ML19224A950
| ML19224A950 | |
| Person / Time | |
|---|---|
| Site: | Crane  |
| Issue date: | 11/12/1976 |
| From: | Metropolitan Edison Co |
| To: | Mullinix W NRC/IE |
| References | |
| 1954, TM-0193, TM-193, NUDOCS 7906130272 | |
| Download: ML19224A950 (4) | |
Text
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TMI DOCUMENTS N'
DOCDENT NO:
0F DOCDENT PROVDED B'l g
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15~',OPOLITMi DISON CCMPMrf.
Wilda R. Mullinix, NRC 179 093 9
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MASTEi COPY 4tisto 00 NOT REMOVE 1 /i2/76
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THREE MILE ISLAND NUCLEAR STATION STATION CHEMISTRY PROCEDURE 1954
.'[i5-CETERMI:iATIO!10F IRO?i-59 CONTROLLED v
Table of Effective Pages Pne Do'e R evision Pace Date R evision Pace Date R evisica 1.0 11/12/76 1
26.0 51.0 2.0 12/14/73 0
27.0 52.0 3.0 11/12/76 1
28.0 53.0 4.0 29.0 54.0 5.0 30.0 55.0 6.0 31.0 56.0 7.0 32.0 57.0 8.0 33.0 58.0 9.0 34.0 59.0 10.0 35.0 60.0 11.0 36.0 61.0 12.0 37.0 62.0 13.0 38.0 63.0 14.0 39.0 G4.0 15.0 40.0 65.0 16.0 41.0 66.0 17.0 42.0 67.0 1 S.0 43.0 68.0 19.0 44.0 69.0 20.0 45.0 70.0 21.0 46.0 71.0 22.0 47.0 72.0 23.0 48.0 73.0 24.0 49.0 74.0 25.0 50.0 75.0 Unit 1 Staff Recc me6ds] Approval Unit 2 Staf f Reco. mends *ppproval l-l1 l
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I Date Date Approval Approval Ccglizant'# 4:t. Head Ccgn!zant'D ept. Hi,3d 0
Unit 1 PO RC f'ecomr ends Approval Unit 2 PORC Recommends Approval 2 vib ?AA Date /$nl?6 Tu m Wu Date /l~II' N
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Chairman of PORC ghairman of PORC PCPC comments of -
included PORC comments of included (date)
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1954 Revision 1 11/12/76 Determination of Iron-59 Station Chemistry Procedure No.1954 1.0 Su mary Radioactive iron and added iron carrier are separated from other contributors to total activity by hydroxide precipitation, liquid, liquid extraction, and finally ion exchange. The separated iron may then be counted either in beta detector or gama spectrometer.
2.0 Accaratus 2.1 Countin; instrument 2.2 Ion exchange column 2.3 Separatory funnel 2.4 Analytical balance 3.0 Reacents 3.1 Ammonium hydroxide; concentrated.
3.2 Anicn exchange resin; chloride form resin, 200 to 400 mesh (Dowex 2-X8 satisfactory). Make a slurry with water and trancfer to the column until a layer about 12 cm deep is formed. Wash with 50 ml of water and 50 ml of concentrated hcl before each use.
3.3 Ferric chloride carrier; (49 g/1) dissolve 49 g of FeCl 6H O in 3
2 100 ml of hcl (1:19) filter and dilute to one liter.
(10 g Fe icn/
liter).
Standardize by precipitation of hydroxide, filtering, and igniting to ferric oxide (Fe2 3)-
0 3.4 Hydrochloric acid; conc.
.5 Hydrochloric acid; (1:19) Mix one volume of conc hcl with 19 volumes of water.
3.6 Hydrogen peroxide; 30 per cent. i 3.7 Nitric acid;> conc.
1.0
,d g/J
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3.8 Nitric acid-hydrofluoric acid; Mix one volume of conc HNO.
3 one volume of conc HF, and 98 volumes cf water.
3.9 Nitric acid-Hydrcqen Peroxide mixture; 'iix 5 volumes of conc HNO, two volumes of 30% H 022 nd thirteen volumes of water.
3 3.10 Thenoyltrifluoroacetone (TTA)-xylene; (111 g/1) dissolve 111 g 9
of TTA in xylene and dilute to one liter.
3.11 Xylene; reagent grade.
4.0 Precedure 4.1
.take the sample just acidic with conc hcl and add 2 ml in excess.
4.2 Add Iml of FeCl3 carrier ar.d boil for 2 min. to ensure solution of all the iron.
4.3 Add excess NH 0H to precipitate the iron and pour the mi ;ture into 4
a centrifuge tube.
4.4 Centrifuce and discard the supernatent.
4.5
'l ash the precipitate with 15 ml of water, discardina the wash, add 3 ml of water and 10 ml of conc HNO -
3 4.5 Stir to dissolve, add 1 ml of H 02 2 ^"
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a.7 Transfer to a separatory funnel, add 15 ml of TTA-xylene and extract for 5 min.
Discard the aqueous (Icwer) phase.
d.3 Wash the extract and vessel walls with approx 10 ml of : vater and discard the wash. Transfer the extract to a clean secaratory funnel.
4.9 Add 15 ml of nitric acid-hydrogen peroxide mixture, shake for one min.
and discard the aqueous phase.
4.10 Transfer the extract to a clean separatory funnel, wash with 15 ml of nitric acid-hydroflouric acid mixture and d'iscard the aqueous phase.
2.0 179 096 t
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1954
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Revision 1 11/12/76 4.11 Transfer the extract to a 4th clean separatory funnel, add 5 ml of conc hcl and mix until the organic phase becomes colorless.
4.12 Discard the organic phase and wash the aqueous phasa and vessel with 10 ml of xylene.
Discard the xylene.
4.13 Evaporate the aquecus phase just to dryness and dissolve in 20 ml of conc 9C1.
Pass through the prepared resin column.
4.14 Wash the column with 40 ml of conc hcl and then with 40 ml of HC.
(1:1).
4.15 Elute the iron fr:m the resin with 30 ml of water.
4.16 Precipitate the ircn with an excess of NH CH and filter on ashless 4
- paper, a.17 Dry the filter and precipitate and ignite to Fe2 3 in a porcelain 0
'leigh for che.tical yield.
crucible.
a.13 " nt the_FegG3 and coun:.
5.0 REFERENCE 5.1 1973 Annual Scok of ASTM 5:anderds, Part 23, D 2461-69.
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