance.
•  To  determine  the importance  c
   crosslink type  and crosslink densit
   upon  FML  behavior  in  wast
   impoundment environments.
•  To  determine the  applicability  c
   higher  exposure  temperatures  i
   performing compatibility tests and  i
   estimating the service  life of an FM
   as  a liner in a  waste  storage an
   disposal facility.

Summary and Conclusions
   The work conducted  on this projec
was in three major areas relating  to th
chemical compatibility  of FMLs wit
waste liquids and leachates:
•  Swelling of  FMLs in   organics an
   calculations  of the  solubilit
   parameters  of the  FMLs and relate
   compositions.
•  Distribution  of organics in  aqueou
   solutions between water and  FMLs.
•  Study of variables in FML/waste liqui
   compatibility testing.

Swelling of FMLs in Organics
and Calculations of the
Solubility Parameters of the
FMLs and Related Composition
   Equilibrium  swelling   of  28  FML
related polymeric  compositions wa
determined in 30 organics and  deionize
(Dl) water. These 28 polymeric material
included thermoplastic, crosslinked, an
semicrystalline compositions, of which 2
were commercial FMLs or sheetings an
six were  laboratory-prepared  com
positions. Within these 28 composition:
basic  polymer and compound  variation
were  included,  such as polymer  type;
level  of crystallinity, crosslink density
filler  level, and amount  and  type  c
plasticizer.
   The organics covered a wide range c
Hildebrand solubility  parameters as we
as the component solubility parameter:
i.e., the dispersive  ( d), polarity ( p),  an
hydrogen-bonding ( h) components. Th
organics were  selected  by a  compute
program from  a list of 131 organics  o
which the solubility parameter  data wer
available and which covered the range
of component solubility parameter value:
as well as the Hildebrand parameter.
   Equilibrium swelling was measured b
weighing   specimens  of  polymeri
compositions that had been immersed i
the individual  neat  organics until ther
was  essentially no  change in weigh
Each  of  the  solubility  parameter:
including the  Hildebrand and componer
parameters,  were then calculated fror

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•he swelling  data  for each  of  the
 olymeric  compositions  through  a
computer program which generated the
curve that  best fit the data  for that
parameter.
   The most  significant results  of  this
swelling study were:
•  The  crystallinity  of the  polymer
   appeared to be the dominant factor in
   reducing the swelling of the polymeric
   composition in all of the  organics and
   appeared  to override both  the
   crosslinking  and   the solubility
   parameters.
•  The crosslinking of an amorphous
   polymer reduced swelling in all of the
   organics   compared  with  the
   uncrosslinked polymer. Increasing the
   crosslinking density reduced  the
   swelling.
   Note: The crystallinity and crosslinking
        factors are not additive. The
        introduction of crosslinking in
        semicrystalline   polymeric
        compositions tends to  reduce
        the amount of crystallinity.
•  Though the magnitude of swelling of
   amorphous polymers could,  in many
   instances,  be estimated from  the
   proximity  of the   values   of  the
   component  solubility parameters of
   the polymer and  those of the organic,
   the  swelling of  the FML  in many
   combinations could  only be  roughly
   estimated  based  upon  the  type of
   organic.   The  matching   of  the
   Hildebrand solubility parameter values
   remains a necessary  but not sufficient
   condition for swelling.  The  swelling
   tests  should be performed to ensure
   that an amorphous FML  will not swell
   in  a  particular  organic.  Thus,
   empirically derived data  are  still
   needed for untested  combinations of
   organics and FMLs.
•  With  waste  liquids  that contained
   dissolved organics, the organics were
   absorbed  by the FML;  the  amounts
   absorbed  depended   on:  (1)  the
   relationship  of  the  solubility
   parameters  of the organic  and the
   FML, and  (2) the  solubility of the
   organic in  water.

Distribution of Organics in
Aqueous Solutions  Between
Water and FMLs
   A  series  of  experiments  was
performed to study the distribution of
organics from dilute aqueous solutions to
FMLs and  the  permeation  of these
organics through  the  FMLs. Three
jreliminary experiments were performed
to  explore the movement of organics with
respect to water and FMLs and to assess
gas  chromatography  as a  means of
measuring the concentrations of organics
so that their movement from one solution
into  another could be  followed.  These
experiments were as follows:
•  Measurement of the distribution of
   seven organics  in mixtures at different
   ratios with water between the organic
   phase  and  water.  The  mixtures
   included organics having a wide range
   of solubilities in water from miscibility
   to almost complete insolubility.
•  Measurement of the distribution of
   organics  between  water  and  a
   paraffinic  oil which was  selected to
   simulate polyethylene because of their
   chemical similarity.
•  Measurement of the distribution of
   organics in  a dilute aqueous solution
   of  organics and  a  high-density
   polyethylene  FML which  was
   immersed in the solution.
   A series of  six additional and  more
extensive experiments  was conducted to
assess  the distribution  of  organics
between water and FMLs:
•  To determine  the  distribution  of
   organics between  saturated aqueous
   solutions of individual organics and a
   polyethylene FML
•  To determine  the  distribution  of
   organics between organic-saturated
   FML specimens and deionized water.
•  To determine,  in a two-compartment
   test apparatus,  the  distribution  and
   transmission of nine organics in  a
   dilute aqueous solution  through  a
   linear  low-density polyethylene FML.
•  To   determine,   in   the  two-
   compartment  test  apparatus,  the
   distribution of trichloroethylene (TCE)
   in  a  dilute  aqueous  solution among
   the air-spaces, the water layer, and
   the  FML   separating   the two
   compartments.
•  To  determine,  in  a  vapor-tight
   three-compartment  test apparatus,
   the distribution of the trichloroethylene
   and toluene  from a dilute solution to
   the vapor, water, and FML layers.
•  To determine the distribution,  in the
   three-compartment  test  apparatus
   separated by polyethylene FMLs, of
   six volatile organics initially in a dilute
   aqueous  solution.  These organics
   covered  the  range  of  solubility
   parameters  from  an alkane  to  an
   organic acid.
   The  results of these  experiments
demonstrated that the  organics,  based
upon their solubility  parameters,  will
transfer from a dilute aqueous solution to
the FML with  which the solution is in
contact and, if volatile, permeate into the
airspace on the opposite side of the FML
as  a  vapor. The  ultimate  ratio,  at
equilibrium, of the concentration  of the
organics in the FML to that in the water
can vary  over  hundreds  of orders  of
magnitude, depending  on  the  solubility
parameters of the organics.
  A multi-compartment test apparatus
with FML specimens between the
compartments to simulate  the  condition
of a waste liquid in service appears to be
an appropriate means of measuring the
movement of  organics  from  dilute
solutions and transmission through FMLs.
The concentration of  the organics  in the
various zones of the  test  apparatus can
be  followed  by gas chromatographic
analysis of the  vapors and liquids and
headspace gas chromatographic analysis
of the FML.
  The  solubility  of an organic  in  water
appears to have been a significant  factor
in its movement through the apparatus.
For example, n-octane, when added  to
water  in   the three-compartment test
apparatus, tended to  volatilize and be
transported into the  airspace above the
top  FML rather than into the lower FML
and  the   airspace  below the  dilute
aqueous solution of organics. TCE,  which
is highly volatile and  yet has a  relatively
high solubility in water, was  transmitted
relatively  fast  throughout  the   three
compartments of the test apparatus, thus
showing its high mobility.
  Considerable time was required for the
organics originally in the dilute solution in
the  apparatus to reach equilibrium  in the
vapor, the water,  and the  FMLs  layers.
This indicates the need for relatively long
exposure  periods, e.g., four months, for
conducting compatibility tests of FMLs in
dilute  solutions  and  waste  liquids.
Because  of  the  long exposure period,
vapor-tight exposure tanks  should be
used.

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  Henry  E.  Haxo,  Jr.,  Thomas P. Lahey, and Mark  L.  Rosenberg are  with
        Matrecon, Inc., Alameda, CA 94501.
  Robert E. Landreth is the EPA Project Officer (see below).
  The complete report, entitled "Factors in Assessing the  Compatibility of FMLs
        and Waste Liquids,"  (Order No. PB 88-173 3721 AS;  Cost:  $19.95,
        subject to change) will be available only from:
            National Technical Information Service
            5285 Port Royal Road
            Springfield,  VA22161
            Telephone:  703-487-4650
  The EPA Project  Officer can be contacted at:
            Hazardous Waste Engineering Research Laboratory
            U.S. Environmental Protection Agency
            Cincinnati, OH 45268
United States
Environmental Protection
Agency
Center for Environmental Research
Information
Cincinnati OH 45268
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Official Business
Penalty for Private Use $300

EPA/600/S2-88/017

         0000329   PS
                                        60404
                                                                           ifrU.S. GOVERNMENT PRINTING OFFICE: 1988—548-013/8'

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