ASTM D5811-08(2013)
(Test Method)Standard Test Method for Strontium-90 in Water
Standard Test Method for Strontium-90 in Water
SIGNIFICANCE AND USE
5.1 This test method was developed to measure the concentration of 90Sr in non-process water samples. This test method may be used to determine the concentration of 90Sr in environmental samples.
SCOPE
1.1 This test method covers the determination of radioactive 90Sr in environmental water samples (for example, non-process and effluent waters) in the range of 0.037 Bq/L (1.0 pCi/L) or greater.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 This test method has been used successfully with tap water. It is the user's responsibility to ensure the validity of this test method for samples larger than 1 L and for waters of untested matrices.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 9.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5811 − 08 (Reapproved 2013)
Standard Test Method for
Strontium-90 in Water
This standard is issued under the fixed designation D5811; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D7282Practice for Set-up, Calibration, and Quality Control
of Instruments Used for Radioactivity Measurements
1.1 This test method covers the determination of radioac-
tive Sr in environmental water samples (for example, non-
3. Terminology
process and effluent waters) in the range of 0.037 Bq/L (1.0
3.1 Definitions—For definitions of terms used in this test
pCi/L) or greater.
method, refer to Terminology D1129.
1.2 The values stated in SI units are to be regarded as the
4. Summary of Test Method
standard. The values given in parentheses are for information
only.
4.1 This test method is based on the utilization of solid
phase extraction of strontium from water samples with detec-
1.3 This test method has been used successfully with tap
water.Itistheuser’sresponsibilitytoensurethevalidityofthis tionoftheradioactivestrontiumbygrossbetagasproportional
counting.
test method for samples larger than 1 L and for waters of
untested matrices.
4.2 An aliquant of the sample is measured into a beaker,
1.4 This standard does not purport to address all of the strontiumcarrieradded,digestedwithnitricacid,sorbedonan
safety concerns, if any, associated with its use. It is the ion exchange column, eluted, evaporated to dryness, dissolved
responsibility of the user of this standard to establish appro- in nitric acid (8M), selectively sorbed on a solid phase
priate safety and health practices and determine the applica- extraction column, eluted with dilute nitric acid, dried on a
bility of regulatory limitations prior to use.Forspecifichazard planchet, and counted for beta radiation.
statements, see Section 9.
4.3 Fig. 1 shows a flow diagram for this test method.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:
5.1 This test method was developed to measure the concen-
D1129Terminology Relating to Water
tration of Sr in non-process water samples. This test method
D1193Specification for Reagent Water
maybeusedtodeterminetheconcentrationof Srinenviron-
D1890Test Method for Beta Particle Radioactivity ofWater
mental samples.
D2777Practice for Determination of Precision and Bias of
6. Interferences
Applicable Test Methods of Committee D19 on Water
D3370Practices for Sampling Water from Closed Conduits
6.1 Significant amounts of stable strontium present in the
D3648Practices for the Measurement of Radioactivity
sample will interfere with the yield determination. If it is
D4448GuideforSamplingGround-WaterMonitoringWells
known or suspected that natural strontium is present in the
D5847Practice for Writing Quality Control Specifications
sample at levels that will compromise the determination of the
for Standard Test Methods for Water Analysis
chemical yield, blank sample aliquots to which no strontium
D6001Guide for Direct-Push Groundwater Sampling for
carrier is added shall be analyzed to determine the natural
Environmental Site Characterization
strontium content. The amount of natural strontium contained
in the sample shall be reflected when calculating the yield
correction factor.
This test method is under the jurisdiction ofASTM Committee D19 on Water
6.2 Strontium-89 present in the sample will cause a high
andisthedirectresponsibilityofSubcommitteeD19.04onMethodsofRadiochemi-
89 90
cal Analysis.
bias in proportion to the Sr/ Sr ratio. This technique is not
Current edition approved June 15, 2013. Published July 2013. Originally 89
applicablewhenitissuspectedorknownthat Srispresentin
approved in 1995. Last previous edition approved in 2008 as D5811–08. DOI:
the sample.
10.1520/D5811-08R13.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.3 Strontium nitrate (Sr(NO ) ) is hygroscopic. This
3 2
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
chemicalpropertymayadduncertaintyinthegravimetricyield
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. determination.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5811 − 08 (2013)
FIG. 1 Flow Diagram for the Procedure
7. Apparatus 7.4 Planchets, stainless steel to match calibration source.
7.1 Analytical Balance, 0.0001 g.
8. Reagents and Materials
7.2 Low Background Gas Proportional Beta Counting Sys-
8.1 Purity of Reagents—Reagent grade chemicals shall be
tem.
used in all tests. Unless otherwise indicated, it is intended that
7.3 Ion Exchange Columns, 10 mL resin capacity, glass or
acid-resistantplastic.Anattachedreservoirofatleast50mLis 3
Stainless steel planchets available commercially have been found satisfactory.
desirable.
D5811 − 08 (2013)
all reagents shall conform to specifications of the Committee 9.2 When diluting concentrated acids, always use safety
on Analytical Reagents of the American Chemical Society. glasses and protective clothing, and add the acid to the water.
Other grades may be used, provided it is first ascertained that
10. Sampling
the reagent is of sufficiently high purity to permit its use
without lessening the accuracy of the determination. Reagent
10.1 Collect a sample in accordance with Practice D3370,
blanks shall be run with all determinations.
D4448, D6001, or other documented procedure.
8.2 Purity of Water—Unless otherwise indicated, reference
11. Calibration
towatershallbeunderstoodtomeanreagentwaterconforming
to Specification D1193, Type III.
11.1 Calibrate the low background gas proportional beta
counting system in accordance with Practice D7282. Prepare a
8.3 Cation Exchange Resin, 100 to 200 mesh, hydrogen
set of three calibration samples according to the calibration
form. 8% cross linked, analytical grade.
procedure outlined in the subsequent steps.
8.4 Nitric Acid (8M HNO )—Add 500 mL of concentrated
11.2 Pipet 0.5 mL of strontium carrier into a small beaker.
HNO to 400 mL of water. Dilute to 1L with water.
11.3 Add 1 mL of traceable Sr solution and evaporate to
8.5 Nitric Acid (0.1 HNO )—Add 6.4 mL of concentrated
near dryness on a hot plate.
HNO to 600 mL of water. Dilute to 1L with water.
11.4 Redissolve the residual in 5 mL of 8M nitric acid.
8.6 Nitric Acid (0.05M HNO )—Add 3.2 mL of concen-
trated HNO to 600 mL of water. Dilute to 1L with water.
11.5 Follow the steps described in 12.10 through 12.23.
8.7 Strontium Carrier (10 g/L)—Preferably use 10000
11.6 Count to accumulate 10 000 net counts in the counting
µg/mL ICP standard.Alternatively, dissolve 24.16 g strontium
period. Counting should be completed within3hof column
nitrate(Sr(NO ) )inwater,add20mLconcentratednitricacid,
elution. Record the time and date of the midpoint of this
3 2
and dilute with water to 1 L. Use the following procedure to
countingperiodast .Counteachsamplemounttwice,oncefor
standardize the prepared strontium carrier: Carefully pipet a
this step having a counting date designated as t and a second
5.0 mL portion of the strontium carrier solution onto a clean,
time as specified below.
dried, and tared planchet. Dry the planchet under the same
11.7 Calculate the net count rate of the count at time t
conditions used for the final evaporation in 12.20. Allow the
(R ) by subtracting the instrument background count rate
n(2)
planchettocooltoroomtemperatureandreweightheplanchet
from the gross count rate.
tothenearest0.0001g.Dividethenetweightby10.Thisresult
11.8 Store the calibration mount for at least 7 days to allow
is the amount of strontium nitrate actually added. Use an
for Y ingrowth.
average of three values in the denominator of the recovery
equationin11.12and13.1.Thisvalueshouldbewithin3%of
11.9 Recount the calibration mount to amass 10 000 counts
12.08 mg/0.5 mL.
in a counting period. Record the time and date of the midpoint
of this count period as t .
8.8 Strontium Extraction Chromatography Column,2mL 3
bed volume consisting of an octanol solution of 4,4’(5’)-bis
11.10 Calculate the net count rate of the second count at
(t-butyl-cyclohexano)-18-crown-6-sorbed on an inert poly-
time t (R ) by subtracting the instrument background count
3 n(3)
meric support.
rate from the gross count rate.
8.9 Strontium-90 Standardizing Solution—Traceable to a
11.11 Calculate the Sr detection efficiency, ε , and
Sr
national standard body such as National Institute of Standards
the Y detection efficiency, ε , for each calibration mount
Y
andTechnology or National Physical Laboratory solution with
using the equations presented below. Calculate the mean and
less than 0.1 mg of stable strontium per mL of final solution
standard deviation of the three ε and ε values. Use the
Sr Y
with a typical concentration range from 85 to 125 Bq/mL.
relative standard deviation of these parameters to estimate the
relative uncertainty of the ingrowth efficiency factor, (defined
9. Hazards
in Eq 5), u(ε) and used in Eq 7.
r I
9.1 Use extreme caution when handling all acids. They are
11.12 Effıciency Calculations— Sr detection efficiency ε :
Sr
extremely corrosive and skin contact could result in severe
R 3IF 2 R 3IF
~ n 2 3! ~ n 3 2!
~ ! ~ !
burns.
ε 5 (1)
Sr
Y 3A 3 ~IF 2 IF !
Sr C~2! 3 2
Y detection efficiency ε :
Y
Reagent Chemicals, American Chemical Society Specifications, American
R 2 R
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not n 3 n 2
~ ! ~ !
ε 5 (2)
Y
listed by the American Chemical Society, see Annual Standards for Laboratory
Y 3A 3 ~IF 2 IF !
Sr C~2! 3 2
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
where:
MD.
5 A = activity of Sr in becquerels (Bq) at the time of the
Thesolesourceofsupplyoftheapparatusknowntothecommitteeatthistime C(2)
isSrResinavailablefromEichromTechnologies,Inc.Ifyouareawareofalternative first count of the calibration mount,
suppliers, please provide this information to ASTM International Headquarters.
IF = ingrowth factor for Y at the midpoint of the count
Your comments will receive careful consideration at a meeting of the responsible
2@λ 3~t 2t !#
Y 2 1
at time t , e
1 2
technical committee, which you may attend.
D5811 − 08 (2013)
12.17 Clean a planchet with a paper towel moistened with
IF = ingrowth factor for Y at the midpoint of the count
2@λ 3~t 2t !#
Y 3 1 alcohol. Wipe the planchet and let it dry.
at time t , e
90 –1
λ = decay constant for Y (0.2600 d ),
Y 12.18 Weightheplanchettothenearest0.0001gandrecord
R = net count rate of the calibration test source at the
n(2)
the weight.
midpoint of the first count, in counts per second,
12.19 Place the planchet under a heat lamp in a fume hood.
R = net count rate of calibration test source at the
n(3)
midpoint of the second count, in counts per second,
12.20 Evaporate the strontium eluate (see 12.16) onto the
t = date and time of Y separation,
planchetbyaddingsmallportions(approximately3mL)tothe
t = date and time of midpoint of first count,
2 planchet and allowing each portion to evaporate to near
t = date and time of midpoint of second count.
dryness between additions.
Y = fractionalchemicalyieldofstrontiumcarrier(seeEq
Sr
12.21 Rinse the liquid scintillation counting vial or centri-
4).
fugetubewithapproximately3mLof0.05MHNO ,addtothe
NOTE 1—The time differences (t − t ) and (t − t ) are expressed in
2 1 3 1
planchet and evaporate.
days.
12.22 After all the solution has dried, cool the planchet to
12. Procedure
roomtemperatureandreweightheplanchet.Recordtheweight
to the nearest 0.0001 g.
12.1 Add 0.5 mLof strontium carrier to a maximum of 1 L
of sample.Add 1 mLof 8M HNO per 100 mLof sample and
3 12.23 Beta count the sample as soon as possible after
mix. Bring sample to a boil for 30 min and then cool.
preparation on a low background gas proportional counting
system.Countanemptyplanchetforanequallengthoftimeto
12.2 Prepareacationexchangecolumncontaining10mLof
measuretheinstrument’sbetabackgroundcountrate.(SeeTest
cation exchange resin.
Method D1890 and Practices D3648.)
12.3 Precondition the column by passing 50 to 55 mL of
0.1M HNO through the column.
13. Calculation
12.4 Pass the sample through the column at a rate of not
13.1 Strontium-90 Radioactivity Concentration (AC ):
Sr
more than 5 mL/min.
R 2 R
a b
AC 5 (3)
12.5 Rinse the column with 25 to 30 mL of 0.1M HNO . Sr 2@λ 3~t 2t !#
Sr 1 0
ε 3V 3Y 3e
I a Sr
12.6 Properly dispose of the feed and rinse.
m 2 m
a b
Y 5 (4)
Sr
m
c
12.7 Elute the strontium (and other cations) with 50 mL of
2@λ 3~t 2t !#
Y m 1
8M HNO into a 150 mL beaker.
ε 5 ε 1~ε 3 ~1 2 e !! (5)
3 I Sr Y
12.8 Evaporatetheeluatetoneardrynessonahotplateina
where:
fume hood. The residue will dissolve more easily in the next
ε = the mean of the values calculated using Eq 1,
Sr
stepiftheevaporationisstoppedjustasthesamplestartstogo
ε = the mean of the values calculated using Eq 2,
Y
dry.
ε = ingrowth efficiency factor,
I
90 –5 –1 6
λ = decay constant for Sr (6.594 × 10 d ),
Sr
12.9 Dissolve the salts in 5 mL of 8M HNO . If necessary,
90 –1
λ = decay constant for Y (0.2595 d ),
Y
cover with a watchglass and heat gently to facilitate complete
R = count rate of sample aliquant, in counts per second,
a
dissolution.
R = count rate of instrument background, in counts per
b
12.10 Prepare a strontium extraction chromatography col-
second,
umn by removing the bottom plug and the cap. Press the top
t = date and time of sample collection,
t = date and time of Y separation,
frit down snugly to the resin surface using a glass rod (or
t = midpoint of count of sample aliquant (date and time),
equivalent) and let the water drain out. Add 5 mL of
m
V = volume of sample aliquant, in litres,
HNO (8M) and let the solution drain by gravity. a
Y = fractional chemical yield of strontium carrier,
Sr
12.11 Carefully transfer the sample solution to the reservoir
m = mass of Sr(NO ) for the sample aliquant,
a 3 2
ofthecolumn.Addhalfandletthesolutiondrainbeforeadding
m = mass of Sr(NO ) for the blank (where appropriate—
b 3 2
the second half.
see Step 6.1), and
m = mass of Sr(NO ) added as carrier.
12.12 Rinse the beaker with 3 mLof 8M HNO and add to c 3 2
NOTE 2—The time differences (t –t ) and (t –t ) are expressed in
1 0 m 1
the column after the feed h
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