ML19224A953
| ML19224A953 | |
| Person / Time | |
|---|---|
| Site: | Crane  |
| Issue date: | 11/12/1976 |
| From: | Metropolitan Edison Co |
| To: | Mullinix W NRC/IE |
| References | |
| 1955, TM-0194, TM-194, NUDOCS 7906130276 | |
| Download: ML19224A953 (6) | |
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TMI DOCDENTS
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DCCUMEtiT NO:
1 CCFf MADE ON OF DOCDZ!iT PROVIDED BY MET 20PCLITMI EDISC:1 COMPriY.
$$Y' Wilda R. Mullinix, NF.C
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71 179 i49
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MASlER COPY 1955 Revision 2
f DO NOT REMOVE THREE MILE ISLAND NUCLE AR STATION STATICN CHEMISTRY PROCEDURE 1955 h
CETERMINATION OF PADIOSTRCNTIUM Table of Effective Pages Pace Date Revision Pye Date Revision Pace Date R evision 1.0 11/12/76 2
26.0 51.0 2.0 C4/30/75 1
27.0 52.0 3.0 04/30/75 1
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,r 1955 Revision 2 11/12/76 T11REE MILE ISUd*D NUCLEAR STATION STATION PLANT CHEMISTRY PROCEDURE 1955 Determination of Radiostrontium 1.0 Su =a ry Sa=ples of fresh fission products, such as fresh reactor coolant, cay contain up to four isotopes of strontium, 2. 7 hr Sr -92, 9. 7 h r S r -91, 51d Sr -89 and 28y Sr-90.
Due to the lengths of their half-lives, enly Sr-89 and Sr -90 are of significant interest.
Contribution o f Sr -91 and Sr -92 may be disregarded if the sample is aged for four days prior to che=1 cal separation.
A count taken i=nediately after separation will censist of the centri-butica from both Sr-39 and "r90.
A count taken 16 -24 h r a f t e r s e pa ra-tien will show an increase in ecunt rate due to the presence of Y-90 ingreuth if Sr -90 is present.
3y estinating the percentage of the Sr-90 to Y-90 equilibrium attained the Sr-90 compenent in the original sample can be determined.
The Sr-89 is then determined by subtracting the Sr -90 counts from the count made i==ediately after separation.
2.0 Accaratus 2.1 Centrifuge 2.2 Centrifuge tubes 2.3 Nine em filter papers
'4 hat =an J42 o r equiv.
2.4 One inch diaceter glass fiber filters - Type GF/C 2.5 Pyrex filter apparatus 2.6 Ice bath 3
- 2. 7 Plastic film (thickness <2 cg/ ca-)
2.3 3 eta counter 2.9 2-incn planchet 1.0
19.55 4/30/75 Revision 1
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3.0 Reacents 3.1 Acetate Buffer Solution (2M); Dissolve 230 ml glacial acetic acid and 154 g of ammonium acetate in reagent water and dilute to one liter.
3.2 Ammonium oxalate (saturated soln); Add 40 g of [(T1H )2 2 4 H 0] to 4 C0 2
500 ml of reagent water and warm to dissolve.
Cool to room temperature and decant the liquid into a bottle containing approx. 20 G of [(NH )2 p 4 C0 4
H 0] crystals.
2 3.3 Barium holdback carrier (10 mg Be/ml); Dissolve 19 g of Ba(NO )2 in reagent 3
water and dilute to cne liter.
3.4 Iron-yttrium carrier (10 mg Fe/ml and 10 mg Y/m1); Dissolve 75 g of
[Fe(NO )3 2 ] and 39 grams of [Y(NO )3 '
H 0] in reagent wa h 3
3 2
Add 3 al conc HNO and dilute to cne liter.
3 3.5 Methyl Red indicator (0.2 mg/ml); Dissolve 20 mg of methyl red in 60 ml of 95% ethanol and dilute to 100 m' with reagent water.
3.6 tiitric Acid (6M); Dilute 400 ml of conc HNO to one l her with rcagent 3
water.
3.7 Sodium Carbonate (Im); Dissolve 106 g of Na C0; in reagent water and dilute 2
to one liter.
3.8 Scdium Chromate (2M); Dissolve 684 g of N 4
1CH 0 in reagent 'ater 2 r0 C
2 and dilute to one liter.
3.9 Strontium Nitrate carrier; Dissolve 35 g of Sr(NO )2 in reagent water 3
and dilute to one liter.
4.0 Procedure 4.1 To a 10 ml aliquot of sample in a 50 mi centrifuge tube, add 1.00 ml of strontium nitrate carrier, two drops of methyl Fed indicator and i
then 6M HNO dropwise until the color changes from fellov to pink.
3 2.0
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1955 4/30/75 Revis ica 1 4.2 Heat to near boiling, add 1 =1 of 1M Na3CO and continue heating and 3
swirling for about 3 min.
4.3 Centrifuge, discard the supernatent and dissolve the precipitate in 2 al of 6M HNO.
3 4.4 Add 15 ml of f uning HNO.
3 CAUTICN:
Fuming HNO3 is very corrossive.
Use appropriate ckin and eye protection.
4.5 Cool the strentium nitrate precipitate with frequent swirling for 5 min. in an ice bath centrifuge and discard the supernatent.
NOTE:
"se large quantities of water to dilute the fuming nitric acid -tstes.
4.6 Dissolve the precipitat2 in 1 ml of reagent water and repeat steps
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an u, a.:.
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4.7 Dissolve the precipitate frca step 4.6 in 10 ml of reagent water, add 1 al af arcn-yttrium carrier and heat to boiling.
Ada conc ?!H CH dropwise until ferric hydroxide is ub t e rved t o f o rm 4.8 4
and coagulate.
Record the time as the ti=e of final Y-90 separation.
4.9 Centrifuge and decant the supernatant solution through a folded b'hatman No. 42 filter paper into a clean centrifuge trbe.
Discard the precipitate.
4.10 Add 1 al of barium holdback carrier, 2 drops of methyl re ni 6M lino 3 dropwise until the solution just becomes pink.
4.11 Add 3 al cf acetate buf fer, heat to boiling and add 1 al of 2M Na3 rO4 dropwise with swirling to induce formatien of 3aCr04 C
sf th occasional swirling.
Cool in an ice bath for 5 min.
179 153 l
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1955 4/30/75
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Revision 1 4.12 Centrifuge, decant the solution throegh a folded Whatman No. 42 filter paper into a clean centrifuge tuba and rinse the filter with several al of reagent water.
Discard the filter and precipitate.
4.12 Add 2 =1 of cane NH,0H, heat to near boiling and slowly add 5 al of 4
saturated (NH,)3C,0.
Continue swirling for several minutes and then 4
4 m
a cool to <30 C in a beaker of water.
4.14 Filter the precipitate onto a tared glass fiber.
Wash with three 10 21 portions of reagent water, followed by two 10 21 portions of 957. ethanol and two 10 ml portions of diethyl ether.
15 Dry the filter at 110 C for 10 min. and allow it to cool in a dissicator.
4 4.16 Weigh the filter and mount it in a 2-inch planchet for counting.
It should be sealed with plastic film.
4.17 Beta count the filter within 1.5 hr. after chemical separation.
This count represents the sum of Sr-89 and 3r-90 counts.
Re:crd as C.
1 4.13 Eeta count the same filter again 16-24 hr. after chemical separation.
Any increase ever the count taken within 1.5 br. of chemical separation is due to ingrowth of Y-90.
Record as C.
3 4.19 Calculate the activity of the Sr-90 as follows:
Sr-90(uCi/ml) = (C -C e af )
i 2
i
-3a-) + (p 40)(1-0_)b-1)]
2.2 X 106 y g. [ (FSr-90) (' -e Y-Where: C = initial beta counts / min from step 4.17.
C, = beta counts / min from step 4.13.
t F
beta ccunts per disintegration for a I-90 source
=
Y-90 (From calibratica curves in 1955.1).
FSr-90 = beta counts per disintegration for a Sr-90 scurce (Frca calibration curves in 1955.1).
Y = chemical yield.
'J 3
t = elapsed time between C and C in hours.
2
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e m
1955
-M.,
Revision 2 11/12/76 A = decay constant for Sr-89 a
A = decay constant for Y-90 b
V = sample aliquot volume in cl.
4.20 Calculate the nu=ber of counts in C due to SR-90 as follows:
y C) = Sr-90(uci/sl) X FSr-90
("
Where C unts/ i in first beta count due to SR-90.
3 F
= beta counts per disintegration for a Sr-90 Sr-90 source (From calibration curves on 1955.1) 4.20 Calculate the activity of Sr-89 as follows:
Sr-89 (uci/al) =
(C, - C,) e*lat2 6
(2.22 x 10 ) (FSr-89) () (Y)
Where: F beta counts per disintegration for a Sr-89
=
3 _gg source.
(Frca calibration curves in 1955.1).
t = time fres sampling to time of first count (C
_ _1). _..
2 5.0 REFERENCE 5.1 5 &'a' Radicchemistry Manual
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