Text

Determination of Low Concentrations of I-129 & I-131 in Milk Samples.
	ML19317H171
Person / Time
Site:	Arkansas Nuclear
Issue date:	09/18/1975
From:	Thomas C; Battelle Memorial Institute, PACIFIC NORTHWEST NATION
To:	;
Shared Package
ML19317H162	List: ML19317H171;
References
	NUDOCS 8004210654
	Download: ML19317H171 (7)
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.. .~.~ . ENCLOSURE 6 n :

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f... > -

' DETEPJ1L.aTION OF LOW CONCENTRATIO.:.3.OF . ; IODINE-129 ,

l R; .

(* , ,,

' AND IODINE-131 IN MIIK SAMPLES ,

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C. W. Thomas Battelle Pacific Northwest Laboratories - -

'. , . o . -

A. procedure.is described for the analysis of 131r and I

,, in milk. samples; which permits very accurata measurements of 0.2

.. . m pCi/Iiter.. At 'these . concentrations, measurements are possible -

A.. ' . . .c . , -'

z, -

i- : -

. .. . ::: witiv af standard': deviation..of' better - + han *10 % . The milk is; prese: -

?..::. m:9-?.., p. p .,.[.+..y :;g :G n.s.

- + : . ::s : . .;.4.:.:6;:= ...~ :' . . . 1

[:,$.$'.&.l.. : att sampling- byjadding .80.: mis'cifformaldehyda con 4

';.l..& : ? :. ;. . - ;'

~

.: . . ,:. .:. v.. : C4..: W ;.

.GJ.EW 'carr. Cier; :;Q:and ... - a afew.

. fdropse of- .

L M:' sodium-hisulfita .- per- four-liters.

. W:.t:m: 4 A;.:g.. - ::

?-

. . . .: ? . '. h ;m.: g :s' t; .; :-; ;~ .:

,.. . . F.:: ;;.M.g.; :

?.3.;.:,?:,.

n:- py . .~%ri.

s of. 'milke sa -

+~. .Thise. . e _ p ::: preservative

a. . - : ..

techniquei has

_ . . .; _ ; ... .: 9. .

been..shown n : ,w to h l

- .fr :p n,... : 0.i him:X .v. .affact .

. . . n:-:3;,.. on. t. . the-overal.1

r. . .. :.: u . . :- Vield-of- the procedure.

w.:w.. 7 . Tha-procedure-invoq

..: : -:.. .~ ._ :- ~ . , : . ::.~--

1,r=gg : st4 v'n.- + vgg. 's ' liters lo_ f milk...with anion exchange resin _ Tliac.radiciod 2 . .i.: - .. , .. *

.' . . . .. v .: < . . .

=

.r- ;:- -

L...l*c\

'fr. ' ist sub'sequently extracted,from the resin using a 5% hypochl

.- . 2. y: -

y..:s. p;.~.-

. . r ... . . .

. . solution After reduction.of the radiciodina with. hydroxylamine' .

. ;R::.t..: .

_- .'_, n. -

~ ~

e;- -

1-g. .. :- hydrochlorido,.. it.:is extracted. into carbon tetrachloride, reduced v

.- : . . - . .with. bisulfite,.. 'and back-extracted into water.

. . . . .h' . .

The radiciodina-

m. .. . - ..

- YE, . is then precipitated as palladous iodide. Chamical yield based or s-added; icaine carrier is determined gravi-=trically. .The 13y I is -

Y mer.sured by counting in a low background properticr4 gs.s.flou

., . .e .

i beta counter. .

i The following list contains the special apparatus, chamical reagents, analytical procedure required in.the procedure; m

7 '

i l

80042.10 bb T. -

l 1

l I

~.

1 -

p -

sp nca.42. ne en a w.= .

. ._ g ,;

~

. 1. . Ascor^ d ci=ac of glaca beakerso - ? .' .

'~

' ' ~ "

2. . Hot" plate

. .i - -

3. .Magne. tic.stirre.r .

f...~. ... .

~

4. Suction filtering apparatus - -

5.. 250-ml and.125.ml separatory funnels

~

6. Low-background beta counter (nominal SacNround.

<1 count per min. )

7. Nylon rings and discs, M'ylar, glass fiSar paper .C2.3

..~ .

cm) (see HASL 300) . .__..,-0 r-a -

' . .s, y,,* . , { - .K.:;[_,"-

. ':~, * = - .. . .. % .,.

_ .,...... s

. , . j...s. .r _ ; , , ny, <.

.. , .Raagents'and Chema..cals-

.: . - ~, ; . :;.

.x v.r ' :,~. i.. ,. ._..*:... ..p. - +. .w:.~

. s.- -

,. . w.. . .a,

. .e..

~

1 *

.1 43odide:- carrier;, 10 mg/ml *

. dissolve.1.181 grass .Nar *

..g y . .e.. . , . . , . ..-

_ . .c . ; y , .,.., . . . .y..

r.-

.. v . . :.. .. ., ....,ut..,; .:. ,

. . . ..a... . . . . ..,-.:..,, ..

.. . ' . .in.,100 .mL. water e ->: .

w ..s . o.:. .. .

=

.;y.u. - . . .: . - . .

,. . ' ' ~ - '

o v. j. :G.;~ ~

. ..~..,...'a

2. ' DowexcI . :c,.50-100' : 8. . .. ... : :: : CL. ch --... ...

mesh., form.- .-... '.;...-:. ;.

. .*M l. * ;~. . r,.1 c

2.'.../ : ',,,.. ~ .. ' 3%.1, 2Mc.NaCf- ' dissolve 116.9 grams NACL ir.1 *er-1waher - m r.. < . t ,.

. . . w ; e . ,. -

4 . MaOC1',.. 5 -6%. :(. commercial strength.1. .

. .~.~.2 .

'4 .

... .~ . [ .l m . , y ._

-. ^ ? ': .

. . 5 .~::.H N O 3 r.. c o n c..e n t r a t e d .:.

.~ '.~a' F ~ ~ '. .

'r, ..

6.- Hydroxylamine hydrochloride, crystals - ..,;. ' ~ .

~

7.. CCl 4 >

.f 8...;1M NaHSO 3 - dissolve 1.041 grams of r m O3.i* ~

'10 ml water (prepare daily)

9. ECl, concentrate <c .

10. Palladous chloride, s10 mg/ml - dissolva 2.00 gra=s of

' 1 PdCl 2 .2HC0 in 100 ml of water I

11. Reagent grades formaldehyde C37%I

?

2 ..

y :4 -

-Samolm Prcotrrtion # -

~

. ~.-

l .. Add 80 mis of formaldehyde containing 2 ml of iodine

._ .e .

carrier (10 mg I /ml) and few drops of freshly prepared

, sodium bisulfite to four liters mb.k. sample at time of

~

collection to prevent spoilage. ,

d.alytical Procedure

1. Pour a 4-liter milk sample into a 4-liter beaker and add E.

a 50-ml: water slurry of anion. resin (Dower 1. x 8[ 50-100

~. '

mesh,..ClI form) to milk. Place.a large (6 cm long)

T.';. -

. m./ : :

Q.5.~; -magnetic

. f'.3';;. y. --.- . Jes.

stirring bar in beaker.and stir vigorously-

~ ' ~ - c. . . . r ..

. T93..a . . .

" ; yi. !for. 20:. minutes . . '(Note 1) ..2."I.5 I '.c.

. .:,7:. .. :- :

c.>r: -:[ec $.'l..;...-

q.c..;, m ~ q. , . s g < _. ., .

_ .; v.:

. ... c: 7 y y .. m .-- . - -

'.E 7 j,. . 2'.a Remove the. stirring bar and allow.the resin to' __c

, settle to

-~ L r

^

, .:... _'.:. :: . .. _ ;^. . . - .

.5:. '

~

ithe- bottom of the beaker for. 20 minutes Caref"17- decan

..)4.(.:::,. . ' : .- . . :.-. o . a..;. 2...e.:"

' tlie milk into .a 'second 4-liter beaker leaving the ion'

- :: . 7-

.,... .,s. .; .

~ _

a exchange resin behind.. Wash.:the resin with distilled

'. .$. f . ., -

r; -. . ,

E

if water inEo . > -

600 ml beab r and save. CF.! ,

. r_, -

. . v. . . .

.].^'.:

.'...'~

r

3. t Place- .

the-magnetic . stirring bar in the second 4-liter -,_.

' beakc.,: add 'a- second 50 ml water slurry of anion. resin

, . to the milk and stir vigorously for 20 minutes.

4. F.emove stirring bar and allow resin to settle to bottom of beaker for 20 minutes. Carefully decant the' milk.and ~

discard. Wash.this resin into the 600 mL beaker con-taining the resin from step 2. Alloir it to se'ttle and decant water to t.raste.

.- 3 e-- -- - , - ,- -- - -- - , - , , , - . -

' ~ .

.'. 5. To this.combincd rc=in add 300 ml of he . water,.Qthout

.. . p 'r

~

80-91 C) .etir briefly, then albk resid to c==pletalf

. =

settle.' Discard the hoti water. Repeat t" ~s hot ' water wash thres times.

r ..

6. Add 100 ml of 5-6% NaOC1 to the resin, placa a s all.

(.2.2 cm long) magnetic stirring bar i . t~.a. hea%er and stir vigorously for 5 minutes,on a =agna" .

stirrer..

7. Filter the resin slurry through a suctic: "fi tar and retain the NaOCl solution. (Note 2) I -

. W. e 8..

Reextract the-resin by repeating steps. 6 and. 7J.l[7.l. . .

.y

.q- . . . .j f

... - . . .n :;- . . f.. . .

94.2 Discard.. the. resi.n, . ccmbine the two 1G0 =1 sol"' wns-m.

.s-. .

. .: ~ .

?;!.,:. of NaOCL.and;.. carefully- add -40 mL of conc .

j

-2. -

, n.:p.

. :. .- w..

2 :.. ..

EIO3.' . .s. .. -.

Note. 3i

, . r. .- y. :3= ~ - f -. :- =. .

g .. ...;.. .~. _

. . . m.:4; -

.'100.!; :s.v.

Pour:.. the, acidified NaOCl solution into a 50CL mL separated

. : e . . , m+ . .-

f. . .r w . ..:Y? funnel;.and add'100 ' ml of CC1, .

. e. ._.

1

.:.y . .,. .,:. *

.~.

3.- - - - . > . ~: - .- -

s a := ..-- - =:u- .

x-

>~ .

11. Add 2 grams ~ of h.ydroxylamine hydrochicrida and ehd =

.n

. J.

. (Nota.4F ~ Extract.

the iodine into tha cr:: nM< - nBaen

- (about . 2. min.. equilibration). . ~. Mota 5}

~

12

' Drain. lower organic phase iniio clean. 501 =L sepa_7 torr

', funnel and.save. .-

13. Add 100 ml CCl 4 ad 1 g= hydrarzia.i.; grc:' .crida .

to the aquaous phasa in tha first sapirat:ri- 4 ---=1 t

and reextract. Combine organic phases a i discard .

aqueous phase.

e

. 4

ACG' DU mL'cnc.2H O Cnc 10 drop:3 Ot trGdtly pr6 pared 1. M

.. 14.

+ *-

to O 'ecoaratorv funnel containg the combined'CCI L an

. 1

.- e w.. .

. - .- , shake. Equilibrate for 2 minutes.. Discard organic (lo l l

. phase' (No'te S.. - s -

l

15. Proceed to mounting procedure. -

\

L'.ounting Procedure .

1. Transfer the, aqueous (upper phase into a clean 100 ml beaker and add 1 ml of. conc. hcl and 10 ml of PdCl 2 - .

i

' . ~ .. ,

.n solution. Stir and. let stand. for- 5 minutes -

~

-.. . .y,; -.- ; - - - . " :

,- c z .l ' : ' . ..

. .:. . /.2L; .Using ?a filter:. funnel setup. similar to that .CTaflon or -

. . ;. g . 1.en .*. - 'yj..

-d':ry!. polyethylene .. ;.. q, . ,. . -

'J-C.

' nylon) described in HASL' 300,;."Procedura .

.:,e.-

7.'l:. ..:s $d.r.. ._-.-

s-

,n ,

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

a.

.. gi'5. Manuara" USAEC'i..: filter with; suction -through, a. tared..

'J .

-: .1 .- ..;q.t ., vi :n . ; . . . :- -

-, f .'J . . . , , ..;..dy glass . fiber paperi(2.4 cm diamater),: us'ing a water wash.

r.

.:. . . .g.,

":. .: - ...', 'ye - n~ * .

- s

[?]W.Q'f.

/

.h . . . M.J. ,: ,..u. . .m

' . O:. - .- .. .. b'ottla .to effeet .a the transfer.

'"?;C-:':-

-:.i .

'_. ;Q

.- n ~

m- . :*

.-- . : ,.: .~.- # W :.! ' .

...._.7.. ..

-!,.L.. Dry the'. precipitate for 20cminutes. in an oven. set at_ _

o

.~.I.. '?

110*C'.and.. weigh.to th's nearest 0. 1 milligram.- '(Alternat.i

" '- ' 6','

the sample may be dried on 'a ' hot plate at low heat .for

.% :. . . . , .a about.30 minutes.1

'. 4.

. Mount the precipitate on a nylon disc,. cover-with Mylar - ~

(1/4 mil thick), and fasten with. ring. (This procedure

^

is describad in HASL 300.) (Note 7) -

5. Count in a low-background counter for 1000 minutes.-

6. If net counting rate of sample is greater tha$t 0.3 cpm (indicating the presence of radiciodine) , recount after 7-8' days to confirm the presence of 13 I by its decay raC-5'

-. .ub .m a We op .-g.

4. . g m e a6, . .*6..6-. . . . - .e NmM mqg _ gg. "' g.O- d

.-..W.. .

--. Calculhto 'es picoeurios I-131 per liter of = ilk. at t' a time ( ,f campling.

U -

. . ~

. . . . r ;-

.t notes *

.~

.- 1. Resin should b's treated to remove any fines. This is acconplished by washing t}ith. water and allos-ing to settle for 5 minutes before decanting sa er.to dr=#-'.

Repeat until any fines are removed. .

2. Resin should be very ligh.t strait color after Nacci

- extraction; if not lighi.' colored, tha NaCC1.is balcr strength, and a fresh. solution should be obtM :.ed.

- ~

. .7. , ' Commercial.

3*

grade clorox has been fo". " to ba.~.ade.ciate.

1

% . .< ;)" ;,.*. ,g .e,- - . .

_ , . ,, . .;. 4- . ,. m. . . ~ .

,- . .3..... Add. tha acid slaulf with. stirring un' # 7 tha. vigorous.

.. ;y_;,:.;... -i .; , - - 2: . _- :. .k::th; .. ,,.y -

^~,,:.. .

,..;g. . . n' .. reaction....:.' subsides... Perform in well vacF#1atecl.

,p.; . :

,.4 hocd._

,, y

. . > ,. s - .. .

Proceed!.with. caution in thisIstep... Excessive. gas p.,,,._._._.......'4...:

..'.JJz .j.' . ........ .. . , . , .

~~' formation during the extraction can. caus .

.a +'-=- stopcock.

..y . . . - .. . - ,

or cap,on..the . ;. -

separatory funnel to " pop" with.conseq~

.a . . . :,.. . .

,- - quent:.. loss of sample.. Start by gentir s.:irlinch -the. .

~

s u,..., . ;.

. solution.to effect mixing. . Invert +'-= saparatorr '.fn-- = T-

, with.the stopcock. pointing up.and releasa the pressure by opening the stopcock.. Close tha stop:: '$, c'-=~m, and repeat the pressure release sequence.

5. Organic phase should be deep red'; id not, allo : sangla.

. to set for few minutes and shake acain. Raceat h*- =

waiting period if necessary.

l l

1 O

6 9 +e.4 .- ee .O .n e.* .N e-.s.. =>e* . * -

em. e . emu.*e e - se, e-ee ee .e - g , e.um 1

-- .- - - , , . . ~ .,,, . , ,_, , % ,.-,,-.-.,-,,f._, , , _ _ , . , . ,,,,%av-,.._.,--r,y-- ,.,+--,,w,,

.----w,

.. / - ,. s/ . ... .. - . ... . .

. 6. 'Afto7 back.cxtraction into vat. \ cc14 chould be color-(.

les,s; if not add additicinal-NaiISO 3 and. reextract..

7. HASL,300." Procedure Manual" Health and Safety Laboratory, U.S. Atomic Energy Commission, 376 Hudson.St., New York,.

New York 10014. .

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ML19317H171

Text

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