ASTM E417-75

Method for Colorimetric Determination of Technetium in Aqueous Solutions (Withdrawn 1977)

General Information

• Status: Withdrawn
• Technical Committee: E10 - Nuclear Technology and Applications
• Drafting Committee: E10.05 - Nuclear Radiation Metrology

Standards Content (Sample)

4~ D•lgnMlon: E 417 - 75
8t11ndard Method for
COLORIMETRIC DETERMINATION OF
1
TECHNETIUM IN. AQUEOUS SOLUTIONS
nil Slalldard le !Ma'!CI undm; tbe med ~on B417; tho 1111111ber lmmedlatlly follawlJll tile dlliaati09 iadic:atel t1ie
Y8I!' of oftalml lldoptioa or, lD the CllC or nmaon, tho JCl1 of 1ul rm.Ion. A •mber ID puentbam lmllcatel tho ,ei.r of
1ul reapproval.
1AU PIMtliod, wAltll liu ~~by E J11, fl Hf"6 ball0tnlpwt1Wrawol by IM~t:a"'rrrtltee.
INTl.ODUCTION
This method• wu developed for the determination of technetium in 1olution1 of nu­
dcar fuel tl!at contain radioactive nuclidcl. The ncod for thil method aroae in laborato­
ries of the nuclear m,ergy industry where a 'wide variety of nuclear-fuel 1olution1 con­
taining technetium are encountered . The tctrapropylimmoniu!D4thioc:yanate method ia
described for the determination of technetium in aqueous aolutions.
1. Scape thiocyanate complex in chloroform. AD the
technetium in tho mea1ured volume of 1am~
1.1 Thi1 method coven quantitative deter­
ia flnt oidcli7.ed to tccbnctiuin (VII) by ba:lic
mination of technetium in known volumes of
hydrQg~n peroxide. Tho alkilinity of the eolu­
aquooUI •olu~on1 of nuclear fuel that contain
tion must be between 2.6 and 3.S M for quan­
radioactive nuclidca. T- aolution1 are from
titative extraction of the tecl\netium-tetra­
the proccaafng of irradiated nuclear fuel and
propyl ammonium ion-a11ociation complex
from the laboratory 1tudie1 on irradiated nu­
into the chloroform solvent. To usure com­
clear fuel.
pkte extraction and recovery of the techne­
l.2 The method 11 described. ia applicable
tium, two extraction• are nece11ary with
to 1olutioo1 that contain a minimum of S 1'11
careful waahin11 of the aqueous phase with
of technetium per 1amplo, but it will detect a1
chlorofo~. Color development ii niade in tho
little u 0.4 µg. At concentrations above 200
chlo~form. pbue with the addition of 1trong
µg/ml, dilutions mu1t be made. The absorb­
~nc acid, tetrapropylammoniwn hyd.rox-
ance ia li~r from 1 to 20 1'11 of technetium in
1de, and potl!.l~um thiocyanate. The colored
the final aolu~ion. The method as delcritied is
chlo~form pba1e ii tranaferrcd to a voiu­
limited to sample volumea of 2 ml or lea, but
~ctric fluk. After diluting to volume, a por­
reagent volumes can be scaled to accommo­
tion of the solution i1 placed in a clean .1-cm
date lar11er aample aliquot•.
absorption cell and it1 ab1orbanc:o measured
1.3. Pbotometcn 11.nd photometric practice
agalnat a ~gent blank. The colored complex
prescribed in this method shall conform to
absorbl at ·s13 nm, baa a molar extinction
ASTM Recommended Practice .B 60, for Pho­
coefficient of 46,000, and i1 stable fdr aevcral
tometric Methods for ChemiCat Analy1i1 of
houn. The concentration of technetium in the
Metala.'
NOT! I-The valvea 1tatcd in U.S. cvatomary
'Tbla .Uod i9 1111cler the juriidictioa of ASTM
unit••~ to be "'1ardcd a1 the standard. The metric
Committee B-10 OD Nucl.ar AppllcatioD1 lllcl Meuurtmmt
!'Quivalent1 of U.S. cultoma,Y uniti may be approx-
of Radi1tloa Bfl'lc:U.
imate. .
C.mat edltloe •JllllO"li ·Ju. 24. 1975. Publilllied
March 1!175 . Orisinll!y plabHllbad u B417 - 70 T Lan
2. Sammuy of Metllod
previou1editionB417 -'10 T. ·
t POiter, Jl. 'E. ~acx:t. W. J., ad Rela, J, B., AIMlyt.
2.1 Thia method ii bued upon the meuurc­
inl CTl•lfllalry, A.NCHA, VoU!I, 1!167; v. 3!1.
•A,._, aoot q/ AnJI .,.,., Pait 12.
mcnt of the absorbance of the technetium~
841

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E417
4.S Tubl Fumoe1, 1-in. (2S-mm) diameter
sample i1 determined from two comparison
1tandard1 bracketing the unknown and proc­ capa~ of reaching a temperature of 1112 F
(600 C). The furnace should be fitted with a
euod coQcurrcntly, or from a 1tandard curve.
quartz tube which extends 3 in. (7S mm) be­
3. JJarren11ee1
yond both end1 of the fumace.
4.6 Quartz Botit.r, 2 in. (SO mm) long by IA
3.1 Thi1 method ia highly 1pecific for tech­
in. (13 mm) wide.
netium. No metal ion interference has been
4.7 Erl111m111r Flmk, l2S ml, fitted with a
found from aluminum, vanadium, cfiromium
(lll), mii.nsane• (11), iron (111), cobalt, nickel, '%. atandard-taper joint.
copper, strontiom, zin:onium, niobium (allo
4.8 R•fla Co"'1.,,8tr, 1traight-tube, frtted
known a1 colwnbium), molybdenum, ruthe­ with a '% standard taper joint-.
1
·nium, rhodium, palladium, lilver, cadmium,
s. a . •• Materlall.
tin, antimony, larithanum, tantalum, tung1ton,
S.1 Purity of R10pnt.r-Reap:nt grade
rhenium, platinum, gold, mercury, bi1muth,
chemical• lltall be UICd in all teats. Unleu
thorium, and uranium. Technetium can ~
otherwise indicated, it i1 intended that all ~
succeu(ully determined in solution• of alumi­
m.~m-clad uranium fuel, aluminum-uranium al­ agents .shall conform to the 1pecification1 of
loy fuel, Zircaloy-clad uranium fuel, 1tainle11
the Committee on Analytical Reagents
...