Text

Forwards Final Rept of Matl Properties of Neutron Shielding Matl to Be Used in Trojan ISFSI & Test Repts That Verified Matl Properties
	ML20196E285
Person / Time
Site:	Trojan File:Portland General Electric icon.png
Issue date:	11/25/1998
From:	Quennoz S; PORTLAND GENERAL ELECTRIC CO.
To:	Kobetz T; NRC OFFICE OF INFORMATION RESOURCES MANAGEMENT (IRM), NRC OFFICE OF NUCLEAR MATERIAL SAFETY & SAFEGUARDS (NMSS)
References
	VPN-076-98, VPN-76-98, NUDOCS 9812030091
	Download: ML20196E285 (82)
	v • d • e

\./ '

.? - -'

} } - l ~]

E <i a a Trojan Nuclear Plant i si *ric c - r 71760 Columbia RurHuy Rainier OR 97048 November 25,1998 (503)556-3713 VPN-076-98 l l

TrojanISFSI Docket 72-017 U. S. Nuclear Regulatory Commission Document Control Desk Washington, DC 20555 Attention: T. J. Kobetz, Project Manager NMSS, SFPO

Dear Sir:

Submittal of Tect Resu!ts for ISFSI Neutron Shielding Material Pursuant to our letter dated October 31,1998 (VPN-068-98), and discussions in our meeting with you on October 8,1998, enclosed are a final report of the material properties of the neutron

! shielding material to be used in the Trojan ISFSI and the test reports that verified the material properties. Enclosure 1 is the PGE Final Report of the Evaluation of Neutron Shielding Material. j Enclosure 2 are the two test reports prepared by Materials Engineering and Testing (ME&T) !

Corporation and includes the procedures used as well as a certificate of conformance.

l l If you have any questions regarding this information, please contact Joel Westvold of my staff at (503) 556-6485. l Sincerely, / 4

/

l gW

^11203oo91981125 I g tephen M. Quennoz 9

! PDR ADOCK 05000344' Vice President Nuclear Y PDRft l

l and Thermal Operations gp[

i Enclosures c: L. H. Thonus, NRC, NRR R. A. Scarano, NRC Region IV David Stewart-Smith, OOE Connecting People, Power and Possibilities ,-

I

l l Enclosure I to VPN-076-98 November 25,1998 l Page 1 of 30 ,

! Final Report l Evaluation of Neutron Shielding Material (RX244) 1

Background

The Trojan Independent Spent Fuel Storage Installation (ISFSI) Transfer Cask has been fabricated in accordance with PGE Specification TD-029 and Purchase Order NQ181906. The

design function and quality requirements ofindividual cask parts have been determined in l accordance with Trojan Engineering Technical Evaluation 9800001. The cask utilizes a neutron absorbing material for shielding, manufactured by Reactor Experiments and designated as number RX244. The material is provided as a dry powder to which water is added at the fabrication shop as the material is cast in place. Certain material characteristics, particularly -

hydrogen and boron concentration, are used as design input in ISFS1 radiation source strength,

! shielding, and dose rate calculations [ reference TI-003 (PGE01-10.02.01-03), TI-004 (PGE01-10.02.01-05), and TI-032 (PGE01-10.02.01-07)].

Since Reactor Experiments does not at present have a quality program that would allow their placement on PGE's Approved Suppliers List, it was decided to qualify the RX244 for use in the

Transfer Cask by chemical analysis of the material, combined with PGE surveillance of l manufacturing and testing activities. PGE QA and Engineering representatives witnessed the l manufacture of RX244 Lot #R0304 at the Reactor Experiments facility. A total of 6 barrels were

, produced for the Transfer Cask project, from which 6 samples (1 from each barrel) were taken by l the PGE team for chemical analysis. Each sample consisted of both dry powder and a 3 inch cube of cast material.

l After a lengthy search for a test lab that could perfonn the necessary chemical analyses, Materials Engineering and Testing (ME&T) Corporation of Oak Ridge, Tennessee, was selected l to perform the work. The scope of work included determination of boron concentration by l titration and inductively coupled plasma (ICP) techniques, and determination of hydrogen

! concentration by thermal conductivity using the Laboratory Equipment Company (LECO) analyzer and by thermal gravimetric analysis (TGA). Boron titrimetry and ICP were in ME&T's scope, while hydrogen by LECO was subcontracted to Galbraith Laboratories and hydrogen by TGA was subcontracted to the University of Tennessee. Dual test methods for each element l were desirable to demonstrate consistency in results.

! Two series of tests took place: Series #1 for the six samples cast at Reactor Experiments, and

Series #2 for three samples taken at the fabrication shop during actual mixing and place. ment of

, RX244 in the Trojan ISFSI Transfer Cask. Test Series #1 was used to release the material for l shipment and use, and Series #2 was used to verify previous results (particularly TGA) on l

l

.- l

! )

Enclosure 1 to VPN-076-98 l November 25,1998 l Page 2 of 30 Final Report Evaluation of Neutron Shieldine Material (RX244) material as mixed and placed in the cask.

Series #1 samples were cast on 7/21/98 at Reactor Experiments. Analysis for hydrogen content by TGA was performed on two of these samples on 9/16/98. Further TGA testing was performed on all six samples on 10/30/98. Series #2 samples were cast on 10/7/98 and tested by )

TGA on 11/3/98. l Sample Preparation Samples from Series #1 were allowed to air dry until the test date, with no special controls on environmental conditions, since no credit was planned for water of hydration freely lost at room temperature. Samples from Series #2, due to the much shorter time between the cast and test dates, were still moist when received at the test lab. Thus, it was necessary to dry the samples to prepare them for testing. The samples were dried at 100 C for 8 hours9.259259e-5 days 0.00222 hours 1.322751e-5 weeks 3.044e-6 months prior to testing. Original and final weights were recorded for two of the three samples. In each case, weight loss was !

highly dependent on where the small test sample was taken from the large 3-inch cube, since the l outer edge of the cube had dried considerably more than the internal volume.

l Test Results l

Test results are contained in two ME&T reports, which are enclosure 2 to this letter. A summary table of results is also attached for each test series. This table presents calculated values for water of hydration loss which may be compared to calculated results provided by the vendor. A sample (alternate) calculation is also attached for ME&T Sample #16621, along with TGA graphs for all samples marked up to show calculation inputs. l l

Boron concentration averaged 4.0 w/o by titration and 4.0 w/o by ICP in Series #1, above the 2.81 w/o value listed in the RX244 data sheet and used in the Transfer Cask shielding analysis.

Boron concentration averaged 3.2 w/o by titration and 3.0 w/o by ICP in Series #2, values lower than for Series #1 but above 2.81 w/o. A possible explanation may be the behavior of the RX244 when cast at the fabrication shop. The RX244 was observed to expand significantly as water was added, and set up quickly. On the advice of the vendor, additional water above the recommended mix proportion was added to produce a workable mixture. Density was measured as 109.7 pcf, ,

103.7 pcf, and 101.2 pcf at the three sample points. These values met the specification I requirement but fell below the nominal 112.0 pcf value listed on the RX244 data sheet.

i i

I Enclosure 1 to VPN-076-98 November 25,1998 Page 3 of 30 Final Report Evaluation of Neutron Shielding Material (RX244) l Hydrogen concentration averaged 3.3 w/o by LECO and 3.0 w/o by TGA in Series #1. Based on j

these results, which fall below the 4.22 w/o value listed in the RX244 data sheet, the Transfer Cask shielding analysis was revised to use an initial hydrogen content of 2.8 w/o, with a further reduction of 10% to model hydrogen loss at elevated temperature. The vendor's response to the )

hwer hydrogen values was that test conditions used for their published values differed from test conditions used for PGE's samples. Specifically, PGE's samples were allowed to dry in open air ;

over a long period of time, resulting in loss of water to the surrounding air. However, as noted previously, PGE's intent was to not credit this source of hydrogen.

In the TGA process, samples were heated fmm ambient to 800 C at a rate of 20 C/ min, with a 10 minute hold at 160 C. Water of hydration was observed to be lost in four distinct steps. The i amount of water lost in each step was fairly consistent between all Series #1 samples with the ,

exception of the first (lowest temperature) step. For the first step, the two samples tested on I 9/16/98 lost an average of 2.3 w/o H 2O (0.3 w/o H 2) whereas the samples tested on 10/30/98 lost an average of 0.18 w/o H2 O (0.0 w/o H 2). This suggests that the samples were still drying between these dates, and that most or all of the water in the first step is available to freely hydrate over time at room temperature. Testing in Series #2 demonstrates that a certain amount of water is available in the first step even after drying the sample at 100 C for 8 hours9.259259e-5 days 0.00222 hours 1.322751e-5 weeks 3.044e-6 months , suggesting that a certa'm equilibrium is attained with moist air.

Hydrogen concentration averaged 2.5 w/o by LECO and 2.6 w/o by TGA in Series #2. When water lost during the 100 C sample preparation process is accounted for in, Sample #17066 changes from 2.4 to 4.4 w/o hydrogen (LECO) or 2.5 to 4.5 w/o hydrogen (TGA). Similarly, Sample #17067 changes from 2.5 to 4.8 w/o hydrogen (LECO) or 2.7 to 5.0 w/o hydrogen (TGA). These values demonstrate that, as claimed by Reactor Experiments, the 4.22 w/o hydrogen concentration from the RX244 data sheet is achieved if the material is not dried in sample preparation.

Comparing test res.ilts from Series #1 and #2, it is apparent that water loss is fairly consistent for i the lowest temperature step and the two higher temperature steps. This further supports the observation that water in the low temperature step is free to hydrate at room temperature and that the samples tested on 10/30/98 had essentially completed the drying process. The main difference in overall water content between Series #1 and #2 occurs in Step #2, where water loss I

averaged 9.68 w/o (1.1 w/o H2 )in Series #1 and 4.17 w/o (0.5 w/o H2 )in Series #2. Whereas the TGA graphs would suggest that Step #2 begins above 100 C, the difference in hydration between the two test series demonstrates that the step begins below 100 C. Apparently the (arbitrary) heatup rate would need to be lower to demonstrate the true temperature at which this l

~

Enclosure 1 to VPN-076-98 l November 25,1998 Page 4 of 30 i Final Report '

Evaluation of Neutron Shielding Material (RX244) !

I step begins. However, it is clear that this step does not begin in the normal range of ambient

, temperatures. Since Step #2 begins above ambient temperature, and the vent holes in the l

Transfer Cask top ring are plugged shortly after the RX244 is cast (ie, within weeks), the data support not including Step #2 hydrogen loss in the shielding analysis. In addition, the data show that hydrogen loss from Step #1 is well below 10% when starting from the dry condition (ie,2.8 w/o) , demonstrating that the 10% loss taken in the shielding calculation is conservative.

l A sample (alternate) calculation for Sample #16621 is attached to this Report, showing the methodology for determining the hydrogen values in the summary table. When comparing the vendor table with this table, note that vendor Steps #1-3 correspond to Steps #2-4, since the vendor did not include the small initial step for hydration loss at ambient conditions. Certain values used in the calculation are taken from marked-up TGA graphs, also attached. Discounting minor numerical differences (due to interpolation off the TGA graphs), one minor error was noted in the vendor calculation results. Total weight loss for sample #16621 is listed as 8.92 mg, I whereas the correct total should be approximately 7.06 mg. This may be typographical (perhaps 1 intending 6.92 mg), as the corresponding w/o loss of 26 percent is correct.

)

l

I

^

Enclosure 1 to VPN-076-98 November 25,1998

j. Page 5 of 30 l i Final Report Evaluation of Neutron Shielding Material (RX244)

Samnle Calculation for Hydrogen Content of Sample 16621 from TGA Original sample weight (from TGA printout) = 26.678 mg Weight loss in Step #1 = 26.678 (1-0.997) = 0.08 mg :

i Weight aRer Step #1 = 26.678 - 0.08 = 26.60 mg Percentage loss = (100)(0.08)/26.678 = 0.30% H2 O or (0.30)(2/18) = 0.03% H2 Weight after Step #2 = 24.195 mg (from TGA printout)

Weight loss in Step #2 = 26.60 - 24.195 = 2.40 mg Percentage loss = (100)(2.40)/26.678 = 9.00% H2 O or (9.00)(2/18) = 1.0% H2 Weight loss in Step #3 = 24.195(1-0.845) = 3.76 mg Weight after Step #3 = 24.195 - 3.75 = 20.44 mg Percentage loss = (100)(3.75)/26.678 = 14.06% H2O or (14.06)(2/18) = 1.6% H2 Weight after Step #4 = 24.195(1-0.811) = 19.62 mg

' Weight loss in Step #4 = 20.44 - 19.62 = 0.82 mg Percentage loss = (100)(0.82)/26.678 = 3.07% H2 O or (3.07)(2/18) = 0.3% H2 l

.~'

)

4

- Enclosure I to VPN-076-98 :

November 25,1998 l

Pane 6 of 30 Summary of RX244 Chemical Analysis Results Test Series #1 4

Sample Number Sample Boron w/o Hydrogen w/o PGE ME&T Galbraith Cast Date Titration ICP LECO Test Date - TGA - Test Date j A 16620 Z-2492 7/21/98 4.278 3.28 9/16/98 2.91 10/30/98 B 16621 Z-2493 7/21/98 3.725 3.30 9/16/98 2.94 10/30/98 I C 16622 Z-2494 7/21/98 4.036 3.19 9/16/98 10/30/98 D 16623 Z-2495 7/21/98 3.948 3.34 9/16/98 2.84 10/30/98 3

E 16624 Z-24% 7/21/98 3.835 3.14 9/16/98 3.02 '10/30/98 i

F 16625 Z-2497 7/21/98 3.937 3.23 9/16/98 10/30/98 Average 4.0 4.0 3.3 -

3.0 -

Standard deviation 0.4 0.2 0.1 -

0.2 -

i i

- . _-___ - . , . - - _ , . . . . . _ _ _ _ . . - - _ . . _ . . . . . _ . . - . - . . . _ . _ _ _ . _ .. _ . _ - . . . - _ . . , _ . _ _ _ . . . _ . _ _ _ . . , . _ . . _ _ . _ . _ . _ . ~ .- . - _ _ _ _ _ _ _ - ._ $

Enclosure 1 to VPN-076-98 November 25,1998 Page 7 of 30 Summary of RX244 Thermal Gravimetric Analysis Results Test Series #1 Weight Loss Sample 8 ""' ""

f-Sample Sample Total Step 1 Step 2 Step 3 Step 4 NW Weight Weight t

[mg] [mg] II2 0 HO2 H2 HO 2 HO2 H2 HO 2 HO 2 H2 HO 2 HO2 H2 HO 2 HO 2 H2

[mg] [%] [%] [mg] [%] [%] [mg] [%] [%] [mg] [%] [%] [mg] [%] [%]

16620 23.571 17.40 6.17 26.2 2.9 0.09 0.38 0.0 2.34 9.93 1.1 3.32 14.09 1.6 0.42 1.78 0.2 16621 26.678 19.62 7.06 26.5 2.9 0.08 0.30 0.0 2.40 9.00 1.0 3.76 14.09 1.6 0.82 3.07 0.3 166228 26.378 18.75 7.63 28.9 3.2 0.48 1.82 0.2 2.64 10.01 1.1 3.56 13.50 1.5 0.95 3.60 0.4 16622 24.237 18.18 6.06 25.0 2.8 0.00 0.00 0.0 2.26 9.32 1.1 3.12 12.87 1.4 0.68 2.81 0.3 16623 25.852 19.25 6.60 25.5 2.8 0.00 0.00 0.0 2.60 10.01 1.1 3.21 12.42 1.4 0.79 3.06 0.3 16624 26.627 19.40 7.23 27.1 3.0 0.00 0.00 0.0 2.88 10.82 1.2 3.44 12.92 1.4 0.90 3.38 0.4 16625: 18.518 13.02 5.50 29.7 3.3 0.50 2.70 0.3 1.59 8.59 0.9 2.65 14.31 1.6 0.76 4.10 0.5 16625 25.304 18.31 6.99 27.6 3.1 0.10 0.40 0.0 2.46 9.72 1.1 3.54 13.99 1.6 0.89 3.52 0.4 Average -

27.1 3.0 -

0.35 0.1 -

9.68 1.1 -

13.52 1.5 --

3.17 0.4 Standard Deviation -

1.6 0.2 -

0.62 0.1 -

0.69 0.1 -

0.71 0.1 -

0.69 0.1 t Test date 10/30/98 except as noted. ! Test date 9/16/98.

s. . _ - _ . . - - - _ _ _ _ _ _ __ .__ . - - - - _ _ _ _ _ _ _ - - - - _ _ - - - - - _ - - _ _ _ _ - - - - - - - - -

4 Enclosure 1 to VPN-076-98 November 25,1998 Pace 8 of 30 Summary of RX244 Chemical Analysis Results Test Series #2 Sample Number Sample Boron w/o Hydrogen w/o t PGE ME&T Galbraith Cast Date Titration ICP LECO Test Date TGA Test Date l 1 17065 Z-9474 10/7/98 11/3/98 2.5 11/3/98

.7 3 i

3.58 2.46 2.38 2 17066 Z-9475 10/7/98 2.44 2.36

" ~ "

2.40

. .54 2.44 3 17067 Z-9476 10/7/98 11/3/98 2.7 11/3/98 3.06 a.22 2.46 ,

Average 3.2 3.0 2.5 -

2.6 -

Standard deviation 0.5 0.7 0.1 -

0.1 - t

? See comments for differences in sample preparation between Test Series # 1 and Test Series #2.

Enclosure I to VPN-076-98 November 25,1998 Page 9 of 30 Summary of RX244 Thermal Gravimetric Analysis Results Test Series #2 Weight Loss Original Final Sample Sample Sample Total Step 1 Step 2 Step 3 Step 4 Number Weight Weight t

[mg] [mg] II 20 HO2 H2 HO 2 HO2 11 2 HO 2 HO 2 H2 HO 2 HO2 H2 HO 2 HO2 H2

[mg] [%] [%] [mg] [%] [%] [mg] [%] [%] [mg] [%] [%] [mg] [%) [%]

i7065 29.388 22.70 6.69 22.8 2.5 0.18 OA1 0.1 1.35 4.60 0.5 4.29 14.60 1.6 0.87 2.96 0.3 ;

i7066 28.357 22.02 6.34 22.4 2.5 0.20 0.71 0.1 0.81 2.86 0.3 4.32 15.23 1.7 1.01 3.56 0.4 17067 30.835 23.38 7.46 24.2 2.7 0.13 0.42 0.0 1.56 5.06 0.6 4.66 15.11 1.7 1.11 3.60 0.4 Average -

23.1 2.6 -

0.58 0.1 -

4.17 0.5 -

14.98 1.7 -

3.37 0.4 Standard Deviation -

1.0 0.1 --

0.15 0.1 -

1.16 0.2 -

0.33 0.1 -

0.36 0.1 i Test date 11/3/98. See comments for differences in sample preparation between Test Series #1 and Test Series #2.

t MET 16622 File:01002.001 TG METTLER 16-Aug-98 i 23.257 mg Rate: 20.0 *C/ min Ident: 0.0 UNIVERSITY OF TENNESSEE !

M 4 -_i , .

d

i. Step Analysis Height -3.33 mg

-14.33 %

- ~

- ResiC. 19.83 mg I to- 23,zsi(o.u<3= is.,s !

c) ,

85.28 % is.3o . i s.v, . o,3s ;

Dpeak 328.0*C !

o- .

c) -

l Step Analysis ;

. 23.m co.ws m.ao Height -0.79 mg l

. j u. m -is o o - s. % -3.39 % !

tri- own w

Vk M ! ResiC. 18.75 mg i"V ^

F 80.62 %

i . Dpeak 424.0'C

. i .

1

o. w . . . . . . . _ . . . . . . _ _ . . . A ._.

O-(D .

. . . . .- i . - = = = > ' ' = * ' ' '

. ..g . .

l g l 1. 1 1 ;

200. 300. 400. .500. 600. 700. 'C l Page 10 of 30

MET 16622_ File: 01001.001 TG METTLER 16-Aug-98

-26.378 mg Rate: 20.0 *C/ min Ident: 0.0 UNIVERSITY OF TENNESSEE x- 8 I

I l 26.3n (o.nzb ts.9o i

2 6.3 n - 23.9 o = o..is t o 832

.W W- .

. yv =

Step Analysis

, Height -2.28 mg l ! -8.63 % !

I

~

ResiC. 23.50 mg i 89.10 %

ui_ Dpeak cn Step Analysis l 0.88 Min '

i Height -0.38 mg i

-1.43 % !

i i ResiC. 25.88 mg. i I

- 98.10 % i i

Opeak 68.0*C

- I I

. i '

I o- i m

l I

I

i. i - -

1 1. i

50. 100. 'C 0. 2. 4. Min i i

Page11 of30

PGE F . .

MET 16625 File: 00200'.001 TG METTLER .ii-Aug-98 18.518~mg Rate: 20.0 *C/ min g Ident: 0.0- UNIVERSITY OF TENNESSEE i s. sis (o.9 s): it.oz.

_ n. sis -is.oz = o.so

- Step Analysis Height -1.77 mg

) -9.56 % '

l ResiC. 16.25 mg 87.75 % is sis (a 55* '6 4 '

. j Dpeak 153.3*C it.oz-is.us = i.33 '

o- ) 1

-,,,,, {

is-sivo-ioib is..z i Step Analysis o,,s- n.o2 = o.w ,

~ ;

Height -2.41 mg

~

-13.01 %

ResiC. 13.79 mg i f_

m 74.49 % Step Analysis Opeak 323.3*C Height -0.64 mg .

-3.43 . ;

,, is.s no.ww oa' ResiC. 13.13 mg oac io.u- n.u = 2.us !

t i:i

~

> 70.90 % !

j i .i . , Dpeak 376.7'C j

o.lo3 c- ! M b :' ,.

g . . . .

g j i . .

g >

200. 400. 600. 'C '

__i Page 12 of 30

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

October 30,1998 PGE A s Sample #16620 File: 00011.001 TG METTLER & Aus-se. .

23.571 mg Rate: 20.0 *C/ min Ident: 0.0 INIVERSITY OF TDMNFF M. I e

t 8

23.su to.910 n.us 8

13.Sh-13,4 2 = o.oq j o-n os A i

E I '

Step Analysis l l Height -2.37 mg

-10.06 % ;

. ResiC. 21.09 mg l 89.49 %

l Opeak i.18 Min

- t 3 -

1 I $ i O- ,

t t '

cn s ^

. I I e e '

I I

l l

l

." I tn- a CD '

. I I

- I i

I g

j . . . .

g . .

g . . .

100.*C0. 5. 10. 15. Min a

Page 13 of 30 l

October 30,1990 PGE A '

Sample #16620 File: 00012.001 TG METTLER 29-Aug-98 21.137 80 Rete:20.0 *C/ min Ident: 0.0 LMIVERSITY OF TU#ESSEE M.

i Step Analysis Height -3.30 mg f_ -15.63 %

m ResiC. 17.82 mg 21.131(o.123)s l'4,t1 o b7

~

g Dpeak o-S

. Step Analysis

. Height -0.42 mg mn (o.m n.n -1.99 %

2us>- n.n e uz ResiC. 17.41 mg f_ l 82.35 %

m 545 j Opeak 517.3*C

~

l.

n.32 3

% ~1 i

- i g

I g

g . . . .

g g

...g . . . .

3 200. 300. 400. 500. 300. 700. *C Page 14 of 30

October 30.1998 PGE B .

s <

Semp10#16621 F11~.4 00013.001 TG METTLER 30-Aug -

28.578 og Rate: 20.0 *C/ min Ident: 0.0 UNIVERSITY OF TDNPMFF w-. .

l 26.613 (o.9mb 26.co .

. t , 26.cas w.<,o.o,os o ~ __

y o.m -

E

~

Step Analysis

~

! Height ~2.54 mg

!. -9.51 %

n ResiC. 24.09 mg in-m i

i 90.30 %

. : Dpeak .0.95 Min 8

l I

l '

g_ , ,

_ _= _

m .

g I !

~

s'

. I I

8 I

. i tn- s e 8 I

' t g . .

j . . . . , .

100.*C0. 5. 10. 15. Min

, i !

1 Page 15 of 30

October 30,1998 PGE B Sample #16621 File: 00014.001 TG METTLER 30-Auc-9e -

.24.195 mg Rate: 20.0 *C/ min Ident: 0.0 UNIVERSITY OF TDedESSEE M.

[ Step Analysis Height -3.72 mg f_

m

-15.36 %

ResiC. 20.46 mg 84.57 % 29.ise,(o.aii w is. a i Opeak 330.7'C 2a "a - n 't o.n o-m _

Step Analysis ,

a.m(o.t90= :o.w Height -0.60 mg 2o.ns- zo.m - 3."

-2.49 s "

$~ o Sd5 ResiC. 19.76 mg

, B1.68 % ,

C peak 533.3*C

}

o.Sn . ,

. i o-m . . .

.. g

. . . .j - . . .

g . . .

j . . .

g . . . j . . . .

g 200. 300. 400, 500. 600. 700. *C i

Page 16 of 30

. _ _ _ _ _ _ - - - _ _ _ _ _ _ _Ue t.ober .10,19911. _ _ PGE C l

Scmp100iS622 24.237 mg File: 00015.001 TG METTLER 31-Aug-98 '

Rate.20.0 *C/ain Ident: 0.0

J ' UNIVERSITY OF TD4ESSEE I

o '

O 1

"- i i

Step Analysis 2 i. m (o. w )= u .9 s

.,. .m - 2..w = , a i

Height -2.29 mg .

l 8

-9.47 %

i tri- ' ResiC. 22.02 mD

90.86 %

! Dpeak i

1.18 Min

- I

- I -

I o,901

.- 4 o- 8

~

en '

- t

- ?

' i 3

3 t

I gg. I e '

i ,

8 s ,

j . . . . g . . . . . . .

3 100.

C O . 5. 10. 15. Min J

Page 17 of 30

October 30,1998 PGE C -

S mpic#16622 Fils: 00015.002 TG HETTLER 31-Aug-98 ~

24.237 e9 Rate: 20.0 *C/ min Ident: 0.0 UNIVERSITY OF TO NESSEE w_! .

I I

~

Step Analysis Height -3.39 mg

~

I

., -13.99 %

$- ResiC. 20.83 mg 85.93 % u.,s to ste is.n ,

i f Dpeak 330.7*C o-on Step Analysis u.9 sto.sss). is.sc. Height -0.57 mg 2i.9s . is.sr. - 3.it -2.34 %

ResiC. 20.17 mg l

.. o sss 83.20 %

g'- : Opeak 528.0*C Y

. . . g . . . .

g g

g

-. ...g . . . . . . ,-

g .

200. 300. 400. 500. 600. 700. *C Page 18 of 30

October 30,1998 PGE D SC plceiSS23 Fils:00017.001 TG METTLER si-Aus-98 25.852 a0 Rate: 20.0 *C/ min Ident: 0.0 UNIVERSITY OF TD NESSEE M. I E

t

. t o_ ' m o . v

- 8 Step Analysis l Height -2.56 mg

' -9.91 %

, j l Res1C. 23.28 mg n_

- 8 i 90.07 %

cn 8 Dpeak i.28 Min i

3 t ,

E l

~

s o- -

_ e CD s

~

l I

. E o_. I m l a

1 g . . . . . . . . . . . . . .

3 g g g . .

100.

C 0. 5. 10. 15. Min L

Page 19 of 30

Octnher 30,1990 PGE D ,

SamplodiS623 F110: 00010.001 TG HETTLER st-Aug-98 .

23.246 mg Rate: 20.0 *C/ain Ident: 0.0 LNIVERSITY OF TD4ESSEE M-Step Analysis

~

Height -3.21 mg

-13.83 %

d-01 ResiC. 20.01 mg

. 86.09 % 23.24cto.sz,)=i9.1s "in.oQ - g%15 = 0.M t Dpeak 333.3*C o-m Step Analysis

- 23.2m.co.v.1)no.oq Height -0.63 mg i n.m-2o.oc 3.z'

~ -2.7i %

o.Scz ResiC. 19.30 mg ;

N in-83.03 %

I' CD i l '

o.125 3

200. 300. 400. 500. 600. -

700. *C l

Page 20 of 30 ;

i

October 30,1998 PGE E '

r S:cplc416624 File: 00019.001 TG METTLER 31-Aug-98

26.627 og Rate: 20.0 *C/ain Ident: 0.0 UNIVERSITY OF TONESSEE M !

t l !

o_ '

, l Step Analysis

~

Height -2.70 mg

-10.13 %

, l ResiC. 23.90 mg to-m l 89.76 %

l Dpeak 1.07 Min E

e

. s I o- t m '

- l !

i :*

a E

. 8 I

l in- a ,

@ a l l g , g . . .

g . . . . . . .

3 ,

100.*CO. S. 10. 15. Min ,

t 1

Page 21 of 30

October 30,1998 PGE E ,

Samplefi6624 File: 00020.001 TG METTLER si-Aug-se 23.744 s0 Rate: 20.0 *C/ min Ident: 0.0 UNIVERSITY OF TENPESSEE x ., -

j

- I

~

Step Analysis

~

. Height -3.44 mg .

$~ ~

-14.49 %

ResiC. 20.27 mg 23.m (o.snp n.qo i

85.38 % zo.3o - i9 9 o - o.so Opeak 328.0*C

} ,

o-ai

- Step Analysis Height -0.64 mg n.aw to.sssw 2o.so n.m -so.2o o.uq

_ -2.71 %

- o. m j ResiC. 19.59 mg i' in- 82.51 %

m '1 ~

' Dpeak 509.3*C l

~

N

- o.S n w j . . . .

g . . .

3 g . .

200. 300. 400. 500. 600. 700. *C .

Page 22 of 30 b

October 30,1998 PGE P s

Sample #16625 25.304 mg Fils: 00021.001 TG METTLER 31-Auo-os Rate: 20.0 *C/ain Ident: 'O.D M -

t LINIVERSITY OF TENNESSEE 8 2s.3on (o.m)- 2s.zo j 2s. 3og - 2 s.ie o.co R- % '

a, o. w ~

Step' Analysis Height -2.35 mg i -9.29 %

u)- ' ResiC. 22.87 mg m 8

' 90.38 %

Dpeak 1.07 Hin

) a f

f I

i ,

- l 1 o- ,

G I

I I

g I

I I

u)- l m ,

1 I

I i

1 g .

100.*C0. 5. 10. 15.

3 Min Page 23 of 30

October 30.1998 PGE F .

Sarp1916625 File: 00022.001 TG METTLER 31-Aug-se

~

22.743 og Rate: 20.0 *C/ min M

Ident: 0.0 (JNIVERSITY OF TD64ESSEE t

Step Analysis

,- Height -3.53 mg in-O

-15.53 %

ResiC. 19.18 mg '27.N 3 (0.%os): IK.31 i.i.yo_,s.3, ,o.33 Dpeak 330 o-Step Analysis

- Height -0.73 mg n.mnto. sawn.w -3.22 %

n. m _in.2 ,3,sq Res AC. 18.36 mg-R- o. sus

~_ _

80.73 %

__- o. sos o-e i

3 . . . . . .

3 i . .

200. 300. 400.. 500. 600. 700. *C Page 24 of 30

sample #17065 k File: 00026.001- TG METTLER 03-Nov-98 29.388 mg Rate: 20.0 *C/ min Ident: 0.0 UNIVERSITY OF TENNESSEE M

i 8

~

I i

l 3 I

I 19.3R1 (o.9%) == 1.9.2.I '

19.ns - 29.si = o.Is oI i ,

,-v o.m i

,j ; t Step Analysis i I

8 Height -1.29 mg i

I -4.40 % . ;

l ResiC. 27.91 mg -

i 8 94.97 % '

l Dpeak 4

8 0.37 Min l l 8

I in-m i

3 y .

I l

I ?

f I

I i I

I

. I I

I i I

3 ,

I

. I o- 8 m l i

i .

i, . .. .

i 100.*C0. 5. 10. 15.

Min I i

Page 25 of 30 '

t

l Sample #17065 1 27.857 mg File: 00027.001 TG METTLER 03-Nov-98

, Rate: 20.0 *C/ min Ident: 0.0

'x. : UNIVERSITY OF TENNESSEE

_J _ i i !

Step Analysis '

Height -4.24 mg

-15.23 % .

I tri-m ResiC. 23.60 mg 84.74 % mse.wh n.w Opeak 320.0*C "'"'" " '"

' *o- .

Step Analysis j _ n.isuo.mi u.s2 Height -0.74 mg u.in - n.s2 , n.m

-2.67 % ,

f_

ResiC. 22.83 mg I I

81.97 % '

Dpeak 528.0*C ,

i o.%ts "

~

l, e'

g

.- r- T ~~ ' ' ~l * '

i

' ' ' ' C l '

I

' ' ' F I

1 200. 300. 400. 500. 600, I

I _

700. *C ,

Page 26 of 30

M

O i; - :

V >

! Sample #17066 as.sf7 se F13a: Cooas.cos TG METTLER o m -se note:ao.o *c/ min Ident: 0.0

_ UNIVERSITY OF TDGERSEE in ' 2035 7 (OMiS)- 18.m m l 20151-11 4 ; 0 2o [

m -

e , ,

n d_ l Step Analysia ,

$ S , , ,

l. Height -0.71 mg n -

-2.5o X

( t -

l e

ResiC. 27.43 og 96.74 X I- [ Opeak

! O.48 Min i a

i i

3 8 l

l 3 vu m l I '

L -

g

e C

k . I U I 3g g I

.g .

s.R .

i 3' l

< .' , i

~~ o- i I

N' CD

.. E E e i "g

i '

i - -

i m*

5.

^

100 '

C 0 - 10.

m s

e,. 15. Min .

em

?=

0 z Page 27 of 30

a O

. ~

i Sample #17066 File: 00029.001 TG METTLER 03-Nov-ee 27.3s1 se m a.o c/ min g Ident: o.o UNIVMBITY OF N m * ~

On 0%

e -

)

n .

Step Analysis Height -4.28 mg ,

n .

y -15.65 %

d- ResiC. 23.04 mg i * .

b -

84.25 X :

Opeak 317.3*C f _23,33,(o.sosb n.on_

i I n.os-u.oz i.oi d-i m -

l <

- Step Analysis y .

Height -0.88 mg ,

c .

i n.v>i(o.mbn.os 5-n.ssi-n.on ut -3 22 X

$y, E- .o. wit ResiC. 22.12 mg

,;y 80.87 %

R Opeak 528.0*C i,' -

( ,- o.so3 0; o- >

~

c e ,

1 j:E 200. 300. 400. 500.

5 i;

ee 600. 700. 'c ,

33 .-

0 7 Page 28 of 30 '

m O ,

Q t i _

! Sample #17067 File: 00030.001 TG METTLER es-+sev ee 30.835 se Rete: 20.0 'C/ain M t e

Ident: 0.0 LMIVERSITY OF TISDESME g g a to.9 M (o.tlQ = 3011

~

i so.y.n- 2o.ai = o.is

$ o.m '

b n i m -

v ;

l Step Analysis ,

n N '

Height ~i.50 mg

, r -4.85 % ,

i

~ ResiC. 29.20 mg ,

t. i

, 94.68 %

, j Dpeak 137.3*C 3 e i i

an- i l.

m

~

- i v ,

i L ' i e i ,

C I i j L - g '

i e g . r M c.

s i

. w. . s 92 ,

i R I l

-ic; i -

i e

< . ' s N'; o- i !

r

.. y, @ 8

.4 c S

.4 g g . . . . . <

3 . . .

g .

@h 100.*C0. 5. 10.

i; 4e

15. Min .

O3 i-i 0 .

z Page 29 of 30 t

i

o '

O . . -

c.t I

Sample #17067 File: 00031.001 TG HETTLER 05-Nov-95 29.161 mg Rete: 20.0 *C/ min M.

Ident: 0.0 IMIVERSITY OF TBGE!SNE g

in -

a m

o .

M

0) .

M N g}

. m Step Analysis Height -4.61 mg z,.isi to.sozb r3.n i f g

. -15.82 X '" "'-'5'" ~ ' "

o-ResiC. 24.51 mg m , 84.06 %

Dpeak 317.3*C

~

E c ,-

22.isi to.39o)= 29.u, Height -0.97 og ta.isi - 29.99 = u."

a, w ,

a

-3.31 %

24, m o.wio u ResiC. 23.48 mg

.E r 80.51 X

.a -

2* ~

< . o.so r. >

N r. _o~ . . _ _

N ~s. G1 .

?;-

i r. . .

3 i

gE 200. 300. 400 500. 600. 700. *C i

ec 03 i-o Page 30 of 30 z

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

I

=' ' .Qo -o , , . \

6 Q Enclosure 25 to.VPN-076-98

- .- November 25, 1998 !

l t

'I I

i PORTLAND GENERAL ELECTRIC l

?

TROJAN NUCLEAR PLANT-71760 Columbia River Highway 3 i Rainer, OR 97048

-l l

t 1

t i

I l

l Materials Engineering and Testing Corporation

- 125 Valley Court, Post Office Box 4536, Oak Ridge,TN 37830 l

i f.

1 l- I i . - . . --. ... .

l ' . L. ... . .

l%

l l

l 1

MATERIALS ENGINEERING AND TESTING CORPORATION 125 VALLEY COURT, P.O. BOX 4536 OAK RIDGE, TN 37830 !

PilONE: (423) 482-7762 FAX: (423) 482-6995 October 8,1998_ ]

CERTIFICATE OF CONFORMANCE l During surveillance the determination was made to use direct NIST standards. Results are i provided on that basis from Inductively Coupled Plasma (ICP) Emission Spectrometery.

The data will be provided from the ICP analysis and by titration for the borons.

s

- mm - ~.amamwmaw *2^""*

TROJAN NUCLEAR PLANT Shsp to: Recenine %rchouw PURCHASE ORDER '

71760 Columbia River Hwy. DATE- 9/8/38 N

Rainier OR 97tkIS ['

THIS PURCHASE ORDER IS SUBJECT TO THE TERMS AND CONDITIONS ON THE REVERSE SIDE. % i a' 7 4 I

AAT DoctMtNT(fDN ttQOtttD Sf TH5 Pt2 CHASE otDtt EftST Acc0MPANY SIEPMEAT kRat 70 00 50 Mty DEttY PaiMExt 08 5t2ECT MAfttiAt.10 BLECTXw.*

NOTICE : w umnTimnu et <ctmo urnoet na minitx Amont av xt Materia 1s Engineering & Testing PO Box 4536 i

an Eme mlim mo at nis nm m mAu et m Ano mo. t1e srtancAur gnum im B5 M AAD 5"u nt or stwotto un novtx et5x;x a tut nxTxws un curaws srtanto 125 Valley Court

' VENDOR 4 R1CHtSt M N G AMARONARPG JWMPMMINWE umptump Oak Ridge, TN 37830 y ma,ctnocrtram artaner- arcar AcmexT ianu . cts

@ n u ntr.xran e acttums two:ct ei sr.nttwoos es inrnkd: O No 0 m wuh Betsy Norris 8/27/98 on Phone # 423-482-7762 FAX # 423-482-6995 pgung Date Payment Terms Ship %4 . FOB Point l Freight Terms Net 30.- .' -

[ ,

em Quintity . Description . ._

Q Stores Code . Code. . Unit Price ,. Total

. 3..,...' -

.4 =. .-s ,.

' ~

See Page 2 for the description. A 5500346 (PS98-230)

' *i w %Aw w %2W For commercial information regarding this order, contact the buyer below.

Tetal This Purchase Order

- f:

i <

See Page 2 Af aulA(oler[t[. 50-556-7568

.a wis e .,m s.y .

totslLntou utiettvit LLLue tut s.va 4 me n a s#c weesu,6 v t sh be s t uhwa ssut. visu s as a s. se q a o .L u is TROJAN NUCLEAR PLANT Date: 9/06/98 supplemert , ,

Page 2 of 2

( ,

Descriotion (continued) {

Provide testing services of RX244 in accordance with Materials Engineering & Testing Corp. Letter dated August 24 and August 25,1998, which by reference are hereby made part of this order.

PGE to witness testing of first sample. Testing of five other samples may proceed following PGE approval of first test. Sample preparation of samples may be done prior to PGE witness (total of six samples).

PGE team shall conduct surveillance on site. -

PROCUREMENT REQUIREMENTS SP 1. General Certificate of Conformance Supply a " Certificate of Conformance" to PO requirements, which meets the following criteria- i

~

a. Identify the PO number, including all supplement numbers applicable to the items being addressed.

b. Identify the specific procurement requirements met by the purchased material or equipment, such as codes, standards, and other .

specifications.

c. Identify any procurement requirements that have not been met, together with an explanation of corrective action to resolve the deficiency.

d. Be attested to by a person responsible for assurance of quality.

SP 6. Riahts of Access PGE or its designee shall be granted a "Right to Access" to supplier facilities and records for QA audits or inspections, if deemed necessary by PGE.

Pricing shall be in accordance with the rates shown on the above-reference letters. The total cost is not to exceed $4,000.

The PGE Project Adminhtrator is Mark Tursa at 503-556-7889. So3-554 %i0 f.

Send invoices in duplicate to: Trojan Nuclear Plant !<'

Cost Control Department 71760 Columbia River Hwy Rainier, OR 97048

.. . . . . _ = - - - . . _ . - . _ . _ . .. . . .

.c..

1 MATERIALS ENGINEERING AND TESTING CORPORATION 125 VALLEY COURT, POST OFFICE BOX 4536 OAK RIDGE, TN 37830 PHONE: (423) 482-7762 FAX: (423) 483-6995 l

Portland ME&T Galbraith A 16620 Z-2492 B 16621 Z-2493 C 16622 2-2494 D 16623 Z-2495 E 16624 Z-2496 F 16625 Z-2497

)

l I

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

~

. (.. ...

1 MATERIALS ENGINEERING AND TESTING CORPORATION 125 VALLEY COURT, P.O. BOX 4536 OAK RIDGE, TN 37830 P1iONE: (423)482-7762 FAX: (423) 482-6995 PROCEDURE FOR DETERMINING TOTAL BORON IN AL2 03-B4C BY INDUCTIVELY COUPLED PLASMA EMISSION SPECTROMETERY 1.0 SCOPE i This procedure covers the determination of total boron in Al23 0 -B4C,

2.0 REFERENCES

2.1 ANSI / ASTM C 751-75,C791-94, and C809-94 !

l 3.0 EQUIPMENT l' 3.1 Analytical balance.

3.2 Plattner, Diamond Mortar and Pestle.

3.3 Glass Tubing, Glass blower's torch. l 3.4 Muffle Furnace. l 3.5 100 ml Class A Volumetric Flasks.

3.6 Vortex Mixer. :

3.7 Reagent grade chemicals and NIST Standards.

3.8 Inductively Coupled Plasma Emission Spectrometer, equipped as specified by the manufacturer for analysis of elements ofinterest.

3.9 Regulator, two-stage, for argon.

3.10 Deionized water (resistivity greater than 1.8 x 106 ohm's).

4.0 PROCEDURE l 4.1 The sample is crushed with a Diamond mortar and pestle to <100 mesh (using a 100 mesh screen to classify the powder).

4.2 Weigh .25g (+/ .00 log) duplicate samples from each pellet into heavy glass tubes.

4.3 Add 2 mis concentrated HNO3 ot each sample and a blank.

4.4 Mix with a vortex mixer and close tubes.

4.5 Place glass tubes into safety containers and heat for six hours at 300'C.

4.6 Cool to room temperature, open tubes and wash into beaker.

4.7 Transfer concentrate to 100ml volumetric flasks and dilute to volume, adding Deionized water.

4.8 Run samples on the ICP compared to NIST traceable standards.

4.9 Calibrate the spectrometer according to the manufactures recommendations.

4.10 Analyze a standard afler every sample.

! 5.0 REPORTING TILE RESULTS 5.1 Report the results using the CERTIFICATE OF ANALYSIS. All test data must be recorded and retained together with the calculations and copy of the final report.

j. 5.2 Report any unusual test conditions. !

t

_ . . _ _ __ __ ____.m _ . _ . . -. . _ _ _ . . _ _ . . _ . . _ . _ __ _ . _ _ _ _ .. _ _ . _ ._

+ e r Ae

- __.m

~

TG SCREEN TG: Screening Method [ SCREEN]

The screer$ng method is chiefly used for making a rapid survey of the thermogravimetric properties of a sample. A relatively high heating rate (20 to 50 K/ min.)is normally used and a wide temperature range is covere.d. The experiment is qualitatively evaluated from the printout ;

in order to define, for example, the experimental conditions for the STEP-method. '

The recorded TG ls, however, also available for numerical evaluation as it is stored in its entirely in the TA Processor. The evaluation part of the screening method makes it possible to plot selected portions of the TG curve as well as its derivative (DTG curve) on the printer / plotter.

- 4 1

6 l

5 l

/ ,

i- i i

f i

4

MATERIALS ENGINEERING AND TESTING CORPORATION L25 VALLEY COURT, POST OFFICE BOX 4536 OAK RIDGE, TN 37830 Ehon3: (423) 482-7762 Fax: (423) 483-6995 f PROCEDURE FOR ' IGA ANALYSIS OF ALUMINUM OXIDE- B.C

5. 0 SCOPE This procedure covers' the Thermal Gravimetric Analysis of AL 03 3-B.C. t I

'.0

$ REFERENCES Manual for TGA with a TG50 Thermal Balance

).O EQUIPMENT A. Metler balance - Serial No. L50324. !'

B. NIST Calibrated weights.

C. TGA - Model No.TG50 Serial No. L50323 5.0 PROCEDURE A. Calibrate the balance.

B. Run 1 of each sample at 20* C per/ min increase time. Hold at 160*C for 10 minutes then continue to 800*C.

C. See reference procedure enclosed, h.O REPORTING THE RESULTS l

A. Report the results using the TGA Printout. All test data must be recorded and retained together with a copy of the final report.

j B. Report any unusual test conditions.

I

\

l l

- . _ _ . . . _ . _ - . _ . . _ _ . . _ . _ _ ___ _ . _ . _ ~ _ _ _ _ _ _ . _ . _ = . _ . . _ .

TG SCREEN l Example of the Use of the Screening Method. hh Study of the dehydration of copper sulphate. i '-

4

- Sample ,

About 10 mg ground copper sulphate (CuSOc+ SH,0. tutorial sample no.11) are weighed in a standard alumina crucible (70 ml).'

4 l Purge gas The investigation can be carried out without purge gas in normal air.

j input of Parameters l .

TG SCREEN *C 25. Standby state with display of the furnace j temperature, i

T[ SCREEN] SCAN PARAMETERS Selection of the screening method with standard values for all parameters.

gg Experimental parameters: -

[RUN] START TEMP. 'C '

25. Initial lefnperature for temperature programme.

j. [RUN] RATE K/ MIN. 20 Heating rate (without sign, the direction is from initial to final temperature). .

G* I

[RUN] END TEMP. .

C 000 Final temperature.'

Y 300 '

[RUN] TIME iso. MIN. O No isothermal measurement phase alter l the temperature programme.

Parameters for on line plot of the TG curve: , ,

j [RUN] PLOT CM 15 Length of diagram. *'

l r.a+

! [RUN] RANGE ES 10 ""

mG Plotting range (full scale deflection).' Larger changes in weight are neverthless accom modated by automatic shilling of the scale.

[RUN] orrsET % 90 Position of first measurement point. The curve starts at 90 % offset from the left hand margin.

Parameters for automatic change of atmosphere:

1

[RUN] VALVE T/t; 1/2 0 No valve switching. T,he second parameter i is thus not requested. .

1

. p.

?y I

k.

w MM

l TG SCREEN

Parameters for associated evaluation:

[RUN] SCREEN Title of evaluation, no input.

[RUN] Dyn/ iso 1/2 0 No evaluation. Thus no further evaluation parameters are requested.

[RUN] TG SCREEN 25. Standby state. The screening method is ready for use.

Execution of Measurement TG SCREEN *C 25. Standby state.

[RUN] IDENT.,NO. 249.7 Sample identification by a number with not more than 5 digits (e.g. molecular weight of sample).

[RUN] WEIGHT mG 10. 560 The momentary weight is displayed if the balance has been tared with the empty crucible. the weight of the sample is displayed directly. For weighing see also page 221.

l [RUN] WEIGitT mG 10. 5 62 The value last displayed is retained. The value can still be altered through the keyboard (e.g. for rounding, input of ,

standard weights etc.)

[B ACKSTEP] can be used to go back to

, the input of the sample identification (Input

! of zero and [RUN] also causes the pro-gramme to step back).

[RUN] INSERT T. *c 27.2 The fumace is now heated or cooled in the i

direction indicated by the arrow on the display to the insertion temperature *).The display flashes as long as the fumace temperature does not coincide with the command temperature.'The furnace temperature can overshoot the insertion temperature, but the sample will not be overheated due to the equilibration time. If the nitial temperature already is atteined this display is sklpped.

) ll the insertion temperature is above the standby temperature, it is equal to the initial

! temperature and if below,it is equal to the standby temperature.

l l

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

o. ..

i TG SCREEN INSERT SAMPLE The insertion temperature is reached to ' S' within i 1 'C. The sample is placed on the ,f !

sample carrier, unless it has already been :-

inserted aller weighing, and the furnace is closed. ;

[RUN] SETTLING 0.60 Temperature equilibration phase: The delay time until the sample reaches the initial temperature is displayed in minutes (see also page 222). With initial tempera-ture of 25 *C the, settling is skipped. If the ,

end temperature'of a method is the same as the start temperature of a linked me-thod, the temperature equilibrium phase is sk!pped (no printout of FORCED START).

SETTLING m.>,

10.557 The experirnent begins with a short iso- ;c thermal period during which the starting point for the diagram is located. The measured value is displayed in milligrams.

TEMP.'C 51.3 The sample temperature is displayed during the temperature programme. if this i

does not coincide with the command temperature, the display flashes. i

[ ROTATE] TG WEIGilT rnG 9. 7250 The momentary weight and the sample temperature can be displayed alternately during the temperature programme.

[ ROTATE] TEMP."C 65.0 During the measurement, the on-line plot is generated on the printer /pletter or on the computer screen.

TG SCREEN *C dh

280 As the parameters indicate that no 1 evaluation is required, i.e., there is no off- !

line plot of the TG curve, the equipment retums to the standby state at the end of l the measurement. The method used can l be executed again without input of parameters.

The TG curve recorded in this measurement is now available in the data memory for evaluation.

11 should be noted that the curve does not quite extend to the final temperature according to the

! on line plot. (For explanation see page 2G7, measurement principles).

, t g .

1

,* .+

l TG SCREEN Analysis Printout m e rum m Title of method.

o-aut-co : ao .

Date and tim'e of execution.

senes ennnnE rcas

$n?"' 'U$iu? N. Printout of parameters. This printout is ab-E:'Oc'5$. n e,2 !

sent when a stored method is used without yr g ,, ca io alteration.

1 OrrsET */c 9 '.'

VnLVE T/t 1/2 0 ECREEN DYN/ISU t/O O IDENT. NO. El 68E 3 0H T mG 10.562 Sample identification and weight.

" ~ ~ " " nn~'..., On.line plot of measured TG curve. The !

. . - ~ .

weight is always plotted in relative values )

~ ~

(bar scale). The curve starts at 90 % of the width of the paper as specified. A broken line indicates that the sample temperature differs l

'"*~

from the command value in this range. I 1 !

l l

The curve shows the three dehydration

, ._ steps.

w .. '

l l

Evaluation of the Screening Method The screening curve obtained by the screening method can now be evaluated by using the STEP-method available in the TA Processor. As no further measurements are to be made, the evaluation part of the required method is called with the key sequence [ EVALUATE][ STEP].

l The screening method also has an evaluation part which is called in the same way. lt produces

an oil-line plot of a selected portion of the recorded curve on the printer / plotter.

l As an example, the first two dehydration steps will be expanded and plotted.

I TG scnEEN 'c 50. Standby state.

[EVA1.UATE] EVAwATE Selection of the evaluation part of the ,

screening method.

i [ SCREEN] ScnEEN l

l

,= ,*

TG SCREEN Input of Parameters:

[RUN] DYN/ ISO 1/2 0 1 - Evaluation in the dynamic portion of 2 1 the curve.

2 = Evaluation in the isothermal portion of the curve.

[RUN] START 40 Initial temperature (or time). .

[RUN]

END 790 Final temperature (or time).

160

[RUN] BASELINE TYPE 1 Baseline type:

1 = Unmodified curve.

11 = Correction by a blank.

[RUN) PLOT CM 10 Overalllength of the diagram.

,g:- f j

(RUN] PLOT MODE 2091 The plotting mode eith up to four digits '

defines what is plotted:

TG curve and filtered DTG curve automati-cally separated.' l

[RUN] WEIGilT mG 10. 5 62 The weigh-in is displayed if necessary, the l value can be changed for the ext .

evaluation (e.g. to compensate for weight loss caused by drying).

![ ~

\

[RUN] *aa CALCULATING *** The off-line plot is now being generated. l DSC SCREEN *C 45. Standby state. Further evaluations may now be carried out.

@ l 9 e 7,,

g,. ,

l

.:.9 A. -- QMidGJ5Et3Uvme

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

MATERIALS ENGINEERING AND TESTING CORPORATION 125 VALLEY COURT, P.O. BOX 4536 OAK RIDGE, TN 37830 PHONE: (423) 482-7762 :

' FAX: (423) 482-6995 _

I

{ I SEPTEMBER 16,1998 1

j CALIBRATION CHECK FOR NETLER Serial NumberL50324 !'

Smg S/N 30833 4.97

, 5.01 5.21 -

100mg S/N 35790 99.81 99.67 99.64 500mg S/N 35789* 499.5 499.6 ;499.32 l

^

i l

I

+

i l

i I

l 1

l

-MET 16622 File: 01001.001 TG METTLER 16-Aug-98 26.378 mg Rate: 20.0 *C/ min Ident: 0.0 UNIVERSITY OF TENNESSEE M- I i '

l 1

Step Analysis

, Height -2.28 mg 1 l ! -8.63 %

I l ResiC. 23.50 mg in'-

l

' 89.10 %

cn Step Analysis Dpeak 0.88 Min Height -0.38 mg l

~

-1.43 % l ResiC. 25.88 mg !

I 98.10 % l Opeak 68.0*C I I

o- !

01 :

l q .__ - ---

E

50. 100. 'CO. 2. 4. Min

PGE C "

MET 16622 File: 01002.001 TG METTLER 16-Aug-98 '.

23.257 mg Rate: 20.0 'C/ min Ident: 0.0 UNIVERSITY OF TENNESSEE et i

d AI

~

l Step Analysis

, Height -3.33 mg

-14.33 %

~

in[

ResiC. 19.83 mg -

m , 85.28 %

_ Dpeak 328.0*C o- t oi Step Analysis

, Height -0.79 mg

. I -3.39 % !

@~ ! ResiC. 18.75 mg 3

80.62 %

i

~

. Dpeak 424.0*C I

}

O- i

. . i i is . . . . . . . . . .

g g i

g . . .

g g, .

g . . .

g 200. 300. 400. 500. 600. 700. *C

~

September.16, 1998 ,

PGE F ?

MET 16625 File: 00200.001 TG METTLER ii-Aug-98 18.518 mg Rate: 20.0 *C/ min Ident: 0.0 UNIVERSITY OF TENNESSEE M

_ Step Analysis Height -1.77 mg I , -9.56 % ,

l -

,ResiC. 16.25 mg

~

87.75 %

. j Dpeak 153.3*C o- i

I l i

. U

~

Step Analysis Height -2.41 mg

-13.01.%

ResiC. 13.79 mg 74.49 % Step Analysis O~

Opeak 323.3*C Height -0.64 mg ,

-3.43 % :

.' ,; ResiC. 13.13 mg

- 'i 70.90 %

' ix

i *

. , Dpeak 376.7'C j

o-N IW

. . . . . . i g . .

i .

j . . .

200. 400. 600. 'C :

r

_ _ . _ . _ _ _. _ _ _ . _ _ _ . _ . . _ ._..______._.__._.___.m_ _ . _ _ _ _ _ _ _ _ _ _ . _ _ _ _ _ _ - -

4 l

l l

l MATERIALS ENGINEERING AND TESTING CORPORATION 125 VALLEY COURT, POST OFFICE BOX 4536 OAK RIDGE, TN 37830 PIlONE: (423) 482-7762 FAX: (423) 483-6995 OCTOBER 30,1998 i

CALIBRATION CHECK FOR METLER Serial Number L50324 5mg S/N 30833 5.001 4.998 5.004 100mg 99.888 100.033 i

99.971

500mg 499.900 499.702 499.760 499.780 1

1 I'

t I

l i

l I

v 4

l

October 30,1998 PGE A '

Sample #16620 23.571 mg File: 00011.001 TG METTLER ae-Aus-ee ; '

Rate: 20.0 *C/ min Ident: 0.0 M.! ' UNIVERSITY OF TENEESSEE s

~ 8 I

g- x ! i w '

_ l Step Analysis

~

Height -2.37 mg

- l -10.06 %

U~

ResiC. 21.09 mg mi : 89.49 %

Opeak 1.18 Min 1

l d_. l !

m a

I .^ f '

- I I E

~

l \

l a

O- 8 m '

e i l

i .

100 .

C O . 5. 10. 15. Min

_. _J '

fy 1 1

October 30,1998 PGE A '

SamplefiS620 F11a:00012.001 TG HETTLER as-Aug-es i 21.137 og Rote: 20.0 *C/ min Ident: 0.0 IMIVERSITY OF TD NDBSEE M. '

i 1

. Step Analysis

. Height -3.30 mg f_

m

-15.63 %

. ResiC. 17.82 mg

[ ,

Dpeak 330 7 C ,

o-m '

Step Analysis Height -0.42 mg +

-1.99 %

ResiC. 17.41 mg d_

m l 82.35 %

. , Dpeak 517.3'C I. .

i .

g g . . .

g

..g . . . .

g . . . .

3 200. 300. 400. 500. 600. 700. *C S

__._.-____.:..-_________m _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ - . . . _ _ _ . _ _ _ _ _ _ _ _ _ _ . _ _ . _ _ _ _ _ - _ _ _ _ _ _ _ _ - - _ _ _ _ _ _ _ - _ _ ___ _ _ -_ . _ _ . _ _ _ _

October 30,1998 PGE B '

Sample #16621 File: 00013.001 TG METTLER 30-Aug-se 28.578 mg Rate: 20.0 *C/ain Ident: 0.0 UNIVERSITY OF TIDeESSEE n '

i

- i l o_ _

O w ~

! Step Analysis

! Height -2.54 mg

!. -9.51 %

l ResiC. 24.09 mg ar'- ! 90.30 %

l Dpeak O.95 Min 1

l 1

E 8

~ .

l !

m _ _ -

I

. I I

to_ a tn 8

. 8 i

r g g . . .

g g . . . .

100.*C0. 5. 10. 15. Min 3

Octolar 30,1998 PGE B '

1 Sample #16621 F13e:00014.001 TG METTLER 30-Aug-es .

24.195 og Rate: 20.0 *C/ min Ident: 0.0 UNIVERSITY OF TDGF!UEFF M. '

- r

[ Step Analysis

. Height -3.72 mg f_

m

-15.36 %

. ResiC. 20.46 mg

, 84.57 %

(

i j . Dpeak 330.7'C ;

~

o_ .

cn ,

Step Analysis 1

Height -0.60 mg

. r

-2.49 %

E- ~

_ ResiC. 19.76 mg 3

81.68 %

} E peak 533.3*C

- (

O-oo j . . .

.j . . . .

.j ...j....j ...g 200. 300. 400. 500. 600. 700. *C 4

October 30,1998 PGE C ,

Sample #16622 I File: 00015.001 TG METTLER 31-Aug-98 '

24.237 me Rate: 20.0 *c/ min w t i

Ident: 0.0 IAdIVERSITY OF TDumeFF

~

i 3 o .

O 1 W~ s Step Analysis i

Height -2.29 mg l i

8

-9.47 %

i I ResiC. 22.02 mg - '

in- :

m s 90.86 %

i Dpeak 1.18 Min e .

- 1 l

[

J e 8

8 O- a

% m m e ,

E E

. I i

3

~

l '

i nn- a m : t 8

5 I l I ,

i , . . . .

g . . . .

5 3

100.

C 0. 5. 10.

15. Min '

S

w

.---------'---a,b,g._.p 4% .e=- . - - - - - ' - ' - - - - - - - - - - - - - - ' - - - ' - - - - - - - - - - - ' ' - - - - - - ' - ' - - - - ' - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - ' - - - - - - ' - - - - - - - - - - - - - - - - - - - - ' - - - ' - - - - ' - - - - - '~-----------------------'-------------c'---

October 30,1998 PGE C .

f SamplefiS622 Fila: 00015.002 TG HETTLER 31-Aug-se 24.237 s0 Rate: 20.0 *C/ain Ident: 0.0

, n. '

UNIVERSITY OF TEmammerr I

a .

[

Step Analysis Height -3.39 mg s

-13.99 % !

$- ~

ResiC. 20.83 mg 85.93 % '

Dpeak 330.7'C o-m

, Step Analysis

, Height -0.57 mg

-2.34 %

ResiC. 20.17 mg

. s 83.20 X

$- Opeak 528.0*C i

.ie s a a a a

~

^

g g a a a g e a a a s e a g a g i :a e g a : , , - -

1 200. 300. 400. 500. 600.

I _.

700. *C

October 30,1998 PGE D '

Sample #16623 Fals:00o17.501 TG METTLER si-Aus-se as.esa se ante: 20.o *c/ min

n. n Ident: 0.0 UNIVERSITY F TENNESSEE

- I o _ 8 O '

m 8

Step Analysis l

Height -2.56 mg

-9.91 I i .

l i

ResiC. 23.28 mg i S~

' 90.07 E

- l Dpeak i.28 Min I

s

! t I ,

a

. ' 1 d_

m ,' _

,I 3

I 30 - 1 (D I l

l '

l ' ' = -

g ....,,,,, , , ,

100. 'C O. 5. 10- 15. Min 7

Oc t obe r_ _ 30,1998 PGE D .

Sample #16623 File: 0001s.001 TG HETTLER st-Aug-se l 23.246 mg Rate: 20.0 *C/ min Ident 0.0

, n. UNIVERS M OF TENNESSEE Step Analysis Height -3.21 mg

-13.83 X r'-

ResiC. 20.01 mg i 86.09 %

I Dpeak 333.3*C I *o-Step Analysis Height -0.63 mg

-2.71 %

ResiC. 19.30 mg in- ,

83.03 %

l I g .

...j....g . . . .

g . . . .

g -

200. 300. 400. 500. 600. 700. *C I

- - - - - - - - - - -_ - - -- - -o

October 30,1998 PGE E '

f -

SamplefiSS24 26.627 og Fila: 00019.001 TG METTLER 31-Aug-98 '

Rate: 20.0 *C/ain Ident: 0.0 M! UNIVERSITY OF TD NESSEE l !

O _

O -

M l Step Analysis

' l Height -2.70 mg

' -10.13 % .

to-ResiC. 23.90 mg m l 89.76 %

l Dpeak 1.07 Min I

~

l l

I i 3 o- a UA '

,8

l I

3 {

I l t I

i

. t in- i I

I l(D -

I l . . . .

j i . . . . . - -

100.

C 0. 5. 10.

15. Min

October 30.1998 PGE E ,

SamplefiSS24 File: 00020.001 TG METTLER si-Aua-se '

23.744 og Rete: 20.0 ' 'C/ain Ident: 0.0 UNIVERSITY OF TE N p'M- l

_ 1 s

Step Analysis

.~ Height -3.44 mg

-14.49 %

j

~

ResiC. 20.27 mg '

~

85.38 %

Opeak 328.O*C O-Step Analysis Height -0.64 mg

-2.71 %

j ResiC. 19.59 mg Dpeak 09

N i

,,...j ...g . . .

3 i . . . .

g 200. 300. 400. 500. 600. 700. *C

/d

October 30,1998 PGE F f Sample #16625 File: 00021.001 25.304 og TG METTLER 31-Aug-es Rate: 20.G *C/ain M - Ident: 'O . 0 LMIVERSITY OF TE70FWIFF t

8 E

. i 8-

~ !

. 8 Step' Analysis l Height -2.35 mg ,

-9.29 %

ResiC. 22.87 mg

$~ j

- 90.38 %

8 Dpeak 1.07 Min 1 9 I

I i ,

- l !

o- .

m j I

I t E

.= i .

n- 8

= l n

i 1

l i . .

100.*C0. 5. 10. 15. Min II

October 30,1998 PGE F -

SamplediS625 22.743 og File: 00022.00s TG METTLER 31-Aus-se Rete:20.0 *C/ain Ident: . 0.0 M . UNIVERSITY OF TDern!tFF

_ _ t, Step Analysis c Height -3.53 mg m-m -

-15.53 %

ResiC. 19.18 mg '

Dpeak 0 O-m-

- Step Analysis .

- Height -0.73 mg

-3.22 %

ResiC. 18.36 mg-E- 80.7.* %

~ -

i O-v '

l j I g . . . .

j . . .

g . . . .

200. 300. 400. 500.

3 ,

600. 700. *C I L. i

4 MATERIALS ENGINEERING AND TESTING CORPORATION 125 VALLEY COURT, POST OFFICE BOX 4536 OAK RIDGE, TN 37830 PilONE: (423) 482-7762 FAX: (423) 483-6995 September 30,1998 ME&T# 16620-25 Mr. Sham Beri

- Po:tland General Electric Trojan Nuclear Plant 71760 Columbia Riverlhvy.

Rainier,OR 97048 2

Dear Mr. Beri:

Per instructions, your 23 Al 4 0 -B C samples were analyzed by Inductively Coupled Plasma (ICP) and following results:

Samole ID PGE ID Boron (wt. %)

! 16620 A A 16620 B 4.14%

I 4.14 l 16621 A B 4.02 16621 B l 3.97

16622 A C 4.18 16622 B 4.22 16623 A D 3.80 16623 B 3.89 16624 A E 3.83 16624 B 3.70 l 16625 A p j 16625 B 4;36 4 04 I hope this information satisfies your needs. If you should have any questions, please feel free to call.

! Si cere y,

\ .

,{ f A ary Beth Norris 1

President, ME&T

i MATERIALS ENGINEERING AND TESTING CORPORATION !

t 125 VALLEY COURT, POST OFFICE BOX 4536 OAK RIDGE,TN 37830 (423) 482-7762 CERTIF2.CATE OF ANALYSIS FOR BORON CONTENT OF AL 2 30 -B.C PELLETS BY TITRIMETRY Customer Portland General Electric Powder Lot # A-F Report Date September 22, 1998 Sample Date August 28,'1998 '

l Comments Crushed to 100 mesh Log No. 16620-25 Specifications:

ASTM C 784-76, ASTMASTM C 751-75, ANSI / ASTM D 1193-77, ASTM C 791-94, C 809-94 i

~

ANALYTICAL RESULTS Lot No./ Boron Content (wt.%) *

(A) =

4.278%

(B) = 3.725 (C) =

4.036 '

(D) = 3.948 (E) = 3.835 (F) 3.937

=

AVERAGE BORON CONTENT Lo t No . A-F = 3. 9 6 0 %

The analytical results reported above were determined by MATERIALS ENGINEERING & TESTING CORPORATION in accordance with ASTM C 809-94.

I

k C ,

i.

i

[

l ry Beth Norris President, ME&T

s ..

%./ D;pirt f of Commerce Mturic m. Stans icti:nsl D Standards

-A. v. ne@.-birector M $ M 66

- L Standard Reference Material 951 Boric Acid -

113 B03 , acidimetric assay, weight percent . . . . . . . . . . 100.00 0.01 Absolute Abundance Ratio,8 D/'8B .............. 0.2473 0.0002 Boron.10, atom percen t . . . . . . . . . . . . . . . . . . . . . . . . . 19.027 i 0.013 Ba ron l l , atom percen t . . . . . . . . . . . . . . . . . . . . . . . . . 80.173 1 0.013 i The atomic weight of the boron, calculated from the absolute abundance ratio using the nuclidic masses 10.0129 and 11.0093,is 10.012.

This lot of boric acid was prepared to ensure material of high purity and homogeneity. As received, it was slightly deficient (approximately 0.01 percent) in moisture, but adjusts to a stoichiometric composition in about 30 minutes exposure to a normal room humidity (approxi- 1 mately 35 percent relative humidity). Once adjnsted to composition, the material is relatively insensitive (<0.01 percent) to moisture changes between 0 and 60 percent relative humidity, and ,

absorbs only about 0.02 percent excess moisture in room temperature humidities as high as 90 !

percem. The material cannot he heated as it decomposes with the loss of considerable water.

Afar was by coulometric litration of samples varying in size from 0.2 to 1.0 g of horic acid, i dissuived in 100 nd of a prenentralized solution 01 in kcl and 0.75.11 in mannitol. The inflection point of the potenti,nnetric curve obtained from measurements with a glass-calomel electrode system was taken as the end point. The pil of LI e maxinnun inflection point was taken as the end point. The pil of the maximum inflection point will vary from approximately 7.9 to 0.5 for the range of sample sizes given above, and the titrati/n must, therefore, he conducted in the absence of carbon dioxiIc or carbonates. The indicated tolerance is at least as large as the 95 percent confidence level for a single determination of any sample in the lot of material, and the average essentially indicates a baron hydrogen ion ratio of 1.0000, since separate examination shows the material contains less than 0.001 percent of free strong acid.

The abundance ratio was determineil by single filament solid sample mass spectronjetry using the inn Na2 HOf Mixtures of known 8 011/8 'll ratio (at a 1:4,1:1, and 4:1 ratio) were prepared from high imrity separated isotope solutions and used as comparison standards. Correction was delcr.

nnned for the 8 60/8 'O ratio (' 'll/O ratio, -0.00079) by measuring mass 90 using the high-purity boron ll separateil isotope. The indicated tolerances are at least as large as the 95 percent confidence limits for a single determination which inchules tenns for inhmnogeneitics in the mate-rial as well as analytical error.

The material was prepared by the J. T. Baker Company of PhiUipsburg, New Jersey, for the Argonne National 1.aboratory. Separaica isotopes were purified and solutions prepared by K. M. Sappenfield and T. J. hinrphy, coulometric titrations were made by G. Marinenko and C. E. Champion, mass spectromeiric measurements were inade by E. J. Catanzaro and E. L. Garner, ,

Analytical Chemistry Division. The various procedures developed have been published and are available in Special Publication 26017. i The overall direction and coordination of the technical measurements leading to certification

! were performed under the chairmanship of W. it. Shichis.

The technical and support aspects involved in the preparation, certification, and issuance of this Standard Iteference Material were coonlinated through the Office of Standard lleference Materials by J. L. llague. .

Washington, D. C. 20234 ,

W. Wayne Meinke, Chief

' February 28,1969 Office of Standard lleference Materials (Revised October 12.197 D j

tt l

l GALBRAITH5' LABORATORIES, INC. !

1 Accuracy with speed - since 1950 '

\

l LABORATORY REPORT !

1 1

1 i Detsy Norris Report Date: 09/17/98 Materials Engineering &

Sample Received: 09/08/93 Testing i Pureliase Order #: verbal 125 Valley Court Oak Ridge TN 37830 i Fax Number: 423-483-6995 l 1

SAMPLE ID LABID ANALYSIS {

RESULT (S) !

16620 Z-2492 flydrogen 3.28 %

16621 Z-2493 11ydrogen

, 3.30 %

16622 Z-2494 llydrogen

3.19 %

16623 Z-2495 flydrogen 3.34 %

16624 Z-2496 flydrogen 3.14 %

16625 Z-2497 Ilydrogen I 3.23 % i Note: Raw data package to follow.

1 i

i r

i l

WML:lc Cl fl1I This report shall not be reproduced, except in full, without the written approval of the laborstory.

qwkma%,,, f U S. Mxt: P.O. Box 51610 Knoxville, TN 37950-1610

,,1% Ottner Carriers: 2323 Sycamore Drive - Knoxville, TN 37921-1750

.. c. .ZL','O ,- .. Tel: (423) 546-1335 . Fax: (423) 546-7209

l GALBRAITH8 LABORATORIES, INC.

Accuracy with speed - since 1950 \

l l

l September 18,1998 Ms. Betsy Norris Materials Engineering and Testing 125 Valley Court Oak Ridge, TN 37830 ,

Dear Ms. Norris:

Enclosed please find the raw data that you requested for samples Z-2492 through Z-2497.

If we can be of any further assistance, please do not hesitate to call.

Sincerely, b .

Ann M. Lescher l Customer Relations Representative 1

l l

l wQ%l U.S. Afail: P.O. Box 51610 . Knoxville. TN 37950-1610 f1,TL Other Camers: 2323 Sycamore Drive Knoxville. TN 37921 1750 t IO"J'1 Tel: (423) 546-1335 . Fax:(423) 546-7209 !

9/18/98 L2: 19:04 l p u,,

; GALBRAITHS LABORATORIES, INC.

.../

Accuracy with speed - since 1950 Summary of Results and QC Runs Galbraith Sample Numbera

Materials EngineeringZ-2492 to Z-2497 ANALYTE =H Hydrogen; Method - ME-11 LECO CHN ------------

S C P O L M F

D O M G

A 5 I I P E S U I <'

I T N N A N N D N Z :

E I S G T D E e

=2492 CONTROL STD 98/09/15 T T E S i

P2493 CONTROL STD 3.278 % 20.50mg S G 483 285 t l 90/09/15 3.290 BHV205Grnd '

b2494 CONTROL STD 98/09/15 % 20.10mg S G 483 285 2495 CONTROL STD 3.192 % 22.60mg S G 483 285 BHV205Grnd 98/09/15 3.343 BHV205Grnd 2496 CONTROL STD 98/09/15

% 24.10mg S G 483 285

2497 CONTROL STD 3.143 % 20.60mg S G 483 285 BHV205Grnd 98/09/15 3.234 BHV205Grnd 0000 METHOD BLK 98/09/15 0.00

% 22.10mg S G 483 285 BHV205Grnd

0000 METHOD BLK 98/09/15 % 200.00mg S G 483 285 0000 METHOD BLK

.002 % 200.00mg S G 483 285

3483 CONTROL STD 98/09/15 0.00 % 200.00mg S G 483 285 )

98/09/15 6.867 % 10.70mg S G 483 285 t

3403 CONTROL STD 98/09/15 6.785 3483 CONTROL STD 98/09/15

% 20.10mg S G 483 285 1 i3483 CONTROL STD 6.955 % 14.20mg S G 483 285 98/09/15 6.637 % 24.30mg S G 483 285 2483 CONTROL STD 98/09/15 15.74 CR 3483 CONTROL STD 98/09/15

% 10.80mg S G 483 285 14.36 % 11.80mg S G 483 285 3403 CONTROL STD 98/09/15 15.8 1483 CONTROL STD 98/09/15

% 12.80mg S G 4G3 285 3483 CONTROL STD 6.825 % 12.10mg S G 483 285 98/09/15 6.741 % 22.10mg S G 483 285 CR 3483 CONTROL STD 98/09/15 6.694 CR 3483 CONTROL STD 98/09/15

% 11.30mg S G 483 285 CR 6.653 % 30.50mg S G 483 285 3483 CONTROL STD 98/09/15 6.597 CR B483 CONTROL STD 98/09/15

% 12.20mg S G 483 285 6.567 % 24.60mg S G 483 285 3483 CONTROL STD 98/09/15 6.881 B483 CONTROL STD 98/09/15

% 10.70mg S G 483 285 6.706 % 30.50mg S G 483 285 J000 METHOD BLK 98/09/15 0.00 % 200.00mg S G 483 285 j BHV205 1

yn*me%, U S Mail: P.O. Box 51610 Knoxvdle. TN 37950-1610

,J.",' Other Carriers: 2323 Sycamore Drive l

.. . 80~1%.. .. Knoxvdle. TN 37921-1750 Tel: (423) 546-1335 -

Fax: (423) 546-7209 l

.. .-m ,__ _._

e - ~ = - = = m ,.,_._._ _

i 13:49 seP_1u-98 N -i. t v o 9 O M h"a ~~-- - ,

g ,.% ,,'8'"=====rw s, s :,m.%

C at 3. 1 -a 3., c.-..\ .,.v_ m=-- 3. On

-- _m.___ ---o ID Code Weight

,~~w=---

^

Nitro 9en Standard

y. Error -

j646 5-3483 I2 2 Timo & Date-

!647 s v43 3 10.39 19 -

654) s-h4gk f' 10.27 i g," h' *2004 12:52 Sep-15-9g 635 s_34g3 '

10.37 10.36 +g.

12:30 sep_15_9g 3, * ",

10.41 10.36 .t. g . esc. . 0 3 1

13: 47 Sep-15-93

i.- 13:42 Sop-15-9s O 2. c1 gv '3 e

.P' o ta e n l

1 C'- =-< 1 a. b i^ st t i o n Nitrogen := 0.00026* Area e + 1 g46* Area - O.1352

-. Range -

g 0000 t- a t == 5.1449e_gg3 to 4.5202 mg Calibration time : 12: g7 Se p--15-98 -

]

New N i g .,... g g g , , ( !

e,, A L b y <n t i a 3, )

Nitrogen n O.poceyygrggm !

,,. l g, g,ggg to 1*5bO*NFeu - O.1369 I

,. Range :

I' I t = S. 1449e-eg3 4.3eg3 gq J Calibration timo 5 13 : 49 Se p- 1::.;-93

~~------=......_... - . ~ . . .

...-==.__.._.._. ---.~,..,.'_

'A T 'i ' .*t ,.;,

-=.=:=:..,_____.._

13:50 Sep-15sjc g y , ( ~., T~~ ~} ~ -- ' "" 5- - ;- . ==- - -----. ._ _ ___ _ m

u. l

"['[ ~" ~==:===-.: .(( .

~

,' { H e s t 3. [d '---~~~"O- -

Code Uoight

_ , _ , , _ _ Carbon Hydhohn tih1 og

" ~ ~ ' ~

~ ' ' - ~ ' ' ' - - :-

~

n Method OO G-a; 16 .

a wv433 ~~'~~~~--'.-.

I d. c.. 71 1", O

+7 G-3483 6.397 ig* 39 24.6

+0 Z-2492 -> 1 17 6.567 'iG-11BH F4 O I.

5f. "1, 10 2~ - 11BH-r9 Z-2493 1.095 3,e73 g 00l* 4m g 7~d494 c,a 0.965 3 96 Mlv:$~11BH c- >::

i I

>l

. 1 22.6 1 g00 0.02G isiE 11gy W l 2-2495 c 4. I a.19P e- W3b-s., e 977 - M.E-11BH l 2--2496 1

gg, g o . 3 4 o.- 9.g34

.??

a ,, y l ,_u, ' . NE-11BH l t-C497 .-

c c, . i i g"19 s.143 -

_U.U.19 4,_-11DH ,

' .+ s s.

. n, o "' '

s . d. s.,4

.'0 _ 10.7 71 gg C.,. L3a o .

irlE.-11BH l <

l c s'ie3 ..

a 0. ,c.,. 6.081 in' 4/

ih. r.c-11BH 8

]

71 bG 6 . < 0 t'

."==-z-..-....--m._____ ,

10.41 ME-11DH

--..___.__m.,,. __

l I

l

'1 e

i!64[ s 3433 Weight =

24.6 ug Op.orat:or: SG Method: NE-11DH 12:30 S*P-15-9G ID Code 2 : ACET _

ID Code o : #

C' = 71.17 H= go.2 )Q P: H.1733 C:7.11M 7:213 B:-3.024P:1.iiil C 1.f47B 1:113 6.567 % N= M.14 %

li: 59.225 A: 2.5118 C:1.B43 T:43 0:1503B:2.06B Prm. =Sli. 8 241. Press.=1031.3 M Pem=7H.4 !s st=79.5 SW88 b MM'^# K1=1.05773 K2=0.%833 K3=?.?4312 K4:0.SiiE6 sin 3=2.331 !=10 IK 34 0 Z-2492 Woiche =

20.O mu

-G 3erator:-SG 15 Code 2 : BH U205 Method: ME-11BH 13:04 Sep-15-98 ID Code 3 : GROUND f fC = 1.095 % H= 3,278 % N= 2.004-4O P: R67 C:0.ll M T:214 St-fE4P:0.tii3 C:1.0476 1:217 B:7.B13 A: 3.12H3 C:1.243 i:43 0:1523B:3.f68 Is hets.=120.4 fal. Press.=1031.4 M Press =iM.4 lase =762.5, K1=1.05764 K2:0.%733 K3=?.3H35 K4=?.Hi51 sin 3=?.3341 !=it.42

?? 49 Z-2493 Wei ht = 20.1 mg Operator: SG Method: ME-11BH 13:09 Sep-15-93 ID Code 2 : BH V205 ID Code 3 : GROUND g a #'

,C=/ 0.955 % H= 3.298 N=

P:1.53% C:t.liH i:2it 5:-?.$24F:3.iiM C:!.0476 Tri:0 5:2.f13 A: 0.134S C:1.f43 T:43 2:1!23 2:0.063

& 02G %

1R h tss.sili.4 !al. Pr m .=li31.3 P1 Press =7 S.4 Pise=762.5 K!=1 sw W &.85774 K2=196730 K3:2.HH5 K4:0.91951 sInhf.3341 D30.3 4G50 Z- 2494 Weight =

22.6 no Method: ME-11BH 13:15 Sep-15-90 Duerator: SG gQ ID Code 2 : BH V205 ID Code 3 : GROUND

'P i l] 7 l't '"""

.l. . Gt

% O( VJ 8

Q r/

/* tt Ua i O '*. s J s.'.

af hl - G eb"r c ./

R: :.93I) C:0.1; M 7:2!? E:-i.0:4;:?.7-!! :::.f473 i:110

.1. /* IN ~

Wa '4.8 *if 'T

. /c 5:f.fE6 A: 2.!F0 C:1.043 i:4 G:1503B:f.CEB

~ 7s irm.=ii?.5 !al. Prm.=!i31.5 si Pms=in.5 im=7515 K!=1.057H 7b3.?5714 Kht.9332J K4:0.H347 s(nkt.3341 !=93.3*6 E=1.f??3 N

Y 4651 2-2495 W l '.soe ra t o r : SG y M eicht ID Code

= 24.1 mg 2 : BH U205 Method: ME-11BH 13:20 Sep-15-9G ID Code 3 : GROUND -

~ V, h'u t . O '"/ ""/ r/ l..] _- 7 7 /, 7 tQ>

Jf f ~ hl s*] e"h ""5 4

/* Ii %.! . O "T s J s/. I'4 ~ r/

1.6H2 C:?.11 % i:li!

/ 1. a au V '"Y

/ =-

5:-2.05 P:2.3153 C::.047B 1:Ita 3:2.f!3 4: ?. 2H2 C:1.043 T:40 2::5?? i:f.fiS 3 ;rm.zili.5 isi. hess.=;?il.1 H ;tess=7H.4 fese=762.5 K!=1.05753 K2:3.%722 kb3.9H32 K4=J.HH2 s(nbi.3341 b?0.332 E=lE23 s 4 4 W V"*'

4652 Z-2496 We i:.h t = 20.6 No Jperator: SG Method: NE-11DH 13:26 Sop-15-93 ID Code 2 : BH U205 ID Code 3 : GROUND s "'

C= 1.155 % H= 3.143 % N= 0. 01"r %

1:1.M51 C:?.11 M i:2;E i:-0 E ,;:2.6725 C:1.f478 i:!:0 5:7.f!8 A: 0.!!!4 C:1.e43 i:4 6:1NJ 3:0.(19

sirm.=i!0.3 !al. iress.=:0 !.I ;i ;'m="H.3 !!!e=P. 5 K!=!.0:753 Phi.M7!4 Kb2.iH31 ?.4=l.iH52 s(ckt.331 !=i3.3!! E=1.?N2 S k u-- U^*

2653 Z-2497 Weicht =

22.1 ma Method: ME-11BH 13:31 Sep-15-98 l)perator: SG g ID Code 2 : BH U205 ID Code 3 : GROUND g,q.f'~

0 = /1. 038

{ :1.EG3 C:2.1;14 i:210

% H= 3.234 % N= %-033 %

i:-?.t N P:f 7271 C::.0478 i:113 i:3.tlB A: 0.1315 C:1.(43 i:43 6:12J 5:7.09

hm.=il?.3 *al.

Pr m .=:231.4 ;i ;7 m =7r.3 im 762.5 K!=1.i5734 K!=?.%7:4 KDP.H13 K4:0.H348 s(nbO.331933.303 E=!.t?N

G34 s-2403 Weight = 70.7 mg Method: ME-11EH 13 : 37 Sep--15-9G uou ra t; n e : SG ID Ceae 2 : ACET ID Code 3 : go, AM G= 71.09 % H= 6.881 % N= 1-0.24 %

' :H.1637 C:0.ll M i:ll! B:-3.fl4 P:0.7511 C:1.c476 i:211 B:0.t28 A: 1.17f0 C:1.043 i:4 G:1RJB:2.i!3 Mrm.=ii?.I fa!. h m .=!i31.2 il Eress=7i6.2 !ase=762.5 K!=1.05753 K2:3.%777 Kbt.97715 K4:0.9H4 sinki.331 bi?.35 K5:!EN

- - .. . _ . . - - - _ - . _ ___ . - . - . _ ~ .

.* ..w .a g . . ,

m New Hydeogen Calibration Hydrogen =

Range -0. :00568* Peak'* + 1. 048* peak - 0. 05553

) Fit = 2.1789e-003 0.0000 to 2.9318 mg '

\

Calibration tice : 12:07 Sep-15-98 !

_ _ _ - - - - \

r=u _.._-___.._

12:07 Sep-15-98 ;

N i t r c) g e n C a 1 i b ic- a t i o n G-ID Code Weight Nitrogen i

Standard f. Error 589 s-0000 Time & Date 590 200.0 0.000 5-0000 200.0 0.000 ---

06:56 Sep-15-98 59i s-0000 -0.006 0.000 595 acet 200.0 0.000 0.000 07:01 Sep-15-98 596 2. 3 10.91 07:0G Sep-15-98 '

acet 5. 4 10.36 +5.204 597 10.23 10.36 07:29 Sep-15-98 acet 10.7 -1.229 07:34 Sep-15-9G 598 acet 10.40 10.36 ,

12.5 10.33 +0.3901 07:39 Sep-15-98 599 acet 15.4 10.36 -0.2685 07:44 Sep-15-98 {

600 acet 10.39 10. 3G ' +0.3179 601 20.7 10.35 10.36 07:4G Sep-15-98 acet 30.4 -0.1256 07:53 Sep-15-98 602 acet 10.34 10.36 40.3 10.37 -0.1511 07:58 Sep-15-98 10.36 +0.06494 08:03 Sep-15-9G

' Old Nitrogen i

I Calibration Ni t rogen = -0. 0021 S*Are a': +

i Hanne : 0.0000 to 1.051xArea 4.5784 ra n

- 0.1354 u.

Fit = 1.4025e-003 \ ,

~ O Calibration time : 11 : 58 Se p - 14 *>6<p '

t i

j 0<

O o a.

ot o w Nitrogen O Calibration p '$ ',

Nitrogen = 0.00026* Area a 04 i

Range : 0.0000 + 1. 046* Area - 0.1352 5 Fit u S.14 f: 9 e-003 to 4.5202 mg Calibration time : 12:07 Sep-15-98 Lu L._.___.-=:=.. . . , . . .

..._2..-.. . _ . _ - - __-

M644 COND Weight =

Opscator: SG 5.2 mg Method: ME-11BH 12:41 Sep-15-90 ID Code 2 : BENZOIC ID Code 3 :

C= 68.60 % H= 5.110

ll.MI6 C:?.ll H i:2!0 B:-?.??4f:2.2?i4 C: .i.73 i:12

% N= 0.178 M h m. ?!0.5 hl. hm.=:23!d R kess@,5 Sist:I!2.5 3:M23 A: 0.13813 C:1.M3 i:43 C:ltiJ 5:0.lii K1:1.t37H KM.35722 XM.H?il KN.93378 shN.33411:sM25 c:MNa t'645 COND Weight =

5.5 mg Method: ME-11BH Doerator: SG ID Code 2 : BENZOIC 12:47 Sep-15-98 ID Code 3 :

C= 68.52 % H= 5.205 F:31.%s5 C:f.11% T:211 Br?.N4 P:0.32ii C:1.N! T:El!

% N= -0.114 :

5:2.72B A: 0.181B C:1.N3 T:43 E:ifta3:M!S H hess.=17.6 kl. Pms.=:011.5 9 hm=79.5 hit = 52.5 .

K:=1.25?) KM.%RS KM.?3354 KN.11W shM.3341 !=M 35 M MN3

646 s-348'3 Weight = 12.2 mg Method: ME-11BH Goerator: SG ID Code 2 : ACET 12:52 Sep-15-98 ID Code 3 : g o.QJ)')

3 C= 71 % H= 6.597 y. N= 1-0.25 '

1

n.wa ca.nu 1:m' i:. u 13 a n e. m = )

l

\m V4 i y

h DW h - o,s0 V e a KMYu - "" ge q-1545 , _,

- \

13 : ~$ Go p 90 L -

(MKtAn ir ,,,.m-mm,ma: n,,,.m,m ,,, -, ,- r t'2 . i 6 i e n t 1

F1onitor =-

'i Pararn et o r- = ~ m m m m m m ,.,m ,,-,, , __.. _ ._ .... l Value ..~. -..- = -_.. _ . .J Min i m ura Maximum Combustion Temp ('C) 1050 Catalyst Heater To:a p (*C) 1050 694 1050 l IR Oven Temp (*C) 50.1 694 694 {

He Flow Controller Tomp (oC) 40.5 50.1 50.2

TC Filament Current (mA) 40.5 40.5 '

90.43 90.41 Ballast Pressure (mia Hg) 700.6 90.45 Carbon IR Cell (Volts) 779.5 013.3 Hydrogen IR Cell (Volts) 8.3650 8.38*73 0.3394 G.7402 Nitrogen TC Cell (Volts) 4.0634 8.7296 8.7573 !,

r.w--a __..m.1-_ ::- : . .

4.GG34 4.0636 i. .

_ .... .. ..._ _.._ ...._ _ m .. ....m=__. _

_5 mw _.. _ rm . . . m - - n i .. ..m- , w. .

w=r =. = -

10 :lle de rs W,

-: i . : '. :> i e . > t :.,

., n. w .n .u an u.e .- .e .. . . r -. -

M o n i t'o v -

-.w..:.--=~.-r.-=.,

Parameb:'* .

s.= .

. . r- :,.e .

-.- -~

{

Value Miniraum Ma x i ta um

. - . - . . . N Combustion reco ( H.~' 1050 1050 Catalyst Heater Tean (cC) 1651 q 693 6%

IR Oven Temp (oCJ 33.0 695 j; Ho F i o w C o n t r o l .t o'r Toup ("C) 49.7 S4. 3 j,'

40. G 4 'd . 5 iC r i l o.m ? n t C'.mr e n t in D 90.33 09.C9 40.9 j bai.insc Pecscure . ni Hy) 90.30 022.7 G22. 3 023.1 N Carbon In Cel1 (Voll3) 6. 26~73 y liydronen 1 3 C o l .'. s,Volty>

i 6.1921 6.2919 0.5370 n.4C62 9.6519 ly Nitrogen TC Cell (Voit3) 4.0639- l

,r.,am-: ce . . - .-ru : .-,e , mu--:-w . . . -

4.0296 4.COSI

-- 0P n- -

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

m <.: r _ . .. . . . _. _ z .=n .. . . .. -

.r-:-- - :- . . . . - - ~ . . .-

1514O Seo-14-90 C o m 1:2i t at i o n L e in k Chec;R

-- i.e=== -g

.-umz=:.- =- . r zer x . ; . :. :. , =.nre. e r=.u .1..: .n..:. . .. : a .

,,i 2 - a.c. ..~:-- - - = = = = - - = = -=. :-A i .

Sysc'cm i.

Pressuro . . . . . 7Gd um Hg

$ h Initial Pressure . . . . . 927 ra m Hg Q

Currone wocsure . . . . . 927 ma Hg g o v

~--- h g 3 -

Chanuo in Pressuno . . . . . U um Hg 04 .I j

4 CC rahal Elapser! T i r.i o X i

. . . . 62 Seconds W !

l !hange in pressure . . . . . O ra m Hg

! i at GO Seconds ,

,'l.

Syatom Look Chock OK l' a

v.n. :=, -=. .- .. .- . . n-=.--. . = - - . . . - .

+8 e8

~

E Vp ye -

9 % -4 c y h S=

y tn g 9 9 s -

mk e k ok

'k E u

x h

h N h h

. N" .o o >> .'.o:B v =C -

b

) S E b $ h

&J 8 4 *$ + g "

s e , 2 I

m x m s -

y i b -

y t

u

~

A 0

>0 d

m wv12 m+ T Q y

R 1:

sl '

+ V\3 % g a

=- g -R -

2 5 3 :

5

% F 8

c

' a~:. ' O2 e

43 2n,;-

.7 mO W C. Q \

^

3 w m *%<c. i f*

m ,a E

V =

u o

- 5 7 Gaun cwa i

3yo wF

- 1W" 2 -t t4.il.

% e g D *1 g >*

%9

=

O L '9 V

aoa E

to-co 0 Q 5

. . . . . _- ._:. . . _ _ . . . m._ _ . . _ _ _ .

. ._ m .,__m ..m_-..__--._....-_m.. --

I C ,

?e [ & k )) b$

o n-p

?+

a.% pn .

hw--

r hhh/ , 3 l

D e o W 4 y

= + + F w e u o % --

4 9 y g 9- b ,

j c )u.eo . -g-4+4 V e%

n m p D s s,s S 8 T $ Y $8Y Y o a 8

% a h v t- 3 %. W N" $~

n p w e .;:

- . s ., r- g p e .n r, . :s 9c 1 r:

a

>D kf

~

n 3

~

% ~

e , : '

E y 2 '> z .o .

Q a ;

M 4 h b D

,S 9y e c e s - %%r w m o s s e s e .=

h D d S 'b b \i\ N $ eY s sO I s

'l y M k .

U e o.

's 8 9 gy 9 9 9 -

% $ m N dr O

z 4 %v3 3 o 8

o t',

353 2 32 (,jv aw 43 o g M 2 2 o 3 9

b9 2 2@3 2 V t1 N N 9 u t

3 a

t e s f -

=l al i !

l N .D M M N D h%F FD M $

cr 4u u -

wc d m $ $ .S M Yu M R $ $ !

e x 4 a s lu! i

^g <, v f K o 9 Q:w=* y r 4y 4m ,o v e .

9 4 9 w w 4 e j

- g

);, Y

$$ -s + y qEs =

l u 3 1 .g

(( !!! $ 1 4

}g $ $~ es t1 1w 5 s

{1( ! {r .

42v EE

. =

$ f f 5 hk h h g

"\

v i 'i \

['\@b i s i

! t, [SL h[ L%

s y ((!

Sg l

w w e w

$ $ p 'y' pJ g

e. o "

5 e g 1 i w % 6 $ - I % $ V. w +ngd 't w wwe

m $4 *W E !

[ N T w u p y g"9 9 9 e e g~ p 9

'8 M m u

%* 4 "-

i y Y V D C.W d <t?h f$4v E !

< 4 3 d 33 fO p 13 S. -a r

( k Y$$3A UU * 'y E

[!d % Iii h hh R ? ? Y h 'sy? --

I *-

Pio D g I

+ g y n $ '! % V 9 % @ e "U i "k'd s4gb 2 yob49

\

8 RE@ $

So5 5 o '

3#

?

3 1

v 3 3' S t #2 h"z7y!g 9 9 3 U i M a 8 7,

* *

E ?cE P E M. 3eo

'(

!- [ A l s = w 53 rIN

! T g g gg _ _ 13 4[4{9 g

v4 gl ll{f E j "$ p ha $

ii E }3 i n 1 h

}w(n{ i i L

!/18/98 l:19i04 q; GALBRAITH* LABORATORIES, INC.

Accuracy with speed - since 1950 Listing of Control Standards Galbraith Sample Numbers Z-2492 to Z-2497 Materials Engineering 3483 NIST 1473 Low Density Pol yethylene Resin 85.72 % C D483 Acetanilide 71.09%C, 6.71%H, 10.36%N 4

n4 men s k,# U.S. Mail: P.O. Box 51610 Knoxville, TN 37950-1610

,,\,%, Other Carriers: 2323 Sycamore Drive Knoxytlle, TN 37921-I750 mu I."J70a ,... Tel: (423) 546-1335 Fax: (423) 546-7209

i MATERIALS ENGINEERING Number: ANALYT-TRAN AND TESTING CORPORATION Rev. Date: l ANALYTICAL SERVICES Supersedes:

I l

Subject:

' ANALYTICAL TR AINING RECORDS l-i f Alary Beth Norris t l

QUALIFIED TESTS:

. Sample Log Balances .

Chemistry Prep Sample Prep for x-ray Spectrometer i

Sample Prep including Cut o!TSaw -

l Doron Carbide Sample Prep !

Liquid Dye Penetrant Prep

~

Alagnetic Particle Prep Pipettes .

i Schoniger Flask Combustion '

Oxygen Bomb Combustion j

-ICP (all instruments) - ' l

- Extraction's

. TCLP Extraction - '

4 Carbon by LECO -

Kjeldahl Nitrogen - -

Fusion's Dionex IC including programming *

. pil Meter '

Charpy impact Tester i

Salt Spray Analyzer Kjeldahl Nitrogen '

instrument Maintenance i t

t l

r ,,

l AIATEttlALS ENGINEEltlNG Number: ANALYT-TRAN l AND TESTING COllPOllATION Rev. Date:

ANA LYTICAI, SICitVICES Supersedes:

l l

Subject:

ANALYTICAL TRAINING RECORDS 1

l QUAllitlED TESTS-YMht/W TMi I -

J TCP *ajninc Sece 24 (417 kS3 )

Oh4 6 bc WNdlmect d'Yler Checa;h y1 4Le_. Abidem i bO 'b 2 a u S 8 x_ty Lq i , W i

l

.W 4

4 I

l i

1 -

I l

1

a , .e

a I

i l MATERIALS ENGINEERING AND TESTING CORPORATION 1 125 VALLEY COURT, P.O. BOX 4536 OAK RIDGE, TN 37830 i

l PIIONE: (423)482-7762 !

FAX: (423) 482-6995 <

i PROCEDURE FOR DETERMINING TOTAL BORON23IN4 AL 0 -B C BY INDUCTIVELY COUPLED PLASMA EMISSION SPECTROMETERY '

t 1.0 SCOPE i lids procedure covers the determination of total boron in Al:0 3-B4C.

l

2.0 REFERENCES

2.1 ANSI / ASTM C 751-75,C791-94, and C809-94 3.0 EQUIPMENT

7 3.1 Analytical balance. *

' 3.2 Plattner, Diamond Mortar and Pestle.

3.3 Glass Tubing, Glass blower's torch. '

a !

3.4 ' Mume Furnace. 4 s 3.5 100 nd Class A Volumetric Flasks. I 3.6 Vortex Mixer. i + '

3.7 Reagent grade clwndcals and NIST Standards.

3.8 j Inductively . Coupled Plasnui Emission Spectrometer, equipped as specified by the i manufacturer for analysis of elements ofinterest.

3.9 Regulator, two-stage, for argon. j t

3.10 Deionized water (resistivity greater than 1.8 x 106 ohms). t 4.0 PROCEDURE 4.1 'lhe sample is crushed with a Diamond mortar and pestic to <100 mesh (using a 100

~

mesh screen to classify the pomicr).

l 4.2 . Weigh .25g (+/ .0010g) duplicate samples from each pellet into heavy glass tubes.

4.3 Add 2 mis concentrated HNO to 3 cach sampic and a blank, 4.4 Mix with a vortex mixer and close tubes. ,

4.5 ' Place glass tubes into safety containers and heat for six hours at 340*C.

i 4.6 Cool to room temperature, open tubes and wash into beaker. '

4.7 Transfer concenirate to 100ml volumetric flasks and dilute to volume, adding Deionized water. !

4.8 Run sampics on the ICP compared to NIST traceable standards. '

i 4.9 Calibrate the spectrometer according to the numufactures reconunendations. !

4.10 Analyze a standard aller every sample. '

5.0 ' REPORTING Tile RESULTS

~~

5.1 Report the results using the CERTIFICATE OF ANALYSIS. All test data must be recorded and retained together with the calculations and copy of the fmal report.

5.2 Report any unusual test conditions. !

Procedure Number: PGE 1 Revision Number:

l 8/98 I

il I B4Ihbh orais -

President,ME&T l'

l' . . - - -_ - - - .

a f oa,, t.m nu ai a ca uar.ns ug[v OF Ita PAGE 02

SUMMARY

OF TGA RESULTS '

l 1

Sample 043: mal l' wt.

2 " w t. 3 " w t. Total wt.

Weight, Weight, 14es Lees Ims 14et.

an8 mg og % mg % mg %

.g %

16620 23.571 17,41 2.37 le 3.30 14 0.42 2 6.16 26 1M21 26.673 19.76 2.54 9.5 3.7 14 040 2 8.92 26 iM22 24.237 20.17 2.29 9.5 3.4 14' O.57 2 6.19 26 16623 25.852 19.30 2.56 9.9 3.2 12 0.63 ,

2 6.55 25 16624 26.627 19.59 2.70 10 3.4 13 0.64 , 2 7.04 26 16625 25.304 18.36 2.35 93 3.5 14 0.73 3 6.94 27 17065 29.344 22.83 1.29 4.4 4.2 14 0.74 2' 64 22 170 4 28.357 22.12 0.71 2.5 4.3 15 0.88 3 6.2 22 17067 30.535 23.48 1.5 4.9 4.6 15 e.97 3 7A 24 l

l 1

l

/

I i

I a

t i

! 7 GALBRAITH* LABORATORIES, INC. !

Accuracy with speed - since 1950 l

l l !

LABORATORY REPORT l

Betsy Norris Report Date: 11/04/98 Materials Engineering &

Sample Received: 11/03/98 Testing Purchase Order #: verbal 125 Valley Court Oak Ridge TN 37830 {

Fat Number -

423-483-6995 SAMPLE ID LABID ANALYSIS RESULT (S) DUPLICATE :

RESULT (S) l

- \

17065 Z-9474 ..

Hydrogen 2.62 % 2.47 %

17066 Z-9475 Ilydrogen i 2.38 % 2.36 % i 17067 Z-9476 11ydrogen 2.44 % 2.46 %

I l

l l

l WMUap Al This report shall not be reproduced except in full, without the wrinen approval of the laboratory, wn

c d". Q ICJE=

U.S. Mail: P.O. Box 51610 Other Carriers: 2323 Sycamore Drive Knoxville, TN 37950-1610 Knoxville, TN 37921 1750 Tel: (423) 546-1335 Fax: (423) 546-7209

's-

,, o- ,

l l

s l

l MATERIALS ENGINEERING AND TESTING CORPORATION 125 VALLEY COURT, POST OFFICE BOX 4536 OAK RIDGE, TN 37830 PIIONE: (423) 482-7762 FAX: (423) 483-6995 November 11,1998 ME&T# 17065-67 i

Mr. Sham Beri Portland General Electric Trojan Nuclear Plant 71760 Columbia River Hwy.

Rainier,OR 97048 ,

Dear Mr. Beri:

Per instructions, your following results:

2 Al 0rB4C samples were analyzed by Inductively Coupled Plasma (ICP) and g Samole ID EQEJR Boron (wt. %)

17065 A 1 3.88 %

17065 B 3.83 1

17066 A 2 2.46 2.41 17066 B 2.43 2.40 17067 A 3 i 2.54

! 170678 !

3.22

{

1 i

i hope this information satisfies your needs. Ifyou should have any questions, please feel free to call. '

I Beth Norris President, ME&T l

l

< ,, e MATERIALS ENGINEERING AND TESTING CORPORATION 125 VALLEY COURT, POST OFFICE DOX 4536 OAK RIDGE, TN 37830 PHONE: (423) 482-7762 FAX: (423) 483-699_5 PROCEDURE FOR TGA ANALYSIS OF ALUMINUM OXIDE-B 4 C 1.0 SCOPE i

This procedure covers the Thermal Gravimetric 2 Analysis of AL20 -y4C.

2.0 REFERENCES

Manual for TGA with a TG50 Thermal Balance. l 3.0 EQUIPMENT

A. Calibrate the balance.

B. NIST Calibrated weights.

C. TGA -Model No. TG50 Serial No. L50323 4.0 PROCEDURE ;

A. Calibrate the balance.

D. Run 1 of each sample at 20" C p' er/ min increase time. Ifold at 160 C for 10 minutes then continue to 800'C.

C. See reference procedure enclosed.

5.0 REPORTING A. Report the results using the TGA printout. All test dita must be recorded and retained together with a copy of the fmal report.

B. Report anylunosual test conditions.

Procedure Number: PGE-1 Revision Number:

Jdary Beth Norris President,ME&T

MATERIALS ENGINEERING AND TESTING CORPORATION 125 VALLEY COURT, POST OFFICE BOX 4536 OAK RIDGE, TN 37830 PHONE: (423) 482-7762 FAX: (423) 483 6995 Portland hie &I Galbraith 1 17065 Z-9474 2 17066 Z-9475

3 17067 Z-9476

. .1 O

"4-9

l . + , ,, q 1

MATERIALS ENGINEERING AND TESTING CORPORATION 125 VALLEY COURT, POST OFFICE DOX 4536 OAK RIDGE, TN 37830 (423) 482-7762 l

CERTIFICATE OF ANALYSIS FOR i t

BORON CONTENT OF AL 2 30 -B.C PELLETS BY TITRIMETRY ,

Customer Portland General Electric Powder Lot;#1-3 Report Date November 11, 1998 Sample Date _10/26/98 i Comments Crushed to 100 mesh Log No. l7.06.5-67 Specifications: ASTMC731-75, ANSI /ASTMD1193h7,kSTMC791-94, i ASTM C 784-76, ASTM C 809-94 ANALYTICAL RESULTS

~

Lo'; No./ Boron Content (wt.%)

(1) = 3.65% I 3.77 (2) = 3.58 2.44 (3) = 2.97 3.06 ,

AVERAGE BORON CONTENT Lot No. 1-3 = 3.25%

The analytical results reported above were determined by MATERIALS E.GINjERING & TESTING CORPORATION in accordance with ASTM C 809-94.

3 I

Mary Beth Norris President, ME&T l

l' l

ML20196E285

Contents

Text

Dear Sir:

Background

2.0 REFERENCES

Dear Mr. Beri:

Dear Ms. Norris:

Subject:

Subject:

2.0 REFERENCES

SUMMARY

c d". Q ICJE=

Dear Mr. Beri:

2.0 REFERENCES

Navigation menu

ML20196E285

Text

Dear Sir:

Background

2.0 REFERENCES

Dear Mr. Beri:

Dear Ms. Norris:

Subject:

Subject:

2.0 REFERENCES

SUMMARY

c d". Q ICJE=

Dear Mr. Beri:

2.0 REFERENCES

Navigation menu

Search