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7500-I A. Introduction
Radioiodine that results from testing nuclear devices or is Of the three methods, the precipitation method (B) is preferred
released during use and processing of reactor fuels is a major because it is simple and involves the least time. Method C, in which
concern in radioactivity monitoring. Fission products may con- iodide is concentrated by absorption on an anion resin, purified, and
tain iodine-129 through iodine-135. Iodine-129 has a half-life of counted in a beta-gamma coincidence system, is sensitive and
1.6 ⫻ 107 years but a relatively low specific activity (1.73 ⫻ accurate. Method D uses distillation. With each method it is possi-
10⫺4 Ci/g for 129I as compared to 1.24 ⫻ 105 Ci/g for 131I). The ble to reach the EPA recommended detection limit of 1 pCi 131I/L.
half-life of 131I is 8 d while for the other isotopes it is shorter
3. Bibliography
(35 min to 21 h). At present, only 131I is likely to be found in
water. When ingested or inhaled, it concentrates in the thyroid KLEINBERG, J. & G.A. COWAN. 1960. The Radiochemistry of Fluorine,
gland and may cause thyroid cancer. Chlorine, Bromine and Iodine. Rep. NAS-NS-3005, U.S. Atomic
Energy Comm.
BRAUER, F.P., J.H. KAYE & R.E. CONNALY. 1970. X-ray and -␥.
Coincidence Spectrometry Applied to Radiochemical Analysis
of Environmental Samples. Advances in Chemistry Ser., No. 93,
Radionuclides in the Environment, pp. 231–253. American
* Approved by Standard Methods Committee, 2000. Editorial revisions, 2011. Chemical Soc.
1. General Discussion d. Iodate carrier: Dissolve 1.685 g KIO3 in distilled water and
dilute to 100 mL. Store in dark flask; 1 mL ⫽ 10 mg I.
a. Principle: Iodate carrier is added to an acidified sample and, e. Nitric acid, HNO3, conc.
after reduction with Na2SO3 to iodide, the 131I is precipitated f. Palladium chloride, PdCl2: Dissolve 3.3 g PdCl2 in 100 mL
with AgNO3. The precipitate is dissolved and purified with zinc 6N HCl; 1 mL ⫽ 20 mg Pd.
powder and H2SO4 and the solution is reprecipitated as PdI2 for g. Silver nitrate, AgNO3, 0.1M: Dissolve 17 g AgNO3 in
counting. distilled water and dilute to 1000 mL. Store in dark flask.
b. Quality control (QC): The QC practices considered to be an h. Sodium sulfite, Na2SO3, 1M (freshly prepared): Dissolve
integral part of each method can be found in Section 7020. 6.3 g Na2SO3 in distilled water and dilute to 50 mL.
i. Sulfuric acid, H2SO4, 2N.
2. Apparatus j. Zinc, powder, reagent grade.
4. Procedure
a. Counting instrument: Low-background beta counter (see
Section 7030B.1) or gamma spectrometer (Section 7030B.5).
b. Fine-fritted glass funnel. a. To a 2000-mL sample, add 15 mL conc HNO3 and 1.0 mL
c. Filter apparatus: Two-piece filter funnel with filtering iodate carrier. Mix well. Add 4 mL freshly prepared 1M Na2SO3
equipment.* and stir for 30 min. Add 20 mL 0.1M AgNO3, stir for 1 h, and
d. Filter materials: Filter paper;† glass-fiber filter, 2.4 cm let settle for 1 h. Decant and discard as much of the supernatant
diam; or 0.8-m pore-diam membrane filter, 4.7 cm diam. as possible. Filter remainder through a glass-fiber filter and
discard filtrate.
3. Reagents b. Transfer filter to a centrifuge tube and slurry with 10 mL
distilled water. Add 1 g zinc powder and 2 mL 2N H2SO4 and stir
a. Ammonium hydroxide, NH4OH, 6N. frequently for at least 30 min. Filter, with vacuum, through a
b. Ethanol, 95%. fine-fritted glass funnel and collect filtrate in an erlenmeyer flask.
c. Hydrochloric acid, HCl, 6N. Wash both residue and filter with a minimum quantity of dis-
tilled water and add wash water to filtrate. Discard residue.
c. Add 2 mL 6N HCl and heat in water bath at 80°C for
* Fisher Filtrator or equivalent. 10 min. Add 1 mL 0.2M PdCl2 and digest for at least 5 min.
† Whatman No. 42 or equivalent. Centrifuge and discard supernatant.
1
RADIOACTIVE IODINE (7500-I)/Ion-Exchange Method
2
RADIOACTIVE IODINE (7500-I)/Distillation Method
reaction go on for a few seconds, add 10 mL 1M NaHSO3, and organic phase. Transfer aqueous phase to a beaker. Add 10 mL
adjust pH to 6.5 with 12N NaOH or 1.6N HNO3. Stir thoroughly 3N HCl. Using a stirrer-hot plate, boil and stir the sample until
for a few minutes. (Stir samples containing a large amount of it evaporates to 10 to 15 mL or begins to turn yellow.
organic material, such as muddy water, for 45 min.) Filter f. Add 1.0 mL PdCl2 solution dropwise. Rinse sides of beaker
through a glass-fiber filter to remove suspended matter. Discard with 1N HCl and add sufficient 1N HCl to make a volume of
residue. 30 mL. Continue stirring until cool. Place beaker in a stainless
b. Pour 20 mL anion-exchange resin into a column and wash steel tray and store at about 4°C overnight.
sides down with distilled water. Pass sample through ion- g. Filter through a tared filter mounted in a filter holder. Wash
exchange column at a flow rate of 20 mL/min. Discard effluent. residue with 1N HCl and then with absolute alcohol. Dry in a
Wash column with 200 mL distilled water and then with 100 mL vacuum oven at 60°C for 1 h. Cool in a desiccator, weigh
2M NaCl at a flow rate of 4 mL/min. Discard wash solutions. precipitate, then seal it between polyester tape and polyester
c. Add 50 mL 5% NaOCl in 10- to 20-mL increments, stirring plastic film,‡ with the film over the precipitate. Count with a
the resin as needed to eliminate gas bubbles, and maintain a flow beta-gamma coincidence system.
rate of 2 mL/min. To the eluted volume of 50 to 60 mL, collected
in a beaker, carefully add 10 mL conc HNO3 to make sample 2 5. Calculation
to 3N in HNO3 and transfer to a separatory funnel. (Add acid
slowly with stirring until vigorous reaction subsides.) Calculate 131
I, pCi/L, as in 7500-I.B.5.
d. Add 50 mL CCl4 and 10 mL 1M NH2OH 䡠 HCl. Extract
iodine into organic phase by shaking for about 2 min. Let phases 6. Bibliography
separate and transfer organic phase to another separatory funnel.
Add 25 mL CCl4 and 5 mL 1M NH2OH 䡠 HCl to the first AMERICAN SOCIETY FOR TESTING AND MATERIALS. 1972 Book of ASTM
separatory funnel and shake for 2 min. Combine organic phase Standards. Part 23. D 2334-68, American Soc. Testing & Materials,
with the one obtained from the first extraction. Discard aqueous Philadelphia, Pa.
phase. Add 20 mL NH2OH 䡠 HCl wash solution to the organic GABAY, J.J., C.J. PAPERIELLO, S. GOODYEAR, J.C. DALY & J.M. MATUSZEK.
phase and shake for 2 min. Let phases separate and transfer 1974. A method of determining 129I in milk and water. Health Phys.
organic phase to a clean separatory funnel. Discard wash solu- 26:89.
tion.
e. Add 25 mL distilled water and 10 drops 1M NaHSO3 to
organic phase. Shake for 2 min, let phases separate, and discard ‡ Mylar, or equivalent.
3. Reagents
4. Procedure
a. Ammonium hydroxide, NH4OH, conc.
b. Carbon tetrachloride, CCl4. a. To a 2000-mL sample in a 3-L round-bottom flask, add
15 mL 50% C4H6O6 and 1.0 mL iodide carrier. Mix well,
cautiously add 25 mL cold conc HNO3, and close distillation
* Fisher Filtrator, or equivalent. apparatus (Figure 7500-I:1).
3
RADIOACTIVE IODINE (7500-I)/Distillation Method