Designation: C1052 − 14

Standard Practice for

Bulk Sampling of Liquid Uranium Hexafluoride1
This standard is issued under the fixed designation C1052; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 2.2 Other Documents:

1.1 This practice covers methods for withdrawing represen- USEC-651 Uranium Hexafluoride: A Manual of Good Han-
tative samples of liquid uranium hexafluoride (UF6) from bulk dling Practices3
quantities of the material. Such samples are used for determin- ANSI N14.1 Uranium Hexafluoride: Packaging for Trans-
ing compliance with the applicable commercial specification, port4
for example Specification C787 and Specification C996. ISO/DIS 7195 Packaging of Uranium Hexafluoride (UF6)
for Transport4
1.2 It is assumed that the bulk liquid UF6 being sampled
comprises a single quality and quantity of material. This 3. Terminology
practice does not address any special additional arrangements
3.1 Definitions of Terms Specific to This Standard:
that might be required for taking proportional or composite
3.1.1 container—the bulk vessel either holding or receiving
samples. When the sampled bulk material is being added to
by transfer, the UF6 to be sampled; it may consist of, for
UF6 residues already in a container (“heels recycle”) additional
example, a fixed vessel in a UF6 handling plant or a cylinder to
arrangements are required to avoid cross contamination of the
be used for the transport of UF6.
bulk UF6, these are addressed in the appropriate section (8.2)
of Specifications C787 and C996. 3.1.2 sample bottle—the small vessel into which the sample
of UF6 is withdrawn for transfer to the laboratory for charac-
1.3 The number of samples to be taken, their nominal terization.
sample weight, and their disposition shall be agreed upon
between the parties. 4. Summary of Practice
1.4 The scope of this practice does not include provisions 4.1 Two methods of withdrawing a sample are described,
for preventing criticality incidents. namely: (1) direct withdrawal from a filled container and (2)
1.5 This standard does not purport to address all of the withdrawal from the inlet-line during the filling of a container
safety concerns, if any, associated with its use. It is the by liquid transfer. The first method involves tilting or turning
responsibility of the user of this standard to establish appro- the container in such a way that its valve is below the surface
priate safety and health practices and determine the applica- of the liquefied UF6, and dependent on the equipment, this
bility of regulatory limitations prior to use. requires that the container holds more than a specified mini-
mum quantity of UF6. Liquid UF6 is withdrawn into a
2. Referenced Documents graduated volume and then transferred to the respective sample
2.1 ASTM Standards:2 bottle(s). In the second method, a small proportion of the UF6
C787 Specification for Uranium Hexafluoride for Enrich- flowing from one container to another is withdrawn into a
ment graduated volume and then transferred to the respective sample
C996 Specification for Uranium Hexafluoride Enriched to bottle(s).
Less Than 5 % 235U 4.2 For both methods of sampling, the presence of residues
may have significant implications for the quality of the UF6.
For safety and quality reasons, containers and bottles shall be
1
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear
clean, dry, and empty before filling.
Fuel Cycle and is the direct responsibility of Subcommittee C26.02 on Fuel and 4.3 Various types of sample bottles are in use and are
Fertile Material Specifications.
Current edition approved Jan. 15, 2014. Published February 2014. Originally
described in detail in the applicable national and international
approved in 1985. Last previous edition approved in 2007 as C1052 – 01 (2007).
DOI: 10.1520/C1052-14.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available from United States Enrichment Corp., 6903 Rockledge Dr., Bethesda,
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM MD 20817.
4
Standards volume information, refer to the standard’s Document Summary page on Available from American National Standards Institute, 11 W. 42nd St., 13th
the ASTM website. Floor, New York, NY 10036.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 C1052 − 14
standards, for example, ANSI N14.1 and ISO/DIS 7195. For a of UF6 corrosion resistance, and hence, internal surfaces are
given type of sample bottle, the detailed configuration, for generally conditioned with a suitable fluorinating agent, some-
example, valve orientation, terminal fittings, and the like, may times UF6 itself.
vary. Hence, the type and configuration of bottles to be used for 7.4 Cross-contamination may occur between subsequent
the withdrawal of samples shall be agreed upon between the samples taken using the same equipment, and appropriate
parties. precautions must be taken to prevent this. It is therefore
recommended that, before taking definitive samples, the equip-
5. Significance and Use ment is flushed through with an aliquot of the material to be
5.1 Uranium hexafluoride is normally produced and handled sampled. This is normally accomplished by taking an initial
in large (typically 1- to 20-ton) quantities and must, therefore, volume which is then rejected and not used for definitive
be characterized by reference to representative samples. The analysis. Alternative procedures to prevent cross-
quantities involved, physical properties, chemical reactivity, contamination are possible and should be validated individu-
and hazardous nature of UF6 are such that for representative ally.
sampling, specially designed equipment must be used and 7.5 If the sample bottles are taken for an analytical need
operated in accordance with the most carefully controlled and such as liquid UF6 subsampling for P10 tubes or liquid UF6
stringent procedures. This practice indicates appropriate transfer for FTIR quantification, it is recommended, in order to
principles, equipment, and procedures currently in use for bulk minimize the gas phase contribution to the sample bottle, to fill
sampling of liquid UF6. It is used by UF6 converters, enrichers, the bottle with more than 10% of its total volume.
and fuel fabricators to review the effectiveness of existing
procedures or as a guide to the design of equipment and 8. Procedure for Sampling Directly from Filled
procedures for future use. Containers (see Fig. 1)
5.2 It is emphasized that this practice is not meant to address 8.1 The equipment consists of a sample manifold that is
conventional or nuclear criticality safety issues. connected directly to the valve of the transport container and
has facilities for connecting one or more sample bottles. The
6. Hazards graduated volume is appropriately sized so that when filled
6.1 Because of its chemical, radiochemical, and toxic either completely or visually to a predetermined level it will
properties, UF6 is a hazardous material. UF6 is very reactive contain a known quantity of UF6. The graduated volume may
and corrosive. It reacts readily with water, atmospheric consist of the manifold and associated pipework, or may
moisture, certain metals, and many organic materials. For include an additional metering volume (pipette). The equip-
reasons of safety and to avoid contamination, precautions must ment may be designed to withdraw either single or multiple
be taken to avoid contact with such materials. Suitable han- sample quantities of UF6 at each operation. The total graduated
dling procedures are described in USEC-651. volume of the connected equipment (excluding the vacuum
system) should not exceed the designated maximum fill vol-
7. Principles ume of the connected sample bottles. Certain valves may be
remotely operated as necessary. The sampling equipment must
7.1 The essential purpose of the sample is to be represen- be heated to prevent solidification of the UF6 and may be
tative of the bulk material for the purpose of determining
compliance with the applicable material specification. To
ensure that the sample is representative for this purpose, certain
principles, as described below, must be observed.
7.2 Special attention must be given to ensuring that the bulk
material from which the sample is withdrawn is homogeneous,
particularly in those circumstances when it has been prepared
by the blending together of materials having different compo-
sitions. In practice, the low viscosity, and hence easy mobility,
of liquid UF6 facilitates the process of homogenization by the
action of convection currents within the bulk upon heating. It
is necessary to determine and establish for each set of sampling
equipment the physical conditions, normally a combination of
the minimum time and temperature for which liquefied ura-
nium hexafluoride is held, which guarantee homogeneity of the
bulk UF6.
7.3 The sampling equipment is fabricated to appropriate
high standards of vacuum integrity, and components in direct
contact with UF6 are made from nickel, high-nickel alloys, or
materials having equivalent resistance to UF6 corrosion. The FIG. 1 Schematic Arrangement for Sampling Directly from a
formation of an inert fluoride layer is often an important feature Filled Container

2
 C1052 − 14
located within the same heated enclosure as the container. The
sample bottles may be heated separately to permit independent
cooling, if necessary.
8.2 Load the container to be sampled into the heating
enclosure (for example, autoclave) and attach the sampling
equipment, including sample bottles. Evacuate and test the
equipment to ensure vacuum integrity.
8.2.1 When local safety regulations permit, a container of
hot, liquid UF6 may be loaded into the sampling equipment and
the sample bottles attached.
8.3 Heat the bulk UF6 for a sufficient period to ensure
homogeneity in accordance with the procedure established for
the equipment (see 7.2). During heating, monitor and check the
vapor pressure against the applicable pressure limit (if any) to
ensure compliance with the relevant specification and mainte-
nance of a safe pressure level. In case of overpressure, follow
appropriate procedures.
8.4 When the conditions for homogeneity have been met,
withdraw the appropriate quantity of liquid UF6 into the
graduated volume. This is usually effected by changing the
position of the container in such a way, for example, by tilting
or turning, that the UF6 flows under the influence of gravity
and any differential pressures established within the equip- FIG. 2 Schematic Arrangement for Sampling During the Filling of
a Transport Container
ment. Restore the container to its original position leaving the
graduated volume filled with liquid UF6. This may be indicated
by the use of suitable temperature sensors or pressure trans- volume is appropriately sized to contain the quantity of UF6
ducers or strain gages. required for a single sample and normally consists of the
8.5 If the equipment is designed to withdraw a single manifold and associated pipework itself or may include an
sample at each operation, open the appropriate sample valve to additional metering volume (pipette). The total graduated
allow the UF6 to flow into the sample bottle. Isolate the sample volume of the connected equipment (excluding the vacuum
bottle from the sampling manifold. system) should not exceed the designated maximum fill vol-
8.5.1 The first sample may be used to condition internal ume of the attached sample bottles. Certain valves may be
surfaces of the equipment (see 7.3) by suitable manipulation of remotely operated as necessary. Heat the sampling equipment
the vacuum system or rejected to prevent cross-contamination to prevent the solidification of UF6. The sample bottles may be
from previously sampled materials or both (see 7.4). contained in a separate enclosure to permit independent cool-
8.5.2 Take successive samples by repeating steps 8.4 and ing if necessary (see 9.6).
8.5 as necessary. 9.2 Conditions for homogeneity must be met within the UF6
8.6 If the equipment is designed to withdraw multiple main container immediately before the run-off to the secondary
samples at each operation, transfer the samples to the sample (for example, transport) container (see 7.2). This main con-
bottles by operating the valves associated with the successive tainer may typically be a plant vessel (for example, condenser)
sample bottles in the appropriate sequence. or another larger transport container (mother-container). In
8.7 At the completion of sampling, close the container valve order to ensure that representative samples are obtained in case
and evacuate the sampling equipment through the vacuum of the presence of particles in the UF6, careful attention should
system to remove residual UF6. be taken when choosing the appropriate time for sampling
because of rapid sedimentation. Alternative sampling methods
8.8 Fill the equipment to atmospheric pressure with dry gas such as a composite of several random samples or analysis
and remove, identify, cap, and weigh the sample bottles. Local based on a sedimented sample may be agreed upon between
safety regulations may demand that the UF6 is allowed to cool buyer and seller.
and solidify (below atmospheric pressure) before this operation
is carried out. 9.3 Attach the sampling equipment, including sample
bottles, at the relevant location to the UF6 runoff line. Evacuate
9. Procedure for Sampling During Filling of Transport and test the equipment to ensure vacuum integrity. Isolate the
Containers (see Fig. 2) sample bottles from the sample manifold.
9.1 The equipment consists of a sample manifold that has 9.4 Establish liquid transfer of UF6 from the main container
facilities for connecting one or more sample bottles and is to the secondary container.
connected to the filling manifold between the main and 9.5 At an appropriate time, open the sampling valve and
secondary (for example, transport) containers. The graduated withdraw the required quantity of UF6 into the graduated

3
 C1052 − 14
volume. This may be indicated by the use of suitable tempera- 9.9 At the completion of sampling, close all the sample
ture sensors or pressure transducers or strain gages. bottle valves. Any residual UF6 in the equipment and sampling
9.6 Close the sampling valve and open the first sample lines is either blown back using dry gas or is evacuated into a
bottle valve to transfer the sample. The equipment should be UF6 trap. Close the sampling valve and evacuate and backfill
designed to allow transfers to take place using the influence of the equipment with dry gas.
gravity and differential pressures induced by temperature 9.10 Remove, identify, cap, and weigh the sample bottles.
gradients. For this purpose, it may be necessary to cool the Local safety regulations may demand that the UF6 is allowed to
receiving sample bottles.
cool and solidify (below atmospheric pressure) before this
9.6.1 The first sample may be used to condition internal
operation is carried out.
surfaces of the equipment (see 7.3) by suitable manipulation of
the vacuum system or rejected to prevent cross-contamination
from earlier materials or both (see 7.4). 10. Keywords

9.7 Isolate the sample bottle from the sampling manifold. 10.1 bulk sampling; nuclear material; uranium hexafluoride
9.8 If successive samples are to be taken, repeat 9.5 and 9.6.
If not, the volume of the pipette should be adapted so that the
sample taken is representative of material transferred from the
main cylinder.

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