ML13323B200

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Attachment 6: CHLE-012, Rev. 3, T1 Mbloca Test Report, Figure 53 Through End
ML13323B200
Person / Time
Site: South Texas  
Issue date: 01/09/2013
From: Leavitt J
Southern Nuclear Operating Co
To:
Office of Nuclear Reactor Regulation
Shared Package
ML13323A673 List:
References
GSI-191, NOC-AE13003040, STI 33762096, TAC MF2400, TAC MF2401 CHLE-012, Rev 3
Download: ML13323B200 (54)
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Text

3.0 Fiber Analysis There were two different types of fiber beds used during test; (1) blender-processed debris beds and (2)

NEI-processed debris beds. The NEI-processed debris bed was used for the duration of the 30-day test followed by the insertion of the blender-processed debris bed exposed to solution for 2 days. At the end of the test, the beds were analyzed by the naked eye to spot any noticeable features (particles, debris, etc.). Sections of the fiber bed with particulate were extracted and sent for SEM analysis. The following images depict samples taken from Test I post-test fiber beds. The name of the sample includes which bed it came from (NEI or Blender) and the approximate description of the visual appearance of the particle being examined is noted in the figure captions. If EDX of a particle was acquired, the location of the particle examined is indicated on the figure by an "X".

Blender, Tight Fiber No Particle, 1 1

Figure 53 - "Blender, Tight Fiber No Particle, 1" Very dirty fiber

Blender, Tight Fiber No Particle, 2 Figure 54 - "Blender, Tight Fiber No Particle, 2" Zoomed in view of dirty fiber Elmt Element %

Atomic %

0 56.77065 69.19812 Na 9.799163 8.312148 Mg 1.583022 1.269783 Al 0.82532 0.596501 Si 26.61184 18.47771 Ca 4.410004 2.145727

Blender, Tight Fiber No Particle, 4 Figure 55 - "Blender, Tight Fiber No Particle, 4" Fiber bonded by precipitate

  1. 1
  1. 2 Elmt Element % Atomic %

0 87.29305 91.56556 Na 7.752471 5.659089 Si 3.919436 2.341958 Ca 1.035042 0.433387 Elmt Element %

Atomic %

0 53.04387 66.44089 Na 8.375714 7.300892 Mg 1.601632 1.320186 Al 1.01925 0.757006 Si 29.04379 20.72318 Ca 6.915733 3.457829

Blender, White Specks, 1 Figure 56 - "Blender, White Specks, 1" Large particle on fiber Elmt Element %

Atomic %

O 38.35108 57.62598 Na 2.812468 2.940913 Al 1.792424 1.596983 Si 1.596614 1.366607 P

21.37774 16.59197 Ca 28.37723 17.02064 Ti 5.69245 2.856915

Blender, White Specks, 2 Figure 57 - "Blender, White Specks, 2" Spider web looking precipitate on fiber

Blender, black strip, 1 Figure 58 - "Blender, black strip, 1" Scattered precipitate Elmt Element %

Atomic %

0 72.39867 80.53704 Na 12.47189 9.654976 Al 8.515695 5.616993 Si 6.613756 4.190985

NEI, white flakes, 1 Figure 59 - "NEI, white flakes, 1" Layered particle on fiber

  1. 1
  1. 2 Elmt Element %

Atomic %

0 52.97784 73.97655 Al 0.577575 0.478219 Si 0.848312 0.674774 Ca 39.60971 22.07835 Ti 5.986553 2.792119 Elmt Element %

Atomic %

0 70.30152 84.59555 Al 3.347521 2.388497 Si 5.693091 3.902419 Ca 10.33824 4.965859 Ti 10.31964 4.147675

Blender, Grey Strip, 1 Figure 60 - "Blender, Grey Strip, 1" Flat precipitate Elmt Element %

Atomic %

0 31.24707 52.46994 Al 0.932475 0.928447 Si 1.000949 0.95745 P

10.25309 8.89307 Ca 45.91915 30.7794 Ti 10.64725 5.971675

Blender, Grey Strip, 2 Figure 61 - "Blender, Grey Strip, 2" Small dump on fiber Elmt Element %

Atomic %

O 60.32007 78.11366 Na 2.673882 2.40969 Al 0.428939 0.329366 Si 0.669457 0.493845 P

1.023016 0.684295 Ca 34.12969 17.6426 Ti 0.754966 0.32655

Blender, Black Spots, 1 Figure 62 - "Blender, Black Spots, 1" Gunk on fiber Elmt Element %

Atomic %

0 97.36662 98.35217 Na 1.190426 0.836816 Si 1.083767 0.62361 P

0.359193 1 0.187412

Blender, Black Spots, 2 Figure 63 - "Blender, Black Spots, 2" Crystal on particle Elmt Element %

Atomic %

0 70.31113 80.97112 Na 2.706346 2.168919 Al 4.024393 2.748053 Si 18.12502 11.89015 Ca 4.833108 2.221762

Blender, Black Speck, 1 Figure 64 - "Blender, Black Speck, 1" Precipitate at fiber crossing Elmt Element%

Atomic %

0 99.25358 99.54417 Na 0.527579 0.368223 Ca 0.218836 8.76E-02

Blender, Black Speck, 2 Figure 65 - "Blender, Black Speck, 2" Small amount of precipitate Elmt Element %

Atomic %

0 57.99848 70.58616 Na 8.362384 7.082506 Mg 1.429282 1.144703 Al 0.63881 0.460992 Si 25.97108 18.00512 Ca 5.599967 2.72053

NEI, Black Specks, 1 Figure 66 - "NEI, Black Specks, 1" Precipitate clump Elmt Element %

Atomic %

F 14.68916 27.62317 Al 1.641468 2.173415 Si 2.80432 3.567157 P

2.11163 2.435594 Ca 37.53921 33.46122 Ti 41.21422 30.73944

NEI, Black Specks, 2 Figure 67 - "NEI, Black Specks, 2" Large amount of particulate

  1. 1
  1. 2 Elmt Element %

Atomic %

F 81.71114 90.61282 Al 0.819067 0.639531 Si 1.33287 0.999803 Ca 7.579323 3.983996 Ti 8.557604 3.763855 Elmt Element %

Atomic %

0 55.41555 68.31646 Na 7.913568 6.78922 Mg 1.477881 1.198962 Al 1.158964 0.847193 Si 29.0257 20.38353 Ca 5.008331 2.46463

NEI, Black Speck, 1 m

'i. ý 4ý 1

r Figure 68 - "NEI, Black Speck, 1" Fiber "sunk" in precipitate

NEI, black speck, 2 Figure 69 - "NEI, black speck, 2" Very clean NEI

NEI, Clean Fiber, 1 Figure 70 - "NEI, Clean Fiber, 1" Wispy fiber

4.0 Baseline Fiber The method of preparation of fiber debris samples for SEM analysis was examined to determine if the procedure contributed to the formation of particulates or attributes that may be of interest. Two batches of NEI-processed fiber were prepared and soaked for 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> in solution of interest. One batch of fiber was allowed to soak in borated-TSP solution, while the other batch was soaked in in deionized (DI) water. Three types of samples were taken from the two batches. One sample was taken from the fiber soaked in the DI water and, a second sample was taken from the borated-TSP solution, and a third sample was taken from the borated TSP solution and quickly rinsed with DI water. All samples were allowed to dry in a desiccator before they were sputter coated. The results of the samples taken are below. A description of the images is given by the caption. If EDX of a particle was acquired, the location of the particle examined is indicated on the figure by an "X".

NEI, Soaked in DI, 1 Figure 71 - "NEI, Soaked in DI, 1"

  1. 1
  1. 2 Elmt Element %

Atomic %

0 41.52557 55.65168 Na 10.70849 9.987221 Mg 1.639075 1.445552 Al 1.025322 0.814782 Si 35.36501 26.99849 Ca 9.031668 4.831653 Fe 0.704875 0.270625 Elmt Element %

Atomic %

0 46.62602 60.80523 Na 10.86826 9.863396 Mg 1.48125 1.271198 Al 0.663484 0.51 3052 Si 29.40307 21.84279 Ca 10.9579 5.704335

NEI, Soaked in DI, 1 Continued

  1. 3 Elmt Element %

Atomic %

0 50.92377 63.92218 Na 13.0194 11.37302 Mg 1.954836 1.61478 Al 0.886411 0.659758 Si 27.35993 19.56361 Ca 5.37906 2.695271 Fe 0.476584 0.171381

NEI, Soaked in Borated TSP, 1 Figure 72 - "NEI, Soaked in Borated TSP, 1" Elmt Element %

Atomic %

0 54.4035 66.84762 Na 13.0756 11.18084 Mg 1.732408 1.400817 Al 0.821988 0.598885 Si 25.17802 17.62315 Ca 4.788505 2.348682

NEI, Soaked Borated TSP, 2 Figure 73 - "NEI, Soaked Borated TSP, 2" Zoomed in picture Elmt Element %

Atomic %

0 83.46626 89.07186 Na 8.438155 6.266585 Mg 0.349496 0.245439 Al 0.212037 0.134171 Si 3.75549 2.282964 P

3.109064 1.713779 Ca 0.669499 0.285197

NEI, Soaked Borated TSP rinsed with DI, 1 Figure 74 - "NEI, Soaked Borated TSP rinsed with DI, 1" Elmt Element %

Atomic %

0 54.5554 66.89457 Na 13.74195 11.72615 Mg 1.973917 1.592774 Al 0.871655 0.633747 Si 24.30052 16.97351 Ca 4.187444 2.049591 Fe 0.369102 0.129656

NEI, Soaked Borated TSP rinsed with DI, 2 Figure 75 - "NEI, Soaked Borated TSP rinsed with DI, 2" Big particles were not found anywhere. This in one of the very few particles that were actually found, but it is very small.

Elmt Element %

Atomic %

0 61.0692 74.41264 Na 7.787324 6.603386 Mg 1.036385 0.831032 Al 1.091318 0.788487 Si 14.75426 10.24106 Cl 4.481705 2.46438 Ca 9.067391 4.410338 Fe 0.712416 0.248686

5.0 Aluminum SEM Aluminum used in the test was taken from aluminum scaffolding obtained from STP. This scaffolding was a non-homogenous sample with unknown constituents from years of use which remained after cleaning and the alloy of aluminum is not known. The samples which were to be submerged were from the side of the scaffolding and had a different texture and appearance than the samples cut for the vapor space. Three types of aluminum samples for submerged and vapor samples were examined using SEM and are as follows: (1) examination of test samples, (2) analysis of pre-test samples (3) examination of test samples after scale removal. Post-test samples were labeled "used", while base line pre-test samples were labeled as "not used". Samples which had scale removed were labeled as "acid washed".

Those that did not have scaled removed were labeled as "not washed". The SEM results of all aluminum samples are shown below. A description of the images is given by the caption. If EDX of a particle was acquired, the location of the particle examined is indicated on the figure by an "X".

Used Submerged, Not Washed, 1 Figure 76 - "Used Submerged, Not Washed, 1"

Used Submerged, Not Washed, 2 Figure 77 - "Used Submerged, Not Washed, 2" Cracking features Elmt Element %

Atomic %

0 55.87518 69.72538 Al 20.307 15.02576 Si 15.05654 10.70287 P

2.40957 1.553127 S

1.918446 1.194529 Ca 1.518032 0.756168 Fe 2.915237 1.042171

Used Submerged, Not Washed, 3 Figure 78 - "Used Submerged, Not Washed, 3"

  1. 1
  1. 2 Elmt Element %

Atomic %

0 16.29551 25.04923 Al 78.43685 71.49327 Si 1.253322 1.097469 P

1.147492 0.911111 S

0.170633 0.130877 Ca 0.754579 0.463016 Fe 1.941611 0.85503 Elmt Element %

Atomic %

0 54.97348 68.3452 Al 33.83013 24.93889 Si 0.833296 0.590143 P

2.316628 1.48767 S

5.929717 3.678442 Ca 1.468387 0.728719 Fe 0.648374 0.230926

Used Submerged, Not Washed, 4 Figure 79 - "Used Submerged, Not Washed, 4" Small cracking Elmt Element %

Atomic %

O 32.17372 44.83123 Na 0.809217 0.78469 Al 58.67721 48.48054 Si 1.536704 1.219754 P

5.502426 3.960309 Ca 1.300734 0.723491

Used Submerged, Acid Washed, 1 Figure 80 - "Used Submerged, Acid Washed, 1" Elmt Element %

Atomic %

O 5.372327 8.731379 Mg 0.723003 0.773273 Al 93.90467 90.49535

Used Submerged, Acid Washed, 2 Figure 81 -"Used Submerged, Acid Washed, 2" Particulate on surface Elmt Element %

Atomic %

0 56.49949 77.71421 Al 3.341963 2.725689 Si 2.877982 2.255002 P

0.707126 0.502398 Ti 36.57345 16.8027

Used Submerged, Acid Washed, 3 Figure 82 - "Used Submerged, Acid Washed, 3" Elmt Element %

Atomic %

0 5.693635 9.241012 Al 94.30636 90.75899

Unused Submerged, Acid Washed, 1 Figure 83 - "Unused Submerged, Acid Washed, 1" Elmt Element %

Atomic %

C 19.28571 33.93004 0

5.485235 7.244866 Al 72.2487 56.58273 Si 2.980362 2.242369 Note: carbon accidentally got checked in this EDS and is probably not correct due to the way that oxygen was being calculated by changing some carbon readings.

Unused Submerged, Acid Washed, 2 Figure 84- "Unused Submerged, Acid Washed, 2" Elmt Element %

Atomic %

0 7.747664 12.41073 Al 91.32348 86.74169 Si 0.928858 0.847577

Unused Submerged, Not Washed, 1 Figure 85 - "Unused Submerged, Not Washed, 1"

  1. 1 EDS of particle
  1. 2 EDS of Face Elmt Element %

Atomic %

0 52.90488 66.05394 Na 1.922631 1.670524 Al 34.75129 25.7272 P

6.952252 4.483571 S

2.695725 1.679398 Ca 0.773231 0.385369 Elmt Element %

Atomic %

0 37.43722 50.60629 Na 1.295838 1.219006 Al 49.83636 39.94533 Si 5.181171 3.989623 P

3.366714 2.35073 S

2.472522 1.667694 Ca 0.410188 0.221334

Unused Submerged, Not Washed, 2 Figure 86 - "Unused Submerged, Not Washed, 2" Shale

  1. 2
  1. 1 Elmt Element%

Atomic%

0 57.54915 70.0183 Al 36.39483 26.25615 Si 0.570515 0.395405 S

5.485495 3.330148 Elmt Element %

Atomic %

0 37.02751 50.01065 Al 57.94616 46.40678 Si 2.04494 1.573336 S

2.981392 2.009242

Unused Vapor, Acid Washed, 1 Figure 87 - "Unused Vapor, Acid Washed, 1"

Unused Vapor, Acid Washed, 2 Figure 88 - "Unused Vapor, Acid Washed, 2" Rough slope of sample Elmt Element %

Atomic %

0 26.18998 37.81557 Al 59.55833 50.99136 Si 11.96874 9.844341 K

2.282946 1.34873

Unused Vapor, Acid Washed, 3 Figure 89 - "Unused Vapor, Acid Washed, 3"

  1. 2
  1. 1 Elmt Element %

Atomic %

0 50.9611 64.47919 Al 5.971625 4.480144 Si 43.06727 31.04067 Elmt Element %

Atomic %

0 22.30666 32.73701 Al 67.56657 58.79698 Si 10.12677 8.466

Used Vapor, Not Washed, 1 I I I

IT Y1.1 I

Figure 90 - "Used Vapor, Not Washed, 1"

Used Vapor, Not Washed, 2 Figure 91 - "Used Vapor, Not Washed, 2" Elmt Element %

Atomic %

0 50.54052 65.42443 Na 2.121558 1.911213 Al 19.7753 15.17896 Si 10.50073 7.743242 P

8.120576 5.429785 S

0.888045 0.573602 Ca 5.156328 2.66444 Fe 2.896936 1.074316

Used Vapor, Not Washed, 3 Figure 92 - "Used Vapor, Not Washed, 3" Elmt Element %

Atomic %

0 60.19044 72.63639 Na 5.997493 5.036749 Al 16.02977 11.47024 Si 5.435722 3.736689 P

4.377243 2.728493 S

4.587612 2.762412 Ca 3.381714 1.629029

Used Vapor, Acid Washed, 1 Figure 93 - "Used Vapor, Acid Washed, 1" Elmt Element %

Atomic %

0 54.62689 67.24589 Al 32.65743 23.83746 Si 12.71568 8.916649

Used Vapor, Acid Washed, 2 Figure 94 - "Used Vapor, Acid Washed, 2" Elmt Element%

Atomic %

0 28.34927 40.30083 Al 59.47025 50.12918 Si 10.89308 8.821161 K

1.2873981 0.748822

Unused Vapor, Not Washed, 1 Figure 95 - "Unused Vapor, Not Washed, 1"

  1. 2
  1. 1 Elmt Element %

Atomic %

0 59.15316 73.00966 Na 0.63718 0.547291 Mg 0.419918 0.341066 Al 14.66136 10.72989 Si 11.93555 8.391659 P

6.691381 4.265929 Cl 0.591235 0.329308 Ca 2.694184 1.327378 Fe 1.676081 0.592639 Zn 1.539939 0.465179 Elmt Element %

Atomic %

0 29.14538 41.61925 Na 0.486218 0.48318 Mg 0.621621 0.584147 Al 58.73953 49.73632 Si 5.083239 4.134928 P

1.69262 1.248474 Cl 0.34045 0.219391 K

1.333805 0.779311 Ca 0.925179 0.52737 Fe 1.631967 0.667619

Unused Vapor, Not Washed, 2 Figure 96 - "Unused Vapor, Not Washed, 2" Elmt Element %

Atomic %

O 31.00385 47.66272 Al 12.4003 11.30353 Si 21.75179 19.04852 P

5.832083 4.631081 Cl 0.62965 0.43682 K

18.24822 11.4783 Ca 5.632656 3.45654 Fe 4.501449 1.982478

Appendix 2 - Aluminum Corrosion, WCAP-16530-NP material release, XPS Summary results

Aluminum Corrosion Calculation I

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1-1-1-1 7 13215515 L35115 mm,.

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Calculated Material Release MBLOCA WCAP Calculation-kjh.xlsx 11/19/20121:07 PM 17 18 19 20 122 0

0 0

60 0

0 0

0 0

0 0

0 0

0 0

0 0

0 1

nt

10~~~~Cluae Material Release MMMINKIMMIM

ý 22 NK21 MAN 2

.2 12 42 EL~

43NLL 44 IN~~

45 48 47Ior 50 I

Calculated Material Release MBLOCA WCAP Calculation-kjh.xlsx 11/19120121:07 PM A

B C

D E

F G

H I

J K

L M

N S

T U

Start of End of NaAIS6O8 AIOOH Ca 3(P0 4)2 Ca conc in Si conc: in A] conc in Interval Interval Interval Average Average Temp Al Release Precipitate Preapitate Precpitate soluUOn solutiOn soluton 1

Duration (min)

(hrs)

(hrs)

Time (d)

Interval pH (F

Ca Release (kg) Si Release (kg)

(kg)

(kg)

(kg)

(kg)

(mg/IL)

(mg/L)

(mg/L) 2 5.0 0.00 0.1 0.00347222 5.555 119.7 0.0037 0.0014 0.0007 0.004 0.001 0.010 0.00 0.00 0.00 3

0.8 0.08 0.1 0.00405093 6.46 155.6 0.00 0.00 0.00 0.0 0.0 0.01 0.00 0.00 0.00 4

0.8 0.10 0.1 0.00462963 6.46 187.45 0.01 0.00 0.00 0.0 0.0 0.02 0.00 0.00 0.00 5

0.8 0.11 0.1 0.00520833 6.46 181.65 0.01 0.01 0.01 0.0 0.0 0.02 0.00 0.00 0.00 6

1.1 0.13 0.1 0.00596065 6.46 177.85 0.01 0.01 0.01 0.0 0.0 0.02 0.00 0.00 0.00 7

0.6 0.14 0.2 0.00636574 6.46 174.85 0.01 0.01 0.01 0.0 0.0 0.03 0.00 0.00 0.00 8

0.8 0.15 0.2 0,00694444 6.595 167.6 0.01 0.01 0.01 0.0 0.0 0.03 0.01 0.01 0.00 9

3.3 0.17 0.2 0.00925926 6.73 156.95 0.01 0.02 0.01 0.0 0.0 0.04 0.01 0.01 0.01 10 1.7 0.22 0.3 0.01041667 6.805 155.95 0.02 0.02 0.01 0.1 0.0 0.04 0.01 0.01 0.01 11 5.0 0.25 0.3 0.013888889 6.935 162.6 0.02 0.03 0.02 0.1 0.0 0.06 0.01 0.01 0.01 12 10.0 0.33 0.5 0.020833333 7.07 166.75 0.04 0.05 0.04 0.1 0.1 0.10 0.02 0.02 0.02 13 10.0 0.50 0.7 0.027777778 7.175 167.3 0.05 0.07 0.07 0.2 0.1 0.13 0.02 0.03 0.03 14 10.0 0.67 0.8 0.034722222 7.2 165 0.06 0.09 0.09 0.3 0.1 0.17 0.03 0.04 0.04 1510.0 0.83 1.0 0.041666867 7.2 162.35 0.08 0.11 0.11 0.3 0.2 0.20 0.04 0.05 0.05 16 5.0 1.00 1.1 0.045138889 7.2 161.9 0.08 0.12 0.12 0.4 0.2 0.22 0.04 0.06 0.06 17 17.0 1.08 1.4 0.056944444 7.2 163.15 0.11 0.15 0.15 0.5 0.2 0.27 0.05 0.07 0.07 18 34,7 1.37 1.9 0.081018519 7.2 163.85 0.15 0.21 0.22 0.7 0.3 0.39 0.07 0.10 0.11 19 33.3 1.94 2.5 0.104166667 7.2 162.6 0.20 0.28 0.29 0.9 0.4 0.50 0.09 0.13 0.14 20 16.7 2.50 2.8 0.115740741 7.2 161.65 0.22 0.31 0.32 1.0 0.5 0.56 0.10 0.15 0.15 21 33.3 2.78 3.3 0.138886889 7.2 161.95 0.26 0.37 0.38 1.1 0.6 0.67 0.13 0.18 0.18 22 16.7 3.33 3.6 0.150462963 7.2 162.25 0.28 0.40 0.41 1.2 0.6 0.73 0.14 0.19 0.20 23 23.3 3.61 4.0 0.166666667 7.2 162.3 0.31 0.44 0.46 1.4 0.7 0.80 0.15 0.21 0.22 24 60.0 4.00 5.0 0.208333333 7.2 161.95 0.39 0.55 0.58 1.7 0.9 1.00 0.19 0.27 0.28 25 60.0 5.00 6.0 0.250000000 7.2 160.75 0.46 0.66 0.69 2.0 1.1 1.20 0.22 0.32 0.33 26 30.0 6.00 6.5 0.270833333 7.2 159.75 0.50 0.71 0.74 2.2 1.1 1.29 0.24 0.34 0.36 27 90.0 6.50 8.0 0.333333333 7.2 159.5 0.61 0.86 0.76 2.7 1.1 1.58 0.29 0.41 0.36 28 960.0 8.00 24.0 1.000000000 7.2 151.95 1.70 2.18 0.90 6.8 0.4 4.39 0.82 1.05 0.43 29 1440.0 24.00 48.0 2.000000000 7.2 138.55 2.35 3.48 1.02 9.9 0.0 6.07 1.13 1.68 0.49 30 1440.0 48.00 72.0 3.000000000 7.2 128.35 2.35 4.40 1.09 10.6 0.0 6.07 1.13 2.12 0.53 31 2880.0 72.00 120.0 5.000000000 7.2 118.85 2.35 5.71 1.19 11.6 0.0 6.07 1.13 2.75 0.57 32 7200.0 120.00 240.0 10.000000000 7.2 108.85 2.35 7.91 1.34 13.0 0.0 6.07 1.13 3.80 0.65 33 14400.0 240.00 480.0 20.000000000 7.2 101.1 2.35 10.83 1.55 15.0 0.0 6.07 1.13 5.21 0.74 34 14400.0 480.00 720.0 30.000000000 7.2 96.05 2.35 12.76 1.70 16.5 0.0 6.07 1.13 6.14 0.82 Pool volume 73399.987 f13 2078.4562 m3

-w _2078456.2 L

40- __

NOTE: This calculation adjusts only the pool volume and aluminum quantity, and eliminates the marinite

XPS Summary Sample Identifier Sub A-wash unused sub A-wash vaporAwash unused yap A-wash Sub non A,&ah Sub unused not A-wash vap non Awh unused vap nrum A-wash Al 2p %

16*

1-4 82 0ls%

Cls%

4&.1 29.

335 5(L2 47.7 3L.6 S102 I54.0 Si 2s%

4.7 1.4 4.2 9.1 N ls%

2.3 2.

2A 1.3 P 2p%

Li 1.9 1.3 U.

Na2CO3 1072.7 Na Is%

8.S 0.3

&.7 A12p%

Os%

Cls%

114

47.

31.

7JA 48.Z M

32*

SU GA 30A 54.

7.*

411.0 30.

6.1 69.3 M37 5.5 3315 51.0 7A 49-4 Z9.7 43 44.S 33.1 Si2s%

4.7 1.*

S.0 44*

7*

U-0 N 1s%

2-5 2-1 1.2 1.9 P2p% Nals% Zn2p% CI2p%

S2p%

2 0.2 0.

1

0.

0.1 15 O4 0.2 2.0 0.7 0.2 0.2 Ca2p%

Fe2p%

Co2p% F15%

CIA 0.2 4.7 30.3 32.1

3.

2.1 3-3 0*.

3an 52*6 U

3.3 L9 44.7 3Z.7 SA 2.3 I.P 0.

43.3 34.7 11.2 2.2 1.4 0..

2.0 3.0 L9 2.3 2.9 3-5 Li1 1.1 0*

0.5 1.2 0*

OA4 0.2 0.3 0*11 015 0.2 0-9 CA U.

0.4 13 LI1 03 21A 0.3 Sub A-wash unused sub A-wash vapor A-wash unused vap A-wash Subnon A-wash Subunused not A-wash vap norn A-wash unused nap nuon A-wash AlZp%

17.9 20.4 15.1 11.9 12.6 12-2 14.2 7.2 01s%

68.4 67.1 689.

69.7 SiZs%

6.7 310 9.3 13.3 N 1s%

3.2 4A 3.1 2.3 PZp%

3.0 3.8 3.0 1.8 Na Is%

0.7 13 0.8 1.1 I

C

.9 a

a a

0

~a a-a..

P2psubmergednon wash 71.7 5.8 2.9 4.8 1.2 71.3 3.8 7.1 3.9 1.7 66.2 12.6 3.5 2.6 1.0 69.5 17.1 3A4 2.1 0.8 Sam lT AJ2p% I Ols%

S12s%

NlS%

P2 2%

Nals%

Su me 12.2 71.3

3.

7.1 3.9 7

lVo.P 7.2 69MS3 17.1 3.4 2,1 0.3 100.0 100.0 C-N=O NO N02 NO/Al, N03/N20 Sample Identifier Sub A-wash unused sub A-wash vapor A-wash unused yap A-wash 400.24083 30.5527 42.216967 45.4369 67.631133 402.5605 11.33939 9.84835 20.6921 9.450227 405.2 407.677 409.636 43.0909 15.017 45.7659 5.44528 30.7312 3.13969 21,2466 1.67211 c-C 284.896 54.8923 60.0041 52.6608 55.0534 C-N C-N=O/COOH 286 288.58 34.8 10.335 33.9 40.1 7.2684 31.9 13.068 P

C-O-PO AISiPOx AIPO4 Na3PO4 134 135.74 49.52 50.477 59.15 40.855 23.17 76.834 81.47 18.527 A1203/AI(OH)3 AIPO4 aluminan AIO(OH) A1203 74.467 75.2926 76.8307 77.922 21.995 46.6889 22.8212 8.4952 34.882 35.2147 21.5717 8.3317 8.5054 39.4153 26.9466 25.133 56.602 32.6624 10.7359 Non-acid washed samples Submerged Test sample 70.6241 9.884277 Submerged background san 91.S441 8.455885 Vapor Test sample 35.3401 21.68825 34.9259 Vapor backgound sample 100 Sub unused not A-wash 91.5441 8.455885 unused yap non A-wash 100 19.3874 0.1042 57.4947 30 12.504 61.0174 26.8 12.21 8.04576 51.7989 28.5 19.732 65,7832 22.8 11.399 10O 100 100 100 0

0 0

50.859 49.1406 57.971 42.0288 86.562 13.4376 83.147 16.8532 61.0174 26.8 12,21 100 0

57.971 42.0288 65,7832 22.8 11,399 100 0

83.147 16.8532

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