104
Appendix A. APPENDIX AI. eLA Y PRETREATMENTS. Removal of carbonates. (Jackson.I969) 1. Prepare the buffered sodium acetate-acetic acid buffer by dissolving 82 g of sodium acetate in 900 mI of distilled water, add 27 ml of glacial acetic acid and adjust to pH 5 by means of adding acetic acid. Dilute to 1 L. 2. Add 109 of powdered sample to a beaker containing 250 mL of the buffered solution. Allow to react at room temperature for 30 min or until no further CO 2 gas is evolved, stirring occasionally. Place a cover glass over the beaker and digest on a hot "place set low enough to avoid boiling. If the reaction is too violent place the beaker in a water bath. Digest for about 1 hour. 3. Wash the residue in distilled water by centrifugation at 2000 rpm for 5 min three times, discarding the supernatant solution in each case. 4. The sample is now ready to proceed to the next stage. Remoyal of iron oxides. (Mehra & Jackson. 1959) 1. Place 4-5 g of powdered sample in a small beaker, to this add 40 mL of 0.3 M sodium citrate solution and 5 mL of 1 M NaHC0 3 solution. Heat at 80°C in a water bath for about 10 min. Add 1 g of solid Na2S204 and stir constantly for 1 min and then occasionally for 15 min. 2. At the end of the digestion period add 10 mL of saturated NaCl solution and 10 mL of acetone to promote flocculation. 3. Mix the solution for about 1 min in the water bath, then transfer the contents of the beaker into IOOmLcentrifuge tubes and centrifuge at 2000 rpm for 5 min. Discard the supernatant solution and wash twice with distilled water by centrifugation. 4. The sample is now ready to proceed to the next stage. 306

APPENDIX AI. eLA YPRETREATMENTS.etheses.whiterose.ac.uk/14669/2/587539_vol2.pdf · 2016. 10. 3. · 4 14 24 34 44 °29 Figure 5.33a .Sample C.13.1 whole rock scan. Whole rock acan

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  • Appendix A.

    APPENDIX AI. eLA Y PRETREATMENTS.

    Removal of carbonates. (Jackson.I969)

    1. Prepare the buffered sodium acetate-acetic acid buffer by dissolving 82 g of sodium

    acetate in 900 mI of distilled water, add 27 ml of glacial acetic acid and adjust to pH

    5 by means of adding acetic acid. Dilute to 1 L.

    2. Add 109 of powdered sample to a beaker containing 250 mL of the buffered

    solution. Allow to react at room temperature for 30 min or until no further CO2 gas is

    evolved, stirring occasionally. Place a cover glass over the beaker and digest on a hot

    "place set low enough to avoid boiling. If the reaction is too violent place the beaker

    in a water bath. Digest for about 1 hour.

    3. Wash the residue in distilled water by centrifugation at 2000 rpm for 5 min three

    times, discarding the supernatant solution in each case.

    4. The sample is now ready to proceed to the next stage.

    Remoyal of iron oxides. (Mehra & Jackson. 1959)

    1. Place 4-5 g of powdered sample in a small beaker, to this add 40 mL of 0.3 M

    sodium citrate solution and 5 mL of 1 M NaHC03 solution. Heat at 80°C in a water

    bath for about 10 min. Add 1 g of solid Na2S204 and stir constantly for 1 min and

    then occasionally for 15 min.

    2. At the end of the digestion period add 10 mL of saturated NaCl solution and 10 mL

    of acetone to promote flocculation.

    3. Mix the solution for about 1 min in the water bath, then transfer the contents of the

    beaker into IOOmL centrifuge tubes and centrifuge at 2000 rpm for 5 min. Discard

    the supernatant solution and wash twice with distilled water by centrifugation.

    4. The sample is now ready to proceed to the next stage.

    306

  • Appendix A.

    Removal of or~anic material. (Moore & Reynolds. 1989)

    l. Place 5 g of powdered sample into a beaker, add 50 mL of 15% NaOCL that has been

    adjusted to pH 9.5 with HCL.

    2. Heat the mixture on a hot plate located in a fume cupboard for about 30 min.

    3. Transfer the contents of the beaker to 100 mL centrifuge tubes and centrifuge at 2000

    rpm for 5 min discarding the supernatant liquid.

    4. This procedure may be repeated until organic matter is sufficiently removed, as

    evident by a change in sample colour from dark grey to white, light grey or red. The

    sample is now ready to proceed to the next stage.

    Calculation ofcentrifu~e speeds usin~ the model MSE Centaur 2.(Jackson, 1969)

    1+-1. ----R I

    LIIomm -50mm_j

    n Centrifuge spin axis.Centrifuge tube 1

    1+-1. ------tiJ 10 mm1 90mm r·...._--s --- ....

    lOmm

    where» TJ - viscosity of water.

    Nm - centrifuge speed in rpm.

    OJ.! - particle diameter in microns.

    ~s - difference in the specific gravity of the sample and water.

    307

  • Appendix A.

    20°C - ~s = 1.652 11 = 0.01005

    21°C - ~s = 1.652 11 = 0.00981

    22°C - ~s = 1.652 11 = 0.00958

    23°C - ~s = 1.652 11 = 0.00936

    S=60mm R= 150mm.

    Worked example:-

    At 20°C, rpm of900 to separate the 2j..lmclay size fraction -

    !min = [(63 X 108) X (0.01005) X loglO(150/60)] I [(9002) X (22) X (1.652)]= 4.7 minutes.

    308

  • Appendix A

    APPENDIX A2. WHOLE ROCK XRD PLOTS.

    Key to whole rock mineral scan annotations.

    Ch - Chlorite. Q - Quartz. G - Goethite.

    I - Illite (including muscovite). PF - Plagioclase feldspar. C - Calcite

    liS - Mixed layer illite/smectite. OF - Orthoclase feldspar. D - Dolomite.

    K - Kaolinite. P - Pyrite. S - Siderite.

    Pa - Paragonite. H - Heamatite.Srn - Smectite.

    Whole rock Ca11.

    .)::!vu

    3000

    i 2500..!:!. 2000~ 1500•c~

    1000500

    04 14 24 34 44

    °29

    Figure 5. Ia . Sample Ca. I. I whole rock scan.

    Whole rock scan Ca12

    .)ow

    3000

    i 2500£. 2000~ 1500•c 1000•.5

    500

    04 14 24 34 44

    °29

    Figure S.2a . Sample Ca. 1.2 whole rock scan.

    309

  • !~---~--------_..._. ----.---- ..----"~-- ------_------ .._------------ -- - __ ------ -- ....----.- ..----~

    Whole rock sean Ca13

    40003500

    -;; 3000a. 2500~~ 2000III 1500c.! 1000.5 500

    04 14 24 34 44

    °29

    L - - _._._.--------_._-----_-.-_-----_" _, .._

    Figure 5.3a . Sample Ca.}.3 whole rock scan._-------. _----_. __ -_ •.._._----

    Whole rock scan 011

    IUVV

    6000

    i 5000~ 4000~ 3000..c.! 2000.5 1000

    04 14 24 34 44

    °29

    Figure 5.4a . Sample 0.1.1 whole rock scan.

    Whole rock scan 012

    30002500

    i 2000~

    ~1500

    c 1000.!.5 500

    04 14 24 34 44

    °29

    Figure 5.5a . Sample 0.1.2 whole rock scan.

    310

    Appendix A

  • Appendix A

    ·----~~------··~·-·lI

    Whole rock scan 021

    5000

    4000..a.3000~

    ~2000IIc

    .I

    .5 1000

    04 24

    ~

    14 34 44

    Figure 5.6a . Sample 0.2.1 whole rock scan.

    Whole rock scan 031

    40003500

    !I

    I

    1 _

    i 3000~ 2500

    f 200015001000500

    24

    ~e34 444 14

    Figure 5.7a. Sample 0.3.1 whole rock scan.

    Whole rock scan S11

    2500

    2000

    I 1500~ 1000I 500

    14 24 4434

    Figure 5.8a . Sample S.l.1 whole rock scan.

    311

  • Appendix A

    ------------- -------------1 ,Whole rock scan S31

    3000

    2500

    i 2000.!!.~ 1500

    "c: 1000.I.5 500

    04 14 24 34 44

    "29

    Figure 5.9a . Sample S.3.1 whole rock scan.r----'--------.-.--~- . -----------

    I

    Whole rock scan S32

    450040003500

    i 3000~ 2500

    IE500

    I 0 l:4~~~~1:;4:::::-::::~~::;24~~::::::::::::;34~~~~44

    l ---------------=----------Figure 5.IOa. Sample S.3.2 whole rock scan.Whole rock scan 011

    40003500- 3000I 2500.!!.

    ~ 2000

    I15001000500

    0

    1 4._.'4___=_ _~ ~ _Figure 5.11a . Sample 0.1.1 whole rock scan.

    312

  • Appendix A

    ----~~~-- ---!

    ----~-------~---

    Whole rock scan 012

    3000

    2500t 2000u-~ 1500.,c 1000•.s 500

    04 14 24 34 44

    --------~----------

    Figure 5.12a. Sample D.l.2 whole rock scan.

    Whole rock scan 021

    25002000-B. 1500~

    ~ 1000.,c•.s 5000

    4 3424~9

    4414

    Figure 5.13a . Sample D.2.1 whole rock scan.

    Whole rock scan C1B1

    18001600

    - 1400B. 1200~ 1000~ 800I 600! 400

    2000

    4 14 24eza

    34 44

    Figure 5.14a . Sample C.l.B.l whole rock scan.

    313

  • Appendix A

    rIII

    I

    3500

    3000- 2500t~ 2000~ 1500•c:

    1000!.5

    500

    04

    Whole rock scan C1B2

    24

    ~

    34 4414

    _______ ~ ,_. __ . . ~ . . ... .. __ .. ~ .._. __ J

    Figure 5.15a. Sample C.I.B.2 whole rock scan.

    Whole rock acan C1B4

    45004000

    t35003000

    ~ 2500~ 2000

    I15001000500

    04 14 3424

    ~

    44

    Figure S.16a. Sample C.I.B.4 whole rock scan.r --- - -

    Whole rock scan C1as

    40003500

    - 3000I 2500~f 200015001000

    5000

    4 14 24

    ~

    34 44

    Figure 5.17a . Sample C.I.B.S whole rock sean.

    314

  • Appendix A

    Whole rock scan C21

    35003000

    i 2500.e 2000~ 1500..r:::.8 1000.5 500

    04 14 24 34 44

    "29

    L. . ~_~ . . - ----.-------------~--.----------------.-. ".-~~--_j

    Figure 5.l8a. Sample C.2.1 whole rock scan.F"" -~--- ----------------~-.-------------------.------- -----,

    Whole rock scan C31

    400035003000

    i 2500~~2ooo! 1500~ 1000

    500

    I 0 4 14 24 34 44

    l________ _ - ---:---------~-----.------------- -----------------------Figure 5.19a . Sample C.3.1 whole rock scan.

    r" --------- ..-,--- ..-,---.------.~-.--- --._--- ..---------.--------- ...- -_..._--------- ..-----'---,. --- ..------ ..-----._----- ----,--" -.------II

    II,

    Whole rock scan C41

    2500

    2000-I1500.e

    f 10005000

    4 14 24 34 44

    iL ._.._.__._,..-.._-,.--,----,.---_.-.-----,--_---.------.,--~----..._----------.---------.--------------.--------,."_--....--- -Figure 5.20a . Sample C.4.1 whole rock scan.

    315

  • ~--- ------------

    Whole rock scan CSi

    35003000.. 2500a.

    ~ 2000~ 1500II)i=:S 100:1.5

    50004 24 34 4414

    Figure S.2Ia. Sample C.S.I whole rock scan.,----I

    3500 _

    3000

    t 2500~ 2000~ 1500!I 100:1 jI

    500104

    Whole rock scan C52

    24'2l

    34 4414

    Figure 5.22a . Sample C.5.2 whole rock scan.---I

    Whole rock ecan e6i

    2500

    2000au 1500-f 1000J 500

    04 14 24

    eze34 44

    Figure S.23a . Sample C.6. 1 whole rock scan.

    316

    Appendix A

  • Appendix A

    ~--------. ---~------- --------

    Whole rock scan C71

    IOVU

    1400

    i 1200~ 1000

    !'•~I

    800600400 ]200 1~-......_--o L-,-,----~------- --_-,--~-4 14 4424 34

    i_________________________________ . . __ J

    Figure 5.24a .Sample C.7.1 whole rock scan.

    Whole rock acan C82

    2500

    2000

    i1500~

    !'1000I

    .5 500

    04 14 24

    "29

    ~- -~.---..-

    34 44

    Figure 5.25a . Sample C.g.2 whole rock scan.

    Whole rock scan C83

    2500

    2000-I1500~

    !' 1000!I 500

    04 24

    "29

    34 4414

    Figure 5.26a .Sample C.g.3 whole rock scan.

    317

  • Appendix A

    ~------ -----

    Whole rock scan C92

    1000800

    i600.2-

    ~ 400!I 200

    04 14 24 34 44

    °29

    Figure 5.27a. Sample C.9.2 whole rock scan.r------I

    Whole rock scan C101

    35003000

    i 2500.2- 2000~ 1500

    I1000500

    04 34 4414 24

    °29

    Figure 5.28a . Sample C.l 0.1 whole rock scan.

    Whole rock ecan C111

    2000

    !1500

    I100050024 34 444 14°29

    Figure 5.29a . Sample C.ll.l whole rock scan.

    318

  • Whole rock scan C112

    3000

    2500

    i 2000~~ 1500I!! 1000! 500

    04 14 24 34 44

    ·29

    Figure 5.30a . Sample C.ll.2 whole rock scan.r-------·-----~---II

    1I

    ----------~--- -_ .._-------_I

    Whole rock scan C121

    2000

    1500!~ 1000

    I 5004 14 24 34 44

    ·29

    Figure 5.31a. Sample C.12.l whole rock scan.

    Whole rock scan C122

    2000

    - 1500'!..!!.~ 1000

    I 50004 14 24

    02E)

    34

    Figure 5.32a . Sample C.l2.2 whole rock scan.

    319

    Appendix A

  • I-----~--~-Whole rock scan C131

    16001400

    0 1200B. 1000a~ 800I!! 600~ 400

    2000

    4 3414 24 44

    °29

    Figure 5.33a . Sample C.13.1 whole rock scan.

    Whole rock acan C132

    6000

    5000

    i 4000u-~ 3000! 2000I 1000

    04 14 24 34 44

    "29

    Figure 5.34a . Sample C.13.2 whole rock scan.

    Whole rock KIIn C133

    2500

    2000

    ! 1500

    4 14 24 34 44

    Figure 5.35a . Sample C.13.3 whole rock scan.

    320

    Appendix A

  • Appendix A

    ~~~--- --~~~~

    Whole rock scan C141

    3000

    2500

    i 2000~~ 1500! 1000~ 500

    04 14 24 34 44

    "29

    L~_~ ~~-

    Figure 5.36a. Sample C.l4.1 whole rock scan.~~ ---------_ ------ ---- -------- --------------l

    Whole rock ecan C151

    35003000

    i 2500~ 2000~ 1500

    I100050004 34 4424

    "29

    14

    Figure 5.37a . Sample C.15.1 whole rock scan.

    Whole rock ecan C161

    16001400

    i 1200~ 1000~ 800

    I 60040020004 24 34 4414

    ·29

    Figure 5.38a. Sample C.16.1 whole rock scan.

    321

  • Appendix A

    ------------------I

    I

    II 5000II 4000

    IIt

    3000.!:!.

    I~

    20001 jI

    1000 ~J

    04

    IL__

    r-I

    II

    5000

    - 4000I3000.!:!.

    Whol. rock acan C171

    34 4414 24

    ~

    Figure 5.39a . Sample C.17.l whole rock scan.

    Whol. rock acan C172

    ~ 2000

    I I.oooI o.f:=~~::;=::=~~~~~~~~

    4 14 24 34 44

    I ~

    l~__~__Figure 5.40a . Sample C.17.2 whole rock scan.

    Whol. rock .can C181

    2500

    2000

    !1500I1000500

    o~~~~~~~~~~~~..____________ . .. . ~ __ .__ .. .. J

    Figure 5.4Ia. Sample C.IS.I whole rock sean.

    322

  • Appendix A

    APPENDIX A3. CLAY MINERALOGY XRD PLOTS.

    Ca11 «2J1m)

    5000

    4500

    4000

    3500

    r 3000"-~ 2500! 2000J

    1500

    1000

    500

    04 9 24

    ~

    29 34 3914 19

    ~--------------------Figure 5.42a . Sample Ca. I. I.

    ~------~-----lCa12 «2J1m)

    I+Q

    3500

    3000

    2500

    -f 2000-~i 1500

    1000

    500

    04 39 4424 29 349 14 19

    ·29

    Figure S.43a . Sample Ca.l.2.

    323

  • Appendix A

    ~--'--'-'----~-I

    I

    I

    (-- Mm

    3500

    3000

    t 2500Co)-~ 2000II 1500

    1000

    500

    04 9

    Ca13 «2J.1m)

    29 39 44

    II

    I

    I

    i

    I

    I.~ __ .~ ~ . .J

    GJy.

    3414 19 24

    "29

    Figure 5.44a . Sample Ca.1.3.

    011 «2J.1m)

    10000

    9000

    8000

    7000-I 8000.!.

    f5000

    4000

    3000

    2000

    1000

    04

    Ch+K

    Ch+K I+IIS

    29 34 39 449 14 19 24

    eze

    Figure S.4Sa . Sample 0.1.1.

    324

  • 8000

    7000

    6000

    i 5000u-:t 4000!~ 3000

    2000

    1000

    04

    Appendix A

    012 «2~m)

    Ch+

    K~

    liS I ~~ Ii Ch+ I+IJS

    l III I+IJS K

    \>1 I ~-- GJ,.V'AJ l~j~_jU A.D.

    9 19 4424

    "29

    29 34 3914

    ___~ J

    Figure 5.46a . Sample 0.1.2.

    ---~--------O-2-1-«-2-J1m-) --------- --~---~----~I10000

    9000

    8000

    7000

    i 6000e

    f 500040003000

    2000

    1000

    04

    L

    I+Q

    Ch

    Ch

    9 14 19 3424

    "29

    29 39 44

    ------- --------------Figure 5.47a . Sample 0.2.1.

    325

  • Appendix A

    326

  • Appendix A

    I----~I

    9000 Ch

    I8000 ,I

    I7000

    ~ /'6000i 5000~ U~! 4000

    L~~ 3000

    2000

    1000 LJ04 9 14

    831 «2J.1.m)

    I+Q

    Ch

    A.D.

    ,IiI!!IL.__ J

    19 24 29 34 39°29

    Figure 5.50a. Sample S.3.1.

    ---_._--- -----------------------------,i832 «2J.1.m)

    9000 Ch

    8000

    7000 Ch

    I LL~6000 Ch!5000 Li _-~~

    I400030002000

    1000 L~~U0

    4 9 14 19 24 29 34 39°29

    Figure S.Sla. Sample S.3.2.

    Gly.

    A.D.

    327

  • Appendix A

    --,

    011 «2~m)

    I+Q16000

    Sm

    14000

    12000

    10000Ch Ch

    8000

    6000

    5 10o~----------------------------------------------------------

    Figure S.S2a . Sample 0.1.1.

    012 «2~m)

    10000

    9000

    8000

    7000-1 6000u Sm-~ 5000! 4000I

    3000

    2000

    1000

    04 9 14 29 34 39 4419 24

    -29

    ____j

    Figure S.53a. Sample 0.1.2.

    328

  • Appendix A

    021 «2J.1m)

    9000

    1000

    Ch8000

    7000 Ch

    6000t~5000

    fCh

    4000

    3000

    2000

    A.D.

    4 9 14 19 24"29

    29 34 39 44

    L_ i._-------_._--_._jFigure 5.54a . Sample 0.2.1.

    ---- -------------1

    C1B1 «2J.1m)

    4 9 14 19 24"29

    29 34 39

    LFigure 5.55a. Sample C.I.B.I.

    329

  • Appendix A

    ~--------------------------------------------------'--,

    C182 «2IJm)

    I+US I+US8000

    7000

    6000

    I 5000~ 4000!I 3000

    2000

    1000

    04

    IIL_____ ..

    9 19 2414 29 34 39 44·29

    iI__ ~ ~ ~~ __ ~ ~ ~ __ ..__ ~ .._.J

    Figure 5.56a . Sample C.I.B.2.

    6000

    5000

    4000

    Gly.

    4 14 19 24.. 3929 349Figure 5.57a . Sample C.I.B.4.

    330

  • Appendix A

    -l

    I

    I

    C1B6 «2J.1m)

    I+USUS I K5000

    4500

    4000

    3500

    t 3000'"-~ 2500•j 2000.=

    1500

    1000

    500

    04 29 34 39 4424

    ~

    L._____ J14 199

    Figure 5.58a . Sample C.I.B.s.

    ,--------- ----------------

    C21 «2J.1m)

    K+Ch7000

    6000

    5000

    -I 4000-~i 3000

    2000

    1000

    04

    A.D.

    US I K+Ch I+US

    KGly.

    34 39 4419 24

    02Q

    299 14

    L _ I___ JFigure 5.59a. Sample C.2.1.

    331

  • 1000 _/~ J

    O~ U4 9

    - 50001~ 4000

    I

    8000

    7000

    6000

    3000

    2000

    C31 «2J.1m)

    K

    I+I1S K

    Appendix A

    44

    IIII

    IJ

    Q

    J

    14 19 3924 29 34·28

    Figure 5.60a. Sample C.3.I.

    ~

    J\j~~~~DO~--4----+--~----+---~---+----~--~--~o

    4500 I4000 r35003000

    12500

    1000

    I:: K

    5 10 25 4030 3515 20

    Figure 5.61a. Sample C.4.1.

    332

    -----.-------.-----1

    Gly.

    45

  • Appendix A

    ------------~CS1 «2J1.m)

    K+Ch9000 liS I I+IIS8000

    7000

    6000i~ 5000

    f400013000

    K

    2000

    1000

    4 9 14 19 24~

    29 34 39 44IIL__

    Figure S.62a. Sample C.S.l.

    CS2 «2J1.m)

    12000 K+Ch

    K+Ch10000 liS I I+IIS

    8000

    4000

    2000

    4 9 14 19 24

    ~29

    l~ ~. .._. . .__ _ ,

    Figure 5.63a . Sample C.5.2.

    333

  • Appendix A

    7000

    6000

    5000

    i 4000Cl-~! 3000!

    2000

    1000

    04

    C61 «211m)

    9 14 19 24~

    29 34 39 44

    7000

    6000

    5000

    -I 4000Cl-f 3000

    2000

    1000

    04

    Figure S.64a. Sample C.6.1.

    ----~----------------!C71 «2J.1m)

    K+Ch K+Ch

    lIS I I : I+I/S

    ~ I ~ i ~7SC

    ~, ~----A 'l__---"__rn,i I !\ ~

    /"\__) '\___~-)~ __j \) ~~___l\~A.D.9 14 24

    ~

    29 3419 39 44

    L._________ ~ ~

    Figure S.64a. Sample C.7.1.

    334

  • Appendix A

    C82 «2J.1.m)

    10000

    9000

    8000

    7000

    K+Ch

    liS II+I/S

    K

    Gly.

    A.D.

    29 34 39 444 9 14 19 24"29 i. J

    Figure 5.65a . Sample C.8.2.

    ---------lI

    I

    II!I

    10000

    9000

    8000

    7000

    ! 6000 Ch

    K+Ch

    I+IIS K+Ch I+IIS

    3000

    2000

    1000

    O~~~~~~~~~~~~~~~~~~~~29 34 39 444 9 14 19 24

    "29I

    l ---------------Figure 5.66a . Sample C.8.3.

    335

  • Appendix A

    I

    II7000 liS I Ch+K I+IIS

    'i ( Ch+K6000 !I ! I5000

    Ch )iU~~eJ-t 4000u-~I 3000I

    2000 u~J10000

    4 9 14 19 24 29 34

    "29

    Figure 5.67a . Sample C.9.2.

    K

    Gly.

    .1-.--.......:::.....:;:::;::::__~:;:............~~~A.D. I39 44 I

    I--~~~--~--__j

    _.__ .._-- --------~-----

    C101 «2~m)

    10000

    9000

    8000

    7000

    - 6000I- 5000f 40003000

    2000

    1000

    04

    lIS I I+I1S!Ki I+~ K~Gly.

    A.D.

    29 34 39 449 14 19 24

    "29

    Figure 5.68a. Sample C.IO.I.

    336

  • Appendix A

    C111 «211m)

    7000

    6000

    5000

    i 4000Co»-~• 3000leI

    2000

    1000

    04

    I+IISI+IIS 1\

    ~ i11 Ch~+K I+IIS Ch+K·.

    Ch 1\ I Ch Q \ rry \__) 1~ 37SoC

    '- I

    !I

    Gly.

    A.D.

    14 19 24-ze

    29 399 34 44

    Figure 5.698 . Sample C.ll.l.

    1-------, 12000

    C112 «211m)

    I+IISI+IIS10000

    8000

    2000

    Gly.--~-

    A.D.

    24-ze

    29 39 4419 344 9 14

    Figure 5.708 . Sample C.ll.2.

    337

  • Appendix A

    C121 «2~m)

    7000

    6000

    5000

    t 4000~~I 3000I

    2000

    1000

    04 39 4429 349 14 19 24

    ~

    --- ---------~

    Figure 5.71a. Sample C.12.1.

    r-----------------------------

    I C122 «2~m)

    I

    I

    8000 K+ChK+Ch

    7000

    6000

    - 5000ICl-I40003000

    2000

    1000

    04

    I+IISJ+IISCh Q

    K

    Gly.

    A.D

    29 34 39 449 14 19 24~

    L _

    Figure 5.72a. Sample C.12.2.

    ------ -------------------------

    338

  • Appendix A

    -------------l

    III

    C132 «2J.1m)

    14000 I12~j10000 -

    -I 8000~f 6000.I.!i

    4000

    2000

    04

    K

    liS I I+IIS Q

    K

    I+IIS K

    _~J___~)750C

    Oly.__,, .._._A~_~~

    A.D.

    9 14 19 2402()

    29 34 39 44

    L _,,

    ----- ------------------------Figure S.74a . Sample C.13.2.

    339

  • Appendix A

    9000

    8000

    7000

    6000t

    5000Co)-~4000I

    ~ 3000

    2000

    1000

    04

    C133 «2~m)

    K K

    K

    Gly.

    A.D.

    9 14 19 24

    ~

    29 39 4434

    I____~i

    Figure 5.75a . Sample C.l3.3.

    3000

    2000

    1000j

    o j ,4

    C141 «2~m)-------1

    I!

    I+IIS

    K+Ch ~I+I~k

    __A~. ~v~LJ~u~_,~ AD.

    Gly.

    i , • i

    9 14 19 24~

    29 39 4434

    Figure 5.76a. Sample C.14.1.

    340

  • Appendix A

    C161 «2~m)

    14000K+Ch

    13000 K+Ch1200011000

    10000

    t 9000 I+IIS Ch I+I/S.2- 8000

    ~ 7000 K 375°C• 6000c:! 5000

    4000 Gly.

    300020001000 A.D.

    0

    I4 9 14 19 24 29 34 39 44

    "29 _jFigure S.77a. Sample C.lS.l.

    ~----IC161 «2~m) i

    II

    12000 K IKII

    10000III

    8000

    t.!!. I+Ch~ 6000 liS I

    I K\ 375°C4000 ~Gly.

    2000A.D.

    04 9 14 19 24 29 34 39 44

    "29IL -'---'~--'~

    Figure S.78a. Sample C.l6.1.

    341

  • Appendix A

    C171 «2~m)

    I+US K+Ch6000

    5000

    4000-&.!!.~ 3000I.a.e 2000

    1000

    04

    Gly .

    A.D.

    19 24~

    29 34 39 449 14

    iI

    ___j

    Figure 5.79a. Sample C.17.1.

    ,-----------~- ------------- ~------

    C172 «2~m)

    8000T7000

    I+US K+Ch

    6000

    5000

    A.D.

    34 4439-29

    ------------~~.----~-Figure 5.80a . Sample C.17.2.

    342

  • Appendix A

    C181 «2J.1m)

    6000

    5000

    4000

    i~~ 3000•c::.a.s 2000

    1000

    04

    KK

    liS 1 :\ I+IISI

    I+IIS K

    i Gly.

    l ~D .19 24

    "29

    29 34 399 14 44

    Figure 5.Sla. Sample C.IS.I.

    343

  • Appendix A

    APPENDIX A4: RAW DATA FOR SEMIQUANTITATIVE eLA YDETERMINA nONS.

    Sample Qtz (I+I1S)-Q Chlorite Kaolinite Paragonite Smectite Gly: III Htd:I11Call 19.125 413.94 37.83 ----- 280 -----Cal2 19.25 391 33.93 ----- 228 -----Cal3 29.75 329.12 62.5 ----- 187.69 -----Oil 12.9 121.1 34.82 ----- ----- ---- 76 143.75012 43 285.94 70.31 ----- ----- ---- 51.5 93.25021 13.125 322.12 37.5 ---- 112 ---031 35.475 346.09 36.61 --- ----- -----Sil 40.312 699.94 46.87 ---- .---- ----- 66.5 97.5S31 30.637 546.86 62.5 ----- ----- -----S32 21.5 280.37 47.77 ---- ----- ----OIl 11.825 382.55 ---- 57.14 ---- 2.53012 45.15 385.91 9.37 ---- ----- 37.1021 25.53 441.72 93.75 ---- ----- -----ClS1 54.556 616.44 22.77 67.86 ----- ----- 310.25 365.75CIS2 146.737 376.51 26.78 100 ----- ---- 101.75 122CIB4 69.606 460.64 19.2 89.29 --- ----- 176.5 216.75CISS 56.437 641.81 5.36 166.7 ----- ----- 151.75 205.25C21 41.925 414.07 23.99 153.9 ----- ---- 84 136C31 56.437 451.94 ----- 157.7 ----- .---- 120.25 176.75C41 161.787 538.84 10.71 91.1 ----- ----- 156 265.75C51 15.05 581.95 21.87 136.9 ----- ----- 395.9 1260.8C52 16.93 367.19 18.58 133.9 --- ---- 102.25 142.5C61 33.86 541.14 20.7 57.14 ---- --- 148 213.5C71 30.1 269.9 44.64 142.86 ----- ----- 66 133.25C82 16.12 243.31 22.1 47.62 ----- --- 174.75 375.5C83 11.82 213.17 20.76 SO ----- ----- 183.5 228.75C92 129 1034.25 34.82 220.24 ----- ----- 187.5 331.5CIOI 51.6 1007.15 37.5 104.76 ----- ----- 141.75 204ClIl 64.5 131.06 IS.30 42.86 ---- - 110.75 254.5CI12 25.S 512.32 24.11 133.33 ----- ----- 209.25 354CI21 93.52 435.85 38.84 104.8 ----- ----- 239.5 323.5CI22 70.95 77.05 10.05 366.68 ----- ----- 43.5 59CI31 3S.7 61.3 ----- 327.38 ----- ----- 17.75 32.5C132 35.47 94.02 --- 252.38 ---- --- 17.75 30.5CI33 ------ 110 ----- 283 ----- ---- 40.75 96.25C141 99.97 680.52 44.2 138.09 --- ---- 166.5 250.75C151 19.35 127.65 19.64 190.48 ----- ----- 33 89.75CI61 38.7 56.3 -- 242.86 ---- --- 16 36.25CI71 38.7 430.3 36.16 130.95 ----- ----- 217.75 281.25CI72 32.25 493.75 29.46 136.9 --- ----- 194 292.75C181 55.9 98.16 22.3 163.69 ---- ----- 23 36.25

    344

  • Appendix A.

    APPENDIXA5. QUANTITATIVE DETERMINATION OF FREEQUARTZ BY SODIUM PYROSULPHATE FUSION.

    ReapDts

    A- 40g NaOH - IOOOcc.H20 - IN.

    20g NaOH - 1000cc. H20 - 0.5N.

    B- [Cone. HCL -10.5-12 N]

    IN HCL - 90cc. cone. HCL - IOOOcc.H20.

    3N HCL - 270cc. cone, HCL - IOOOcc.H20.

    Method.

    1. Weigh 20Omg. sand/silt size fraction, dried at IOsoC into a SOmI. vitreous silica

    crucible and 1O-1Sg. of sodium or potassium pyrosulphate [X2S207] powder, mix

    thoroughly using a glass rod.

    2. Fuse the mixture under a fume hood using a low flame to start, until vigerous

    bubbling of melt ceases, then a full flame of the meker burner is applied. When a

    heavy N~S04 crust covers the surface at full heat the fusion is complete. Whilst

    cooling the crucible is swirled to spread the melt onto the crucible sides.

    3. The solidified melt is transfered as a cake to a lS0cc. beaker with 60cc. 3N. HCL.

    using a rubber tipped glass rod. The cake is slaked by gentle boiling and the resultant

    suspension is transferred to a 70cc. pointed centrifuge tube. Seperate the insoluble

    material by centrifugation and discard the supernatant liquid, wash a further 2 times

    with 3N. HeL. each time discarding the supernatant liquid.

    4. Transfer the residue from the tube to a SOOcc.nickel or stainless steel beaker with

    O.SN. NaOH making a total volume of 100-ISOcc. Bring the suspension to a rapid

    boil then boil for 2.Smin., then cool rapidly in a cold water bath.

    345

  • AppendixA.

    5. Transfer the suspension to 2 x 70cc. pointed centrifuge tubes (transfer solid residue

    quantitatively). The residue is seperated and washed 3 times using 3N. HCL. (care to

    wash lip of tube) and once with distilled water.

    6. Transfer residue to a polyethylene centrifuge tube, add 5-10cc. of 30%

    hydrofluosilicic acid (H2SiF6 treated with pure quartz to remove any HF) stir

    contents twice daily keep in a dark place between IS-20°C (to prevent HF formation)

    for 3 days.lf sample has much feldspar repeat with fresh acid for further 3 days.

    7. After acid treatment wash and centrifuge 3 times with 50cc. portions of distilled

    water and transfer to a pre-weighed platinum or teflon crucible. Obtain weight of

    crucible and residue after total evaporation of water overnight at 105°C - check

    residue by XRD or under microscope for purity.

    CalculaUQo:-

    %Free quartz = [Wt.residue+Wt.sample] x 100.

    346

  • Appendix A

    APPENDIX A6: RAW DATA FOR XRD QUARTZ DETERMINATION.

    Sample %B Hr:QIB %Q %B Hr:Q/B %Q LOI% Ql-corr Q2-corrCall 10.18 0.76 16.23 10.35 0.75 16.27 3.32 15.7 15.7Cal2 9.48 0.992 20.06 10.15 0.91 19.63 2.85 19.5 19.1Cal3 9.29 1.04 20.66 9.29 1.06 21.07 2.99 20.0 20.4011 10.4 0.528 11.17 10.4 0.44 9.11 6.99 10.4 S.S012 12.28 0.361 8.58 12.28 0.324 7.56 7.92 7.9 7.0021 10.25 1.08 23.71 10.25 1.l02 24.22 4.62 22.6 23.1031 10.06 0.897 19.14 11.07 0.808 IS.8S 4.44 18.3 18.0511 10.54 0.872 19.46 10.54 0.897 20.05 4.0 . 18.7 19.2531 9.97 0.966 20.51 9.97 0.887 18.74 4.22 19.6 IS.0532 9.64 1.263 26.26 9.64 1.333 27.78 4.48 25.1 26.5011 9.88 0.874 18.29 9.88 0.956 20.10 8.51 16.7 IS.4012 '10;99 0.53 11.85 10.99 0.58 13.08 11.66 10.5 '11;6021 11.81 0.412 9.6 11.81 0.479 11.38 4.18 9.2 10.9CIBI 10.07 0.25 4.52 10.07 0.23 4.07 26.64 3.3 3.0CIB2 8.94 0.69 12.85 . 8.938 0.73 13.65 5.S6 12.1 12.9CIB4 9.21 1.09 21.51 9.21 1.053 20.75 6.1S 20.2 19.5CIBS 9.92 1.195 25.51 9.92 1.21S 26.02 5.63 24.1 24.6C21 10.03 0.907 19.31 10.03 1.05 22.53 16.0 16.2 18.9C31 10.45 1.69 38.49 10.45 1.74 39.67 11.24 34.2 35.2 -C41 8.98 0.396 6.98 8.98 0.365 6.35 20.08 5.6 5.1C51 10.44 0.744 16.27 10.44 0.867 19.16 7.55 15.0 17.7C52 11.135 1.3 31.26 11.135 1.36 32.76 4.95 29.7 31.1C61 10.4 0.558 11.87 10.4 0.551 11.70 5.60 11.2 11.0C71 11.64 0.68 16.47 11.64 0.69 16.73 9.96 14.8 15.1C82 10.11 0.395 7.83 10.11 0.436 8.77 11.38 6.9 7.8C83 9.96 1.129 24.14 9.96 1.26 27.07 5.77 22.7 25.5C92 9.93 0.35 6.69 9.93 0.317 5.96 56.45 2.9 2.6CIOI 10.31 0.957 21.00 10.31 1.03 22.69 5.12 19.9 21.5Clli 10.03 0.346 6.67 10.03 0.303 5.7 13.08 5.8 5.0C1l2 9.97 1.15 24.63 9.97 1.20 25.75 7.03 22.9 23.9Cl21 13.8 0.316 8.25 13.8 0.27 6.82 9.56 7.5 6.2CI22 11.10 0.417 9.15 11.10 0.462 10.27 16.36 7.7 8.6CI31 12.11 0.226 4.79 12.10 0.239 5.14 21.54 3.8 4.0CI32 10.65 1.094 24.97 10.65 1.002 22.77 8.81 22.8 20.SCI33 10.93 0.52 11.54 10.93 0.523 11.61 11.19 10.2 10.3CI41 11.92 0.622 15.31 11.92 0.688 17.08 8.72 14.0 15.6CI51 10.035 0.81 11.13 13.035 0.766 20.96 8.53 15.7 19.2CI61 12.235 0.307 7.06 12.235 0.314 7.26 23.66 5.4 5.5C171 11.22 1.574 38.41 11.221 1.423 34.60 7.04 35.7 32.2CI72 12.43 1.095 29.17 12.43 1.053 28.00 6.41 27.3 26.2CI81 10.51 0.80 17.70 10.51 0.85 18.88 9.2 16.1 17.1

    347

  • Appendix A.

    APPENDIX A7. DETERMINATION OF PYRITE BY CHROMIUM

    REDUCTION.

    ~======~@

    Experimeptal Apparatus.

    @-

    (1) Reaction flask: (2) Reagent inlet port and treservoir : (3) Argon inlet port: (4) Condenser: (5) Bev -O-Line tubing™. (6) Trapping vessel.

    Reapnts.

    Chromic chloride hexahydrate.

    Conc. HCL.

    Ethanol (95%).

    2% Copper sulphate solution.

    Argon gas.

    For the Jones reduetor:-

    Granulated zinc (20-30 mesh).

    Mercuric nitrate.

    348

  • Appendix A.

    Metbod.

    1. Prepare the Jones reductor (see Vogel,1978 p.395) by packing the zinc which has

    been amalgamated (usingan acidic 2% mercuric nitrate solution) into a glass column.

    2. Draw the 1 M chromic chloride solution (which has been acidified to 0.5 N with

    HCI) under vaccum through the Jones reductor. On reduction the green chromic(III)

    solution changes valence state to blue chromic (II). Due to atmospheric oxidation this

    solution is unstable and should be prepared every two days. Store the prepared

    solution in a glass vessel out of direct light.

    3. Weigh out 1 g of the powdered sample into the digestion flask, add 10 ml of ethanol,

    connect to the condenser and flush with argon for a few minutes. To the trapping

    vessel add 75 mL of 2% CUS04 solution, in addition retain a 10 mL fraction as a

    stock solution for analysis.

    4. Through the side arm add 40 mL of the CrCl2 solution and 20 mL of concentrated

    HCI apply a bunsen flame and boil the mixture for two hours.

    5. When the digestion has been completed, filter the contents of the trapping vessel,

    thus removing any CuS precipitate from the solution and retain 25 mL of the reacted

    copper sulphate solution for ICP-AES analysis.

    CalculatioQ example.

    Reaction- FeS2+ 2H2= 2H2S + 2CUS04 = 2CuS + 2H2S04·

    Therefore by atomic weights:- CuS = S/Cu =0.504.

    FeS2 = FeS2/S2 = 1.871.

    :. Blank CUS04 solution by ICP-AES = 9640 ppm Cu.

    :. Test CUS04 solution by ICP-AES = 8750 ppm Cu.

    349

  • Appendix A.

    Convert concentrations of the solutions used into concentration of copper in test

    quantity ie. 75 mL and convert ppm (concentration) into mg (weight) where 0.001 mglg

    = 1 ppm.

    :. In the 75 mL stock solution = (9640 x 75)/1000 = 723 mg Cu.

    In the 75 mL test solution = (8750 x 75)/1000 = 656.25 mg Cu.

    Therefore the reaction uses up (723 - 656.25) = 66.75 mg ofCu.

    S used = Cu(66.75 mg) x 0.504 = 33.68 mg.

    FeS2 detected = S(33.68) x 1.871 =2lmg.

    Therefore in 612.5 mg of test sample there is 63 mg of FeS2 (pyrite)

    :.(63 x 100)/612.5 = 10.3% pyrite.

    Notes.

    1. It is advisable to split the gas supply line into two or four outlets so that multiple

    digestions may be run at the same time.

    2. Make sure the reaction digestion vessel is washed out as soon as it is cooled enough

    to be handled as the contents solidify.

    3. Only use H2S- resistant line (ie. Bev-A-Line IV®) as the connection to the

    absorption cell as other rubber lines will react giving off sulphur gas.

    4. Care must be taken with the ICP analysis, the equipment must be carefully calibrated

    against a standard and checks run to make sure there are no instrument fluctuations

    which may result in errors.

    5. IfICP or AA are not available the absorbant solution may be titrated with 0.1 M

    EDTA (see Vogel 1978).

    350

  • Appendix A.

    APPENDIX A8. DETERMINATION OF NON ORGANIC CARBON

    (C02) AND ORGANIC CARBON (Corg) IN MUDROCKS.

    Experimental apparatus.

    Rea&enQ.

    (1) Reaction flask: (2) Condenser: (3) Argon

    inlet: (4) Arnold bubbler: (5) Glass bead water

    trap: (6) Absorbant solution reservoir: (7) Rea-

    ction cell: (8) Micro burette: (9) Titrant soluti-

    on reservoir: (10) Gas outlet port.

    Concentrated orthophosphoric acid.(H3P04)

    Chromic acid (analar).

    Silica gel (self-indicating).

    Soda asbestos 6-12 mesh.

    Absorbant solution:- 300mls of dimethyl fonnamide mixed with 10 mls of

    ethanolamine and 3m1s of thymolphthalain indicator solution (0.1% in dried methanol).

    Titrant:- 0.1 N Tetra-n-Butyl Ammonium hydroxide.

    351

  • Appendix A.

    Method.

    1. Weigh out the appropriate amount of sample «O.Sg depending on carbon content),

    place the sample into a clean dry distillation flask. Stop the carrier gas flow and

    attach the distillation flask to the condenser, restart the gas flow, then blank for S

    minutes. Titrate the absorbent with the titrant to the first permanent blue colour. (RI)

    2. Stop the gas flow, add 2Smls of concentrated H3P04 through the gas entry port.

    Restart the gas flow at a steady rate and commence to boil with a 2.Scm high bunsen

    flame. Boil for IS minutes then titrate back to a blue end point which is permanent.

    (R2)

    3. Let the flask cool for a few minutes then add 5 grams of chromic acid through the gas

    entry port. Continue to heat for a further 30 minutes then titrate back to the blue end

    point. (R3)

    4. Stop the gas, wash and dry the distillation flask as soon as it is cool enough to handle

    as the contents solidify on cooling. .

    CalculatioDs.

    %C02 = [RrRl(mls) x 4.4] / [Wt. ofsample(gms) x 10]

    %COI'I= [R3-R2(mls) x 1.2] / [Wt. ofsample(gms) x 10]

    Nmca.

    1. Do not get any traces of moisture into the absorbent cell.

    2. Before proceeding with the determinations blank until stable, and run a known CO2

    standard.

    352

  • Appendix A.

    3. Ensure that the silica trap is blue; the soda asbestos is brown; the chromic acid is red;

    the absorbent is clear.

    4. Be careful of the burette tap. It is stiff because it must be greaseless.

    5. Ifmore than about lOmls of titrant are used the results become less accurate therefore

    repeat on a smaller sample weight.

    353

  • APPENDIX A9: RAW DATA FOR CARBONATES AND ORGANICCARBON DETERMINATIONS.

    %C02 o/oCOI'IlSample Run I Run2 Ave%. Carbonate Min. Ratios. I Run I Run2 Ave%.Call 0.12 0.14 0.13 0 0.18 0.17 0.2Ca12 0.37 0.35 0.36 0 0.1 0.1 0.1Ca13 0.08 0.10 0.09 0 0.11 0.13 0.1011 1.19 1.23 1.21 C 0.18 0.17 0.2012 0.96 1.01 0.985 C 0.37 . 0.32 0.3021 0.07 0.06 0.065 C 0.49 0.50 0.5031 0.11 0.27 0.19 S:C=1.7: 1 0.35 0.41 0.4SII 0.55 0.58 0.565 C 0.3 0.28 0.3S31 1.25 0.70 0.975 0 0.48 0.67 0.6S32 0.47 0.49 0.48 C 0.67 0.79 0.7011 5.21 4.73 4.97 S:0=5.S: I . 0.21 0.79 0.5.012 7.2 8.7 7.95 0:C==4.6: 1 0.19 0.17 0.2021 0 0 0 ---------------------- 0.17 0.2 0.2CIBI 4.8 5.28 5.04 C 14.94 15.17 15.0CIB2 1.28 2.49 1.885 C 0.45 0.87 0.7CIB4 1.77 1.96 1.865 C 0.71 0.73 0.7CIBS 0 0 0 ---------------- 0.75 0.79 0.8C21 1.1 1.6 1.35 S:C=2.27: I 7.74 7.25 7.5C31 9.58 9.15 9.365 S 1.28 1.23 1.2C41 13.85 14.54 14.195 0 3.19 2.22 2.7CSI 2.32 2.95 2.635 S:C=1.26: 1 0.40 0.43 0.4CS2 0.11 0.13 0.12 C:S-1.9: 1 0.39 0.28 0.3C61 1.0 1.0 1.0 S:C=1.82: 1 0.86 0.87 0.9C71 1.34 1.28 1.31 S:C-3.2: 1 2.35 3.6 3.0C82 5.77 5.78 5.775 S 1.02 1.38 1.2C83 2.05 1.99 2.02 S:C=3.33: I 1.70 2.75 2.2C92 5.65 7.72 6.685 S 41.96 40.98 41.5CIOI 0 0 0 ------------------- 0.67 0.58 0.6Clli 1.1 0.76 0.93 C:S-1.04: I 6.0 5.79 6.0CI12 4.31 3.4 3.8S5 S 0.92 0.66 0.8CI21 4.41 4.21 4.31 S:C==4.35: I 1.60 1.27 1.4CI22 1.44 1.39 1.415 S:C-2.1 : 1 6.2 6.09 6.1Cl31 1.04 2.49 1.765 S 9.91 9.71 9.8CI32 LSI 3.04 2.275 S 1.14 1.15 1.1cus 0 0 0 --------------------- 2.56 1.39 2.0CI41 1.92 2.06 1.99 S:C=4.21 : I 2.05 2.10 2.1CI51 1.61 1.88 1.745 S:C==4.43: 1 1.01 0.81 0.9CI61 14.11 14.28 14.195 S 6.5 6.3 6.4CI71 3.6 3.72 3.66 S:C-3.6: I 1.04 1.05 1.0CI72 2.36 2.42 2.39 S:C'"'2.21 : I 0.83 0.80 0.8CISI 1.46 1.38 1.42 S:C-I.87: 1 1.2 1.12 1.2

    C'" Calcite; 0- Dolomite; S- Siderite.

    354

  • Appendix A

    APPENDIX Al O. THE METHYLENE BLUE ADSORPTION TEST.

    Method.

    1. Prepare the methylene blue solution.- oven dry the methylene blue crystals

    (CI6HloN3SCI) for several hours at 105°C to expel water as methylene blue is

    hygroscopic. Prepare a 0.0094 N solution ie. 3.0 g crystals in 250 mL distilled water,

    then dilute to 1 L. (Molecular Wt. ofdry methylene blue is 319.9 g/mol.).

    2. Prepare the rock by drying, crushing in a TEMA mill and sieving «75f.lm) a

    representative sample. If the sample has a high organic content then pretreat by low

    temperature thermal oxidation. This involves heating the sample to 380°C for a

    minimum of 16 hours, or overnight (Keeling, 1962). Make a suspension of the rock

    powder by accurately weighing out -2.0 g of the aggregate and diluting in 50 mL of

    distilled water. Place the suspension in a water bath for 30 min.

    3. Add 2 mL of methylene blue solution to the aggregate slurry from a 50 mL burette,

    shake the solution using a magnetic stirrer for 2 min. After the first 2 mL titration

    place a drop of the slurry using a glass rod onto the edge of a piece of filter paper

    (Whatmans No. 40) if a sharp boundary between the spot and the water halo is

    evident then continue adding the titrant and allow at least 2 min of stirring. When

    after placing a drop of the slurry onto the filter paper a diffused halo around the

    coloured spot is evident then suspend the titration for 2-5 min continuing mixing,

    after this period place another drop of the slurry onto the filter paper if the halo is still

    diffused then the end point has been reached, if not then continue the titrations (

  • Appendix A

    Since the normality of the MB(methylene blue) solution is known, the net cation

    exchange capacity (CEC) can be calculated.

    CEC=[(lOO x n x p (mL. MB)] + A (g) [mEq/lOOg].

    X= Weight of dry methylene blue crystals used.

    Y= Volume of dilute methylene blue solution used,

    p= Volume of methylene blue solution added.

    A= Weight ofrock powder used.

    n= Normality of the methylene blue solution.

    356

  • AppendixB

    APPENDIX Bl. RESULTS FOR THE WATER ADSORPTION ANDABSORPTION TESTS.

    Sample Water ADI % WaterA02% Water ABI % WaterAB2% WaterAB3 %Call 0.01 0.08 0.21 0.19 0.19Cal2 0.00 0.09 0.05 0.07 0.17Ca13 0.07 0.09 0.16 0.15 0.15011 1.95 2.13 5.27 5.42 5.34012 2.67 2.28 7.37 6.69 7.16021 0.55 0.09 1.12 1.03 1.04031 0.15 0.19 2.16 2.20 2.18SII 2.06 2.04 3.89 3.90 3.97S31 0.55 0.53 2.24 2.60 2.32S32 0.13 0.11 1.12 0.63 0.91Dll 0.68 0.37 4.71 4.72 4.76Dl2 1.24 1.20 3.68 3.69 3.68021 0.73 0.58 1.37 1.47 1.44CIBI 1.13 1.19 2.52 2.72 2.66CIB2 0.95 1.00 2.36 2.34 2.32CIB4 0.81 0.79 1,49 1.50 1.51ClB5 0.54 0.61 2.42 2.37 2.45C21 1.84 1.12 6.54 11.13 9.26C31 0.78 0.73 1.74 1.87 1.84C41 1.14 1.13 7.22 6.60 6.52C51 1.68 2.10 8.85 8.79 8.82C52 0.60 0.63 4.11 4.63 4.37C61 0.97 1.33 3.92 3.96 3.97C71 1.42 1.21 6.28 5.20 5.67C82 1.99 1.98 7.00 7.07 6.79C83 0.77 0.75 3.54 3.56 3.56C92 0.20 0.30 2.40 2.43 2.41CIOI 1.62 1.49 6.05 5.87 5.86Clll 2.47 2.51 12.08 14.87 12.31C1l2 1.49 1.50 3.85 4.06 4.02Cl21 1.89 1.85 5.67 5.65 5.70

    .J2122 1.75 1.51 2.97 2.51 2.80C131 2.76 2.66 5.84 5.99 5.84Cl32 1.61 0.71 2.96 2.82 3.00Cl33 0.82 1.00 4.10 4.32 4.20C141 1.85 2.08 9.68 10.35 10.26

    vCISI l.S9 1.60 4.00 4.20 4.11CI61 0.80 0.88 6.41 6.08 6.25Cl7l 1.04 1.00 4.14 4.15 4.15Cl72 1.04 0.93 2.59 2.69 2.66Cl81 1.18 1,48 3.56 3.70 3.60.

    AD. = Adsorption. AB. = Absorption.

    357

  • Appendix B

    APPENDIX B2. RESULTS FOR THE SPECIFIC GRAVITY AND DRYDENSITY DETERMINATIONS.

    Sample Gs. I. Gs.2. Gs.3. yd. I. yd.2. yd.3.Call 2.90 2.92 2.91 2.82 2.82 2.82Cal2 2.88 2.87 2.88 2.81 2.81 2.80Cal3 2.88 2.89 2.88 2.83 2.83 2.84011 2.79 2.80 2.84 2.62 2.64 2.65012 2.82 2.80 2.79 2.61 2.61 2.62021 2.90 2.87 2.88 2.71 2.73 2.71031 2.85 2.85 2.85 2.72 2.72 2.71Sll 2.76 2.77 2.77 2.56 2.57 2.56S31 2.83 2.83 2.83 2.67 2.66 2.67S32 2.81 2.82 2.82 2.73 2.73 2.73011 2.78 2.80 2.79 2.64 2.65 2.64012 2.76 2.77 2.74 2.62 2.64 2.60021 2.76 2.77 2.79 2.59 2.59 2.59CIBI 2.30 2.32 2.31 2.20 2.20 2.21CIB2 2.73 2.74 2.74 2.65 2.65 2.65CIB4 2.76 2.75 2.76 2.66 2.66 2.66ClBS 2.69 2.69 2.69 2.61 2.62 2.61C21 2.48 2.48 2.48 2.30 2.30 2.31C31 2.81 2.81 2.81 2.66 2.66 2.65C41 2.70 2.70 2.70 2.50 2.50 2.50CSI 2.73 2.73 2.73 2.53 2.53 2.52CS2 2.63 2.65 2.64 2.46 2.46 2.46C61 2.67 2.82 2.74 2.63 2.62 2.63C71 2.65 2.67 2.66 2.52 2.52 2.51C82 2.79 2.80 2.78 2.49 2.50 2.49C83 2.70 2.79 2.75 2.48 2.47 2.49C92 1.87 1.79 1.83 1.76 1.76 1.77CIOI 2.73 2.75 2.74 2.52 2.53 2.54Clli 2.58 2.59 2.59 2.49 2.49 2.50C1l2 2.73 2.79 2.75 2.50 2.51 2.50CI21 2.77 2.75 2.76 2.57 2.57 2.56CI22 2.46 2.48 2.47 2.39 2.38 2.39Cl31 2.45 2.45 2.44 2.39 2.40 2.39C132 2.62 2.66 2.64 2.48 2.48 2.48CI33 2.59 2.60 2.60 2.49 2.49 2.48CI41 2.78 2.76 2.78 2.50 2.50 2.50CISI 2.72 2.70 2.71 2.51 2.50 2.51CI61 2.70 2.71 2.73 2.60 2.60 2.60Cl71 2.73 2.70 2.71 2.59 2.59 2.58CI72 2.71 2.71 2.71 2.61 2.62 2.61Cl81 2.65 2.66 2.66 2.51 2.51 2.50

    Gs ...Specific gravity. yd = Dry density.

    358

  • Appendix B

    Appendix:B3:PSD plots for the slake durability test debris.

    1009080

    f :J :

    10o0.001

    I i ! I iii! T : i j ; , Illi Il"iiil! i I I! I i ill I

    ,III 'i :ilI I i i I ,\ j :;

    I i I! :1 I I r i ill II 1:( i::I I, , II I iII !!III I ! 'II If i

    ,!! li,l I, I

    u i I I I I I : ; . :1" II III' I' I I /1 I I: i! i;1 iII I i I /1 ! .llil!! j I I I I I! 'i iiii i I ! I J I I· :!ii:I

    I l'llil ! I! I , I' : I 'I !, I0.01 0.1 1 10 100

    PartIcle .In (mm)

    Figure 6.1b . Sample 0.1.1. Platy and elongated shards.

    Partlele .Izt (mm)

    _ .. ) i--,._ -.·cl i,e,

    Figure 6.;2b.:Sample 0.1.2. Blocky, almondy rare platy.

    i 1OQ:·.,..:...._..,........_,..,~ ........""r""':''''t''!"I'~~-':"''.,..,.,."I''r'r:'-------..,...,.-+,...,....r'i'!'mI 9C):,,-, .....;.....1-4.,H~·~H;...y.+t+!+---+-+:4-f-f+j'*"'-...;..;.......;;.....-:-71~-f-+.;.....;...t+tffi

    .i'_"4'· :...-.!4~+#l>~F+-++4++!+-"-H*H+t+---+-----+~!-:f-+--'-+t-Httifij!~.~~~##--4#fJ++*,,""--t-'-'~*+=""~~7-4-r-+-++++Hif'i·.t:i.....44~~;.....;.p.:~++H+l-"""++-+i4+Ht-..;..:~~~---;,~+H-I+ti

    2O'."'....;;.;..,#.;....;4~~""'44++fH.~";';'O;r-+-ii'+H~:;...p;-+...:..o..r;.~IE:4+f-tttt+f

    10·r:±f~m=~::±:3Ee::TI~:tttttl1lPartIcle ••• (mm)

    FiaaJe6.3b . Sample S.1.1. Bl~ky, a1mondy and platy.

    359

  • AppendixB

    1009b80

    i:J :

    2010o0.001

    I 1 i i 11:1 , , i III1I1 i i I I1III i , , I i! II;I , , I ..j I I Ii II I I Ii j :Ili I I II 1111 I i I I l'lli, , . ! i !I i i I'll i 1111il , i I I IIiI i I I , :11i ' .

    ! I ! ! Ii 11 I I III :11 I ! 1III i i i,

    : 'ill, I ,I I I I liil I I I Illlil I , ! 1IIIi I ! I i' .' , I I ! i Ii!, I , ,. i·' , ,j I i I Ii I ! Illill ; Ii I I

    ,i i 1'1,'

    , ' II]I " I : I i I ! :.,I I I I , II i iii III II :1 I I I i! . : , , : iiiI \ Illi I

    I I , I I II I J II1II II I i I I ILl: I .,l I I, ITII ,I I II 1111 i I ! i i III i : I II i II I"Y' : I , III:1, II I i ; II!I! I I i : i ill! J 1 II il ~ii;1 , i I 'll, Ii'

    0.01 0.1

    PIrtIcIe size (mm)

    10 100

    Figure 6.4b .Sample C~l_.B.l. platy.

    1009080

    I10eo50J 4103020

    10

    , i 'Ii I j! :Iil I ill I i i /. : ; . ii'i I ii i , Ii ,11 I I i ill I , , r , I ! : '! , I ,, .

    1 il. I i ilii I I i .liJ i i : ! :1 I ,I',Ii! HTil, 1 I I Ii, ! , 1 i r :, : i1 . I , II : ii I I II /II , I :1' i I , .f,I' i , I j

    I II il i II i' I I 11 , :1 I ! , :1:I ! ,,! i if 'Iii I ' I I i II: , i , ; i Ii, i , , I

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    0.001 0.01 0.1 1 10 100

    ;:') ,Fipre 6.,sb. Sample C.1.B.2. platy, occasioDally blocky.

    *:,1, 1&1 ,III r: I iii i i ii .'. I /;

    , , \1~

    , r i i ! I , :~:, I : 101 t " 1 ,

    ,H , I til , I .1 ij4~ eo i ! r

    j 1ti I rH II iii iII i I It, I :il I 1 i:l I, . II 111 I: : f I i r I I I I jj I: i i ,;'.., ~ 1 , ;-- , I! I I t II " ./ ~ 'I:J : i , :1so , I , i' I I ~:, .' 1-: ,;~.' ~1'4j III t I , !1::'· I IJ «'.

    ··,[,,-1; , ! i "

    :'Ht!1 1',-. ! , : II t II }I\" : I: '. I , i , 1130 _",- ,..+- ....""7-t(: ft-.... t 1TI, , -- ! I , YI! ,. i I20, , I ,; ~ !.-:;; I I !

    ,.111" Iii :1 i. , ilt/' I i j I ' .10 , , . ~l : , : ! ,

    i I i 'F';"4 t.'I14H1 !, ,

    ; .:0 i : 1 I; i , I ;

    0.001 0.01 0.1 1 10 100

    Fp 6.6b.Samp1eC.1.B.5.Blocky and almondy.

  • AppendixB

    10090

    ! ii' ';! ,; I,

    i , III80 . ,·1 I

    I70, :' 'j i I !k

    I,: ; I, I!!eo l: I,:, ' ' , I! i Ii50 I;;

    JI;'! I ; ! I40 ,

    30 i ; Ii II I j i I [I20 I i i ~: i : ; ! J TI r !10

    T , UH ! ! I I i:10 I ' ' !I iii 1 T[0.001 0.01 0.1

    i lIt I I !TIlll' ! I IIT I I I iii: 1;,11 .. !IlI rr 111 I ! i : i; tli ! i ! ii', ,L,' I'\'

    I~ .I f i :: ill l i i:;'

    'I

    I

    1

    PartIcle .tze (1ft ... ,

    ~ ! I i l : : i in ii, I '!

    10 100

    Figure6.1b . Sample C.2.1. Platy and elongated.

    I 100I

    I : II80 :; "80 :'

    f! ; i ::170

    eo :50

    ! II.

    J

  • AppendixB

    1001 Iii! ,

    •iii iii i!il 1 ! ~I

    ,: )!

    90 I l l i r, : ,

    I , I i IT " i 1 !!I, , II 1 ~:,i i,

    i i i.'80 , ,

    f 70 !! i I ! ii, I ! : III I!III I [1 \ : :i ! 1 r Ii :1,

    i r I; ! :'! 1 1:1 I; I :il! I 1 I ! ;1; i Ieo i I , : ,I i ' I , I i i]!' I~ i i ~; ! i i I ! !50 , , l j " I' " !

    ,

    I, i i i i I ! iii I! i ~ 'I dl I ii i 'iii ! !40 i ,~ !! : ,i I , i I II! If! __vr i I I I I

    , ! I , fl:30 , ! 1 ~ i,

    20 ! ! " i u..H"i 'j ! : I I ! !!: :'1I ! : i~ ; ,t

    I I i iJJ ~ , iii! , i ! 1 i, : !li !

    , I ,; I:

    10 ! i " jl !

    0 ~lrr 11 ! i I IT I i II iii! I i i I! ii0.001 0.01 0.1 1 10 100

    PMIcIe ea (m...)

    Figure 6.1Ob. Sample C.S.I. platy.

    100 ,i 1:1 I , I ! i Iii! i I I i !1Lif.T' i i80 I I .:

    i !, ; i !I I I ; I;,!: I Iii

    , I ill, ;~ i80 I

    I i ! '!i,' i !; i:PI I !L 1 P" I : :10 , I ;,ly

    Ii I' 1: i ::,: ! : II id TI! I i;'it I , : ,80 ,, IT! i I 1 , : I , ! i :Iil' II i I 'j ;j I i I I50 , , . ,: ,

    I; u : I I ill ; : Ii 11 ! !i i40 , i ! !!! ! i ,i:1 i ,I II!! I

    , I ' , 'I: ; i' ,30 , ! i i I I, I t ! i i i ;! II I ILl: ! /: 1 Ii20 , : i i I,i I ; i , ' I I I llil ! u '!I / ; i I ! if I10 ,I , :1 Iif , il I i i i IIII i I i~,~ II I :1 " j

    ,I

    0 ; , f f I0.001 0.01 0.1 1 10 100

    ......... aC"'...'

    Fipn '.llb .SanlpleC.S.2. Platy.

    1~~~ ~~ ~-- ~ __ ~~----------~J ii: i ;..l! ! i i ,I i'8O~~~~~--~~+H~~~H4H#--+-~~~~~~~Ii 'l I;' ;.r-~++~~~~~~~~+H~--~~-+~~~~~

    I10 ,,': rT Ii ,i,' ii" ;,' I' 'i, i, ",;., ': ,,'" u ,'1:1:1: ,:::,.' SO !,J!! :;11" il: I ! ,1:li/ i1;11I'402030 ,I , 'Ii I I ' il! !, I I ~ Ii :,,i:• ;::t Ii 1; i: Ii; l..l 1,1 ,/: I:, :Jil : ;·rrP

    ; I 11 II I ! ! :' 'il T: 'i! I! I I , ;:!! ' ': I ji! .:

    1, ! r , I I, : ill ' I,,

    I'III

    362

  • r-------------------.--------------------------------------~II· 100

    r • 90Ii 80I

    I f 7080I 50II J

  • Appendix B

    I 100I ' ' I'

    ,r I : I ! ! I if I i ! \: l!ll i i :: iii90 ,I , , i

    I 'I I I T ! i I i: i III I :: ilI 80 • i i' I ! I ' I" ,i:i! I i I I ! ! !! I ,'I : i I U

    It 70 , i i i 111'I i ' 'IH , i 11 : 1 I I i I: i! i(, eG ; 1::1 I, :::\! I : l : I, i I ,I I;! i I

    I50 , ! I , i

    1: iI ! ~; ! i I , i I , 'Ii I , iii' I ! I II4() , ,

    1 3C) I i , i!l!! f ! : 11!, , I i I I ,v' !: !!II! i I ! 'I'il : I Ii] Vi i i: i I ii2Q ! 'I , , ,I I i!11I : i 1 i II i I I 11 ;j10 I0 ~;I I I TIT I , j , ! II Ii0~OO1 0.01 0.1 1 10 100

    Figure6.16b. Sample C.9.2. Platy. occasionally blOCky.

    100Ilii I i I 1111 I ! i I ! ; : II Iii I i I : ~!to i:" I:!;ij i : Ii I II I

    ,I i illii I I ! , i :l!80 I

    f 'IQ' ,: 1i i II I, ! , I :!i: I i ii,, ,

    i , ; , 'r ! !, IT ! I filii I I i ' ,eo , ~ .i I

    I I ; Ii:! I I ! II; , ! : i if,ill I : , ! ill., , , ,J ,i:ii

    ! 1 !iIi,

    'I i II I til I : ,!i40 I I It Ii r ,j:;i I i I I ,i l"/ , I , , 'I30 : I , I': ::: , I I ! i ! I r :: i;ito /: , , I I' ;;! : I',::1 iii Ii ! ! j i'ii' , t I I I Ii,10

    I ii'·1 ,'It· " i! I, ! I i i tj! : f

    ,0 40.001 o.Ot 0.1 1 10 100

    1WtICIe,11ft,(mm)

    Figure 6.17b.,,5ampIeC.IO.l. 810Cky aad platy.

  • AppendixB

    Figure 6.l9b. Sample C.Il.1. Platy aad shards.PIaty mudstonelalmondy siltstone.

    tOOi , l:l:! ! , if!1 ! I:: I

    ,i ! !Vl ' , II!80 , i i " ! I'

    I !iil. ; I: : lIT I Ii , i n ' I'80 1 I I·· "1 :'!:! ! i!: I i, I i I' I , .1

    f 70:. i r d u :i!

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    10 : !, : , 1 , , !I!

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    I; iTiii : , ' ~! i I n 1 I Ii , , !

    "40, 1

    : i !!II! ' i ll i ii, Vi I / I il. t ii:., ,i I :!In , !) ;1 ! :'1: I ! , !W ::i20 , 1 illi ! II Ii! ! , :1'1 I I u.v 1 i i I! , ' 'Ii,0 , 1 , 1 :!IiI, : I,'" I 1 . .1 jI I'! J ~T;j! I' ! ~:0 , ,

    0.081 0.01 0.1 1 10 100

    ..,......(...)Fi&Ul'-6~ •SImpleC.U.l.Pllty IIld shards.

    r!rit .

    !

    ~I (fiji I ::Ii III I ~II ;ji ::il i: li'I,: i "1

    ; 1 ir~l r : lll .1 i : in7 I: : ij;1 :; i'iT i ! l!i': ; I! ! J v! ;: i.:!; i ~I :; I ~

    ii, n 11 i;'1 iT ! j 11 •.. l lJi; :: I i r1111 ;Xl, I " '. :1,

    I ·i' I.: L!! i 1 i ,:./ :;: ;II I!', ,IT!frlT,·r l.:.:J',i,!!I:j ::',i'

    1 1

    II

    1 10 100

    t·II. L~ ~ __~~~.~~ __~ __-- __--~~--------------------~

    ,',-.,_.

  • AppendixB

    II 100II

    I iii!' i .: ;!! 'i':ii I Ii; "j 90 I III 80 ; ! I: ' liii I I ; I ii I I V:" III i :ji! 1I ! I : : I nr I 1III 1/1 ,Ii: i I! ;:1I I70 !eo i , i r::; 1II J. ! ! ii:1 ! , l: 1;150 ! I' 'ilii I :: i il Ii i I illl i I i 1 ;!!i , i ' , "j

    J

  • AppendixB

    10r-~i~i~ll~II~#-__ ~~I~'-;~II;__ ~!L~I~I~II~4-~~~~~I+~1.o~~i__,~!.I~rd~I~'~~i.il~T~~~T~1~!~I~L:l~~~~~~~ruir~0.001 0.01 0.1 1

    PartIcle .Ize (mm)

    100

    Figure 6.2Sb. Sample C.14.1. Blocky and platy.

    100r-~~~~~~~~~~~~~~~~~~~~90 +--+-+-' ....! ~; i+: :i+,-' __ +-1 -+;.i;~;I;,_' -+-+i -Hi !-+' ++i lti-II__ 1-1+i -+i'1-' ++' '+t' i if-:i ._I.~4-'-ji:..,lh':"'!"". t+tI' i :I~r--1i~:T-j'IH+,I~i, __ ~:-+!~~:*,ll-i~_+;~il-+I~II!__ !l-+i-+I+·~:i~!~~+I-1I~!h,+:~iil

    I807050.L.._"""-.,.._' -1' f+i f.;..' __ +-1-+T-+-' -,,' ....: 1,....1 --+'-t-Mli-+++!' !~:!__ '~! ..;.1 ~i++,:J,1+I~II--+:-ji....,'-+'....' H+j! ~:y- "II i; I I l IT, T ;; ; ,'i I I Jrl :Ij I j 1 !, iI; ;, Ii' ! : I ,:;'1 ! I iii, . » ::11', I! i j,il11 10 100¢1

    ,.,... alze (mm)

    Fiaure 6.26b . Sample C.lS.l. AJmondy to blocky. occasionally platy.

    IIIIIcJ

    III.1<

    1C1O "80 !',:; i: i: i,: :1: I Ii ! ii'';;'1" ~!,I Hii:·,,!!lliI1F 1!lil I70 .:!; r: [ii, r:i ,p, 1 i i llleo"'" ',!i:T , : ! i!' ,I: , i I !5Ot~ :: filii ;ril, 1 Ill'if!!40 k;; !. j WfI;,j; ! III III!30 ~;;IIi:, I,' l,nll! ! I !1

    '\' .. "jq, I ,n; j.I'j I, I20 : " , ,"ii,10';1' i :," in'Hi ' I

    '''.; ..y,'" ,,1,'1:' , , .1,0: ~---' I r ! ~'l: .1 f ; I !- i, l

    0.0011 O.lL~!c; 1........ ·.IU(mM)

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    : 1_ 1 : j

    ; It 11 Ii: i' i I:

    .j' U

    1 J .IA1Hl10 100

  • AppendixB

    1oor---~~~--~--~------~~~----~~ ~9Ot--+~!_i~il~'!~;I~!__ ~~i _,~:~,~;__ ~~iJ'~i~:I*i!__ 41-+'4!+:+':~'+!'__ +-~:++I~' ~~r--+~I~:I~!~T':__ +-~~'~1:7:__ ~~I+!4!I~q__+-I~'~li!_'~:iLi ~-+~!,~!~:70 +----t--+-:"j-I,t-:t-I, ...,'i+-1 __ .__!_~I' ..,.,-''~ ~i-+i I++I,""+-!!__ .L;+i..J..i.,_1'....' :....: _ _._iL.l+li'-+'.:...j'80 -f--+-+ .........I, 4' ff';--' i,~'_,''_'i_-l--+-;:JI..J..i ! '-4+I:!--+--i-I+' +' +,'-l.+--_'_'_'_! "-,I !..l.l~!i50+--+-+-" ....,It-!~Ii~lt-'__ ~~~~'~-l-~14i~i+'~I,*!I __ _,_~f+!+:~li~!i..J..i__ ~iH-'~I-+'~!1~~~~:~i+ll~i~:! __ ~~~~~4'~!-+!+i'~"~i','__ ~ii~I'!T,,~li~:__ ~~i~,~:!i30 r--+'-+-' ,_iHi'H-! l+tII:-!, __ y_,l-i,'---'-;+----r-+, -+'-+: ~!I"i-i! __ +' .L+i +' +-I' '+:; '+I, ~ ...~' ....j'__L.1W' :_j..I;...j:'~r_-r++!+i~lrt,:!r_~t_i~!,~,~'4!1--+;~I~i4!+II~'~ii--I~I~!+I++;:~:j~I!~~'~I~i'~i'~i~i10

    0t=t:!!:t111tT~I,!l:, ::!1~T~ti' ~I ';' 'g;'! ~!~I± i!~!I~i:~II:::crli='it II,,:"Jj~I' "'it: :,,=ttil!r! :11,~·:\ 1 I I ,:, I 1 , I . j r i :-rr[

    0.001

    iI

    I i! II J

    0.01 0.1

    Particle .Iz. (mm)1 10 100

    Figure 6.28b . Sample C.17.1. Platy, elongated occasionally blocky.

    10090 I f I iI'80 i

    1 :!,

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    "

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    PIrtle.. liz. (mm)

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    10 100

    I I j

    Figure 6.29b . Sample C.17 .2. Blocky, aImondy, occasionally platy.

    100" ,. II iiiI , : I :80 I:: ,

    i : .;' Ii I! ii!~ ,j ! I ! 'I!

    f 70; ; ,

    i , I I ! 1 I ~II80 , I I i"50

    I 1[: I, , I 1 ! :','I'i I" !,il I :iII i'l, !

    ~ i I ;

    30 I , , ''I , i , i ,'I,I

    ,:1 :ij~ I ; I "

    I : r I j "10, " ~i : ~ ; 11 Ii' ._..._ I I I 11 0110 ,

    0.001 0.01 0.1 1

    PIrtle .. liz. (mm)

    1 I I I! :i I I 1:'"i:ii' '! I,':I 'J ,

    I I, :"" I : , '! I,1 ; :, i' ; i I I 'ii',: ! i:i

    '-.., ,I, ': ,

    10 100

    FilUle 6.3Ob. Sample C.18.1. Almondy.

    368

  • Appendix.B

    APPENDIX B4. TRIAXIAL SWELLING TEST PLOTS.

    0.0090.0080.007

    I0.0080.005I0.0040.003

    0.0020.001

    00

    YlZaxis

    1000 2000 3000

    TIm. (mm)

    4000 5000 6000

    Figure 6.31b . Sample Ca.1.1.

    0.025

    0.02

    i i 0.015....I 0.01eo

    0.005

    00

    0.040.04O.~

    I 0.030.025J 0:020.015

    •.·0.01O.oat

    00

    ___ Xaxis-B

    VIZ axis

    100002000 4000 6000 8000

    TIm. (min)

    Figure 6.32b . Sample Ca.I.2.

    2000 4000 6000 8000

    TIm. (mm)

    Figure 6.33b . Sample Ca.1.3.

    369

  • Appendix B

    1.4 Yaxia-B

    1.2

    1

    i 0.8 X axis-I0.80.4 Zaxis0.2

    00 50 100 150 200 250 300 350 400 450

    TIm. (min)

    Figure 6.34b . Sample 0.1.1.

    1 Xaxia - B

    0.90.80.7

    I0.80.5J 0..40.3

    0.2 Zaxis

    0.1 Yaxis00 200 eoo 800 1000 1200 1400 1600

    TIm. (min)

    Figure 6.35b . Sample 0.1.2.

    1 Xaxia - B

    0.80.10.7

    I 0.8.".... 0.5I0.40.3

    0.2 Zaxia

    0.1 Yaxia00 200 400 eoo eoo 1000 1200 1400 1600

    TIm. Cmin)

    _.4 ____ -

  • Appendix B

    0.180.16 Xaxis- B

    0.14

    I 0.120.1J 0.080.06

    0.04 Yaxis0.02 laxis

    00 1000 2000 3000 4000 5000 eooo 7000 8000 9000

    TIm. (min)

    Figure 6.37b . Sample 0.3.1.

    I1.4

    1.2Xaxis- B

    I

    I1

    I 0.8I I

    0.8

    0.• Yaxis

    i 0.2 laxis!i 200 400 600 -800 1000 1200 1400 1600

    TIm. (mm)

    Figure 6.38b . Sample S.I.I.

    0.460•• Xaxis- 8

    0.35

    I 0.30.25I 0.20.1a

    0.1 laxis0.0$ Y lXis

    00 1000 2000 3QQO 4000 5000 6000 7000 8000

    nm.(mln)

    ._-_-- _-_--_.-Fi&un:6.39b. Sample S.3.1.

    371

  • Appendix B

    0.035 X axis - B0.03

    0.025

    I 0.02.& 0.015i 0.01

    0.005 ZaxisYaxis

    00 1000 2000 3000 4000 5000 6000

    TIm. (mm)

    Figure 6.40b . Sample S.3.2.

    0.7Z axis - B

    0.6

    0.5

    I 0.4...t 0.3CIO 0.2

    0.1 X ax.Yaxis

    500 1000 1500 2000 2500 3000 3500 4000

    TIm. (min)

    Figure 6.41b. Sample 0.1.1.

    0.9 X axis - B0.8o.r

    rI 0.8O.S-J 0.49·3O.~0.1 YIZ axis00 1000 2000 3000 4000 5000 6000 7000 8000 9000

    TIm. (mm)

    Figure 6.42b . Sample 0.1.2.

    372

  • AppendixB

    373

  • Appendix B

    0.45 ~

    0.4 .:. Xaxil- B0.35 .1.

    - 0.3 .;_I 0.25 +-J 0.2 +0.151 i0.1 t Yaxil

    0.05 Zaxil01

    0 500 1000 1500 2000 2500 3000 3500

    TIm. (min,

    Figure 6.46b. Sample C.l.B.4.

    1.S

    1.8 Z axil- B1.4

    - 1.2I 1I0.80.8 Xaxis

    0.4 Yaxis0.2

    2000 4000 6000 8000 10000 12000 14000 16000

    TIm. (min'

    Figure 6.47b . Sample C.I.B.S.

    3.5 Xaxil- B3

    2.5

    I 2-I1.51Yaxis

    0.5 Z axil

    tOOO 1500 2000 2500 3000

    TIm.(mm,

    ._----Figure 6.48b . Sample C.2.1.

    374

  • Appendix B

    1.2

    X axis

    I0.8

    0.6c:J 0.4(I)

    0.2 YaxisZaxis

    00 500 1000 1500 2000 2500 3000 3500 4000 4500

    Tim. (min)

    Figure 6.49b . Sample C.3.1.

    1.2X axis - B

    j 0.80.6

    I0.40.2 Zaxis

    Yaxis0

    0 200 400 600 800 1000 1200 1400 1600 1800

    nn. (min,

    FiJure 6.s0b . S8IIlpieC.4.1.

    1.61.4

    I1.2

    1.0.8

    I0.60."0.200

    Yaxis-B.

    X axis.

    Z aOcs.

    800

    TIm. (min)1000 1200 1400 1600

    Fipre6.S1b. Sample C.S.I.

    315

  • Appendix B

    0.40.35

    - 0.3E 0.25- 0.2.& 0.15S 0.10.05

    00

    __ ----------------- Xaxis-B.

    Z axis._------------------Yaxis.

    1000 2000 3000 4000 5000 6000 7000 8000

    TIm. (min)

    Figure 6.S2b. Sample C.S.2.

    t.61.41.2

    I 0.8I0.60.4

    0.200

    Yaxis-B.

    ~-_---------------- Zaxis.X axis.

    500 1000 1500 2000 2500

    Tim. (min)

    Fipe 6.S3b . Sample C.6.1.

    2'.5

    2

    IJ 10;5

    00

    _--------------------- Yaxis-B.

    Zaxis~------------------------------ Xaxis.1000:. 2000 3000 4QOO 5000 6000 7000 8000 9000

    l'IIn.(mIn,

    --,_.'--- #'ipn 6.S4b . Sample C.7.1.

    376

  • AppendixB

    43.53

    I 2.52.s 1.5i 10.500 1000 2000 3000 4000

    TIm. (min)

    5000 6000 7000 8000

    __ ------------------ Xaxis·B.

    z axis.__ -------------------------------------Yaxis

    Figure 6.SSb . Sample C.8.2.

    0.350.3

    I 0.250.2J 0.150.1

    0.05

    00

    __ ----------- Yaxis.z axis

    4000 6000 8000 100002000TIm. (min)

    Figure 6.S6b . Sample C.8.3.

    0.40.35 ~_--------- Xaxis·B.0;3I0.25 .

    .. 0.2I0.150.10.05.O~_.=====;===:::;:===;::==:;::==:::;::=-----.

    o

    Yaxis.laxis

    8000 12000 1400010000

    Figure 6.S7b . sample C.9.2.

    377

  • Appendix B

    2.5

    2

    I 1.5II

    I0.5

    00 1000 2000 3000

    TIm. (min)

    4000 5000 6000

    ~ --------------- X axis·8

    ::================== Yaxis/. Z axis

    Figure 6.S8b . Sample C.IO.I.

    6

    5

    I43i 2

    1

    00

    r--------------------- Xaxis·8

    Yaxlslr-------------------- Zaxls

    500 1000 1500 2000 2500 3000 3500

    TIm. (min)

    Figure 6.S9b . Sample C.II.I.

    0.35

    0.3

    0.25

    t 0.2...I0.150.1

    O.OS

    q

    _.,. X axis·8

    Yaxis~2_-:~~~~~~~::::::::::::::::::::::-:Zaxis

    2000 2500 3000

    TIme (min)

    Figure 6.60b . Sample C.ll.2.

    378

  • Appendix B •

    3.5

    3 X axis· B

    2.5

    I 2J 1.51 Yaxis

    0.5 Zaxls

    00 500 1000 1500 2000 2500 3000 3500 4000

    Tim. (min)

    Figure 6.6Ib. Sample C.12.1.

    0.8 X axis • B0.7

    0.6

    I 0.50.4J 0.3

    0.2 Yaxis0.1 Zaxls00 1000 1500 2000 2500 3000

    TIm. (min)

    IFigure 6.62b. Sample C.12.2.

    ,2.5

    X axis • B2

    I 1.5I,. 1

    0.5 Yaxis! Z axis

    0(j 500 1000 1500 2000 2500 3000

    nne (min,

    ;".-------- Figure 6.63b . Sample C.13.t.

    379

  • Appendix B

    0.9O.S X axis - B

    0.7

    I 0.60.5-I0."I

    0.30.2

    YaxisI 0.1I' Zaxisi 0I 0 1000 2000 3000 4000 5000 6000 7000 8000 9000

    TIm. (min)

    Figure 6.64b . Sample C.13.2.

    0.9X axis - B

    0.80.7

    I 0.60.5 Zaxis....I0.40.3 Yaxis

    0.20.100 200 400 600 800 1000 1200 1400

    TIm. (min'

    Figure 6.6Sb • Sample C.l3.3.

    X axis - B

    II,1.$1

    0.5oL.~~~~~~~~==~~~~o

    Yaxis

    Zaxis

    eoo eoo 1200 1400100011m. ("'in)

    ~ _ .. -~---.-._._.--- -Figure 6.66b . Sample C.14.1.

    310

  • Appendix B

    0.45 X axis - B0.4 laxis

    0.35

    I 0.30.25 Yaxil-i 0.20.150.1

    0.050

    0 2000 4000 6000 8000 10000 12000 14000 18000

    TIm. (min)

    Figure 6.67b . Sample C.l 5.1.

    0.160.14 X axis • B

    0.12

    I 0.1 laxis0.06J 0.08

    0.040.02 Yaxis

    00 500 1000 1500 2000 2500 3000

    TIm. (min)

    FIgure 6.68b . Sample C.16.l.

    0.9 X axis - B0.80.7

    i 0.80.5I0.40.3 laxis

    0.20.1 Yaxis00 500 1000 1500 2000 2500 3000

    TIm. (min)

    ----------- Ficure 6.69b . Sample C.17.1.

    381

  • Appendix B

    382

  • Appendix C

    APPENDIX Cl : Roof weathering experiment ICP-AES chemical data.N."... Weathering,C1B1-1 (ppm)

    Alsjstad WMIIwlngC1B1-1 (ppm)

    AJ ca Fe SI AJ Ca Fe SIS.95 33.8 321.6 4857,7 15,5 Aug-95 3,2 7.0 3,0 3,8

    Oct-95 13.6 161,5 1288,5 7,6 S.95 69.7 504.0 5957.0 35,5

    Nov-95 0.6 48,1 129.5 0,9 Od-95 19,7 137,0 1046.0 11,0

    0ec-95 1,7 18,5 138.7 1,3 Nov-95 47.5 255.5 3194,0 22,4

    Jan.96 0.4 12,7 74.5 1.3 Dec-95 10.9 519.0 71.5 5.1

    Mar-96 0.1 6.4 8,8 2.8 Jan-96 2,4 11,6 67.0 2.0

    Jul..96 0,9 20,9 60,8 0,0 Mar-96 10,2 43.6 119,3 9,4

    C1B1-11 (ppm) C1B1-11(ppm)

    AJ , Ca Fe SI AJ Ca F. SIS.95 ,~1,2 84,5 4.8 1.3 Aug-95 1.08 13.04 3.75 1.06

    Od-95 23.0 204.2 813.4 10.3 S.95 59.66 269.99 2960.1 27.28Nov-95 3.4 57.5 124,4 1.5 Od-95 2.37 87.10 78.20 2.90

    0ec-95 4.2 43,3 140,8 3.0 Nov-95 1.74 17.30 52.60 1,98

    Jan.96 1.4 13,1 58.3 1.3 Dec-95 1.41 12.02 28.35 1.80

    Mar-96 2.3 15.8 20.4 185.7 J.,..98 0.98 8.35 23,52 1.35

    ~Jul.96 3.7 27,0 129,7 1.0 Mar-98 2.19 8.44 28.68 2,91

    C1B1-111(ppm) C1B1-111(ppm)

    AJ Ca F. SI AJ Ca Fe SISep-95 54.175 131.457 1360.28 14.56 Aug-95 0.711 7.334 4,8997 0,834

    Od-95 28.33 96,5 1399 18.52 Sep-95 9,9598 30.932 279,009 4.0758

    Nov-II5 9,3 23.06 371.9 4.117 Od-95 3.856 27.41 318.8 4.915

    0ec-95 8.97 25.35 424.7 5.03 Nov-95 4,284 20.83 261.5 2.188

    .Ifn-9I 2.902 9.33 129,7 2.937 Dec-95 2,179 8.1 107,9 2.216Mar-ge 5.08 16.02 218.8 193.9 Jan.98 2.981 26.73 208.8 3.838Jul-96 3.978 17,81 210.9 3.97 Mar-96 0,899 6,85 18.58 1,884

    C1B1-1v (ppm) C1B1-1v (ppm)

    AJ Ca F. SI AJ Ca F. SIsep.95 .. ' 2.425 34.038 3.454 2.858 Aug-95 3.106 22.04 2.3487 3,748

    Oct-95 1.458 45.38 1.• 2.522 Sep-85 2.832S 20.1818 5,0573 3.7062

    Nov-95 0.586 20.08 0,828 1.031 Oct-95 4.244 61.8 5.58 6,03

    Dec-95 0.728 27.79 0.738 1.148 Nov-95 3,385 19,58 2,789 4,395

    JM.88 0.4325 8.03 1,016 0.78 Dec-95 2.606 15,59 1.514 3.393

    Mar-96 0.501 8.51 0.471 31.97 J.,..96 3.255 18.81 1,945 4.137

    Jul.1l8 0.0125 3.438 0.856 2.895 Mar-98 1.88 1.65 1.74 15.59C1B1.., (ppm) C1B1.., (ppm)

    AJ Ca F. SI AJ Ca Fe SiSep-85 5.03 95058 48.54 2.718 Aug-95 1.9416 10.1328 48.6332 4.091

    Od-95 1.327 41.54 57.8 2.009 S.95 0.277 7.2118 11.3758 0.4204

    Nov-95 1.187 35.88 35.92 0.983 Od-95 0.813 43.48 18,12 1.023

    Dec-95 0.3414 4.588 8.08 0.351 Nov-95 19.n 50.95 84,3 32,9

    Jan.88 0.1571 2.431 2.524 0.3749 Dec-95 0.957 5.985 8.395 1.6215

    Mar'" 1.402 50.4 47.78 192.S J.,..88 0.466 3.964 1.055 0,396Ju1-88 0.787 14.4 17.48 4,388 Mar-98 1.25 23.98 11.27 200.8

    C181oN8t.(ppm,/IJ ca Fe SI

    _95 0.373 5.256 0.151 0.8548

    Od-95 0.0299 1.9203 0.014 0.5825

    Nov-95 0.0447 4.087 0.0013 0.27490ec-95 0.1567 3.894 0.0027 0.4748

    Jan.96 0.0593 2.178 0.0057 0.4535

    Mar-96 0.087 4.025 0.0013 26.25

    JuI..88 0.1192 5.58 0.2172 2.167

    .ISEYi•HCI treatment.U• HNO, treatment.II• Citric acid treatment.Iv.Calgan solution treatment.V. EDTA treatment.Nat.• Naturaly weathered sample.

    383

  • Natural Weathering.C21-1 (ppm)

    AI Ca

    384

    Appendix C

    Assisted WeatheringC21-1 (ppm)

    AI Ca

    KEYi=Hel treatment.II = HNO, treatment.iii • Citric acid treatment.Iv • Calgon solution treatment.v» EDTA treatment.Nat.= Naturaly weathered sample.

  • Natural Weathedng.C31-1 (ppm)

    AI Ca Fe Si

    Appendix C

    ASSisted WeatbedngC31-1 (ppm)

    AI Ca Fe Si

    385

    KEYi= HCI treatment.ii = HN~ treatmentiii = Citric acid treatment.iv = C8Igon solution treatment.v = EDTA treatment.Nat.= Naturaly weathered sample.

  • Natyral WeathedngC83·1 (ppm)

    AI Ca Fe Si

    Appendix C

    Assisted weatheringC83-i (ppm)

    AI Ca Fe Si

    386

    i= Het treatment.ii = HNC, treatment.iii = Citric acid treatment.iv = Calgon solution treatment.v = EDTA treatmentNat.= Naturaly weathered sample.

  • Natural WeatheringC92-1 (ppm)

    AI Ca Fe Si

    "ppendix C

    Assisted WeatheringC92·1 (ppm)

    AI Ca Fe Si

    387

    KEYi= Hel treatment.iI = HN03 treatment.iii = Citric acid treatment.iv = C8lgon solution treatment.v = EDTA treatment.Nat.= Naturaly weathered sample.

  • NirturalVV@i¢hedngC133-1 (ppm)

    AI Ca Fe Si

    Appendix C

    Assisted WeatheringC133-1 (ppm)

    AI Ca Fe Si

    388

    KEYi = Het treatment.jj = HN~ treatmentiii= Citric acid treatment.iv = catgon solution treatment.v = EOTA treatmentNat.= Naturaly weathered sample.

  • Appendix'C

    Natural Weathering.C141·' (ppm)

    AI Ca Fe Si

    AsSisted WeathedngC141·' (ppm)

    AI Ca Fe Si

    iii = Citric acid treatment.iv = Calgon solution treatment.v = EOTA treatment.Nat. = Naturaly weathered sample.

    * = No sample obtained for analysis.---r.'~id-""""_-+ __ -f"""'~~+-":I""'l,,,...-t - = Sample removed from testing.

    389

  • AppendixC

    APPENDIX C2: Roof weathering experiment ICP-AES data plots.

    Aluminium concentration of the leachates 1 month after chemicaltreatment

    60.0

    I 50.0- 40.0ci 30.020.08 10.08 0.0

    Sep-95 act-95 t-ev-95 Dac-95 Jan-96 MElr-96DIle.

    _....__C1B1-i.•. []. .• C1B1-i__.._C1B1-ii_. +-. C1B1-iv_ .•. _C1B1-v

    --e-C1B1-Nal

    JuI-96

    Figure C.I. Aluminium concentration of the leachate from sample CI B I. 1 month after reagent addition.

    Calcium concentration of the leachates 1 month after chemicaltreatment

    350.0~C1B1-i

    I300.0 _____ C1B1-i250.0 •• "A" •• C1B1-ii

    J200.0 _. ~" C1B1-iv150.0 _ ••. _C1B1-v100.050.0 --e- C1B1-Nal

    0.0-..._

    Sep-95 act-95 Nov-95 Dac-95 Jan-96 MElr-96 JuI-96DIle.

    Figure C.2. Calcium concentration of the leachate from sample CIBI. I month after reagent addition.

    Iron concentration of the le.chate.1 month after chemical treatment

    390

    5000.0

    I 4000.0-

    J3000.0

    2000.0

    1000.0

    0.0Sep-95 act-95 Nov-95 Dlc-95 Jan-96 MElr-96 JuI-96

    01•.

    --+--C1B1-i...... C1B1-i_ _._ _C1B1-i

    --.oM- C1B1-iv_ ••. _C1B1-v_ ..... C1B1-Nat

    Figure C.3. Iron concentration of the leachate from sample CI B I. I month after reagent addition.

  • AppendixC

    Silica concentration of the leachate.1 month after chemicaltreabnent

    I200.0

    1SO.0-c:

    J100.0

    SO.O

    0.0 ..•-Sep-95 Oct-95 Nov-95 CIc-95 Jan-96 Mar-96

    om.JuI-96

    ....... C1B1-j_ ......._C1B1-i

    --..- C1B1-ii_.,.._C1B1-iv

    1------C1B1-v_ .... C1B1-Nat

    I~------------------------------------------------------------------~Figure C.4. Silica concentration of the leachate from sample Cl B 1. 1 month after reagent addition.-l

    I

    Aluminium concentration of the leachate.24 hours after chemicaltreabnent.

    i70.060.0- SO.O

    j 40.030.020.010.00.0Aug-95 Sep-95 Oct-95 Nov-95

    om.Dec·95 Jan-96

    --+-C1B1·j I_ ......._C1B1-i

    ....... Cla1.. I_.,.. _ C1B1-1V

    _.lIG-. C1B1-v

    Mar-96

    Figure C.S. Aluminium concentration of the leachate from sample Cl B 1. 24 hours after reagent addition.

    Calcium concentration of the leachate.24 hours after chemicaltreabnent.

    I~OJ500.0- 4100.0J

    300.0200.0100.0

    0.0Aug-95 Sep-95 Oct-95 Nov-95 Dec-95 Jan-96 Mar-96

    0....

    --+-C1B1-j_ ......._C1B1.i

    ....... C1B1-ii_.,.. _ C1B1-iv

    _ .lK-. C1B1-v

    II

    I

    L-- JFigure C.6. Calcium concentration of the leachate from sample C lB 1. 24 hours after reagent addition.

    391

  • AppendixC

    Iron concentration of the leachatea 24 hours after chemical treatment

    6000.0

    I 5000.0- 4000.0I3000.02000.08 1000.0

    0.0Aug-95 Sep-95 Oct-95 ttw-95 0ac-95

    Date.Jan-96 Mar-96

    _._C181-j

    _~_Ct81.ii I

    ••••••• Ct81-ii

    _. K-. C181-JY

    - .Il. _Ct81-y

    '----------------------- __J

    Figure C.7. Iron concentration of the leachate from sample CI B I. 24 hours after reagent addition.

    Silica concentration of the leachate.24 hours after chemicaltreatment

    2SO.0

    I 200.0-

    J1SO.0

    100.0

    SO.O

    0.0Aug-95 Sep-95 Oct-95 ttw-95

    Date.Jan-96 Mar-96

    _ ...... _C181-j

    ....... Ct81-i_ ...... Ct81-JJJ

    1_·*·_C181.iv___ C181-Y

    Figure C.S. Silica concentration of the leachate from sample CIBI. 24 hour after reagent addition.

    Aluminium concentration of the 'eachatea1 month after chemicaltreatment

    I700.00800.00500.00

    J400.00300.00200.00100.00

    0.00Sep-95 Oct-95 ttw-95 Dlc-95 Jan-96 Mar-96

    Date.

    _ ...... _C21-j

    ....... C21-i__.__ C21-ii----- , I

    I!I

    II

    I:i

    I

    _.*. _C21-JY_.IK-. C21-Nat

    Figure C.9. Aluminium concentration of the leachate from sample C21. 1 month after reagent addition.

    392

  • AppendixC

    Calcium concentration of the le.cha.8i month after chemicaltreatment.

    Oct-95 Nov-95 Dec-95

    1liIa.

    Jan-96 MElr-96 JuI-96

    _ _..._C21-i

    ~C21-i••••••• C21-ii_. K ._C21-;"_ ..... C21-Nat.

    Oct-95 Nov-95 Dec-95

    Date.

    Jan-96 MElr-96 JuI-96

    _. K ._C21-;"_ ..... C21-Nat.

    Figure C.II. Iron concentration of the leachate from sample C2I. I month after reagent addition.

    Silicon concentration of the leacha.8i month after chemicaltreatment.

    3500.00

    I-

    J

    3000.002500.002000.001500.001000.00500.00

    O.OO ... -- ..... -- .. -- .......... ::::.:::~~- ..Sep-95 Nov-95 Dec-95 Jan-96

    1liIa.

    MElr-96 JuI-96

    I ___.,__ C21-i•••••• C21-i_ ..... C21-iii_ "*" _ C21-i11l:~lI!.- C21-Na~

    L- __

    Figure C.12. Silicon concentration of the leachate from sample C21. I month after reagent addition.

    393

  • AppendixC

    Aluminium concentration of the leachates 24 hours after chemicaltreatment.

    400.00

    i 300.00-

    J200.00

    100.00

    0.00Aug-95 Sep-95

    ,..'.'. ,................. '

    Oct·95 flbv·95

    CIte,Dec-95 Jan-96 Mar-96

    F-+-_C21.~1 •••••• C21·,_,.._C21·iij_. ~._C21·jy

    Figure C.13. Aluminium concentration of the leachate from sample C21. 24 hours after reagent addition.

    calcium concentration of the leachates 24 hours after chemicaltreatment.

    I3000.002500.00- 2000.00I1500.00 •1000.00500.008 0.00

    Aug-95 Sep-95 Oct-95 Nov-95 Dec-95 Jan-96 Mar-96DD.

    F-+-_C21.j

    1--+-C21-iiI ....... C21-iii_. ~. _C21-iv

    Figure C.14. Calcium concentration of the leachate from sample C21. 24 hours after reagent addition.

    12000.00 _-+- _C21·j

    I •10000.00 --+-C21-ii- 8000.00 ....... C21-iii

    18000.00 _. ~. _C21·JY4000.00

    2000.00

    0.00Aug-95 Sep-95 Oct-95 flbv-95 Dec-95 Jan-96 Mar-96

    CIte.

    Iron concentration of the leachates 24 hours after chemical treatment.

    Figure C.I S. Iron concentration of the leachate from sample C21. 24 hours after reagent addition.

    394

  • AppendixC

    Silicon concentration of the l.achate.24 hours after chemicaltreatment.

    250.00 II 200.00 .Do.-

    J150.00

    100.00

    50.00

    0.00Aug-95

    ».,.'\.,." .,'\.' ."\. ..'\.~".'" ......•...." -..'\.

    .,.,.

    Sep-95 Oct-95 New-95 Dec-95

    DIa.Jan-96

    _-+-_C21-i

    • ...... C21-i

    __...,_ C21-ii

    - • K • _ C21-iv

    MBr-96

    Figure C.16. Silicon concentration of the leachate from sample C21. 24 hours after reagent addition.-l

    II

    Aluminium concentration of the leachate.1 month after chemicaltreatment.

    Oct-95 New-95 Dec-95

    r.t..M1tr-96 JuI-96

    _ ..... C31-i____ -C31-ii

    ---6- C31-ii••• )C••• C31-1v_ ••. _C31-v-.-. C31-Nat

    I~-------------------------------------------------------~Figure C.17. Aluminium concentration of the leachate from sample C31. I month after reagent addition.

    Calcium concentnltlon of the leachate.1 month after chemicaltreatment.

    I800.00800.00

    J400.00

    200.00

    0.00~95 Oct-95 New-SS DIe-SS Jan-98 MItr-98 JuI-98

    r.t..

    _ .•• _C31-i____ C31-ii

    _ ........._C31-iii

    ... )Coo. C31-1v

    - . le-. C31-v1-.-.C31-Nat I

    Figure C.II. Calcium concentration of the leachate from sample C31. 1month after reagent addition.

    395

  • AppendixC

    Iron concentration of the leacha .. s 1 month after chemical treatment

    I

    J

    ....... C31-i

    ~C31-ii_ ....... _C31-i

    _. K-. C31-iv

    - .ll. _C31-v

    , ---.- C31-Nal

    Oct-95 Nov-95 Dac-95 Jan-96 Mar-96 Ju~96

    CIte.

    Figure C.19. Iron concentration of the leachate from sample C31. I month after reagent addition.

    Iron concentration of the leacha .. s1 month after chemical treatment

    3500.00- 3000.00i 2500.00j 2000.001500.001000.00500.00

    0.00Sep-95 Oct-95 Nov-SS' Dlc-95 Jan-96 Mar-96

    CIte.

    Ju~96

    I

    II_ ....... _C31.. I

    1 C31-i

    ~C31-i

    _.~. C31-iv

    - .II.- C31-v

    1---.-C31-Nat·1

    Figure C.20. Iron concentration of the leachate from sample C31. ] month after reagent addition.

    Aluminium concentration ofthele.chates 24 hou.... fter chemicaltreatment

    I60.0050.00

    J40.0030.0020.0010.000.00Aug-95 Sep-95 Oct-95

    -+-C31-i

    _ .... C31-i

    _ .•. _C31-i

    .•. )(..• C31-iv

    _"*" _C31-v

    I~---------------------------------------------------------------~Figun: C.21.Aluminiwn conc:cntration of the leachate from sample C31.24 months after reagent addition.

    396

  • Appendix C

    Calcium concentration of the leachatea 24 hours after chemicaltreatment

    - 1~OOii 800.00-c: 600.001 400.00200.008 0.00

    Aug-95 Sep-95 Oct-95 Nov-95 Dac-95 Jan-96 Mar-96

    CIte.

    ~C31-i.•••.. C31-i_ ...... C31-iii_.* ._C31-iv_ .... _C31-v

    Figure C.22. Calcium concentration of the leachate from sample ClI. 24 hours after reagent addition.

    Iron concentration of the leachatea 24 hours after chemical treatment

    7000.00

    i 6000.005000.00

    J4000.003000.002000.001000.00

    0.00Aug-95 Sep-95 Oct-95 Nov-95 Dec-95 Jan-96 Mlr-96

    CIte.

    1~C31-i

    tl_:=~::~1_K- _ C31-iv I·lIC- __ C31-v IFigure C.2l. Iron concentration of the leachate from sample C31. 24 hours after reagent addition.

    Silica concentration of the I•• chatea 24 hours after chemicaltreatment

    160.00

    I 140.00120.00-

    I100.0060.0060.0040.0020.000.00Aug-95 Sep-95 Oct-95

    rI,,

    III,,

    Dac-95 Jan-96 Mar-96Nov-95

    Date.

    ~C31-~.1_ .... C31-1 I_ •• - _C31-ii I• _·x .. - C31-iv I1_ .... _C31-V i

    Figure C.24. Silica concentration of the leachate from sample ClI. 24 hours after reagent addition.

    397

  • AppendixC

    Aluminium concentration of the leachates1 month after chemicaltreatment

    I 80.0060.00-J

    40.00

    20.00

    0.00Sep-95 Oct-95 Nov-95 Dac-95 Jan-96 Mlr-96 Ju~96

    DIte.

    _-+-_C83-i_ ••. _C83-i

    ~C83-i... )(•.. C83-iv_.Ir-. C83-Nat

    Figure C.2S. Aluminium concentration of the leachate from sample CS3. I month after reagent addition.

    Calcium concentration of the leachates1 month after chemicaltreatment

    Nov-95 Jan-96 Mlr-96 Jul-96Oct-95

    _.,._C83-i_ ....... _C83-i

    •••••.. C83-ii_.*._C83-iv_ . ~. C83-Nat

    Figure C.26. Calcium concentration of the leachate from sample CS3. I month after reagent addition.

    I

    II I

    ,

    Iron concentration of the leachate.1 month after chemical treatment

    _-+-_C83-i.•.•.. C83-i~C:a3-ii

    _.*._C83-ivI - • 11:-. C83-Nat I

    2500.00

    I2000.00

    I1500.00

    1000.00

    500.00

    0.00Sep-95 Oct-95 tGv-95 1lIc-95 Jln-98 MIr-96 Ju~96

    DIte.

    L_ ~

    Figure C.27.1ron concentration of the leachate from sample CS3. I month after reagent addition.

    398

  • AppendixC

    Silica concentration of the leachate. 1 month after chemicaltreatment

    5000.00

    i 4000.00-J

    3000.00

    2000.00

    1000.00

    0.00Sep-95 Oct-95 Nov-95 Dec-95 Jan-96 MIiIr-96 JuJ.96

    1JiIa.

    --

    1-·K'-C83-;" I... )K... C83-Nat

    L-._ ~ _

    Figure C.2S. Silica concentration of the leachate from sample CS3. I month after reagent addition.

    Aluminium concentration of the leachatee 24 hours after chemicaltreatment

    '---------------------

    Calcium concentration of the 'eachate.24 hours after chemicaltreatment

    I 200.00150.00-

    J100.00

    50.00

    0.00Aug-95 Slp-95 0et-95 NIw-95 Dlc-95 Jen-96 MIiIr-96

    1JiIa.

    Figure C.29. Aluminium concentration of the leachate from sample CS3. 24 hours after reagent addition.

    I2000.001500.00 ~1J

    C83-i1000.00

    500.00 t;;"~C83-1V0.00

    IAug-95 Sep-95 0et-95 Nov-95 DIe-95 Jan-96 Mlr-96 I

    DID. III

    ______j

    Figure C.30. Calcium concentration of the leachate from sample CS3. 24 hours after reagent addition.

    399

  • AppendixC

    Iron concentration of the leachates 24 hours after chemical treatment.

    i C83-i__ C83-i

    _ ..,._ _ C83-ii

    _.~._C83-iv

    Figure C.31. Iron concentration of the leachate from sample CS3. 24 hours after reagent addition.

    Silica concentration of the leachate.24 hours after chemicaltreatment

    120.001100.00

    JSO.OO60.00

    40.00

    20.00

    0.00Aug-95 Oct-95 Nov-95 DIc-95

    DID.

    Jan-96 MIlr-96

    ....... C83-i__ C83-i_ ..,._ _ C83-ii

    _.~._C83-iv

    Figure C.32. Silica concentration of the leachate from sample CS3. 24 hours after reagent addition.

    Aluminium concentration of the leachate. 1 month after chemicaltreatment.

    I 8.006.00-J

    ".00

    2.00

    0.00Sep-95 Oct-95 Nov-95 Dlc-95 Jan..96 Mar-96 Ju..96

    DID.

    _ _.__C92-i

    ....... C92-i

    _.,.__ C92-ii

    _.~._C92-iv

    _ •lK-. C92-Nat.

    ~-------------------------------------------------------------~Figure C.33. Aluminium concentration of the leachate from sample C92. 1month after reagent addition.

    400

  • AppendixC

    Calcium concentration of the leachates1 month after chemicaltreatment.

    - 250.00i 200.00Go-~ 150.001 100.00I 50.00

    0.008Sep-95 Oct-95 Nov-95 0ec-95 Jan-96 Mar-96 Ju~96

    CIte.

    --+-C92-i_ ...... _C92-i

    ••• &••• C92-i_ . ~ •_ C92-iv

    _ •lK-. C92-Nal

    Figure C.34. Calcium concentration of the leachate from sample C92. I month after reagent addition.

    Iron concentration of the leachates 1 month after chemical treatment

    - 2000.00 ri 1500.00 t

    J1000.00 ,.--- .-

    50000 " .&••..t' .....=>«,.'0.00 .......... •

    Sep-95 Oct-9S Nov·95...

    DIe·95

    CIte.

    Jan-96

    --+-C92-i_ _C92·i

    ... & C92·ii_.~._C92·1v

    - • lK-. C92.Na~

    Figure C.3S. Iron concentration of the leachate from sample C92. I month after reagent addition.

    Silica concentration of the leachate.1 month attar chemlcal __ ~~-_ltreatment. ~, I

    --+-C92-i II_ ..... C92-i I

    _ ••• _C92-ii

    _~_C92-iv... )1( ... C92-Nall

    Nov-95 0ec-95

    DD.

    Jan-96 Mar·96 Ju~96Oct-95

    Figure C.36. Silica concentration of the leachate from sample C92. I month after reagent addition.

    401

  • AppendixC

    Aluminium concentration of the leachate.24 hours after chemicaltreatment

    Calcium concentration of the leachate.24 hours after chemicaltreatment

    i 2000.001500.00

    J1000.00

    500.00

    0.00Aug-95 Sep-95 Oct-95

    ..-'....,.

    I SO.OO60.00-

    J40.00

    20.00

    0.00Aug-95 Sep-95 Oct-95 Nov-95 DIc-95 Ja~96 MIr-96

    DIt8.

    --+-C92-i_..__C92-i__• __C92-ii

    - - -x- - - C92-iv

    Figure C.37. Aluminium concentration of the leachate from sample C92. 24 hours after reagent addition.

    --+-::l._C92-1C92 -I

    /--.-_ --I: .. x.. - C92-iv! I

    Nov-95 Dlc-95 Jan-96 Mar-96 IDIt8. I

    '-- JFigure C.3S. Calcium concentration of the leachate from sample C92. 24 hours after reagent addition.

    -IIron concentration of the l.achate.24 hours after chemical treatm.nt

    30000.00

    I215000.0020000.00

    J15000.0010000.005000.00

    0.00Aug-95 Sep-95 Oct-95 Ncw-95 Dlc-95 Jan.96 Mar-96

    DIt8.

    1-+-C92-~ I1_ --- _C92-0 I

    PI

    Figure C.39. Iron concentration of the IeKbate from sample C92. 24 hours after reagent addition.

    402

  • AppendixC

    ~Silica concentration of the leachates 24 hours after chemical 1

    treatment

    60.00-i 50.00Do 40.00-I30.00 1I20.00 II 10.008 0.00

    Aug-95 Sep-95 Oct-95 1Ibv-95 Dec-95 Jan-96 Mar-96

    CIte.

    I-+- al2-~.I04- C92.

    ..

    Figure C.40. Silica concentration of the leachate from sample C92. 24 hours after reagent addition.,----------------------------------------------------------------1

    II'.-.. -.. -.-. C1=33-;;-Ci:-----11/1'_04- _ C133-i

    =:.=~:: II i

    - • JIG-. C133-Nal

    Aluminium concentration of the leachates 1 month after chemicaltreatment.

    I 1000.00800.00-

    J600.00400.00200.00

    0.00Sep-95 Oct-95 1Ibv-95 Dlc-95 .Jan-96 MIIr-96 Juf-96

    CIte.

    Figure C.4l.Aluminium concentration of the leachate from sample C133.l month after reagent addition.

    Calcium concentration of the leachate.1 month after chemicaltreatment.

    Ir- ....._C133-i [Ii --- C133-i I:_ .... _C133-ii I II ••• )C ••• C133-iY I Ij _.JIG-. C133-Nall II I

    I

    III

    ~------------------------------------------------------------~Figure C.42. Cak:ium concentration of the leachate from sample C133. I month after reagent addition.

    I1200.001000.00

    J800.00600.00400.00200.00

    0.00Sep-95 Oct-96 NDv-96 Dlc-95 ... 96 """-96

    CIte.

    JuI-96

    403

  • AppendixC

    Iron concentration of the 1•• ch.... 1month .fter ch.mlcal tre.tm.nt

    I" ..... C133-i1~C133-i

    I=:=~::~l

    1800.00 I1600.00_I1400.00 +1200.00 +

    81':::

    u 600.00400.00200.00

    0.00 1t=~=.,t:=~IoWI ...........-t~;.;,,;:; .... ~~~;.:.:;.~ ...Sep-95 Oct-95 Nov-95 Dec-95 Jan-96 Mar-96 Ju~96

    CIte.

    Figure C.43.lron concentration of the leachate from sample C133. 1month after reagent addition.

    Silica concentration of the 1•• ch.te.1 month .b, ch.mlcaltre.tm.nt

    ....... C133-i_ ...... C133-i_ ...,_ _ C133-i

    ~C133-1v_ .•• _ C133-NIIl

    Figure C.44.1ron concentration of the leachate from sample Cl33. 1month after reagent addition.

    Aluminium concentrlltion of the 1•• ch.... 24 houra .b, chemicaltre.tment

    I500.00400.00-

    J300.00200.00100.000.00Aug-95 Sep-85 0ct-95 Nov-95 Dlc-95 Jan-96 Mar-96

    DID.

    -+-C133-i_ .. _C133-i

    I _ ••• - C133-ii

    I ... )(... C1~iv I

    ~-------------------------------------------------------------~Figure C.4S.Alwninium concentration of the leachate from sample C133.24 hours after reagent addition.

    404

  • AppendixC

    Calcium concentration of the leacha •• 24 hours after chemlc.ltreatment

    Nov-95 DIIc-95 Jan-96 MIIr-96

    DIta.

    _ -+- _O133-i••••.• O133-i_ ••. _0133-i

    I-M-- 0133-;"

    ~--------------------------------------------------------------~Figure C.46. Calcium concentration of the leachate from sample C133. 24 hours after reagent addition.

    Iron concentnltlon of the leacha •• 24 hours after chemic. I treatment.

    _ -+- _O133-i,-.-0133-ii_ ••• _0133-11

    ••• )(..• 0133-;"

    I300.00250.00- 200.00

    J150.00100.0050.000.00Aug-95 Sep-95 Oct-95 Nov-95 Dllc-95 Jan-96 Mar-96

    DIta.

    Figure C.47. Iron concentration of the leachate from sample C133. 24 hours after reagent addition.

    SIlica concentration of the leacha •• 24 hours after chemicaltreatment.

    I300.00250.00

    J200.00150.00100.0050.000.00Aug-95 Sep-95 0ct-95 Nov-95 Dllc-95 Jan-96 Mar-96

    illite.

    1_ -+- - O133-i•••••• 0133-i

    I_ ••• _0133-i

    -M--0133-;"

    Figure C.4I. Silica concentration oftbe leachate from sample C133. 24 hours after reagent addition.

    40S

  • AppendixC

    Aluminium concentration of the leachatea1 month after chemicaltreatment.

    - 2500.00 Ti: 2000.00 t )

  • Appendix C

    Silica concentration of the leachatea1 month after chemicaltreatment

    3500.00- 3000.00i 2500.00-II: 2000.00i 1500.001000.00I 500.008 0.00

    Sep-95 Oct-95

    ~,,,I ,I ,I ,, ,, ,, ,

    Nov-95 DIe-95 Jan-98 Mlr-96 Juj.96

    CIte.

    1

    - ...... _C141-i

    ....... C141-i

    I-.._.~:~~:41-v

    41-Nat

    Figure C.S2. Silica concentration of the leachate from sample C] 33.] month aiter reagent addition.

    Aluminium concentration of the leachate.24 hours after chemicaltreatment

    I2000.00 ~C141-iJC ....... C141-i1500.00 ,

    J, _ ....... _C141-i

    1000.00 .- •k-. C141-iv

    500.00 _ ••• _C141-v

    0.00Aug-95 Sep-95 Oct-95 Nov-95 D8c-95 Jan-96 Mlr-96

    CIte.

    Calcium concentration of the leachatea 24 hours after chemicaltreatment

    - 3000.00i 2500.00

    J2000.001500.001000.00500.00

    0.00Aug-95 Sep-95 Oct-SS

    Figure C.S3. Aluminium concentration of the leachate from sample C133.24 hours after reagent addition.

    .....Nov-95 D8c-SS Jan-96 Mar·96

    CIte.

    ~C141·i

    ....... C141-i

    _ ••• _C141-i

    _.k-' C141-iv I_ ..... _C141-v

    Figure C.54. Calcium concentration of the leachate from sample C133. 24 hours after reagent addition.

    407

  • AppendixC

    I

    Iron concentration of the 1•• ch.... 24 hour8 .fter chemical tre.tm.nt. I

    __ Cl.'