Ice Plugging of Piping

Keywords: EPRI TR-016384R1
Maintenance Final Report

System isolation November 1997
Refrigerants
Freeze sealing
NMAC Tech Note
Freeze Sealing (Ice Plugging)

of Piping, Revision 1
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R E P O R T S U M M A R Y
Freeze Sealing (Ice Plugging) of Piping

Freeze sealing, or ice plugging as it is sometimes called, has proven
over time to be a relatively safe and cost-effective procedure for tempo-
rary piping system isolation when performed by experienced technicians.
This guide consolidates information on the freeze sealing process.
BACKGROUND In the course of performing certain nuclear plant maintenance

activities, piping system isolation is sometimes required. When this cannot be
accomplished through the use of existing valves, draining of the system be-
comes necessary. This can be a time-consuming and costly procedure. As an
alternative, some operators have turned to the use of freeze sealing, or creation
of an ice plug within the pipe by applying an external refrigerant in a local area,
to resolve their temporary system isolation requirement. Freeze sealing has
proven to be a relatively safe, reliable, and cost-effective solution to temporary
piping system isolation requirements when performed by experienced techni-
INTEREST CATEGORIES
cians employing safe operating practices. Using this procedure, pipes of various
materials in sizes up to 48 inches (120 cm) have been successfully isolated for
Nuclear plant operations periods as long as one month.
and maintenance
Engineering and technical
OBJECTIVES To reorganize the information presented in the original document
support along a more process-oriented approach, thereby providing plant engineering
and maintenance personnel with the necessary information to more effectively
KEYWORDS manage the planning and performance of their freeze sealing operations.
Maintenance
APPROACH To revise this document, EPRI first began with a thorough review
System isolation of the original guides contents, subsequently matching that information against
Refrigerants requirements learned during conversations with selected utility personnel
Freeze sealing involved in the planning and performance of freeze sealing operations at their
sites. After reorganizing the content, additional information was added to clarify
specific issues raised by users since the document was first published. Like-
wise, some information presented in the original document that has proved to
be particularly controversial has been removed, as has some vendor-specific
information. Representative industry experience data, in the form of summary
data of past freeze sealing operations, were solicited from a major service
provider for inclusion as an appendix. General troubleshooting guidance was
also solicited from the service provider, based upon their experience over the
course of many years.
RESULTS The revised document now provides a comprehensive discussion

on the subject of freeze sealing of piping, with emphasis on commercial nuclear
power plant operations where appropriate. In addition to extensive sections on
the planning and performance aspects of freeze sealing, greater emphasis has
been placed on the relative effects and stresses on piping materials caused by
the application of cryogenic materials.
EPRI TR-016384R1s Electric Power Research Institute November 1997

EPRI PERSPECTIVE EPRI believes that this document will be of
particular interest to plant engineers, work planners, trainers, and mainte-
nance personnel and that through its application, the relative safety and
effectiveness of planned freeze sealing operations can be significantly
improved.
Project
TR-016384R1
EPRI Project Manager: John M. Jenco
Nuclear Maintenance Applications Center (NMAC)
Nuclear Power Group
For further information on EPRI research programs, call EPRI Technical
Information Specialists, 415/855-2411.
TR-016384R1
Final Report
November 1997
Revision 0
Prepared by:
Ted Delong
Babul Patel
Phil Galanti
Bechtel Power Corp.
50 Beale Street
San Francisco, CA 94119
George Howard
Freeze Technology International, Inc.
11331 Charles Street
Houston, TX 77041
Revision 1
Prepared by:
John M. Jenco
Prepared for
Nuclear Maintenance Applications Center
1300 W.T. Harris Boulevard
Charlotte, North Carolina 28262
Operated by
Electric Power Research Institute
3412 Hillview Avenue
Palo Alto, California 94304
EPRI Project Manager
John M. Jenco
Nuclear Maintenance Applications Center
Plant Technology
Nuclear Power Group
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PREFACE AND ACKNOWLEDGMENTS
Freeze sealing, or ice plugging as it is sometimes called, has proven over time
to be a relatively safe and cost-effective procedure for temporary piping
system isolation when performed by experienced technicians. This guide
consolidates information on the freeze sealing process. The purpose of this
guide is to familiarize the reader with freeze sealing as a planning and project
management tool, as well as many of the most important considerations that
come into play during activity planning and performance.
This document is not intended to provide sufficient information to qualify an
inexperienced technician to plan or perform a freeze seal in a critical location.
NMAC recommends the use of this guide as a primer or reference, and
suggests that freeze sealing in potentially critical applications be attempted
only by qualified and experienced personnel.
Preparation of this document owes much to many people. NMAC would like
to take this opportunity to thank all those who provided guidance or input,
and especially the following individuals for their contributions to improve
the quality of this document.
Steve Hunt, Dominion Engineering, Inc., Mclean, VA., for his assistance in
developing the piping stress/strain equations presented in Chapter 3.
George Howard, Freeze Technology International, Inc., Houston, TX., for the
provision of industry experience information and troubleshooting tips, as well
as general guidance on the art of safely conducting freeze seal operations.
Philippe Pons, Electricite de France, Paris, France, for his thoughtful review of
the original document and suggestions for particular areas of improvement.
NMAC Tech Note iii

CONTENTS
1.0 INTRODUCTION ......................................................................................... 1

1.1 Historical Background ......................................................................... 1
1.2 Equipment and Materials .................................................................... 3
1.2.1 Refrigerants ............................................................................. 3
1.2.2 Equipment ................................................................................ 5
2.0 FREEZE SEAL PLANNING CONSIDERATIONS..................................... 13

2.1 Understanding the Process .............................................................. 16
2.2 Precautions ....................................................................................... 16
2.3 Freeze Seal Process Limitations ...................................................... 17
2.3.1 Size Limitations ...................................................................... 17
2.3.2 Pressure Limitations .............................................................. 17
2.3.3 Temperature Limitations ......................................................... 17
2.4 Pipe Preparation ............................................................................... 18
2.5 Process Flow .................................................................................... 18
2.6 Effects of Hydrostatic Pressure on Plug Formation .......................... 18
2.7 Use of Freeze Seals to Permit Hydrotesting ..................................... 18
2.8 Contingency Plans ............................................................................ 19
2.9 Fire Protection System Maintenance ................................................ 19
3.0 EFFECTS ON PIPING AND MATERIALS ................................................ 21

3.1 Mechanical Properties Versus Temperature ..................................... 21
3.2 Fracture Toughness Versus Temperature .......................................... 24
3.3 Ferritic Materials ............................................................................... 26
3.4 Austenitic Materials ........................................................................... 26
3.5 Pressure Rise in a Closed Pipe ........................................................ 27
NMAC Tech Note v

3.6 Unknown or Uncontrolled Loads ....................................................... 30

3.6.1 Built-In Longitudinal Stress .................................................... 30
3.6.2 Stresses Arising from Handling .............................................. 30
3.6.3 Impact Loads ......................................................................... 30
3.7 Defects .............................................................................................. 31
3.7.1 Criterion for Acceptance/Rejection of Defects ....................... 31
3.7.2 Kinds of Defects ..................................................................... 31
3.7.3 Defects That Should Be Excluded Automatically ................... 32
3.8 Corrosion Pit Size Criterion .............................................................. 32
3.8.1 Application of the Criterion ..................................................... 35
4.0 PERFORMING A FREEZE SEAL ............................................................. 37

4.1 Location Selection ............................................................................ 37
4.1.1 Seal Considerations on Welds ............................................... 38
4.2 Freeze Seal Method Selection .......................................................... 38
4.3 System Preparation .......................................................................... 39
4.4 Pipe Restraints and Limits ................................................................ 41
4.5 Staging Equipment ........................................................................... 41
4.6 Insulation Removal ........................................................................... 41
4.7 Preliminary Inspection ...................................................................... 42
4.7.1 Visual Examination ................................................................ 42
4.7.2 Liquid Penetrant ..................................................................... 42
4.7.3 Ultrasonic Examination .......................................................... 43
4.7.4 Magnetic Particle Inspection .................................................. 43
4.8 Equipment Installation ...................................................................... 43
4.9 Initiating the Freeze Seal .................................................................. 44
4.10 Maintaining the Freeze Seal ............................................................. 45
4.11 Removing the Freeze Seal ................................................................ 45
5.0 TROUBLESHOOTING ISSUES ................................................................ 47

Problems Associated with Freeze Sealing ................................................ 47
Flow in the Line ................................................................................. 48
Vibration of the Pipe ......................................................................... 48
Turbulence ........................................................................................ 48
Heat ............................................................................................... 48
Contamination ................................................................................... 48
Lined Pipe ......................................................................................... 49
Air or Gas .......................................................................................... 49
Pressure ........................................................................................... 49
Convection ........................................................................................ 49
APPENDIX A: INDUSTRY EXPERIENCE ......................................................... 51
APPENDIX B: REFERENCES AND BIBLIOGRAPHY ..................................... 57

References ................................................................................................ 57
Bibliography ............................................................................................... 57
vi NMAC Tech Note

LIST OF FIGURES
Figure 1 CO2 Pipe Boat ................................................................................ 5
Figure 2 Typical Liquid Nitrogen Freeze Jacket ............................................ 6
Figure 3 Prefabricated Copper Freeze Jacket .............................................. 7
Figure 4 Sample Pipe Jacket Flow Path and Configuration .......................... 8
Figure 5 Liquid Nitrogen Gas-Pressured Freeze Seal Arrangement ............ 9
Figure 6 Coil Arrangement for 1/2-Inch (1.27 cm) Pipe for Freon
Freeze Sealing Method ................................................................. 10
Figure 7 Coil Arrangement for 1- to 4-Inch (2.54- to 10.17-cm) Pipe for

Freon Freeze Sealing Method ...................................................... 11
Figure 8 Yield Strengths of Metals at Low Temperatures ........................... 22
Figure 9 Ultimate Tensile Strengths of Solids at Low Temperatures ........... 23
Figure 10 Generic PlotTemperature Dependence of the Fracture

Toughness Parameter ................................................................... 25
Figure 11 Water Temperature and Flow Rates at Which Ice Plugs

Can Be Formed Using CO2 ...................................................................................................... 40
NMAC Tech Note vii

LIST OF TABLES
Table 1 Maximum Flow through Pipe Freeze Sealed in Tests ....................... 40
Table 2 Freeze Sealing Applications ............................................................. 52
NMAC Tech Note ix

1
INTRODUCTION
Freeze sealing refers to the process of applying an external refrigerant to a

point in a process piping system in order to cause the formation of a solid
internal plug from the frozen process fluid contained in the pipe. Because the
process fluid in question is commonly water or some mixture thereof, this
process is also sometimes referred to as ice plugging.
Freeze sealing is most often used to isolate a section of a piping system where
no other ready means of isolation, such as valving, is available. In many
cases, freeze sealing is performed specifically to perform maintenance or
repairs to a system isolation valve. Freeze sealing can also be used to isolate a
section of a piping system for hydrostatic testing. Three routine applications
for freeze sealing at nuclear power plants are to:
Enhance maintenance capabilities during shutdown or outage periods
Provide blocking in lines where valves or stops are not placed
Eliminate the necessity of taking a full system out of service during plant
operation, which might cause a limiting condition for operation
The earliest recorded patents for freeze sealing technology date back to 1904,
1.1 Historical
Background but the widespread use of freeze sealing for repair or modification work
began with the U.S. Navy during the 1940s. The Navys technical manual,
describing the methods and uses of freeze sealing, has been the classic
reference for years. It has often been the only source for decisions made
regarding freeze sealing.
NMAC Tech Note 1

A popular myth was that no pipe larger than 4 inches (10 cm) can be frozen
successfully. Using modern technology, operators have successfully frozen
lines as large as 36 inches (90 cm) in power plants and up to 48 inches (120
cm) in other industries, with no apparent problems. Similarly, many techni-
cians and maintenance personnel believe that freeze sealing cannot be
performed on carbon steel piping because of the brittle characteristics it
adopts at low temperatures. While it is true that carbon steel pipe does
become brittle at low temperatures, large carbon steel piping has been
successfully frozen with the use of liquid nitrogen (LN2) at temperatures as
low as -320F (-195C).
The transfer of freeze sealing technology to the nuclear power industry was a
logical outgrowth of the increasing role that former Navy personnel began to
play in the field. The first recorded uses of freeze sealing technology by the
U.S. nuclear power industry were in 1978. However, the Canadian nuclear
power industry was using freeze sealing technology as early as 1968.
As freeze sealing has become more accepted by industry, the methods used
have also evolved. Carbon dioxide (CO2), refrigerants such as freon and
liquid nitrogen, and other refrigerated mixtures have been used effectively
on small diameter (less than 4 inch [10 cm]) pipe. Today, liquid nitrogen is
often the most effective sealing refrigerant. Its extremely low temperature
permits more rapid freezing of the process fluid, particularly if some level of
process flow remains.
The basic method for freeze sealing can be classified based on the type of
operation or type of refrigerant used. Types of operation include:
Manual feeding of refrigerant
Remote manual control of the freeze seal process
Remote automatic freeze seal method
Types of refrigerants commonly used include:
Liquid nitrogen
Dry ice (CO2)
Freon
A mixture of any of the above refrigerants with alcohol or glycol
Some freeze sealing methods use mixtures of the primary refrigerants along
with alcohol or glycol. In these cases, use the precautions for the most severe
component of the mixture or, preferably, precautions for all components used
if they do not conflict.
2 NMAC Tech Note

The following sections describe commonly used freeze sealing refrigerants

1.2 Equipment and
Materials and related materials.
1.2.1 Refrigerants
Evaluate using any type of refrigerant on the basis of:
Location of the freeze plug
Flow in the pipe at the freeze point
Acquisition of the particular refrigerant
Size of the pipe to be frozen
Type of pipe
Duration of the work to be done after the plug is formed
Temperatures of the contents
Pressure in the pipe
Temperature of the surrounding area
Evaluate the advantages of one type of refrigerant or one type of freeze
plugging system over another based on:
Availability of equipment
Qualifications of freeze sealing personnel
Time available
Quantity of freezes
Location of the freezes
Sizes of pipe to be plugged
Liquid Nitrogen. Liquid nitrogen is the most commonly used refrigerant for
freeze sealing applications and is used in virtually all applications for pipe
diameters over approximately 4 inches (10 cm). It is available from com-
pressed gas vendors and is generally provided in various size Dewar flasks.
Larger volumes of liquid nitrogen can also be obtained in tube trailers to
support large diameter freeze seals, multiple freeze seals, or for applications
where the potential need might exist to maintain the freeze seal for some
extended period of time. The operative temperature of liquid nitrogen is
approximately -320F (-195C).
WARNING! Due to the extremely low temperature of liquid nitrogen, work

planners and technicians must thoroughly understand its properties and
its potential effect upon all equipment and materials with which it will come
in contact during use. Improper application or use of improper equipment
and materials with liquid nitrogen can result in equipment or material
failure, serious personal injury, or death.
NMAC Tech Note 3

Carbon Dioxide. Liquid carbon dioxide is available in cylinders and some-

times available at plant sites in bulk storage tanks for displacing hydrogen
from generators and for fire protection. The liquid is not commonly used for
freeze sealing but can be effectively used to freeze seal a pipe with a properly
designed pipe jacket. Liquid carbon dioxide, when expanded into a freeze
sealing jacket, solidifies as dry ice. The information for dry ice can be applied
to liquid CO2. Note that the liquid CO2 cylinders used for freeze sealing
should be of the siphon type so that they can be used in the upright position.
The operative temperature of carbon dioxide is approximately -109F (-78C).
Solid carbon dioxide (dry ice) can also be used for freeze sealing. When
broken up in small pieces and mixed with a fluid, such as ethylene glycol
(that is, antifreeze) or isopropyl alcohol, it absorbs heat well enough to be
used as a freeze seal refrigerant.
Freon. Freon is a commercially available refrigerant. It has been used to form
freeze seals in pipes up to 2 inches (5 cm) in diameter. Two types of commer-
cially available freon (freon R-12 or freon R-22) have been used for refrigera-
tion equipment. The choice of freon depends on the flexible hoses, couplings,
and other items used for the freeze sealing application. Use only hoses and
connectors approved for use with the freon selected. Evaluate the effect of
chlorides on the pipe metal and base the use of freon on stainless steel pipes
on this evaluation.
Note: Technicians who handle freon must be trained and licensed

according to the requirements of 40 CFR, Part 82, Subpart F.
Alcohol. Isopropyl alcohol is one of several media usable as a temperature
moderator and conductor with carbon dioxide, liquid nitrogen, or freon. It
provides thermal conductivity between dry ice (solid carbon dioxide) and
the pipe while inside the seal boat or jacket. Thermal conductivity between
dry ice and the pipe metal is very poor without some medium other than air,
which is a poor conductor. The freezing point of isopropyl alcohol is about -
128F (-89C), well below the operative temperature for carbon dioxide.
Ethylene Glycol. Commercial antifreeze or ethylene glycol can be used to
increase thermal conductivity for pipes surrounded with carbon dioxide in
the form of dry ice. Antifreeze can also be used as a temperature moderator
by using a mixture of 3040% antifreeze by volume with water. This mixture
has a freezing point of about -40F (-40C).
You can achieve a fairly constant temperature for the freeze sealing process
by premixing antifreeze with the refrigerant and then adding antifreeze or
refrigerant as required. Then pour this mixture into the boat or jacket sur-
rounding the pipe. Specifics of the freezing temperatures of ethylene glycol
and water mixtures are generally furnished on the containers. You can vary
the freezing temperatures by adjusting the mixtures. Note that the refrigerant
will boil off, leaving just the ethylene glycol solution. Remove some of this
solution to make room for the new refrigerant mixture.
4 NMAC Tech Note

This process can use either carbon dioxide or liquid nitrogen as the refriger-
ant in conjunction with moderators, such as antifreeze or ethylene glycol.
Evaluate the use of antifreeze and mixtures of other refrigerants also based
on the corrosive properties of the mixture on the pipe material and freeze
sealing equipment. Also, develop proper precautions and special plans to
handle any spills and cleanup.
1.2.2 Equipment
Oxygen Monitors. Oxygen monitors are hand-held devices that measure
oxygen depletion in the air. They are normally dual-function monitors that
can also detect the presence of combustible gases in the air. Oxygen monitors
can provide remote or local readings. Advanced oxygen monitors have
ceramitized gas sensing elements with no moving pans. Set a continuous
oxygen monitor with an alarm to give an audible signal whenever oxygen
concentrations in the working environment drop below 20%.
Pipe Boats. Pipe boats are built like pipe jackets except that the jacket tops are
open. Thus, a pipe boat is more like a trough or sleeve (see Figure 1). A solid
refrigerant (like crushed CO2) is placed into the trough and packed into the
pipe portion where the freeze seal is to take effect. The advantages of pipe
boats are easy construction and installation. They do not require elaborate
piping, fitting, or hookups. Also, highly skilled operators are not needed to
maintain the refrigerant system. The disadvantage is that it takes a long time
to form a reliable seal due to poor heat transfer between the solid refrigerant
(for example, crushed CO2) and the pipe.
Pipe Boat
Pipe
Figure 1
CO2 Pipe Boat
NMAC Tech Note 5

Pipe JacketsLiquid Nitrogen. The pipe jacket required to hold liquid nitrogen
should have a configuration similar to the one shown in Figure 2. It should
be made of low-temperature polystyrene with a density of 1.8 to 2.2 1b/ft3
and a thermal conductivity of 0.24 Btu/hr/ft2 at 40F (5C). Seal the joints of
the pipe jacket with a heavy mastic. Use worm-drive hose clamps to hold the
jacket halves together. Refer to Figure 3 for prefabricated copper freeze jacket
sizes available based on nominal pipe sizes from 1/2 inch (1.25 cm) to 4
inches (10 cm). Refer to Figure 4 for sample pipe jacket flow path and piping
configurations. Refer to Figure 5 for a diagram of a liquid nitrogen gas
pressured flask or Dewar connected to a freeze seal jacket. When the flask or
Dewar is connected to multiple jackets as shown in the figure, each freeze
jacket nitrogen flow is controlled independently.
Gas Vent Thermocouple Gas Vent
Liquid
Nitrogen
Supply
Liquid
Nitrogen
Supply
Figure 2
Typical Liquid Nitrogen Freeze Jacket
6 NMAC Tech Note

F
3-A
C C
G G 45
Radius B
A
E 45
D
3-A
Elevation-Assembled Jacket End View 3-A
Notes:
Template Hole Size 1. Jacket halves should be
to Suit Plug Cap 4 cleaned after assembly.
2. Jackets should be installed
on the proper size pipe,
hydrostatically tested to 110
psi using clean fresh water
and to 75 psi using liquid
nitrogen. No leaks are
allowed. Provide adequate
vapor space and
pressure relief.
3. Inner shell 1 should be
formed from tubing of
Half-Jacket the size shown in the IPS
Exploded View column in the Table
of Dimensions.
Table of Dimensions (All Figures in Inches)

Dimension IPS A B C D E F G
1/2 0.840 3/8 1-1/4 9 0.65 1/8 2
Jacket
for 3/4 1.050 3/8 1-1/4 9 0.65 1/8 2
1 1.315 3/8 1-1/4 9 0.65 1/8 2
Long 1-1/4 1.660 3/8 1-1/4 9 0.65 1/8 2
Jacket 1-1/2 1.900 3/8 1-1/4 9 0.65 1/8 2-1/2
2 2.375 3/8 1-1/4 9 0.65 1/8 3
2-1/2 2.875 3/8 1-1/4 9 0.65 1/8 3
3 3.500 3/8 1-1/4 10 0.65 1/8 4
4 4.500 3/8 1-1/4 12 0.65 1/8 5
1/2 0.840 3/8 1-1/4 6 0.65 1/8 2
Jacket
for 3/4 1.050 3/8 1-1/4 6 0.65 1/8 2
Short 1 1.315 3/8 1-1/4 6 0.65 1/8 2
Jacket 1-1/4 1.660 3/8 1-1/4 6 0.65 1/8 2
1-1/2 1.900 3/8 1-1/4 6 0.65 1/8 2-1/2
2 2.375 3/8 1-1/4 6 0.65 1/8 3
Figure 3
Prefabricated Copper Freeze Jacket
NMAC Tech Note 7

Liquid
Nitrogen
Supply
Vent Above Funnel

3/4-Inch (1.91-cm) Tubing Funnel
Funnel
60-Inch (152.50-cm)
Maximum Main Jacket
Location of Repair
Backup
Jacket
Temperature
Recorder
Minimum of Discharge/Control
30-Inch (76.2-cm) Nominal
Pipe Diameter
Note: Thermocouple points should be located as shown above

(i.e., 1 through 8) when two or more jackets are in series.
Figure 4
Sample Pipe Jacket Flow Path and Configuration
8 NMAC Tech Note

Quick Disconnect
Transfer Tube Assembly
Nitrogen Supply
010 psi (0.7 bar)
Ball
Valve
Jacket
Vent
Valves
Insulated Liquid
Nitrogen
Transfer Line
Liquid Nitrogen Inlet

(on bottom)
Freeze Laboratory-Type
Jacket Dewar Flask
To Test
Insulation Connection
Readout
Equipment
Pipe Line
to be Isolated
To Other
Freeze Jackets
Thermocouples
Figure 5
Liquid Nitrogen Gas-Pressured Freeze Seal Arrangement
Pipe JacketsCarbon Dioxide. Pipe jackets for holding carbon dioxide are
similar to those used for holding nitrogen, except that the tops have a large
opening to facilitate manual placement of dry ice, either ground or broken up
into small pieces and mixed with ethylene glycol or isopropyl alcohol. Figure
1 shows a typical configuration.
Freon Pipe Wrap Compressor Systems. Freon seals using a compressor-driven,
closed-loop system (that is, a commercial refrigerator unit) are very depend-
able and good for long-term seals. A commercial refrigeration unit consists of
a skid with the proper size condenser, dryer, expansion valve, built-in
vacuum pump, pressure gauges, temperature indicators, refrigeration hoses,
and copper refrigeration tubing. When backed up by a second compressor
system and two sets of coils and placed on two independent power supplies,
commercial refrigeration units become extremely dependable. The commer-
cial supplier of the refrigerant system must provide properly calibrated
instrumentation to monitor the function of the system in operation. These
systems require operating personnel who understand the equipment and the
refrigeration cycle.
NMAC Tech Note 9

Freon Pipe Wrap. Figures 6 and 7 show copper coil arrangements that have
been successfully used as freon pipe wraps in the freeze seal application.
Fully annealed tubing should be used because it conforms easily to the
piping. Three sixteenth copper tubing is used for freeze sealing pipes that are
1/2 inch (1.25 cm) or smaller. The 1/4 inch (.625 cm) copper tubing can be
wound around pipes larger than 1/2 inch (1.25 cm).
Copper Cloth Thermal Bulb Strapped

to Suction Line
Thermocouple
3/16-Inch (.48-cm) OD x Suction

0.030-Inch (.08-cm) 3/16-Inch (.48-cm) x
Wall Copper Tubing 6/16-Inch (1.0-cm) x
1/4-Inch (.64-cm) OD Tee Expansion
Valve
Supply
Figure 6
Coil Arrangement for 1/2-Inch (1.27-cm) Pipe for Freon Freeze Sealing Method
10 NMAC Tech Note

Copper Cloth
Thermal Bulb
Strapped to
Suction Line
Suction
Thermocouple
1/4-Inch (.64-cm) OD x
1- to 4-Inch 0.030-Inch (.08-cm)
(2.54- to 10.17-cm) Wall Copper
Pipe Tubing
Expansion
Valve
Supply
Figure 7
Coil Arrangement for 1- to 4-Inch (2.54- to 10.17-cm) Pipe for
Freon Freeze Sealing Method
NMAC Tech Note 11

2
FREEZE SEAL PLANNING
CONSIDERATIONS
Use of freeze seals can be problematic. You must carefully observe the limits
and precautions because some of the associated hazards are subtle in presen-
tation. There are at least three known fracture failures of piping mentioned in
the literature. Several deaths have been attributed to freeze sealing, resulting
from asphyxiation, not plug or pipe failure. In each case, these fatalities were
preventable, and thus serve to emphasize the care that must be taken to
follow established procedures and safety practices.
The first step is to examine the original pipe design and the as-built configu-
ration with respect to supports and their placement.
CAUTION: Supports and/or restraints must often be added during freeze

sealing, and existing restraints must be relaxed or monitored carefully
during cooling or restoration periods to minimize external stresses upon
the pipe.
From these design and as-built configurations, select an optimum location .
Items to consider for the physical placement of the plug include:
Piping vents and drains. A vent is necessary to prevent an unwanted
increase in internal pressure as the plug forms, between the plug and
another fixed blocking point in the line, for example, second ice plug,
valve, or blind flange. A drain is necessary to estimate plug formation
time by monitoring process flow through the ice plug as it forms within
NMAC Tech Note 13

the pipe. A cessation of process flow indicates that the plug has formed
sufficiently to close off process flow and is now growing primarily
axially within the pipe.
Weld location. Do not locate a freeze seal over the top of a weld, due to the
potential damage that might occur at the weld location.
The area upstream of an elbow. If ice plug should fail in-service, the pres-
ence of a downstream elbow in the piping system prevents unwanted
plug travel beyond that point.
Horizontal pipe runs. Horizontal pipe runs are less susceptible to convec-
tive currents in the process fluid, and it is therefore easier to establish an
ice plug in them.
Once a location has been determined, there are other considerations to
evaluate for the freeze plug . As before, analyze the pipe design, along with
the limitations of the freeze seal system under consideration. For this activity,
consider these items:
Pipe material
Pipe size
Line pressure
Flow in the piping to be selected
Maximum possible pressure differential across the plug
Pressure relief in the piping
Length of the plug
Spacing between seals, between a seal and fittings, valves, weld, etc.
Freeze methods available
Freeze time
Thaw time
Length of time the plug must be held
These items interact, and the selection of the method and refrigerant depends
on your analysis of these and other factors.
Personnel safety and precautions are important. Adhere to established
procedures and safeguards. Personnel must not forget that, in many cases,
they are dealing with temperatures far below any they have previously
encountered. Use an oxygen monitor with a low-oxygen sensor alarm.
Ensure that adequate ventilation is available, because the lack of ventilation
has allegedly caused three deaths in freeze sealing operations. Other safety
precautions include the preparation of contingency plans, such as:
14 NMAC Tech Note

Area evacuation planto protect the safety of freeze seal technicians and
other plant personnel
Action plan for plant equipment protectionto ensure that plant equipment
and systems will be protected in the event of a freeze plug failure
Medical support alertto provide briefing information for medical support
personnel who respond to cryogenic burns, asphyxia, or other freeze
seal-related conditions
Action plan for the freeze seal techniciansto ensure that the freeze seal
activity will continue without incident in the event of the loss of one or
more freeze seal technicians
Another aspect of safety is to use approved tools and equipment for the
freeze applications. Make certain that all instruments and monitors are
properly calibrated.
If the work is being performed in the radiation work area, obtain health
physics support and input for contingency planning.
Establish the plug acceptance criteria. Factors to be considered in determin-
ing plug effectiveness include process temperature and differential pressure
monitoring, which should be clearly and concisely defined. Once established,
enforce these acceptance criteria strictly. Most of the problems encountered
with freeze sealing come from a desire to begin work before the seal is fully
formed. The key question to ask in determining the plug acceptance criteria
is, When can I safely work there?
Plug maintenance is another area to be considered. Effective maintenance
requires continuous monitoring of the plug, in terms of both temperature and
differential pressure if possible (but at least temperature). Other requirements
are an adequate coolant supply and the availability of back-up blocking
systems.
WARNING!: Plug maintenance is extremely important. There are no

partial plug failures. When a plug begins to go, it cannot be restored.
NOTE: Releasing the plug is the last step of the operation. It must be done
properly with consideration given to downstream effects. If possible, refill
drained lines to prevent water hammer, and try to thaw the plug on one
side to establish minimum flow without losing the entire plug downstream
where it might hang up or damage valves.
Plants should consider surveying their systems to determine locations where
freeze sealing might be useful as a maintenance or operational tool.
Electricit de France has performed such surveys and determined that there
are some 70 primary side locations where freeze seal applications might be
useful. After locations are determined, preapproved procedures can be
prepared for contingency purposes.
NMAC Tech Note 15

As previously mentioned, the freeze sealing process consists of placing a

2.1 Understanding
the Process refrigerant around a pipe and removing heat until the medium in the pipe
(usually water or some mixture of water) freezes and provides a plug or seal
against further fluid movement through the pipe.
It is generally accepted that the ice plug forms in concentric rings from the
pipe wall towards the center of the pipe until a plug is formed. It then
proceeds axially in both directions to the limits of the pipe jacket. Under
normal humidity conditions, a frost band 12 inches (2.55 cm) wide forms
around the end of the seal.
CAUTION: Do not use the frost band by itself as an indicator that the seal
is fully formed.
NOTE: If the ambient conditions are unusually dry, placing a small amount
of water on this area forms the frost band, indicating that portion of the
pipe that is below 32F (0 C).
Always rely on pipe metal temperatures to determine whether the seal has
been formed. Use downstream vents and drains to verify conditions. Frost
bands can form quickly on areas of empty or partially filled pipe. If the freeze
times are less than expected, it is likely that the pipe is empty or that voids
are present. In such cases, take precautions to verify the integrity of the seal
prior to using it for system isolation.
Be sure to follow this (partial) list of precautions:

2.2 Precautions
Provide adequate ventilation before starting the freeze sealing applica-
tion. Because many common refrigerants are heavier than air, ventilation
is most effective if configured to draw from the lowest point in the area.
Monitor air quality and oxygen concentrations continuously for person-
nel safety.
Use nonporous gloves, face shields, and protective clothing for handling
refrigerants and other equipment.
Ensure that the pipe is adequately supported and not subject to shocks or
impact forces.
Maintain proper recommended distances for the freeze seal areas and
other components.
Monitor the temperature and status of the freeze seal after it has formed.
Use only approved hoses and fittings for the selected refrigeration
system.
16 NMAC Tech Note

While proven effective as a piping system isolation methodology, freeze

2.3 Freeze Seal
Process Limitations sealing has some limitations in applicability that relate to pipe size, process
and ambient temperature, head pressure, and differential pressure across the
plug boundary. The following sections provide some guidance in each of
these areas.
2.3.1 Size Limitations

With regard to pipe size limitations, pipes up to 36 inches (90 cm) in diameter
have been successfully and economically freeze sealed in the utility industry.
Sufficient data are available from vendors on the time and refrigerant re-
quired, as well as the permissible pressure, flow, and temperature for pipes
28 inches (70 cm) or less.
Commercial freeze chambers are also available that can fit standard pipe
sizes from 1/2 to 48 inches (1.25120 cm) in diameter. Thus, pipe sizes up to
48 inches (120 cm) can be frozen using liquid nitrogen. Naturally, there is an
increase in the time and refrigerant required for larger size pipes. It is critical
for the maintenance engineer to evaluate the overall economics of freeze
sealing for larger size pipe versus draining the system and isolating it.
2.3.2 Pressure Limitations

With regard to pressure limitations, freeze seals have been attained where
system pressure was as high as 2244 psig (155 bar). Further, testing on a 3 1/2-
inch (8.75 cm) pipe where system pressure in the pipe was raised to 10,000 psi
(690 bar)the failure point for the pipe materialhas shown that although the
pipe yielded at a point away from the freeze seal, the freeze seal remained
intact. From the available data, it is known that plugs formed under additional
pressure are more resistant to any movement and flow in the pipe than plugs
formed under no pressure. Normal pressure limits for pipe sizes 1/2-inch
through 4 inches (1.2510 cm) are:
System pressure <400 psig (27.5 bar)
Differential pressure across the plug <400 psig (27.5 bar)
Thus, pressure limits on the freeze seal application are normally based on an
evaluation of the design limits of the pipe and the plugging system used. The
primary consideration is that means are provided to vent the pipe and relieve
the pressure buildup during the freeze sealing process. Be sure that no
section of the pipe being freeze sealed exceeds the design parameters for
pressure in that section and that a way is provided to bleed off this pressure.
2.3.3 Temperature Limitations

With respect to temperature, normal freeze sealing temperature limits speci-
fied in the literature are as follows:
Ambient condition < 110F (43C)
Fluid temperature < 225F (107C)
NMAC Tech Note 17

However, freeze seals have been performed at ambient temperatures above

110F (43C). If the temperature of the fluid (that is, water) in the piping is
much higher than the ambient temperature, reduce the fluid temperature in
the piping to as near the ambient temperature as possible before starting the
freeze sealing process.
Reduce the temperature and pressure of the pipe to be freeze sealed to as

2.4 Pipe Preparation
near the ambient conditions as possible. Make sure that the pipe section to be
freeze sealed is full of fluid. If possible, select a horizontal run of the pipe for
the freeze seal. Remove the insulation and clean the piping in the area where
the freeze seal will be made. Be sure to remove enough insulation, that is, at
least four pipe diameters more than the required length of the freeze jacket or
the evaporator. Cover the open ends of the unremoved insulation with
waterproof tape to keep it dry.
Freeze sealing experts agree that excessive process flow through the freeze
2.5 Process Flow
seal location is the single greatest factor in failing to achieve a successful ice
plug formation during a freeze sealing application. If possible, make certain
that all related valving is identified through a walk down inspection prior to
initiation of the freeze seal and that the valving is fully closed.
Observations have shown that freeze plugs formed without the recom-
2.6 Effects of
Hydrostatic Pressure mended pressure are of lower quality than those that are formed under
on Plug Formation pressure. If substantial differential pressure is to be applied to the seal after
formation, do not form the freeze seal without pressure.
The advantage of forming a freeze seal under pressure is that at higher
pressure the water is denser, which allows it to freeze quicker and form a
harder plug.
You can use freeze seals for hydrotesting partially completed systems if the
2.7 Use of Freeze
Seals to Permit pressure for the hydrotest is within the limits of the maximum allowable
Hydrotesting differential pressure across the freeze plug. Properly formed ice plugs easily
resist differential pressure equal to the nominal operating pressure of the
process pipe and do not develop leaks.
18 NMAC Tech Note

Formulate contingency plans before beginning freeze sealing applications in

2.8 Contingency
Plans case of freeze seal or refrigeration failures. Be sure to include in your contin-
gency plans:
Communication with operations
Identification of pumps and flow paths
Equipment shutdown plans
Personnel evacuation routes
Staging of the necessary equipment to handle a failure of the seal or
failure of the freeze seal apparatus
Actions to be taken in the event of work delays while the freeze seal is
being maintained
To handle spills, develop emergency plans that ensure flow will be caught
and directed toward a drain or tank. Give consideration to the possibility of
minimizing differential pressure across the freeze seal to reduce the flow, and
manually isolating the leak by blocking the pipe. Some types of equipment
that could be staged for use if problems develop with the seal are:
Jaws capable of crushing pipe
Mechanical stops
Plugs
Polyethylene bags
Clamps
Diversion devices
Make certain that on-site medical personnel are familiar with treatment
approaches for cryogenic burns and asphyxia.
Locate alternate sources for refrigerant supply, equipment, and expert techni-
cal assistance, in the event that something happens to your primary sources.
One method of ensuring seal integrity is to place two seals in series, thus
requiring a double failure before losing the seal. Take care to avoid captured
water problems between the seals, because the ice expansion between the
two seals can develop excessive pressure in the confined liquid.
Freeze seals are often used to isolate and perform maintenance on segments
2.9 Fire Protection
System Maintenance of the plant fire protection system without completely shutting it down.
However, be sure to develop an emergency response plan before the freeze
seal is applied.
NMAC Tech Note 19

3
EFFECTS ON PIPING AND MATERIALS
Previous studies have investigated the technical effects of the freeze sealing
process on the materials involved. These studies have improved the under-
standing of the stresses induced during freeze sealing, their magnitude, and
locations. Tests performed for these studies have produced data that show
that many early industry concerns regarding the potential impact of freeze
sealing on components were very conservative.
Testing [Flaman and Shah, 1984] has shown that samples with flaws that
were intentionally placed in the section of a pipe subjected to freezing and
expected to fail did not. Some of these flaws reduced the wall thickness of the
pipe by half and were designed to raise piping stress levels to a point that
would barely contain the maximum pressure at ambient temperatures. The
assumption was made that if the stress levels were raised to the failure point
at ambient temperatures, then the pipe would surely fail with the effect of the
transition caused by low temperature. Test results indicate that freeze sealing
areas with normal flaws may not be a serious problem if the flaws are ana-
lyzed properly. The strength of piping materials greatly increases as tempera-
ture decreases. This is an effect that was not fully considered in the early
analysis of failures at low temperatures.
The mechanical properties of metal at low temperatures are significantly

3.1 Mechanical
Properties Versus different from those same properties at room temperatures. Figure 8 shows
Temperature the yield strengths of various metals at low temperatures. The yield strength
of most metals increases with a decrease in the temperature.
NMAC Tech Note 21

Temperature, F and C
-400F -300F -200F -100F 0F

(-240C) (-184C) (-129C) (-73C) (-18C)
200
Invar 36
12 to 15%
Cold Drawn
150
K-monel
45% Cold 9% Nickel Steel
Drawn
Yield Strength, ksi
100 Be-Cu Cold

Drawn
1/2 Hard
304 SS Brass 70-30

Annealed Cu-OFHC 3/4 Hard
Cold Drawn
50
AL 6061-T6 Inconel
10% Cold
Drawn
0 100 200 300 400
Temperature, R
Figure 8
Yield Strengths of Metals at Low Temperatures
Figure 9 shows the ultimate tensile strengths of various materials versus

temperature under cryogenic conditions. For most metals, the tensile
strength increases with lowering of the temperature. In general, ductility also
decreases with decreasing temperature, although this trend is more pro-
nounced for ferritic materials (carbon and low-alloy steel) than for austenitic
22 NMAC Tech Note

materials (stainless steels). A decrease in ductility reduces the materials

ability to plastically deform under loads exceeding the yield strength. Al-
though the overall strength of a material might increase at cryogenic tem-
peratures, the material may be susceptible to rapid crack propagation (brittle
cleavage fracture) if stresses induced in the material approach the yield
strength.
-400F -300F -200F -100F 0F

(-240C) (-184C) (-129C) (-73C) (-18C)
250
K-monel
45% Cold 304 SS
Drawn Annealed
200
Ti-6 AL-4V
Annealed
Ultimate Tensile Strength, ksi
150 9% Nickel
Inconel
10% Cold
Drawn
100
Cu-OFHC Brass 70-30

Cold Drawn 3/4 Hard
50
AL 6061-T6
0 100 200 300 400
Temperature, R
Figure 9
Ultimate Tensile Strengths of Solids at Low Temperatures
NMAC Tech Note 23

During the freeze sealing process, stresses are thermally induced in the
material due to temperature differentials in the metal associated with pipe
cooldown and heatup. Generally, it is observed that the maximum pipe
stresses are tensile and always occur close to the boundary of the jacket
during ice plug formation. Stresses are higher at the edge of the ice plug than
in the areas within the jacket or downstream of the plug. Usually, these
thermally induced stresses should not be a concern regarding structural
integrity of the pipe section; however, the stresses induced during the pro-
cess are a function of pipe geometry, that is, discontinuities in the pipe due to
diameter reductions, fittings, etc. Such geometric discontinuities can increase
the stresses induced in the material during the freeze sealing process. If a
freeze sealing process is to be performed in a location that contains a geomet-
ric discontinuity, the impact of the discontinuity on the thermally induced
stresses should be considered prior to the freeze sealing operation.
Although the materials mechanical properties change as a function of freeze
sealing temperature, an important conclusion from previous studies is that the
low-temperature cycle should not have any permanent effect on the steel
properties that would alter performance when the material is returned to
normal temperatures. This does not mean that stresses at low temperatures do
not cause damage. Be careful to avoid any potential structural overload of the
pipe section to prevent permanent damage from occurring to the material.
In addition to strength behavior under cryogenic temperatures, the potential
impact of freeze sealing on other material properties should be considered.
These thermal expansion characteristics (related to the amount of stress
thermally induced in the material) and the behavior of flaws at low tempera-
tures are prime considerations for the freeze seal application.
In general, carbon steels undergo a ductile-brittle transition as a function of

3.2 Fracture
Toughness Versus temperature. At a temperature above the transition region, carbon steels
Temperature exhibit increased impact toughness and resistance to crack propagation.
Material fracture above the transition temperature generally is ductile in
nature. Below the transition temperature, the impact toughness (and resis-
tance to crack propagation) can markedly decrease, increasing the likelihood
of brittle fracture. Evaluate the effects of low temperatures before choosing a
freeze sealing method. For example, carbon and low-alloy steel pipes are
susceptible to brittle failure (that is, exhibit a ductile-brittle transition) at
temperatures below -40F (-40C) and, therefore, should not be subjected to
impact loading during the freeze sealing application. During repair work,
avoid external static or impact forces exerted on the frozen pipe.
Fracture toughness is a material property (expressed as a number with units
of ksi in or MPa m ), reflecting a given materials tolerance to flaws when
stressed. A low fracture toughness number indicates low flaw tolerance. With
knowledge of the material fracture toughness, the stress level at which
unstable crack propagation might occur can be determined. Conversely, for a
24 NMAC Tech Note

given stress level, the defect size that will be predicted to initiate unstable
crack growth can be determined. Figure 10 illustrates the generic temperature
dependence of the fracture toughness parameter. Therefore, at low tempera-
tures, the pipe material may be more susceptible to failure due to a combina-
tion of stresses and material flaws.
150
125
100
Klc (ksi in)
75
50
25
-300F -200F -100F 0F 100F 200F

-184C -129C -73C -18C 38C 93C
Figure 10
Generic PlotTemperature Dependence of the Fracture
Toughness Parameter
NMAC Tech Note 25

Ferritic materials (that is, carbon and low-alloy steels) exhibit a ductile-brittle
3.3 Ferritic Materials
transition as described in Section 3.2. The transition temperature for carbon
steel is typically less than -40F (-40C); however, transition temperatures for
carbon steel can vary from -100F (-73C) to +200F (93C), depending on the
material composition and heat treatment. Manufacturers of carbon steel
piping should be able to supply data on transition temperatures. Toughness
data can be obtained from Certified Mill Test Reports (CMTRs).
Some organizations limit freeze sealing temperatures of carbon steel pipes to
not lower than -40F (-40C) by using freon refrigerant systems (because a
-40F (-40C) transition temperature is above the temperatures experienced
with the use of liquid nitrogen and carbon dioxide freeze sealing). Because
freon refrigeration systems cannot function at temperatures below -40F
(-40C), use of these systems prevents brittle transition of carbon steels
during freeze sealing. However, larger pipe diameters most likely preclude
the use of anything other than liquid nitrogen to adequately freeze the liquid
in the pipe and maintain plug integrity during downstream maintenance.
Freeze sealing of ferritic materials at temperatures much lower than -40F
(-40C) can be performed if the following precautions are taken:
Move or remove pipe supports near the freeze seal area so that the pipe
has free contraction capability at the freeze seal.
Install adequate temporary supports to make up for the removal of the
permanent support during freeze seal operation.
Be sure that the pipe is not subject to any impact forces during the entire
freeze sealing and thawing process.
Other successful methods of freeze sealing of ferritic materials include using
mixtures of alcohol or ethylene glycol and carbon dioxide or liquid nitrogen.
These methods rely on temperature monitoring and the addition of alcohol
or glycol to prevent temperatures from going below -40F (-40C). It is very
difficult to control and monitor all contact points for minimum temperature.
As described above, tests have shown that freeze sealing below the transition
temperature does not change the crystal structure or characteristics of ferritic
material. However, strength characteristics do change (that is, higher yield,
lower elongation, lower toughness) while the material is below the transition
temperature. Exercise appropriate operational precautions as discussed.
Austenitic stainless steels are well suited for service at cryogenic tempera-
3.4 Austenitic
Materials tures. They generally do not exhibit transition temperature behavior and,
therefore, maintain excellent toughness and good ductility at very low
temperatures. In fact, austenitic stainless steels (for example, Type 304L) are
generally used for handling, storage, and transport of cryogenic liquids.
Although stainless steel generally has a very low transition temperature and
is not subject to brittle fracture during freeze sealing applications, good
26 NMAC Tech Note

engineering practice would dictate that similar precautions as those recom-

mended for carbon steel be taken during freeze sealing operations.
Wrought austenitic stainless steels can also undergo a martensitic transforma-
tion of the austenite phase at very low (cryogenic) temperatures. Extensive
literature reviews indicate that this transformation is primarily a function of
material composition and deformation (strain). Secondary factors include
temperature, rate of temperature change, amount of time at the temperature,
and material grain size. However, no information is presently available indicat-
ing the additional impact, if any, of a potential martensitic transformation at
cryogenic temperatures on the mechanical properties of stainless steel piping.
An international study is presently underway to investigate this phenom-
enon for nuclear piping applications. It is anticipated that this effort will
characterize the impact of freeze sealing (at cryogenic temperatures) on the
mechanical properties of stainless steel piping. Until results from this study
are available, it is recommended that the following parameters be recorded
during the freeze sealing application for future possible evaluation:
Material composition
Cooldown rate during freeze sealing application
Lowest temperature
Amount of time at the lowest temperature
Exposure of stainless steel to chlorine is a concern that should be addressed
due to the potential for stress corrosion cracking. The principle sources of
chlorides during freeze sealing applications are insulation and freon (if freon
is used as a refrigerant). The existing pipe insulation might contain some
chlorides that can leach out if the insulation gets wet. Be sure that existing
insulation is removed from the pipe area where the freeze seal will be ap-
plied. Also, check for freon leaks during the freeze sealing application when
freon is used, or simply avoid the use of freon as a refrigerant for freeze
sealing applications on stainless steel.
Pressure in a closed vessel full of liquid rises when the volume of the liquid is
3.5 Pressure Rise in
a Closed Pipe increased by adding liquid or the volume available is decreased (for example,
from expanding the liquid by heating without removing any fluid). The effect
of a volume change follows.
Purpose: The purpose of this calculation is to determine the pressure increase
in a capped pipe as a result of a freeze plug growing A inches into the pipe.
NMAC Tech Note 27

Model: The analysis model is as follows:
t
A
Ice Plug End Capped but Free to Expand Axially
Analyses: At equilibrium conditions, the increase in internal volume of the

pipe plus the decrease in volume of the water due to increasing internal
pressure must equal the decrease in volume produced by growth of the
freeze plug.
Vpipe Vwater = plugR2

From Roarks, Formulas for Stress and Strain, Fifth Edition, Table 29, Case 1c,
the changes in pipe radius and length as a function of the internal pressure.
PR2
R = 1
Et 2
PRL
L = (0.5 )
Et
From Lindeburgs, Engineer-in-Training Reference Manual, 8th Edition, Equa-
tion 14.34(a) the change in water volume as a function of internal pressure is,
PV
Vwater =
B
Where B is the bulk modulus 300,000 psi . (Note: The bulk modulus is
equal to 1/, where is the coefficient of compressibility.)
28 NMAC Tech Note

Making the simplifying assumption that the change in volume of the pipe is
the change in radius times the circumference times the length, plus the
volume change due to increase in axial length, results in the following
expression,
Vpipe = 2RRL + R2 L
Combining all of the expressions,
PR2 2 PRL PR2 L

2RL 1 + R ( 0.5 v) + = R2
Et 2 Et B
Cancelling out and R2 ,
2 PRL PRL PL
1 + ( 0.5 ) + =A
Et 2 Et B
Solving for P,
A
P =
2 RL RL L
(1 0.5 ) + (0.5 ) +
Et Et B
A/ L
=
R 1
(2.5 2 ) +
Et B
For the normal condition where Poissons ratio = 0.3, this reduces to the
expression,
A/ L
P =
1.90 R 1
+
Et B
Sample Calculation:
R = 6.375 inches
t = 0.250 inches
L = 100 feet = 1200 inches
B = 308,642 psi
E = 30x106 psi
= 1 inch
Using these parameters,
P = 172 psi
NMAC Tech Note 29

3.6.1 Built-In Longitudinal Stress

3.6 Unknown or
Uncontrolled Loads In a piping system, there can exist built-in longitudinal stresses arising from
the original construction or from subsequent settlement in the case of buried
pipelines. These can impose stresses as high as the ambient temperature
yield strength of the material. When the stress due to restraint is added to
these, yielding takes place. However, because the yield strength of the cold
region at the plug is well above the ambient temperature value, the yielding
occurs outside the plug region. The case of large longitudinal loads coupled
with restraint stresses is one of the few in which ice plug use might induce a
failure in a location other than at the ice plug.
Although you cannot readily tell beforehand when high built-in stresses are
present, the likelihood of failure is small unless a significant
circumferentially-oriented defect is present. You can greatly reduce the
chances of such a defect being present in the plug regions by not forming a
plug at a girth weld. If it is know or suspected that longitudinal stresses
might be high, it would be a good idea to radiograph the exposed girth
welds even though they are not located in the plug region.
3.6.2 Stresses Arising from Handling

In cases where ice plugs are used in maintenance of plant piping or a buried
pipeline, it is likely that a portion of the pipe will be removed. This can
involve release of stress when the pipe is cut and added bending stress as the
ends are handled by side booms or other equipment. One way to minimize
the effects of these handling stresses on the ice-plugged regions in a buried
pipeline is to excavate plug locations far enough away from the maintenance
area so that undisturbed backfill separates the ice plug trenches from the
maintenance trench. If this cannot be done, take care to minimize movement
of the pipe ends when a portion of the pipe is removed. In plant piping, be
sure to support the pipe adequately when cuts are made.
3.6.3 Impact Loads

The effect of impact loads on defects in the ice plug region could be disas-
trous. Therefore, prohibit any actions such as hammering on the pipe or
cropping the ends of the pipe for a distance of several pipe diameters from
the ice plugs while the pipe is cold.
Impact effects could also arise from pressure surges. As indicated previously,
however, the line must be under static conditions to use ice plugging. There-
fore, surges due to pumping or valve closure should not occur. In the case of
a hydrostatic test, test failures can produce significant surges. Because these
surges represent a sudden droprather than a risein pressure, they should
not cause defects in the ice plug region to fail.
30 NMAC Tech Note

Defects that might coincide with the ice plug region are of primary concern,
3.7 Defects
especially longitudinally-oriented defects because they are the ones that most
often produce pipeline ruptures. Circumferentially-oriented defects occur
most often in girth welds and can be avoided by not locating ice plugs at
girth welds. The behaviors of circumferential defects can, of course, be
described analytically, but a criteria for circumferential defects would be of
little use if you could not determine the longitudinal stress in the pipe.
3.7.1 Criterion for Acceptance/Rejection of Defects

Presented here is a criterion for judging whether to permit an ice plug to be
located in an area containing certain kinds and sizes of defects. Because it is
often difficult to predict the amount of longitudinal stress that is present, the
criterion is limited to longitudinally-oriented defects that are subjected to
stresses arising from internal pressure. Girth welds, which are the most likely
sources of circumferentially-oriented defects, and locations containing
circumferentially-oriented crack-like defects that are discovered in the body
of the pipe upon inspection should be automatically eliminated from consid-
eration.
3.7.2 Kinds of Defects

The kinds of defects most likely to be discovered are:
Mechanical damage
Gouges or scratches
Plain dents
Gouges and dents
External corrosion
Internal corrosion
Stress corrosion cracking
Fatigue cracks
Manufacturing defects (most prevalent in seam welds)
Toe cracks (submerged arc welding seams)
Penetrators (electric resistance welding seams)
Hook cracks (electric resistance welding seams)
To be able to evaluate a defect, you must first be able to find it. You can
evaluate external corrosion by visual inspection. You can also visually evalu-
ate gouges without dents or cracks of sufficiently small size if they are
NMAC Tech Note 31

ground down until the crack or tear no longer shows up in the dye penetrant
inspection. The limits on the size of such ground areas are discussed later
along with the limits of corrosion. The resulting smoothly contoured pits can
then be treated like corrosion.
3.7.3 Defects That Should Be Excluded Automatically

Exclude regions of pipe containing any of the following from consideration
as ice plug locations:
Girth welds
Fittings
Repair welds
Cracks
Pits that are too large to meet the corrosion criterion
Internal corrosion
Dents with or without gouges
Leaking defects
As is already well known to liquid pipeliners, regions containing cracks or
pits that are too large to meet the corrosion criterion, dents containing
gouges, internal corrosion, and leaks must be repaired or the pipe replaced
according to the Code of Federal Regulations, Title 49 Part 195. The only
requirement suggested here that is more restrictive than Part 195 is to not
permit plain dents in a ice plug region. All plain dents should be excluded
from ice plug regions because of the possibility that they might tend to pop
out during or after freezing under certain pressure conditions. Plastic flow,
such as that accompanying a dent popping out in carbon-manganese steels at
-320F (-196C), can lead to brittle fracture initiation at low levels of strain.
External corrosion pits, singly or in groups, gouges without dents, and small
3.8 Corrosion Pit
Size Criterion cracks that can be smoothly contoured by grinding and checked with dye
penetrant to see that all of the crack is eliminated can be accepted in an ice
plug region if they meet the following criterion which has been developed
through research sponsored by the Pipeline Research Committee of the
American Gas Association.
32 NMAC Tech Note

Because pits are relatively blunt defects, you can use this equation to predict
the remaining strength in the metal:
A
1 Mt 1
Ao
Mp = = Equation 1
hp 1
A
Ao
where:
A = Projected profile area of an array of pits
A0 = L x t
L = Length of the corroded area
t = Wall thickness
It is also possible to define a simpler approximate equation for MT in terms of
L and the pipe diameter, D, and t as follows:
0.8L
M = 1+
Dt
Solving Equation 1 for hp, you obtain
A
1 A
hp = o

1

A
Ao
M 1 ( )

To base the criterion on the simplest of measurements, a parabolic approxi-

mation of the actual profile area, A, of the pits is used. Hence, you can char-
acterize an array of pits by measuring only the quantities L and d, the maxi-
mum depth of the pits. Note that the area A of the parabola is 2Ld/3. Also,
note that d is always taken as the deepest measurable depth even though it
might or might not coincide with the center of the approximating parabola.
The approximate equation becomes
2d
1 3t
hp =
2d
1
3tM 1
NMAC Tech Note 33

The criterion is now defined such that the failure stress level of the defect
shall never be less than 100% of specified minimum yield strength (SMYS). In
addition, you can define flow stress, , conservatively as 1.1 SMYS. Thus
2d
1 3t
SMYS = 1.1SMYS
2d
1
3tM 1
2d
1
1.1 3t = 1
2d
1
3tM 1
Through arithmetic steps that are omitted here, you arrive at the criterion
that
L 1.12B Dt Equation 2
2
d

B= t 1
d
1.1 0.15
t
What this says is that any array of pits (or crack-free area that has been
smoothly contoured by grinding to remove an existing gouge or crack) of
length L and maximum depth d is acceptable as long as the L is less than or
equal to 1.12 B Dt , where B is based upon d/t. Note that two other
restrictions are imposed:
B cannot exceed 4; otherwise, a maximum value of 4 must be used in
Equation 2.
The criterion should not be used if d/t is less than or equal to .125 or
greater than .80.
The first restriction is necessary because the parabolic approximation tends
to break down for long, shallow flaws. The two limits on d/t are for the
following reasons. If d/t is less than or equal to 0.125 (that is, the defect
depth is less than or equal to 12.5% of the wall thickness), it is acceptable in
the pipeline industry regardless of the length of the defect. Secondly, if the
depth exceeds 80% of the wall thickness, it is so near to being a leak that the
criterion is of questionable validity.
34 NMAC Tech Note

3.8.1 Application of the Criterion

It is useful to consider why this criterion ought to be used in ice plug situa-
tions. Pipes are seldom completely free of defects. Yet, we know from experi-
ments that some defects can be tolerated. It unreasonable to demand that all
defects be eliminated when it is reasonably clear that sufficiently small, blunt,
pit-like defects pose no real hazard.
The criterion proposed is already widely accepted in the pipeline industry (it
is contained in the ASME B31.4 Code), and it has been shown to be quite
conservative. For operating pipelines or plant piping systems in which ice
plugs are to be used for maintenance in which the stress level will not exceed
72% of SMYS at any time, the criterion provides a considerable margin of
safety against failure.
The only case in which you might question the use of the criterion is that of
ice plug use in a hydrostatic test where the pressure level might exceed 100%
of SMYS. In this case, much of the margin of safety built into the criterion is
removed. In such a case, defects that meet the criterion could conceivably
fail. However, if you are willing to accept some risk of failure (an appreciable
risk of failure exists in a hydrostatic test anyway) and if personnel can be
absolutely excluded from the ice plug areas while the pipe is at pressure
levels exceeding 72% of SMYS, then the criterion might still prove useful. The
rationale for using the criterion even in this extreme case is based upon the
results of experiments, namely:
The region of the ice plug is either warm proof loaded when the plug is
formed at maximum pressure or the region of the ice plug is isolated
from stress increases as the pressure is increased above that at which the
plug was solidly frozen.
The flow stress at -320F (-196C) greatly exceeds the room temperature
flow stress on which the criterion is based.
The experiments themselves showed the criterion to be conservative.
NMAC Tech Note 35

4
PERFORMING A FREEZE SEAL
Choose the freeze seal area carefully so that it will not hinder the intended
4.1 Location
Selection maintenance activities. Provide enough room to cut the pipe or reinstall
components that are removed. Do not include any fittings or transition
between dissimilar metals in the freeze seal area. Place freeze seals in hori-
zontal runs of pipe rather than vertical runs, where possible, to avoid compli-
cations caused by convection currents in the process fluid. Freeze seals can be
made in vertical runs, but the convective flow and the resulting heat transfer
make the formation of a seal much more difficult. In vertical seals, it can be
necessary to place two or three seals in series to slow down the convective
flow enough to obtain a reliable seal.
If practical, locate the freeze seal area at least 24 inches (60 cm) away from the
heated sections of the pipe to reduce thermal stresses on the pipe and to
ensure that the heat does not melt the ice plug. When freeze plugs are used to
isolate a single pipe section, locate them at least 30 nominal pipe diameters
apart. Always apply freeze seals more than 20 pipe diameters from a compo-
nent or obstruction that completely blocks the flow of expansion water as the
ice plug forms, unless a vent path exists between the two freeze plugs or
between the freeze seal and the obstruction.
NOTE: The water trapped between two ice plugs or an ice plug and a block
in the piping is the main source of piping stresses. These stresses can
result in pipe failure. Do not allow water to trapped between two ice plugs
without a way to relieve the pressure upon final freezing.
NMAC Tech Note 37

4.1.1 Seal Considerations on Welds

Welds are potential locations for flaws and residual stress. Depending on the
location of a weld, a freeze seal in the pipe can induce tensile or compressive
stresses on it. Consider these stresses when selecting the freeze seal location.
There is no information available on the effects that freeze sealing or extreme
temperatures have on welds. However, for stainless steels, depending on the
material chemistry and the original fabrication process of the weld, the
material may potentially be sensitized (particularly if no post-weld heat
treatment was performed). Weld sensitization results in an increased precipi-
tation of metal carbides at the grain boundaries, which reduces the materials
resistance to intergranular stress corrosion cracking and intergranular frac-
ture in general.
Exercise care if a freeze sealing operation is to be performed at a stainless
steel weld location. A prior knowledge of the weld fabrication history would
possibly indicate if additional caution should be taken to ensure that no
impact or excessive loading is induced on the material during the freeze
sealing operation. In general, it is good engineering practice to place freeze
seals away from any welds in the pipe.
When welding or brazing is to be performed as a part of the maintenance on
the pipe being freeze sealed, maintain sufficient distance between the ther-
mal operation and the freeze seal. If practical, locate the freeze seal at least 24
inches (60 cm) away from the heated sections to minimize thermal stress and
ensure that the heat does not melt the ice plug.
Selection of the right freeze sealing method for a particular application

4.2 Freeze Seal
Method Selection depends on the following factors:
Pipe Material. Carbon and low-alloy steel become brittle at low tempera-
tures. For such metals, it is necessary to have them undergo nondestruc-
tive evaluation (NDE) before and after the freeze seal application to find
flaws and other defects resulting from freeze sealing. Also, assume that
the metal surrounding the freeze seal area will be brittle and take appro-
priate precautions to avoid brittle failure. Stainless steel pipes are suscep-
tible to intergranular stress corrosion cracking when they are exposed to
chlorides. In selecting the freeze sealing process, ensure that the selected
refrigerant or equipment will not leave any chloride residue on the
stainless steel piping.
System Conditions. Consider high system water temperatures and com-
partment ambient temperatures in determining the adequacy of the
refrigerant capacity for the freezing method chosen.
Environmental Conditions. When the freeze seal will be located in an
environment detrimental to personnel, give consideration to the time
required for setup, operation, and monitoring by maintenance personnel.
38 NMAC Tech Note

A remotely operated system can be advantageous under such circum-

stances. Ventilation of the workplace is essential. Accumulation of nitro-
gen or carbon dioxide leads to an oxygen-deficient environment and can
lead to dangerous working conditions.
Size of Pipe and Location of Repair. Determine the refrigeration load to make
and hold a freeze seal when selecting the refrigeration method.
The most common problem encountered during freeze sealing is heat trans-
4.3 System
Preparation fer that is caused by flow of the medium in the pipe past the sealing point.
Reduce flows to an absolute minimum. If it is not possible to completely stop
the flow, refer to Table 1, which shows flow rates that have been successfully
sealed in testing. (The table is included here only as a reference and should
not be extrapolated.) Values in the table indicate only that a freeze seal might
be formed in line with a leaky valve; however, every effort should be made to
stop or minimize the flow before attempting a freeze seal. Allow extra freez-
ing time if any flow is present. The problem of flow has been overcome to
some extent by placing seals in series to drop the temperature and slow the
flow before it arrives at the area being sealed.
CAUTION: When using multiple seals in-line, avoid the problem of water
captured between two seals without a means of pressure relief. Captured
water between the seals can freeze and expand, thus exerting pressures
that might lead to pipe rupture. Avoid this problem by proper spacing of
seals or by not completing the upstream seals after the primary seal is
solid. This problem is particularly prevalent in vertical freezes and is one of
the reasons vertical seals should be avoided if possible. Induced stresses
are determined by specific piping system design, configuration, and
material. Before initiating multiple in-line freeze seals or a single seal
located in close proximity to any component that might block the flow and
thus increase internal pressure as the plug forms, determine the minimum
distance between a seal and system component by calculating the appli-
cable piping stresses.
Table 1 and Figure 11 provide guidelines for the maximum allowable flow
when freeze sealing with liquid nitrogen. Successful results have been
obtained with dry ice and freon refrigerant when flow is present, but the time
required with these two refrigerants is longer. No study has been docu-
mented for flow through pipes larger than 4 inches (10 cm) where freeze
sealing was successful.
NMAC Tech Note 39

Table 1
Maximum Flow through Pipe Freeze Sealed in Tests
Nominal Pipe Size, Maximum Flow, Nominal Pipe Size, Maximum Flow, lph
inches gph cm
0.5 30.00 1.25 8
0.75 23.16 2.0 6
1.0 17.28 2.5 4.5
1.25 11.10 3.25 3
1.50 7.62 3.75 2
2.0 4.62 5.0 1.25
2.5 3.36 6.25 .875
3.0 1.90 7.5 .50
3.5 1.15 8.75 .30
4.0 0.60 10.0 .15
The last line in Table 1 is still a critical limit to the allowable flow past the
area to be sealed and is highly dependent on the temperature of the fluid is
the pipe, as shown in Figure 11.
810 180
720 160
630 140
540 Cannot 120
Flow Rate, gals/hr

Flow Rate, L/hr
Be Frozen
450 100
360 80
270 60
180 40
90 20
C 0 5 10 15 20 25
F 32 41 50 59 68 77
Water Temperature
Figure 11
Water Temperature and Flow Rates at Which Ice Plugs
Can Be Formed Using CO2
40 NMAC Tech Note

As the pipe is cooled for freeze sealing purposes, it contracts in the longitudi-
4.4 Pipe Restraints
and Limits nal direction while the ice plug is being formed. This contraction induces
longitudinal stress in the restrained section of the pipe. The amount of
contraction can be calculated using the thermal expansion/ contraction
formula:
L = e x L x T
where:
L = Length of the cooled region
e = Coefficient of expansion for the pipe material
T = Change in temperature
Be sure that pipe sections to be frozen are not restrained for at least three
diameters on either side to prevent inducing additional bending stresses. The
longer the span of non-restrained pipe, the lower the maximum longitudinal
stress imposed by cooling.
NOTE: Although the pipe should not be restrained from the contraction, be
sure that it is adequately supported to prevent additional stress.
Stage and inspect all equipment and materials, including the refrigerant
4.5 Staging
Equipment supply, before beginning to set up to perform the seal. Ensure that all re-
quired items needed are available and at hand before beginning equipment
setup. Inspect all the equipment to be sure that it is properly labeled, if
necessary, and that it meets existing requirements for performance and
personnel safety. Pay particular attention to the integrity of equipment and
materials that will come in contact with the refrigerant, such as regulators,
gauges, supply lines, pipe boats, and sleeves.
Ensure that an adequate supply of the refrigerant is available before starting.
Normally, this is an amount equal to twice the quantity expected to actually
form the seal and maintain it for the period of time necessary to perform the
maintenance work. Identify the logistics necessary to obtain a backup refrig-
erant supply in the event of an emergency or prolonged operation.
Remove sufficient insulation to ensure that what remains does not get damp
4.6 Insulation
Removal or wet from condensation. Tape over the ends of the insulation around the
pipe to keep the insulation dry. Some insulation materials will cause chloride
damage to stainless steel pipes if the insulation gets wet and remains in
contact with the pipe.
NMAC Tech Note 41

Prior to freeze sealing, visually examine the pipe surface at the freeze seal
4.7 Preliminary
Inspection location for defects or flaws. In the past, it was considered good practice to
perform pre- and post-freeze application measurements of the pipe for
evidence of deformation caused by the process. Subsequent experience
indicates that little or no significant change in piping size or geometry occurs
and such occurrences may be attributable to the measurement process itself.
Therefore, continuation of this practice is left to the discretion of the indi-
vidual technician.
Where possible, determine flaw characteristics. Use liquid penetrant or
ultrasonic methods to quantify these characteristics. On ferromagnetic
materials (that is, carbon steels, ferritic stainless), conduct magnetic particle
inspections to find cracks and discontinuities near the surface of the pipe.
Use an inspection method that is consistent with the original construction
requirements. If significant flaws are found, select another section of pipe for
inspection. Small flaw indications are normal and use of the original require-
ments for acceptance would be normal practice. Refer to the original require-
ments for ASME B31.1 and ASME Sections III, V, VIII, or XI for repair. Inspect
flaw indications before and after freeze sealing and compare in order to
detect changes. Report any defects found and carefully evaluate them prior
to application of the freeze seal. Repair as required.
For all critical piping, inspect before and after application of the freeze seal.
Use the same inspection method for both inspections.
NDE methods are useful in determining the suitability of pipes for freeze
sealing applications and in selecting suitable freeze seal locations. The NDE
methods available are visual examination, liquid penetrant examination,
ultrasonic examination, and magnetic particle inspection. The following
sections provide specific information on the applicability for each of these
methods.
4.7.1 Visual Examination

Visual examination is generally used to determine the surface condition and
pipe shape and to detect evidence of leaks. Direct visual examination can be
carried out by the naked eye or with a magnifying glass. Evaluate indications
of poor surface quality and/or deformed and out-of-shape piping. Use visual
indication results as a basis for further investigations. Perform additional
NDE tests if necessary.
4.7.2 Liquid Penetrant

The liquid penetrant examination method is an effective means for detecting
discontinuities (that is, cracks) that are open to the surface of nonporous
metals and other materials and are not detectable with the naked eye. In
addition to cracks, typical discontinuities detected by this method include
seams, laps, cold shuts, lamination, and porosity. For this test, clean the
surface and wet it with a liquid that penetrates any cracks or flaws. Follow
this by applying a developer that shows surface flaws where any exist.
42 NMAC Tech Note

4.7.3 Ultrasonic Examination

The ultrasonic examination method is useful in determining wall thickness
and the quality of longitudinal and circumferential welds of pipes and
tubing.
4.7.4 Magnetic Particle Inspection

Magnetic particle inspection (MPI) can be used to find cracks and other
discontinuities on or near the surface of ferromagnetic piping and pipe
materials. The sensitivity of this method is greater for surface discontinuities
and diminishes rapidly with their increasing depth. Typical discontinuities
that can be detected by this method are cracks, laps, seams, cold shuts, and
laminations on the pipe surfaces. Before MPI, dry the surface to be examined
and all areas within at least 1 inch (2.5 cm) of the examination point. Clean
the surface free of all dirt, grease, lint, scale, welding flux, spatter, oil, or other
extraneous matter that could interfere with the inspection. Surface prepara-
tion by grinding or machining might be necessary where surface irregulari-
ties could mask indications of discontinuity.
Be sure that the freeze sealing boat, jacket, or piping is well insulated from
4.8 Equipment
Installation the ambient temperature to increase the rate of freezing and conserve the
refrigerant use. When selecting insulating materials, consider:
The insulation performance characteristics at cryogenic temperatures
The chloride content in order to avoid stress corrosion cracking in stain-
less steel piping
The weight of the insulation for seismic and loading considerations
The influence of moisture and condensation on the insulation
When using split-sleeve style freeze jackets that surround the pipe, maintain
extra seam sealant (clay) for use in manually plugging any small leaks that
might develop as thermal contraction of the pipe or sleeve takes place.
When handling liquid nitrogen, wear nonporous gloves, face shields, protec-
tive clothing, and other safety equipment to avoid serious injuries. Be sure
that areas where the seal will be installed are ventilated and provided with
the necessary equipment to ensure that no nitrogen gas is allowed to accu-
mulate in low or confined spaces to replace the breathable atmosphere. This
is a serious hazard; monitor accumulations by a continuous oxygen meter,
with a low-oxygen alarm if available.
Review the valve arrangement of the nitrogen fill system to make sure that no
liquid nitrogen can be trapped between two closed valves without a relief valve
to vent excess pressure. The valve configuration should prevent this possibility.
A safety relief valve is normally installed in the refrigerant supply system so
that the refrigerant does not overpressurize the freeze seal apparatus.
NMAC Tech Note 43

Record all refrigerant levels on the appropriate gauges after completing the
hookup of all equipment and before initiating the sealing operation.
Inspect by walk-down all refrigerant delivery equipment from the refrigerant
source to the pipe boat or jacket. Note any signs of leakage and repair as
necessary. Make certain that all appropriate signage is in place. If the refriger-
ant source is located away from the immediate work location, take all neces-
sary precautions to prevent the interruption of refrigerant flow due to
delivery system damage resulting from activities associated with other
unrelated, concurrent operations.
Generally, seals should be at least two times the pipe diameter in length, but
4.9 Initiating the
Freeze Seal seal lengths can vary for the following reasons:
Location of the seal
Number of seals to be formed in the pipe
Pressure in the system
Temperature of the system
Type of refrigerant system being employed
On pipe sizes of 14 inches (35 cm) and larger, if multiple freeze plugs are
formed, the plug size can be equal to the pipe diameter. For smaller pipes,
plug sizes can be as large as four times the pipe diameter.
Ensure that the pipe to be freeze sealed is completely full of water and free of
any air pockets. The appearance of frost band lines on the freeze seal areas
before the expected completion of the seal is a good indication that the pipe
being frozen is not full or contains air pockets.
Confirm that all isolation valves are closed to minimize flow through the seal
area.
Record the start time. Slowly introduce the refrigerant to the pipe, adjusting
the flow of refrigerant until a steady state between refrigerant addition and
boil-off is reached. Inspect the freeze seal containment for signs of refrigerant
leakage as thermal contraction in the materials occurs. Plug refrigerant leaks
as appropriate.
Monitor the refrigerant supply pressure to ensure a continuous flow of
refrigerant to the seal area. Monitor the pipe surface outside the freeze seal
containment for signs of frost bands forming on the pipe. Frost lines by
themselves are not reliable indicators of freeze seal formation. Normally,
metal temperatures indicated by thermocouples or handheld thermometers,
the elapsed time, and pressure differential across the seal are the criteria used
to determine if a freeze seal is established, based upon the technicians
experience.
44 NMAC Tech Note

Confirm the formation of the freeze seal before initiating the repair activity
by opening a vent path downstream of the freeze seal or between the freeze
seals if two are needed. There will be a slight flow from water trapped
between the freeze seals or between the freeze seal and the isolating compo-
nent. If the flow continues, the freeze plug is not completely formed. If no
vents are available, it might be possible to add a fitting or coupling or to
make other modifications to permit venting. Make similar provisions also for
draining the lines.
Monitor pipe surface temperatures with thermocouples and record these

4.10 Maintaining the
Freeze Seal values at regular intervals. Surface temperature measurement helps to
indicate the integrity of the seal.
If the freeze seal is incompletely formed and the pipe is cut, consider using a
pipe patch or pipe plug. If a hole has been drilled in the pipe and the ice plug
fails, a tapered steel plug can be used. It as essential that the temperature be
monitored on pipe walls inside the freeze chamber. This provides the first
reliable information on freeze plug formation and also on plug release
conditions if the refrigeration process is stopped.
Melt the ice plug as rapidly as possible from one side of the pipe. Do this by
4.11 Removing the
Freeze Seal thawing the plug with electrowrap heat trace, strip heaters, or infrared
lamps. Do not use open flames to thaw ice plugs. Fast thawing of an ice plug
on one side of the pipe can result in water flowing through and eroding the
ice in place, which helps prevent a sudden release of the ice plug.
NOTE: Slow thawing of the pipe results in dislodging and free movement of
the plug in the pipe; avoid this if possible. The freeze plug travels with the
flow or with gravity and can end up at a location where it could damage
equipment or block flow.
Analyze the possible impact of freeze plug remnants moving downstream as
a block during the thawing process before melting is complete. Placement of
the seal upstream of an elbow is one method to prevent movement of a large
block down the pipe.
Backfilling of the pipe is another option to mitigate plug movement during
thawing. If the system is refilled where it was drained for repair before
thawing the freeze plug, the movement of the plug is restricted by the pres-
ence of water in the pipe. If the space is left empty and there is pressure
behind the plug, it can move to the first obstruction with enough force to
cause damage, depending on the driving pressure. If there is no pressure or
nothing that can be damaged downstream, then the backfilling process might
not be necessary.
NMAC Tech Note 45

CAUTION: Sudden, rapid plug movement during thawing has resulted in

significant water hammer to plant piping systems with detrimental effects
when steps, such as backfilling, are not taken to mitigate that circum-
stance.
46 NMAC Tech Note

5
TROUBLESHOOTING ISSUES
Typical problems associated with freeze sealing are:

Flow
Line not filled with water
External heat
Insulation on the pipe
Convection
Inadequate pressure in the line
Position of pipe
No pressure relief point
Restriction of the pipe
Starting work too soon
Problems Associated with Freeze Sealing

In some circumstances, the location or position of the pipe will increase the
time required to obtain a freeze plug. Also, the condition and status of the
contents in the pipe could prevent the development of a plug, regardless of
the amount of time allocated for the freezing operation.
NMAC Tech Note 47

The following conditions describe some problems that can occur during a
freezing operation and possible solutions. Any freeze situation can have one
or more of these conditions; therefore, evaluate each situation individually.
Flow in the Line

Flow in the line is indicated by a partial frost at the end of the freezing
equipment and possibly an excessive accumulation of condensation on the
bottom of the pipe in one direction away from the freeze site.
Review the position of all valves downstream of the freeze site, including
any branch line valves, for secure closure. Also review the holding capability
of any upstream valves if the indications of flow persist.
Vibration of the Pipe

Vibration of the pipe is indicated by complete lack of frost on either end of
the equipment being used to develop the freeze plug.
The severity of vibration can prevent obtaining a plug. If the vibration cannot
be eliminated, relocate the freeze site to a more stable section of pipe.
Turbulence
The quantity of water flow through a main header or branch connection
located below or next to a freeze site can create a turbulence sufficient to
eliminate the formation of a plug.
Location of the freeze site on a branch connection of a flowing header should
be below or, if on the side of the header, past a horizontal or vertical change
in pipe direction, that is, past an ell or tee joint.
Heat
Excessive heat in the fluid contents of the pipe to be frozen can prohibit the
formation of a plug. Temperatures greater than 130F with a minimal flow
can prolong or prohibit forming a plug.
Cool the pipe and its contents by stopping the flow through the proposed
freeze area and allowing the pipe to cool down before installing the freezing
equipment. If circumstances permit, spray cold water on the pipe to acceler-
ate the cooling process.
Contamination
Contamination will become evident when attempting to freeze plug a pipe
containing a large quantity of glycol or bromate because of the greater length
of time required to develop a plug.
Make provisions to displace the contaminated fluid with clean water or a
smaller concentration of the contaminated fluid.
48 NMAC Tech Note

Lined Pipe
When freeze plugging lined pipe, there is no significant indication that the
plug is not forming. The frost line appears normal, the temperature indica-
tions also are normal, but the plug does not form.
The only solution is to move the freeze location to a section of unlined pipe.
Air or Gas
The formation of frost on the top section of pipe on each end of the freezing
equipment prior to frost formation on the bottom of the pipe is normally an
indication that there is no fluid in the pipe or that it is only partially filled.
Make provisions for completely filling the pipe before attempting the freeze
operation.
Pressure
When the pipe is full of clean water and has no flow, turbulence, or convec-
tion, the plug forms but will not remain in place or hold pressure.
Pressurize the contents prior to attempting the freeze. The pressure com-
presses the contents, thereby packing and diffusing any residual air or gas.
This contributes to a more dense and harder plug, which will restrain more
pressure.
Convection
Large diameter pipe, in the horizontal or vertical position, that is full of clean
water with no flow and no turbulence can develop a convection current that
extends the freezing time or does not permit a plug to be formed.
If possible, place the freeze location near a closed valve or blind flange, but
with a vent or relief between the freeze and the closure. This can impede the
continual movement created by the convection and allow the successful
formation of the plug.
NMAC Tech Note 49

APPENDIX A
INDUSTRY EXPERIENCE
Table 2 illustrates the extent and variety of freeze sealing applications under-
taken in the commercial nuclear power industry. The table presents data
compiled by a major freeze sealing services vendor, from 19921995, for
freeze sealing activities performed at U.S. and Canadian nuclear power
stations during that period.
The rows in Table 2 indicate the number of freeze seals performed for a client,
type of pipe, differential pressure sustained, and affected plant system. The
data are ranked first by pipe size, then piping material and plant system. The
data cover pipe diameters from .7530 inches (1.875120 cm), made of both
carbon and stainless steels, copper, and several of unknown material. Pres-
sure differentials sustained during these activities ranged from 101,600 psi
(.7110 bar).
NOTE: The following data are provided for information only. No attempt has
been made to verify, substantiate, or disprove this information; however,
EPRI has no reason to believe that it is incorrect. Experiences by other
vendors and individual utilities might exceed these parameters.
NMAC Tech Note 51

Table 2
Freeze Sealing Applications
Qty. NPS (in.) Material Pressure Plant System/Component

(psi)
3 3/4 CS 125 Service water
8 3/4 CS 100 Various systems
1 3/4 SS 20 Control rod drive
22 3/4 SS 10 HCV
1 3/4 SS 20 Heat exchanger
3 3/4 SS 30 Instrumentation
20 3/4 SS 60 Main steam isolation valve
2 1 CS 125 Service water
9 1 CS 100 Various systems
3 1 SS 20 Control rod drive lines
40 1 SS 10 HCV
6 1 SS 10 HCV
3 1 SS 30 Instrumentation
20 1 SS 60 Main steam isolation valve
1 1 SS 155 Sample line
17 1.25 SS 20 Control rod drive lines
1 1.25 SS 90 HCU-04-37
2 1.5 CS 30 Core cooling water
1 1.5 CS 120 RNP
14 1.5 SS 10 Reactor coolant
1 1.5 SS 20 Spray additive sodium hydroxide
3 2 CS 50 Fuel pool
1 2 CS 120 RNP
1 2 CS 50 Service water hydrotest
4 2 SS 10 Charging pump
1 2 SS 150 Fuel pool
4 2 SS 10 Reactor coolant
2 2 SS 20 Reactor make-up
1 2 SS 80 Safety injection system
1 2 SS 1,600 Strainer
2 2 SS 70 Vessel drain
1 2.5 CS 80 Bottom head
2 2.5 CS 115 CCS lines
2 2.5 CS 15 Off vessel bottom
1 2.5 CS 60 Service water
1 2.5 CS 125 Service water
6 2.5 CS 100 Various systems
2 2.5 SS 20 Spray additive sodium hydroxide
52 NMAC Tech Note

Table 2
Freeze Sealing Applications (cont.)

(psi)
1 3 CS 20 Service water sump pump
1 3 CS 90 WCS line off vessel
1 3 SS 30 Safety injection system
3 3 SS 10 Safety injection system off vessel
4 4 CS 20 Containment sumps
1 4 CS 115 Core cooling system line
2 4 CS 175 DBA-11 (Sch. 160)
3 4 CS 20 DFR
3 4 CS 20 Feed water make-up
2 4 CS 30 Shield cooling system
1 4 CS 20 Steam generator
1 4 Cu 50 Treatment plant
1 4 SS 80 Demineralized water chiller
3 4 SS 25 PHT
2 4 SS 30 Reactor coolant
2 4 SS 20 Sodium Hydroxide (20%)
1 6 CS 20 Auxiliary pump
1 6 CS 80 Cooling water
7 6 CS 80 Demineralized water chiller
2 6 CS 40 EWS
1 6 CS 200 Fire water
2 6 CS 80 HVIC
1 6 CS 30 RB CCW
2 6 CS 30 RB CCW
4 6 CS 30 Various containment systems
5 6 SS 60 Low-pressure injection system injection
2 6 SS 25 PHT
2 6 SS 175 Service water hydrotest
1 8 CS 20 Auxiliary pump
2 8 CS 20 Condenser system
2 8 CS 80 Diesel generator
6 8 CS 80 High-pressure cooling system
3 8 CS 25 PHT off vessel
NMAC Tech Note 53

Table 2

(psi)
1 8 CS 30 RB CCW
1 8 CS 30 RB CCW
2 8 SS 80 ISWB (906 WT)
1 8 SS 25 PHT
2 10 CS 20 A & B loop off vessel
2 10 CS 10 Fuel pool
1 10 CS 20 Heat exchanger
1 10 CS 80 High-pressure cooling system
4 10 CS 25 PHT
2 10 CS 30 RB CCW
8 10 SS 25 PHT
1 10 SS 25 SI system
1 10 SS 80 Spent fuel pool
2 12 CS 20 A & B loop off vessel
10 12 CS 10 Jet pump risers off vessel
3 12 CS 20 Recirculation
3 12 SS 150 Unknown
6 12 SS 35 Core spray
1 12 SS 10 Fuel pool outlet
1 12 SS 25 PHT
1 12 SS 20 Pressurizer
1 12 SS 80 SI system
2 12 SS 80 SI header
4 14 Unknown 50 Fuel building cooling system
2 14 CS 115 CCS lines
5 14 CS 80 Emergency fire water
54 NMAC Tech Note

Table 2

(psi)
3 14 CS 30 End shield cooling
2 16 Unknown 50 Fuel building cooling system
2 16 Unknown 25 WS system
2 16 CS 150 Emergency fire water
2 16 CS 30 End shield cooling
1 16 CS 150 Fire water
2 18 Unknown 25 WS system
1 20 CS 20 Condensate short cycle
1 28 CS 20 Residual heat remover off vessel
1 30 CS 200 Demonstration
Events
No attempt has been made to catalog all industry events related to the
application of freeze seals. However, the Institute for Nuclear Power Opera-
tions (INPO) has published a number of event reports, listed in Appendix B,
that provide a good indication of the range of unusual events that can occur
related to freeze sealing.
NMAC Tech Note 55

APPENDIX B
REFERENCES AND BIBLIOGRAPHY
References
M. T. Flaman, and N. N. Shah. Structural Integrity Investigation of Feed Pipe Ice
Plugging Procedures, Report No. 84 462-K, Ontario Hydro Research Division,
March 1984.
Bibliography
Advances Made in Freezing Technique for Pipeline Plugging during Test-
ing. Oil & Gas Journal, April 1982, p. 108110.
ASME Boiler and Pressure Vessel Code, Section V, Nondestructive Examination.
Barnes C. R. Freeze Sealing for Maintenance and Repair. Palo Alto, CA: Electric
Power Research Institute, September 1986.
Baumeister, T. and L. S. Marks. Standard Handbook for Mechanical Engineers.
McGraw-Hill, 1967.
Burton, M. J. and C. W. Bishop. Recent Developments in Pipefreezing
Technology for the Oil Industry. Paper No. SPE 23069, presented at the
Offshore Europe Conference, Aberdeen, Scotland, September 1991.
Cryogenic Pipe FreezingA Research Project to Determine the Basic Mechanisms of
Plug Formation. Department of Mechanical Engineering, The University,
Southampton, England.
Effect of Convection on Plug Formation during Cryogenic Pipe Freezing.
Institution of Chemical Engineers, March 1989, p. 121126.
NMAC Tech Note 57

Emmons, F. R., L. D. Hudspeth, J. P. Clancy, D. R. Zornes, and J. E. Philcox.

Nitrogen Management at the East Binger Unit Using an Integrated Cryo-
genic Process. Paper No. SPE 15591, presented at the 61st Annual Technical
Conference and Exhibition of the Society of Petroleum Engineers, New
Orleans, LA, October 1986.
Experimental Analysis of the Obturation of Pipes by Ice Plugs. Nuclear
Engineering and Design, December 1984, p. 305313.
Freeze Plug Tests 40 Inch Pipe for Colonial Loop Line. Pipe Line News, p. 44.
Frost-Service fr Abdichtungen im Khlwasserkreislauf. atomwirtschaft,
February 1989, p. 8990.
Howard, G. J., Ice-O-Lator ProcessThe Freeze Plug for Pipelines. OCG
Journal, April 19, 1987.
Ice Plugs Isolate Pipe Sections. Ocean Industry, April 1979, p. 172176.
INPO (INP) Subject: Significant by Others (SO) Report 91-01.
INPO Recurring Significant Event Notification: 92-02.
INPO SER 15-89, Internal Flooding Resulting from Freeze Plug Failures.
INPO SER 19-91, Loss of Decay Heat Removal Capability Due to Inappropri-
ate Maintenance and Testing.
INPO Significant Operating Experience Report 85-5, Internal Flooding of
Power Plant Buildings, dated December 30, 1985.
INPO SOER 85-5, Internal Flooding of Power Plant Buildings, Recommenda-
tion Clarifications.
Kiefner, J., C. Barnes, P. Scott, and G. Andrews. Development of Guidelines for
Use of Ice Plugs in Pipeline Maintenance and Hydrostatic Testing. Unpublished
report, Battelle, Columbus Division, November 15, 1982.
Laurov, V. V., Deformation and Strength of Ice, Gidrometeorologicheskoe,
Izdatel stvo, Leningrad, 1969.
McKenna and Sullivan. Remote Pipeline Isolation for Maintenance Operations.
Mobils Pipe Freeze Breaks New Ground. Pipes & Pipelines International.
July/August 1987, p. 2223.
Nuclear Network. Entry OE 3322. May 5, 1989.
On the Prediction of Stresses in Pipes Caused by Ice Plug Formation.
Journal of Process Mechanical Engineering. April 1996, p. 151158.
Peckner, D. and I. M. Bernstein, Handbook of Stainless Steels. New York:
McGraw-Hill, 1977.
Pipefreezing Cuts Time in Refinery Valve Maintenance. Plant in Action.
March 1981, p. 19.
58 NMAC Tech Note

Pipeline Isolation Techniques. Shell UK, Exploration and Production: February

1990.
Quick Freeze Plug Reduces Testing and Repair Costs. Pipe Line Industry.
March 1977, p. 3739.
Samuelson, Brown G., Pipe Freezing Method. Building Services Research
and Information Association (BSRIA). Bracknell, England.
Tavner, C. R., R. J. Bowen, and C. W. Bishop. Heat Flux Monitoring during
Cryogenic Pipe Freezing: A Case Study. Institution of Chemical Engineers. Vol.
74, Part A, 1996, p. 239-241.
Thygesen, J. E., E. Abraham, S. Clouston, D. Olie, and J. P. Kenny. A Com-
parison of Subsea Isolation Systems and Recommendations for Future
Development. Presented at the Offshore Pipeline Technology Conference,
Oslo, Norway, February 1994.
U.S. Navy, Procedure to Apply Freeze Seals. Navship-NPM 9890, 6C1, Rev A,
1.90 1.0
The Use of Thin Foil Heat Flux Gauges to Determine Plug Closure in Cryogenic
Pipe Freezing. Institute of Cryogenics, University of Southampton, Highfield,
Southampton.
UT Ice Plug Detection. Report P119/79/020. Electricit de France, June 1979.
Wigley D. A. and M. Burton, Basic Mechanisms of Plug Formation during
Cryogenic Pipe Freezing, presented at the Tenth International Cryogenic
Engineering Conference, Helsinki, Finland (July/August 1984).
NMAC Tech Note 59

EPRI
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Keywords: EPRI TR-016384R1

Maintenance Final Report

NMAC Tech Note

Freeze Sealing (Ice Plugging)

Freeze Sealing (Ice Plugging) of Piping

BACKGROUND In the course of performing certain nuclear plant maintenance

RESULTS The revised document now provides a comprehensive discussion

EPRI TR-016384R1s Electric Power Research Institute November 1997

A) MAKES ANY WARRANTY OR REPRESENTATION WHATSOEVER, EXPRESS OR IMPLIED, (I) WITH

Important Notice Regarding This Document:

PREFACE AND ACKNOWLEDGMENTS

NMAC Tech Note iii

1.0 INTRODUCTION ......................................................................................... 1

2.0 FREEZE SEAL PLANNING CONSIDERATIONS..................................... 13

3.0 EFFECTS ON PIPING AND MATERIALS ................................................ 21

NMAC Tech Note v

3.6 Unknown or Uncontrolled Loads ....................................................... 30

4.0 PERFORMING A FREEZE SEAL ............................................................. 37

5.0 TROUBLESHOOTING ISSUES ................................................................ 47

APPENDIX A: INDUSTRY EXPERIENCE ......................................................... 51

APPENDIX B: REFERENCES AND BIBLIOGRAPHY ..................................... 57

vi NMAC Tech Note

Figure 1 CO2 Pipe Boat ................................................................................ 5

Figure 2 Typical Liquid Nitrogen Freeze Jacket ............................................ 6

Figure 3 Prefabricated Copper Freeze Jacket .............................................. 7

Figure 4 Sample Pipe Jacket Flow Path and Configuration .......................... 8

Figure 5 Liquid Nitrogen Gas-Pressured Freeze Seal Arrangement ............ 9

Figure 7 Coil Arrangement for 1- to 4-Inch (2.54- to 10.17-cm) Pipe for

Figure 8 Yield Strengths of Metals at Low Temperatures ........................... 22

Figure 9 Ultimate Tensile Strengths of Solids at Low Temperatures ........... 23

Figure 10 Generic PlotTemperature Dependence of the Fracture

Figure 11 Water Temperature and Flow Rates at Which Ice Plugs

NMAC Tech Note vii

Table 1 Maximum Flow through Pipe Freeze Sealed in Tests ....................... 40

Table 2 Freeze Sealing Applications ............................................................. 52

NMAC Tech Note ix

Freeze sealing refers to the process of applying an external refrigerant to a

NMAC Tech Note 1

2 NMAC Tech Note

The following sections describe commonly used freeze sealing refrigerants

WARNING! Due to the extremely low temperature of liquid nitrogen, work

NMAC Tech Note 3

Carbon Dioxide. Liquid carbon dioxide is available in cylinders and some-

Note: Technicians who handle freon must be trained and licensed

4 NMAC Tech Note

NMAC Tech Note 5

Gas Vent Thermocouple Gas Vent

6 NMAC Tech Note

Table of Dimensions (All Figures in Inches)

NMAC Tech Note 7

Vent Above Funnel

Note: Thermocouple points should be located as shown above

8 NMAC Tech Note

Liquid Nitrogen Inlet

NMAC Tech Note 9

Copper Cloth Thermal Bulb Strapped

3/16-Inch (.48-cm) OD x Suction

10 NMAC Tech Note

NMAC Tech Note 11

CAUTION: Supports and/or restraints must often be added during freeze

NMAC Tech Note 13

14 NMAC Tech Note

WARNING!: Plug maintenance is extremely important. There are no

NMAC Tech Note 15