xvEPA
               United States
               Environmental Protection
               Agency
               Municipal Environmental Research  EPA-600/2-79-071
               Laboratory           Jury1979
               Cincinnati OH 45268
               Research and Development
Comparison of
Three Waste
Leaching Tests

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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-600/2-79-071
                                             July 1979
        COMPARISON  OF THREE WASTE  LEACHING TESTS
                          by

                   Robert K. Ham
                   Marc A. Anderson
                   Rainer Stegmann
                   Robert Stanforth

   Department of Civil and Environmental Engineering
           University of Wisconsin-Madison
               Madison, Wisconsin  53706
                 Grant No. R-804773-01
                   Project Officers

                   Michael Gruenfeld
       Resource Extraction and Handling Division
Industrial  Environmental  Research Laboratory-Cincinnati
               Edison,  New Jersey  08817

                    Donald Sanning
      Solid and Hazardous Waste Research Division
      Municipal Environmental  Research  Laboratory
                Cincinnati,  Ohio  45268
     INDUSTRIAL  ENVIRONMENTAL  RESEARCH  LABORATORY
          OFFICE OF RESEARCH AND DEVELOPMENT
        U.S. ENVIRONMENTAL PROTECTION  AGENCY
                CINCINNATI, OHIO  45268

     MUNICIPAL  ENVIRONMENTAL  RESEARCH  LABORATORY
          OFFICE OF RESEARCH AND DEVELOPMENT
        U.S. ENVIRONMENTAL PROTECTION  AGENCY
                CINCINNATI, OHIO  45268

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                             DISCLAIMER


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

      The selection or design of any leachate test will ultimately
be decided by a number of practical, rather than theoretical consid-
erations.  The classification of whether or not a waste is hazardous,
via a leaching test, must assume less than ideal disposal conditions,
in order that, its potential for causing environmental harm can be
minimized.   It is recognized that a single test will not be optimal for
all disposal conditions.  Nevertheless, from a regulatory point of
view, developing different tests for each different waste and disposal
option  is clearly impractical and probably unworkable.
                                    11

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                                  FOREWORD
     This research effort is a combined response to an environmental need by
two Office of Research and Development Laboratories.  The Edison, New Jersey
office of the Industrial Environmental Research Laboratory assisted the Munic-
ipal Environmental Research Laboratory in this effort.

     The Industrial Environmental Research Laboratory-Cincinnati develops
cost effective techniques to prevent, control, or abate multimedia  (air,
water, solid wastes, etc.) pollutional impacts associated with the extrac-
tion, transportation, processing, benefication, conversion, and use of min-
eral resources and with industrial processing and manufacturing.  The Munic-
ipal Environmental Research Laboratory develops new and improved technology
and systems for preventing, treating, and-managing waste water and solid and
hazardous waste pollutant discharges from municipal and community sources,
for preserving and treating public drinking water supplies, and for minimiz-
ing the adverse economic, social, health, and aesthetic effects of pollution.
The related pollutional impacts on our environment and the interplay between
its components require a concentrated and integrated attack on the problem.

     This report deals with the investigation of three leaching tests as re-
liable predictors of the potential environmental effects of the disposal of
thirteen industrial wastes.  The advantages and disadvantages of each test
based on the leaching characteristics of the thirteen wastes and the useful-
ness of each procedure as a standard test are analyzed and compared.  The
report will provide data for decision makers of both government and industry
alike contemplating residue leachate control from industrial sludge impound-
ment/municipal landfill co-disposal  operations.
David G. Stephen
Director
Industrial Environmental
Research Laboratory
Francis T. Mayo
Director
Municipal Environmental
Research Laboratory
                                     m

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                             ABSTRACT
     A comparison of three leaching tests was performed with four-
teen industrial wastes to evaluate the potential  of each test for
use as a standard leaching test.  The study was done in conjunction
with a background study on the development of a standard leaching
test.

     The advantages and disadvantages of each test, based on the
leaching characteristics of the fourteen wastes and the usefulness
of each procedure as a standard test, are analyzed and compared.
Finally, some comments on the need for careful interpretation of
test results are provided.

     This report was submitted in partial fulfillment of Grant No.
R-804773-01 by the University of Wisconsin under the sponsorship
of the U.S. Environmental Protection Agency.  This report covers
the period July 1, 1976 to February 1, 1978, and work was com-
pleted July, 1978.

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                              CONTENTS
Foreword	    iii
Abstract	     iv
Figures	    y-ji
Tables	, .	    xvl.
Abbreviations and Symbols  	  xviii
Acknowledgements	    -xtx

     1.  Introduction  	      1
     2.  Summary and Conclusions	      2
     3.  Test Procedures and Analytical Methods  	      8

              Leaching tests used	      8
              Wastes used	  . . .....      8
              Waste sample preparation .	      8
              Selection of measurement parameters  ........     18

                   — Inorganic	     18
                   —Organic	     18

              Analytical  methods .	     19
              Reproducibility  	     21
              Release calculations 	     23

     4.  Test Comparison	 .     24

              Leachate composition 	     24
              Solid-liquid ratio 	     32
              Multiple elutions  	     34
              Agitation technique and surface
                   area of contact	     35
              Elution time and temperature	     38
              Maximum concentration and
                   maximum release	     38
              Solid-liquid separation  	     38
              Organic analysis 	     39

     5.  Detailed Results  .	     41

              Adhesive waste #1  	     44
              Ink and paint waste	     52

                   —Discussion	     67

              Coal  tar sludge from steel  manufacturer	     69

                   —Discussion	     81

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                      CONTENTS (continued)
              Health and beauty care waste	      83
                   —Discussion	      96
              Food grade waste	      97
              Adhesive waste #6	     107
                   —Discussion	     114
              Petrochemical  industry water-oil  sludge  	     115
              Grain processing lipids and fats  waste	     125
              Food industry  clay waste	     134
              Marble wash	     144
              Copper oxide-sodium sulfate sludge  	     153
                   —Discussion	     163
                        SLT	     163
                        test comparison	     166
              Electroplating sludge 	     167
                   —Discussion	     176
              Wastewater treatment sludge 	     177
                   —Discussion	     189
              Papermill sludge-EPA	-	     190
References	.,	     196
Appendix ~ Mass Spectra of  Compounds Identified
            in Waste Hexane  Extracts  	     197
                                   VI

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                                 FIGURES

Number                                                            page

   1    Cu and Mg concentration and release curves for
            CuO-Na2S04 Sludge, test comparison 	     31

   2    Variation in Na and K concentration and release
            for Ink and Paint Waste with solid-liquid
            ratio (gm waste/100 ml  leachate)  using
            a distilled water leachate 	     33

   3    Napthalene and Quincline concentration and re-
            lease curves for Coal Tar Waste,  test
            comparison	     35

   4    Na concentration and release from a CiiO-Na^S'O.
            Sludge in test leachates		     37

   5    pH and specific conductance  curves  for
            Adhesive Waste #1,  SLT  .........  	     45

   6    Na and K concentration  and release  curves
            for Adhesive Waste  #1,  SLT ,  .	     47

   7    Mg and Zn concentration  and  release curves
            for Adhesive Waste  #1,  SLT	     48

   8    COD concentration and release curves for
            Adhesive Waste #1,  SLT  .  .	     49

   9    pH,  specific  conductance,  and Na  concentration
            and release  curves  for  Adhesive Waste #1,
            test comparison	     50

  10    K  and Zn concentration and release  curves  for
            Adhesive Waste #1,  test comparison 	     51

  11    pH,  specific  conductance,  and  Na concentration
            and release  curves  for  Ink and Paint
            Waste, SLT	     54

  12    K  and  Mg concentration and release  curves  for  Ink
            and Paint Waste, SLT	     55

  13    Zn  and  Pb  concentration  and  release curves  for
            Ink and  Paint  Waste, SLT	     56

  14    COD  concentration and release  curves for Ink and
            Paint Waste, SLT	     57

  15    Cyclohexanone and Napthalene concentration and
            release  curves for  Ink  and Paint Waste, SLT  ....     58

                                 vi i

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                        FIGURES (continued)
Number
  16    pH, specific conductance and Na concentration
             and release curves for Ink and Paint
             Waste, test comparison 	      59

  17    K and Mg concentration and release curves for
             Ink and Paint Waste, test comparison	      60

  18    Zn and Pb concentration and release curves for
             Ink and Paint Waste, test comparison	      61

  19    Cyclohexanone and Napthalene concentration and
             release curves for Ink and Paint Waste,
             test comparison	      62

  20    Total ion reconstructed gas chromatogram of
             Ink and Paint Waste, hexane extract  	      63

  21    Representative total ion reconstructed gas
             chromatogram of SLT H?0 leachate of Ink
             and Paint Waste   .  .	      64

  22    Representative total ion reconstructed gas
             chromatogram of IUCS test HgO leachate
             of Ink and Paint  Waste	      65

  23    Representative total ion reconstructed gas
             chromatogram of Minn, test I-^O leachate
             from  Ink and Paint Waste	      66

  24    pH and specific conductance curves for Coal Tar
             Waste, SLT	      71

  25    Na and K concentration and release curves for
             Coal  Tar Waste, SLT	      72

  26    Mg and COD concentration and release  curves  for
             Coal  Tar Waste, SLT	     73

  27    Napthalene and  Phenol  concentration and  release
             curves for Coal Tar Waste, SLT	     74

  28    Creosols and Quinoline concentration  and release
             curves for Coal Tar Waste, SLT	     75

  29    pH,  specific conductance,  and  Na  concentration
             and release  curves  for Coal  Tar  Waste,
             test  comparison	     76
                                 vm

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                        FIGURES (continued)
Number
Page
  30    K and Mg concentration and release curves
             for Coal  Tar Waste, test comparison	    77

  31    Phenol and Creosol concentration and
             release curves for Coal  Tar Waste,
             test comparison	    78

  32    Total ion reconstructed gas chromatogram
             of distillate of SLT ^0 leachate from
             Coal Tar Waste  .  . .  .  .	    79

  33    Total ion reconstructed gas chromatogram of
             distillate of IUCS test  H20 leachate
             from Coal  Tar Waste	    80

  34    pH and specific conductance curves for Health
             and Beauty Care Waste, SLT	    85

  35    Na and K concentration and  release curves for
             Health and Beauty Care Waste, SLT	    86

  36    Mg and Zn concentration and release curves
             for Health and Beauty  Care Waste, SLT	    87

  37    Cu and Cd concentration and release curves
             for Health and Beauty  Care Waste, SLT  .......    88

  38    Fe and Pb concentration and release curves
             for Health and Beauty  Care Waste, SLT	    89

  39    COD concentration and release curves for
             Health and Beauty Care Waste, SLT	    90

  40    pH, specific conductance, and Na concentration
             and release curves for Health and Beauty
             Care Waste, test comparison	    91

  41    K and Mg concentration  and  release curves for
             Health and Beauty Care Waste, test com-
             parison 	    92

  42    Zn and Fe concentration and release curves  for
             Health and Beauty  Care Waste, test comparison  ...    93

  43    Cu and Pb concentration and release curves  for
             Health and Beauty  Care Waste, test comparison  ...    94
                                  IX

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                        FIGURES (continued)
Number
Page
  44    Total ion reconstructed gas chromatogram
             of Health and Beauty Care Waste,
             hexane extract 	     95

  45    pH and specific conductance curves for
             Food Grade Waste, SLT	     99

  46    Na and K concentration and release curves
             for Food Grade Waste, SLT	    100

  47    Mg and Zn concentration and release curves
             for Food Grade Waste, SLT  . . . .	    101

  48    COD concentration and release curves for
             Food Grade Waste, SLT  . . .	    102

  49    pH, specific conductance, and Na concentration
             and release curves for Food Grade Waste,
             test comparison	•	    1°3

  50    K and Mg concentration and release curves for
             Food Grade Waste, test comparison   	    104

  51    Zn concentration and  release curves for  Food
             Grade Waste, test comparison	    105

  52    Total ion reconstructed gas chromatogram of
             Food Grade Waste, hexane extract  	    106

  53    pH and specific conductance curves for Adhesive
             Waste #6, SLT	   1Q9

  54    Na and K concentration and release curves for
             Adhesive  Waste  #6, SLT	   11°

  55    COD  concentration  and release curves  for
             Adhesive  Waste  #6, SLT  .  .  .	    'I1

  56    pH,  specific  conductance,  and Na  concentration
             and release  curves for  Adhesive  Waste  #6,
             test  comparison	    H2

  57    K and  Zn concentration and release curves for
             Adhesive Waste  #6, test comparison	    1'3

  58    pH and specific  conductance  curves for Petro-
             chemical  Sludge, SLT .  .  .  .  '	    117

   59    Na and K concentration and release curves for
              Petrochemical  Sludge, SLT   	    118

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                        FIGURES (continued)

Number                                                           Page

  60    Mg and Zn concentration and release curves for
             Petrochemical  Sludge, SLT	    119

  61    Pb and COD concentration and release curves for
             Petrochemical  Sludge, SLT	. .	    120

  62    pH, specific conductance, and Na concentration
             and release curves for Petrochemical  Sludge,
             test comparison	    121

  63    K and Mg concentration and release curves  for
             Petrochemical  Sludge, test comparison	    122

  64    Zn and Pb concentration and release curves for
             Petrochemical  Sludge, test comparison .  . .  .  .  .    123

  65    Total ion reconstructed gas chromatogram of
             Petrochemical  Sludge, hexane extract   ,	    124

  66    pH and specific conductance curves for Grain
             Processing Lipids and Fats, SLT	    127

  67    Na and K concentration and release curves  for
             Grain Processing Lipids and Fats, SLT	    128

  68    Mg and Zn concentration and release curves for
             Grain Processing Lipids and Fats,'SLT .  . .  .  .  .    129

  69    COD concentration and release curves for Grain
             Processing Lipids and Fats, SLT	    130

  70    pH, specific conductance, and Na concentration and
             release curves for Grain Processing Lipids
             and Fats,  test comparison	    131

  71    K and Mg concentration and release curves  for
             Grain Processing Lipids and Fats, test
             comparison  ..... 	 .........    132

  72    Zn and Pb concentration and release curves for
             Grain Processing Lipids and Fats, test
             comparison	    133

  73    pH and specific conductance curves for Food Wastes,
             Clay, SLT  .........:...........    136

  74    Na, K, and Mg concentration and release curves for
             Food Wastes, Clay, SLT . .  .  .... . ...  ......    137


                                  xi

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FIGURES (continued)
Number
75

76

77


78

79

80

81

82

83

84


85

86

87

88
89
90
91



Zn and Pb concentration and release curves for
Food Wastes, Clay, SLT 	
COD concentration and release curves for Food
Wastes, Clay, SLT 	
pH, specific conductance, and Na concentration
release curves for Food Wastes, Clay, test
comparison 	 	
K and Mg concentration and release curves for
Food Wastes, Clay, SLT 	
Zn, Pb and COD concentration and release curves
for Food Wastes, Clay, test comparison 	
Total ion reconstructed gas chromatogram for
Food Wastes, Clay, hexane extract 	
pH, specific conductance, and Na concentration
and release curves for Marble Wash, SLT ....
K, Mg, and Pb concentration and release curves
for Marble Wash, SLT 	
COD and concentration and release curves for
Marble Wash, SLT 	
pH, specific conductance, and Na concentration
and release curves for Marble Wash, test
comparison 	
K and Mg concentration and release curves for
Marble Wash, test comparison 	
Pb and COD concentration and release curves for
Marble Wash, test comparison 	
Total ion reconstructed gas chromatogram for
Marble Wash, hexane extract 	
pH and redox curves for CuO-Na2S04 Sludge, SLT ...
Na concentration curves for CuO-Na2S04 Sludge, SLT .
Na release curves for CuO-Na2S04 Sludge, SLT ....
K concentration and release curves for
CuO-Na2S04 Sludge, SLT 	
xii
Page

138

139


140

141

142

143

146

147

148


149

150

151

152
155
156
157

158


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                        FIGURES (continued)

Number                                                           paqe

  92    Mg concentration and release curves  for
             CuO-Na2S04 Sludge, SLT 	   159

  93    Cu concentration and release curves  for
             CuO-Na2S04 Sludge, SLT	160

  94    pH curves  for CuO-Na?S(h  Sludge,  test
             comparison .  .  7	161

  95    Zn and  K concentration  and  release curves  for
             CuO-Na2S04 Sludge, test comparison 	   162

  96    pH vs Cu concentration  solubility diagram
             for Cu  and CuO  system	164

  97    pH and  specific conductance curves for
             Electroplating  Sludge, SLT  	   169

  98    Na and  K concentration  and  release curves
             for Electroplating Sludge, SLT  	   170

  99    Mg and  Zn  concentration and release  curves
             for Electroplating Sludge, SLT	171

 100    Pb and  Cd  concentration and release  curves
             for Electroplating Sludge, SLT  	   172

 101     pH and  Na  concentration and release  curves
             for Electroplating Sludge, test comparison  . .. , .   173

 102    K  and Mg concentration  and  release curves
             for Electroplating Sludge, test  comparison  ....   174

 103    Zn  and  Cd  concentration and  release curves
             for Electroplating Sludge, test  comparison  ....   175

 104    pH  curve for Wastewater Treatment Sludge, SLT 	  179

 105     Na  concentration and release curves for
            Wastewater Treatment Sludge, SLT 	  180

 106     K concentration and release curves for
            Wastewater Treatment Sludge, SLT 	 ...  181

 107     Zn  concentration and release curves for
            Wastewater Treatment Sludge, SLT 	   182

 108     Mg  concentration and release curves for
            Wastewater Treatment Sludge, SLT 	   183

                               xi i i

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                         FIGURES (continued)
Number
                                                                  Page
 109     Cu concentration and release curves for
              Wastewater Treatment Sludge, SLT 	   184

 110     COD concentration and release curves for
              Wastewater Treatment Sludge, SLT 	   185

 111     pH and Na concentration and release curves
              for Wastewater Treatment Sludge,
              test comparison	186

 112     K and Mg concentration and release curves
              for Wastewater Treatment Sludge,
              test comparison	187

 113     Cu and Zn concentration and release curves
              for Wastewater Treatment Sludge,
              test comparison	188

 114     pH curve for Papermill Sludge, EPA, SLT	192

 115     K and  Mg concentration and release curves
              for Papermill Sludge, EPA,  SLT	193

 116     Zn and Fe concentration and release curves
              for Paper-mill Sludge, EPA,  SLT	194

 117     Cu concentration  and  release curves for
              Papermill  Sludge, EPA, SLT  .  .  .	195

 A-l     Mass spectrum  of  xylene identified  in  Ink
              and Paint Waste"hexane extract   	    Iy/

 A-2     Mass spectrum  of  cumene identified  in  Ink
              and Paint Waste  hexane extract   	    l98

 A-3     Mass spectrum  of  m-ethyltoluene  identified
              in  Ink and Paint Waste  hexane  extract	199

 A-4     Mass spectrum  of  cyclohexanone  identified
              in  Ink and Paint Waste  hexane  extract	200

 A-5     Mass spectrum  of 2-nor-butoxyethanol  identified
               in  Ink &  Paint Waste hexane extract   	201

  A-6      Mass  spectrum  of 3,3,6-trimethyl bicyclo (3.1.0)
               Hexan-2-one or.3,5,5-trimethyl-2-
               cyclohexanone identified  in Ink and Paint
               Waste hexane extract	   202
                                   xiv

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Number

  A-7   Mass


  A-8   Mass


  A-9   Mass


  A-10  Mass


  A-ll   Mass


  A-12  Mass


  A-13  Mass


  A-14  Mass


  A-15  Mass


  A-16  Mass


  A-17  Mass
            FIGURES (continued)

                                                    Page

spectrum of dimethyl glutarate identified
in Ink and Paint Waste hexane extract ......    203

spectrum of napthalene identified in Ink
and Paint Waste hexane extract  .........    204

spectrum of methyl napthalene identified
in Ink and Paint Waste hexane extract	    205

spectrum of octadecane identified in Food
Grade Waste hexane extract  ............   , 206

spectrum of hexadecane identified in Food
Grade Waste hexane extract  ......;....    207

spectrum of tetradecane identified in Food
Grade Waste hexane extract	    208

spectrum of napthalene identified in Petro-
chemical  Waste hexane extract .....  	    209

spectrum of hexadecane identified in Petro-
chemical  Waste.hexane extract	    210

spectrum of dodecane identified in Food
Industry Clay Waste hexane extract  . .  	    211

spectrum of tridecane identified in Food
Industry Clay Waste hexane extract  	    212
spectrum of tetradecane indentified in
Food Industry Clay Waste hexane extract .  .  .  .  .
                                                                 213
                                 xv

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                              TABLES
Some Features of an Ideal Standard Leaching Test
Number

   1

   2    Abilities and Limitations of Each Test in
             Comparison to an Ideal Test ..............    4

   3    SLT Test Procedure ....................    9

   4    Description of the IUCS Modified 48-Hour
             Shake Test  .....................   13

   5    Description of the Minnesota Test  ............   14

   6    A Summary of the Leaching Tests Used in
             the Test Comparison .................   '5

   7    Description of the Real Leachate Test  ..........   16

   8    Wastes Used in the Test Comparison ............   17

   9    Analytical Methods for Routine or Inorganic
             Analyses  .......  •  ..............   20

   10    Standard Deviation Calculations for Multiple
             Replicates of Paint Waste Leached with
             Synthetic Leachate Using SLT Procedures  .......   22

   11    A Summary of Test Comparison  Results for
             Selected Parameters from Selected Wastes   ......   25

   12    The  Number of Times  Each Test Leaching
             Solution Gave the  Highest Concentra-
             tion of an  Inorganic  Parameter from  a
             Waste for the Different  Test Leachates   .......  27

   13    The  Number of Times  Each Test Leaching Solution
             Gave the Highest Release of an Inorganic
             Parameter from  a Waste for the Different
             Test Leachates   ...................  28

   14    The  Number of Times  Acid or H20 Leaching  Solutions
             Gave Highest Concentrations or Release  of an
              Inorganic Parameter from a Waste   ..........  29

   15    Test Factors Affecting Parameter Concentrations
              in  Leachates  ....................  30

   16     Format for  the  Description of Wastes  and Summary
              of Leaching Test Results  ..............  42
                                   xvi

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                          TABLES (continued)

Number                                                              Page

  17    Summary of Symbols Used in Presenting SLT and
             Test Comparison Data	   43

  18   Adhesive Haste #1:   Description and Summary of
            Results	     44

  19   Ink and Paint Waste (IPW):   Description and Sum-
            mary of  Results	     52

  20   Coal  Tar Sludge:   Description  and  Summary  of
            Results	     69

  21   Health  and Beauty Care  Waste  (HBC):
            Description  and Summary of Results   	     83

  22   Food  Grade Waste:   Description and Summary of
            Results	     97

  23   Adhesive Waste #6:   Description and  Summary
            of Results	    107

  24   Petrochemical  Industry  Water-Oil Sludge:
            Description  and Summary of Results   	    115

  25   Grain Processing  Lipids  and Fats Waste:
            Description  and Summary of Results   	    125

  26   Food  Industry  Clay  Waste:  Description
            and Summary  of Results	    134

  27   Marble  Wash:   Description and  Summary of
            Results	    144

  28   Copper  Oxide-Sodium Sulfate Sludge
            (CuO-Na2S04  Waste):  Description
            and Summary  of Results	    153

  29   Electroplating  Sludge (EPS):   Description
            and Summary  of Results	    167

  30   Wastewater  Treatment Sludge (WTS):   Description
            and Summary  of Results	    177

  31    Papermill  Sludge  (PMS-EPA):  Description
            and Summary of Results	    190
                                 xvn

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                    ABBREVIATIONS AND SYMBOLS
TESTS

SLT—Leaching test developed by Ham et al. (1)
IUCS Test—I.U.  Conversion Systems, Inc.  Modified 48-hour shake  leaching
                                                         .  .
Minn. Test—Leaching test developed  by  the Minnesota Pollution Control
     Agency
Proc C-Procedure Cl t   procedures  in  the SLT
Proc R—Procedure RJ     ^
RLT—Leaching test using municipal landfill leachate
S/L—Solid/Liquid ratio or separation

LEACHATES

SL—synthetic municipal landfill  leachate used in SLT
Acet—Acetate buffer used in Minn. Test
HO—distilled, deionized water leachate

WASTE SUPPLIERS

ECHO—Environmental Clearinghouse Organization, Inc.
Chem-Trol— Chem-Trol Pollution Services,  Inc.

CHEMICAL ABBREVIATIONS

Na—Sodium
K—Potassium
Mg—Magnesium
Zn—Zinc
Cu—Copper
Cd—Cadmium
Pb—Lead
Cr—Chromium
 Fe—Iron
COD—Chemical  Oxygen  Demand
Q—Quinoline
 6S-MS—Gas  Chromatography  - Mass Spectrometry
TIR6C—Total  Ion Reconstructed Gas Chromatogram

 LIST OF WASTES—SEE TABLE  8
                                  xvm

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                          ACKNOWLEDGEMENTS
      Lawrence Burkhard and Jean Behrens-Tepper of the University of
Wisconsin Water Chemistry Laboratories performed the gas chromatog-
raphy-mass spectrometry analysis and compound identification.

      This work was supported by the U.S. Environmental Protection
Agency, Solid and Hazardous Waste Research Division, under Grant
Number R-804773-01.  Mr. Michael Gruenfeld of the EPA Edison, New
Jersey, laboratories was the Project Officer.  The authors wish to
acknowledge the help of Messrs.  A.  Corson and D. Viviani of the EPA,
and especially, the help and support of Messrs.  Gruenfeld and D.
Sanning of EPA who worked closely with project personnel throughout
the project.
                                xix

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                             SECTION  1

                           INTRODUCTION
     Developing awareness of the potential of landfilled industrial
wastes to pollute groundwater has led to an interest in a standard-
ized test to discern the relative leaching potential of a waste.  A
background study on such a test done by the authors for the U.S.
Environmental Protection Agency'(EPA) is detailed in Ham, et a1_ (1).
During this background study a leaching test was developed, called
the SLT.  In order to evaluate the SLT, and other leaching tests
which might be used as the standard test, a comparison of three
leaching tests were made by running the tests on a wide variety of
industrial wastes and comparing the relative ease, practicality and
amount of information obtained in each of the tests.  The tests used
were the SLT, a 48-hour shake test developed by IU Conversion Systems,
and a 24-hour acid leach test developed by the Minnesota Pollution
Control Agency.  The results of the test comparison are given in this
report.  Note that this test comparison serves as a practical evalua-
tion of the workability of the SLT on a variety of wastes.

     The development of the SLT and the SLT evaluation and test com-
parison are presented in separate reports in order to keep the length
of each report reasonable.

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                             SECTION 2

                      SUMMARY AND CONCLUSIONS
      Three leaching tests, as specified by EPA, were used on 14 dif-
ferent industrial wastes, supplied by EPA, which were specifically
chosen to be of widely differing characteristics.  Some wastes were
predominantly liquid, others were solid; some wastes were primarily
inorganic, others organic; some wastes were complex with several dis-
tinct solids and/or liquid layers; and some were sticky or like glue
and so were extremely difficult to handle.  The SLT was the only test
able to handle all wastes using only procedures specified by the test
protocol.  Note that no obviously dangerous (explosive, carcinogenic,
etc.) wastes were tested, because such wastes would have provided lit-
tle or no information beyond that provided using the 14 wastes..

      The SLT test was the most aggressive of the three tests yielding
the highest concentrations of inorganic parameters (mg/A) 79% of the
time, and the highest release of inorganic parameters (mg/kg waste)
55% of the time  (Tables 12 and 13).  It is the only test able to give
information about both potential concentration and release of param-
eters leached from an industrial waste.  Because the SLT is an aggres-
sive test, providing information about what could happen in a worst
case (but realistic) situation, its results need to be interpreted with
care.  For example, the concentration of leachate arising from large
amounts of waste through which small amounts of water (leaching medium)
are moving will  probably approach the maximum concentration indicated
by the SLT, but  this may never happen with a particular landfill.

      The importance of using different leaching media was indicated
by the results.  Acidic leaching media  (pH 4.5)  gave the highest con-
centrations of inorganic parameters 89% of the  time, and the highest
release 96% of the time  (Table 14).  Without the use of several leach-
ates, test results could be very misleading and  have no relation to
the actual landfill for a  particular waste.

      Certain features of  an  ideal  standard leaching test following the
concepts  discussed  in  section 4  are given in Table  1.   An
ideal leaching test  is defined herein as  a standardized procedure which
works on  all wastes and  is able  to  predict quickly and with accuracy the
potential water  quality  degradation within a landfill represented by the
landfill  disposal of a particular waste.   It does not evaluate  any
changes  in  leachate quality arising  from  passage through soils  or dilu-
tion.  The major abilities and limitations of  each test used  in this
study with  regard to these features  are given  in Table  2.  Column tests
are  not  included in  the  concept  of  an  ideal  leaching test because of
the  difficulty of using  a  column test  on  a wide variety of wastes.

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     A number of different tests could be designed which meet the cri-
teria of Table 1 and, yet, have considerable differences between them.
Thus, once a standard leaching test has been designed, interpretation
of the test results becomes a crucial  factor in determining the
applicability of the test.  A standard leaching test provides a
reproducible set of numbers that are a function of the interaction
of a waste with a specific leaching solution,under a specific set
of conditions.  It is up to the decision maker to evaluate those num-
bers and make a prediction regarding the behavior of the waste


      TABLE 1.  SOME FEATURES OF AN IDEAL STANDARD LEACHING TEST*
1.    Use of leaching media corresponding to liquids  likely to be in con-
     tact with the waste in the landfill (such as use of both an acid
     synthetic municipal landfill  leachate and distilled water leaching
     solutions for modeling, leaching in actively decomposing and stabi-
     lized municipal landfills, respectively).

2.    Incorporates procedures to indicate both concentration and release
     of parameters likely to be leached from a waste.

3.    Use of multiple elutions so secondary effects can be observed.

4.    Use of an effective agitation procedure which does not unnat-
     urally or unnecessarily abrade waste particles.

5.    Use of a solid/liquid ratio high enough to minimize analytical
     and sampling errors, yet low enough to allow rapid determination
     of critical  concentration and release information for most param-
     eters.

6.    Use of convenient, yet justifiable, elution times and numbers  of
     elutions.
      It is assumed that any useable test would incorporate sampling pro-
cedures and sufficient replicates to gain statistical  reliability.

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         TABLE 2.   ABILITIES AND LIMITATIONS OF EACH TEST IN

                    COMPARISON TO AN IDEAL TEST*


SIT.

  Positive aspects:

     1.  Use of two separate procedures to allow prediction of both con-
         centration and release of parameters from waste.

     2   Flexibility of leaching media selection such as the use of both
         acid synthetic municipal landfill leachate and distilled water
         as leaching solutions to model co-disposal with municipal solid
         waste.

     3.  Use of an effective, yet gentle, agitation technique.

     4.  Use of multiple elutions.

     5   Use of an intermediate solid/liquid ratio which lessens the
         change of analytical errors of the Minn, test while generally
         allowing more rapid evaluation of release characteristics
         than does the IUCS test.

     6.  Incorporates procedures which allowed  its direct  use on all the
         wastes tested in  this  study.

   Limitations:

     1   Use  of an oxygen  sensitive leachate,  required  for proper  model-
          ing  of leachate generated  in  actively decomposing municipal
          solid waste landfills.

     2   The  laboratory  procedures  and the  amount of information  obtained,
          especially  if both concentration and  release results are  desired,
          require  more laboratory effort  and interpretive care.

 IUCS TEST

   Positive aspects:

      1.  Use of a generally effective agitation technique.

      2.  Use of multiple elutions.

      3.  Use of a high solid/liquid ratio gives relatively high concen-
          trations of many parameters.

      4.  Use of a relatively straightforward laboratory procedure.


                                                         (continued)
i.e., Table 1.

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                          TABLE 2.  (continued)

  Limitations:

     1.  Use of only a distilled water leachate.

     2.  Lack of a procedure to evaluate the maximum concentration of a
         parameter in leachate.

     3.  Use of an elution time and number such that work needs to be
         continued over weekends.

     4.  Required adaptations on a waste by waste basis to allow some
         wastes to be tested.

     5.  The fewer numerical results require more careful interpreta-
         tion and extrapolation of data than the SLT to apply the re-
         sults to actual landfill  situations.

MINNESOTA TEST

  Positive aspects:                                  .

     1.  Use of both acid and distilled water leachates.

     2.  Simple and rapid to perform.

  Limitations:

     1.  Acetate buffer models only one aspect of municipal  solid waste
         leachate affecting its leaching aggressiveness.

     2.  Low solid/liquid ratio emphasizes subsampling,  weighing, and
         analytical errors.

     3.  Use of only one elution gives much less information than either
         of the other two tests.  No information is provided regarding
         the approach testable results, the rate at which such stability
         is reached, or possible secondary effects.

     4.  Agitation technique allows significant concentration gradients
         in the bulk solution, raising the time needed to approach equi-
         librium and reducing the  reproducibility of the  results.

     5.  Required adaptations on a waste by waste basis to allow some
         wastes to be tested.

     6.  Neither concentration nor release information can be obtained
         with confidence because it is not known how close the results
         are after one elution to  maximum values attainable  or to prac-
         tical values reached in actual landfills.   Application of test
         results to actual  landfills is difficult to justify.

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in a landfill.  Unfortunately, the multiplicity of factors affecting
the leaching characteristics of a waste, both in the test and in the
landfill, and the variability of landfill  conditions, dictate that
interpretation be done with care and with consideration of the waste
and landfill characteristics.  Test results should not be interpreted
rigidly, e.g., developing criteria stating that a certain concentra-
tion of a given parameter in the test leachate automatically and
without further consideration indicates that the waste is hazardous
in the landfill.  Rather, consideration should be given to such fac-
tors as the amount of waste to be disposed, the annual net infiltra-
tion of water in the area of the landfill, the factors affecting the
leaching of the waste (as far as can be determined from the test
results), possible waste—leachate interactions, and the fate of the
landfill leachate after it leaves the waste and passes through addi-
tional wastes or soil.

     As an example of the need for careful interpretation, consider the
distilled water leachates from the CuO - Na2SC>4 sludge.  These leachates
contained low concentrations of copper (<1 mg/1), yet very high concentra-
tions of Na (-10,000 mg/1 in the SLT Elution 1 leachates).  With regard to
Na, the leachate is probably not very hazardous, at least no more hazardous
than sea water which has approximately the same Na concentration.  Yet, in
a landfill or in the soil underneath, the high ionic strength could solu-
bilize potentially hazardous trace metals through ion exchange mechanisms.
Thus, the leachate itself may not be hazardous, but it may solubilize;
hazardous materials in landfill environments.  Likewise, several wastes
(ink and paint waste, health and beauty care waste, food grade waste,
and adhesive waste #6) released large amounts of unidentified organic
compounds, as evidenced by the very high COD values in the distilled
water leachates.  The potential hazard of these wastes may not come
from the organic compounds released by the waste, if these are not
hazardous, but from the ability of the released organics to solubilize
otherwise insoluble hazardous compounds, such as chlorinated organic
pesticides or heavy metals.  On the other hand, a waste may release  small
amounts of hazardous materials which will most likely be removed from the
leachate by passage through  the soil under the landfill.  The waste might
appear to be  hazardous due to the release of this material, yet in the
landfill it would actually be relatively innocuous.  Several wastes  which
released trace metals in low concentrations might fall into this category.
It should be  noted that leaching modeled by the test in one or two days
may simulate years of leaching in the field.  During this time, bacteria
may convert hazardous compounds into innocuous ones, or vice versa,  or
they may completely alter the leaching characteristics of a waste through
their action  on the waste matrix.

     When interpreting test  results, it is important to consider the
physical condition of the landfilled waste.  For example, a waste which
is landfilled in large stable chunks or with a stable  impervious coating
could behave  far differently in a landfill than in a test in which it
were ground.  The test results need to be  interpreted  in light of the
conditions  around the waste  and the condition of the waste itself in
the landfill.

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     An evaluation of the hazardous nature of a waste must include an
evaluation of the landfill environment.  A waste's hazardous nature
is a situation specific characteristic.  A waste may be hazardous to
an organism under one set of environmental conditions yet completely
innocuous under a different set of conditions.  Furthermore, its
hazard may be organism specific; i.e., it may be hazardous to one
organism and not to another under the same set of conditions.  Thus,
a determination of the hazardous nature of a waste must include an
evaluation of its hazardousness to specific organisms under specific
conditions.

     The limitations of a standard leaching test and the care needed
in interpreting the results do not mean that a standard test is not
worth developing and using.  A standard test should provide a rapid
evaluation of the parameters that are likely to be leached from a
waste, and an indication of their maximum concentrations in the leach-
ate and the total amount to be released per unit weight of waste.  That
the test is not perfect in predicting the long term leaching pattern of
a waste or the precise concentration of a particular parameter in a par-
ticular landfill means that the test results need to be interpreted with
care to avoid unnecessary expanditures for control of waste that are
not actually hazardous in a particular landfill, or to avoid unexpected
environmental degradation from improper land disposal of a waste.

     In summary., of the three tests compared in this study, the SLT
gave the most information in the shortest amount of time.  The IUCS
test could be improved if several modifications were incorporated,
such as use of an acidic synthetic municipal landfill leachate when
co-disposal of the waste being tested with municipal solid waste is
possible, and if a procedure for measuring maximum concentration were
added.  The Minn, test would require several modifications in order to
be a widely applicable standard test.

     Whatever standard test is used, interpretation of test results is
the crucial factor in determining the test's ultimate value in predict-
ing whether a waste is hazardous when placed in a landfill.  Virtually
any leaching test which is properly interpreted would be more useful
in making such a prediction than would be a well designed leaching test
which is poorly interpreted.

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                            SECTION 3

              TEST PROCEDURES AND ANALYTICAL METHODS
LEACHING TESTS USED

    The two tests used in addition to the SLT were selected by EPA as
being among the best tests currently available and as having some vari-
ety in the test conditions.  A survey of existing leaching tests by the
Miter Corp. (2) gives a good overview of existing leaching tests.

    The tests used in the test comparison were the SLT, an IU Conversion
Systems modified 48-hour shake test (the IUCS test) and a test developed
by the Minnesota Pollution Control Agency (the Minn. test).  These tests
are described in Tables 3, 4, and 5, respectively.  There are several
IUCS shake tests available, so particular care should be taken to specify
the test conditions when discussing the test.  A summary and comparison
of the test conditions is given in Table 6.

    In addition to the tests mentioned above, a municipal leachate was
used as a leaching medium, using a modified SLT procedure R.  The dif-
ficulty in working with highly air sensitive real leachate necessitated
the modifications.  The purpose of the real leachate test (RLT) (Table 7)
was not to verify the accuracy of the synthetic leachate used in the SLT,
as might be supposed, but rather to obtain an idea of the leaching ability
of a real leachate sample.  The leachate was not used as aggressively as
the leachate upon which the synthetic leachate was modelled, and so cannot
be used as a verification of the synthetic leachate.

WASTES USED

    Ten of the wastes used in the test comparison were supplied by
Environmental Clearinghouse Organization, Inc., Hazel Crest, Illinois,
at EPA's request.  Two wastes were supplied by Chem-Trol Pollution
Services,  Inc., Model City, New York, for the use in the background study
and were reused in the test comparison.  One of these, the wastewater
treatment  sludge, was used in only the SLT and the Minn. test.  One
locally obtained waste was also used.  In addition, one waste termed
papermill  sludge  (EPA), was used only in the SLT.  The wastes, their
sources, and the tests in which they were used are given in Table 8.
Descriptions of the wastes and available chemical and physical analyses
for the wastes are presented  in tables at the start of the  test results
section for each waste.

WASTE  SAMPLE PREPARATION

    Since  the  intent  of the comparison was to evaluate the  tests  them-
selves, the  sample preparation procedure was  kept the  same  for all tests.
This  preparation  included  a solid/liquid separation  procedure that is
recommended  for  sample preparation  in the  SLT background  study  (_!).   This
technique  is not  included  "in  either  the  IUCS  or  Minn tests.  Both of

                                     8

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                    TABLE 3.   SLT TEST PROCEDURE
 Preparation of Sample

 1.   Representative samples  of waste are taken  using  standard  techniques
     appropriate for waste (e.g.,  ASTM standard techniques  for sampling
     wastes) when available.

 2.   Wastes  that are not  obviously solid are  separated  into solid  and
     liquid  components, using  the  suggested solid/liquid  separation
     scheme.   Percentage  solid (net weight) in  waste  is measured or
     estimated.

 3.   The  liquid  portion of the waste is  analyzed  directly.   If the liquid
     is hazardous,  an assessment is made of the total waste's  hazardousness
     due  to  the  liquid component.   If the waste is assessed as  hazardous,
     the  test  is  terminated.

 4.   The  moisture content  of the solid component  of the waste  is determined
     by drying at 105°C for 24 hours,  or other  procedure  as  appropriate.
     The  waste sample used for moisture  content determination  is discarded.

 Selection of Leaching Solution

     Leaching solutions are selected  for use  in the test  based on the type
 of landfill into which the waste might  be disposed, as follows:

             Landfill                      Leaching Solution

     stabilized municipal   landfill        distilled deionized water*
     or mono!andfill

     actively decomposing                synthetic municipal  landfill
    municipal landfill                  leachate"1"

     co-landfilled with other           distilled, deionized water*,  plus
    wastes in industrial  landfill       other leaching solutions deemed
                                       useful for modeling industrial
                                       landfills.

SLT Procedures

    The solid portion of  the waste sample is  leached  with the  selected
leaching  solutions using  two elution procedures—C and R—described
    —
     Meeting ASTM Specifications D-1193 for distilled, deionized water,
or equivalent.

    ^A synthetic municipal  landfill  leachate, of pH 4.5, and composed of:
0.15M acetic acid, 0.15 M sodium acetate, 0.050 M glycine, 0.008  M pyrogallol,
and 0.024 M ferrous sulfate.
                                                   (continued)
                                     9

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                     TABLE 3 (continued)

below.  Elution time, temperature, agitation technique, and filtration
procedure are the same for both elution procedures.   Sufficient replicates
are run for statistical reliability.

  Elution time-an elution time of 24 hours is used for all elutions.

   Temperature-the test is conducted at ambient temperatures (~20°C)
                unless major changes occur in waste characteristics at
                temperatures close to 20°C.  In sijch cases the test is
                run at 20°C constant temperature.

      Agitation-a circular shaker tilted such that the_shaking circle
                radius is vertical or nearly vertical  is used.  Square
                or rectangular flasks are used so that the waste
                gently tumbles through  the leaching solution as the
                flasks turn.  The rotation speed is 2-3 rpm.
                •square  or rectangular  flasks  are needed.  Glass or plastic
                may be  used,  depending on  parameters  to  be analyzed.
Sample bottles


Procedure C (for estimation of maximum concentration)

1    In the first elution, leachate is added to the waste solid to_
     give a solid/liquid ratio of one part waste by weight (dry weight)
     to ten parts leaching solution by volume (e.g., 1  gm (dry weight;
     waste to 10 ml leaching solution).  The sample used in the test
     should not be dried prior to use.  The total leachate volume used
     should be more than three times the leachate volume needed for
     analysis.
2    The sample is agitated for 24 hours, then filtered through a 0.4b micron
     pore size filter, using the filter aids described in the solid-
     liquid separation scheme as necessary (1).  The filtered waste is  ens
     carded.
 3    A sample of the filtered leachate, not more than one-third of the
     total volume, is removed for analysis.  The volume of the remain-
     ing leachate  is measured and the  leachate returned to the test flask.
     Fresh waste is added  to give a  solid-liquid ratio of l:7.b.

 4.   Step 2  is  repeated.
 5.   A sample of the filtered leachate, not more than one-half of the
     filtered volume, is taken for analysis.  The volume of the remain-
     ing leachate  is measured and the  leachate returned to the test flask.
     Fresh waste is added  to give a  solid-liquid ratio of 1:5.

 6.   Step 2  is  repeated, and the filtered leachate  is used for analysis.
 	                                   (continued)
     *
       If other  temperatures are more  suitable for modeling a particular
 landfill, appropriate temperatures can be used but  should be noted.
                                       10

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                     TABLE 3 (continued)
Procedure R (for estimation of maximum release)
 4.

 5.

 6.

 7.
     JinnfS  «t?t eiut1on' leachate is added to the waste  to  give a solid
     liquid  ratio of one part waste by weight (dry weight)  to ten
    The sample is agitated for 24 hours,  then  filtered through a 0 45um
    pore size fUter, using the filter aids  described in the so'ld-llSuld
    separation as necessary.   The filtered leachate is used for analyses
       p         WSSt? 1sureturned t°  the  test flask and fresh leachate
    added   The same leachate volume used  in the first elution is usS
    maintaining the 1:10 solid-liquid  ratio.           eiution is used

    Step 2 is repeated.

    Step 3 is repeated.

    Step 2 is repeated.

    The test  is  terminated and the waste discarded  unless  an  indicator

    ^ec^Vt^ea'c^^
    continued until  the  Indicator parameter returns  to  baseline vl?ue.
      Procedure C
                          Elution  1
120 gm wet weight (60  gm  dry
weight) is added  to  540 ml
leaching solution.   (1:10
solid/liquid ratio).
         Agitate  24  hours at room temperature, filter
                                                Procedure R
                                      40 gm weight (20 gm dry weight)
                                      of waste is added to 180 ml
                                      leaching solution.   (1:10
                                      solid/liquid ratio).
                                               (continued)
                                 11

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                      TABLE 3 (concluded)
        Procedure C
                                                   Procedure R
                            Elution 2
Discard filtered waste.  Remove
150 ml leachate for analysis.
Measure remaining leachate and
return to flask.  If remaining
volume is 450 ml, add 120 gm* wet
weight waste.   (1:7.5 solid/
liquid ratio.)
                              Remove filtered leachate for analy-
                              sis.  Return filtered waste to
                              flask and  add 200 ml fresh leach-
                              ate.  (1:10 solid/liquid ratio.)
           Agitate 24 hours at room temperature, filter
 Discard filtered  waste.   Remove
 150 ml  filtered leachate for
 analysis.   Measure remaining
 leachate and return to flask.
 If remaining volume is 300 ml,
 add 120 gmf wet weight waste.
 (1:5 solid/liquid ratio.)T
                               Remove filtered leachate for analy-
                               sis.  Return filtered waste to
                               flask and add 200 ml fresh leach-
                               ate.  (1:10 solid/liquid ratio.)
            Agitate 24 hours at room temperature, filter
 Discard filtered waste.  Use
 filtered leachate for analysis.
                                Remove  filtered  leachate for analy-
                                sis.   If  indicator  parameter indi-
                                cates more  elutions are needed,
                                return  waste  to  flask  and  add  200 ml
                                fresh  leaching  solution and continue
                                elutions  until  indicator parameter
                                returns to  base line value.  Other-
                                wise discard  waste.
        450 ml  x
                	 x 2 am waste (wet) = 120 gm waste
                leaching solution   1 gm waste (dry)   jwet wel-ght)
   1  gm waste (dry)
7.5 ml
.
300 ml
                    1  am waste (dry)       x 2 gm waste (wet)  = 120  gm waste
                 5>0 ml  leaching solution   1 gm waste (dry)    jwet weight)


       %lote that leaching media lost by removal of used waste will approx-
  imately equal the liquid added with the new wet waste.
                                      12

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    TABLE 4.   DESCRIPTION OF THE IUCS MODIFIED 48 HOUR SHAKE  TEST
  SCOPE
  mnt^niinH  i  »  u +	  the determination of the long-term diffusion-
  controlled  leachate properties of a soil or waste material.  The pro-

  Sm+^iJV?  es*a°1lsn representative values of the long-term diffusion-
  controlled  leachate properties of a soil or waste material ai niIr*H ?«
  embankments   landfills,  and other disposa? or use Sites   These proper
  ties result from prolonged water contact both on the surface of the soil
  or waste materials and on a portion of the interior of a mass of soil  or
  waste material as limited by the permeability coefficient of the material.


  PROCEDURE


  1.   Measure an aliquot of water specific for the  field site  or standard
      water as defined  by ASTM Committee  D-19 such  that the ratio of ml
      of water to g, dry weight,  of test  specimen  is  4  to 1.   IUCS tvoical
      practice is to use 500 g.,  dry weight,  of specimen to 200  ml ofwater
      Record  measured water volume in liters.                         water.

 2.



 3.





 4.


 5.




 6.
7.
 and we?ahTwMeh Water1to *he sPecimen of Predetermined  surface  area
 and weight which was placed in a non-leaching  container.


 Seal container and place in the box  carrier  of a  reciprocating shaker

 c^in'th^i10" ^ °I SP t0 7° °ne-inch  strokes  P^r minute.  Be
 movement!    placement of the container allows for maximum water


 Shake container for  48 hours.


 Immediately after the  shake  period,  sample a 100 ml aliquot for total
 suspended solids  analysis.   Vacuum filter at least 500 ml of the
 remaining leachate using  .45 micron membrane or glass fiber filters.


 Decant off any  leachate left  in the non-leaching container, allowing
 the  test  specimen to remain  in the container.  Note and record the

 nhwc-  ?Vr  ^e  te^  sPe^men, be1n9 sure to include comments on
 SnSSl  StSn9.r?*1Jn-  These comments shall  be as quantitative as
 possible  to facilitate any necessary modification  in  apparent sur-
 face area for subsequent 48-hour shake periods.


 Repeat steps 1 through 6 four times,  thus obtaining five  sets  of
 faS%ea[:  set,C0nsist1ng of one  100 ml aliquot of unfiltered
 leachate to be analyzed for total  suspended solids and one  500 ml
aliquot of filtered leachate.
                                  13

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           TABLE 5.  DESCRIPTION OF THE MINNESOTA TEST
     12 5  gm dry weight  of  solid  is  placed  in  a  1000 nl separately









carded and the remainder is kept for analysis.
filtering technique for all tests.
                                   14

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       TABLE 6.  A SUMMARY OF THE LEACHING TESTS USED IN

                      THE TEST COMPARISON
Leaching
 Solution
Solid/Liquid
 Ratio
                       SLT
Synthetic Leachate

        H20*
               1:10   (Process R)
               Varied (Process C)
                      IUCS Test
H20
                         '•
              Minnesota Test
                                                      Acetate Buffer,
                   '-40
Shaking Slow Tumbling
Technique
Time per 24 hrs
Elution
Number of 3 or more
Elutions
Temperature Room
Back and 1 min. shake,
Forth
Shaking 24 hr. rest
48 hrs 24 hrs
5 1
Room Room
      Distilled,  deionized water.
                                 15

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         TABLE 7.  DESCRIPTION OF THE REAL LEACHATE TEST

     (Leachate Collected August 13 from a Madison Landfill)
     Leachate was collected in fifteen 250 ml acid-washed glass pre-
scription bottles.  Four bottles (3 wastes + 1 duplicate) had the
wastes to be leached already inside.  A solid/liquid ratio of 1:10
was used.  Eight bottles were used to anaerobically store the leach-
ate until use in the experiment, and three bottles were collected to
store leachate for a daily background analysis during the duration of
the test.  The test bottles were stored at room temperature and shaken
intermittently throughout the day.  After a 24-hour elution time, the
leachate was decanted from the prescription bottles into screw top
polycarbonate centrifuge tubes.  The tubes were closed then centrifuged
for 20-30 minutes at 10,000 RPM on a Son/all Centrifuge, then filtered
through a 0.45 micron membrane filter.  Sufficient leachate was filtered
for analysis.  (Even after centrifugation, the filtering process was
slow.)  pH readings were taken as rapidly as possible, however, even in
a few minutes a  brown flocculant precipitate formed.  After the readings
were taken, the  leachate was acidified to approximately pH 1 and stored
at 4°C until analysis.  The four waste sample bottles plus one background
bottle were sampled daily.  The background sample was split into two
aliquots, and each aliquot sampled and analyzed separately.  New leachate
was used for each of the three elutions.

                   Leachate Background Values
      COD
      Cond

      PH
      Na

      K
      Mg
      Fe

      Zn
      Cu
27,200 mg/1
1 x 10  umhos/cm
5.5 (varied from 5.15-5.81)

465 rag/1 ±15 (range)

720 + 40 mg/1
250 +_ 10 mg/1
very unstable (variable)

31 + 1 mg/1
1 mg/1, unstable
                                    16

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TABLE 8.  WASTES USED IN THE TEST COMPARISON
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.

12.
13.
14.
Waste
Adhesive Waste #1
Ink & Paint Waste
Coal Tar Waste
Health & Beauty
Care Waste
Food Grade Waste
Adhesive Waste #6
Petrochemical Industry
Water/Oil Sludge
Grain Processing
Lipids & Fats
Food Wastes,
Clay
Marble Wash
Copper Oxide-
Sodium
Sulfate
Sludge
Electroplating
Sludge
Wastewater Treat-
ment Sludge
Papermill Sludge,
EPA
Waste Abbreviation Source
ECHO
I.P.W. ECHO
ECHO
H.B.C ECHO
ECHO
ECHO
Petrochemical Sludge ECHO
Grain Fats ECHO
ECHO
ECHO
CuO-Na2S04 Sludge Chem-trol

EPS Local
WTS Chem-trol
PMS-EPA Chem-trol
Test
SLT,
SLT,
SLT,
SLT,
SLT,
SLT,
SLT,,
SLT,
SLT,
SLT,
SLT,

SLT,
SLT,
SLT
Used
Minn,
Minn,
Minn,
Minn,
Mi nn ,
Mi nn ,
Minn,
Minn,
Minn,
Mi nn ,
Minn,

Minn,
Minn,

in
IUCS
IUCS
IUCS
IUCS
IUCS
IUCS
IUCS
IUCS
IUCS
IUCS
IUCS
-RLT

IUCS
-RLT
-RLT

                           17

-------
these tests, however, were designed for solid or semi-solid wastes rather
than for predominantly liquid wastes.  As many of the wastes used in the
test comparison were predominantly liquid, the designers of both the IUCS
and Minn tests were asked how to prepare predominantly liquid wastes for
their tests.*  Both agreed that a solid/liquid separation might be one
approach to sample preparation, although both emphasized that their tests
were not designed for such wastes, and that a solid/liquid separation
might not be the approach they would use to prepare predominantly liquid
wastes for their tests.

     Different wastes required different sample preparation procedures.
The preparation used for each waste is given in the tables at the start
of the test results section for each waste.
SELECTION OF MEASUREMENT PARAMETERS
Inorganic

     Several trace metals were selected for analysis in leachates from
tests on the wastes supplied by ECHO, Inc.  Selection, made by EPA in
consultation with the authors, was based on their prevalence in the
waste as determined by ECHO, Inc. and on their general toxic nature.
These metals are listed as "metals of interest" in the table at the
start of each waste's data section.

     Other parameters were measured to obtain an overview of the leaching
process (conductivity, pH) or in order to have additional parameters with
which to compare the leaching tests (Na, K, Mg, various trace metals).


Organic

     COD was measured as a general indicator of organic materials in
leachate.  With the exception of coal tar waste, identity of Teachable
organic compounds which might be present in a waste was not known.
Therefore, a first step in analysis of leached organic compounds was
identification of organic compounds present in the waste.  Once these
were identified, compounds were chosen for analysis in leachates, in
order to evaluate the ability of different leaching solutions to solu-
bilize organic compounds of differing polarity.  Compounds were classi-
fied as polar, slightly polar or nonpolar.
     *B.  Roberts  and C.  Perket,  respectively.
                                    18

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ANALYTICAL METHODS

     Analytical methods for determination of inorganic parameters and
COD are given in Table 9.  These procedures are all from Standard
Methods (3).

     For organic parameters, except COD, identification arid 'analysis of
a parameter was much more complicated, as discussed previously.  The
first step in analysis was a determination of major organic constituents
of a waste.  A standard method for determination of an unknown organic
compound in a waste of unknown composition and consistency was not avail-
able, so a-method, described below, was devised for preparing a hexane
extract of a waste for analysis oh gas chromatography-mass spectrometry.
1.
2.
3.
4.
Ten grams of the solid portion of a waste (i.e., after the liquid/
separation step) were placed in an extraction thimble.

The waste was extracted with 100 ml hexane for six to eight hours
in a soxhlet extraction apparatus.
The hexane extract, brought to 100 ml volume if necessary.
analyzed using gas chromatography—mass spectrometry.
                                                               was
Major peaks in the reconstructed ion chromatogram were analyzed
to see if the mass spectra could be identified.
A Finnigan model 1015 gas chromatograph—mass spectrometer was used in
conjunction with a Finnigan 6110 MS data analysis system.  This procedure
allowed the identification of several compounds in the extracts from
several wastes.  The adhesive wastes could not be analyzed by this method,
since both wastes solidified during analysis and clogged the apparatus
they were in at the time of solidification.  (One glued the GC injection
syringe shut.)  Hexane extracts from several wastes contained precipitates.
The analytical procedure for evaluating waste organic composition was
sufficient for this study, but obviously it is not a complete analysis
of all wastes.

     Mass spectra of major peaks were identified either using a computer
comparison with spectra of known compounds, or by major peak comparison
with published spectra.  If the identified compound was available, iden-
tification, was confirmed by running a standard and comparing retention
times and mass spectra.

     The ink and paint waste was chosen for organic analysis  because
of the variety of the identified compounds, and because the high  COD
levels in the ink and paint waste leachates indicated that high concen-
trations of organic compounds were being leached.
                                    19

-------
             en
                                                LO
                                                O
                                  LO    o
                                  o    r—
                                                            LO

                                                            O
                                                            LO

                                                            CM
             CU
             O
CO
LU
to



«=c


                                    
 a. o  o r—
   •r-  Q. CO
   «(-     O
   •r-  X •!-
    O  O E
    CUT3 CU
    a. cu j=
    coo; cj
                              (13
                                                        CU
                                                        Lu
                                                                     •a
                                                                     o
                                                   20

-------
      Ink  and  paint  waste  leachates  were  extracted  with  methylene  chloride
 using a procedure based on  the  ASTM procedure  for  the extraction  of  oil
 and  grease  from water  (4).   Three 3 ml extractions from a measured amount
 of leachate (approximately  75 mis)  were  made.   The extractions were  dried
 with anhydrous sodium  sulfate,  brought to  10 ml  total volume, then analyzed
 using GC  -  MS.  Quantification  was  done  by comparing peak areas in the
 TIRGC with  peak areas  of  standards  run under the same conditions.  The
 pH of the leachates were  not altered prior to  extraction.  Methylene
 chloride  was  used rather  than hexane primarily because  the higher density
 of methylene  chloride  simplified the solvent - leachate separation.

      For  the  coal tar  waste, a  good estimation of  the compounds of interest
 was  available without  having to use GC - MS identification.   Coal tar
 wastes are  known to frequently  contain phenols and cresols.   The  leach-
 ates  from the coal  tar wastes were  distilled according  to the procedures
 given in  Standard Methods (3) for the analysis of  phenols.  The dis-
 tillates  were analyzed using GC - MS.  In  addition to phenol  and  cresol,
 naphthalene and quinoline were  also identified in  the distillates.  Stand-
 ards  for  all  four compounds  were run and the amounts in  the distillates
 determined.   Since  the distillation procedure  is not a  standard method
 for  analyzing napthalene or quinoline, the  recovery of these compounds
 from  the  original leachate is unknown.  The same procedure was used for
 all  leachate  samples;  their  relative concentrations can  be compared.
 The measured  concentrations  and releases for napthalene  and quinoline
 may  be underestimates  of the actual  concentrations.
REPRODUCIBILITY

     Replicates were run throughout the test series on most wastes.
Generally the replication was good.  Replicates are plotted separately
on the data figures for each waste, allowing a visual estimation of
the reproducibility.  Generally the replication for the acid and dis-
tilled water leachates in all tests were comparable.

     In addition to the above use of replicates, 18 replicates were
run on a single waste (a paint waste from an auto assembly plant) with
synthetic leachate:  nine replicates using SLT procedure R and nine using
SLT procedure C.  Six parameters were determined.  (pH was also measured,
but as the pH of the synthetic leachate was not affected by the paint
waste, the pH value in the leachates did not vary.)  The mean values and
standard deviations for each parameter on each of the three elutions are
presented in Table 10.   The deviations  are for the  complete test,  and
include errors due to waste subsample differences,  test procedures,
leachate instability, and analytical procedures.  Fe data also include
errors in weighing the FeS04 used in the synthetic  leachate.  The stand-
ard deviations are generally under 15% unless near  the detection limit.
The consistent exceptions are Zn and Fe in procedure C,  which  have quite
high deviations.  Why the Zn data should show a high variation in pro-
cedure C^and not in procedure R, particularly on the first day when they
are replicates,  is unknown.   The Fe data in procedure C show that over
a three-day period, a significant amount of Fe is precipitating out of
solution.   This precipitation illustrates a compromise made in the SLT.

                                    21

-------
  TABLE 10.  STANDARD DEVIATION CALCULATIONS FOR MULTIPLE

      REPLICATES OF PAINT WASTE LEACHED WITH SYNTHETIC

              LEACHATE USING SLT PROCEDURES
                Procedure R
                   (N = 9)
Procedure C
  (N = 9)
Both Procedures
     Day 1*
3aram-
eter
K


Mg
3

Zn


Pb


Cu


Fe



Day
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Mean
Value
3.86
2.10
1.58
9.9
1.4
0.51
16.92
-. 3.40,
1.44
0.52
0.27
0.22
b.d.1"
bid.'
b.d.
1180.
1166.
1094.

a
0.16
0.22
0.18
0.87
0.07
0.03
1.31
0,23
0.08
0.02
0.02
0.04



87.
80.
58.

%
4.1
10.7
11.6
8.8
4.9
6.1
7.74
6.8
5.4
4.4
8.2
17.2



7.4
7.0
5.6
Mean
Value
4.00
6.49
10.50
8.6
16.3
33.
22.68
70.5
123.
0.50
0.93
1.32
b.d.
b.d.
0.32
1123.
904.
585.

a
0.17
1.84
0.49
0.69
2.3
7.5
10.33
22.5
51.
0.03
0.14
0.18


0.09
71.
146.
204.

01
h
'.
4.3
28.3
4.7
8.1
14.0
22.7
45.6
31.9
41.3
6.0
15.4
13.8


28.3
6.4
16.3
35.
Mean
Value a %
3.93. 0.17 4.7


9.3 1.1 11.9


19.4 7.8 40.


0.51 0.025 5.0





1152. . 80. 7.0


On Day 1, procedures C and R are the same.
 .d. = below detection.
                                  22

-------
      In order to  model  the  anaerobic  nature  of municipal  landfill  leachate,
 an  anaerobic  synthetic  leachate  is  used.   However,  working  with  the
 synthetic  leachate  under  completely anaerobic conditions  (filtering  in
 a glove bag,  etc.)  is too complicated for  a  routine test.   Therefore,
 an  anaerobic  leachate which has  some  redox buffering capacity was
 designed and  the  lack of  perfect redox control accepted as  a necessary
 compromise.   The  loss of  iron  in procedure C over the three-day  period
 is  a  result of this compromise.   A  non-anaerobic synthetic  leachate,
 described  by  Ham, et al_ (1) avoids  the problem by not modeling the
 anaerobic  nature  of municipal  landfill leachate. " Note that the  Fe
 concentrations in the procedure  R leachates  are relatively  stable,
 indicating minimal loss of Fe  due to  oxidation-precipitation.

      Standard  addition was used  to  determine the detection  limits for
 different metals  and to determine if  any matrix effects could be seen
 in  the  synthetic  leachate.  Various amounts  of K, Mg, Cu, Zn, Pb, and
 Cr  were  added  to  fresh synthetic  leachate  and analyzed using atomic
 absorption or  emission.   The results  indicated no major matrix effects
 in  the  analysis of any of the metals.  The detection limits estimated
 for each metal are given  in Table 9.


 RELEASE  CALCULATIONS

      The release  of a parameter  per unit mass waste 'for each of the tests
 was calculated using the  equation given below:
Release
       !elution(i)
  N
(J  Conc(i),  mg/1)(leachate volume,  ml)(l  L/1000 ml)

      (dry weight of solid  in test, g)(l  kg/1000  g)
where i is the elution number and n the total number of elutions.  Leach-
ate volume and dry weight of solid is constant for each test, except for
SLT procedure C.  Calculation of release in SLT procedure C is more com-
plicated and is described in Ham, et^ a]_ (1).  Since the purpose of pro-
cedure C is to evaluate maximum concentration, release using this procedure
was not calculated.   Except for unusual  release patterns, release in pro-
cedure R will be greater than or equal  to that in procedure C.
                                    23

-------
                                SECTION 4

                              TEST COMPARISON
     There are a number of ways to compare the different leaching tests.
A comparison can be made of the concentrations in the different test
leachates of a single parameter leached from a waste.  This has been
done in Table 11 for the more important or interesting parameters from
selected wastes.  The table indicates the aggressiveness of each test
and the wide range in results from three tests designed to indicate the
same thing—the leaching characterises of a waste.  This single parameter
comparison does little good in understanding the relative aggressiveness
of the tests, however, unless the factors affecting the parameter concen-
trations in the leachates are known.

     The relative aggressiveness of the tests can also be analyzed by
comparing the number of times each test gave the highest concentration
(or release) of a parameter for all the parameters analyzed throughout
the test comparison.  This is done in Tables 12  (concentration) and
13 (release).  As can be seen, the SLT gave the highest concentration
or release much more frequently than the other tests.  Table 14 shows
a similar comparison for acid and water leachates, comparing only param-
eters that are measured in both.  Obviously, the acid leachates are much
more aggressive than distilled water leachates.  Such a comparison is
good for analyzing the general aggressiveness of a test.

     A more complete comparison of the tests entails an analysis of the
effects of the  differences between the tests on  the  test results, and
the importance  of these differences for interpreting the test results.
A list of the major test variables or factors which  must be set in devel-
oping a standardized leaching test is provided in Table 15.  As the
effects of the  different components or factors of the tests were not
analyzed separately, but rather the tests were compared as whole units
with several factors differing between them,  it  is not possible to isolate
the effect of any one factor and explain  differences between the tests
as being due due to that specific  factor.   Rather, it  is only possible
to say that  a given factor varied  between tests  and  in some cases  it
seems reasonable to ascribe a  given difference in the  test results to
this factor.  The major factors will be discussed individually  in  the
following sections.


LEACHATE  COMPOSITION

     The  profound  effect  of leaching solution composition  on  the materials
and  concentrations  leached  from  a  waste  is  shown with  several wastes  used
 in  the  test comparison, most  notably CuO  -  Na2S04  sludge.  Acidic  leach-
 ates—the synthetic leachate  and the acetate buffer—leached  potentially
 hazardous trace metals  in  significant  concentrations that  were  either
 below detection or leached  in  very low concentrations  in  the  water leachates
 (Figure 1).   This  is  not  surprising, since  many  metals are more soluble  in
                                      24

-------
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                                                                        in en ro r^ in
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                                                 26

-------
TABLE 12.  THE NUMBER OF TIMES  EACH  TEST  LEACHING  SOLUTION GAVE THE
 HIGHEST CONCENTRATION OF AN INORGANIC PARAMETER  FROM A WASTE. FOR
                  THE DIFFERENT TEST LEACHATES

Na
K
Mg
Fe
Zn
Pb
Cu
Cd
COD
Total
Number
Total, %
Total
for Each
Test, %
i
SLT
Proc C Proc R Minn. IUCS
H20 SL H20 SL Acet UQ H 0
*
8 - - - 4
1 10 i
17 11
1 -- 1 - 1
6 5 2
1 1 : 4
1 2 !
2
4 — — —
16 24 111 8 06
60.6 18.2 12.0 0 9
SLT Minn. IUCS
79% 12% 9%
   *Not measured.
                                27

-------
  TABLE 13.  THE NUMBER OF TIMES EACH TEST LEACHING SOLUTION

       GAVE THE HIGHEST RELEASE OF AN INORGANIC PARAMETER

         FROM A WASTE FOR THE DIFFERENT TEST LEACHATES
Total %
                      SLT
Procedure R

HO      SL
                                           Mi nn.
                                    Acetate
13
          42
30
                                                      4.5
                                        IUCS
                                 H2°     H2°
Na
K
Mg
Fe
Zn
Pb
Cu
Cd
COD
Total Number
5
8
1 8
1
8
1
1
2
2
9 28

4
2
2
4
5
2
1

20
2 5





1

1 1
3 7
                                           0.5
Total for
each test,
    SLT

    55%
                            MINN.
                            34.5%
                      IUCS
                     10.5%
                                  28

-------
            TABLE 14.  THE NUMBER OF TIMES ACID OR H20 LEACHING

             SOLUTIONS GAVE HIGHEST CONCENTRATIONS OR RELEASE

                   OF AN INORGANIC PARAMETER FROM A WASTE

       (Only for Parameters Measured in Both Acid and H^O Leachates)



K
Mg
Zn
Pb
Cu
Cd



K
Mg
Zn
Pb
CU
Cd


SLT
Acid(SL) H20
Number of
10 1
8 1
11
2
2 1
1


Number
8
8 1
8
1
1
2


Minn.
Acid H£0
Times Giving

1
2
4




of Times Givi
4
2
4
5
2
1


IUCS Total
H20 Acid

H2U

TOTAL TESTS
Maximum Concentration
1 10
9
13
6
1 2
J_
41
Total, % 89
ng Maximum Release
12
10
12
6
1 3
_3
46
Total , % 96
2
1
0
0
2
0_
5
n

0
i
0
0
i
0.
2
4
12
10
13
6
4
1
46*


12
11
12
6
4
3
48*

     K
      Totals are not equal because  two  tests  may  both  give the maximum
concentration but have different maximum  releases.  In cases where the
maximum concentration or release were the  same,  the results were not  tabu
lated.
                                   29

-------
           TABLE 15.   TEST FACTORS AFFECTING PARAMETER
                  CONCENTRATIONS IN LEACHATES
1.   Sampling Technique and Sample Pretreatment
     A.  Sampling technique in waste stream
     B.  Sample storage and shipment
              age, temperature, air contact, mixing, etc.

2.   Subsampling in Laboratory

3.   Solid Sampling and Preparation
     A.  Particle size reduction
     B.  Particle size selection
     C.  Solid/liquid separation
     D.  Other preparatory procedures

4.   Test Conditions
     A.  Leachate composition
              pH, complexing,  etc.
     B.  Solid/liquid  ratio
     C.  Number  of  elutions
     D.  Agitation  technique  and  surface  area  contact
     E.  Time per elution
      F.  Temperature
      6.  Waste  or leachate replacement in each elution.
5.    Separation Procedure after Leaching-
6.    Leachate Handling after Separation
7.    Analysis

                                   30

-------
    CuQ-Na2S04
         Cu
        A SLT- SL
            SLUDGE' TEST COMPARISON

         RELEASE 8 CONCENTRATION
        O SLT - H20

        D IUCS - H20

 Cu CONCENTRATION,ppm
4000-r
3000--
2000--
 I 000- -
    Mg CONCENTRATIONS, ppm

       150 -r H20 LEACHATES
            2345
            ELUTIONS
                    V MINN - ACETATE BUFFER
                    W MINN - H20

                    A REAL LEACHATE

                     Cu RELEASE,  Eg/kg
                    160-r
                    120-•
                    80--
                    40--
                                    ^^r- "f "t- - 1
                     Mg RELEASE, 2g/kg

                    60-r
                             45--
                             30--
                              15--
                          I   234
                             ELUTIONS
Figure 1.
Cu  and Mg concentration  and release curves for CuO-Na?SCL
sludge, test comparison.
(Cu concentrations in all distilled water leachates were
less than 0.6 ppm.)
                           31

-------
acidic than in neutral or slightly basic solutions.   The copper concen-
trations in the acidic leachates fromthe CuO - Na2S04 sludge were four
orders of magnitude (10,000 times) higher than the copper concentrations
in the water leachates.  The copper concentrations in the acidic leach-
ates could not be predicted with water leachates alone.   Since municipal
landfills generally have acidic leachates for much of their lifespan and
would leach Cu from the CuO - NaeS04 sludge, the need for an acidic leach-
ate in the leaching test is apparent.  This is supported by the results of
a leaching test using municipal landfill leachate (RLT).  Although not as
acidic as either of the acid leachates, the municipal landfill leachate
still leached high concentrations of copper, concentrations that could
not be obtained using distilled water as the leachate.

     The synthetic leachate gives a more accurate view of the leaching
that would occur in a young municipal landfill, since it models other
aspects of municipal  leachate in addition to pH when compared to the acetate
buffer which models only pH.  The disadvantage of the synthetic leachate
comes from the attempt to fully model municipal leachate.  Since municipal
leachate is anaerobic, the synthetic leachate is also anaerobic.  Being
anaerobic, it is air  sensitive and requires more careful handling than
aerobic leachates.  Furthermore, a precipitate forms on oxidation, intro-
ducing the possibility of a loss from solution of materials, either
occluded in or adsorbed on the precipitate.  Thus, improper handling of
the  synthetic leachate may cause  inaccurate results.  An alternative
aerobic synthetic  leachate has been  developed as described  in Ham, £t
al  (1).  This leachate avoids  the oxidation-precipitation problem, but
Hoes  so at the cost of not modeling  real leachate as completely as does
the  anaerobic synthetic leachate.
      The  synthetic leachate  is designed to  model  the leaching  environment
 found in  actively  decomposing  municipal  landfills.   Since many wastes will
 not be subjected to  such  leaching conditions,  because the  landfill  is
 stabilizing  or because of the  placement of the  waste, distilled water is
 used to model  a  less  aggressive leaching situation.   This  also happens
 to model  landfilling  the  waste in question  by itself, or with  stabilized
 industrial  wastes.  All  three  leach  tests  use distilled water for this
 purpose.

 SOLID-LIQUID RATIO

      The importance  of the solid to  liquid ratio could  frequently be  seen
 in the test results.   There are several  possible effects of the  solid/
 liquid ratio on  a  parameter's  concentration in  leachate.   For every soluble
 component, the concentration will  be directly dependent on  the solid/liquid
 ratio, simply because the more solid present, the more  parameter there is
 to be dissolved and the higher the concentration.   This situation was seen
 with very soluble  parameters,  such as Na and K, quite frequently.   Good
 examples of this are the Na and K from ink and paint waste.  A graph  of  the
 Na or K concentrations in the  first HeO leachate from ink and paint waste
 versus the amount of solid present per 100 ml leachate  (Figure 2) shows
 that the Na or K concentrations fall nearly on a straight line.   This  indi-
 cates that the concentration in solution is directly dependent on the
 amount of solid present.
                                      32

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                   INK B PAINT  WASTE
                                    GRAMS  WASTE
     CONCENTRATION  a RELEASE vs.
                                    100 ml LEACHATE

          OSLT, DIUCS, V MINNESOTA,  H90  LEACHATE
         No CONCENTRATION, ppm,
        450-r
        300--
        150- •
  Na RELEASE, 2mg/kg
2250T
I500--
 750-1
                                                        D
         K CONCENTRATION, ppm
         30-r
         20--
         IO--
  K RELEASE, Smg/kg
  I2O-T
  80--
  40--
                                          H
                  10  15 20  25            5  10  15  20  25
                       gm WASTE / 100 ml LEACHATE
Figure 2.  Variation in Na and K concentration and release for ink
         and paint waste with solid/liquid ratio (gm waste/100 ml
         leachate) using a distilled water leachate.
                             33

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     At the other extreme is a parameter whose concentration is controlled
strictly by a solubility equilibrium.  In this case, the concentration in
solution would be independent of the amount of solid present and would be
the same in all tests.  Such a situation has not been encountered with the
wastes studied.  For most parameters, concentration will probably be con-
trolled by a number of competing factors—amount present, solubility,
sorption or desorption, etc.—and the effect of solid/liquid ratio on the
concentration will be complex.

     Several practical considerations enter into the choice of a solid/
liquid ratio for a good standard test.  A very low ratio, such as that
used in the Minnesota test, leads to very small amounts of waste being
used in the test, and to generally low concentrations.  Both results
emphasize analytical or subsampling errors, particularly when calculating
release.  Also, a very low solid/liquid ratio models a much longer leach-
ing time in a landfill than does a higher ratio.  While this might at
first appear to be an advantage, the accuracy with which a short test
models long-term leaching in a landfill probably decreases as the time
span modeled gets longer.  Thus, a test with a very low solid/liquid
ratio is less accurate for modeling reasons as well as analytical ones.
On the other hand, a test with a very high solid/liquid ratio requires
more elutions to leach a partially soluble parameter and so to determine
maximum release than does a test with a lower ratio.  A solid/liquid
ratio intermediate between the very  low and very high ratios should be
used in a good standard test.  The 1:40 ratio used  in the Minnesota test
appears to be rather low for a good  test.  Both the 1:10 and T;4 ratios
used in the SLT and IUCS tests, respectively,
and either could be used.

     It is important to note how the weight of waste material  is measured
when calculating the solid/liquid  ratio.  Dry weight, which is commonly
used, can present analytical difficulties for wastes containing volatile
or semi volatile components other than water.

     The choice of  a  solid/liquid  ratio  generally  is not directly based
on landfill  conditions  (unless calculated from waste and rainfall con-
ditions), -and, within  a  range of intermediate  values,  is therefore  arbi-
trary.


MULTIPLE ELUTIONS

      Both  the  SLT and IUCS  tests use multiple  elutions.  Far more infor-
mation  can  be  obtained from these  multiple  elutions than from  a  single
 elution as  used  in  the Minnesota test.   The  IUCS  test  uses  five  elutions,
while  the  SLT  uses  three (unless the pH  in  the SL  samples  has  not returned
 to below 5.0).   The extra  elutions in the IUCS;test provide more  informa-
 tion than  the  three elutions in  the SLT, however,  they also require more
 work.   A compromise needs  to be  made between  the  added information  ob-
 tained from the  extra elutions,  and the  added work involved in obtaining
                                     34

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 it.  One factor in the selection of the number of elutions for a standard
 leaching test is simply convenience.  As long as there is no technical
 reason for selecting one number of elutions over another, the number of
 elutions chosen should be convenient for lab personnel.  The IUCS test
 was more inconvenient than the other tests in that it required working
 on weekends.   One of the reasons for selecting three elutions in the SLT
 was simply convenience.  The test can be started on Monday, samples taken
 on Tuesday, Wednesday, and Thursday, with Friday left for analysis of the
 samples.   Four elutions could also be taken without inconvenience.

      Note that no matter how many elutions are chosen, an argument can
 always be made for using one more elution.  For some wastes, one elution
 will  give all  the information obtainable from the waste;  some wastes will
 require three  elutions, some five, some fifty.   There is  no way of know-
 ing the optimum number of elutions for a given waste without running
 extensive tests to determine when some acceptable degree  of equilibration
 is reached.  This, obviously, is contrary to the concept  of a standard
 test.   Selection of the optimum number of elutions  should be based on the
 optimum number of elutions for a variety of extensively tested wastes,
 and on convenience.   Experience with the SLT suggests that three elutions
 is generally adequate (1).
 AGITATION  TECHNIQUE  AND SURFACE AREA OF CONTACT

     The  SLT and the  IUCS  tests had  generally effective agitation  tech-
 niques  in  that  little particle  abrasion was  observed  and  particle  and
 leaching media movement was  sufficient  to  avoid  visually  obvious concen-
 tration profiles  in the media.   The  Minn,  test developed  pronounced  con-
 centration differences  which  were  observable between  the  liquid  located
 near the waste particles and  that  located  away from the particles when
 colored components were being leached.   These concentration  differences
 are not surprising, since  the waste  is  not agitated for 24 hours follow-
 ing the initial  shaking.

     For two wastes,  namely,  the coal tar waste  and the CuO-Na2S04 waste,
 the SLT agitation method in  itself appeared  to be one  reason for the higher
 release with the SLT  test than  with  the  IUCS test.  In the SLT agitation
 procedure, the waste  is always  gently tumbling through the leachate.  This
 exposes more surface  area of  the waste  to  leachate contact.  The IUCS test
 agitation procedure did not provide  such particle agitation of the waste,
 resulting in approximately the  same waste surface being in contact with the
 leachate.  With coal  tar waste, the concentration of napthalene was higher
 in the SLT H20 leachates than in the IUCS H20 leachates (Figure 3).  Given
 the physical nature of  coal tar, it is  reasonable to ascribe the higher
 concentrations to the greater surface area in contact with the leachate.
 Coal tar is impervious  to water and viscous enough to inhibit internal dif-
 fusion.  Thus,  for unsaturated parameters, the concentration in leachate
 will depend on the surface area of contact with the waste.
     Another probable example of the effects of agitation  on release can
 be seen in the Na release from the CuO-Na2S04 sludge (Figure 4)   A com-
 parison of the Na release in the H20 leach SLT and IUCS tests shows a
more rapid drop off in release in the IUCS test such that  the fifth elu-
 tion, for example, provided little additional release beyond that of the
                                     35

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        COAL TAR  WASTE  TEST  COMPARISON
   NAPTHALENE a QUINOLINE'  CONCENTRATION a RELEASE
           A SLT -S.L.
           O SLT - HpO          V MINN - ACETATE BUFFER
           D1UCS-H0          V MINN - HO
                     NAPTHALENE
   CONCENTRATION, ppm
  SOT-
   10-
       RELEASE, 2mg/kg
    750T
                           500--
    250--
   CONCENTRATION, ppm
  100-r
  75--
  50--
  25-•
QUINOLINE
     RELEASE, Zmg/kg
   4000T
   3000--
   2000- -
    IOOO--
                  -I	1
        1234
           ELUTIONS
              234
              ELUTIONS
Figure 3.  Napthalene and quinoline concentration and curves for
         coal tar waste, test comparison.
                           36

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E
Q.

^ 30000
z
LU
   20000
8  10 000
              1234

                ELUTIONS

            A SLT-S.L.

            O SLT-H20

            D IUCS-H20
Ul
en
<
UJ
_j
LU
CE
   300i—
   200
100
                                                I
                   I
      01234

             ELUTIONS


V  MINN -ACETATE BUFFER

V  MINN - H20

A  REAL  LEACHATE
       Figure 4.  Na concentration and release from a CuO-Na?SCL
                sludge in test leachates.
                                  37

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fourth elution.  The SLT data indicate that the Na is continuing to be
released in the later elutions.  It appears that the waste in the IUCS
test formed a thick layer in the test vessel and was subsequently re-
leased slowly by diffusion.  In the SLT, the tumbling agitation con-
stantly mixed the waste and leachate in order to minimize the amount of
stagnant interstitial water.  Thus the more complete mixing in the SLT
promoted continued dissolution of very soluble components.

ELUTION TIME AND TEMPERATURE

     The effects of two test conditions—time per elution and temperature-
could not be analyzed from the test results.  All the tests were run at the
same temperature, ambient or 20°C.  The IUCS test uses a 48-hour elution
time, while both the Minnesota and SLT tests use 24-hour elution times.
However, the effects of the longer elution time in the IUCS test could not
be ascertained from the data.  Ham, et al_ (1) investigated and discussed
the effects of elution time on leaching test results.

MAXIMUM CONCENTRATION AND MAXIMUM RELEASE

     The SLT uses two procedures:  one in which fresh waste is contacted
with leachate from the previous elution (procedure C) and one in which
fresh leachate is contacted with a previously eluted waste (procedure R).
The IUCS test uses a procedure similar to procedure R, whereas the Minne-
sota test uses only one elution.  Procedure C gives an indication of what
will happen to a given parameter as the leachate passes through a large
volume of waste, i.e., the procedure will approximate or approach maximum
concentrations or saturated conditions.  As landfills will generally have
very high solid/liquid ratios at a given time and the leachates could
often be saturated, this information should be very useful.  On the other
hand, an estimation of the amount of a parameter potentially available to
groundwater requires maximum release under landfill conditions per unit
mass of waste.  The two procedures in the SLT allow estimation of both
maximum concentration and maximum release.  Neither of the other tests,
nor any other tests known to the authors, allow both estimations.  The
IUCS test gives an estimation of maximum release, since it also involves
multiple Teachings of the same waste sample.  The Minnesota test, with
only one elution, cannot be relied upon to provide either maximum concen-
tration or release.

SOLID/LIQUID SEPARATION

     Since the solid/liquid separation was run for all tests, a comparison
of the behavior of separated versus nonseparated wastes is not possible.
However, the procedure is unique to the SLT preparation and is not sug-
gested for either the IUCS or Minnesota tests.   (Neither of the latter
tests gives directions for dealing with predominantly liquid wastes.)
Some comments on the solid/liquid separation are therefore in order.

     The  IUCS  test, specifiq.ations^ read .as follows:

        The  procedure  is to  establish  representative values  of  the
        long-term...leachate properties  of  a waste material  as  placed
        in...landfills  and other disposal sites.   (See Table  4.)
                                     38

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 I ianS?m   ll     ?"S  0V^  obJectlves of a standard leaching test.  In
 a landfill,  the  solid  and  liquid components of the waste should separate
 as  the  liquid percolates down or is absorbed by surrounding material.
 w?thethIecJ-H?i-er^lea^1ng °ccurs on the Sol1d P°rtion of the waste.
 With  the  solid/liquid  ratios  used in the leaching tests, several years
 may be  modeled by  the  tests.  In this time span, certainly a S Id/liquid
 fnS10" Wi-i/?-CU^1n the  landfi11- " is reasonable, therefore  to
 include a solid/liquid separation step in the preparation of wastes having
 liquid  components.  Furthermore, this preparatory step can make the test

 solids  rn±naS^/-H A "*?*£ S^ ™ ^ 'nd ^ waste wi™ a *ery low
 solids  content (6% dry weight) in organic solvents would be very difficult
 to  work with if not separated prior to the test.   First, a 1:10 solid to
 liquid  ratio on dry weight basis would be almost a 2:1  waste to leachate

 third5 nf thftnf I9?-  bar-  The l6aChate WOUld make »P °^ abo"t one-
 inn ?h   tfV0*?1 Jlquid Present.   Second,  the difficulties in separat-
 ing the solid and liquid components  in the ink  and paint waste would
 only be exacerbated by mixing the waste with  the  Teaching solution
 instead of a mixture of organic  solvents  with  some solids,  the waste
would now consist of an emulsion with  a very  low  solids  content.  Separat-
 ing the liquid and solid components  would  now be  even more  difficult
and there would be more samples  to be  separated.   A  solid/liquid separa-
tion scheme  prior to the test makes  the test more  realistic and simpler
 ORGANIC ANALYSIS

      Several  identified organic compounds were quantified in the coal
 tar waste and ink  and  paint waste leachates.   Identified compounds  were
 classified as polar, nonpolar, or slightly polar, as follows:
          Polar:
              cyclohexanone
              phenol
              cresol

          Nonpolar:

              aromatic ring compounds with aliphatic side chains:

                 xylene
                 isopropyl benzene
                 m-ethyl toluene

          Slightly polar:

              quinoline

     The release curves of the polar compounds  from both  wastes were
similar and follow the general release' curve for a  very soluble compound.
The acid leachates are no more effective at solubilizing  these compounds
than were the H20 leachates,  and in the case of cyclohexanone, consider-
ably less effective.
                                   39

-------
     Three of the four nonpolar compounds were not solubilized in  either
acid or H20 leachates.  Naphthalene was solubilized in both acid and
H?0 leachates at about the same concentrations.  These concentrations
were lower and followed a different release pattern than found with polar
compounds.  In the coal tar waste leachates, napthalene appeared to be
saturated.

     Quinoline showed different behavior in acid and H20 leachates,
presumably due to its basic nature (K^ = 3 x 10-'°).  It would be
expected to be more soluble in acidic than in neutral solutions, as
was found in the leachates.

     In short, the acid and H20 leachates exhibited similar leaching
aggressiveness towards polar and nonpolar organic compounds, while the
acid leachate was more aggressive towards quinoline, which is a base.
                                    40

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                             SECTION 5

                          DETAILED RESULTS
     The data are  presented  in  the-following  format:

1.   Description of the waste and a summary of the leaching test results.
2.   Graphical presentation of the SLT data.
3.   Graphical presentation of the test comparison data, including

     A.  SLT procedure R data,
     B.  IUCS test data, and
     C.  Minnesota test data

4.   GC-MS Total Ion Reconstructed Gas Chromatograph


Mass spectra of identified TIRGC peaks are presented in the Appendix.
The format for the description of the waste and summary of test results
is given in Table 16.  The physical and chemical descriptions of the
wastes given by ECHO, Inc. or Chem-Trol, Inc.  are presented as received.
The analytical methods used for the determinations presented by the
companies are not known.

     The complete SLT data is presented separately from the test compari-
son data to avoid cluttering the test comparison graphs.  SLT procedure R
data are presented on both the SLT and test comparison graphs.  The test
comparison graphs thus present only half of the SLT data.  The IUCS and
SLT procedure R procedures are directly comparable.

     A summary of the symbols used in presenting the SLT and test com-
parison data is given in Table 17.

     A discussion of the results for wastes with particularly interest-
ing leaching results follows the graphical  presentation of the data.
                                   41

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       TABLE 16.   FORMAT FOR THE DESCRIPTION  OF WASTES AND

                SUMMARY OF LEACHING TESTS RESULTS
Waste No.
Waste Name

  Source
Physical description
Chemical analysis, if available

     inorganic
     organic

Sample preparation, including S/L sep. procedure.
necessary.
                           Special comments as
                   Maximum Concentration, mg/1

  Acid leaching solutions

     Wisconsin test procedure C, SL
     Wisconsin test procedure R, SL
     Minnesota test, Acetate buffer

  HpO leachates

     Wisconsin test, procedure  C
     Wisconsin test, procedure  R
     IUCS
     Minn.

             Maximum  (Cumulative) Release, mq/kg Waste

  Acid  leaching  solutions

     Wisconsin test, procedure  R,  SL
     Minnesota test, Acetate  buffer

   HpO  leachates

     Wisconsin test, procedure  R
      IUCS test
     Minnesota test
                                  42

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TABLE 17. . SUMMARY OF SYMB.OLS USED IN PRESENTING
           SLT AND TEST COMPARISON DATA
         Standard Leaching  Test Symbols
              Synthetic Leachate
O
                                                —Procedure  C
                   O   Distilled,  Deionized  HgO— Procedure  C
                   /\   Synthetic  Leachate       — Procedure  R
                   O   Distilled,  Deionized  FLO— Procedure  R
            Test Comparison Symbols
               SLT— Synthetic Leachate
           O  SLT— Distilled, Deionized H20
         IUCS Test— Distilled, Deionized H20
    Minnesota Test— Acetate Buffer
    Minnesota Test — Distilled, Deionized H?0
               Real  Leachate Test
                        43

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  TABLETS.   ADHESIVE WASTE #1:   DESCRIPTION  AND  SUMMARY  OF  RESULTS
Waste Number 1, ECHO, Inc.

Description:

     An adhesive manufacturing waste, contains plasticizers DPB and SAIBF
and resins polyvinyl acetate and styrene butadiene, as well as filler and
pigments.  It consists of large chunks of an amber colored gel, sticky to
the touch, which melt at just over room temperature.
Analysis:

ECHO, INC.


Wisconsin:


Organics:

Metals of
Interest:
pH (water slurry) 8.5, Ash 1.1%,  Cd 0.87 ppm,
Pb 3.31 ppm, Cr 0.61 ppm, Zn 6.74 ppm, Cu "1.04 ppm,
no phenol.
99.7% volatile at 600°C, 66% volatile at 105°C for 24
hours, partically soluble in hexane and in acetone.

not analyzed, glued GC injection syringe shut.

Pb, Zn, Cu
 Sample  Preparation:

      Obvious  solid,  cut  into  1-inch cubes.

 Comments:

      Tests  run  at  20°C to  prevent  glue  from melting.   In a test at room
 temperature (25°C),  the  glue  melted,  then  resolidified  incorporating much
 of the  leaching solution in the  resolidified  gel.
                                              (continued)
                                     44

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                      TABLE  18  (continued)

               Maximum Concentration  and  Release
Concentration
Acid leachates
SLT procedure C, SL
SLT procedure R, SL
Minn. Acetate
H20 leachates
SLT procedure C
SLT procedure R
IUCS
Minn.
Release
Acid leachates
SLT procedure R, SL
Minn. Acetate
FLO leachates
SLT procedure R
IUCS
Minn.
(mg/1)
Na_ K_
	 9.0
	 2.75
	 0.85

4.70 24.2
0.88 1.20
7.0 0.15
1.3 0.05
(mg/kg)
Na_ JC
	 65
	 34

15.9 14.4
40.7 2.7
52. 20.
In
0.84
0.58
0.32

0.58
0.10
B.D.
0.34
In
15
6.8

2.8
2.0
0.
Pb, Cu:  all samples below detection.
B.D.:    below detection.
                               45

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                     ADHESIVE  WASTE  NO.I
                     	PROCEDURE C   * SYNTH. LEACH.
                     	PROCEDURE R  • HgO
                      PH
                     5-1-
                      4--
                      3--
                   CONDUCTIVITY, ^MHOS/CM
                   1500-r
                    IOOO--
                    500 -
                                   2
                              ELUTIONS
Figure 5.  pH and specific conductance curves  for adhesive waste  #1, SLT.
                                 46

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                  ADHESIVE  WASTE NO.I
            Nd a  K' CONCENTRATION  a RELEASE

           — PROCEDURE C     A SYNTHETIC LEACHATE
                              © H20
	PROCEDURE R

 Na CONCENTRATION, ppm  ""'Nd RELEASE, Smg/kg
 6.0-r                      60-r
      4.0
      2.0
                           40--
                                 20
                                               _- — —*
       K CONCENTRATION, ppm
       12 T         f24.2
       8--
       4--
               ELUT10NS
                           K RELEASE,  2mg/kg
                           I20T
                          80--
                          40--
                                I       2
                                  ELUTIONS
Figure 6.  Na and K concentration and release curves for Adhesive
         Waste #1, SLT.
                          47

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                  ADHESIVE  WASTE  NO. I
             Mg a Zn »  CONCENTRATION a  RELEASE
             —— PROCEDURE C    * SYNTHETIC LEACHATE
             	PROCEDURE R    • HgO
        Mg CONCENTRATION, ppm
        2.0 T-
         1.5 - -
         I.O--
        0.5--
                           Mg RELEASE,Smg/kg
                           16..-
                           12--
                           6--
                           4--   /
                            T
                                    /    /
        Zn  CONCENTRATION, ppm
         1.5-r
1.0--
         0.5--  *=r--.-_
            2      3
         ELUTIONS
                           Zn  RELEASE, SmgAg
                                    10"
                           5--
                                                  //
                                            ELUTIONS
Figure 7.  Mg and Zn concentration and release curves for Adhesive
         Waste #1, SLT.
                            48

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           ADHESIVE  WASTE NO. J
  	PROCEDURE C	PROCEDURE R
COD  CONCENTRATION, ppm    COD RELEASE, 2g/kg
1200-r
800
      400- •
       •i	1—	1
        I      2      3
           ELUTIONS
                               15-r
                               IO-

                                     \       2
                                        ELUTIONS
Figure 8.  COD concentration and release curves for Adhesive Waste #1,
         SLT.
                            49

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        ADHESIVE WASTE  NO. I  TEST  COMPARISON
          pH,  CONDUCTIVITY, Nd' CONCENTRATION a RELEASE

          ASLT-S.L.
          O SLT - H20               V MlNN - ACETATE BUFFER
          DlUCS-HoO              ^
          DH                    CONDUCTIVITY
         6-r                       75-r
         5--
50--
                                  25--
         Na CONCENTRATION, ppm
         12-r
               1   234
                  ELUT10NS
 Na RELEASE, 2mg/kg
60-
                                   40--
                                   20--
                                            +—\	1	1
       1234
          ELUT10NS
Figure 9.  pH, specific conductance,  and Na concentration and release
         curves for Adhesive Waste  #1, test comparison.
                            50

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         ADHESIVE  WASTE NO.  I  TEST COMPARISON
          K a Zn =  CONCENTRATION a RELEASE
        A SLT- S.L.
        O SLT - H20             V MINN - ACETATE BUFFER
        D IUCS - HgO             W MINN- HgO
      K CONCENTRATION, ppm        K RELEASE,  Smg/kg
      3.0-r     >A                 90T
      2.0-•
      1.0 --
60--
30--
      Zn CONCENTRATION, ppm
    0.75
     0.50- -
    0.25--
 Zn RELEASE, 2mg/kg
 15-r
 10--
 5--
               2345
               ELUTIONS
         2345
         ELUTIONS
Figure 10.  K and Zn concentration and release curves for Adhesive
          Waste #1, test comparison.
                            51

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        TABLE 19.   INK AND PAINT WASTE (I.PVJ):   DESCRIPTION

                      AND SUMMARY OF RESULTS



Waste Number 2, ECHO, Inc.

Description:

     Contains alky! resins, vinyl acrylics, aromatic and aliphatic
solvents.  A black slightly viscous fluid with no noticeable solids
on the bottom of the container.

Chemical Analysis:
ECHO, INC:


Wisconsin:



Organics:
 Trace Metals
 of Interest:
flash point 100°C, ash 4.6%, Cd 110 ppm, Hg 0.02 ppm,
Pb 0.51 ppm, Cr 0.12 ppm, Zn 190 ppm, Cu 0.11  ppm.

97.2% volatile at 600°C, 78% volatile at 105°C for
24 hours, specific gravity 0.88.  Solids 49% volatile
at 105°C, dry solids were 5.9% by weight of waste.

Xylene (o,m, + p, CgH10), isopropyl  benzene (cumene-CgH12)

m-ethyltoluene (1-methyl-3 ethyl benzene (CgH12))

cyclohexanone (CgH^O), 2-nor-butoxyethanol (CgH-,^),

3,3,6-trimethylbicyclo(3.1.0)hexan-2~one or
3,5,5-trimethyl-2-cyclohexanone  (CgH140),

Dimethyl glutarate  (C7H1204), napthalene (C-,gH8),

methylnapthalene  (C-,^^).

Zn,  Pb,  Cd
 Sample Preparation:

      Waste is very difficult to separate into solid and liquid components.
 It dissolves Mi 11ipore MF filters and plastic centrifuge tubes and so will  not
 filter through Teflon 0.45 ym filters.  Finally separated using glass
 centrifuge tubes.

 Comments:

      Due to difficulty in separating large quantities of waste, procedure C
 in the SLT, which requires a lot of waste, was not run.  H20 leachates in
 all tests were colored, either green or orange, depending on elution.
                                       52

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     TABLE 19 (continued)



Maximum Concentration and Release
Concentration, ing/1
Acid leachates
SLT procedure R,
Minn. Acetate
H20 leachates
SLT procedure R
IUCS
Minn.
Acid leachates
SLT procedure R,
Minn. Acetate
H20 leachates
SLT -procedure R
IUCS
Mi nn .
Na^
SL —

190
455
35
Rel
Na_
SL

2410
2862
1400
K_
24.5
9

10
30.5
2.5
ease,
K_
505
360

169
274
100
Mg_
23
1.9;

5.5
18
1.3
mg/kg
Mg_,
292
72

83
137
52
Fe_
, .46

3.2
.20
0
Fe
18.4

34
1.8
0
Zn_
36
38-

.27
1.17
0
Zn_
681
1520

2.7
5.8
0
Pb
4.2
10.2

0
.24
0
Pp_
85.5
406

0
0
0
CM.
.20
.14

.34
1.15
.09
Cu_
3.8
5.6

3.9
5.3
0
Cd_
.28
.11

0
0
0
Cd_
4.2
4.4

0
0
0
                   53

-------
              INK  a  PAINT  WASTE
  pH CONDUCTIVITY, a  Nd' CONCENTRATION a RELEASE

---PROCEDURE R  ^YNTHETIC^ACHATE^ *Hg/ ^
8-


7-


6-



5-

4
ouu-
^«
•*
*^
,&'
/ 600-
x»


400-



200-
A 	 ^- 	 *
	 1 	 -l 	 1
"\
\
\
\
\
\
\
\
\
\
\
\
^--^
*"*•<
	 , 	 i 	 1
 Na CONCENTRATION, ppm

200T  >
 I50--
 IOO--
 50--
              +
        I      2      3
           ELUTIONS
                              No RELEASE,  2mg/kg

                             3200-r
                          2400-
                           1600-
                           800--
                                      I      2      3
                                         ELUTIONS
Figure 11.
        PH, specific conductance  and Na concentration and release
        curves for Ink and Paint waste, SLl.
                          54

-------
                   INK a PAINT  WASTE
           K a Mg» CONCENTRATION S RELEASE
      •	PROCEDURE R  A SYNTHETIC  LEACHATE  ©
      K CONCENTRATION, ppm   K RELEASE,  Smg/kg
     30-r                   600-r
20--
10--
                           400- -
                           300--
     Mg  CONCENTRATION, ppm   Mg RELEASE, 2mg/kg
    40r                   400r
    30--
     20--
     10- •
           \
\\
  \\
   v
                      300--
                       200--  A--
                       100
           I      2      3
              ELUT10NS
                              I      2
                                ELUTIONS
Figure 12.  K and Mg concentration and  release curves for Ink and Paint
          Waste, SLT.
                             55

-------
              INK a PAINT  WASTE
           Zn a  Pb» CONCENTRATION a RELEASE
   	PROCEDURE R  ^SYNTHETIC LEACHATE  ® H£C
    Zn  CONCENTRATION, ppm    Zn  RELEASE, Smg/kg
                         900T
   30--
    15
//
        4	*
              600--
300--
                                         /
                           -9-
   Pb CONCENTRATION, ppm    Pb RELEASE, Smg/kg
o-
6-

4-


2-
12-
9-
\
\
\ 6-
\
j^^ \
"^---^A 3-
a m ft
4
X
X A
x xx
J^ ^f*
,'
^^
^ »f
a a 	 a
                2     3
             ELUTIONS
                        ELUTIONS
Figure 13.  Zn and Pb concentration and release curves for Ink and
          Paint Waste, SLT.
                           56

-------
                 INK  a  PAINT  WASTE
    COD CONCENTRATION, ppm
40000-]
30000-

20000-

10000-
* 9 H90
r *
\ 	 PROCEDURE R
\ COD RELEASE, 2g/kg
\ 600y
\
\
\ 400-
\
\
\ 200-
""""--*
	 1 	 1 i
_ — • — *
*"

	 1 	 1 	 4
I       2      3
   ELUT10N3
                                     I       2
                                        ELUTIONS
Figure 14.  COD concentration and release curves for Ink and Paint
          Waste, SLT.
                            57

-------
           INK  a PAINT  WASTE'  S.L.T.
      O H20   A SYNTHETIC LEACHATE	PROCEDURE R
     CONCENTRATION, ppm          RELEASE, 2g/kg
  400-r        CYCLOHEXANONE   4T
  300--
   200--
   100--
          \\
          -fc-
                                3--
2--
     CONCENTRATION,  ppm          RELEASE, 2mg/kg
    I.QT           NAPTHALENE   87
  0.75-
   0.5--
   0.25--
                _Qn "* "" *—-"^
                 2      3
              ELUTIONS
6-
                                4.-
                                p. -
                                        . — — -o— — -y—-O
      I      2
        ELUTIONS
Figure 15.  Cyclohexanone and Napthalene concentration  and release
          curves for Ink and Paint Waste, SLT.
                           58

-------
        INK  a  PAINT WASTES^ TEST COMPARISONS
        PH
      9 i
       8--
       7--
       6--
       5--
   A SLT - S. L.
   o SLT- H20
   0 IUCS - H20
   V MINN - ACETATE BUFFER
   * MINN-H?0

CONDUCTIVITY, //.MHOS / CM
3000-
2000- -
 1000 •-
     Na  CONCENTRATION, ppm
    600-r
    400--
    200--
               2345
                ELUTIONS
   Na  RELEASE, 2mg/kg
4000-r
3000--
2000-
                               1000
            234
           ELUTIONS
Figure 16.  pH, specific conductance and Na concentration and release
          curves for Ink and Paint Waste, test comparison.
                             59

-------
   INK a  PAINT WASTES'  JEST COMPARISONS
              K  &  Mg -  RELEASE a  CONCENTRATION

       A SLT- S. L.        V MINN - ACETATE BUFFER
       O SLT - H20        W MINN - HgO
       DIUCS- H0
    K CONCENTRATION, ppm
  40-r
  30--
  20--
   Mg CONCENTRATION, ppm
  30r
   20--
   10--
            2345
            ELUTIONS
                   K RELEASE, 2mg/kg
                 600 T
                 400--
                  200--
                              Mg RELEASE, 2mg/kg
                  300-r
                  200--
                   100--
                            2345
                            ELUTIONS
Figure 17.
K and Mg concentration and release curves for Ink and
Paint Waste, test comparison.
                          60

-------
    INK a PAINT  WASTES' TEST COMPARISONS
         Zn &  Pb:  CONCENTRATION a  RELEASE
      A SLT-S.L.
      O SLT -  H20
      D IUCS- H20
   Zn CONCENTRATION, ppm
 40--
 30--
 20--
  10--
10.0--
 7.5--
 5.0--
 2.5--
                 VMINN - ACETATE  BUFFER
                       - H20
                      Zn  RELEASE, Smg/kg

                  1600-j-

                         v
                  1200--
                  800-
                  400-
       v
Pb CONCENTRATION,    Pb RELEASE, Smg/kg
    PPm           450-r
                  300--
                  150--
                                    234
                                    ELUTIONS
       12345
          ELUTIONS
Figure 18.  Zn and Pb concentration and release curves for Ink and
          Paint Waste, test comparison.
                          61

-------
       INK 8 PAINT  WASTE-- TEST COMPARISON
           A SLT - SYNTHETIC LEACH ATE
           O SLT - H20         V MINN -  ACETATE BUFFER
           DIUCS- H20         ^ MINN-  H20
         CONCENTRATION, ppm         RELEASE, 2g/kg
                      CYCLOHEXANONE   *
             V
      400
      300--
      200-•
       100- •
                    NAPTHALENE
 CONCENTRATION, ppm
     v
I.5T  v
        1.0- •
       0.5- •
                 234
               ELUTION5
                           3--
                           2-
                                   I • •
 RELEASE, Smg/kg
      T
60-r   „
                          40-•
                                  20--
                                   2345
                                    ELUTIONS
Figure 19.
   Cyclohexanone and Napthalene concentration and release
   curves for Ink and Paint Waste,  test comparison.
                              62

-------
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-------
Discussion

     The inorganic parameters are not of great interest.   Pb and Zn were
released in acid leaching solutions but not in H20 leachates, and both
were released in higher concentrations in the Minnesota leachates than
in the SLT leachates.

     The organic parameters are of interest and were thoroughly investi-
gated.  COD in the SLT H£0 leachates shows that very large amounts of
organic compounds were being released.  The h^O leachates in all tests
were colored—the first day the color was a combination of green and
orange, while on subsequent elutions the color was orange.  The relatively
low conductivity indicates that nonionic compounds were being released.

     Extensive gas chromatograph—mass spectrometry analysis of both the
waste hexane extract and the leachates was done.

     The waste hexane extract showed that the waste contained at least
six aromatic ring compounds with alky! side chains.  Th.ese elute in the
total ion reconstructed gas chromatogram (TIR6C) at peaks numbered 42,
47, 59, 104, 126, and 135 (see Figure 20).  Three were identified as
xylene (peak number 42), isopropylbenzene (also called cumene, peak
number 47), and m-ethyltoluene ^peak number 59).  The structures for
these compounds are given below.
  (xylene,o,m, p)
isopropyl  benzene
                                                   m-ethyltoluene
                                            (1-methyl-3-ethyl  benzene)
The other aromatic compounds with alkyl side chains could not be further
characterized.  Five other compounds were positively identified in the
waste.  Their structures and peak numbers are given in the following
drawings:
                                    67

-------
   cyclohexanone
    peak No. 66
                        -C4HgnOCH2CH2OH

                      2-nor-butoxyethanol

                          peak No. 76
                                                  Dimethyl  glutarate

                                                     peak  No.  229
 napthalene
peak No. 309
                           methylnapthalene (a and/or 3)
                                    peak No. 450
     In addition, peak number 188 was identified as either 3,3,6-trimethyl
bicyclo (3.1.0.) hexan-2-one or 3,5,.5-trimethyl-2-cyclohexanone.
     Six of the identified compounds were analyzed in the leachate extracts.
The three identified aromatic compounds with alkyl side chains were found
to not elute in any of the test procedures or with any leaching solution.
The substance in peak 188 was found to e-Tute in leachates from all tests
in significant concentrations.  No standards of either compound were avail-
able, so neither positive identification nor quantification could be made.
     Cyclohexanone and napthalene were quantified in the leachates.  The
release patterns of both compounds are given in Figures 15 and 19.  Cyclo-
hexanone is released in high concentrations, with the highest concentra-
tions coming in the first elution.  In the IUCS test, the cyclohexanone
reached a constant concentration after the first elution, whereas, in the
SLT the concentration decreased with each elution.  In both the SLT and
the Minnesota tests, the HeO leachates had higher cyclohexanone concen-
trations than the acid leachates.  Napthalene was released in low concen-
trations in a pattern that is very difficult to interpret.  The Minnesota
test had the highest napthalene concentrations and release.
     The high COD concentrations leached from the waste and the comparatively
small amounts of materials identified indicate that much of the leached
organic material was not identified.  The use of a relatively nonpolar
solvent for extracting the waste or leachate emphasizes the analysis of
compounds of lower polarity,  Noting the lack of aromatic compounds  _
with side chains in the leachates, it is apparent that the high organic
leaching from the waste, as indicated by the high COD concentrations,
does not cause solubilization of these nonpolar compounds.  The high COD
concentrations should be of concern when considering landfill ing of this
waste.
     The use of GC-MS for analysis of unidentified or unclassified organic
compounds is not recommended for routine use in a standard test.  GC-MS
analyses require highly trained personnel and considerable time.  The
identification of a specific compound in a waste when the identity or
general classification of the compound is not known is very difficult
and time consuming.  Note that Figures A-l through A-9 present additional
GC-MS results.

                                      68

-------
   TABLE 20.   COAL TAR SLUDGE:   DESCRIPTION  AND  SUMMARY  OF  RESULTS




Haste Number 3. ECHO,  Inc.

Physical Description:   Thick, viscous tar floating on water layer.

Chemical Description:

     ECHO
     Wisconsin
        (solid)

     Organics
     Trace Metals of
     Interest

Sample Preparation:
- BTU - 14000/lb, flash point 98°C, Ash 2.7%,
  Cd 1.15 ppm, Pb 29.9 ppm, Cr 51.5 ppm,
  Zn 107 ppm, Cu 9.7 ppm.

- 62% volatile at 600°C
  29% volatile at 105°C, 24 hours

- phenol, cresol, napthalene and quinoline identi'
  fied in leachate
- Cu, Zn, Cr, Pb
     Floating tar sampled directly.  Homogenization of water and tar
layers would have been impossible given consistency of tar.   Tar dif-
ficult to clean.
                                              (continued)
                                    69

-------
                     TABLE 20  (continued)


                Maximum Concentration  and  Release

                      Concentration, mg/1

  Acid  leachates  Na_   K_    Mg_   Zn_   COD    Napt.   Phenol   Cresol   Quinoline
   SLT proc.  C, SL
   SLT proc.  R, SL
    Minn. Acet.
54    1.4  .50
 9.3   .56 .42
  .94  .15 .12
12.7
21.9
 2.8
493
 96
  2.6
138
 58.5
  1.4
307
 93.5
  0
  HO  leachates
Ol_ 1
SLT
IUCS
Minn
pi uv..
proc.

.
o
R


U •
4.
0.
1.
I W
0
49
2
"T
1


.9
.40
.14
.65
.59
.17
w
0
0
0
20.1
20.9
5.7
2.4
193
112
67.9
2.7
80.2
58.1
36.5
1.3
64.0
62.0
26
0
                          Release,  mg/kg
 Acid  leachates   Na
       Ma.  ZH
        Phenol  Cresol  Quinoline
SLT proc. R,

FLO leachates
SLT proc. R
IUCS
Minn.
SL


59
7.
48
167
37.

25.
5 2.
5.

6

5
9
6
10.9
6

11
3.7
6.8
11.0
4.8

0
0
0
624
112

15390 578
4492 81.2
4560 96
1644
104

1949
472
108
1290
56

1338
288
52
2176
0

1726
333
0
     Cu,  Cr,  Zn  and  Pb were below detection.

     Note that the Napthalene and Quinoline concentration and release
test comparison curves were presented earlier as Figure 3.
                                      70

-------
                     COAL TAR  RESIDUE
                   ^SYNTHETIC LEACHATE  ®
                        	PROCEDURE C
                    PH	PROCEDURE R
                   8 T
                   6--
                   4--
                 CONDUCTIVITY, jiMHOS/CM
                 1500-r
                 1000- -
                 5 00--
                            I      2      3
                           ELUTIONS

Figure 24.  pH and specific conductance curves for Coal Tar Waste, SLT.
                             71

-------
                  COAL TAR  RESIDUE
              PROCEDURE C    A SYNTHETIC  LEACHATE
              PROCEDURE R   ® HO
   Na CONCENTRATION,ppm     Na  CUMULATIVE RELEASE,
   80-r
   60--
   40-.
   20--
   T
 75-
 5O--
 25--
                                   Zmg/kg
    K CONCENTRATION, ppm
    15-r         ts4
    10-•
    5--
    0--
          I
K CUMULATIVE RELEASE,
200T 2mg/kg
 I50--
 100--
 50--
                                                  -{
Figure 25.  Na and K concentration and release curves for Coal  Tar
          Waste, SLT.
                           72

-------
                 COAL TAR  WASTE
              Mg& COD= CONCENTRATION a RELEASE
        	 PROCEDURE C      «H2O
        	PROCEDURE R      A SYNTHETIC LEACHATE
        Mg CONCENTRATION, ppm    Mg RELEASE, Smg/kg
       3-r
                              20--
                              10--
                                           	®
                                               .-A
    COD CONCENTRATION, ppm      COD RELEASE, Eg/kg
s-uuu-
3OOO-



2000-
1000-
2O-
15-



/ 10
*^^^ 5"
	 1 	 ! 	 — J
X*
X
X
X
/x
	 1. 	 1 -,.,,.J
            I      2      3
               ELUTIONS
I      2      3
   ELUTIONS
Figure 26.  Mg and COD concentration and release curves for Coal Tar
          Waste, SLT.
                           73

-------
               COAL  TAR RESIDUE

     	 PROCEDURE C        © HgO
     	PROCEDURE R        A SYNTHETIC  LEACH ATE
                      NAPTHALENE
     CONCENTRATION, ppm        RELEASE.Zmg/kg

     30-r
     20-
      10-
r-r=t
           500-
           250--
                        PHENOL
     CONCENTRATION, ppm
    800T
    600-
    400-•
     200--
            RELEASE, 2mg /kg

          2250T
           1500- -
           750--
                                                    H
            I      2
               ELUTIONS
                  "j	2~"   3
                      ELUTIONS
Fjgure 27.  Napthalene and Phenol  concentration and release curves
          for Coal  Tar Waste, SLT.
                           74

-------
                   COAL TAR  RESIDUE

       	 PROCEDURE C        ®HgO
      	PROCEDURE R        A SYNTHETIC LEACHATE
                      CREOSOLS (O.M.aP)
     CONCENTRATION,ppm          RELEASE, 2mg/kg
    200T
     100- -
 1500-
  750
     CONCENTRATION, ppm
           400 T
    200T  200- -
     I50--
     IOO--
     50--
                       QUINOLINE
RELEASE, Smg/kg

 3000T
 20OO- -
 1000--
           o- —
                                        .'  *v
         f
                                      I       2
                                        ELUTIONS
           I       2
             ELUTIONS
Figure 28.  Creosols and Quinoline concentration  and release curves
          for Coal Tar Waste, SLT.
                           75

-------
             COAL TAR  WASTED JEST  COMPARISON
       PH
      8-r
       6--
           ASLT - S.L.
           o SLT - H20
           D IUCS-H20
                       V MINN-ACETATE BUFFER
                       V MINN-H20

                           CONDUCTIVITY, ^.MHOS/CM
                         600 T
                                   400--
                                    200--
      Na  CONCENTRATION, ppm
      1.51         of 6.9
      I.O--
      0.5--
                234
                ELUTIONS
                        Na  RELEASE, 2rng/kQ
                       90-r
                       60
                       30--
                                 234
                                ELUTiONS
Figure 29.
pH, specific conductance,  and Na concentration and release
curves for Coal Tar Waste, test comparison.
                            76

-------
        COAL TAR  WASTE * TEST  COMPARISON
              K a Mg= CONCENTRATION a RELEASE
           A SLT - S.L.            , V MINN - ACETATE BUFFER
           O SLT - HpO             V MINN - Hp 0
           DiUCS- HoO
       K CONCENTRATION, ppm
      !6T
      12--
       8--
       4-
K  RELEASE, Smg/kg
I50--
IOO--
 50--
       Mg CONCENTRATION, ppm
     0.9-r
     0.6--
     0.3--
            12345
               ELUTIONS
  Mg RELEASE, 2mg/kg
 18-r
 12--
  6--
                                                4—H
       1234
          ELUTIONS
Figure 30.  K and Mg concentration and release curves for Coal Tar
          Waste, test comparison.
                          77

-------
   COAL TAR WASTE  TEST  COMPARISON
      PHENOL  a CRESOL-- CONCENTRATION a RELEASE
      ASLT-S.L.
                        V MINN - ACETATE BUFFER
     OSLT- H20
     DIUCS- H20
 PHENOL CONCENTRATION,
125 T
  100-
  75--
  50--
  25--
                          MINN- H20
                           PHENOL RELEASE, Smg/kg
                          2500-r
                         2000--
                         1500--
                         IOOO--
                          500--
                   CREOSOL (0, M, 8 P)
   CONCENTRATION, ppm        RELEASE, 2mg/kg
  60-r  A                  I500T
   40--
   20--
                          1000--
                          5OO--
            2345
            ELUTIONS
                                    23   45
                                    ELUTIONS
Figure 31.  Phenol  and Creosol concentration and release curves for
          Coal Tar Waste, test comparison.
                          78

-------
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                                                                                      o

                                                                                      .£=
                                                                                      o  •
                                                                                         O)
                                                                                      to -t-»
                                                                                      fO CO
                                                                                      CD 
                                            80

-------
 Discussion

     The waste's  physical composition, much  like  road  tar,  seems  to  be an
 important factor  in controlling  the  leaching test results.

     The inorganic parameters are not of much interest.  Na,  K, Mg,  and
 Zn  are  leached  in low  concentrations, while  Cu  is below detection.

     Organic  parameters are of interest.   Phenols and  cresols  (ortho,
 meta and para)  were presumed to  be present due  to their common occurrence
 in  coal tar wastes, and so test  leachates  were  analyzed for these compounds.
 The leachates were distilled using the distillation procedure given  in
 Standard Methods  (3),  then analyzed  on a GC-MS.   Napthalene and
 quinoline were  also found in the distillates.   The structures for these
 compounds are given below:
     phenol
cresol
quinoline
napthalene
     Phenol and cresol are both polar compounds due to the OH group.
Quinoline is slightly polar and napthalene nonpolar.  Phenol and cresol
show similar behavior—increasing concentrations in both SL and H2<3
leachates using procedure C and decreasing concentrations in procedure R.
From the concentrations in procedure C leachates, it is  apparent that the
solutions are not saturated with either phenol or cresol at the end of the
test, while the decreasing concentrations in procedure R show that the
waste has not been completely depleted of either component.  Napthalene,
on the other hand, behaves as if it were saturated in both SL and H20
leachates.  The napthalene concentrations in both leachates maintains
steady values throughout the test.  The similarity in napthalene concentra-
tion in the SL and H20 leachates show that the leachate composition does
not have a great effect on solubilizing naphthalene.

     Quinoline, on the other hand, shows different leaching patterns in
SL and HgO leaching solutions.  The H20 leachates have constant concen-
trations, indicating saturation, while the SL leachates have a rising
concentration in procedure C leachates and a falling concentration in
procedure R.

     Quinoline is a base (K.  = 3 x 10~10) and should be more soluble in
acid solutions than in neutral or basic solutions.   Quinoline concentra-
tions in the  SL and H20 leachates from procedure C of the SLT shows the
differing solubilities quite well.   In SL samples,  the quinoline con-
centration rises in each procedure C elution, suggesting that the amount
of quinoline  available for leaching controlled the concentration, and
                                     81

-------
that quinoline was not near saturation.  In the M leacha,tes, on the
other hand, the quinoline behaves as if it were saturated, i.e., the
concentration is constant in procedure C leachate,  At the pH of the
SL (4.5), much of the quinoline (Q) should t»e protonated (i,e,, be in
the form HQ+) and should be more spluble than the unprotonated quinqline.
At the pH of the HeO leachates ( 7), quinoline should be predominately
unprotonated.  In short, at a pH of about 7, qwinoline (in an unprotonated
form) appears to be saturated in the SIT HgQ leachates a,t a concentration
of around 60 mg/1, while in the acid SL, quinoline (in a protonated form)
appears to be unsaturated at concentrations over 300 mg/1.
                                     82

-------
          TABLE 21.  HEALTH AND BEAUTY CARE WASTE (HBC):

                .DESCRIPTION AND SUMMARY OF RESULTS


       (Including Latex from Paint Manufacture.and Some Basic

                    Chemical Salt Wash Water)
Waste Number 4, ECHO, Inc.

Physical Description:


Chemical Analysis:

     ECHO



     Wisconsin



     Organics

     Trace Metal  of Interest

Sample Preparation:
slightly viscous emulsion, black,
some noticeable solids.
pH-5.9, sus. solids-1%, Ash 6.1%, Cd.07 ppm,
Hg .02 ppm, Pb 1.1 ppm, Cr .40 ppm, Zn 18 ppm,
Cu 2.8 ppm.
99.2% volatile at 600°C
27% volatile at 105°C for 24 hours
specific gravity, 0.85

None specified.

Pb, Zn, Cu

separates with centrifugation
solids  - 38.9% volatile at 105°C, 24 hours
solids  (dry weight) compose 2.8% of waste
                                                         (continued)
                                      83

-------
      TABLE 21 (continued)
Maximum Concentration and Release
Acid leachates
SLT proc. C,
SLT proc. R,
Minn. Acet.
FLO leachates
SLT proc. C
SLT proc. R
IUCS
Minn.

Acid leachates
SLT proc. R,
Minn. Acet.
O leachates
SLT proc. R
IUCS
Minn.
Concentration, mg/1
Na_ K Mg Zn
SL
SL


630
294
570
58

Na_
SL


3590
3211
2320
182
67
1.7

88
48.9
84
1.1
Rel
1<
921
68

615
500
44
32
12.2
2.6

18
8.70
18.4
1.8
ease,
Mg_
154
104

123
98
72
25.0
12.8
2.9

11.0
5.9
11.5
1.4
mg/kg
ZD_
174
116

73
67
56
Cd Fe
.92
.39
52

122
.14 37.0
81.0
11

Cd Fe
6.0
2080

1.4 543
440
440
Cu Pb
5.60 0.86
1.55 0.69
9.6 .40

14.0 0
5.9 0
10 0
1.5 0

Cu Pb
38 18.8
384 16

112 0
79.2 0
60 8.4
COD




93,600
12,760
33,600


COD



1.49 1
1.86 1

                       84

-------
           HEALTH a BEAUTY  CARE WASTE
                     e  H20
                     A  SYNTHETIC LEACHATE
                  	  PROCEDURE C
                  	  PROCEDURE R
                    pH
                   5-r
                   4--
                   3--
                    2--
                6000--
Figure 34.
        CONDUCTIVITY, ^MHOS/CM
      8000-r
                    A



      4000+    ' '      *
                2000
              I       2      3
                 ELUTIONS

pH and specific conductance curves for Health and Beauty
Care Waste, SLT.
                           85

-------
400-•
200--
     HEALTH a BEAUTY CARE  WASTE
      Na a K: CONCENTRATION a RELEASE
                         • H20
                         A SYNTHETIC LEACHATE
                           No RELEASE, 2mg/kg
                         6000T
      	PROCEDURE C
      	PROCEDURE R
     Na CONCENTRATION, ppm
    600-r         *
          \
                            4000--
                             2000--
  K CONCENTRATION, ppm      K RELEASE, Smg/kg
200-r                    1000-
 150-•
 IOO--
     50--
       I       2
         ELUTIONS
                              750 •-
                              5OO--
                          250--
                                           2
                                       ELUTIONS
Figure 35.
      Na and K concentration and release curves for Health and
      Beauty Care Waste, SLT.
                      86

-------
         HEALTH  a  BEAUTY  CARE  WASTE
          Mg aZn>  CONCENTRATION  a RELEASE
      	PROCEDURE C        9 H20
      	PROCEDURE R        A SYNTHETIC LEACHATE
     Mg CONCENTRATION
    40-
    30--
    20--
     10-
 Mg RELEASE,  2mg/kg
200-T-
 I50--
 100--
 50-
    Zn CONCENTRATION, ppm
    3O-r
    20--
          I      2      3
           ELUTIONS
 Zn RELEASE,  Smg/kg
200-r
 I50--
                              IOO--
                              5O--
                                  •H	1	1
                                    I      2      3
                                       ELUTIONS

Figure 36.  Mg and Zn concentration and release curves for Health and
          Beauty Care Waste, SLT.
                            87

-------
    HEALTH a BEAUTY CARE WASTE
     Cu a Cch CONCENTRATION  a RELEASE
     PROCEDURE C
	PROCEDURE R
Cu CONCENTRATION, ppm
     4--
                               H20
                               SYNTHETIC LEACHATE
                               Cu RELEASE, 2mg/kg
                              150-r
                         100-•
                               50--
     Cd CONCENTRATION, ppm
    1.5-r
     I.O--
    0.5- •
           I      2
             ELUTIONS
                          Cd RELEASE, 2mg/kg
                         7.5T
                          5.0-
                          2.5--
                                I       2
                                  ELUTIONS
Figure 37.
    Cu and Cd concentration and release curves for Health and
    Beauty Care Waste, SLT.
                             88

-------
            HEALTH  a BEAUTY  CARE WASTE
            Fe a Pb: CONCENTRATION a RELEASE
       	PROCEDURE C       ©H20
       	PROCEDURE R       ^SYNTHETIC LEACHATE
       Fe CONCENTRATION, ppm    Fe RELEASE, 2mg/kg
       i£tj-          •            -
I£U-
80-
40-
Pb
1.5-1
.0-
).5-
* 600
400-
*. 400-
\
. — |- T""*?
CONCENTRATION, ppm Pb
20-
f. ,,,11 A
^ ^w**
• --**' I0
DETECTION LIMIT
n ' — — -X
	 Q .g> O
— -«
/*~-~~
S
*'

— 	 1 	 f
RELEASE,2mg/kg
,**
**'
^
«''
	 1 	 — i 	 	 i
I      2      3
   ELUTIONS
                                          2     3
                                      ELUTtONS
Figure 38.  Fe and Pb concentration and release curves for Health
          and Beauty Care Waste, SLT.
                          89

-------
         HEALTH a BEAUTY CARE  WASTE
                             • H20
                             T IUCS
                            COD RELEASE,  Sg/kg
                            lOOr
                            75-
                            50-
                            25--
    	 PROCEDUREC
    	 PROCEDURE R
   COD CONCENTRATION, ppm
35000T
30000-
25000-
20000
15000
10000- -
 5000- -
         1234
            ELUTfONS

Figure 39.  COD concentration and release curves for Health and
          Beauty Care Waste, SLT.
                                  12345
                                     ELUTIONS
                         90

-------
   HEALTH 8 BEAUTY CARE WASTE TEST COMPARISON
       pH, CONDUCTIVITY, Na« CONCENTRATION a RELEASE
       ASLT-S. L.
                               V MINN - ACETATE  BUFFER
                               V MINN - H20
                              CONDUCTIVITY,  ^MHOS/CM
                             800C-T
O SLT - H20
DIUCS-H20
     5--
     4--
     3--
                     6000- •
                     4000- •
                     2000-
     No CONCENTRATION, ppm     Na RELEASE, 2mg/kg
   600-r  _                 4500-
   400--
   400--
             2345
             ELUTIONS
                    3000--
                     I500--
                            12345
                               ELUTIONS
Figure 40.  pH, specific conductance, and Na concentration and release
          curves for Health and Beauty Care Waste, test comparison.
                            91

-------
HEALTH a BEAUTY  CARE WASTE TEST COMPARISON
              K a Mg = CONCENTRATION a RELEASE
        A SLT -  S. L.
        O SLT -  H20
         DlUCS-H20
      K CONCENTRATION, ppm      K RELEASE, Smg/kg
                              V MINN - ACETATE BUFFER
     90i
                               900i
                              600-
                              300--
      Mg CONCENTRATION, ppm
      18-r  ~
           12345
              ELUT10NS
                                 Mg RELEASE,   2mg/kg
                                I50T
                               100--
                               50--
                                        4-
                                            4-
                                      12345
                                         ELUTIONS
Figure 41
           K and Mg concentration and release curves for Health and
           Beauty Care Waste, test comparison.
                           92

-------
HEALTH a BEAUTY CARE  WASTE TEST COMPARISON
      Zn a Fe= CONCENTRATION a RELEASE
     A SLT - S. L
     OSLT - H20            y MINN-ACETATE BUFFER
     DIUCS- H20            VMINN-H20
   Zn CONCENTRATION, ppm       Zn RELEASE, Smg/kg
                           180-r
                           I20--
                            60--
   Fe CONCENTRATION,ppm
 40--
       1234
          ELUTIONS
  Fe RELEASE, 2mg/kg
2000 T  V
                          I500--
IOOO--
                          500--
                                        1-
        1234
          ELUTIONS
Figure 42.  Zn and Fe concentration and release curves for Health and
          Beauty Care Waste, test comparison.
                           93

-------
HEALTH a BEAUTY CARE  WASTE TEST COMPARISON
        Cu  a Pb=  CONCENTRATION a RELEASE
          ASLT-S.L.
          OSLT-  H20
          D1UCS - H20
                  VMINN- ACETATE  BUFFER
       Cu CONCENTION, ppm
      I2T
                  VMINN -H20
                    Cu RELEASE, Smg/kg
                   120 T
                                80-
                                40--
       Pb CONCENTRATION, ppm
      1.0 -r
      0.5-•
DETECTION LIMIT  x


—IS	fH	$	EC
  2345
 ELUTIONS
                    Pb RELEASE,  Smg/kg
                   20-r
                    10- •
                                      H	1	h
                                       1234
                                        ELUTIONS
 Figure 43.  Cu and Pb concentration and release curves for Health and
           Beauty Care Waste, test comparison.
                             94

-------
 LU
 I—
 CT3
 cn
 UJ
 Hi
 cc
cr o
UJ C3
CO CK
    I—I
Q *—

cr

re
_
cr
UJ
re

•>*
*
                                                                                       O
                                                                                       to


                                                                                      4->
                                                                                       X
                                                                                       0)
                                                                                      (C
                                                                                      X
                                                                                      OJ
                                                                                       
 o
 3
 S-
                                                                                      O
                                                                                      o
                                                                                      ai


                                                                                      c:
                                                                                      o
 a>
cn

tZ
                                          95

-------
Discussion


SLT-

     The H?0 leachates contained a significant oil  layer, one which was
emulsified when passing through a filter but which  rapidly separated on
standing.  The heavy oil layer, particularly in the procedure C leachates
made analysis difficult.  Several samples were not  analyzed for parameters
measured by atomic absorption for this reason.

     The waste gave leaching results which are difficult to explain.  For
example, the pH data for H20 leachates indicate the release of acidic mate-
rials   Both procedure C and procedure R HoO leachates become more acidic
in successive elutions.  However, one of the procedure R duplicates and
the procedure C leachate show a pH minimum in the second elution, while
the other procedure R duplicate shows a steadily decreasing pH.  The
duplicates are two pH units apart on the second elution.  Why the dupli-
cates should be so far apart, and why the procedure C leachates should show
a minimum are not known nor easily explained.

     The inorganic elements behave normally, with the exception of Cu.  The
H?0 leachates had higher Cu concentrations than the corresponding SL leach-
ates    Cu was released  in fairly high amounts.  Cd was detectable although
was not released in high concentrations.  Thp COD concentrations were  very
high indicating the observed oil release.

     The TIRGC from GC-MS analysis of organics is shown  as Figure  44.
Peaks were not required to be  identified for  this waste.
 Test Comparison--

      Test comparison results  are interesting primarily  in  the  higher  Fe
 and Cu concentrations,  seen in the IUCS leachates  than  in  the  acid  leach-
 ates.  pH does not seem to be the controlling factor in the  release of
 these metals.   The COD  of the IUCS leachates was considerably  higher  than
 that of the SLT procedure R HeO leachates.   Perhaps Fe  and Cu  are corn-
 pi exed with organics or are in organic form and are released with the
 organic materials.
                                     96

-------
      TABLE 22.  FOOD GRADE WASTE:  DESCRIPTION AND
                        SUMMARY OF RESULTS
Haste Number 5, ECHO, Inc.
Physical Description:
Chemical Analysis:
     ECHO

     Wisconsin (solid):
     Organics:
     Trace Metals of Interest
Sample Preparation:
Comments:
Fatty layer floating on water.   Fat
layer looks like oily brown corn mush.
pH 8.7, sus. solids 1.3%, Ash 1%, Cd .003 ppm,
Hg 0, pB .001 ppm, Cr .40 ppm, Zn .011  ppm,
Cu .001
20% volatile at 105°C for 24 hours
None specified
None
Solid layer sampled directly
Some leachate absorbed by waste in
procedure C samples.
                                              (continued)
                                      97

-------
                      TABLE 22 (continued)
                Maximum Concentration and Release
                       Concentration, mg/1
Acid leachates

     SLT procedure C, SL
     SLT procedure R, SL
     Mi nn.

HpO leachates

     SLT procedure C
     SLT procedure R
     IUCS
     Minn.
                                 Na
            JC

          36.5
          11.5
           1.4
              Ma

             19.9
              5.45
               .45
  Zn_

147.
 26.3
  1.8
106.9
24.0
45.
2.4
18.0
5.1
8.5
.39
16.0
5.0
8.
.37
4.9
3.3
3.9
1.0
                           Release, rhg/kg
Acid leachates
Na
     SLT procedure R, SL
     Minn.
   K.

209.
 56.
                      74.6
                      18.
  Zn_

627.
 72.
FLO leachates
     SLT procedure R
     IUCS
     Minn.
319.
234.
96.,
64.
44.
16.
56.8
41.1
15.6
42.
27.8
38.
                                  98

-------
                  FOOD  GRADE  WASTE
                — PROCEDURE  C  * SYNTH. LEACH.
                •—PROCEDURE  R  • H£0

                   PH
                  7 T-
                   6--

                 CONDUCTIVITY,  aMHOS/CM
                I500T
                IOOO--
                500--
                        I      2      3
                         ELUTIONS


Figure 45.  pH and specific  conductance curves for Food Grade Waste, SLT.
                             99

-------
              FOOD  GRADE  WASTE
          Na a K *  CONCENTRATION a RELEASE
    	PROCEDURE C     A SYNTHETIC LEACHATE
    	PROCEDURE R     ® HO
    Na CONCENTRATION, ppm
    125 T
    IOO--
                    Na  RELEASE,2mg/kg
                   50O-r
                   400"
                             300 --
                             200--
                              100--
     K CONCENTRATION, ppm
    40 T
     30-
     20--
      10- •
                     K RELEASE,  mg/kg
                    320 T
                    240-
                              160-
                               80--
                                ,*•'
                                           -f
                                     I      2      3
                                       ELUT10NS
Figure 46.
 I       2      3
    ELUTIONS
Na and K  concentration and release curves for Food Grade
Waste, SLT.
                          100

-------
            FOOD GRADE  WASTE
       Mg  a Zn= CONCENTRATION  a RELEASE

       	PROCEDURE C      A  SYNTHETIC LEACHATE
     	PROCEDURE R

     Mg CONCENTRATION,ppm
     20-r
      15-
      10--
*  H2°
   Mg RELEASE, Smg/kg
  80T
  60--
  40-
                               20--
                                    &•'
     Zn CONCENTRATION, ppm
     150-r
     100--
     50--
           I      2
            ELUTIONS
  Zn RELEASE, Smg/kg
 750-r
 500--
 25O--  *
                                         s/
        \      2
          ELUTIONS
Figure 47.  Mg and Zn concentration and release curves for Food Grade
          Waste, SLT.
                         101

-------
             FOOD GRADE WASTE
             PROCEDURE C
     	 PROCEDURE R
  COD CONCENTRATION, ppm    COD RELEASE, 2g/kg
  8000-r                   40-r
  6000-
  4000--
  2000- -
                30--
                 20--
                 10--
^
                                       4-
                                   ^
I      2      3
   ELUTIONS
                                 I      2      3
                                    ELUTFONS
Figure 48.  COD concentration and release curves for Food Grade Waste,
          SLT.
                            102

-------
FOOD GRADE WASTE   TEST  COMPARISON
  pH, CONDUCTIVITY, Na«. CONCENTRATION a RELEASE
ASLT-S.L
                      V MINN-ACETATE BUFFER
                      VMINN- H^O
     OSLT- H20
     DIUCS-H20
    pH
   7-r
   6--
   5--
   4
                       CONDUCTIVfTY, ^MHOS/CM
                       600-r
                       400--
                       200--
      H	\	1-
   Na CONCENTRATION, ppm
  60-r
  4O -
  20--
           234
          ELUTIONS
                        Na RELEASE, Zmg/kg
                       450-r
                       3OO
                        150
                                      •4	1	1	1
                                 234
                                ELUTIONS
Figure 49.  pH,specific conductance, and Na concentration and release
          curves for Food Grade Waste, test comparison.
                           103

-------
     FOOD GRADE WASTE  TEST  COMPARISON
        K a Mg: CONCENTRATION a RELEASE
      A SLT - S.L.
      OSLT - H20
      DIUCS- H00
V MINN-ACETATE BUFFER
^ MINN- H00
    K CONCENTRATION, ppm
    12-r
    8-
   K  RELEASE, Zmg/kg
  300T
                            200-
                             100--
     Mg CONCENTRATION, ppm
    I2T
             234
            ELUTIONS
    Mg RELEASE, 2mg/kg
   75T
                              50-
                              25--
                                    v
                                                 \
          12345
           ELUTIONS
Figure 50.  K and Mg concentration and release curves for Food Grade
          Waste, test comparison.
                           104

-------
       FOOD GRADE  WASTE  TEST COMPARISON
            Ziv  CONCENTRATION  S RELEASE
       A SLT- S.L.
       O SLT - HoO           V MINN - ACETATE BUFFER
       niucs-
H20
H20
   Zn CONCENTRATION, ppm
   40-r
   30--
   20--
   10--
         1234
           ELUTIONS
V MINN
H2O
               Zn RELEASE, 2mg/kg
              800-r
              600--
              400--
              200--
                        234
                        ELUTIONS
Figure 51.  Zn concentration and release curves for Food Grade Waste,
          test comparison.
                           105

-------
CVK
                                            *- ED

                                             r^
- O
  U3
                         O)
                         c:
                         03
                         O
                         O)
                         •o
                         (C
                         •»->
                         o
                         o
                         CO
                         
•r-
LL_
CU
CU
oo


                                           O
                                           to

                                           +J
                                           X
                                           Ol

                                           
                                           CO
                                           O)
                                          -a
                                                                           -a
                                                                            o
                                                                            o
                                          q-
                                           o
                                                                            to-
                                                                            S-'
                                                                            CT>
                                                                            O
 O

J=
 o

 co
 (C
 CD

-a
 cu
4->
 O
 3
 S-
                                                                            o
                                                                            o
                                                                            cu
                                           (O
                                           +j
                                           o
                                           CM
                                           LT>
                                            C1J
106

-------
           TABLE 23.  ADHESIVE WASTE #6:  DESCRIPTION AND

                        SUMMARY OF RESULTS



Waste Number 6, ECHO, Inc.


Description:

     Pressure sensitive adhesives, will contain tackifiers, NBR, and
SBR cuts in hexane, and some filler, predominately carbonates and metal
oxides.  Very sticky, viscous liquid.  Difficult to work with or to
clean from glassware or hands.
Chemical Analysis:

     ECHO:



     Wisconsin:


     Organics:
     Trace Metals of
     Interest:
pH 7.2, suspended solids 0.17%, Cd 0.06 ppm,
Pb 0.54 ppm, Cr 0.13 ppm, Zn 1.21  ppm,
Cu 0.08 ppm

99.7% volatile at 600°C, 34% volatile at 105°C
for 24 hours

Not analyzed.  Sample solidified and clogged
soxhlet extractor.
Zn, Pb, Cr
Sample Preparation:

     Would not filter, sampled directly.

Comments:

     Difficult waste to work with.  Glues caps onto bottles, filters onto
filter frits.  Glassware was cleaned by burning the waste off glass-
ware at 600°C, then washing.

     In procedure C, SLT, some leachate was absorbed by the solid.   It
was very difficult to remove all the solids from the test vessel  in this
procedure, so old waste was not completely removed before fresh waste was
added.
                                   107

-------
                       TABLE  23  (continued)

                 Maximum Concentration and Release

                        Concentration,  mg/1
Acid leachates
     SLT proc. C, SL
     SLT proc. R, SL
     Minn.
 Na
 K_

2.7
2.5
 .99
                    2.20
                     .94
                     .16
         Pb

        b.d.
        b.d.
 C_r

b.d.
b.d.
H?0 leachates
SLT proc.
SLT proc.
IUCS
Minn.
C
R

31.1
2.5
2.9
.6
1.0
.35
.16
.05
2.85
.51
.82
.05
Acid  leachates
      SLT  proc.  R,  SL
      Mi nn.
Release, mg/kg

 Na_        K,

          53.6
          39.6
          ID.

          18.4
          6.4
     leachates

      SLT proc.  R
      IUCS
      Minn.
 46.8
 18.4
 25.6
 5.7
 6.5
 2.
5.1
3.3
2.
      Pb and Cr below detection.
                                  108

-------
                    ADHESIVE WASTE NO. 6
                   '	PROCEDURE C  A SYN. LEACH.
                   —- PROCEDURE R  «H90
                     pH
                     5T
                     4--
e
                    CONDUCTIVITY, /iMHOS/CM
                   400T
                   300-
                   200-
                   100--
                           ELUTIONS


Figure 53.  pH and specific conductance curves for Adhesive Waste #6,
          oL I •
                           109

-------
              ADHESIVE WASTE NO. 6
         No & K * CONCENTRATION  a RELEASE
         - PROCEDURE C     * SYNTHETIC  LEACHATE
    	 PROCEDURE R
   Na CONCENTRATION, ppr
   30-r
    20--
    10--
H20
  Na RELEASE,  Smg/kg
 60-r
                             40-
  20- •  •-•
     K CONCENTRATION, ppm
          I      2
           ELUTIONS
  K RELEASE,  Smg/kg

  60T         ^"'"
                              30-•


        I      2      3
          ELUTIONS
Figure 54.  Na and K concentration and release curves for Adhesive
          Waste #6, SLT.
                           110

-------
                ADHESIVE WASTE NO. 6
              PROCEDURE C
              PROCEDURE R
        H2°
    COD CONCENTRATION, ppm    COD  RELEASE, 2g/kg
 lOOOOO-r               /   400T
  75000--
  50 000--
  25 000- -
300"
200--
 100"
                  2      3
               ELUTJONS
             2      3
          ELUTIONS
Figure 55.  COD concentration and release curves for Adhesive Waste #6,
          SLT.                    . . .  ,
                            m

-------
 ADHESIVE  WASTE  NO. 6  TEST  COMPARISON
     pH, CONDUCTIVITY, Na= CONCENTRATION a RELEASE
        A SLT - S. L.
        O SLT - H20              V MINN- ACETATE BUFFER
        D IUCS- H20              V MINN - H 20
    pH                       CONDUCTIVITY,  /^MHOS/CM
  5.0-r
  4.5--
  4.0--
100-
                              50--
    Na CONCENTRATION, ppm
    3-r
            •2345
            ELUTIONS
 Na RELEASE, Zmg/kg
 GOT
                              40-
                              20--
           2345
          ELUTIONS
Figure 56   pH, specific conductance, and Na concentration and release
          curves for Adhesive Waste #6, test comparison.
                            112

-------
     ADHESIVE  WASTE NO.  6  TEST  COMPARISON
              K  a Zn'  CONCENTRATION  a RELEASE
         ASLT -S. L.
         OSLT - H20              v MINN - ACETATE BUFFER
         D IUCS - H20              V MINN - H20

       K CONCENTRATION, ppm        K  RELEASE, Smg/kg
      4-r                       80-
      Zn CONCENTRATION, ppm
      I.OT
     0.5--
               234
              ELUTIONS
 Zn RELEASE, 2mg/kg
20T
 10- •
         2345
        ELUTIONS
Figure 57.  K and Zn concentration and release curves for Adhesive
          Waste #6, test comparison,. ,
                           113

-------
Discussion

SLT—

     The waste released very high concentrations of COD.   The COD in  the
procedure C H?0 leachate in the third elution was over 100,000 mg/1.   The
total COD release in procedure R ^ leachates was 360,000 mg/1.   These
very high COD values show that a significant portion of the waste is
dissolved in the leaching test.  The low conductivity indicates that  non-
ionic species are being dissolved.  No metals of interest were leached.
Test Comparison—

     pH data for the
acidic components.
                         leachates indicate the slow release of slightly
                    No metals of interest were leached in any of the tests,
                                     114

-------
       TABLE 24.   PETROCHEMICAL INDUSTRY WATER-OIL SLUDGE:

                DESCRIPTION AND SUMMARY OF RESULTS

                      (Petrochemical  Sludge)


Waste Number 7, ECHO., Inc.


Description:

     A black, goopey sludge.
Analysis:

     ECHO, Inc.



     Wisconsin:
     Organics:

     Trace metals of
     interest:
flash point  > 150°F, Ash 0.20%, B.T.U.-
19,350 BTU/lb, Zn- 187 mg/1, Cu - 39.0 mg/1
Pb - 23.2 mg/1 , Cr - 2.38 mg/1 , Cd - 0.60 mg/1

Waste contains 3 fractions:  an oil  layer,
a water layer and solids.  Dry solids are
11% by weight.  Liquid, 42% H20 by volume;
58% oil by volume.   Solids are 51.3%
volatile.
Hexadecane
Cu, Pb, Zn
                   , napthalene
Sample Preparation:

     Sludge stirred vigorously prior to sampling.   Centrifuged to separate
solids.  Liquid layers after centrifuge were filtered separately but con-
tained no solids.
                                              (continued)
                                    115

-------
                 TABLE 24 (continued)
         Maximum Concentration and Release

Acid Leachates Na_
SLT Proc C, SL
SLT Proc R, SL
Minn
H£O Leachates
SLT Proc C 62
SLT Proc R 20.5
IUCS 144
Minn 4.2

Acid Leachates
SLT Proc. R, SL
Minn
H00 Leachates
2
SLT Proc R 327
IUCS 780
Minn 168
Concentration mg/1
K.- M£L . Zn, Pb Cu*
10 360 5.0 .73 b.d.
3.5 128 7,0 ,98 b.d.
2.9 22 1.5 .80 b.d,

4.9 53 .15 .25 b.d.
.4 17,2 0 .19 b.d.
2.3 26 0 0 b,d.
.2 4.7 0 .30 b,d.
Release mg/kg

•75 1770 173 24.3 b.d.
88 880 60 32 b.d.

6.2 279 0 1.9 b.d.
14.4 238 0 " 0 b.d.
6 188 0 12 b.d.
*Below detection limits.
                           116

-------
              PETROCHEMICAL SLUDGE

         PROCEDURE C     A SYNTHETIC LEACHATE
    	PROCEDURE R
H20

 CONDUCTIVITY, /iMHOS/CM
2000-r
                            1600--
                            1200-
                            800- -
                            400--
                                        "fcx--.-.-
               2
           ELUTIONS
        I      2      3
         ELUTIONS
Figure 58,  pH and specific conductance curves for Petrochemical
          Sludge, SLT,
                         117

-------
            PETROCHEMICAL  SLUDGE
        No  a K * CONCENTRATION a RELEASE
 	PROCEDURE C
 	PROCEDURE R
Na CONCENTRATION,ppm
80-r
60--
                                 & SYNTHETIC LEACHATE

                                 * H2°
                                Na RELEASE,  Smg/kg
                              400-r
                               300
                         200--
                          100-
                                          	e
                                  X
                                 X  X
K CONCENTRATION, ppm
        ELUTIONS
                                K RELEASE, 2mg/kg
                               LOOT
                          75--
                          50-
                          25-

                                      I      2
                                       ELUTIONS
Figure 59.
    Na and K concentration and release curves for Petrochemical
    Sludge, SLT.
                     118

-------
              PETROCHEMICAL  SLUDGE
           Mg a Zn«  CONCENTRATION a  RELEASE
          - PROCEDURE C         A SYNTHETIC LEACHATE
       	PROCEDURE  R
  © H20
      Mg CONCENTRATION, ppm     Mg RELEASE, 2mg/kg
    400-r                    2000 T
    300--
    200--
     100-
1500--
1000- •
500--
                                        X S
                                       X X
     Zn CONCENTRATION, ppm
     8 -r
 Zn RELEASE,  2mg/kg
200 T
                              150--
                              I50--
                              50--
                                              ,4'
            ELUTIONS
             2
         ELUTIONS
Figure 60.  Mg and Zn concentration aid release curves for Petrochemical
          Sludge, SLT.
                            119

-------
                PETROCHEMICAL SLUDGE
                 Pb  CONCENTRATION a RELEASE
       	PROCEDURE  C         © H20
       	PROCEDURE  R         A SYNTHETIC LEACHATE
       Pb CONCENTRATION, ppm
        I.O-r   •                     2°T
       0.5--
             DETECTION LIMIT
                           ^
                     2      3
                 ELUT10NS
  • I I* I I II— I I W »__ C_«—*^->« •«-• I ft.
  Pb RELEASE,Smg/kgxxx
                                    10--
            ELUTIONS
       COD CONCENTRATION,ppm
      400-r
      300--
      200--
       100--
              I       2      3
                 ELUTIONS
COD RELEASE,  2g/kg
4-r
                                3-
                                 2-
        /
        //
       //
            2      3
         ELUTIONS
Figure 61.  Pb and COD concentration and release curves for Petrochemical
          Sludge, SLT.
                              120

-------
  PETROCHEMICAL SLUDGE  TEST COMPARISON
  pH, CONDUCTIVITY, Na= CONCENTRATION a RELEASE
     ASLT - S.L
     OSLT - H20
     niucs- H2o
    VMINN- ACETATE BUFFER
    ¥M!NN- H20
 CONDUCTIVITY, /^MHOS/CM
1500-r
                         1000
                          500--
 Na CONCENTRATION, ppm

KX)T
 75-
 50--
 25--
  Na RELEASE, Zmg/kg
I600T
I200--
800--
400--
          2345
         ELUTIONS
           2345
          ELUTIONS
Figure 62.  pH, specific conductance, and Na concentration afid release
          curves for Petrochemical Sludge, test comparison.
                           121

-------
     PETROCHEMICAL SLUDGE  TEST  COMPARISON
           K  a Mg = CONCENTRATION a RELEASE
         ASLT- S.L.
         OSLT- H20
         DIUCS-H20

   K CONCENTRATION, ppm
                        VMINN- ACETATE BUFFER
                        VMINN- H20

                    K RELEASE, 2mg/kg
                    120-r
                              80--
                              40--
    Mg CONCENTRATION, ppm
   !60T
   120--
                    Mg RELEASE, Smg/kg
12345
  ELUTIONS
                   1500-1
                            1000-
                             500
                                          4-
                                    1234
                                       ELUTIONS
Figure 63.  K and Mg concentration and release curves for Petrochemical
          Sludge, test comparison.
                            122

-------
      PETROCHEMICAL SLUDGE  TEST  COMPARISONS
             Zn a Pb' CONCENTRATION a RELEASE
         ASLT- S.L.
         O SLT - H2O            V MINN - ACETATE  BUFFER
         DIUCS-H20           VMINN-H20
      Zn CONCENTRATION, ppm      Zn RELEASE, 2mg/kg
      12-r                      180-r
      8--
      4 - -
 V

HH—S-
                     ft
                     120--
                      60--  v
      Pb  CONCENTRATION, ppm
     1.5-r
     I.O--
     O.5--
              DETECJI_ON_
                LIMIT
H	1	1	1	1
 12345
   ELUTIONS
                      Pb RELEASE, Smg/kg
                      30--
                      15--
                                     o
                                     h
                                      I   2345
                                        ELUTIONS
Figure 64.  Zn and Pb concentration and release curves for Petrochemical
          Sludge, test comparison.
                             123

-------
I—
~

g
t-i

LU

5
en
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Hi
a.
UJ
tn
r.i o
ZD CD
_ i ct:
 O

 Q-:
 LU

 tr
 tv
                                                                           3
                                                                           to
                                                                           QJ


                                                                           t/5
                                                                               O
                                                                               to
                                                                               s~
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                                                                               X
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                                                                               OJ
                                                                               c
                                                                               (O
                                                                               X
                                                                               0)
                                                                                a>
                                                                               •a
                                                                                3
                                                                               OO
                                                                                (C
                                                                                O
                                                                               •r—


                                                                                
     (O   O
     p-•   i ^

     O   (O

     "~   o
 a)
 fO
                                                                                o
T3

 rtS
     to
 S-   rO
 O   O5
M-
     •a
•*   O)
I—   -p
     o
     3
     S-
     -a
^    c
 ca.   
          10
           S-
           3
           CO
                                         124

-------
        TABLE 25.  GRAIN PROCESSING LIPIDS AND FATS WASTE:

                DESCRIPTION AND SUMMARY OF RESULTS
Waste Number 8, ECHO. Inc.


Description:


Analysis:

      ECHO:



      Wisconsin:

      Organics:

      Trace Metals of
      Interest:


Sample Preparation:
Solid, hard fat
pH - 7.8, suspended solids - 18.75%, As.h-11.4%
Zn - 11.4 mg/1, Cu - 0.40 mg/1, Pb - .,01  mg/1,
Cr - 1.3 mg/1, Cd - 0.3 mg/1

52% volatile at T05°C for 24 hours

Not analyzed


Zn, Cr


Sampled directly
                                                      (continued)
                                   125

-------
                       TABLE 25 (continued)
                 Maximum Concentration and Release
Acid leachates
     SLT proc. C, SL
     SLT proc. R, SL
     Minn.
Concentration, mg/1

  Na        K        MS.


12.5
11.0
1.1
95.
28.
8.7
2.3
2.2
.74
.4
.4
.5
HpO leachat.es
SLT proc.
SLT proc.
IUCS
Minn.
C
R
6.2
2.9
24.5
1.4
4.5
7.1
1.5
.15
5.0
1.1
14.5
.4
0
0
0
0
0
0
0
                                                                 .2
 Acid leachates
      SLT proc.  R,  SL
      Minn.
                          Release, mg/kg
           137.
            44.
570.
348.
49.
30.
 9.
18.
 H«0 leachates
SLT proc.
IUCS
Minn.
R
60.
163.
56.
78.
11.9
6.
30.5
165.
15.
0
0
0
0
0
0
       *Cr below detection.
                                      126

-------
      pH
     8r
     7--
     6--
     5--
   GRAIN  PROCESSING  LIPIDS  a  FATS
• PROCEDURE C     ASYNTHETIC LEACHATE
 PROCEDURE  R    «H20
                     CONDUCTIVITY, »MHOS/CM
 r      ^_            1000-r
                     750--
                     500--
                     250--
                 2
            ELUTIONS
                            I      2
                               ELUTIONS
Figure 66.
 pH and specific conductance curves for Grain Processing
 Lipids and Fats, SLT.
                            127

-------
       GRAIN PROCESSING  LIPIDS a FATS
        Na & K «  CONCENTRATION a RELEASE
      	PROCEDURE C      * SYNTHETIC LEACH ATE
                           • H20
 	 PROCEDURE R
Na CONCENTRATION, 0ppm    Na RELEASE, 2mg/kg

6-r
  4-
   2--
                            60-r
                            40-
                            20--
                                       x
                                    x
                                   x
   K CONCENTRATION, ppm

   15-r
   10-
                          K RELEASE, Smg /kg
         I      2
           ELUTIONS
                            100-
                             50--
                                 I      2
                                   ELUTIONS
Figure 67.  Na and K concentration and release curves for Grain
          Processing Lipids and Fats, SLT.
                           128

-------
        GRAIN PROCESSING  LIP1DS a FATS
         Mg  a Zn ' CONCENTRATION a RELEASE
       	PROCEDURE C       SYNTHETIC LEACHATE
     	PROCEDURER

   Mg CONCENTRATION, ppm
   100-r
   75--
   50--
   25--
                        H20

                          Mg RELEASE, Smg/kg
                        800r
                        600--
                        400--
                        200--
                                   f	-r
Zn CONCENTRATION, ppm
3-r
         I      2
          ELUTiONS
                             Zn RELEASE,  Zmg/kg
                             75-r
                             50--
                             25--

                                     2
                                 ELUTIONS
Figure 68.  Mg and Zn concentration and release curves for Grain
          Processing Lipids and Fats, SLT.
                         129

-------
         GRAIN PROCESSING  LIPIDS  a  FATS
         	 PROCEDURE  C     ft H o
         	 PROCEDURE  R        2
       COD CONCENTRATION, ppm     COD RELEASE,
      3000T
      2000- -
      1000- -
              I       2      3
                  ELUTIONS
I5T
10+
 5--
      I       2
        ELUTIONS
Figure 69.  COD concentration and release curves  for Grain Processing
          Lipids and Fats, SLT.
                             130

-------
 GRAIN  PROCESSING LIPIDS  a FATS TEST COMPARISON
      pH, CONDUCTIVITY, Ncr CONCENTRATION a RELEASE
     pH
        A SIT- S.L.
        OSLT - H20
        DIUCS- H20
    10
    8-
           ^,
        ACETATE  BUFFER
        H20
VM1NN-
¥ MINN
CONDUCTIVITY, /iMHOS/CM
600T
400--
                             200--
    Na  CONCENTRATION, ppm      Na RELEASE, 2mg/kg
   40T                     4OOT
                            300--
                             200--
                             100--
                                   H	h
         12345
           ELUTIONS
       12345
          ELUTIONS
Figure 7Q.  pH, specific conductance, and Na concentration and release
          curves for Grain Processing Lipids and Fats, test comparison,
                            131

-------
GRAIN PROCESSING  LIPIDS a FATS  TEST COMPARISON
                K a Mg:  CONCENTRATION a RELEASE
           ASLT- S.L.
           O SLT - H20          V MINN - ACETATE BUFFER
           DIUCS-H20          VMINN-H20
       K  CONCENTRATION, ppm      K RELEASE, Smg/kg
       15 T                       150-r
       10"
        5--
                      100--
       Mg CONCENTRATION, ppm
       30-r
       20--
       10--
             12345
                 ELUTIONS
                       Mg RELEASE, Zmg/kg
                     600-r
                     400--
                     200--
                                2345
                                ELUTIONS
 Figure 71.
K and Mg concentration and release curves for Grain Process-
ing Lipids and Fats,  test comparison.
                             132

-------
 GRAIN PROCESSING LIPIDS a FATS TEST COMPARISON
                Zn a Pb' CONCENTRATION a RELEASE
         A SLT -  S. L.
         O SLT -  H20
         D IUCS- H20
        Zn  CONCENTRATION, ppm
                   V MINN - ACETATE BUFFER
                   V MINN-  H20
        3-r
        2 -
                      Zn RELEASE, Zmg/kg
                     60-r
                     40--
                    m
        Pb CONCENTRATION, ppm
        .0-r
      0.5--
                   DETECTION
                    LIMIT
12345
   ELUTIONS
                     Pb  RELEASE, Smg/kg
                           v


                      10+
                                        1234
                                            ELUTIONS
Figure 72.  Zn and Pb concentration and release curves for Grain Process-
          ing Lipids and Fats, test comparison.
                              133

-------
               TABLE 26.   FOOD INDUSTRY CLAY WASTE:
                DESCRIPTION AND SUMMARY OF RESULTS
Haste Number 9, ECHO. Inc.
Description:
Clay-like suspension in water
Analysis:

     ECHO:
     Wisconsin:

     Organ ics:
pH - 6.6, Ash < 1%, Zn - .011 mg/1 , Pb - .001  mg/1,
Cr - .02 mg/1, Cu - .001 mg/1, Cd - .003 mg/1

(solids) 37,1% volatile at 103°C

dodecane (C12H26), tridecane (C-,3H38),

tetradecane (CH)
     Metals of Interest:

Sample Preparation:
None

Solids settled; liquid decanted, centrifuged
and filtered.  Centrifuged, filtered solids
returned to those left behind in the decant-
ing and stirred thoroughly.  Sampled.
                                                          (continued)
                                     134

-------
       TABLE 26 (continued)
Maximum Concentration and Release
Concentration, mg/1: , , ,•
Acid

H20

Acid

H20

leachates
SLT proc. C, SL
SLT proc. R, SL
Mi nn .
leachates
SLT proc. C
SLT proc. R
IUCS
Minn.
leachates
SLT proc. R, SL
Minn.
leachates
SLT proc. R
IUCS
Minn.
Na. K_
12
6
2.

22 2.
5.7
15 4.
2
Release,

94
104

116 12
124 29
80 13
Mg_
27
22
6 57

7 9.0
8 2.8
6 5.1
3 .7
mg/kg

570
2280

41
49
29
Zn_
1.8
2.0
1.5

0
0
0
0

51
60

0
0
0
                                      Pb_

                                      .95
                                     3.8
                                     6.5
                                     0
                                     0
                                     0
                                     0
                                    56
                                   260
 COD
                                      0
                                      0
                                      0
 340
 190
 128
   4
3340
1800
 160
                 135

-------
                   FOOD WASTES,  CLAY
           PROCEDURE C    A SYNTHETIC LEACH ATE
     	PROCEDURE  R

       pH

      8-r
      7-
      6--
       5--
H2°
            I      2
              ELUTIONS
  CONDUCTIVITY, /zMHOS/CM
   800 T
                               600-
                               400--
                               200--
           I       2
            ELUTIONS
Figure 73.  pH and specific conductance curves for Food Wastes, Clay,
          SLT.
                            136

-------
        FOOD WASTE, CLAY
  Na, K, MQ « CONCENTRATION a RELEASE
  - PROCEDURE C
  --- PROCEDURE R
                              YNTHETIC LEACHATE
 Na CONCENTRATION, ppm
 30T
 20
 10--
 K CONCENTRATION, ppm
15 T
 10- •
  5--
  Mg CONCENTRATION, ppm
 30-r
 20--
 * H2°
 Na RELEASE, 2mg/kg
I50T
                         IOO--
                          50--
                           K RELEASE, 2mg/kg
                          150-
                         100-
                          50--
                             RELEASE, 2mg/kg
                         6OO-r
                        400
                          200--



                                             -I
       123            123
         ELUTIONS                 ELUTIONS
Figure 74.  Na, K, and Mg concentration and release curves for
          Food Wastes, Clay, SLT.
                        137

-------
              FOOD WASTES, CLAY
          Zn a Pb' CONCENTRATION  a RELEASE
   	PROCEDURE C      A SYNTHETIC LEACH ATE
   	PROCEDURE R      « H90
   Zn CONCENTRATION.ppm
  3 *"


 Zn RELEASE, Img/kg
60T
                           40
                            20--
   Pb CONCENTRATION, ppm
   £51~
   4* -
          \
        1      2      3
           ELUTIONS
 Pb RELEASE, Smg/kg
60r
40--
                            20--
             2     3
         ELUTIONS
Figure 75.  Zn and Pb concentration and release curves for Food
          Wastes, Clay, SLT.
                        138

-------
                FOOD  WASTES,  CLAY
               PROCEDURE C
         	PROCEDURE R
   COD CONCENTRATION, ppm ^* COD RELEASE, 2mg/kg
     300T
     200--
      100--
3000-r
2000--
 1000- -
            I       2     3
               ELUTIONS
        I       23
           ELUTIONS
Figure 76.  COD concentration and release curves for Food Wastes,
          Clay, SLT.
                           139

-------
   FOOD  INDUSTRY-CLAY WASTE  TEST  COMPARISON

     pH, CONDUCTIVITY,  Na = CONCENTRATION ft RELEASE

           A SLT - S.U
           OSLT-H20             V MINN-ACETATE  BUFFER
           DIUCS-HgO            VMINN-H20
       pH                       CONDUCTIVITY, ^MHOS / CM
                              I20C-T
8-r
      6--
                              800-•
                         400--
      Na CONCENTRATION, ppm
     20-r
      I5--
      10--
      6--
              2345
             ELUTIONS
                           Na RELEASE, 2mg/kg
                          160-r
                          I20--
                          80--
                          40 -
                                            H	H
                                   2345
                                  ELUTIONS
Figure 77.
    pH, specific conductance, and Na concentration and release
    curves for Food Wastes, Clay, test comparison.
                            HO

-------
  FOOD  INDUSTRY-CLAY  WASTE TEST COMPARISON
              K  a Mg-« CONCENTRATION S RELEASE
           A SLT - S.L.
           OSLT - H20         V MINN- ACETATE BUFFER
           DIUCS-H20         V MINN-H20
        K CONCENTRATION, ppm        K RELEASE, 2mg/kg
        61-4      H             I20r
                                80--
                                40-|-        n	0—*-P
       Mg CONCENTRATION, ppm
       60T
      40 -
      20--
            12345
               ELUTIONS
 Mg RELEASE, 2mg/kg
9bO-r
       i 2280
       v

600--
300- •
       1234
          ELUTIONS
Figure 78,  K and Mg concentration and release curves for Food Wastes,
          Clay, SLT.
                           141

-------
   FOOD INDUSTRY - CLAY WASTE  TEST  COMPARISON
           Zn, Pb a COD=  CONCENTRATION  a RELEASE
         A SLT - S.L.
         O SLT - H20             V MINN- ACETATE BUFFER

         DIUCS- H20
      Zn CONCENTRATION, ppm
      p
                       Zn RELEASE,  Smg/kg
                      60T  v
                               30-
                 m
       Pb CONCENTRATION, ppm    Pb RELEASE, Smg/kg
                              300 T
                                     S7
           V


                               150-
      COD  CONCENTRATION,ppm     COD RELEASE, ^P 2mg/kg
     200T  -                  3000-r
     IOO--
Figure 79.
                     1500--
                  -I	1	1
            1234
              ELUTIONS
                            I   2345
                              ELUTIONS
Zn, Pb, and COD concentration and release curves for Food
Wastes, Clay,  test comparison.
                            142

-------
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143

-------
    TABLE 27.  MARBLE WASH:  DESCRIPTION AND SUMMARY OF RESULTS
Haste Number 10. ECHQ^Jnc.
Description:
Analysis:
     ECHO:
     Wisconsin:
     Organics:
     Trace Metals of
     Interest:
Sample Preparation:
Suspension

Unavailable.

Tetradecane (C-,4H30), hexadecane
Octadecane  (C-igHog)-
Unavailable.
     Similar to food industry, clay waste.  Solids were allowed to
settle.  The liquid was decanted, centrifuged and filtered, and the
solids removed from the decanted liquid and mixed thoroughly with the
original solids.  The solids were then sampled directly.
                                                   (continued)
                                  144

-------
                        TABLE 27 (continued)
                  Maximum Concentration and Release
Acid leachates

   SLT proc. C, SL
   SLT proc. R, SL
   Minn.

FLO leachates

   SLT proc. C.
   SLT proc. R
   IUCS
   Minn.
                         Concentration, mg/1
             20.0
             10.0
              1.1
 24.0
  8.9
 22.5
  3.1
 4.4
 1.7
 3.9
 0.6
             Mg_

             109
              60
              77
21
10.0
  .47
 1,8
           Pb.

           .60
           .63
          3.5
0
0
0
0
                                                 COD
 142
 128
 116
  72
Acid leachates

   SLT proc.  R. SL
   Minn.

HpO leachates

   SLT proc.  R
   IUCS
   Minn.
127
301
124
                           Release, mg/kg
            196
             44
37
45
26
             1105
             3080
192
  6.4
 72
         16.6
        140
0
0
0
2230
1576
2880
                                    145

-------
                      MARBLE WASH
              -PROCEDURE C     A SYNTHETIC LEACHATE
              PROCEDURE  R
      pH
     8-r
     7-
     fi- •
 • H20
 CONDUCTIVITY, /iMHOS/ CM
300T
                              200--
                               100--
    No CONCENTRATION, ppm
    30T
    20-
     10--
           I      2
            ELUTIONS
  Na RELEASE, Smg/kg
 I50T
                               100- -
                                50--
                                             •4-
        I       2
          ELUTIONS
Figure 81.  pH, specific conductance, and Na concentration and release
          curves  for Marble Wash, SLT.
                             146

-------
                    MARBLE  WASTE
            K, Mg, Pb' CONCENTRATION a  RELEASE
           PROCEDURE C        A SYNTHETIC LEACHATE
                              e  H20
                                 K RELEASE, 2mg/kg
                               200T    .'  '   '   •  .-
                               IOO--
	PROCEDURE R
 K CONCENTRATION, ppm
20T
10--
      Mg CONCENTRATION, ppm
     150-r
     100--
     5O--
                           Mg RELEASE, Smg/kg
                         1500-r
                         1000--
                                        ---dt-—^^
 Pb CONCENTRATlON.ppm
I.O-r
                  2     3
              ELUTIONS
                                 Pb RELEASE, Smg/kg.
                                20
                                  ELUTIONS
Figure 82.  K, Mg,  and Pb concentration and release curves for Marble
          Wash, SLT.
                           147

-------
                       MARBLE WASH
         	 PROCEDURE C
         	 PROCEDURE R
       COD CONCENTRATION, ppm
       l5O-r
       100
       50-•
  ©H20

COD RELEASE, 2g/kg
                ELUTIONS
     I       2.     3
         ELUTIONS
Figure 83.  COD concentration and release curves for Marble Wash,  SLT.
                            148

-------
       MARBLE WASH  TEST COMPARISON
pH, CONDUCTIVITY, Na= CONCENTRATION 6 RELEASE
  pH
 10-r
 8--
 6 —
      A SLT-
      O SLT -
                    S.L.
                    H20
      D  IUCS- H20
V MINN - ACETATE BUFFER
VMINN- H20

 CONDUCTIVITY, ^MHOS/CM
 600-r
                               400-•
                               200--
 No CONCENTRATION, ppm
SOT-
      12345
        ELUTIONS
                                Na RELEASE, 2mg/kg
                               300-r
                         2OO--
                          100--
                                      12345
                                        ELUTIONS
Figure 84.
    pH, specific conductance, and Na concentration and release
    curves for Marble Wash, test comparison.
                     149

-------
          MARBLE WASH  TEST COMPARISON
            K & Mg: CONCENTRATION a RELEASE
          A SLT - S. L.
          O SLT - H20         V MINN - ACETATE BUFFER
          DIUCS - H20         T MINN - H20
     K CONCENTRATION, ppm      _A RELEASE, Smg/kg
     I2T
     8--
                    300-1
                    200-
                              100- •
     Mg  CONCENTRATION, ppm
    80T  „
    6O-
    40--
     20--
                     Mg RELEASE, 2mg/kg
                   4000-r
                   3OOO-
                   2000
                              1000--
             -
-------
              MARBLE  WASH  TEST  COMPARISON
             Pb a COD •  CONCENTRATION a RELEASE
             ASLT - S.L.
                                V MINN-ACETATE BUFFER
                                VMINN-H2O
                                Pb RELEASE, 2mg/kg
                               200-r
                         100- -
     OSLT -H20
     niucs-H2o
Pb CONCENTRATION.ppm
4-r
       2- -
               &
              -*	4
       COD CONCENTRATION.ppm    COD RELEASE, Smg/kg
      I50r                    3000r  _
      IOO--
      50--
            1234
               ELUTIONS
                       2000- -
                       1000- •
                               1234
                                  ELUTIONS
Figure 86.  Pb and COD concentration and release curves for Marble Wash,
          test comparison.
                            151

-------
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                                                   ED
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                                                              U-
                               152

-------
   TABLE  28.   COPPER OXIDE-SODIUM  SULFATE  SLUDGE  (CuO-Na2S04 WASTE)

                 DESCRIPTION  AND SUMMARY OF  RESULTS
 Waste  Number  11,  Chem-Trol
 Description:
Analysis:
   Chem-Trol:
Sample Preparation:
Generated by large chemical manufacturer.
Black, low viscosity liquid containing both
fine particulates and large (soft-ball size)
translucent crystals.  Large crystals had
apparently precipitated during shipment, as
analysis by Chem-Trol did not mention them.
Less than 5% solids, sp. gr. 1.28, pH 10.4, phenol
20 ppm, total carbon 200 ppm; total inorganic
carbon 50 ppm, Cu 9 ppm.
     Liquid decanted and filtered.  Solids returned to sample pail
These were stirred to get as homogeneous a sample as possible   A sub-

andPiL??P nSff ^V largS b!a?er' then the S"bsanPle ground in mortar
flltSSrf  aS il the.!;r9e crystals were broken up.  This mixture was
filtered, and the solid portion used for analysis.
                                                   (continued)
                                   153

-------
                         TABLE  28  (continued)
                 Maximum  Concentration  and  Release
                        Concentration, mg/1
Acid leachates      Na
                       t
   SLT proc. C, SL
   SLT proc. R, SL
   Minn.

HgO  leachates

   SLT proc. C     42000
   SLT proc. R      9740
   IUCS            23000
   Minn.            4970
                             K_

                            32.4
                             5.2
                             4.4
39
 4.30
24
 3.5
                  3281
                  1970
                   380
153
132
  6.4
 12
                 2916
                 3120
                 1450
 ZL

7.65
6.84
3.7
                                                0.57    .20
                                                0.38   0
                                                0.27    .12
                                                 .18   0
                                             Fe
                          120
                                              1.55
                                                .1
                                                .31
                                                .18
Acid leachates

    SLT  proc.  R, SL
    Minn
                         Release, mg/kg
         171      4.32xl04  1.04xl05 155
         185      1.53x104  7.42xl04 155
                                   5.1x10^
   O  leachates

   SLT proc. R
   IUCS
   Minn
2.20x10°  90       6734
1.70x105 140        104
2.07x105 150        616
                     6.9   .6
                     2.0   .7
                    13.6  2
                            3.8
                            2.2
                           18
      Note that the Na and  the  Cu  and  Mg  concentration and release
 test comparison curves were  presented earlier as Figures 4 and 1, respec-
 tively.
                                   154

-------
   pH
 H.OT
10.0
 9.0--
 8.0--
 7.0-
 6.0-•
 5.0-
COPPER  OXIDE- SODIUM SULFATE  SLUDGE
        A SYNTHETIC  LEACHATE  © H£0
 4.0
              .- A---A
          2345
         ELUTIONS
                       	PROCEDURE C
                       	PROCEDURE R
                         REDOX, mV
                       200
                       150-•
                       IOO--
                        50--
                         O--
                      + 50
                                 2345
                                 ELUTIONS
Figure 88.  pH and redox curves for CuO-Na^SO,, Sludge, SLT.
                        155

-------
 COPPER OXIDE-SODIUM SULFATE SLUDGE

         No  CONCENTRATION
      ppm    MOLAR
    50,000
    40,000-
    30,000-
                    PROCEDURE C
          ppm
     IO,000T
        500--
      5,000--
      2,500--
PROCEDURE R
                        2     3
                         ELUTiONS
Figure 89.  Na concentration curves for CuO-Na2S04 Sludge, SLT.
                        156

-------
  COPPER  OXIDE-SODIUM  SULFATE SLUDGE
         Nd CUMULATIVE RELEASE

     2g/kg  	PROCEDURE C
    225-r
    200--
    I75--
    I50--
     I25--
    100-
    75-
     50-
     15-
                •- PROCEDURE R
                          3     4
                      ELUTIONS
Figure 90.  Na release curves for CuO-Na2S04 Sludge, SLT.
                      157

-------
   COPPER OXIDE-SODIUM  SULFATE SLUDGE
             K  CONCENTRATION a  RELEASE
           A SYNTHETIC LEACH ATE  ® HgO
                    PROCEDURE  C
     CONCENTRATION, ppm
                    RELEASE, Smg/kg
                  150-r
                            125-
                            100 •-
                             75--
                   PROCEDURE  R
     CONCENTRATION, ppm
     4--
                             RELEASE, Zmg/kg
                             50--
             2345
             ELUTIONS
                            2345
                            ELUTIONS
Figure 91
K concentration and release curves for CuO-Na2$04 Sludge.
SLT.
                          158

-------
       COPPER OXIDE -  SODIUM SULFATE  SLUDGE
                Mg CONCENTRATION a  RELEASE
             A SYNTHETIC LEACHATE   © HgO
                      PROCEDURE C
      CONCENTRATION, pprn          RELEASE, Sg/kg
4OOO-r
    3000
    2000--
    IOOO--
                               40-r
                           30"
                           20--
                            10--
                      PROCEDURE R
      CONCENTRATION, ppm
    2500T
   2000--
    I50O--
    1000--
     500
                           RELEASE, 2g/kg
                           50-r
                            10
Figure 92.
        12345
          ELUTIONS
      Mg concentration and release curves for CuO-Na0SO,, Sludge.
      SLT.	                        2  4    y
                                        2345
                                       ELUTIONS
                          159

-------
    COPPER OXIDE - SODIUM SULFATE SLUDGE
           Cu  CONCENTRATION & RELEASE
            A SYNTHETIC  LEACHATE  »HgO
                   PROCEDURE  C
    CONCENTRATION,ppm        RELEASE, 2g/kg
3,000-r   -                60-
2,000--
 1,000--
40--
20--
                    PROCEDURE  R

   CONCENTRATION, ppm         RELEASE, 2g/kg
                         125 T
                         100-
          I   2345
            ELUTIONS
          2345
          ELUTIONS
 Figure 93.  Cu concentration and release curves for CuO-Na2$04
          Sludge, SLT.
                        160

-------
    CuO-Nd2S04  SLUDGE' TEST COMPARISON

               A SLT - S.L.
               V MINN- ACETATE

              •* MINN-H20BUFFER
D IUCS-H20    A REAL LEACHATE
               O SLT- H20
                      2      3     A . .
                         ELUTIONS
Figure 94.  pH curves  for CuO-Na2S04 Sludge, test comparison.
                        161

-------
          CuO-Na2S04 SLUDGD TEST  COMPARISON
        ASLT-s L
                       niucs- H2o
                       VMINN- ACETATE BUFFER
Zn CONCENTRATION,ppm      Zn RELEASE, 2mg/kg
8-r                      200-r
        OSLT-H20
              2345
              ELUTIONS
                               150-
                               100-
                               50--
                                    2345
                                    ELUTIONS
    K CONCENTRATION, ppm
    30-r
              2345
              ELUTIONS
                           K RELEASE, 2mg/kg
                         300 r
                              200--
                               100
                                               -\	1
                                   234
                                   ELUTIONS
Figure 95.  Zn and K concentration and release curves for CuO-Na2S04
          Sludge, test comparison.
                            162

-------
 Discussion
 SLT—

     This was  the most  interesting and  informative of the wastes.
 si on of  each parameter  of  interest will  be done separately.
Discus-
      pH—Distilled water  leachates show that the waste is basic, buffer-
 ing  solutions at a pH between 9.9 and 10.7.  SL procedure C leachates
 show the strong basic nature of the waste.  By the fourth elution, the
 pH in the SL leachate was equal to that in the t^O leachates.  Procedure
 R SL samples show that the basic salt is removed by the third elution.
     Na— The Na concentration curves in the procedure C and R ^0 leach-
ates are characteristic of a .very soluble parameter.  Na concentration
in the procedure C f^O leachate rises and is almost a straight line,
reaching over 40,000 mg/1 (almost 2M) by the fourth elution.  Procedure R
curves show a first elution maximum with much lower values thereafter.
There is no hint of a concentration plateau in the procedure C leachates,
so even after four elutions the maximum concentration cannot be estimated
from the procedure C data.
     K--K curves are interesting in that they are similar to the Na curves
but at much lower concentrations.  Whereas the Na concentration in the
first elution leachates is about 10,000 mg/1, K concentration is only
5 mg/1.


     Cu--Cu leaching curves show the effect pH can have on the release
of trace metals.  In the first elution, Cu concentration in SL leachates
was approximately 3,000 mg/1, while in the H20 leachates, it was only
0.5 mg/1.  Procedure R SL samples continue to extract high concentrations
of Cu until all available Cu is extracted, while the distilled water
leachates1 Cu concentrations remain near the detection limit.  After
five elutions, SL leachates had extracted v ver 100 g/kg Cu, while the
H20 leachates extracted only 3 mg/kg.   The major reason for the
different leaching behavior of the SL  and H20 leachates is explained
by a pH versus Cu concentration phase  diagram, as shown in Figure 96.
Cu solubility increases rapidly with decreasing pH below pH 9.   From the
diagram, one would expect a Cu concentration in solution at pH 4.5 to
be about four orders of magnitude (10,000 times) higher than the concen-
tration at pH 10.4, assuming no complexing agents are present other than
hydroxide.  Also plotted in Figure 96  are the Cu concentrations found in
the test leachates.  The points are generally close to the CuO-Cu++ lines,
                                   163

-------
                                                A SLT, SL, PROC R
                                                O SLT, H O, PROC R
                                                O IUCS, H O
                                                ^ MINN, ACET.
                                                V MINN, H O
                                                ARLT
Figure 96.  pH vs. Cu  concentration solubility diagram for Cu  and  CuO
            system.
            (Cu concentrations in leachates from CuO-Na2$04  Sludge,  using
            various  leaching tests are also plotted.)
*Detection limit  using Atomic Absorption spectrometer.
                                    164

-------
 indicating that pH is probably th.e major controlling factor for Cu concen-
 tration.  The seemingly oversaturated conditions found in th.e SL and real
 leachates samples probably show the effect of complexing in solubilizing  Cu.

      Falling Cu concentrations in procedure C SL samples indicate that
 Cu is being lost from solution in each elution after the first.   The
 rising pH of these leachates explains the loss of Cu from solution.
 Apparently, however, the strong complexing capacity of SL maintains  Cu
 concentrations well  above that predicted from pH considerations  alone.
      Mg—The procedure C SL Mg curve also  shows  a  pH  effect, with a fall in
 Mg concentration as the pH rises.   The procedure R SL curve  shows almost
 complete extraction of Teachable Mg on the first elution  with  low con-
 centrations  thereafter.   Mg concentrations in  first elution  SL samples
 in procedures C and R do not duplicate well.   Concentrations range from
 750 to 2500  mg/1  in the three replicates.   This  range is  far beyond usual
 Mg deviations (~10% standard deviation).   Whether  the lack of  duplication
 was caused by subsampling differences or by changes in the SL  causing
 changes in the Mg concentration is  unknown.

      There is an interesting rise  in Mg concentration in  1^0 leachates
 in both procedures C and R samples  to around 100 mg/1.  Why Mg should
 elute in later elutions  and not in  the initial elutions is not known.
      Summary—The waste  is a mixture of basic salts of Cu, Mg, and Na,  Cu and
 Mg  are  leached  in high concentrations  by acid media, but not by HgO
 leachates.   In  the acid  environment of a municipal landfill, this waste
 would probably  release .significant amounts of Cu to the surrounding
 environment.  This release is foreseen in the acid media but is completely
 missed  by the H20 leachates.  The differences in the Cu concentrations
 are so  large that one could not predict the Cu concentrations possible
 under acid conditions,from the ^0 leachates alone.  The HeQ.leachates,
 on  the  other hand, show  that the waste will not leach high concentrations
 of  Cu unless subjected,to acid or strongly complexing conditions.  Both
 acid  and HgO leachates are needed to obtain a clear picture of the leach-
 ing characteristics of the waste.           	

      The high releases from the waste  indicate that most of the waste is
 dissolving in the acid leachates.  Assuming that Na is present in the
 waste as Na2S04 and is leached equally well under H20 and acid conditions,
 and that Cu and Mg are present as CuO and MgS04, respectively, the per-
•centage of waste dissolved can be calculated from the release figures.
 For SL  samples, the calculated percentages are around 100% (98.4% for one
 duplicate, 105.3% for the other).  Whether or not the assumptions regard-
 ing  the waste composition are correct, it is obvious from the calculations
 that a  urge portion of the waste is dissolved in SL.
                                     165

-------
     It would be surprising if large quantities of this waste were
actually landfilled.  With large amounts of Cu easily extractable
from the waste, it is a prime candidate for Cu recovery.
Test Comparison —

     The test comparison data show the same general trends as the SLT
data discussed previously, namely, high Na release in H20 leachates
and high Mg and Cu releases in acid leachates.

     There is an interesting difference between the Na release patterns
in the IUCS and SLT procedure R ^0 leachates (Figure 4).  Na concentra-
tion in the SLT procedure R h^O leachate drops from an initial high
(10,000 mg/1) in the first elution to steady values of around 1000 mg/1
in subsequent elutions.  The IUCS leachate Na concentrations, on the
other hand, fell steadily for four elutions.  When transformed into
release, these concentrations and the different solid-liquid ratios
indicate a release in the first elution of the SLT comparable to the
cumulative release attained with the IUCS test after five elutions,
both on a grams Na released per kg waste basis.  In other words, the
SLT leached in one day more than the IUCS test leached in 10 days.
Further, the SLT continued to leach more Na in three of the four elu-
tions performed beyond the first; whereas the IUCS leached very little
additional Na in the third, fourth, or- fifth elutions.  The test
results indicate that the. Na is present as a very  soluble and rapidly
leached salt (probably NagStty, given the name of the waste).  One pos-
sible explanation of the slower release of Na in the IUCS test is that
the agitation procedure in the IUCS test does not  mix the waste and
leachate as thoroughly as the agitation procedure  in the SLT, thus
delaying release of the Na.  In the IUCS test, the waste lies on the
bottom of the flask while the leachate is sloshed  back and forth on
top of the waste.  The SLT agitation procedure gently tumbles the waste
as the flask is turned through a verticle circle.  Anyone who has tried
to dissolve a large amount of salt in  a volumetric flask can attest to
the fact that just swirling the flask  is not as effective at dissolving
the salt as tilting it back and forth.  The same situation may be pre-
sent here.

     Cu concentrations in the RLT demonstrated that municipal landfill
leachate was able to solubilize significant amounts of Cu.  The concen-
trations in the  RLT leachates were not as high as  those  in the acid
leachates, but the pH  of the RLT  leachates was higher than that in the
acid leachates.  The very large difference  in Cu concentrations between
 acid and  H?0  leachates observed  in the SLT  was also  seen  in  the other
test leachates.  The acetate buffer contained very high  concentrations
of Cu  (-1500 mg/1), while h^O leachates were  less  than 0.5 mg/1.
                                   166

-------
             TABLE 29.  ELECTROPLATING SLUDGE (EPS):

                DESCRIPTION AND SUMMARY OF RESULTS
Waste Number 12, Obtained Locally
Description:

     Two jars of the sludge were obtained.  One had red spots on the
outside, the other was black.  Both had very little free liquid.  Sludge
was not homogeneous, but rather had pockets of a clay-like material  dis-
tributed throughout.
Analysis:

     pH (of free liquid) 8.40; 72% volatile at 105°C for 24 hours.


Sample Preparation:

     Liquid removed by filtration through a Whattman 42 filter, then
through a 0.45 micron filter.  Sample homogenized by gentle grinding
with mortar and pestle.
                                                  (continued)
                                  167

-------
                       TABLE  29  (continued)
                Maximum Concentration and Release
Concentration, mg/1
Acid leachates
SLT proc. C, SL
SLT proc. R, SL
Minn.
H20 leachates
SLT proc. C
SLT proc. R
IUCS
Minn.
Na,


167
79
92
29.8
K.
69.9
42.3
21.5

43.3
16.6
22
6.3
Mg_
532
343
125

190
83.4
28
8.3
Zn_
45
160
210

0
0
0
0
£4.
7,50
19.9
7.4

0
0
0
0
Acid leachates
                          Release mg/kg
SLT proc. R, SL
Minn.
tLO leachates
SLT proc. R
IUCS
Minn.


1081
593
1420
914
1014

251
160
336
6542
5400

1428
346
508
6570
9540

0
0
0
943
344

0
0
0
                                    168

-------
         ELECTROPLATING  SLUDGE
                pH a CONDUCTIVITY
           SYNTHETIC LEACHATE
	—PROCEDUREC
	-PROCEDURE R
-'•—PROCEDURE R,  'B1
                        'A1   CONDUCTIVITY, ju.MHOS /CM x I03
                            3.0T
        23456
        ELUTIONS
                             2.0-•
                             1.0- •
                                     2      3
                                 ELUTIONS
Figure 97.  pH and specific conductance curves for Electroplating
          Sludge, SLT.
                           169

-------
         ELECTROPLATING  SLUDGE
          Ma a  K «  CONCENTRATION & RELEASE
                   ] *
  	PROCEDURE R,  'B1

Na CONCENTRATION, ppm
200-r
 150-
 100-
  50--



           I
     K CONCENTRATION, ppm
     80-r
  60-
     40- -   ^
  20--
           23456
             ELUT10NS
                                 *
                                 ® M2U
                                Na RELEASE, 2g/kg
                               4-r
                             2-
                            K RELEASE,2g/kg

                                     /
                                        2345
                                          ELUTIONS
Figure 98.
       Na and K concentration and-release curves for Electroplating
       Sludge, SLT.
                         170

-------
             ELECTROPLATING SLUDGE
          Mg a  Ziv CONCENTRATION a RELEASE
   	PROCEDURE C] , ,
   	PROCEDURE RJ A
   	PROCEDURE R, 'B1

 Mg CONCENTRATION, ppm
750-r
  500- •
250-f
                                SYNTHETIC LEACHATE
                                H20
                               Mg RELEASE,  2g/kg
                              7.5-r
                           5.0
                             2.5-1-
                                     v
   - Zn CONCENTRATION, ppm
                             Zn RELEASE,  2g/kg
C.W
150-
100-
5O-
«-
6-
f'' ^ 4-
/ ^A
/ S"-^-*"'
' & / 2"
	 	 $ 	 f==$_ 	 fe A A
1
/^ /
	 »"'' 1 	 1 	 1 	 1 J
         I   23456
             ELUTIONS
                                    23456
                                     ELUTIONS
Figure 99.  Mg and Zn concentration  and release curves for Electro-
          plating Sludge, SLT.
                          171

-------
               ELECTROPLATING  SLUDGE
           Pb a Cd» CONCENTRATION  a RELEASE
                      C
                       R
                          'A1
     	PROCEDURE R,  'B1

    Pb CONCENTRATION, ppm
    1.5-r
    I.O--
   0.5--
         DETECTION LIMIT
    A SYNTHETIC  LEACHATE
    ® H20

  Pb RELEASE.Smg/kg
 75-r
 50-
 25-
                                       _l	1	1	1	1
     Cd CONCENTRATION,ppm
    20-r
     15-
    10-
   Cd RELEASE,  2g/kg
  1.0-r
0.75-
 O.5--
                             0.25--
                                                /

       4	H
                                              1 — 1
          I   23456
               ELUTIONS
           23456
            ELUTIONS
Figure 100.  Pb and Cd concentration and release curves for Electro-
           plating Sludge, SLT.
                          172

-------
          ELECTROPLATING SLUDGE A' TEST COMPARISON
                                   A SLT-S.L.
                                   o SLT-H20

                                   D IUCS-H20

                                   V MINN - ACETATE BUFFER
                                   T MINN - H20

                                   A REAL  LEACHATE
        Na CONCENTRATION, ppm      Na RELEASE, Smg/kg
      IOOT                       1600-r
                                 I2OO- -
                                 800--
                                 400- •
             12345
                ELUTIONS
                                               -I	\	1
1234
   ELUTIONS
Figure 101.  pH and Na concentration and release curves for Electro-
           plating Sludge, test comparison.
                            173

-------
ELECTROPLATING  SLUDGE A' TEST COMPARISON
        K a  Mg '  CONCENTRATION a RELEASE
      A SLT - S L.            V MINN - ACETATE BUFFER
      O SLT- H20            * MINN-H20
      D IUCS-H20            A REAL LEACHATE
  K CONCENTRATION, ppm        K RELEASE, 2mg/kg
40-
30-
 20--
 10--
                         1600-
                         1200-
                          800--
                          400-
      -A-
 Mg  CONCENTRATION,ppm
400-r
300-
200--
 100--
                  Mg RELEASE, 2mg/ kg
           2345
           ELUTIONS
                          234
                          ELUTIONS
Figure 102.
K and Mg concentration and release curves for Electro-
plating Sludge, test comparison.

                174

-------
                             V MINN- H20
                             V MINN-ACETATE BUFFER
 ELECTROPLATING SLUDGE  A = TEST  COMPARISON
       Zn a Cd = CONCENTRATION a RELEASE
      ASLT- S.L.
      O SLT - HO
      D IUCS - H20            A REAL LEACHATE
  Zn CONCENTRATION, ppm      Zn RELEASE,   2g/kg
200-r  X                    12-r
 100--
  0--
-100
                4—4-
  Cd CONCENTRATION, ppm       Cd RELEASE, Smg/kg
 20-r                  ^  IOOOT
 15--
  10--
  5--
          a
      12345
          ELUTIONS
                          750
                          500- •
                          250- •
                                 I   23456
                                     ELUTIONS
 Figure 103.  Zn and Cd concentration and release curves for Electro-
           plating Sludge, test comparison.
                           175

-------
Discussion

     Two samples of the sludge (A and B) were used.   At testing time it
was not knowK whether the samples were duplicates  so both were run using
procedure R.  Sample A was run with procedure C.   Later it was determined
that the samples were duplicates.

     The sludge is a very strongly buffered neutral  sludge   Six elutions
with SL in procedure R were required to return the PH of the leachate to
below 5.0, indicating very strong neutralizing power.  However, thegO
leachates maintained a PH of just over 8.0, indicating a strongly buffered
neutral waste, rather than a strongly basic waste.

     As with the CuO-Na2S04 sludge, the effects of pH on the release of
several trace metals can be seen, although the pH range with electro-
plating sludge is not as great.  Zn, Pb, and Cd show pH effects.  The
concentration! of these metals drop.in  the procedure C SL leachates as
the  pH  rises.  The concentrations rise  in similar patterns for all three
metals  in  the procedure R SL  leachates   The PH of the Procedure R SL
leachates  steadily falls from an initial value of 7.0.™  thej^rs*f"   .
tion to 5  in the sixth elution.  These  results emphasize, again, the need
for  an  acid leachate to model the acid  conditions likely  to be found in
municipal  landfills.

     Cd release  is  particularly  interesting  In that  it.reaches quite high
 concentrations  (20  mg/1)  in  one  duplicate while  remaining below.detection
 in the  other   The  two samples were a different  color  when  received,
  Sdicat?ng at  least some difference between  them.   Leachate redox  values
  showed that the waste was  a very strong reducing agent,  much stronger
 than the SL.   A possible explanation for the different Cd release  behavior
 was that one sample had become much more oxidized than the other during
 shipping and sample pretreatment,  which also gave rise to the different
 co Srs"9and that this oxidation  difference affected the Cd please in  some
 way.  Other explanations are also possible.   The difference in Jd release
 shows the need for strict control  of sample treatment prior to the test,
 the need for duplicates, and the need for cautious interpretation of test
 results.
                                     176

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          TABLE 30.  WASTEWATER TREATMENT SLUDGE (WTS):

                DESCRIPTION AND SUMMARY OF RESULTS
Haste Number 13, Chem-Trol
Description:

     A suspension from a typical  industrial  wastewater treatment plant
employing coagulation/precipitation and lime softening.   It will  consist
of various heavy metals and other metals precipitated as hydroxides,
chelated, chemisorbed, or otherwise "fixed"  in the sludge.
Analysis:

     CHEM-TROL:



     Wisconsin:

     Solids:
Fe 11%, Cu 2.9%, Cr 0.6%, Zn 1.3% (% of dry weight),
pH 11.0, sp. gr. 3.4, approximately 80% water,
high viscosity.

pH of liquid 12.57, redox -45 mV vs S.C.E.

51.2% volatile at 105°C for 24 hours
79% volatile at 600°C
Sample Preparation:

     Liquid decanted, filtered, solids from filtered liquid returned to
settled solids and mixed.   Solids then refiltered.
                                   177

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                      TABLE 30  (continued)
               Maximum  Concentration and  Release
                               Concentrati on, mg/1
Acid leachates
  SLT procedure C, SL
  SLT procedure R, SL
  Minn.
Real leachate
 H20  leachates
   SLT procedure  C
   SLT procedure  R
   Minn.
                                                       Zn
Cu
 Acid leachates
   SLT procedure R, SL
   Minn.
 Real leachate
   O leachates
   SLT  procedure  R
   Minn.



480
3200
1425
95
Release,
Na_

5000
26100
3800
190
40
15

146
29
4
mg/kg
K.
923
600

334
160
1.4
250
78
loss from
solution
0
0
0

Mg_
5670
3120
loss from
solution
0
0
2.0
18.5
9.2
loss from
solution
1.0
0.9
0

Zn_
464
368
loss from
solution
23
0
156
292
69
30
6.8
3.5
0.2

Cu.
5820
2760
640
55

                                    178

-------
            ® COINCIDENT VALUES
                             PROCEDURE  C

                             PROCEDURE  R
     WASTEWATER  TREATMENT SLUDGE

                 A SYNTHETIC  LEACHATE

             1    ©HgO
             I2.0--
11,0--
             10.0-
             9.0--
             8.0--
             7.0--
             6.0-•
             5,0--
              4.0
         \\
         I

          \
          \\
           \\
           \\
            \\
                    12345

                      ELUTIONS
Figure 104.  pH curve fpr Wastewater Treatment Sludge,  SLT.
                        179

-------
    WASTEWATER TREATMENT  SLUDGE
        No  CONCENTRATION a RELEASE
                   PROCEDURE C
   CONCENTRATION, ppm
4,000j
                   RELEASE, 2g/kg
                 20-r
                             15-
                             10
                    PROCEDURE R
    CONCENTRATION, ppm
 I,500T
 1,000-
   500--
                     RELEASE, 2g/kg
                  30 T
             2345
              EUJTIONS
                         12345
                            ELUTIONS
Figure 105.
Na concentration and release curves for Wastewater
Treatment Sludge, SLT.
                        180

-------
    WASTE WATER  TREATMENT SLUDGE
            K  CONCENTRATION  a RELEASE
               & SYNTHETIC LEACHATE  © HgO
                      PROCEDURE C
      CONCENTRATION, ppm          RELEASE.Smg/kg
200-r
    I50--
    IOO--
     50--
                             1500-r
                         1000--
                          500
                          250--
                       PROCEDURE R
      CONCENTRATION, ppm
     40T
              2345
              ELUTIONS
                            RELEASE, Smg/kg
                         lOOOr
                             750 --
                             500--
                             25O--
                                 I   2345
                                    ELUTIONS
Figure 106.
       K concentration and release curves for'Wastewater Treat-
       ment Sludge, SLT.
                          181

-------
         WASTEWATER TREATMENT SLUDGE

                Zn CONCENTRATION a RELEASE
                A SYNTHETIC  LEACHATE ®H?0
                        PROCEDURE  C
  2.0
    CONCENTRATION, ppm
  RELEASE, 2mg/kg
 20-r
                             15 -
                             10--
                              5--
                      PROCEDURE  R

    CONCENTRATION, ppm         RELEASE, 2mg/kg
   25-r
   20--
   15--
   10-
    5--
500-r
400--
300--
200--
 100- •
         12345
            ELUTIONS
       1234
          ELUTIONS
Figure 107.  Zn concentration and release curves for Wastewater
           Treatment Sludge, SLT.
                         182

-------
         WASTEWATER  TREATMENT SLUDGE

             Mg CONCENTRATION  a RELEASE
                   A SYNTHETIC LEACHATE  ©HoO
                         PROCEDURE C
        CONCENTRATION, ppm
      2.0T
       I.5--
       1.0--
      0.5--
                        RELEASE, Smg/kg
                      20 T
                       5--
                        PROCEDURE R
       CONCENTRATION, ppm
     400 T
     3OO--
     200--
      100- •
               2345
               ELUT10NS
                        RELEASE, 2g/kg
                       O - r.
                            1234
                              ELUTIONS
Figure 108.
Mg concentration and release .curves for Wastewater Treat-
ment Sludge,  SLT.
                           183

-------
           WASTEWATER TREATMENT  SLUDGE
             Cu CONCENTRATION 8. RELEASE
               A SYNTHETIC LEACHATE • HgO
                      PROCEDURE  C
      CONCENTRATION, ppm           RELEASE, 2g/kg

   200-r
     150-
     100-
     50-
                        PROCEDURE R
       CONCENTRATION, ppm
     300-r
     EOO--
     100--
Figure 109.
            12345
              ELUTIONS
                      RELEASE, 2g/kg
                     7.5 T
                     5,0--
                                2.5--
                           12345
                              ELUTIONS
Cu concentration and release curves for Wastewater Treat-
ment Sludge, SLT.
                            184

-------
         WASTEWATER TREATMENT SLUDGE
         —	 PROCEDURE C
         	PROCEDURE R
        COD CONCENTRATION,  ppm
       6000T
      4000--
       2000--
               I   2345
                  ELUTIONS
  ®H20

 COD RELEASE,  2g/kg
30-
20--
 10--
                                                 -®
      12345
        ELUTIONS
Figure 110.  COD concentration and release curves for Wastewater Treat-
          ment Sludge, SLT.
                           185

-------
     WASTEWATER TREATMENT SLUDGE' TEST  COMPARISON
                                   A SLT - S.L.
                                   O SLT - H20
                                   D IUCS- H20
                                   V MINN- ACETATE BUFFER
                                   V MINN- H20
                                   A REAL LEACHATE
       No CONCENTRATION, ppm
      I500T
      1000- -
       500--
              12345
                 ELUTIONS
No RELEASE,  Zg/kg
30T
                                   20-
                                    10--

          2345
          ELUTIONS
Figure 111.  pH and Na concentration and release curves for Wastewater
           Treatment Sludge, test comparison.
                             186

-------
WASTEWATER TREATMENT SLUDGE' TEST  COMPARISON
         K 8 Mg« CONCENTRATION a RELEASE
         ?MINN-H20                ASLT-  S. L.
         VMINN-ACETATE BUFFER      OSLT-  H  0
       K CONCENTRATION.ppm
      40-r
      30--
      20--
       10-
     Mg CONCENTRATION, ppm
    40O-r
     300--
     200- •
     100--
              2345
              ELUTIONS
                     K RELEASE, 2mg/kg
                    1000 T
                               750-•
                              500-
                               250-
                      Mg RELEASE, 2g/kg
                      8-r
                             234
                             ELUTIONS
Figure 112.
K and Mg concentration and release curves for Wastewater
Treatment Sludge, test compariso.n.
                           187

-------
  WASTEWATER TREATMENT SLUDGE* TEST COMPARISON
             Cu a  Zn *  CONCENTRATION & RELASE
       VMINN-H20
       V MINN-ACETATE  BUFFER
   Cu CONCENTRATION, ppm
   300-r
   20O--
   100--
                              A SLT - S . L .
                              O SLT- H20
                           Cu RELEASE,
                           6-r
                                4-
                                2-
 Zn CONCENTRATION, ppm
20-r
     10-•
           12345
              ELUTIONS
                               Zn  RELEASE,  2mg/kg
                              800T
                              400--
                                 12345
                                    ELUTIONS
Figure 113.  Cu and Zn concentration and release curves for Wastewater
           Treatment Sludge, test comparison.
                             188

-------
 Discussion

      Wastewater treatment sludge is a strongly basic waste,  raising the pH
     hVlrfi?L el"?1on t°.around 1K   The PH of subsequent  procedure  R SL
 leachates fell  until  reaching below 5.0 in the fifth elution.   The  H?0
 leachates maintain pH values  of 12.0 to 12.5.  Cu,  Mg,  and Zn  have  par-
 ticularly interesting release curves,  primarily due to  the apparent
 effect of pH on their solubility.   The Cu  concentration in procedure C
 SL leachates reaches  a maximum (200 mg/1 )  in  the first  elution  and  falls
 steadily thereafter.   The pH  of the second through  fourth  and  last  elution
 leachates is relatively constant,  so the observed drop  in  Cu concentration
 during these elutions must be due  to removal  of Cu  by the  fresh waste
 rather than  simply precipitation  due to the high pH.  Since  the Cu  con-
 centrations  are well  above those  expected  on  the basis  of  pH considerations
 (see  Figure  96),  it is apparent that complexing is  instrumental in  maintain-
 ing the high Cu concentrations.  Adding fresh waste  may either decrease the
 complexer concentration  in solution,  replace  the Cu  in  the complex  with
 another metal,  or add a species to the system which  can extract the Cu
 from  the  complex  and  precipitate  it.   Hrocedure  R SL  leachates have  a Cu
 maximum in the  second elution,  with  falling concentrations thereafter.
 Possibly  during the first  two  elutions  the Cu concentration  is controlled
 by pH,  while after  the  second  elution  most of the extractable Cu has been
 leached.  Note  that as with both CuO - Na2S04  sludge and electroplating  sludge
 the Cu  concentrations  in the  H20 leachates are  very low and  give no  indica-
 tion  of the  Cu  leaching potential  under acid  conditions.
Test Comparison —

     Minn., SLT, and RLT tests were run on the waste.  Cu concentrations
in the RLT leachates are lower than those in the acid leachates, but are
much higher than those in the H20 leachates.  The same pattern was found
in the CuO-Na2S04 tests, and the same comments apply.

     pH values in the Minn,  acetate buffer leachates  showed that the
greater buffering capacity of the acetate buffer compared to SL and the
lower solid to liquid ratio  in the Minn,  test compared with the SLT
compensate for the strongly  basic nature  of the waste.
                                     189

-------
              TABLE 31.   PAPERMILL SLUDGE  (PMS-EPA):

                DESCRIPTION AND SUMMARY OF RESULTS
Waste Number 14. CHEM-TROL
Descri pti on:

     31% clay slurry with the following characteristics:  bi-layered
liquid, 20% top layer, cloudy while low-viscosity aqueous suspension;
80% bottom layer, opaque, off-white sludge.
Analysis:

     CHEM-TROL:
pH 7-8, sp. gr. 1.28;
solids—total carbon 45 ppm, total  inorganic
carbon 15 ppm
 Sample Preparation:

      Mixture stirred  to  obtain  a  uniform  suspension,
 centrifuged to obtain solids.
                                  A subsample was
                                   190

-------
                        TABLE 31  (continued)
                 Maximum Concentration and Release
Acid leachates

  SLT procedure C, SL
  SLT procedure R, SL


H20 leachates

  SLT procedure C
  SLT procedure R
Acid leachate

  SLT procedure R


H20 leachate

  SLT procedure R
                            Na
                          430
                          450
                                      Concentration,  mg/1
K.
12
5.3
1.5
0.9

Ba
73
58
0.25
0.2
Release,
•~* *
Fe


0.6
0.5
mg/kg
In
2.43
0.6
0
0

                                                                 2.65
                                                                 0.85
                                         0
                                         0
   Na      K      Mg_      Fe      Zn      Cu_

          121   1225            18.3    15
13850
                                  23
8     13.6    0
                                191

-------
          PAPER MILL SLUDGE, EPA

            pH
          8.0-r
          7.0-
          6.0--
          5.0--
           4.0
	 PROCEDURE C
	 PROCEDURE R
  A  SYN. LEACH ATE.
                 12345
                    ELUTIONS
Figure 114.  pH curve for Papermill  Sludge, EPA, SLT.
                        192

-------
                 PAPER MILL  SLUDGE, EPA

                a K'  CONCENTRATION a  RELEASE
            PROCEDURE C  	   A SYN. LEACHATE
            PROCEDURE R	   ® H^O
     K CONCENTRATION, ppm
      20 T
      15--
      10--
       5--  V

                     K RELEASE, 2mg/kg
                    200 T
                     150--
                     100-•
                     50-
                     H	1
                                       /s
     Mg CONCENTRATION, ppm
     75-
     50--
     25--
Figure 115.
              2345
              ELUTIONS
                      Mg RELEASE, 2mg/kg
                    1500-r
                   1000--
                    500--
                                               tl
                                              It
                          H	1	1	1	\
                           12345
                             ELUTIONS
K and Mg concentration and release curves for Papermill
Sludge, EPA, SLT.
                           193

-------
             PAPER MILL SLUDGE,  EPA
          Zn a Fe ' CONCENTRATION a RELEASE
    PROCEDURE C, — - PROCEDURE R,  * SYN. LEACHATE,
 Zn CONCENTRATION,ppm
4.0-r
                                RELEASE,  2mg/kg
                            15-
                            10
                                 -?	«?	9	9-
   Fe CONCENTRATION, ppm
                              Fe RELEASE,2rng/kgX
1.5-


1.0-



0.5-



10-


10-


/ \
K \ 5
^v \
--••^ ^4 '+
-JL-^-Jpi-H-H
^,'
i
1 0
/ /
1 /
' /
i XX
. 0-^
/ xx
/
S
	 , 	 1 	 1 	 \ 	 i
A ~t A f>
                                      ELUTIONS
         12345
           ELUTIONS
Figure 116.  Zn and Fe concentration and release curves for Papermill
           Sludge, EPA,  SLT.
                            194

-------
               PAPER MILL  SLUDGE, EPA
             Cu CONCENTRATION a RELEASE
        	PROCEDURE C         0HpO

        	PROCEDURE R         A SYNTHETIC LEACHATE
         Cu CONCENTRATION, ppm   Cu RELEASE, Smg/kg
        4-
        3--
        2-
15--
10--
                                5--
             12345
               ELUTIONS
 /
 \r
I!
                                             -*
     12345
        ELUTiONS
Figure 117.  Cu concentration and release curves for Papermill Sludge
           EPA, SLT.
                           195

-------
                            REFERENCES
1.
2.
3.
4.
Ham, R.K'., M.A. Anderson, R. Stegmann, and R. Stanforth.  Back-
ground Study on the Development of a Standard Leaching Test.
Final Report on EPA Contract R-804773-01, submitted to EPA
August, 1978.

Abel son, H. and W. Lowenbach.  Procedure Manual for Environmental
Assessment of Fluidized Bed Combustion Processes.  Mitre Corp.,
M77-34 (1977).

American Public Health Association.  Standard Methods for the
Examination of Water and Wastewater, 13th Edition, APHA, Inc.,
New York, 1971.

ASTM.  Standard Test Method for Solvent Extraction of Organic
Matter from Water, D-2778-7Q.
                                  196

-------
                         APPENDIX

            MASS SPECTRA OF COMPOUNDS  IDENTIFIED
                  IN WASTE HEXANE EXTRACTS
INK
 42
               HI  WRSTE
                    WR8TE
                                                             35
                                                              r
1
            50
150
290
    Figure  A-1.  Mass spectrum of xylene  identified in
             Ink and Paint Waste hexane extract.
                           197

-------
»

100
  INK
   47
  PRINT  WfiSTE
     -45,  WflSTE
              jL
           ^Hs^ta^sfss/^s
                                                    45
I
       50
                                            150
                                                    200
Figure A-2.  Mass  spectrum of cumene identified in
       Ink and Paint Waste hexane extract.
                      198

-------
*
100
   INK
    59
 PRINT  NflSTE
   -56,  WflSTE
        I
              ,
1
     50
                                                              200
Figure A-3.  Mass  spectrum of m-ethyltoluene identified
   in Ink and Paint Waste hexane extract.
                   199

-------
»2   INK
«     69
100
 PRINT WRSTE   DRY 1,  ELUTION 1
    -73, (67 SflT.), ELUTION
                                                    10
      50
                        71i(13?£ijC^^

                                100            150
200
Figure A-4.  Mass spectrum of cyclohexanone identified
      in Ink  and Paint Waste hexane extract.

(Spectrum in hexane extract was too close to background
for a clear spectrum, so corresponding spectrum from SLT
H20 leachate,  day 1, is presented.)
                     200

-------
«2   INK
«     76
ISO
WRSTE
 WRSTE
                              10Q
                          150
                                                              200
       Figure A-5.  Mass spectrum of 2-nor-butoxyethanbl  identified
               in Ink and Paint Waste hexane extract.
                             201

-------
*2   INK
*    188
100
     PRINT WRSTE  DRY  1,  ELUTION 1
        -178,  ELUTION
                                                         65
                         130
                                                 150
200
Fiaure A-6.  Mass spectrum of 3,3,6-trimethyl bicyclo (3.1.0)
     hexan-2-one or 3,5,5-trimethyl-2-cyclohexanone
     identified in Ink and Paint Waste  hexane extract.

(Spectrum in hexane extract was too close to backgrounder
a clear spectrum, so corresponding spectrum from SLT H20
leachate, day 1, is presented.)
                          202

-------
*2 INK * PRINT WfiSTE DRY 1, ELUT!
* 229 -221, ELUTION
LOO
^^^.J J






           50
.08
Figure A-7.  Mass spectrum of dimethyl  glutarate  identified  in
            Ink and Paint Waste hexane  extract.

(Spectrum in hexane extract was too close  to  background for  a
clear spectrum, so corresponding spectrum  from SLT H00 leachate,
day i  is presented.)                               £
                           203

-------
            ol-
            io
                                                                   o
                                                                  •s
o
rC

-l->
X
OJ

C1J

(O
X
OJ
JC

(1)
-p
CO
 CO
                                                                                (O
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FOOD GRRDE HflSTE
»   274     -264,   F.6.W. *S

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      Fiqure A-10.  Mass spectrum  of  octadecane identified
             in Food Grade Waste hexane extract.
                           206

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FOOD GRflOE WflSTE
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  Figure A-^IK  Mass  spectrum of hexadecane  identified
           in Food  Grade Waste hexane extract.
                           207

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FOOD GRROE WRSTE
*   54     -58.   F.G.H-
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  Figure A-12.  Mass  spectrum of tetradecane identified
           in Food  Grade Waste hexane extract.
                             208

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      in Food. Industry, Clay Waste hexane  extract.
                            211

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«10  FOOD INDUSTRY, CLRY WRSTE
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        in Food  Industry Clay Waste hexane extract.
                               212

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«    75     -79,  *10 CLflY WRSTE

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         in Food Industry  Clay Waste hexane  extract.
                             213

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                                   TECHNICAL REPORT DATA     .
                            (Please read Instructions on the reverse before completing)
1. REPORT NO.
 EPA-600/2-79-071
4. TITLE AND SUBTITLE
 COMPARISON OF THREE WASTE LEACHING TESTS
                                   REPOI
                                  July  1979  (Issuing Date)
                                                            6. PERFORMING ORGANIZATION CODE
7.AUTHOR(S)
 Robert K. Ham,  Marc A. Anderson,  Rainer Stegmann,
 and Robert  Stanforth        	
9, PERFORMING ORGANIZATION NAME AND ADDRESS

 Department of Civil and Environmental  Engineering
 University of Wisconsin-Madison
 Madison,  Wisconsin  53706
                                                            10. I
                                   1DC818.  SOS 1, Task 38A
                                  11. CONTRACT/GRANT NO.

                                   Grant No. R-804773-01
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
                                   Final
                                  14. SPONSORING AGENCY CODE


                                   EPA/600/14
 15.SUPPLEMENTARY NOTES                                                            rnn/o in nn
 See  also "Comparison of Three Waste Leaching Tests;  Executive Summary," EPA-600/8-79-00
 Project Officer:  Donald  Sanning  513/684-7871.	
 16. ABSTRACT

 A  comparison of three  leaching tests was performed with fourteen industrial  wastes to
 evaluate the potential  of each test for use  as  a  standard leaching test.   The study
 was  done in conjunction with a background study on the development of  a  standard
 leaching test.

 The  advantages and  disadvantages of each test,  based on the leaching characteristics
 of the fourteen wastes and the usefulness of each procedure as a standard test, are
 analyzed and compared.   Finally, some comments  on the need for careful interpretation
 of test results are provided.
 17.
                                 KEY WORDS AND DOCUMENT ANALYSIS
                   DESCRIPTORS
                                               b.lDENTIFIERS/OPEN ENDED TERMS
                                                                             COSATI Field/Group
  Waste disposal
  Tests
  Assessments
  Leaching
  Methodology
  Selection
  Interpretation
Industrial wastes
Evaluation
Solid waste management
Leachate
Methods
Leaching  tests
Industrial  sludges
Landfill
                                                       14B
 18. DISTRIBUTION STATEMENT
                      19. SECURITY CLASS (ThisReport)
                      UNCLASSIFIED     	
                                                                                  234
 L
  RELEASE TO PUBLIC
                      20. SECURITY CLASS (Thispage)

                      UNCLASSIFIED
                                                                           22. PRICE
  EPA Fo»m 2220-1 (Rev. 4-77)
                                              214
                                      U. S. GOVERNMENT PRINTIHG OFFICE: 1979 — 657-060/5308

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