Standard Test Method for Nuclear-Grade Activated Carbon

SIGNIFICANCE AND USE
The results of this test method give a conservative estimate of the performance of nuclear-grade activated carbon used in all nuclear power plant HVAC systems for the removal of radioiodine.
SCOPE
1.1 This test method is a very stringent procedure for establishing the capability of new and used activated carbon to remove radio-labeled methyl iodide from air and gas streams. The single test method described is for application to both new and used carbons, and should give test results comparable to those obtained from similar tests required and performed throughout the world. The conditions employed were selected to approximate operating or accident conditions of a nuclear reactor which would severely reduce the performance of activated carbons. Increasing the temperature at which this test is performed generally increases the removal efficiency of the carbon by increasing the rate of chemical and physical absorption and isotopic exchange, that is, increasing the kinetics of the radioiodine removal mechanisms. Decreasing the relative humidity of the test generally increases the efficiency of methyl iodide removal by activated carbon. The water vapor competes with the methyl iodide for adsorption sites on the carbon, and as the amount of water vapor decreases with lower specified relative humidities, the easier it is for the methyl iodide to be adsorbed. Therefore, this test method is a very stringent test of nuclear-grade activated carbon because of the low temperature and high relative humidity specified. This test method is recommended for the qualification of new carbons and the quantification of the degradation of used carbons.
1.1.1 Guidance for testing new and used carbons using conditions different from this test method is offered in Annex A1.
1.2 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.

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 3803 – 91 (Reapproved 2004)
Standard Test Method for
Nuclear-Grade Activated Carbon
This standard is issued under the fixed designation D 3803; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This test method is a very stringent procedure for 2.1 ASTM Standards:
establishing the capability of new and used activated carbon to D1193 Specification for Reagent Water
remove radio-labeled methyl iodide from air and gas streams. D2652 Terminology Relating to Activated Carbon
Thesingletestmethoddescribedisforapplicationtobothnew D2854 Test Method for Apparent Density of Activated
and used carbons, and should give test results comparable to Carbon
those obtained from similar tests required and performed E300 Practice for Sampling Industrial Chemicals
throughout the world. The conditions employed were selected E691 PracticeforConductinganInterlaboratoryTestStudy
to approximate operating or accident conditions of a nuclear to Determine Precision of a Test Method
reactor which would severely reduce the performance of 2.2 Code of Federal Regulations:
activatedcarbons.Increasingthetemperatureatwhichthistest CFR Title 49, Section 173.34, “Qualification, Maintenance,
is performed generally increases the removal efficiency of the and Use of Cylinders’’
carbon by increasing the rate of chemical and physical absorp- CFR Title 49, Part 178, Subpart C, “Specifications for
tion and isotopic exchange, that is, increasing the kinetics of Cylinders’’
the radioiodine removal mechanisms. Decreasing the relative 2.3 Military Standards:
humidityofthetestgenerallyincreasestheefficiencyofmethyl MIL-F-51068D Filter, Particulate High Efficiency, Fire Re-
iodideremovalbyactivatedcarbon.Thewatervaporcompetes sistant
with the methyl iodide for adsorption sites on the carbon, and MIL-F-51079A Filter, Medium Fire Resistant, High Effi-
as the amount of water vapor decreases with lower specified ciency
relative humidities, the easier it is for the methyl iodide to be MIL-STD-45662 Calibration Systems Requirements
adsorbed.Therefore, this test method is a very stringent test of 2.4 Other Standards:
nuclear-grade activated carbon because of the low temperature ANSI/ASME N45.2.6 Qualifications of Inspection, Exami-
and high relative humidity specified. This test method is nation, and Testing Personnel for Nuclear Power Plants
recommended for the qualification of new carbons and the
3. Terminology
quantification of the degradation of used carbons.
3.1 Definitions of Terms Specific to This Standard:
1.1.1 Guidance for testing new and used carbons using
conditions different from this test method is offered in Annex 3.1.1 counter effıciency (CE)—the fraction of the actual
number of disintegrations of a radioactive sample that is
A1.
1.2 This standard does not purport to address all of the recorded by a nuclear counter.
3.1.2 effıciency (E)—the percentage of the contaminant
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- removed from a gas stream by an adsorption bed; expressed
mathematically as E = 100 − P, where E and P are given in
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. percent.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Published by the General Service Administration, 18th and “F’’ St., N. W.,
This test method is under the jurisdiction of ASTM Committee D28 on Washington, DC 20405.
Activated Carbon and is the direct responsibility of Subcommittee D28.04 on Gas AvailablefromStandardizationDocumentsOrderDesk,Bldg.4SectionD,700
Phase Evaluation Tests. Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
Current edition approved April 1, 2004. Published June 2004. Originally Available from American National Standards Institute, 11 W. 42nd St., 13th
approved in 1979. Last previous edition approved in 1998 as D3803–91 (1998). Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 3803 – 91 (2004)
3.1.3 penetration (P)—the percentage of the contaminant separate units each capable of containing carbon to a depth of
(CH I) which passes through the equilibrated test bed of 25 mm.Two backup canisters, each of 50 6 1 mm total depth,
standard depth, and is collected on the backup beds during the are required. Canisters may be reused after being decontami-
feed and elution periods under specified conditions. nated to remove residual radioactivity. An acceptable bed
3.1.4 relative humidity (RH)—for the purpose of this test construction is shown in Fig. 1 with critical dimensions noted.
method, relative humidity is defined as the ratio of the partial 6.2.2 Clamping assemblies are needed for sample and
pressure of water in the gas to the saturation vapor pressure of backup beds. The only requirements for these assemblies are
water at the gas temperature and pressure. At temperatures that they provide a smooth sealing face, uniform alignment of
below 100°C, this is the normal definition and relative humid- bedcanisters,andsufficientclampingforcesothattheleaktest
ity can range from 0 to 100%. in10.2canbemet.Asuggesteddesignforclampingassemblies
3.2 Definitions—for additional terms relating to this stan- is shown in Fig. 2.
dard, see Terminology D2652. 6.3 A schematic of a generalized test system is shown in
Fig. 3. This system is designed to operate at approximately
4. Summary of Test Method 30°Cand95%relativehumidity,withagasflowof24.7L/min
at atmospheric pressure. If test conditions which differ signifi-
4.1 Both new and used carbons are first exposed to humid
cantly from these are required, then separate calibrations or
air (pressure, approximately 1 atm; temperature, 30.0°C; rela-
instrumentation, or both, may be required.
tive humidity, 95%) for a pre-equilibration period of 16 h.
Duringthispre-equilibrationperiod,thetestsystemmayberun
unattended with the required parameter monitoring and ad-
equate control devices. Following pre-equilibration, the air
flow is continued for a two-hour equilibration period, during
which the acceptable variability of all parameters is reduced.
The test system must be closely monitored and controlled
during the final four hours of the test. Qualification of
personnel to perform this testing must meet or exceed ANSI/
ASME N45.2.6—1978, Level II, which requires a combina-
tion of education and actual test system operation experience.
During the challenge or feed period, radio-labeled methyl
iodide at a mass concentration of 1.75 mg/m of humid air
flow is passed through the beds for a period of 60 min.
Following the feed period, humid air flow without test adsor-
bate is continued at the same conditions for a 60-min elution
period.Throughouttheentiretest,theeffluentfromthesample
bed passes through two backup beds containing carbon having
a known high efficiency for methyl iodide. The two backup
beds trap essentially all the radio-labeled methyl iodide that
passesthetestbedand provide a differential indicationoftheir
efficiency.At the end of the elution period, the gamma activity
of I in the test and backup beds is measured by a gamma
counter,andthepercentofadsorbatepenetratingthetestbedis
determined.
5. Significance and Use
5.1 The results of this test method give a conservative
estimate of the performance of nuclear-grade activated carbon
used in all nuclear power plant HVAC systems for the removal
of radioiodine.
6. Apparatus
6.1 Sample Preparation Apparatus:
* Standard canister dimension may be used in multiples if desired.
Single test canisters of full depth may be used.
6.1.1 Riffle Sampler, in accordance with 32.5.2 of Practice
1—Bed holder
E300.
2—Adsorption media
6.1.2 Feed Funnel and Vibrator, in accordance with the 3—O-ring gland
4—Perforated screen (both ends)
Procedure Section of Test Method D2854.
5—Retaining snap ring (both ends)
6.2 Sample and Backup Bed Assemblies:
6—Baffle (both ends)
6.2.1 The sample bed canister and backup bed canisters 7—Holes for assembly tie-rods (four)
must each be either a single unit capable of containing carbon
FIG. 1 Adsorption Media Test Bed Holder (Canister)
to a depth of 50 6 1 mm, or they may be assembled from two
D 3803 – 91 (2004)
control should be accurate and stable to within 6 2% of
specified flow rate. System capacity shall meet or exceed the
volumetric flow requirements as calculated from the specified
facevelocity.Asurgetankandpressurecontrolvalveshouldbe
employedineithertypeofsystemtoensurestableandaccurate
flow measurement and control. For safety, it is important that
thepressuresystembeequippedwithapressurereliefvalve.It
is important that the pipe diameter and inlet air filters for a
vacuum system be designed and maintained to minimize the
pressuredropfromambienttoensurethatthespecificationsfor
absolute pressure at the test bed are met (see Table 1).
6.6 Moisture Separator—A moisture separator should be
used to protect the HEPAfilter by removing large quantities of
entrained particulate water, if present, after humidification. A
HEPA filter (or equivalent) is required to function as a final
droplet trap to remove small amounts of fine particulate water
from the carrier gas ahead of the test bed.
6.7 Adsorbate Supply—This system shall consist of a stain-
lesssteelcylinder,pressuregage,pressureregulator,andaflow
regulator capable of providing a steady flow of the challenge
gas,thatis,radio-labeledmethyliodideindrynitrogen,forthe
duration of the test feed period. The point of injection into the
main gas flow of the system must be such that the cross-
sectionaldistributionoftheadsorbateatthefaceofthetestbed
canbeensuredtobehomogeneous.Amixingchamber,baffles,
glass beads, etc. should be used to achieve adequate mixing.
6.8 Constant Temperature Cabinet—An enclosure and as-
sociated thermoregulatory system must be used that is capable
of maintaining the inlet gas stream temperature from the point
ofhumiditycontroltothetestbed,andthesurfacetemperature
of all carbon canisters at 30.0 6 0.2°C, except during the first
several hours of pre-equilibration, during which the adsorption
of water by the carbons may increase these temperatures
slightly. All tubing downstream of the moisture separator, the
carbon bed canisters and holders, temperature and pressure
ports and measurement devices upstream and downstream of
the test bed, and an upstream port and tubing to the dew point
sensor all must be included within the temperature controlled
enclosure. In addition, it is highly recommended that a bypass
1—Canister (four shown)
line be included around the sample bed assembly to avoid
2—Inlet cap
exposing the sample to start-up conditions possibly outside
3—Outlet cap
4—Thermocouple
those specified.
5—Thermocouple fitting
6.9 Flow Measurement and Control—Mass flow control-
6—Static tap
7—Tie bar (four) lers, control valve and orifice meter, rotameter or any other
8—O-ring seals
device with adequate stability and demonstrated measurement
FIG. 2 Canister Assembly (Test or Backup Beds)
system accuracy of 6 2% of specified flow rate at the test
conditions. All flow measuring devices must use correction
factors for interpretation and application to actual test condi-
6.4 Saturator System—This system may be a controlled
tions. These factors must be carefully predetermined and
temperaturesaturator(bubbler)orspraychamber(environmen-
documented. No flow measuring device should be located
tal condition generator), or any other device of sufficient
directly downstream of the test bed such that it is subject to
stabilityandcapacitytosupplytherequiredmassflowofwater
variabletemperatureandhumidityconditionsduringatestasa
vapor at test conditions.
result of water absorption by the carbon.
6.5 Flow Generator—This system may be an air compres-
6.10 Interconnecting Tubing—Tubing must be non-reactive
sorupstreamofthetestsystemoravacuumpumpdownstream
of the test system. A dryer, carbon adsorber, and HEPA with methyl iodide, such as stainless steel, glass, etc., with a
minimum of ⁄8-in. outside diameter, and kept as short as
(high-efficiency particulate air) filter are required for either
system to condition the inlet air. Flow measurement and possible to reduce the system pressure drop.
D 3803 – 91 (2004)
FIG. 3 Schematic of Activated Carbon Test System
TABLE 1 Parameter Specifications
measurement of test bed inlet air temperature and dew point.
The placement of the air temperature RTD must be such that it
NOTE 1—Temperature,relativehumidity,pressure,andgasvelocityare
isnotsubjecttoradiativeheatingfromthetestbed.Itiscritical
to remain constant within the specified maximum variations throughout
the entire test, that is, for each test period. Parameter excursions outside to the exact measurement of relative humidity that the chilled
the limits specified in this table will invalidate the test results. If results
mirror RTD and the inlet air temperature RTD be matched
based on a test containing such variations must be reported, then these
exactly (6 0.1°C) or that differences are exactly corrected for
variations must be noted in the comments section of the external report
in relative humidity calculations.
form and flagged in the parameter monitoring portion of the internal
6.12 Pressure Measurement Devices—Absolute pressure
report.
measuring devices must be accurate to within 6 1% of the
Equilibration, Chal-
Pre-Equilibration
Parameter lenge, and Elution reading at standard atmospheric pressure and be capable of
(First 16 h)
(Final 4 h)
digital or analog output to meet the specified recording
Temperature, °C 30.0 6 0.4 30.0 6 0.2
requirements. The sensors and output devices must be cali-
Range 29.6 to 30.4 29.8 to 30.2
brated as a unit to ensure system accuracy. The differential
Relative humidity, % 91.0 to 96.0 93.0 to 96.0
pressure device required for measurements across the test bed
Flow, m/min 12.2 6 0.6 12.2 6 0.3
Face velocity, m/min 11.6 to 12.8 11.9 to 12.5
mustbecapableofdetectinga0.25kPapressuredifferenceand
Absolute pressure, kPa 101 6 5 101 6 5
be accurate to within 6 2% of the reading at the normal
Bed diameter and depth, mm 50 6150 6 1
operating differential pre
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