DRAFT
Proceedings of the ASME 2015 Pressure Vessels & Piping Division Conference
ORNL SPECIAL FORM TESTING OF SEALED-SOURCE ENCAPSULATIONS
Oscar Martinez, PhD
Oak Ridge National Laboratory
Oak Ridge, TN, USA
ABSTRACT
In the United States of America all transportation of radioactive
material is regulated by the Department of Transportation
(DOT), along with input from the Nuclear Regulatory
Commission. Beginning in 2008 a new type of sealed-source
encapsulation package was developed at Oak Ridge National
Laboratory (ORNL); these packages contain radioactive
material and are regulated and transported in accordance with
the requirements set for DOT Class 7 hazardous material. DOT
provides regulations pertaining to specific package contents
categorized as special form designs. The special form
designation indicates that the encapsulated radioactive contents
have a very low probability of dispersion even when subjected
to significant structural conditions. All ORNL DOT designs
have been certified by DOT as being special form materials.
The special form designs have been shown to simplify the
delivery, transport, acceptance, and receipt process.
Simplification of the transportation process makes the sealed-
source encapsulation designs very advantageous for shipment
to various facilities throughout the lifetime of the special form
material. To this end, DOT Certificates of Competent Authority
(CoCAs) have been sought for the design suitable for
containing high-alpha-activity actinide materials. This design
consists of a core of porous zirconia matrix pre-encapsulated
within triangular canister (ZipCan) tiles that are then enclosed
by a spherical shell. This new ZipCan design and a similar
rectangular ZipCube design were tested for compliance with
the regulations found in Title 49, Code of Federal Regulations,
Part 173.469, Tests for Special Form Class 7 (Radioactive)
(49 CFR 173.469). The spherical enclosure was subjected to 9
m impact, 1 m percussion, and 10-minute thermal tests. Before
and after each test the designs were subjected to a helium leak
check and a bubble test. The ZipCan tiles and core were
subjected to the tests required for ISO 2919:2012(E), including
a Class 4 impact test and heat test, and were subsequently
PVP2015
July 19-23, 2015, Boston, Massachusetts, USA
PVP2015–46003
Christopher Blessinger
Oak Ridge National Laboratory
Oak Ridge, TN, USA
subjected to helium leakage rate tests [49 CFR
173.469(a)(4)(i)]. The impact tile test unit contained a
nonradioactive surrogate; however, the thermal test unit
contained a radioactive source. All three designs are still
undergoing regulatory special form testing, and all three sealed-
source encapsulation designs are to be submitted to DOT for
CoCAs.
INTRODUCTION
Since the 1940s Oak Ridge National Laboratory
(ORNL) has been at the forefront of the early development of
regulations pertaining to the transport of radioactive shipments
and regulatory testing. A testing capability to develop, support,
and comply with transport regulations has been maintained at
ORNL from the 1960s to the present day [1]. Early testing at
ORNL primarily focused on developing information that would
support the development of regulations for the International
Atomic Energy Agency as well as assist package designers in
meeting radioactive material shipment requirements. For the
past 15 years, ORNL package testing has taken place under the
Package Testing Program (PTP) at the Package Research
Facility (PRF) located at the National Transportation Research
Center (NTRC). Package design and testing has been a key part
of the PTP operations for more than 50 years. As a result, the
PTP that manages the PRF provides a one-stop shop for design,
testing, and certification of a wide variety of packages needed
for the shipment of radioactive materials.
Special form materials are limited to those materials
which, if released from a package, would present a hazard from
direct external radiation only. Normally, a special form material
is composed of material with high physical integrity; therefore,
radioactive material contamination is not expected under severe
accident conditions. Occasionally a special form material is
composed of a nondispersible solid form. However, most often,
1 Copyright © 2015 by ASME
special form materials are hermetically sealed (encapsulated) with two fill holes (Figure 2). Radioactive materials are added
into an extremely durable metal capsule. The special form by depositing drops of nitrate through the fill tubes. After
designation indicates that the encapsulated radioactive contents deposition the nitrate solution is converted to an oxide. Final
have a very low probability of dispersion even when subjected encapsulation is accomplished by welding plugs into the fill
to significant structural conditions tests. holes.
Beginning in 2008 a new type of sealed-source
encapsulation package (SSE) was developed at ORNL. The
transport of SSE packages containing radioactive material is
subject to regulation by the US Department of Transportation
(DOT) with input from the US Nuclear Regulatory
Commission [2]. Additionally, the packages must be
transported in accordance with the requirements set for DOT
Class 7 hazardous material. DOT provides regulations
pertaining to specific package contents categorized as special
form designs. All of the ORNL SSE designs are categorized as
special form designs. These designs have been shown to
simplify the delivery, transport, acceptance, and receipt process, Figure 2 ZipCube test unit.
which helps streamline movement of SSEs to various facilities.
SSEs are intended to be shipped to various facilities throughout For some SSE designs there is an outer titanium
their lifetimes, making it advantageous for them to be certified spherical shell that serves as the principal encapsulation. The
as special form designs. two hemispheres of the sphere are welded together to
To this end, DOT certificates of competent authority accomplish final encapsulation (Figure 3). Within this outer
(CoCAs) have been sought for SSE designs that are suitable for spherical shell there is an internal framework that holds
containing high-alpha-activity actinide materials. The ORNL radioactive material (e.g., ZipCans or ZipCubes) in a fixed
SSE design consists of three parts: (1) a special form core, (2) position.
triangular zirconia pre-encapsulated canister (ZipCan) tiles, and
(3) a spherical shell that encloses the tiles. This new design was
tested for compliance with the regulations found in Title 49,
Code of Federal Regulations, Part 173.469, Tests for Special
Form Class 7 (Radioactive) (49 CFR 173.469). All regulatory
special form testing activities were conducted at NTRC under
the PTP. This paper details the regulatory special form tests and
results.

DESCRIPTION OF THE TEST UNITS

The ZipCan is a type of SSE. It is composed of an
equilateral triangle made of various layers (Figure 1).
Radioactive materials are added by depositing drops of a nitrate
solution into the wells through the fill tubes. After deposition
the nitrate is converted to an oxide and then covered with
potting cement. The final encapsulation is accomplished by
welding a plug to the fill tube.
Figure 3 Spherical shell test unit.
SPECIAL FORM TESTS
Two prototype ZipCans and spherical shells were
tested to demonstrate compliance with the requirements of
49 CFR 173.469. Prototype 1 was loaded with a nonradioactive
surrogate weight, and prototype 2 was loaded with radioactive
oxide. The special form tests for the ZipCan and spherical shell
are as follows:

• Impact Test [49 CFR 173.469 (b)(1)]

Figure 1 ZipCan article used as test unit 1 and test unit 2.
A rectangular encapsulation geometry, dubbed
“ZipCube,” was developed to achieve functions not readily
achieved by the ZipCan. The ZipCube is a stainless steel box
The specimen must fall onto the target from a height of
9 m (30 feet) or greater. The target must be as
specified in Sec. 173.465(c)(5).
• Percussion Test [49 CFR 173.469 (b)(2)]
(i) The specimen must be placed on a sheet of lead that
is supported by a smooth solid surface, and struck by
the flat face of a steel billet so as to produce an impact

2 Copyright © 2015 by ASME

 equivalent to that resulting from a free drop of 1.4 kg
(3 pounds) through 1 m (3.3 feet).
(ii) The flat face of the billet must be 2.5 cm (1 inch) in
diameter with the edges rounded off to a radius of 3
mm ±0.3 mm (0.12 inch ±0.012 inch).
(iii) The lead must be of hardness number 3.5 to 4.5 on
the Vickers scale and thickness 2.5 cm (1 inch) or
greater, and must cover an area greater than that
covered by the specimen.
7.4.1.2 Steel anvil, the mass of which is at least ten times that
of the hammer. It shall be rigidly mounted so that it does not
deflect during impact and shall have a flat surface, large
enough to support the entire sealed source.
According to Table 1 from ISO2919:1999(E), the
weight of the steel hammer for the Class 4 impact test shall be
“2 kg from 1 m or equivalent imparted energy.” Additionally,
the ZipCube was subjected to leak test 49 CFR 173.469(a)(4)(i)
and heat test 49 CFR 173.469(b)(4).

• Heat Test [49 CFR 173.469 (b)(4)] TEST MATRIX

The specimen must be heated in air to a temperature The following tables provide the sequence of tests and
of not less than 800 °C (1475 °F), held at that processes performed on each test unit. The numbers indicate the
temperature for a period of 10 minutes, and then sequence in which the process or test was performed on the test
allowed to cool. unit. The test units that were subjected to an impact test were
tested without radioactive material. The test units that were
• Leak Test [49 CFR 173.469 (a)(4)(i)] subjected to the heat test were loaded with radioactive material.
Demonstration of leak tightness of 10-4 torr-1/s (3.1 x Table 1 Sequence of tests and processes for the ZipCube
10-4 atm-cm3/s) based on air at 25oC (77oF) and one
atmosphere differential for solid radioactive content… Test or Process Test Unit
Description TU-1 TU-2
Two prototype ZipCubes were tested to demonstrate Leak Test - 1
compliance with the requirements of 49 CFR 173.469 and 10
Impact Test (ISO 2919) - 2
CFR 71.75 (d)(1) Qualification of special form radioactive
material and ISO2919:1999(E) Radiological protection-Sealed Heat Test 1 -
radioactive sources–General requirements and classification. Leak Test 2 3
The special form tests for the Zipcube are as follows:
Table 2 Sequence of tests and processes for the ZipCan
The 10 CFR 71.75 requirement states: Test Unit
Test or Process Description
TU-1 TU-2
The impact test and the percussion test of this section, provided
Leak Test 1,3,5,7 2
that the specimen is:
• (i) Less than 200 grams and alternatively subjected to the Plug Seal Percussion Test 2
Class 4 impact test prescribed in ISO 2919:1999(E) Vertex Percussion Test 4
“Radiological protection –Sealed radioactive sources – Impact Test 6
General requirements and classification”
Heat Test - 1
Since the ZipCubes are less than 200 g they were subjected to a
Class 4 impact test only as prescribed in ISO2919:1999(E) in Table 3 Sequence of Tests and Processes for the Spherical Shell
lieu of the percussion and impact tests.
Test or Process Test Unit
The ISO2919:1999(E) impact test is specified below: Description TU-1 TU-2
Helium Leak Test 1,3,5 1,3
7.4 Impact Test Impact Test 2 -
7.4.1 Apparatus
Percussion Test 4 -
7.4.1.1 Steel hammer, the upper part of which is equipped with
a means of attachment, and the lower part of which shall have Heat Test - 2
an external diameter of (25±1) mm and a flat striking surface
with its outer edge rounded to a radius of (3.0±0.3) mm. PERCUSSION TEST RESULTS, ZIPCAN
As shown in Table 2, test unit 1 of the ZipCan was
The center of gravity of the hammer shall lie on the axis of the subjected to percussion tests. The percussion tests were carried
circle, which defines the striking surface; this axis itself passing out at the indoor drop pad at the NTRC. This drop pad has a
through the point of attachment. The mass of the hammer for total mass of ~13.6 metric tons and meets the specifications for
each test class is given in Table 1. the impact test target (see Design and Certification of Targets

3 Copyright © 2015 by ASME

for Drop Testing at the NTRC Package Research Facility Rev. (Figure 7). After the second percussion test, the test unit was
0, May 2003, ORNL/NTRC-001). For the plug seal test, a 12 × subjected to a leak test.
12 × 1 in. thick sheet of pure lead (ASTM B749-97) was
centered on the indoor drop pad, and TU-1 was placed on an
undented surface of the lead sheet (Figure 4). A 1 in. diameter
steel billet, weighing 1.4 kg, was raised to a height of 1 m
directly above the plug seal. When released, the billet impacted
the center plug seal. The impact of the billet resulted in a slight
blemish and deformation of the plug, as shown in Figure 5.
After the test, the test unit was subjected to a helium leakage
rate and a bubble test.

Figure 6 Vertex impact test setup.

Figure 7 Vertex impact test result.

Figure 4 Impact billet 1 m above the ZipCan.
HEAT TEST RESULTS, ZIPCAN
Since the heat test unit contained radioactive materials,
the thermal tests were completed in a glove box in a
radiological facility at ORNL (Figure 8). A tube furnace was
used for the heat test. The furnace was preheated for a period of
3 hours at 850oC to ensure full thermal soak. After the 3-hour
preheat, the furnace door was opened and the 10-minute special
form test was started (Figure 9). After the 10-minute period the
test unit was removed from the furnace and allowed to cool
under ambient conditions. The test unit was subjected to a leak
test after the heat test, as shown in Figure 10.

Figure 5 Plug impact damage of the ZipCan.

After a successful helium leakage and bubble test, the
test unit was subjected to a secondary vertex percussion test.
The test unit was placed on a fresh surface on the lead sheet.
The test unit was oriented such that the billet would squarely hit
the vertex of the test unit from a height of 1 m, as illustrated in
Figure 6. After impact from the billet, the vertex compressed
slightly toward the center and slightly deformed out of plane

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Figure 8 Muffle furnace used in the heat test and 7920 lab
210 hood.

Figure 11 ZipCan impact at 9 m.

LEAK RATE TESTING

Figure 9 Thermal test temperature profile. Evacuated Envelope (with Back Pressurization)
Leak rate tests that meet the test requirements of 49
CFR 173.469 (a)(4)(i) were performed individually on each test
unit after each test. The leak rate tests were performed using
ANSI N14.5-1997, American National Standard for
Radioactive Materials–Leakage Tests on Packages for
Shipment, Table A.1, Test Description A.5.5, Evacuated
Envelope (with back pressurization) and Test Description A.5.6
Gas bubble techniques. The ANSI document indicates that the
back pressure method “…is ideal for welded capsules from
very small sizes up to the sizes limited by the dimensions of the
pressurizing chamber,” that the “nominal test sensitivity =
10-3- 10-8 ref-cm3/s,” and that the bubble test method is used for
hermetically sealed test specimens.
Section A.5.5 of ANSI N14.5-1997, Evacuated
Envelope with Helium Back Pressure of the ANSI document
Figure 10 Post heat test.
references ASTM E 493, Standard Test Methods for Leaks
Using the Mass Spectrometer Leak Detector in the Inside-Out
IMPACT TEST RESULTS, ZIPCAN
Testing Mode. This standard provides the method for converting
Test Unit 1 was subjected to the 49 CFR 173.469(b)(1)
a measured leak rate using the evacuated envelope with helium
impact test. This test was carried out at an indoor facility with a
back-pressure method into the standardized leak rate that must
9 m pit located in Building 7603 at ORNL. A steel plate was
be compared with the pass/fail criteria stated in 49 CFR
placed on top of a concrete slab and used as the unyielding
173.469(a)(4)(i), which is 10-4 torr-l/s (1.3 x 10-4 atm-cm3/s).
impact target. The weight of the steel plate was 510 kg and
meets the specifications for the impact test target. There was no
The equation provided in Sect. 11.1.9 of ASTM E493 is:
specified orientation for the impact test since the test unit is an
equilateral triangle. A 30 ft plumb bob was used to measure the
S l = (P e /P a ) * (1- e(-3600*a*T)) * (e(-a*t)) * L , (1)
drop height. The unit impacted the steel plate target, bounced,
and reimpacted the steel plate target a second time. Subsequent
where:
inspection of the test unit showed minor deformation of the
Sl = indicated (measured) leak rate (cm3/s)
impact location, which was at a vertex (Figure 11). After the
Pe = bombing pressure of helium (absolute)
impact test, the test unit was subjected to a helium leakage rate
Pa = atmospheric pressure (absolute)
test and a bubble test.
T = bombing time (hours)
t = waiting time between bombing and testing (s)
L = actual (standardized) leak rate (atm-cc/s)
a = L/V where V = internal volume
e = 2.71 (natural logarithm).

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 Since we are measuring S l and wish to solve for L, the
equation requires an iterative solver to find the solution. The
equation was solved using spreadsheet iteration. Note that the
ASTM standard uses the term “bombing,” whereas the ANSI
standard uses the term “back pressure.” These terms have the
same meaning. To solve Equation 1, the internal volume (i.e.,
void space) within the test units must be known. For the test
units, this internal volume consisted of accessible internal void
spaces. The internal void was measured from the computer-
aided design models.
The test units were leak tested at ORNL by a certified
ASNT Level II and Level III leak tester before and after each
special form test. The test apparatuses used employed a mass Figure 13 Diagram of the helium leak testing system.
spectrometer configured to detect helium, a calibrated helium
leak to calibrate the system, and two separate vessels: one for GAS BUBBLE TECHNIQUE
helium back pressurization and one for the subsequent helium The gas bubble test was done using the methods
leakage rate testing under vacuum conditions. Figure 12 shows described in ANSI N14.5-1997, American National Standard
a schematic of the system used for helium back pressurization, for Radioactive Materials–Leakage Tests on Packages for
and Figure 13 shows a schematic of the system used for the Shipment, Table A.1 test description A.5.6 (b) Vacuum Bubble.
helium leakage rate test. Table 4 lists the variables and results The method involves immersing the test unit in a liquid and
for each test. then producing a vacuum above the liquid (e.g., water/glycol or
isopropyl alcohol) in which the test item is submerged. A leak is
indicated by a stream of bubbles. This method is applicable to
welded capsules. The nominal test sensitivity is 10-3 ref-cm3/s
(10-4 Pa-m3/s). Table 4 and Table 5 show the results for the
helium leak test and gas bubble leak test for the ZipCan.

Figure 14 Vacuum bubble test.

For the ZipCan leak test the following values were used:

Pe = 30.0 psia
Pa = 14.69 psia
Figure 12 Diagram of the helium back pressurization T = 1 hour
system. t = <3,600 s
a = <2.7 × 10-4
e = 2.71 (natural logarithm)
V = 0.37 cc

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 Table 4 ZipCan leak rate test variables and results for TU-1 and TU-2

Test Unit

Parameter TU-1 TU-2

Leak Test 1 Leak Test 3 Leak Test 5 Leak Test 7 Leak Test 1
Measured leak
rate (cm3/s)–S l 4.7 × 10-9 4.3 × 10-9 3.2 × 10-9 3.0 × 10-8 6.0 × 10-8
(atm-cc He/s)
a = L/V <2.7 × 10-4
<2.7 × 10-4 <2.7 × 10-4 <2.7 × 10-4 <2.7 × 10-4
(s-1)
Standardized
leak rate–L <1.0 × 10-4
<1.0 × 10-4 <1.0 × 10-4 <1.0 × 10-4 <1.0 × 10-4
(atm- cm3
He/s)
Parameter Bubble Test 1 Bubble Test 3 Bubble Test 5 Bubble Test 7 Bubble Test 1
Bubble test pass pass pass pass pass
pass/fail

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 Leak Test
IMPACT TEST ISO2919:1999(E) The ZipCube test unit was subjected to a helium leak
The ZipCube test unit that contained the surrogate test test and a bubble leak test after each regulatory test to ensure
weight was subjected to the ISO2919:1999(E) impact test. The that the welds had not failed. Table 6 and Table 7 list the results
impact test was performed at the NTRC in accordance with the of the helium leak test and bubble test. For the ZipCube leak
test procedure. The ZipCube was centered on the indoor drop test the following values were used:
pad, as shown in Figure 15. A 1 in. diameter steel billet,
weighing 2 kg, was placed on the release mechanism and raised Pe = 30.0 psia
to a height of 1 m. The steel billet was released such that the Pa = 14.69 psia
billet directly impacted the test unit on a weld line (Figure 16). T = 1 hour
After the impact test, the ZipCube was subjected to the t = <3,600 s
aforementioned helium leak test and bubble test. a = <1.67 × 10-5
e = 2.71 (natural logarithm)
V = 6 cc
Table 5 ZipCube leak rate test variables and results for
TU-1 and TU-2

Test Unit

Parameter TU-1 TU-2

Leak Test Leak

Leak Test 1
2 Test 1
Figure 15 Impact billet 1 m above the ZipCube. Measured leak
3
rate (cm /s)–S l 5 × 10-6 5 × 10-6 5 × 10-6
(atm-cc He/s)
a = L/V <1.67 × <1.67 ×
<1.67 × 10-5
(s-1) 10-5 10-5
Standardized
<1.0 ×
leak rate–L <1.0 × 10-4 <1.0 × 10-4
3 10-4
(atm- cm He/s)
Figure 16 Before and after impact of the ZipCube. Bubble Test Bubble Bubble
Parameter 1 Test 2 Test 1
HEAT TEST Bubble Test pass pass pass
The heat test for the ZipCube was conducted at the pass/fail
same time as the heat test for the ZipCan. The same preheat
profile and heat test temperature profile that was used for the
ZipCan was used for the ZipCube. After the heat test, the test SPHERICAL SHELL
unit was removed from the furnace and allowed to cool, as
shown in Figure 17. IMPACT TEST, PERCUSSION TEST AND HEAT TEST
The spherical shell with a nonradioactive, surrogate
test weight was subjected to the percussion and impact test as
described in 49 CFR 173.469. The spherical shell was dropped
on a steel plate weighing 510 kg. The steel plate created the
“essentially unyielding surface” for the impact test. A 30 ft
plumb bob was used to verify the drop height. When ready, the
sphere was dropped and then inspected (Figure 18). Posttest
visual inspection revealed scuffs but no significant structural
damage to the test unit, as can be seen in Figure 18. Following
the impact test the test unit was subjected to a helium leak test
Figure 17 Post heat test. and a bubble test. Finally, the test unit was subjected to the
percussion test. The sphere was placed on a fresh surface on the
lead sheet. A 1.4 kg steel billet was raised to a height of 1 m

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and dropped on the sphere. The posttest damage inspection
showed no discernible damage from the steel billet (Figure 19).
The heat test for the sphere is pending and should be completed
in 2015. The special form tests for the sphere are projected for
completion in 2015.
Figure 18 Post impact test.
Figure 19 Post percussion test.
CONCLUSION
Two prototype ZipCan test units, a ZipCube test unit,
and a spherical shell test unit were subjected to the tests
specified in 49 CFR 173.469, 10 CFR 71.75, and ISO
2919:1999(E). All test units surpassed the leak rate criteria
following each special form test. The special form testing
process has shown that the design of the ZipCan and the
ZipCube meets the special form criteria.
ACKNOWLEDGEMENTS
This manuscript has been authored by UT-Battelle, LLC, under
Contract No. DE-AC0500OR22725 with the U.S. Department
of Energy. The United States Government retains and the
publisher, by accepting the article for publication,
acknowledges that the United States Government retains a non-
exclusive, paid-up, irrevocable, world-wide license to publish
or reproduce the published form of this manuscript, or allow
others to do so, for the United States Government purposes.
The Department of Energy will provide public access to these
results of federally sponsored research in accordance with the
DOE Public Access Plan (http://energy.gov/downloads/doe-
public-access-plan).
REFERENCES
1 Shappert L.B., Ludwig S.B., “44 Years of Testing
Radioactive Materials Packages at ORNL,” Proceedings of
14th International Symposium on Packaging and
Transportation of Radioactive Materials (PATRAM2004),
Berlin, Germany, September 2004.
2 U.S Nuclear Regulatory Commission, 10 Code of Federal
Regulations Part 71, Washington, DC, USA, January 2013.
3 ASTM International, Standard Practice for Thermal
Qualification of Type B Packages for Radioactive Material,
E2230-08, West Conshohocken, Pennsylvania, 2008.
4 Martinez O.A., Test Report of Special Form Qualification
Testing for the Zirconia Pre-Encapsulated Canister,
ORNL/NTRC-069, Rev. 0, Oak Ridge, TN, USA,
December 2014.
5 Martinez O.A., Test Report of Special Form Qualification
Testing for the ZipCube Canister, ORNL/NTRC-068, Rev.
0, Oak Ridge, TN, USA, December 2014.
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