Publication Date: 5/1/74
    Pages: 5
    Date Entered: 2/22/84
    Title: DESIGN CONSIDERATIONS FOR MINIMIZING RESIDUAL HOLDUP OF SPECIAL NUCLEAR MATERIAL IN DRYING AND FLUIDIZED BED OPERATIONS (6/73)
    Revision 1
    May 1974
    U.S. ATOMIC ENERGY COMMISSION
    REGULATORY GUIDE
    DIRECTORATE OF REGULATORY STANDARDS
    REGULATORY GUIDE 5.8
    DESIGN CONSIDERATIONS FOR MINIMIZING RESIDUAL HOLDUP
    OF SPECIAL NUCLEAR MATERIAL IN DRYING AND FLUIDIZED BED OPERATIONS
A. INTRODUCTION
    Section 70.22, "Contents of Applications," of 10 CFR Part 70,
    "Special Nuclear Material," requires, in part, (*)that each application
    for a license to possess at any one time more than one effective
    kilogram of special nuclear material (SNM) contain a full description of
    the applicant's procedures for control of and accounting for SNM which
    will be in his possession under license, including procedures for
    controlling SNM during its processing or use in the facility.
    Furthermore, Section 70.51, "Material Balance, Inventory, and Records
    Requirements," requires, in part, that certain licensees conduct at
    specified intervals physical inventories of the SNM in their possession
    under license. The control of and accounting for SNM can be made more
    effective by minimizing the residual holdup after shutdown, after
    draindown, and after cleanout of the equipment used to process SNM,
    thereby reducing the component of uncertainty contributed by residual
    holdup to a physical inventory and lessening the severity of problems
    associated with determination of residual holdup. This regulatory guide
    describes acceptable design features and characteristics for minimizing
    the residual holdup of SNM in drying and fluidized bed operations after
    shutdown, draindown, or cleanout in order to facilitate material control
    and accountability procedures. These features and characteristics are
    not expected to interfere with process operations.
B. DISCUSSION
1. Background
    Certain unit processes permit accumulation of sizable amounts of
    SNM which are referred to as residual holdup, or hidden inventory. A
    characteristic amount of this material that is difficult to locate,
    sample, identify, quantify, and analyze is held up in equipment for a
    given design, mode of operation, and type of process material. This
    holdup may be decreased as the status of the equipment changes
    progressively through the four stages consisting of operation, shutdown,
    draindown, and cleanout. Simultaneously, the number of sources of
    uncertainty and thenlevels of uncertainty in the physical inventory may
    be reduced.
    ----------
    (*) Indicates changes from previous issue.
    ----------
    The accumulation of SNM in process equipment in the form of
    residual holdup following shutdown, draindown, and cleanout could have
    adverse effects on a materials control program. Minimizing that
    quantity of material retained in process equipment enhances the
    effectiveness of a materials protection program in the following ways:
    a. The quality of a physical inventory is improved by reducing
    uncertainty due to holdup. For example, the contribution of unmeasured
    holdup material to the category of material unaccounted for (MUF) may be
    lessened, and the influence of uncertainty associated with measured
    holdup on the limit of error on material unaccounted for (LEMUF) in a
    material balance may be lessened. Furthermore, the extent to which the
    uncertainty in holdup contributes to a physical inventory depends on the
    magnitude of the amount present and how precisely and accurately that
    amount is amenable to being measured. Therefore, reducing the quantity
    of holdup directly decreases the uncertainty contributed to a physical
    inventory.
    b. A reduction in the quantity of holdup material that must be
    recovered following the three stages of shutdown, draindown, and
    cleanout of process equipment decreases the quantity of SNM susceptible
    to diversion during sampling, identification, and subsequent separation
    or recycle of this material as may be necessary to complete a physical
    inventory. A reduction in holdup also can enhance process operations by
    decreasing the extent and time of unit process interruptions for
    material accountability. For example, for a process amenable to dynamic
    inventory techniques, credibility in such a technique may be increased
    by reducing the detrimental effects of residual holdup on such an
    inventory.
    c. The effort required to establish the presence of and to
    remove residual material for a physical inventory is reduced.
    Consequently, the amount of time and the number of people who need
    access to SNM are reduced. The opportunity for unauthorized individuals
    to gain access to SNM during this stage of a physical inventory also may
    be reduced.
    This guide is addressed mainly to two unit processes-drying and
    fluidized bed operations. The unit drying operation is commonly applied
    to remove moisture, vapors, and/or solvent from a wet feed material to
    produce a dry solid product. A unit operation for dewatering slurries
    normally precedes drying. Commercial applications of fluidized beds are
    manifold. Generally, the fluidized bed is used for gas-solid, gas-gas,
    or gas-liquid contacting to effect dewatering, drying, calcining,
    chemical reaction, or particle coating. Frequently, shutdown and/or
    draindown of process equipment used for drying or fluidized bed
    operations results in a substantial quantity of residual material held
    up in the equipment. Consequently, design guidance is provided to
    facilitate minimizing holdup material in driers and fluidized bed
    equipment after shutdown and after draindown as well as after cleanout.
2. Holdup in Driers
    A variety of driers is used in nuclear fuel fabrication. The
    holdup problems associated with each are peculiar to the state of the
    material being processed, the mode of operation, and particularly the
    specific type of drier.
    With directly heated driers using a heated stream, fines may be
    entrained in the gas stream and must be collected in filters and
    recovered from the process. The entrainment contributes to holdup of
    fines in ductwork and filters. On the other hand, directly heated
    driers using infrared heat lamps are advantageous since entrainment then
    is minimal. Use of agitators in directly heated driers may be desirable
    from an operating standpoint However, driers with agitators are
    difficult to empty and clean.
    Continuous driers are desirable for a high-throughput low-holdup
    operation. This arises largely from increased continuity of operation
    and increased uniformity of material handling. Continuous operations
    have the advantages of minimal physical handling as well as greater
    potential for process automation.
    For certain processes, however, batch drying is advantageous.
    With individual batches it is possible to maintain batch identity.
    However, batch driers require more physical handling of material than
    continuous driers, may be difficult to automate, and may necessitate
    additional equipment cleanout between batches.
    For directly heated fluid-bed driers and spray driers, there is a
    tendency for dry product to adhere to the walls and bottom of the drier,
    particularly if the product is very fine. Internal mechanical scrapers
    constitute an additional impediment to cleaning the drying chamber.
    For indirectly heated driers in which the material being dried
    contacts a heated surface, sweep gas may be used to carry away the vapor
    from the drying solid. Unless the exit velocity of this vapor is low,
    some material will be entrained in the gas and may be retained in ducts.
    Also, for indirectly heated continuous screw conveyor driers, as the
    feed drys to an adhesive paste it has a tendency to cake and choke off
    the flow or to spill out of the drier. Furthermore, the screw conveyor
    is difficult to clean and tends to be a significant source of holdup.
    Rotary driers have been used to combine a drying operation with a
    calcining operation in separately heated zones. An intermediate paste
    having a high bulk density and viscosity has a tendency to adhere to
    most materials which it contacts such as flight carriage surfaces. Such
    surfaces contribute to holdup by impeding material flow during emptying.
    Therefore, special attention may be necessary for cleanout or draindown.
    Directly heated rotary driers also may be accompanied by carry over of
    dust or ultrafine powder which becomes a form of holdup.
    Woven metal belt driers have a high surface area and high
    porosity. Consequently, they may be a significant source of material
    holdup.
    Batch pan driers are completely enclosed and usually are equipped
    with agitators which constitute a source of material holdup upon
    emptying. Agitators also cause more difficulty for a complete cleanout.
    Continuous driers with open static beds such as pans, boats, or trays do
    not contribute significantly to holdup unless they are accidentally
    tipped or the contents are otherwise spilled. Trays, pans, and boats
    also may be easy to empty and clean if necessary.
3. Holdup in Fluidized Bed Operations
    Because of the numerous interrelated components of a fluidized bed
    operation that contact the process material, there exists a large number
    of locations where holdup may occur and numerous sources initiating its
    occurrence. However, holdup in fluidized beds commonly depends upon the
    size and growth of particles throughout the system. Beginning with the
    input, screw conveyors, pneumatic carriers, dip pipes, seal legs,
    injectors, or other means are used to introduce solids into the reactor
    proper. Difficulties with holdup arise and special techniques become
    necessary when solids are not free flowing, such as filtered
    precipitates and other moist solids. Since it is difficult by means of
    a screw conveyor to feed wet material to a reactor, it may be necessary
    to assist handling by wetting the material to attain a slurry
    consistency before feeding. If slurry consistency is undesirable for
    the material, the solid product may be recycled to mix with the feed to
    dry it and thereby achieve better handling qualities. Nonhomogeneous
    feed containing lumps of dry or semidry solids tend to compound the
    problem by agglomerating and fusing together instead of breaking apart.
    Agglomerates which are much larger than the original particle size
    subsequently tend to segregate out of the bed. After a period of time,
    the fluidized bed may become static thereby necessitating shutdown and
    cleanout.
    Liquid feed necessitates use of an injection nozzle and atomizing
    gas. The liquid input system consists of (1) a spray injection nozzle,
    (2) a liquid chemical injection system, and (3) a fluidizing gas system.
    Injection nozzles have been shown to be a source of localized cake
    formation and holdup. Furthermore, the area of the equipment directly
    across the fluidized bed opposite the nozzle also has been shown to be
    susceptible to cake formation. An additional consequence which further
    propagates holdup formation is interference of cake with normal
    operation. Agglomerates deposited at the bottom of the fluidized bed and
    on the gas distribution plate interfere with fluidization and may cause
    localized hot spots. Also, the product overflow tube may become
    blocked. Typical causes of this agglomeration are impurities in feed,
    fines from the recovery system, poor gas distribution, poor spray nozzle
    operation, generally poor fluidization, and other unfavorable operating
    conditions.
    The fluidized bed chemical reactor system may consist of one of
    several configurations. A series of individual reactors as well as a
    single reactor with individual compartments have been used to provide
    multiple contacting stages. Unfortunately, multiple compartments as
    well as the series configuration provide multiple locations for holdup.
    In either case, a sufficient flow rate of gas is necessary to forestall
    plugging and channeling.
    In general, process conditions influence the formation of holdup.
    Variables which may induce this formation are inlet gas composition and
    velocity, bed temperature and depth, and feed material temperature and
    consistency. The generation of fines especially is dependent on the
    operating range of process variables. Buildup of fines may cause
    bridging of solids in the reactor structure. In addition, deposition of
    substances on internal surfaces of the reactor structure and in
    connecting lines is sensitive to process variables such as temperature.
    Severe operating conditions such as temperature excursions are
    particularly conductive to severe segregation and packing of SNM against
    the base and interior walls. The existence of holdup may compound an
    excursion by its sudden release to the fluidized bed for reaction, which
    induces further excursion and additional resulting holdup by the
    mechanisms of packing and fusion.
    Existing material consists of product and offgases. Product may be
    batch removed by freely draining through a bottom outlet valve or by a
    screw conveyor. However, depending upon the characteristics of the
    particulate matter, solids may adhere to the walls or the gas
    distribution plate. If excessive caking occurs, larger agglomerates may
    form that do not drain through openings in the exit valve.
    Other types of outlets for continoous product removal are: (1) a
    simple weir permitting overflow, (2) a flapper-type check valve to
    restrict gas flow through the exit, and (3) a seal leg with a solids
    flow control valve to equalize external and internal pressures. In each
    case, obstruction and accumulation as a result of inadequate design may
    result in large quantities of holdup material.
    Offgases are discharged near the top of a fluidized bed reactor
    through a variety of components which are sources of holdup. These
    include cyclones for dust removal, carbon or sintered metal filters, and
    cold traps. Holdup in these devices occurs to such an extent that it is
    necessary to recover the solids which are carried by gases leaving the
    fluidized bed.
    One of the advantages of utilizing a fluidized bed is its
    favorable heat transfer performance. Unfortunately from the viewpoint
    of minimizing holdup, heat exchanger tubes manifolded at the bottom and
    top or bayonets internal to the reactor are sometimes used. Such use
    should be avoided where possible since it aggravates the problems of
    holdup and cleanout.
    In general, the absence of moving parts contributes significantly
    to effective cleanouts. For tall reactors, however, or for a mixture of
    fluidized solids with different characteristics, mechanical mixing may
    be utilized to reduce segregation. Without adequate mixing,
    agglomeration may occur because of particle fusion or poor dispersion of
    adhesive feed solids.
    In contrast to particle growth, size reduction in fluidized beds
    contributes to the generation and subsequent deposition of fines. Major
    size reduction mechanisms in fluid beds are attrition, impact, and
    thermal decrepitation. All three mechanisms produce fines which may
    contribute to holdup, especially in filters or components downline from
    the fluidized bed reactor. Exceptionally fine particles may necessitate
    an offgas cleanup system on-line rather than a complete shutdown
    periodically. An alternative is to use an internal fines filter.
    Instrumentation of fluid bed reactors largely consists of
    temperature and pressure sensors. Thermocouple wells and pressure taps
    are potential locations for retaining SNM during shutdown and draindown.
C. REGULATORY POSITION
    For purposes of facilitating (1) control of SNM during processing
    of use, including shutdown, draindown, and cleanout, (2) determination
    of process losses by lessening the magnitude of the contribution of
    residual holdup to process losses, and (3) performance of a physical
    inventory, which may include an uncertainty component due to residual
    holdup, it is appropriate to minimize the amount of SNM retained inside
    equipment as residual holdup. The design of equipment used to carry out
    physical or chemical changes on SNM by drying or fluidized bed
    operations should include an evaluation of the desirability of
    incorporating features for purposes of minimizing residual holdup after
    shutdown, after draindown, and after cleanout. Appropriate features
    acceptable to the Regulatory staff for consideration include the
    following:
1. General Design
    a. Surface are free from crevices, cracks, protrusions, and
    other irregularities that could entrap material.
    b. Overlapping metal surfaces in contact with process material
    are sealed by welding; internal welds are ground flush with inner
    surfaces.
    c. The internal angles and corners, particularly in tray
    driers, are rounded with a radius larger than a minimum radius, for
    example, one fourth inch.
    d. Seams that promote corrosion are absent.
    e. Materials of construction that contact SNM are compatible
    with the contents so that surfaces do not corrode, dissolve, or erode
    during operation or during contact with rinse solutions used for
    cleaning after shutdown.
    f. Surfaces that contact SNM are selected, coated, polished or
    machined to prevent or resist the adherence of liquids and solids.
    g. Structural integrity is adequate to resist formation of
    leaks, cracks, and crevices due to localized stresses such as thermal
    and vibratory stresses during operation.
    h. Containers, for example, boats, pans, and trays, are
    constructed with adequate strength to preclude breakage and deterioration.
    i. Trays in tray driers are designed not to tip and spill the
    contents during handling and operation. For example, when fully loaded,
    the distance of the center of gravity from any side is at least four
    times its distance from the bottom of the tray.
    j. All equipment in which material is agitated, sprayed, or
    removed mechanically is enclosed with side walls, covers, or other means
    of containment to prevent spilling or release of the contents during
    operation.
    k. The feed material is properly prepared to minimize the
    potential for holdup formation within a fluidized bed. Also, sizing
    operations prior to introduction of particles are evaluated.
    l. The influence of operating variables such as gas flow rate
    and temperature is evaluated to reduce undesirable formation of holdup
    such as caking which may be induced by operating in an undesirable range
    of operating conditions.
2. Internal Design
    a. Equipment has a minimum of internal components upon which
    process material can collect; equipment is free from internal structural
    supports, flanges, support rings, trays, or devices that are not
    essential to operation.
    b. Racks, carriages, conveyors, guides, or drive mechanisms
    that are used to assist or direct the transport of trays through a tray
    drier are designed so that individual trays cannot be tipped or ride
    over one another. For example, for "walking-beam" drives, vertical
    travel is constrained to less than one-fourth the height of the tray to
    minimize the probability of tray override.
    c. Mechanical agitators are designed to permit surfaces to
    drain freely and present minimum surface for collection of solids.
    d. Sensing devices such as thermocouples are installed in a
    manner that minimizes the amount of solid material that can be retained
    by sensing devices.
    e. Pressure taps projecting into the equipment have the
    capability for being gas purged.
    f. Because of highly abrasive wear in fluidized beds and
    potential for SNM retention on horizontal elements and protection tubes,
    installation of internal elements are positioned, for example vertical,
    to reduce surface erosion and holdup. Examples of such elements may be
    sensing elements, bayonet heaters, mechanical mixers, and heat transfer
    fins.
    g. Permanently mounted process equipment internals that cannot
    be removed for cleaning allow rinsings and normal contents of vessels
    such as fluidized bed driers to drain freely from the bottom of the
    equipment.
    h. The height of the disengaging section above the expanded bed
    is adequate to reduce particle entrainment which contributes to holdup
    in the offgas recovery system for the fluidized bed operations.
    i. Filters and/or cyclones are provided above the expanded bed
    to separate elutriated particulates, fines, and dust from the exhaust
    gases. These are designed to return accumulated solids to the bed; for
    example, filters are equipped with an automatic cyclic blowback feature,
    or an external bin is designed to accumulate solids.
    j. Cyclones are equipped with suitable solids return lines that
    can be completely emptied for draindown of the reactor.
    k. Flow control valves and spray nozzles for feeding solutions
    to the fluidized bed are designed and installed to minimize cake
    formation on the nozzle or within the equipment.
    l. Components such as seal legs and valves having fixed
    openings are designed to minimize accumulation and obstruction by
    particulate matter.
    m. Holes drilled in perforated support plates are conical to
    reduce the area of flat surfaces on which solids may stagnate and cake
    during reaction.
    n. If the operation of the bed can result in the buildup of
    large particles that cannot be drained readily, the reactor is equipped
    with a gas-jet grinder.
    o. The vessel for the fluidized bed has a tapered bottom to
    preclude the accumulation of material such as sintered SNM in corners at
    the bottom.
3. External Design
    a. Clearance is provided to permit external use of
    nondestructive assay instruments or internal probes to detect the
    presence of or to identify the location of residual material not
    visually accessible.
    b. The body of the fluidized bed reactor is equipped with
    vibrators or external impactors to reduce or prevent packing and
    adhesion of SNM.
    c. Extended heat transfer surfaces, for example fins and tubes,
    for both heating and cooling are external to the fluidized bed
    containment structure. An alternate source of heat may be preheated
    inputs.
    d. Fluidized bed structures are electrically grounded to
    prevent buildup of static charge which causes bed expansion and
    consequent occurrence of holdup.
4. Design for Cleanout Where Necessary
    a. Driers are provided with access ports, removable covers, or
    removable sides for visual inspection of the internal surfaces.
    b. Access ports or removable panels are provided for cleaning
    internal surfaces by appropriate methods such as brushing, vacuuming,
    washing, scraping, or rinsing to remove, dislodge, or dissolve SNM
    particles.
    c. Equipment is provided with fittings for connections for
    washdown and rinsing with liquids that will remove, dislodge, or
    dissolve all particulate process material, residual liquid, and
    condensed vapors that may remain on internal surfaces after the
    equipment has been shut down.
    d. Provision is made for draining and collecting rinsings in
    which SNM may be entrained or dissolved.
    e. If multiple stages in fluidized bed reactors employ
    horizontal surfaces such as perforated gas distributor plates,
    downcomers, flanges for segmentation, deflection baffles for mixing, and
    plate baffles for partitioning, these are accessible for cleanout.
    f. Supplementary internal mechanical equipment not permanently
    mounted such as scrapers, agitators, rinsers, or atomizers inside
    equipment is capable of being disassembled and removed for cleaning and
    inspection.
    g. A bottom outlet is provided to facilitate draindown and
    cleanout.
    h. A gas plenum region or suitable packing material is used to
    prevent the bottom outlet from becoming encrusted, which may hinder the
    discharge of fluidized bed material during equipment draindown and
    cleanout.
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