Beruflich Dokumente
Kultur Dokumente
1. Scope only in this range (see 4.3). Use outside this range requires determination
of the temperature dependence.
1.1 This practice covers the procedures for preparation,
1.4 This standard does not purport to address all of the
testing, and using the ceric-cerous sulfate dosimetry system to
safety concerns, if any, associated with its use. It is the
determine absorbed dose (in terms of absorbed dose to water)
responsibility of the user of this standard to establish appro-
in materials irradiated by photons (gamma radiation or
priate safety and health practices and determine the applica-
X-radiation/bremsstrahlung) or high-energy electrons. The sys-
bility of regulatory limitations prior to use.
tem consists of a dosimeter and appropriate analytical instru-
mentation. For simplicity, the system will be referred to as the 2. Referenced documents
ceric-cerous system. It is classified as a reference–standard
dosimetry system (see ISO/ASTM Guide 51261). Ceric-cerous 2.1 ASTM Standards:3
dosimeters are also used as transfer–standard dosimeters or C912 Practice for Designing a Process for Cleaning Techni-
routine dosimeters. cal Glasses
E170 Terminology Relating to Radiation Measurements and
1.2 This practice describes both the spectrophotometric and Dosimetry
the potentiometric readout procedures for the ceric-cerous E178 Practice for Dealing With Outlying Observations
system. E275 Practice for Describing and Measuring Performance of
1.3 This practice applies provided the following conditions Ultraviolet and Visible Spectrophotometers
are satisfied:. E666 Practice for Calculating Absorbed Dose From Gamma
1.3.1 The absorbed-dose range is between 0.5 and 50 kGy or X Radiation
(1).2 E668 Practice for Application of Thermoluminescence-
1.3.2 The absorbed-dose rate is less than 106 Gy s−1 (1). Dosimetry (TLD) Systems for Determining Absorbed
1.3.3 For radionuclide gamma-ray sources, the initial pho- Dose in Radiation-Hardness Testing of Electronic Devices
ton energy is greater than 0.6 MeV. For bremsstrahlung E925 Practice for Monitoring the Calibration of Ultraviolet-
photons, the energy of the electrons used to produce the Visible Spectrophotometers whose Spectral Bandwidth
bremsstrahlung photons is equal to or greater than 2 MeV. For does not Exceed 2 nm
electron beams, the initial electron energy is greater than 8 E958 Practice for Estimation of the Spectral Bandwidth of
MeV. Ultraviolet-Visible Spectrophotometers
2.2 ISO/ASTM Standards:3
NOTE 1—The lower energy limits are appropriate for a cylindrical
dosimeter ampoule of 12-mm diameter. Corrections for dose gradients 51261 Guide for Selection and Calibration of Dosimetry
across an ampoule of that diameter or less are not required for photons, but Systems for Radiation Processing
may be required for electron beams (2). The ceric-cerous system may be 51400 Practice for Characterization and Performance of a
used at lower energies by employing thinner (in the beam direction) High-Dose Radiation Dosimetry Calibration Laboratory
dosimeters.
51707 Guide for Estimating Uncertainties in Dosimetry for
1.3.4 The irradiation temperature of the dosimeter is above Radiation Processing
0°C and below 62°C (3). 2.3 International Commission on Radiation Units and Mea-
NOTE 2—The temperature dependence of dosimeter response is known surements (ICRU) Reports:4
ICRU Report 14 Radiation Dosimetry: X-Rays and Gamma
1
This guide is under the jurisdiction of ASTM Committee E61 on Radiation Rays with Maximum Photon Energies Between 0.6 and 60
Processing and is the direct responsibility of Subcommittee E61.02 on Dosimetry MeV
Systems, and is also under the jurisdiction of ISO/TC 85/WG 3.
Current edition approved June 18, 2008. Published June 2009. Originally
3
published as ASTM E1205–88. Last previous ASTM edition E1205–99. ASTM For referenced ASTM and ISO/ASTM standards, visit the ASTM website,
E1205–93 was adopted by ISO in 1998 with the intermediate designation ISO www.astm.org, or contact ASTM Customer Service at service@astm.org. For
15555:1998(E). The present International Standard ISO/ASTM 51205:2009(E) is a Annual Book of ASTM Standards volume information, refer to the standard’s
major revision of ISO/ASTM 51205-2002(E) which replaced ISO 15555. Document Summary page on the ASTM website.
2 4
The boldface numbers in parentheses refer to the bibliography at the end of this Available from International Commission on Radiation Units and
standard. Measurements, 7910 Woodmont Ave., Suite 800, Bethesda, MD 20814, USA.
1
ISO/ASTM 51205:2009(E)
Procedures for making such calculations are given in ASTM approximately 2 mL. Quick-break glass ampoules, or Type 1 glass
Practices E666 and E668 and ISO/ASTM Guide 51261. colorbreak ampoules or equivalent containers, are commonly used.
Commercially available ampoules have been found to give reproducible
NOTE 4—For a comprehensive discussion of various dosimetry methods results without requiring additional cleaning.
applicable to the radiation types and energies discussed in this practice,
see ICRU Reports 14, 34, 35, and 37. 7. Reagents
5. Interferences 7.1 Analytical reagent grade chemicals shall be used for
preparing all solutions.5
5.1 The ceric-cerous dosimetric solution response is sensi-
tive to impurities, particularly organic impurities. Even in trace 7.2 Water quality is very important since it is the major
quantities, impurities can cause a detectable change in the component of the dosimetric solutions, and therefore may be
observed response (7). Organic materials shall not be used for the prime source of contamination. The water quality is more
any component in contact with the solution unless they have important for ceric-cerous dosimeters used for measurements
been tested and shown to have no effect. The effect of trace in the lower absorbed-dose range than for those used in the
impurities is minimized by the addition of cerous ions to the upper absorbed-dose range. For high-range dosimeters double-
solution (8, 9). Water purification methods found to be ad- distilled water from coupled all-glass and silica stills can be
equate for use in preparing ceric-cerous dosimeters are de- used. For low-range dosimeters, use triply-distilled water.
cribed in 7.2. Alternatively, use water from a high-quality commercial puri-
fication unit capable of achieving Total Oxidizable Carbon
5.2 Undesirable chemical changes in the dosimetric solution (T.O.C.) content below 5 ppb. Use of deionized water is not
can occur if care is not taken during sealing of the ampoules recommended.
(see 8.7).
NOTE 7—Double-distilled water distilled from an alkaline potassium
6. Apparatus permanganate (KMnO4) solution (2 g KMnO4 plus 5 g sodium hydroxide
(NaOH) pellets in 2 L of distilled water) has been found to be adequate for
6.1 Spectrophotometric Method—For the analysis of the routine preparation of the dosimetric solution. High-purity water is
dosimetric solution, use a high-precision spectrophotometer commercially available from some suppliers. Such water labeled HPLC
capable of measuring absorbance values up to two with an (high-pressure liquid chromatographic) grade is usually sufficiently free
uncertainty of no more than 1 % in the region from 254 to 320 from organics to be used in this practice.
nm. Use quartz cuvettes with 10-mm path length for spectro- 7.3 Do not store purified water used in this practice in
photometric measurements of absorbance of the solution. plastic containers or in containers with plastic caps or plastic
6.2 Potentiometric Method—Use an electrochemical cell, cap liners.
similar to that described in Annex A1 (see Fig. A1.1). Measure 8. Preparation of the dosimeters
the electropotential across the cell with a high-precision digital
potentiometer that is capable of measuring dc potentials in the 8.1 The recommended concentrations for the ceric-cerous
range from 1 to 100 mV within an uncertainty of 1 %. dosimeter to measure absorbed doses from about 5 to 50 kGy
(high-range dosimeter) are 15 mmol dm−3ceric sulfate
NOTE 5—As shown in Fig. A1.1, the electrochemical cell has two [Ce(SO4)2 · 4H2O] and 15 mmol dm−3 cerous sulfate
compartments separated by a porous junction, such as a glass frit, a
ceramic or kaolin junction, or a fibreglass wick. The inner compartment is [Ce2(SO4)3 · 8H2O]. For measurement of absorbed doses from
filled with unirradiated solution. The lower compartment is filled with about 0.5 to 10 kGy (low-range dosimeter), the recommended
solution transferred from an irradiated or unirradiated ampoule. The concentrations are 3 mmol dm−3 [Ce(SO4)2 · 4H2O] and 3
electropotential, E, generated between the platinum electrodes in the two mmol dm−3 [Ce2(SO4)3 · 8H2O].
compartments is measured by a digital potentiometer.
8.2 The dosimetric solutions specified in 8.1 may be formu-
6.3 Glassware—Use borosilicate glass or equivalent chemi-
lated from the following nominal stock solutions: (a) 0.4 mol
cally resistant glass to store the reagents and the prepared
dm−3 and 4 mol dm−3 sulfuric acid (H2SO4), (b) 0.1 mol dm−3
dosimetric solution. Clean all glassware, except ampoules,
Ce(SO4)2 · 4H2O, and (c) 0.1 mol dm−3 Ce2(SO4)3 · 8H2O.
using chromic acid cleaning solution or an equivalent cleaning
Procedures for preparing these solutions are given in Annex
agent (see ASTM Practice C912). Rinse at least three times
A2. (Warning—Concentrated sulfuric acid is corrosive and
with double-distilled water. Dry thoroughly and store under
can cause serious burns. Ceric-cerous solutions are skin irri-
conditions that will minimize exposure to dust.
tants. Appropriate precautions should be exercised in handling
6.4 Glass Ampoules—If required, clean glass ampoules in these materials.)
boiling double-distilled water. Rinse twice with double-
distilled water and oven dry. 5
Reagent specifications are available from American Chemical Society, 1115
NOTE 6—The dosimetric ampoule normally used has a capacity of 16th St., Northwest, Washington, DC 20036, USA.
8.3 Use the following equations to determine the volume in 8.7 Prepare dosimeters by filling ampoules with approxi-
millilitres of each stock solution necessary to prepare 1 L of mately 2 mL of dosimetric solution. Take care not to contami-
dosimetric solution: nate the dosimetric solution with impurities. Exercise care in
High Range Low Range filling ampoules to avoid depositing solution in the ampoule
neck. Subsequent heating during sealing may cause an unde-
V1 0.015 V1 0.003 sirable chemical change in the dosimetric solution remaining
5 5 (4)
1000 c1 1000 c1 inside the ampoule neck. Flame seal the ampoules, exercising
care to avoid heating the body of the ampoule during sealing.
V2 0.015 V2 0.003 8.8 Store dosimeters in a dark place at room temperature (23
5 5 (5) 6 5°C).
1000 c2 1000 c2
Calibration irradiations shall be performed at a national or 10.5.3 When the cell is being used for the first time, the
accredited laboratory using criteria specified in ISO/ASTM filled cell should be left to stand for at least 24 h before making
Practice 51400. any measurements.
10.2.1 Specify the dose in terms of absorbed dose to water. 10.5.4 If the cell is not going to be used for more than three
10.2.2 When the ceric-cerous dosimeter is used as a routine days, drain all solution from the cell. Rinse both the inner and
dosimeter, the calibration irradiation may be performed by outer compartments three times with distilled water, and allow
irradiating the dosimeters at (a) a national or accredited the cell to air dry. Refer to 10.5.1 and 10.5.2 before reusing the
laboratory using criteria specified in ISO/ASTM Practice cell.
51400, (b) an in-house calibration facility that provides an 10.5.5 Drain the inner compartment and refill it with the
absorbed dose (or an absorbed-dose rate) having measurement contents of another unirradiated dosimeter.
traceability to nationally or internationally recognized 10.5.6 Connect the digital potentiometer across the cell. If
standards, or (c) a production irradiator under actual produc- the electropotential, E, is equal to zero (within 60.2 mV), the
tion irradiation conditions, together with reference– or trans- cell is ready for use. Read at least three unirradiated
fer–standard dosimeters that have measurement traceability to dosimeters, and determine average value Ēo.
nationally or internationally recognized standards. 10.5.7 Expel the unirradiated solution from the outer com-
10.3 Measurement Instrument Calibration and Perfor- partment and draw in the solution from each irradiated dosim-
mance Verification—For the calibration of instruments (spec- eter (ampoule) in turn, starting with the lowest and proceeding
trophotometer or multimeter), and for the verification of to the highest absorbed dose. In each case, before measuring
instrument performance between calibrations, see ISO/ASTM the electropotential for any particular dosimeter, rinse the cell
Guide 51261 and/or instrument-specific manuals. by drawing in a little less than half of that dosimeter’s solution
in order to reduce the effects of the previous dosimeter. Expel
10.4 Spectrophotometric Measurement:
the rinse solution into a waste container, and then draw in
10.4.1 For the spectrophotometric measurement, separate at
sufficient solution from that remaining in the dosimeter am-
least five dosimeters from the remainder of the batch and do
poule to fully cover the porous junction.
not irradiate them. Use them in determining Āo.
10.4.2 For spectrophotometric measurement of both unirra- NOTE 13—Inadequate rinsing of the cell between dosimetric solutions
diated and irradiated dosimeters, dilute high-range dosimetric can lead to errors due to solution carryover. If the approximate absorbed
solutions by a factor of 100 and low-range dosimetric solutions doses are known, read the dosimeters that received similar absorbed doses
together to minimize the errors from this effect.
by a factor of 50.
10.4.2.1 Pipette 0.25 mL of high-range dosimetric solution 10.5.8 Read the electropotential, E, in millivolts, across the
or 0.5 mL of low-range dosimetric solution into a clean, dry cell for each dosimeter after temperature equilibrium is estab-
25-mL volumetric flask. lished within the cell. Subtract the average electropotential, Ēo,
10.4.2.2 Rinse the pipette with 0.4 mol dm−3 H2SO4 into the to determine ∆E, the net electropotential value. Measure the
flask and make up to volume with 0.4 mol dm−3 H2SO4. readout temperature near the electrochemical cell, and apply
10.4.2.3 Stopper the 25-mL flask, and mix well. correction for this temperature.
10.4.3 Transfer an appropriate amount into a quartz spec- NOTE 14—The electropotential, E, within the electrochemical cell, has
trophotometric cuvette (sample cell) from the 25-mL volumet- a positive temperature coefficient of 0.33 % per °C between 25 and 30°C
ric flask. (8).
10.4.4 Read the absorbance, A, in the spectrophotometer at 10.6 Analysis:
320 nm. 10.6.1 Obtain a response function for ∆A or ∆E as a
10.4.5 Calculate the mean absorbance of the unirradiated function of the absorbed dose, D. Fit the data by means of a
dosimeters, Āo. Calculate the net absorbance, ∆A, for each least-squares method with an appropriate analytical form that
irradiated dosimeter: provides a best fit to the data. The data for these ceric-cerous
∆A 5 Ā o 2 A (8) dosimeters should fit a third or fourth order polynomial of the
form:
10.5 Potentiometric Measurement:
10.5.1 Place contents of an unirradiated dosimeter (am- v 5 b 0 1b 1 D1b 2 D 2 1b 2 D 3 1b 4 D 4 (9)
poule) into both compartments of the electrochemical cell. See where:
Annex A1 for a description of the electrochemical cell.6 v = ∆A or ∆E,
10.5.2 Allow the solution to remain in the electrochemical b4 = 0 for third order polynomial, b4 ≠ 0 for fourth order
cell for about 30 min in order to establish equilibrium across polynomial.
the porous junction. For a new batch of dosimeters, or if a cell NOTE 15—Computer software is available commercially for performing
has not been used for one or more days, solution should be left least-squares fits of data with polynomials or other analytical forms.
in both compartments for at least 16 h to ensure equilibrium Further information on mathematical methods for handling calibration
across the porous junction. data is given in ISO/ASTM Guide 51707.
10.6.2 The inverse of the response function determined in
10.6.1 will provide the calibration–temperature dose for irra-
6
Electrochemical cells can be obtained from MDS Nordion, 447 March Road, diations performed at the temperature, Tc, used for the calibra-
Ottawa, Ontario, Canada K2K 1X8. tion irradiations.
11 antilog
c4
∆E
59.16
DG (13)
T(°C), for the high range and low range solutions is given by
where:
the following equations:
ρ = density of the dosimetric solution, kg m−3,
where: G(Ce3+) = average value for G(Ce3+) determined from Eq
G ~ Ce31 ! T 5 ~ 2.33544 2 0.0052 3 T ! 3 1.036 3 1027 ~ high range! A3.11,
(10)
∆E = electropotential minus average electropotential
for unirradiated dosimeters, and
G ~ Ce31 ! T 5 ~ 2.42452 2 0.0052 3 T ! 3 1.036 3 1027 ~ low range! c4 andc5 = concentrations of the ceric and cerous ions in the
(11) unirradiated dosimetric solutions, respectively,
mol dm−3.
10.6.4 The absorbed dose is approximately inversely pro-
portional to G ~ Ce31 ! over the absorbed-dose range for the 10.7.3 Determine the relationship for the calculated ab-
solution. For irradiations at an effective irradiation sorbed doses as a function of the absorbed-dose values used for
temperature, Teff, correct the absorbed dose by the ratio the calibration irradiations. The function describing this rela-
G ~ Ce31 ! T /G ~ Ce31 ! T . tionship may be used for the determination of the absorbed
c eff
dose.
10.6.5 For quality control, compare the net absorbances or
net electropotentials determined for a given calibration with the NOTE 16—The calculated absorbed dose values should be close to the
absorbed dose values used for the calibration irradiations, providing a
results obtained from previous batches. Agreement should be good fit to a low order (first to third order) polynomial. If the calculated
within 3 % if the dosimetric solutions were properly prepared absorbed dose values differ by more than the expanded uncertainty with a
and all associated analysis equipment was properly calibrated. coverage factor k=2 from the absorbed-dose values used for the calibration
irradiations, there is an indication of possible contamination of the
10.6.6 Estimate the component of uncertainty that can be solution, or some other problem that needs to be resolved.
evaluated by statistical methods (Type A) of the individual
dosimeter results from the results of replicate measurements at 11. Application of dosimetry system
a given absorbed-dose level. Type A uncertainty provides a
11.1 For use as a transfer-standard dosimeter, use a mini-
measure of acceptable performance of the dosimetry system.
mum of two dosimeters for each absorbed-dose measurement.
For the high-range dosimeter, the Type A uncertainty, ex-
The number of dosimeters required for the measurement of
pressed as one standard deviation, should not exceed 0.005 absorbed dose on or within a material is determined by the
absorbance units for an optical pathlength of 10 mm or 2 % of estimated uncertainty of the dosimetry system and the required
the electropotential value. For the low-range dosimeter, the uncertainty associated with the application. Appendix X3 of
Type A uncertainty should not exceed 0.010 absorbance units ASTM Practice E668 describes a statistical method for deter-
or 2 % of the electropotential value. Suspected data outliers mining this number.
should be tested using statistical procedures, such as those
found in ASTM Practice E178. 11.2 Use the irradiation and measurement procedures in
accordance with Section 10.
10.7 Alternative Method for Determining Absorbed
11.3 Determine the absorbed dose from the net absorbance
Dose—If the procedures for quantifying dosimetric solution
values or net electropotential values and the calibration curve.
parameters given in Annex A3 are carried out, approximate
values for the absorbed dose can be obtained from analytical 11.4 Record the calculated absorbed dose values and all
functions. other relevant data as outlined in Section 12.
10.7.1 For spectrophotometric readings, calculate an ap-
12. Minimum documentation requirements
proximate value for the absorbed dose, Ds, in grays, using the
following equation: 12.1 Calibration of the Dosimetry System:
12.1.1 Record the dosimeter type and batch number (code).
f·∆A
Ds 5 (12) 12.1.2 Record or reference the date, irradiation temperature,
G ~ Ce31 ! ·ε m ·ρ·d
temperature variation (if any), absorbed-dose range, radiation
where: source, and associated instrumentation used to measure the
f = dilution factor for the irradiated dosimeters, dosimeter response.
∆A = change in absorbance of irradiated dosimeter, 12.2 Application:
G(Ce3+) = average value for G(Ce3+) determined from Eq 12.2.1 Record the date and temperature of irradiation, tem-
A3.9, perature variation (if any), and the date and temperature of
εm = molar-linear absorption coefficient (m2 mol−1), absorbance measurement for each dosimeter.
ρ = density of the dosimetric solution, kg m−3, and
12.2.2 Record or reference the radiation source type and
d = path length of spectrophotometer cell, m.
characteristics.
10.7.2 For potentiometric readings, calculate an approxi- 12.2.3 Record the absorbance or electropotential, net absor-
mate value for the absorbed dose, Dp, in grays using the bance or net electropotential value, temperature correction (if
following equation: applicable), and resulting absorbed dose for each dosimeter.
Reference the calibration curve or response function used to k = 2 (which corresponds approximately to a 95 % level of
obtain the absorbed-dose values. confidence for normally distributed data).
12.2.4 Record or reference the components of uncertainty in
NOTE 17—The identification of Type A and Type B uncertainties is
the value of the absorbed dose. based on methodology published in 1995 by the International Organiza-
12.2.5 Record or reference the measurement quality assur- tion for Standardization (ISO) in the Guide to the Expression of
ance plan used for the dosimetry system application. Uncertainty in Measurement (15). The purpose of this type of character-
ization is to promote an understanding of how uncertainty statements are
13. Measurement uncertainty developed and to provide a basis for the international comparison of
measurement results.
13.1 To be meaningful, a measurement of absorbed dose NOTE 18—ISO/ASTM Guide 51707 defines possible sources of uncer-
shall be accompanied by an estimate of uncertainty. tainty in dosimetry performed in radiation processing facilities and offers
procedures for estimating the magnitude of the resulting uncertainties in
13.2 Components of uncertainty shall be identified as be- the measurement of absorbed dose using a dosimetry system. The
longing to one of two categories: document defines and discusses basic concepts of measurement, including
13.2.1 Type A—those that are evaluated by statistical meth- estimation of the measured value of a quantity, “true” value, error, and
ods or uncertainty. Components of uncertainty are discussed, and methods are
13.2.2 Type B—those evaluated by other means. provided for evaluating and estimating their values. Methods are also
provided for calculating the combined standard uncertainty and estimating
13.3 Other ways of categorizing uncertainty have been expanded (overall) uncertainty.
widely used and may be useful for reporting uncertainty. For
example, the terms precision and bias or random and system- 14. Keywords
atic (non-random) are used to describe different categories of 14.1 absorbed dose; ceric-cerous sulfate dosimeter; dose;
uncertainty. dose measurement; dosimeter; dosimetry system; electron
13.4 If this practice is followed, the estimate of the ex- beam; gamma radiation; ionizing radiation; irradiation; pho-
panded uncertainty of an absorbed dose determined by this tons; radiation; radiation processing; reference-standard dosim-
dosimetry system should be less than 4 % for a coverage factor eter; X-radiation; ICS 17.240
ANNEXES
(informative)
A1.1 The electrochemical cell shown in Fig. A1.1 has both A1.5 The small open tip of compartment B is inserted into
an inner and outer compartment, A and B, respectively, the neck of a dosimeter ampoule, D. The glass syringe, E, is
separated by a porous junction, C, such as a glass frit, a used alternately to draw into compartment B the dosimetric
ceramic or kaolin junction, or a fibreglass wick. solution and then expel the solution after measurement.
A1.2 Compartment A contains the unirradiated dosimetric A1.6 Leads F and G provide a means for measuring the
solution. potential difference across the electrochemical cell when they
are connected to a potentiometer or multimeter.
A1.3 Compartment B contains either unirradiated or irradi-
ated dosimetric solution.
A1.4 The porous junction, C, provides contact between the
two solutions and shall have a porosity of less than 2 µm.
A2. PROCEDURE FOR PREPARING NOMINAL STOCK SOLUTIONS FOR THE DOSIMETER
A2.1 Nominal 0.4 mol dm−3 Sulfuric Acid (H2SO4): A2.2.2 Carefully cool contents and make up to volume with
−3 double-distilled water, stopper, and mix well.
A2.1.1 Transfer 22.2 mL of 18 mol dm H2SO4 into a
clean, dry 1-L volumetric flask containing about 700 mL of A2.2.3 Standardize resulting solution similarly as for 0.4
double-distilled water. mol dm−3 H2SO4.
A2.1.2 Carefully cool contents and make up to volume with A2.3 Nominal 0.1 mol dm−3 Ceric Sulfate:
double-distilled water, stopper, and mix well.
A2.3.1 In a 1-L volumetric flask, dissolve 58 g of ceric
A2.1.3 If desired, the resulting solution can be standardized sulfate, Ce(SO4)2 · 4H2O, in 600 mL of 0.4 mol dm−3 H2SO4.
using sodium carbonate primary standard or equivalent.
A2.3.2 Shake contents until all Ce(SO4)2 · 4H2O is dis-
NOTE A2.1—Add H2SO4 cautiously to the water as a considerable solved. Allow solution to stand at least two weeks in the dark.
amount of heat is released.
A2.3.3 Add enough 0.4 mol dm−3 H2SO4 solution to dilute
A2.2 Nominal 4 mol dm−3 Sulfuric Acid (H2SO4): to 1 L. Filter if necessary through a clean sintered-glass filter
(medium porosity).
A2.2.1 Transfer 222 mL of 18 mol dm−3 H2SO4 into a clean,
dry 1-L volumetric flask containing about 700 mL of double- A2.3.4 Transfer into a glass bottle provided with a ground
distilled water. glass stopper, and store in a dark place.
A2.4 Nominal 0.1 mol dm−3 Cerous Sulfate: A2.5 Concentration of Cerous-Sulfate Stock Solutions:
A2.4.1 In a 1-L volumetric flask, dissolve 36 g cerous A2.5.1 Pipette with a to contain pipette 1 mL of the
sulfate, Ce2(SO4)3 · 8H2O in 600 mL of double-distilled water. cerous-sulfate stock solution into a 100-mL volumetric flask,
NOTE A2.2—Cerous sulfate may require recrystallization before use (6). followed with a rinse of the pipette with double-distilled water.
A2.4.2 Shake contents until all Ce2(SO4)3 · 8H2O is dis- Make up to volume with double-distilled water, stopper, and
solved. Allow solution to stand at least two weeks in the dark. mix well.
A2.4.3 Add enough double-distilled water to dilute to 1 L. A2.5.2 Read the absorbance, A, at 254 nm in a spectropho-
Filter if necessary through a clean sintered-glass filter (medium tometer with double-distilled water in the reference cuvette.
porosity). The concentration, c2, of the stock cerous-sulfate solution is
A2.4.4 Transfer into a glass bottle provided with a ground given, in mol dm−3, by the following equation:
glass stopper, mix well, and store in a dark place. c 2 5 ~ 0.146! A (A2.1)
linear absorbance coefficient, εm, by the slope of the plot of εm = molar-linear absorption coefficient (m2 mol−1),
absorbance versus concentration as expressed by the following ρ = density of the dosimetric solution, kg m−3,
equation: d = path length of spectrophotometer cell, m, and
A i 5 103 ε m c i d (A3.5) Dj = absorbed dose to dosimetric solution, Gy.
A3.5.7 Plot Dj versus G ~ Ce31 ! j . The results should be linear
where:
with a slope equal to zero. If a significant deviation from zero
Ai = absorbance of sample i, slope is observed, that is, an apparent dependence of G ~ Ce31 !
ci = concentration of sample i, mol dm−3 , on absorbed dose, the solution may be unacceptable, (for
d = path length of spectrophotometer sample cell, m, and
example, contaminated by organic impurities).
i = 1, 2,..., 5 (representing samples prepared in A3.3.2).
A3.5.8 Plot ∆A versus D in accordance with the following
NOTE A3.2—The value of εm should be equal to 561 m2 mol−1 6 0.4 %
or 5610 L mol−1 cm−1 6 0.4 %, at 320 nm (3). equation:
∆A ij 5 β D j (A3.8)
A3.4 Density of Dosimetric Solution—Determine the den-
sity of the dosimetric solution at 25°C. where:
NOTE A3.3—The density should be 1.032 (60.002) × 103 kg m−3 at ∆A = net absorbance of irradiated sample,
25°C (8). D = absorbed dose to the dosimetric solution, Gy, and
β = slope, kgJ−1, of the plot determined by a least-squares
A3.5 Radiation Chemical Yield of Cerous Ion, G(Ce+3), by
linear regression fit of the data.
the Spectrophotometric Method:
A3.5.1 Prepare a sufficient number of dosimeters (at least
¯
A3.5.9 Determine the average G ~ Ce31 ! , mol J−1, from the
18) by filling 2-mL ampoules with the dosimetric solution. following equation:
After filling, flame seal the ampoules. f·β
¯
G ~ Ce31 ! 5 ε ρd (A3.9)
A3.5.2 Irradiate dosimeters, three at a time, at a calibrated m
rinse the cell with that dosimeter’s solution in order to reduce D = absorbed dose, Gy,
the effects of the previous dosimeter. ρ = density of the dosimetric solution, kg m−3, and
A3.6.7 Read the electropotential, E, in millivolts, across the j = 1,2,...n (number identifying absorbed dose
cell for each dosimeter after temperature equilibrium is estab- levels).
lished within the cell. ¯
A3.6.9 Calculate the average G ~ Ce31 ! from the following
NOTE A3.4—The electropotential, E, within the electrochemical cell has equation:
a positive temperature coefficient of 0.33 % per °C between 25 and 30°C n
(8). For the best accuracy, normalize measurements to a constant ¯ 1
temperature, thereby accounting for this effect.
G ~ Ce31 ! 5 n ( G ~ Ce
j51
31
!j (A3.12)
A3.6.8 Average the ∆E values for the three dosimeters A3.6.10 Plot Dj versus G ~ Ce31 ! j . The results should be
irradiated to the same absorbed dose level. Use the average linear with a slope equal to zero. If a significant deviation from
¯ , to calculate G ~ Ce31 ! in accordance with the
values, ∆E zero slope is observed, that is, an apparent dependence of
following equation: G ~ Ce31 ! on absorbed dose, the solution may be unacceptable,
103 c 4 1c 5 (for example, contaminated by organic impurities).
G ~ Ce31 ! j 5
3 1
c 2
ρD j 4
11
c5
c4
antilog10
¯
∆E
59.16
24 (A3.11) NOTE A3.5—The values of G¯ ~ Ce31 ! determined in accordance with
A3.5.9 and A3.6.9 should be equal approximately to 2.3 × 10−7 to 2.5 ×
10−7 mol J−1 at 25°C for the concentrations of ceric and cerous ions
where: specified for the dosimetric solution in this practice.
Bibliography
(1) Bjergbakke, E., “The Ceric Sulfate Dosimeter,” Manual on Radiation Impurity-Insensitive Megarad Dosimeter,” Int. J. Appl. Radiat, Isot.,
Dosimetry, Holm, N. W. and Berry, R. J., Eds., Marcel Dekker, New 22, 1971, pp. 199-207.
York, 1970, pp. 323-326. (10) Weidner, V. R., Mavrodineanu, R., Mielenz, K. D., Zelapoldi, R. A.,
(2) Sharpe, P. H. G., and Burns, D. T., “The Relative Response of Fricke, Eckerie, K. L. and Adams, B., “Standard Reference Materials:
Dichromate and Alanine Dosimeters to 60Co and High Energy Holmium Oxide Solution Wavelength Standard from 240-650
Electron Beam Radiation,” Radiat. Phys. Chem., 46, 1995, pp. nm–SRM 2034,” NBS Special Publication 260-102, 1986.
1273-1277. (11) Burke, R. W., Deardoff, E. R., and Menis, O., “Liquid Absorbance
(3) Matthews, R. W., “Effect of Solute Concentration and Temperature on Standards,” J. Research NBS, 76A, 1972, pp. 51-64.
the Ceric-Cerous Dosimeter,” Rad. Res., 55, 1973, pp. 242-255. (12) Burke, R. W., and Mavrodineanu, R., “Standard Reference Materi-
(4) Fricke, H., and Hart, E. J., “Chemical Dosimetry,” Radiation als: Certification and Use of Acidic Potassium Dichromate Solutions
Dosimetry, Vol II, Second Edition, Attix, F. H. and Roesch, W. C., as an Ultraviolet Absorbance Standard—SRM 935,” NBS Special
Academic Press, New York, 1966, pp. 167-239. Publication 260-54, 1977.
(5) Matthews R. W., “Aqueous Chemical Dosimetry,” Int. J. Appl. Rad. (13) Mavrodineanu, R., and Baldwin, J. R., “Standard Reference Mate-
Isot., 33, 1982, pp. 1159-1170. rials: Metal-on-Quartz Filters as a Standard Reference Material for
(6) Matthews, R. W., Mahlman, H. A., and Sworski, T. J., “Kinetics of the Spectrophotometry—SRM 2031,” NBS Special Publication 260-68,
Oxidation of Cerium (III) by Peroxysulfuric Acids Induced by 1980.
Cobalt-60 Radiation,” J. Phys. Chem., 74, 1970, pp. 2475-2479. (14) Burke, R. W., Smith M. V., Powell, L. J., and Mavrodineanu, R.,
(7) Taimuty, S. L., Towie, L. H., and Peterson, D. L., “Ceric Dosimetry: “Performance Characteristics of NBS Glass and Metal-on-Quartz
Routine Use at 105−107 Rads,” Nucleonics, 17, 1959, pp. 103-107. Transmittance Standards,” American Laboratory, July, 1986, pp.
(8) Matthews, R. W., “Potentiometric Estimation of Megarad Dose with 67-76.
Ceric-Cerous System,” Int. J. Appl. Radiat. Isot., 23, 1972, pp. (15) “Guide to the Expression of Uncertainty in Measurement,” Interna-
179-185. tional Organization for Standardization, 1995, ISBN 92-67-
(9) Matthews, R. W., “An Evaluation of the Ceric-Cerous System as an 10188-9.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.
This standard is copyrighted by ISO, Case postate 56, CH-1211, Geneva 20, Switzerland, and ASTM International, 100 Barr
Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States. Individual reprints (single or multiple copies) of this
standard may be obtained by contacting ASTM at the above address or at 610-832-9585 (phone), 610-832-9555 (fax), or
service@astm.org (e-mail); or through the ASTM website (www.astm.org). Permission rights to photocopy the standard may also be
secured from the ASTM website (www.astm.org/COPYRIGHT/).