distribution sheet to distribution analytical services

/ f

DISTRIBUTION SHEET To From

ANALYTICAL SERVICES of 1

DISTRIBUTION From ANALYTICAL SERVICES Date: 03/06/95

Project Title/Work Order EDTNO.: EDT-610404 WHC-SD-WM-DP-097, Rev. 0, - "Tank Characterization 40-Day Crust Burn Report for Double Shell Tank 241-AW-101" ECN NO.: N/A

Name MSIN Text With all Attach

Addendum 1A Only

EDT/ECN Only

ONSITE Pacific Northwest Laboratory J. R. Gormsen K7-28 Westinahouse Hanford Company R. A. Esch T6-30 X G. D. Johnson S7-15 J. G. Kristofzski T6-06 X N. G. McDuffie S7-15 X P. Sathyanarayana R2-12 2 R. D. Schreiber R2-12 X Central Files L8-04 2 EDMC H6-08 X LTIC T6-03 OSTI L8-07 2 TFIC (Tank Farm Information Center) Rl-20

X X

DISCLAIMER

This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, make any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof.

DISCLAIMER

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MAK08 1395 55 W p ^

ENGINEERING DATA TRANSMITTAL Pag* 1 of.

1.EDT 610404 2. To: (Receiving Organization)

Distribution 3. From: (Originating Organization) Program Support

4. Related EOT Ho.:

N/A 5. Proj./Prog./Dept./Div.:

Tank 241-AW-101/Waste Hanagement/PS/AS

6. Cog. Engr.:

Ruth A. Esch 7. Purchase Order No.

N/A

8. Originator Remarks: This document is being released into the Supporting Document System for re t r ievabi l i ty purposes.

9. Equip./Component No.:

N/A 10. System/Bldg./Facility:

N/A 11. Receiver Remarks: For Release.

12. Major Assm. Dug. No.

N/A 13. Permit/Permit Application No.

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03/08/95 15. DATA TRANSMITTED ( F ) _i£L JJli. -iil. (A) Kern No.

(B) Document/Drawing No. (C)

Sheet No.

(D) Rev. No.

(E) Title or Description of Data Transmitted

Approval Designator

Reason for

Transmittal

Originator Disposition

Receiver

Disposition

WHC-SD-WM-DP-097 N/A Tank Characterization 40-Day Crust Burn Report for Double Shell Tank 241-AW-101

16. KEY Approval Designator (FJ Reason for Transmittal (G) Disposition (H) & (I)

E, S. Q. D or N/A (see WHC-CM-3-5, Sec.12.7),

1 . Approval 4. Review 2. Release S. Post-Review 3. Information 6. Dist. (Receipt Acknow. Required)

1. Approved 2. Approved w/comment 3. Disapproved w/comment

4. Reviewed no/comment 5. Reviewed w/comment 6. Receipt acknowledged

(G) (HI 17. SIGNATURE/DISTRIBUTION (See Approval Designator for required signatures)

(G) (H)

Reason

Disp. (J) Name (K) Signature (L) Date (M) MSIN (J) Name (K) Signature (L) Date (Ml MSIN Reason

Disp.

Cog.Eng. R. A. Esch />,.

Cog. Hgr. J. G. Kristofzski

QA EFnC u>. A . V\«>«i5>i£kc8.A

Safety

Env.

18.

A. E. Young

Signature q&EDT Originator

_2tkl5 Date

19.

Authorized Representative Dote for Receiving Organization

21. DOE APPROVAL (if required) Ctrl. No.

[] Approved [] Approved w/comments U Disapproved w/comments

BD-7400-172-2 (04/94) GEF097

BD-7400-172-1

<

RELEASE AUTHORIZATION

Document Number: WHC-SD-WM-DP-097, REV.O

Document Title: Tank Characterization 40-Day Crust Burn for Double Shell Tank 241-AW-101

Release Date: March 8, 1995

This document was reviewed following the procedures described in WHC-CM-3-4 and is:

APPROVED FOR PUBLIC RELEASE

WHC Information Release Administration Specialist:

£^7^04/? ~^/j£iJZ—> M a r c h 8 > 1995

/ yf ^ffa MT Broz

TRADEMARK DISCLAIMER. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise, does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof or its contractors or subcontractors. This report has been reproduced from the best available copy. Available in paper copy and microfiche. Printed in the United States of America. Available to the U.S. Department of Energy and its contractors from:

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Available to the public from: U.S. Department of Commerce National Technical Information Service (NTIS) 5285 Port Royal Road Springfield, VA 22161 Telephone: (703) 487-4650

A-6001-400.2 (09/94) WEF256

<r

SUPPORTING DOCUMENT 1. Total Pages

2. Title

Tank Characterization 40-Day Crust Burn for Double Shell Tank 241-AW-lOl

3. Number WHC-SD-WM-DP-097

4. Rev No. 0

5. Key Words Tank Characterization, 40-Day, Crust Burn, Double Shell Tank, Tank AW-101, Tank 241-AW-lOl, 241-AW-101, AW-101

6. Author

Name: Ruth A. Esch

Signature

Organization/Charge Code 8E480/MDR21

7. Abstract

N/A

RELEASE STAMP

OFFICIAL RELEASE BYWHC

DATE HAR 0 8 55 i <^tQL.

A-6400-073 (08/94) UEF124

<r

® Westinghouse Hanford Company

P.O. Box 1970 Richland, WA 99352

WHC-SD-WM-DP-097, REV. 0

ANALYTICAL SERVICES

Project: TANK CHARACTERIZATION 40-DAY CRUST BURN REPORT FOR DOUBLE SHELL TANK

Tank: 241-AW-101

Date Pr inted: MARCH 2, 1995

DISTRIBUTION OF THiS DOCUMENT IS UNLIMITED

54-7600475 Hanford Operations and Engineering Contractor for the US Department of Energy

<


TABLE OF CONTENTS

Narrative 1 Sample Data Summary 5 Undigested Sample Analyses - Direct 10

Differential Scanning Calorimetry Worklist #538 12 Worklist #539 21 Worklist # 540 . . . 27 Worklist #541 . 35 Worklist #547 39 Thermal Gravimetric Analyses Worklist #545 47 Worklist # 546 53 Worklist #548 59

This Document consists of pages 1 through 64.

ii


NARRATIVE

1

c

WHC-SD-WM-DP-097,REV.O 40 DAY CRUST BURN SAFETY ISSUE RESULTS FOR TANK 241-AW-101

AUGERS 95-AUG-001, 95-AUG-004, 95-AUG-005

Summary Three auger samples from tank AW-101 were received by the 222-S laboratories. They were analyzed to support the crust burn safety issue. No sample results exceeded the notification criteria. Sample Receipt and Extrusion Riser 13A One 10 inch auger (95-AUG-001) was used to sample the tank AW-101 contents at riser 13A. The sample was taken on 1/25/95, and received at the 222-S laboratory on 1/27/95. Extrusion took place on 2/7/95. The total amount of solid material recovered was about 78 grams. There was less than 5 mL of drainable liquid which was not recovered. Based on the texture and type of material sampled, the recovery is estimated to be 85%. Most of the solid was a damp, dark brown, sludge material that was located on all nine flutes, with the heaviest accumulation on flutes 7, 8 and 9. The sample found on flutes 1 through 3 (top of the auger) consisted of this sludge with crystalline, crust material dispersed throughout (approximately 26 grams of material). This material was sampled separately, designated as a facie (crust), and assigned sample number S95T000107. The sludge material from flute 4 was subsampled (approximately 3 grams collected), designated as the Upper Half, and assigned sample number S95T000102. The sludge material from flute 9 was subsampled (approximately 2 grams collected), designated as the Lower Half, and assigned sample number S95T000103. The remaining material from flutes 4 through 9 (approximately 49 grams recovered) was collected and saved for further analysis. The initial results for the crust burn safety issue (DSC and TGA) for Riser 13A appear on page 1 of Table 1 and in Table 2. The final report will contain all other analyses.

Riser 12A One 10 inch auger (95-AUG-004) was used to sample the tank AW-101 contents at riser 12A. The sample was taken on 1/26/95, and received at the 222-S laboratory on 1/27/95. Extrusion took place on 2/7/95. The total amount of solid material recovered was about 12 grams. There was less than 5 mL of drainable liquid collected. Based on the texture and type of material sampled, the recovery is estimated to be 60%. The solid was a damp, dark brown, sludge material that was located on flutes 4 through 9 only, with the heaviest accumulation on flutes 8 and 9. There was no crust material observed. The sludge material from flutes 5 and 6 was subsampled (approximately 0.5 grams collected), designated as the Upper Half, and assigned sample number S95T000110. The sludge material from flute 9 was subsampled (approximately 2 grams collected), designated as the Lower Half, and assigned sample number S95T000111. The remaining material from flutes 4 through 9 (approximately 10 grams recovered) was collected and archived. The initial results for the crust burn safety issue (DSC and TGA) for Riser 12A appear on page 2 of Table 1 and in Table 2. The final report will contain all other analyses.

2

WHC*SD-WM-DP-097,REV.O Riser 24B One 10 inch auger (95-AUG-005) was used to sample the tank AW-101 contents at riser 24B. The sample was taken on 1/27/95, and received at the 222-S laboratory on 1/27/95. Extrusion took place on 2/8/95. The total amount of solid material recovered was about 18 grams. There was less than 5 mL of drainable liquid which was not recovered. Based on the texture and type of material sampled, the recovery is estimated to be 60%. The solid was a damp, dark brown, sludge material that was located on flutes 6 through 10 only, with the heaviest accumulation on flutes 9 and 10. There was no crust material observed. The sludge material from flute 6 was subsampled (approximately 1 gram collected), designated as the Upper Half, and assigned sample number S95T000113. The sludge material from flute 10 was subsampled (approximately 3 grams collected), designated as the Lower Half, and assigned sample number S95T000114. The remaining material from flutes 6 through 10 (approximately 15 grams recovered) was collected and archived. The initial results for the crust burn safety issue (DSC and TGA) for Riser 24B appear on page 3 of Table 1 and in Table 2. Analytical Results

There are two result tables attached. The first, Table 1, is the summary table from the Laboratory Information Management System (LIMS). Table 2 provides additional calculated results for net exothermic energy and the total energy, requested by the Flammable Gas Safety Program cognizant scientist. The data used for these calculations was obtained from the summary report and additional information that is reported in the comment section for each sample in the LIMS.

TGA (Moisture)

The weight percent water by thermogravimetric analysis (TGA) was performed on a Mettler Model 20 thermogravimetric analyzer, using procedure LA-560-112 with an air purge. All samples results met the accuracy and precision criteria of 20%. The results were all within the range of 31.81% water to 42.46% water. There were no notification (action) limits for these analyses.

DSC

Differential thermal calorimetry (DSC) was performed using procedure LA-514-113, and a Mettler Model 20 differential scanning calorimeter under an air purge. There were no results which exceeded the notification limit of 586 Joules/g. One sample (S95T000107) exceeded the precision limit of 20%. This sample was from the portion of Riser 13A that consisted of crust material mixed with sludge. The initial sample result was 86.4 Joules/g and the duplicate was 0 Joules/g. A third sample was run giving a result of 111.3 Joules/g, which was reported as the duplicate in the summary report. The duplicate had a second endotherm at 300°C that did not appear in the other two analyses. No further reruns were requested due to the small exotherm, the dose rate and the heterogeneous nature of this sample. All samples met the accuracy criterion of 20%.

3

<• t

WHC-SD-WM-DP-097, REV. 0 Sample S95T000102, collected from Riser 13A just below the crust layer, produced three exotherms. The first was 14.7 Joules/g, the second 30.5 Joules/g, and the third 77.7 Joules/g. The sum of the three is reported in Table 1. The dry weight calculations for the exothermic energy were calculated using the sum of all measured exotherms. The sample result for dry weight was calculated using the percent water result reported as sample, and the duplicate used the percent water result reported as duplicate. Due to the heterogeneous nature of these samples, this method of calculation may introduce an additional precision error. This is exemplified in sample S95T000102 by the increase in the relative percent deviation (RPD) between the sample and duplicate from 11.5% for exothermic energy based on wet weight to 23.3% based on dry weight. Since the duplicate result for sample number S95T000107 was 0 Joules/g, the result of 111.3 Joules/g, measured on the third sample portion, was used for the dry weight calculation for the duplicate.

Reference WHC-SD-WM-TP-229, REV. 0, "Tank 241-AW-101 Tank Characterization Plan", dated November 22, 1994, Westinghouse Hanford Company, Richland, WA 99352

4

jf I


SAMPLE DATA SUMMARY

5

06-mar-1995 11:58:06 A-0002-1

Page: 1

Table 1: 40 DAY CRUST BURN SAFETY ISSUE RESULTS AW-101

CORE NUMBER: n/a SEGMENT #: 95-AUG-001 SEGMENT PORTION Facie

Sample* R A# Analyte Unit Action Limits

Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% Sample* R A# Analyte Unit Lower Upper Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% S95T000107 % Water by TGA using Mettler % n/a n/a 98.67 n/a 41.33 41.01 41.17 0.78 n/a 0.000 n/a S95T000107 DSC Exotherm Dry Calculated Joules/g Dry n/a :;$8&;$QS: n/a n/a 147 189 168.0 25.0 n/a 0.000 n/a S95T000107 DSC Exotherm using Mettler Joules/g n/a n/a 105.4 n/a 86.4 111.3 98.85 25.2 n/a 0.000 n/a SEGMENT PORTION: U Upper Half of Segment


Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% Sample* R A# Analyte Unit Lower Upper Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% S95T000102 % Water by TGA using Mettler % n/a n/a 98.67 n/a 38.82 37.24 38.03 4.15 n/a 0.000 n/a S95T000102 DSC Exotherm Dry Calculated Joules/g Dry n/a ;*5&™e: n/a n/a 201 159 180.0 23.3 n/a 0.000 n/a S95T000102 DSC Exotherm using Mettler Joutes/g n/a n/a 105.4 n/a 122.9 99.6 111.2 20.9 n/a 0.000 n/a

SEGMENT PORTION: L Lower Half of Segment


Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% Sample* R A# Analyte Unit Lower Upper Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% S95T000103 % Water by TGA using Mettler % n/a n/a 98.56 n/a 39.94 40.62 40.28 1.69 n/a 0.000 n/a S95T000103 DSC Exotherm Dry Calculated Joules/g Dry n/a ISS&H® n/a n/a 190 217 203.5 13.3 n/a 0.000 n/a S95T000103 DSC Exotherm using Mettler Joules/g n/a n/a 103.0 n/a 114 128.9 121.5 12.3 n/a 0.000 n/a

=> Limit violated => Selected Limit

<T»

06-mar-1995 11:58:23 A-0002-1

Page: 2


CORE NUMBER: n/a SEGMENT #: 95-AUG-004

SEGMENT PORTION U Upper Half of Segment


Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% Sample* R A# Analyte Unit Lower Upper Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% S95T00O110 % Water by TGA using Mettier % n/a n/a 98.56 n/a 41.90 42.13 42.02 0.55 n/a 0.000 n/a S95T000110 DSC Exotherm Dry Calculated Joules/g Dry n/a •^MMsm n/a n/a 175 193 184.0 9.78 n/a 0.000 n/a S95T000110 DSC Exotherm using Mettler Joules/g n/a n/a 103.0 n/a 101.5 111.6 106.5 9.48 n/a 0.000 n/a SEGMENT PORTION: L Lower Half of Segment

Sample# R A# Analyte Unit Action Limits

Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% Sample# R A# Analyte Unit Lower Upper Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% S95T000111 % Water bv TGA using Mettler % n/a n/a 97.91 n/a 39.21 38.75 38.98 1.18 n/a 0.000 n/a S95T000111 DSC Exotherm Dry Calculated Joules/g Dry n/a MSSil^ n/a n/a 119 114 116.5 4.29 n/a 0.000 n/a S95T000111 DSC Exotherm using Mettler Joules/g n/a n/a 104.4 n/a 72.4 69.8 71.10 3.66 n/a 0.000 n/a


< ! O o

o -a <b to

ID rn

06-mar-1995 11:58:35 A-0002-1

Page:

CORE NUMBER: n/a SEGMENT #: 95-AUG-005


SEGMENT PORTION U Upper Half of Segment


Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% Sample* R A# Analyte Unit Lower Upper Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% S95T000113 % Uater by TGA using Mettler % n/a n/a 97.91 n/a 31.81 35.80 33.80 11.8 n/a 0.000 n/a S95T000113 DSC Exotherm Dry Calculated Joules/g Dry n/a i^^i n/a n/a 248 270 259.0 8.49 n/a 0.000 n/a S95T000113 DSC Exotherm using Mettler Joules/g n/a n/a 104.4 n/a 168.9 173.1 171.0 2.46 n/a 0.000 n/a

SEGMENT PORTION: L Lower Half of Segment

Sample# R A# Analyte Unit Action Limits

Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% Sample# R A# Analyte Unit Lower Upper Standard % Blank Result Duplicate Average RPD % Spk Rec % Det Limit Count Err% S95T000114 % Water by TGA using Mettler % n/a n/a 99.43 n/a 42.46 38.13 40.30 10.7 n/a 0.000 n/a S95T000114 DSC Exotherm Dry Calculated Joules/g Dry n/a sSSMQa; n/a n/a 177 162 169.5 8.85 n/a 0.000 n/a S95T000114 DSC Exotherm using Mettler Joules/g n/a n/a 102.6 n/a 101.8 100.1 100.9 1.68 n/a 0.000 n/a


0a o

o

s

Table 2: Additional Calculated Results for Tank 241-AW-101 Crust Burn Flammable Gas Safety Issue

95-AUG-001 Riser 13A

Sample # Segment Portion

Net Exothermic Energy (Joules/g Dry)

Net Exothermic Energy (Joules/g)

Net Endothermic Energy (Joules/g)

Total Energy (Joules/g)

Notification Limit 586.6

S95T000107 Facie (Crust) 147.0 86.40 1285 -1198

S95T000102 Upper half sludge 201.0 122.9 1129 -1006

S95T000103 Lower half sludge 190.0 114.0 842.1 -728.1

95-AUG-004 Riser 12A







S95T000110 Upper half sludge 175.0 101.5 1095 -993.4


95-AUG-005 Riser 24B







S95T000113 Upper half sludge 248.0 168.9 976.6 -807.7


t I


UNDIGESTED SAMPLE ANALYSES- DIRECT

10

LABCORE Data Entry Template for Worklist# 583

Analyst: ^"""ffif/ Instrument: DSC01 Method:

Worklist Comment: Calculated AW-101 dry DSC. bdv

Seg Type Sample# RepAI Test Matrix

1 SAMPLE S95T000107 0 DSC-02 SOLID

2 DUP S95T000107 0 DSC-02 SOLID







9 SAMPLE S 9 5 T 0 0 0 1 1 1 0 DSC-02 SOLID

10 DUP S 9 5 T 0 0 0 1 1 1 0 DSC-02 SOLID





LA-514-113- n/».f

Wt -T3A D& da r\T\J -Actual

III. 3

I1U

(00.1

Analyst Signature Q~

Final page for worklist # 583

41-33 41.0/

Analyst Signature

ty Date

Unit

m 122.3 3%.R2> Z0\ <¥\.f> 37.i4 159 H4.0 3QM i%

\i£.<\ 10.U Zil-101.5 M.% 1̂ 5

42-/3 1̂ 3 7 i l4 31.21 11̂ k°i.% 38.15 |i4 ! # . ? J/.g) 24? 173.1 3 5 ft) 5-70

m 38-13

Joule

Joule <* Joule

JouleT

Joule*"

Joule^

Joule*

Joule^

Joule^

Joule^

Joule

Joule*1

Joule

Joule


Data Entry Comments: «*. u-mH - 3bo-\«/g

Uh/& shown for QC (SPK) may not reflect the actual units.

1 1

Page: 1

LABCORE Data Entry Template for WorkhW 538 • »

Analyst: .bios Instrument: DSC01 Method: LA-514-113 B-l WorWist Comment: Please run AW-101 DSC UNDER AIR. bdv

WHC-SD-WM-DP-097, REV. 0 Seg Type Sample# RepAl Test Matrix Actual Found DL Unit

1 STD tWIHA DSC-01 SOLID AIH5 60.0 N/A T 1 ^ J o u l e

2 SAMPLE S 9 5 T 0 0 0 1 0 7

S 9 5 T 0 0 0 1 0 7

0

0

DSC-01

DSC-01

DSC-01

SOLID

SOLID

SOLID

N/A

•Or N/A

N/A

J o u l e

3 DUP

S 9 5 T 0 0 0 1 0 7

S 9 5 T 0 0 0 1 0 7

0

0

DSC-01

DSC-01

DSC-01

SOLID

SOLID

SOLID

8U 32M5

•Or N/A

N/A

J o u l e

4 STD

S 9 5 T 0 0 0 1 0 7

S 9 5 T 0 0 0 1 0 7

0

0

DSC-01

DSC-01

DSC-01

SOLID

SOLID

SOLID

8U 32M5 «#.?

N/A

N/A J o u l e "^

5 DUP2 S 9 5 T 0 0 0 1 0 7 0 DSC-01 SOLID ®(oA ///. -2 N/A J o u l e

6 SAMPLE S 9 5 T 0 0 0 1 0 2

S 9 5 T 0 0 0 1 0 2

0

0

DSC-01

DSC-01

SOLID

SOLID

N/A

I3.| J o u l e Hf

7 DUP

S 9 5 T 0 0 0 1 0 2

S 9 5 T 0 0 0 1 0 2

0

0

DSC-01

DSC-01

SOLID

SOLID I*? I3.| N/A J o u l e *


Analyst Signature ' « Q cJ Date

^ l^w ̂ - 3bu.Ws l<\

g( ia^.b^/a. S15TD00IQ^ prsduxx^ an wcfoihcrm ajr \*pcL ajiih ^ dilfa. M U l̂.Z /̂a ; -/hi Sample oJso JMUL Z ctfw .QMcrtfWmp ar\o aJc

^!6 TC arith a dllta, H- <l 30.5 JA *M Mo Unto shown for QC (SPK) may not reflect the actual units. ^ l ^ ' T ^ »u I m u. wxw u, VQ ^ ^ . ^ 1 Oih&r (U- 4 3 U ' G c0i+*i a fllttf* H ̂ ^ 7 . ? ^


Analyst: rWS

Worklist Comment: Please

Instrument: DSC01 Method: LA-514-113 - £ - (

run AW-101 DSC UNDER AIR. bdv WHC-SD-WM-DP-097, REV. 0

Seg Type

1 STD

2 SAMPLE

Sampled

S95T000107

S95T000107

S95T000102

S95T000102

Rep AI

0

0

0

0

Test

DSC-01

DSC-01

DSC-01

DSC-01

DSC-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

Actual

N/A

Found

30.0 8^4

DL

N/A

Unit

Joule

Joule

3 DUP

Sampled

S95T000107

S95T000107

S95T000102

S95T000102

Rep AI

0

0

0

0

Test

DSC-01

DSC-01

DSC-01

DSC-01

DSC-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

01.1 N/A

Found

30.0 8^4

N/A

N/A

Joule

4 SAMPLE

Sampled

S95T000107

S95T000107

S95T000102

S95T000102

Rep AI

0

0

0

0

Test

DSC-01

DSC-01

DSC-01

DSC-01

DSC-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

01.1 N/A

N/A

N/A

Joule

5 DUP

Sampled

S95T000107

S95T000107

S95T000102

S95T000102

Rep AI

0

0

0

0

Test

DSC-01

DSC-01

DSC-01

DSC-01

DSC-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

N/A

N/A Joule

IX Analyst Signature

«™&Z^ -


2-/£-<r.r Date

Data Entry Comments:

Units shown for QC (SPK) may not reflect the actual units. Page:

13

DSC STD wm 6.465 mg Rate: 10.0 *C/min

File: 00035.001 Ident: 0.0

DSC METTLER i2-Feb-95 222-S Laboratory

Integration Delta H 194 mJ

30.0 J/g Peak 158.6*C

-14.5 mW o CO o o

m

SIGNATURE BELOW REPRESENTS CHEMICAL TECHNOLOGIST/CHEMIST THAT COMPLETED/VERIFIED THE CALIBRATION/ANALYSIS ON PAGES 14 TO 20

120 140. 160 180 'C

-iv-VJ"

DSC STD 12N14A F i le : 00057.001 DSC METTLER 13--Feb-95 6.465 mg Rate: 10 0 *C/min Ident: 0. 0 222-•S Laboratory

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1 i I t I I I I I t l i It I I 11 11 li li

Delta

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H 192 mJ 2 9 . 7 J / g

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P-097, REV. 0

i 1 1 i - '"T" 1 ' i 1 ' l 1 •

120. 140 . 160 . 180 . •c

)

AjJLh-^t

S95T000107 AIR 17.406 mg Rate: 10.0 *C/min

F i le : 00037.001 DSC METTLER Ident: 0.0 222-S Laboratory

• i

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^ — 1 1

12-Feb-95

BEST AVAILABLE COPY

Integration' Delta H 1504

86.4 Peak 399.6'

3.0

Integration Delta H22360 mJ

1284.6 J/g Peak 132.9*C

-53.2 mW

mJ J/g c mW

o CO

to

m

i 1 1 1 1 r

100. — I — 400. •c 200. 300

S95T000107(DUP) AIR 23.346 mg Rate: 10.0 *C/min

Fi le :00039.001 Ident: 0.0

DSC METTLER 222-S Laboratory

12-Feb-95


91.1 J/g Peak 302.4*C

-13.0 mW o en o

o

o

100 200 300 400 "C

S95T000107 (DUP2) AIR 19.4B1 mg Rate: 10.0 *C/min

F i l e : 00058.001 Ident : 0.0

DSC METTLER l3-Feb-95 222-S Laboratory


1077.3 J/g Peak 132.7'C

-55.4 mW


1 i i. 3 J, g Pea* 3?5.7*C

4.8 mW

BEST AVAILABLE COPY o CO

o

o

<o

m o

100. 200 300 " ~ 1 — 400. •c

S95T000102 21 .990 mg

A o x Q)

AIR Rate: 10.0 *C/min

F i l e : 00041 .001 Ident: 0 . 0


12-Feb-95

3: E

O in


14.7 J/g Peak 241.3' •c

1.7 mW

J™ Del ta H 671

30.5 Peak 315.7

5.6

I n t e g r a t i o n Del ta H24831 mJ

1129.2 J/g Peak 130. r c

-63 .8 mW

mJ J/g C mW Integration Delta H 1708

77.7 Peak 431

4 6 5

DO

o mJ J/g C mW

100. 200. 300. 400. •c


F i l e : 00043.001 DSC METTLER 12-Feb-95 Ident : 0.0 222-S Laboratory

317 .6 3 . 3

c mW

10

o in

nnrn^_

BEST AVAILABLE COPY


983.9 J/g Peak 130.5' 'C

-57.3 mW

o CO

o to

a Integration Delta H 1139 mJ

62.3 J/g Peak 421.6'C

2.9 mW

100. 200. 300. ~~1— 400. 'C


Seg Type Sample? Rep Al Test

1 STD I2AMMA DSC-01

2 SAMPLE S95T000103 0 DSC-01

3 DUP S95T000103 0 DSC-01

4 SAMPLE S95T000110 0 DSC-01

5 DUP S95T000110 0 DSC-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

Actual

4 MS Found

J1A

%d^2^>_ "/. I ^uJ^, Analyst Signature

^ >


'^[{mirnd^ (duru-

Date

N/A

/

^

Analyst: "^Jfttf Instrument: DSC01 Method: LA-514-113 / / S /

Worklist Comment: Please run AW-101 UNDER AIR. bdv WHC-SD-WM-DP-097, REV. 0 DL Unit

N/A m.o

101.5 I I I . b

m.o m.o

101.5 I I I . b

N/A

N/A

m.o

101.5 I I I . b 10/.5

m.o

101.5 I I I . b N/A

Joule

Joule

Joule

Joule

Joule


- ]Q£ I \^AJoX^ Z12UP5.

Units shown for QC (SPK) may not reflect the actual units. 21

DSC STD I2WM/4 6.465 mg Hate: 10.0 *C/min

F i l e : 00046.001 DSC METTLER 13-Feb-95 Ident : 0.0 222-S Laboratory


29.3 J/g Peak 158.7"C

-13.7 mW

SIGNATURE BELOW REPRESENTS CHEMICAL TECHNOLOGIST/CHEMIST THAT COMPLETED/VERIFIED THE CALIBRATION/ANALYSIS ON PAGES 22 TO 26 .

_, , j r

140 .

o t

CO o

o

120 180

'Y. yj£*J''fern^ *C

< z ^

2 / 2 2 / ^


File: 00051.001 Ident: 0.0


Integration Delta H15364

1094.S Peak 135.4'

-37.8


1 1 4 . 0 J / g Peak 3 1 5 . 6 ' C

4 . 3 rnVi

BEST AVAILABLE COPY

mJ J / g C mW

9 CO o

o

J*4

m

100 ~ " 1 — 200.

~ I — 3 0 0 .

~ ~ I — 4 0 0 . # C


File: 00053.001 Ident: 0.0


13-Feb-95


5 .9 J /g Peak 2 3 1 . l ' C

- 1 . 8 mW

Integral ion f j t l t a H P.iAS mJ

i ? 8 . 9 J / g t rf Ps 3 2 1 ,~ '*C

6 . ~i ml

BEST AVAILABLE COPY Integration Delta H16539 mJ

993.3 J/g Peak 141.0*C

- 4 4 . 6 mW

o CO

5 CO

m .<: o

100. 200 300. 400. •c


File: 00047.001 Ident: 0.0


en

EST AVAILABLE COPY

CO

o

o •D <S > l

m . < o

100 — 1 — 200. 3 0 0 . 4 0 0 . %C


File: 00049.001 Ident: 0.0

DSC METTLER 13-Feb-95 222-S Laboratory

IS) (7).

3* o

I

o

EST AVAILABLE COPY

o

m :< o

I n t e g r a t i o n Del ta H 6677 mJ

623.4 J /g Peak 124.4*C

- 1 7 . 5 mW

100. ~ ~ l — 200.

~ ~ 1 — 300.

_ _ 1 —

400. *C


Analyst: DUB Instrument: DSC01

WorkMst Comment: Please run AW-101 UNDER AIR. bdv

Seg Type Sample# RepAI Test Matrix

1 STD \2titt-A DSC-01 SOLID


3 DUP S 9 5 T 0 0 0 1 1 1 0 DSC-01 SOLID


5 STD 12-MlH-A DSC-01 SOLID

6 DUP S 9 5 T 0 0 0 1 1 3 0 DSC-01 SOLID

Method: LA-514-113 B ' l

WHC-SD-WM-DP-097, REV. 0 Actual Found DL Unit

J17A5 S°iA N/A -*•£. H


Analyst Signature 0

Verifcrn ^ 1 ^ ^ ^ r Date

^ / / ? 5 "

N/A Joule^

Joule^

1lA 6^-ff N/A Joulef

N/A \loB -^ Joule"*

N/A Joule 5*

\M>°I 173.1 N/A Joule-*

>f aw ̂ _s = jiouAes/«

ItaaE/rtry wwwtt. ^ 5 T D Q Q H j p r D 0 [ t L a ( ( faro J / V ^ Q ^ A W OlOg A> 13?-, 3°G

LUrJ-ffi QL djulfzc H ̂ ^18.1- ^/a^Quniih dudimd oJr 33-5.0°C yjiiha. (ktt(tW s^ ACS T/a. 395"Tt)0D//3 pwdMdul m wdoifaiMvi af 135",2'6 Units Shoffar QC (SPK) may not reflect the actual units. UJJTrl A flUTO, n ^ ^rh.b fa Page: I

27 °


Analyst: Instrument: DSC01

Worklist Comment: Please run AW-101 UNDER AIR.

Method: LA-514-113 £ - 1

bdv WHC-SD-WM-DP-097, REV. 0

Seg Type

1 STD

Sample# Rep Al

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 3 0

S 9 5 T 0 0 0 1 1 3 0

Test

DSC-01

DSC-01

DSC-01

DSC-01

DSC-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

Actual Found DL

N/A

N/A

N/A

Unit

J o u l e

2 SAMPLE

Sample# Rep Al

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 3 0

S 9 5 T 0 0 0 1 1 3 0

Test

DSC-01

DSC-01

DSC-01

DSC-01

DSC-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

N/A

DL

N/A

N/A

N/A

J o u l e

3 DUP

Sample# Rep Al

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 3 0

S 9 5 T 0 0 0 1 1 3 0

Test

DSC-01

DSC-01

DSC-01

DSC-01

DSC-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

DL

N/A

N/A

N/A

J o u l e

4 SAMPLE

Sample# Rep Al

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 3 0

S 9 5 T 0 0 0 1 1 3 0

Test

DSC-01

DSC-01

DSC-01

DSC-01

DSC-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

N/A

DL

N/A

N/A

N/A

J o u l e

5 DUP

Sample# Rep Al

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 3 0

S 9 5 T 0 0 0 1 1 3 0

Test

DSC-01

DSC-01

DSC-01

DSC-01

DSC-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

DL

N/A

N/A

N/A

J o u l e

Analyst Signature


2-/g- <rT-Date


Units shown for QC (SPK) may not reflect the actual units. Page: 1

DSC STD IzMW'A 6.465 mg Rate: 10.0 'C/mln

File:00076.001 Ident: 0.0

DSC METTLER 18-Feb-95 222-S Laboratory

E o


29.7 J/g Peak 158.5*C

-14.0 mW

SIGNATURE BELOW REPRESENTS CHEMICAL TECHNOLOGIST/CHEMIST COMPLETED/VERIFIED THE CALIBRATION/ANALYSIS ON PAGES 29 TO 34

~ T ™ ~ 120.

9 CO

o CO

m <£ O

140 160. 180. *C

S95T000111 AIR 16.623 mg Rate: 10.0 * C/min

F i le : 00077.001 DSC METTLER i8-Feb-95 Ident: 0.0 222-S Laboratory


20.5 J/g Peak 233.0*C

-4.6 mW


978.7 J/g Peak 137.2*C

-39.5 mW


72 .4 J /g Peak 319 .7 'C

3 .8 mW

o CO

o -o <b

5S o

100. —T— 200. 300 400.

~T" *C

S95T000111 (DUP) AIR 80.028 mg Rate: 10.0 *C/min

T "

Fi le:00079.001 DSC METTLER i8-Feb-95 Ident: 0.0 222-S Laboratory

^yfiiV; . i • * 1


31.0 J/g Peak 232.8'C

-7.5 mW

100.


961.5 J/g Peak 134.6*C

-48.0 mW

T 200. 300


69.8 J/g r L d ix 317 7*C

D . b mw

BEST AVAILABLE COPY

4 0 0 .

CO o

o <b

rn .<

_ ~ J >

r S95T000113 AIR 17.158 mg Bate: 10.0 *C/min

Fi le: 00081.001 Ident: 0 .0



976.6 J/g Peak 135.2"C

-40.3 mW

Integration Delta H 2 8 Si 7 mJ

168.3 J/g Peak 3?i,?"C

5.2 mW

BEST AVAILABLE COPY 9 CO o

I

o _"vl ID

rn o

T

100. 2 0 0 . 3 0 0 . — 1 _

4 0 0 . •c

DSC STD 12N14-A 6.465 mg Rate: 10.0 *C/min

File: 00083.001 DSC METTLER l9~Feb-95 Ident: 0.0 222-S Laboratory

I n t e g r a t i o n D e l t a H 185 mJ

28 .6 J /g Peak 158.9*C

- 1 3 . 5 mW o CO

o

2 ID m . < o

160. 120. 140. 180. *C

UJolZX ^ t^-^

S95T000113(DUP)AIR 24.605 mg Rate: 10.0 *C/min

3: £

O in


1043.1 J/g Peak 131.6*C

-70.9 mW

T ™

100. 200.

F i le : 00085.001 DSC METTLER l9-~Feb-95 Ident: 0.0 222-S Laboratory


173.1 J/g Peak 3?i.9*C

8.7 mW

BEST AVAILABLE COPY

o CO

o

to

m

300. -T——T"

400. - C J


Analyst: •^tP Instrument: DSC01

Worklist Comment: Please run AW-101 UNDER AIR. bdv

Method: LA-514-113/^-^- fa/is

WHC-SD-WM-DP-097, REV. 0 Seg Type

1 STD

2 SAMPLE

3 DUP

Sample# Rep Al

S95T000114 0

S95T000114 0

Test

DSC-01

DSC-01

DSC-01

Matrix Actual Found

N/A ici.g SOLID

SOLID IOL6 (00.1


Analyst Signature

Venfe (g^ (W— 0-YaJk^>-^

Date

DL Unit

SOLID o?f, *^5 <^<?- 2- N/A Joule

Joule

N/A Joule

-Hf u.m-V-s = -i^u-\£.%j.

Data Entry Comments: :S4swoons prodjucjicL -hjoo jmclo-Uwrmv cm aJr \3o,3*c tnfffia. (idJtvL H of ^-8^/j oM^k MtmcL /g.o J/j oJ- £35.z°c


35

DSC STD l^m 6.465 mg Rate: 10.0 *C/min

File:00061.001 Ident: 0.0

DSC METTLER -±4=-Feb-95

BEST AVAILABLE COPY

SIGNATURE BELOW REPRESENTS CHEMICAL TECHNOLOGIST/CHEMIST THAT COMPLETED/VERIFIED THE CALIBRATION/ANALYSIS ON PAGES 36 TO

T

222-S Laboratory ^ C | « , 5

I n t e g r a t i o n D e l t a K 189 mJ

9.9.2 J / 'g Peak 5 8 . 7 * C

-i?.

o I

v>

•

38


File: 00062.001 Ident: 0.0


i4^Feb-95

! ! t

!

. i MM i i

ii tf i ; 1 , i ; i? V '< U • :

S/8 X 1 5 »/ S \« B ! y • \f

' !..!..!

u Integration / Delta H 205 mJ ' 18.0 J/g

Peak 235.2* c ~2.5 mW

Integration Oelta H10922 mJ

956.8 J/g Peak 130.3*C

-21.4 mW

.Hi L q r a i i o n ijf.-;.. •.. d r: „ :'.bf- rr-'u

10 1 .6 J 'g

3 . 9 mW

3EST AVAILABLE COPY

HI o

I CO

o -a <b to

3 o

100. 200. ~ ~ l — 300.

~~! 400. *C


F i le : 00064.001 Ident: 0.0


A O X 0)

e

o CM

a-TT"


23.0 J/g Peak 235.0'C

-5.6 mW

Integr "•ation Del ta H16695 mJ

876.9 J /g Peak 137.2 ' 'C

- 4 0 . 0 mW

Integration l.'e?. ta r' 190b mJ

' 100 . 1 u/'n Peak. 323.8*C

BEST AVAILABLE COPY

o CO o

o <b

m o

100. 200. ~ 1 — 300.

" 1 — 400. •c


Analyst: b^S


Instrument: TGA01 Method: LA-560-112 A ~Z.

run AW-101 TGA UNDER AIR. bdv WHC-SD-WM-DP-097, REV. 0

Seg Type

1 STD

Sample*

S 9 5 T 0 0 0 1 1 1

S 9 5 T 0 0 0 1 1 1

S 9 5 T 0 0 0 1 1 3

42.M8-A

S 9 5 T 0 0 0 1 1 3

RepAl

0

0

0

0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

SOLID

Actual

N/A

Found

51.1 S" 6°iZ\

38.15 31.81 51.^5 35.80

DL

N/A

Unit

%

2 SAMPLE

Sample*

S 9 5 T 0 0 0 1 1 1

S 9 5 T 0 0 0 1 1 1

S 9 5 T 0 0 0 1 1 3

42.M8-A

S 9 5 T 0 0 0 1 1 3

RepAl

0

0

0

0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

SOLID

Actual

N/A

Found

51.1 S" 6°iZ\

38.15 31.81 51.^5 35.80

%

3 DUP

4 SAMPLE

Sample*

S 9 5 T 0 0 0 1 1 1

S 9 5 T 0 0 0 1 1 1

S 9 5 T 0 0 0 1 1 3

42.M8-A

S 9 5 T 0 0 0 1 1 3

RepAl

0

0

0

0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

SOLID

N/A

Found

51.1 S" 6°iZ\

38.15 31.81 51.^5 35.80

N/A

N/A

%

5 STD

Sample*

S 9 5 T 0 0 0 1 1 1

S 9 5 T 0 0 0 1 1 1

S 9 5 T 0 0 0 1 1 3

42.M8-A

S 9 5 T 0 0 0 1 1 3

RepAl

0

0

0

0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

SOLID Si.81

Found

51.1 S" 6°iZ\

38.15 31.81 51.^5 35.80

N/A

N/A %

6 DUP

Sample*

S 9 5 T 0 0 0 1 1 1

S 9 5 T 0 0 0 1 1 1

S 9 5 T 0 0 0 1 1 3

42.M8-A

S 9 5 T 0 0 0 1 1 3

RepAl

0

0

0

0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

SOLID Si.81

Found

51.1 S" 6°iZ\

38.15 31.81 51.^5 35.80 N/A %


Analyst Signatured (_J n~*~ Date

\ aJkn^wi^


Units shown for QC (SPK) may not reflect the actual units. • J < 4 Page:


Analyst: £$uK Instrument: TGA01 Method: LA-560-112 -4= A-Worklist Comment: Please run AW-101 TGA UNDER AIR. bdv

Analyst: £$uK Instrument: TGA01 Method: LA-560-112 -4= A-Worklist Comment: Please run AW-101 TGA UNDER AIR. bdv

Seg Type

1 STD

Sample# Rep Al

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 3 0

S 9 5 T 0 0 0 1 1 3 0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

Actual Found DL Unit

N/A %

2 SAMPLE

Sample# Rep Al

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 3 0

S 9 5 T 0 0 0 1 1 3 0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

N/A %

3 DUP

Sample# Rep Al

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 3 0

S 9 5 T 0 0 0 1 1 3 0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

N/A %

4 SAMPLE

Sample# Rep Al

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 3 0

S 9 5 T 0 0 0 1 1 3 0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

N/A %

5 DUP

Sample# Rep Al

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 1 0

S 9 5 T 0 0 0 1 1 3 0

S 9 5 T 0 0 0 1 1 3 0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID N/A %


?-/*~?J-Date


Date £nfry Comments:

Units shown for QC (SPK) may not reflect the actual units. 40

Page: 1

4*

TGA STD 42/J&-A File: 00075.001 TG METTLER 17-•Feb-95 ie i.595 mg Rate: 10.0 *C/min Ident: 0.0 222-S Laboratory

^ s . S t e p A n a l y s i s H e i g h t - 9 . 5 8 mg

- 5 7 . 7 5 % R e s i C . 7 . 0 1 mg

4 2 . 2 5 % Dpeak B3.0*C

D) p E GO <?

in

WM-DP-097, RE

?c

•

o

SIGNATURE BELOW REPRESENTS CHEMICAL TECHNOLOGIST/CHEMIST THAT COMPLETED/VERIFIED THE CALIBRATION/ANALYSIS ON PAGES 4 1 TO 4 6 .

I.

1 j 1 1 i i 1 " i « "™! 1 1 I

5 0 . 100 . 1 5 0 . • i

•c

^/7 ^ J

S95T000111 AIR Fi le : 00078.001 TG METTLER 17-Feb-95 20.885 mg

j Rate: 10.0 #C/mln Ident: 0.0 222-S Laboratory

i\

Step Analysis Height - 8 . 1 9 mg

- 3 9 . 2 1 % ResiC. 12.70 mg |

D> 60.79 %

C-S

E Dpeak 105.0*C o •

in

\

i/VM-DP-097, REV.

o

T 1 1 r- —r T— T 1 1 — I — T - i i 1 — -i — i — T r . 1 . . . . , 100. 200. 300. 400. *C

S95T00011KDUP) AIR Fi le : 00080.001 TG METTLER 17-Feb-95 25.585 mg Rate:

i 10.0 *C/min Ident: 0.0 222-S Laboratory

K Step Analysis Height - 9 . 9 1 mg

- 3 8 . 7 5 % ResiC. 15.67 mg

61.25 %

WHC-SD-

CJ) E Dpeak 111.0'C § in

-DP-097, REV.

.

X i

o

i

o

*T 1 • I 1 1 1 1 i | i 1 i i I k i i • • i i i • 1 100. 200. 300. 400. •c

S95T000113 AIR 22.734 nig Rate: 10.0 *C/min

File: 00082.001 TG METTLER 17-Feb-95 Ident: 0.0 222-S Laboratory

CD E

in

Step Analysis Height -7.23 mg

-31.81 % ResiC. 15.50 mg

6 8 . 1 9 % Dpeak l l l . C T C

— » - • -

100. ~~T— 200.

~ i — — T ~ 1 r ~ T 300.

T r

O i

CO

o o

DO m O

~n— 400. •c

TGA STD 42N8-A File: 00084.001 TG METTLER l8-Feb-95 15.459 mg Rate: 10.0 *C/min Ident: 0.0 222-S Laboratory

T - i : j — ; "T- '—i ! 1 T ~ — j •—r — r — — 1 — — — T : j 1— 1 . ,- — r

5 0 . 100 . 1 5 0 . 'C

S95T000113(DUP)AIR Fi le : 00086.001 TG METTLER 18-Feb-95 24.736 mg Rate:

• < •

10.0 *C/min Ident: 0.0 222-S Laboratory

i\


-35 .80 % OHM

5.

mg ResiC. 15.88 mg

64.20 % Dpeak 113.O'C

-SD-WM-DP-097, REV.

o

T 1 1 1 1 1 1 1 i | i i t i i i I I • i I I • 1 1 100. 200. 300. 400. •c


Analyst: pud S


Instrument: TGA01 Method: LA-560-112-R—&• A-2.

run AW-101 TGA UNDER AIR. bdv W H C . S D . W M . D p ^ 7 p ^ ^ l *

Seg Type

1 STD

Sample?

S 9 5 T 0 0 0 1 0 7

S 9 5 T 0 0 0 1 0 7

S95TQ00102

S 9 5 T 0 0 0 1 0 2

RepAl

0

0

0

0

Test Matrix i

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

i j Actual

N/A

Found

58,40 Ml.33 m.oi 38.82-31.7A

DL Unit

N/A %

2 SAMPLE

Sample?

S 9 5 T 0 0 0 1 0 7

S 9 5 T 0 0 0 1 0 7

S95TQ00102

S 9 5 T 0 0 0 1 0 2

RepAl

0

0

0

0

Test Matrix i

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

i j Actual

N/A

Found

58,40 Ml.33 m.oi 38.82-31.7A

O

3 DUP

Sample?

S 9 5 T 0 0 0 1 0 7

S 9 5 T 0 0 0 1 0 7

S95TQ00102

S 9 5 T 0 0 0 1 0 2

RepAl

0

0

0

0

Test Matrix i

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

Hi. 33 N/A

Found

58,40 Ml.33 m.oi 38.82-31.7A

N/A %

4 SAMPLE

Sample?

S 9 5 T 0 0 0 1 0 7

S 9 5 T 0 0 0 1 0 7

S95TQ00102

S 9 5 T 0 0 0 1 0 2

RepAl

0

0

0

0

Test Matrix i

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

Hi. 33 N/A

Found

58,40 Ml.33 m.oi 38.82-31.7A

"5

5 DUP

Sample?

S 9 5 T 0 0 0 1 0 7

S 9 5 T 0 0 0 1 0 7

S95TQ00102

S 9 5 T 0 0 0 1 0 2

RepAl

0

0

0

0

Test Matrix i

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID

TGA-01 SOLID 388Z

Found

58,40 Ml.33 m.oi 38.82-31.7A N/A %


2 - /-2,-^LT Date

^ W x « ^ DValingJ^ 4 - ^ - 9 5

Ztaia £>z#y Comments:


47

TGA STD 4ZW8A F i l e : 00034.001 TG METTLER 12 -Feb-95 18.771 mg Rate: 10.0 *C/min Ident: 0.0 222-S Laboratory

•

i 1 j

1 ^ s .

Step Analys i s Height -10.96 mg

-58 .40 % %. ResiC. 7 .81 mg O

i 41.60 % o O) Dpeak 90.3*C E i

o # -a in

-097, REV.

^""""~*-»^ ^ ^ > ~ ^

o

SIGNATURE BELOW REPRESENTS CHEMICAL TECHNOLOGIST/CHEMIST THAT COMPLETED/VERIFIED THE CALIBRATION/ANALYSIS ON PAGES 4 8 TO 52 .

I i | i i i i | i i i i i i i i

5 0 . 1 0 0 . 1 5 0 . 1

"C

S95T000107 AIR F i l e : 00036.001 TG METTLER 12-Feb-95 IS 1.243 mg Rate: 10.0 *C/min Ident : 0.0 222-S Laboratory

\

Step Analysis -OHM

Ol Height - 7 . 9 5 mg o E - 4 1 . 3 3 %

W in ResiC. 11.29 mg

58.67 % Dpeak 105.O'C

\ •

-DP-097, REV. 0

'

' ' ' ' 1 ' 100.

» • • - — - — — - — • - - • • • . - — • — — — — — — • — — • — • • -

, _,. ..., ... . 1 — ...T_. ,,... , . , ,.. ,

200. 300. i | i r i

400. ' 1

•c


F i l e : 00038.001 Ident: 0.0

TG METTLER 12-Feb~95 222-S Laboratory

en E in

Step Analysis Height

ResiC.

Dpeak

-8.32 mg 41.01 % 11.97 mg 58.99 %

109.0' 'C

o I c/> o

a

100. 200 300. —\ 400.

S95T000102 AIR 20 .611 mg Rate: 10.0 *C/min

File:00040.001 Ident: 0.0

TG METTLER 12-Feb-95 222-S Laboratory

e

in


- 3 8 . 8 2 % ResiC. 12.61 mg

6 1 . 1 8 % Dpeak 117.0*C

100 2 0 0 .

o •

CO o

o -o <b CO

ID ss

3 0 0 . ~ T — 4 0 0 . 'C

S95T000102(DUP) AIR Fi le :00042.001 TG METTLER 12-Feb-95 2C .088 mg Rate: 10.( ) 'C/min Ident : 0.0 222-S Laboratory

\

Step Analysis

en

Height - 7 . 4 8 mg - 3 7 . 2 4 %

ResiC. 12.61 mg

WHC-S

OT E 62.76 % o

1 _

tt ID

\.

VM-DP-097, REV. 0 i

"1 1— "I 1 1 1 ' 1 " " 1 1 ' | i i i r— " i "i - - i 1 — T 1 1 1 1 " - ' 1 100. 200. 300. 400. "C


Analyst:

Worklist Co mment: Please

'instrument: TGA01 Method: 'LA-560-112./^-

run AW-101 TGA UNDER AIR. bdv

-9 A- z 6fc>V

Seg Type

1 STD

2 SAMPLE

Sample#

\\m-k S 9 5 T 0 0 0 1 0 3

S 9 5 T 0 0 0 1 0 3

S 9 5 T 0 0 0 1 1 0

S 9 5 T 0 0 0 1 1 0

RepAl

0

0

0

0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

Actual

N/A

Found

At bz 41%

4i.\5

DL

N/A

Unit

%

%

3 DUP

Sample#

\\m-k S 9 5 T 0 0 0 1 0 3

S 9 5 T 0 0 0 1 0 3

S 9 5 T 0 0 0 1 1 0

S 9 5 T 0 0 0 1 1 0

RepAl

0

0

0

0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

N/A

Found

At bz 41%

4i.\5

N/A %

4 SAMPLE

Sample#

\\m-k S 9 5 T 0 0 0 1 0 3

S 9 5 T 0 0 0 1 0 3

S 9 5 T 0 0 0 1 1 0

S 9 5 T 0 0 0 1 1 0

RepAl

0

0

0

0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID

N/A

Found

At bz 41%

4i.\5 %

5 DUP

Sample#

\\m-k S 9 5 T 0 0 0 1 0 3

S 9 5 T 0 0 0 1 0 3

S 9 5 T 0 0 0 1 1 0

S 9 5 T 0 0 0 1 1 0

RepAl

0

0

0

0

Test

TGA-01

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

SOLID 4*. r10

-42.12)

Found

At bz 41%

4i.\5 N/A "5

yam 6E>V

—^ Analyst Signature


,^-/^-7^> Date

/-95-

Data £ntry Comments:


Unity shown for QC (SPK) may not reflect the actual units. Page:

TGA STD H2.M8-A 15.357 mg Rate: 10.0 *C/min

F i l e : 00044.001 TG METTLER 12-Feb-95 Ident : 0.0 222-S Laboratory

-+

BEST AVAILABLE COPY

en

in


-58.34 % ResiC. 6.40 mg

41.66 % Dpeak 80.0'C

o I CO o

to

m :<

+ SIGNATURE BELOW REPRESENTS CHEMICAL TECHNOLOGIST/CHEMIST THAT I COMPLETED/VERIFIED THE CALIBRATION/ANALYSIS ON PAGES 54 TO ! 58

T T ~t r ~t r ~1 200.

T r 50 100 150. *C

S95T000103 AIR 10.541 mg Rate: 10 .0 *C/min

O) E

CM


- 3 9 . 9 4 % ResiC. 6 .33 mg

60 .06 % Dpeak 93.0*C

F i l e : 00048 .001 Ident: 0 . 0

TG METTLER 222-S Laboratory

12-Feb-95

9 CO

o

o CO

za m < : o

_J J J ( x { !

200. 300 100. I

400. *C

S95T000103(DUP) AIR File: 00050.001 TG METTLER 12-Feb-95 22.196 mg Rate:

• 10.0 *C/min Ident: 0.0 222-S Laboratory

i *

N T ~"t BEST AVAILABLE COPY

Step A n a l y s i s H e i g h t - 9 . 0 2 mg

- 4 0 . 6 2 % i OJ R e s i C . 13 .18 mg o E 59 .3B % CO

o in Dpeak 127 .0*C

WM-DP-097, RE

**" \ < :

+ \ •

\ i

o

1 I i 1

i i • • 1 i i i

100.

1 1 l 1 1 1 1 1 1 1 1 1 l l 1

2 0 0 . 3 0 0 . 4 0 0 . • 1

"C

S95T000110 AIR F i le : 00052.001 TG METTLER 12-Feb-95 7.301 mg Rate: 10.0 *C/min Ident : 0.0 222-S Laboratory

T 1 i 1 1 1 1 1 1 1 1 1 r 1 1 1 1 1 1 1 1 1 r

1 0 0 . 2 0 0 . 3 0 0 . 4 0 0 . *C

S95T000110 (DUP) AIR 19.890 mg

en E

in

Rate:10.0 *C/min F i le : 00054.001 TG METTLER Ident: 0.0 222-S Laboratory

12-Feb-95

ResiC


•A?.. 13 % 51 mg

0/ 5"7.B7' ,c Dpeak 97.0'C

BEST AVAILABLE COPY

o I

CO

o "O

m . < o

T r T 1 1 r T 1 1 r T r T r

100. 2 0 0 . 300 4 0 0 . •c


Analyst: SMF


Instrument: TGA01 Method: LA-560-112//?"^

run AW-101 TGA UNDER AIR. bdv WHC-SD-WM-DP-097, REV. 0

Seg Type

1 STD

Sample?

S95T000114

S95T000114

S95T000114

RepAl

0

0

0

Test

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

Actual

N/A

Found

SB.85 DL

N/A

Unit

%

2 SAMPLE

Sample?

S95T000114

S95T000114

S95T000114

RepAl

0

0

0

Test

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

Actual

N/A 4-ZAb %

3 DUP

Sample?

S95T000114

S95T000114

S95T000114

RepAl

0

0

0

Test

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

4-2.U

42 Ab

3S.\3 N/A %

4 DUP2

Sample?

S95T000114

S95T000114

S95T000114

RepAl

0

0

0

Test

TGA-01

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

SOLID

4-2.U

42 Ab M.n N/A %

Analyst Signature/u 0


Date

VerifoL h ' ^ U ; U V WuahjJih^

Date i&ziry Comments:


LABCORE Data Entry Template for Worklist# 548 < ' i -i

Analyst: ^'y^f Instrument: TGA01 Method: LA-560-112

Worklist Comment: Please run AW-101 TGA UNDER AIR. bdv WHC-SD-WM-DP-097, REV. 0

Seg Type

1 STD

Sample# Rep Ai

S 9 5 T 0 0 0 1 1 4 0

S 9 5 T 0 0 0 1 1 4 0

Test

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

Actual Found DL

N/A

Unit

a

2 SAMPLE

Sample# Rep Ai

S 9 5 T 0 0 0 1 1 4 0

S 9 5 T 0 0 0 1 1 4 0

Test

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID

N/A o

3 DUP

Sample# Rep Ai

S 9 5 T 0 0 0 1 1 4 0

S 9 5 T 0 0 0 1 1 4 0

Test

TGA-01

TGA-01

TGA-01

Matrix

SOLID

SOLID

SOLID N/A


Analyst Signature Date


Units shown for QC (SPK) may not reflect the actual units. Page:

60

TGA STD W&b File: 00060.001 TG METTLER 13 -Feb-95 16.259 mg Rate: 10.0 *C/min Ident: 0.0

. SIGNATURE BELOW REPRESENTS CHEMICAL TECHNOLOGIST/CHEMIST THAT 222-S Laboratory

J COMPLETED/VERIFIED THE CALIBRATION/ANALYSIS ON PAGES 6 1 TO 6 4 -

S t e p A n a l y s i s H e i g h t - 9 . 5 7 mg

- 5 8 . 8 5 % R e s i C . 6 . 6 9 mg

4 1 . 1 5 %

WHC-SI

5.

mg Dpeak 8 5 . 0 ' C

D-WM-DP-097, REV. 0

i •

1 1 i •

i l l i i i i i i • • i • i • i • 1 i I I •

50. 100. 150. /? ^ -7§00-n, sr. •c

c ^ 4lmfo5 m


E

OJ

Step A n a l y s i s H e i g h t - 4 . 5 6 mg

'-tC- , f C /C

ResiC. 5.3i mg

Doeak Sb.O'C

i 1 1 r

100. T — — r

2 0 0 .

File: 00063.001 TG METTLER i3-Feb-95 Ident: 0.0 222-S Laboratory

BEST AVAILABLE COPY

o I en o

o «b

33 a

1 1 1 1 1 1 1 1 1 1 r—

3 0 0 . 4 0 0 . *C


Step A n a l y s i s Height - 3 . 1 1 mg

- 3 8 . 1 3 % Res iC . 5 . 1 5 mg

63 .20 % Dpeak 91.0"C

E

cu

File: 00065.001 TG METTLER l3-Feb-95 Ident: 0.0 222-S Laboratory

o I

o

o

a

100 200. 300. 400. *C

S95T000114(DUP) AIR File: 00066.001 — — — - — — •

TG METTLER l3-Feb-95 12.110

•

mg Rate:10.0 *C/min Ident: 0.0 222-S Laboratory

i

! i i


- 4 1 . 7 7 % ResiC. 7 .27 mg o

i _ 60.00 % CO

o Dpeak 93.0*C i

2.

mg . i

i \ 1 \ A

i-DP-097, REV.

o

1 f

! 1 — . .„ — « — . .,.—, _.. 3—.._

\Kk fv / V \ f\A.I\j*ji\l\Aji ^^^

i I I t

T 1 1 ' 1 * i i i 1 i i i . , . . . . | - - - * • I

__ 100. 200. 300. 400. *C

distribution sheet to distribution analytical services

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