Everything about Microspheres
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  • Calculating microspheres per gram

    During scientific experiment design and analysis it is common to need to know the number of spheres per gram of dry material.  We have put together the table below to help speed up the process.

    If you have material of a density different from those listed in the table, divide the number of spheres per gram in the density ~1.0 g/cc column by the true particle density of your material to get an estimate of the number of spheres per gram.

    Product Size Polyethylene
    Density ~1.0 (g/cc)
    Soda Lime Glass
    Density ~2.5 (g/cc)
    Lower (um) Upper (um) Spheres per Gram Spheres Per Gram
    20 27 147,162,715 58,630,564
    27 32 74,393,558 29,638,868
    32 45 33,467,185 13,333,540
    45 53 16,233,536 6,467,544
    53 63 9,788,528 3,899,812
    63 75 5,813,720 2,316,223
    75 90 3,401,258 1,355,083
    90 106 2,029,192 808,443
    106 125 1,239,525 493,835
    125 150 734,672 292,698
    150 180 425,157 169,385
    180 212 253,649 101,055
    212 250 154,941 61,729
    250 300 91,834 36,587
    300 355 54,371 21,662
    355 425 32,196 12,827
    425 500 19,305 7,691
    500 600 11,479 4,573
    600 710 6,796 2,708
    710 850 4,025 1,603
    850 1000 2,413 961
    1180 1400 890 354
    1400 1700 513 204
    1700 2000 302 120
    2000 2360 184 73
    2360 2800 111 44
    2800 3350 66 26

    Note: This table assumes the mean diameter is half way between the upper and lower size.

  • Patent Review: Use of Adsorbent Carbon Microspheres for Treatment of Irritable Bowel Syndrome

    United States Patent 7,749,497 was recently issued to Ocera Therapeutics, Inc. (San Diego, CA) regarding the use of adsorbent carbon microspheres for the treatment of irritable bowel syndrome.

    The patent invention primarily describes the use of adsorbent carbon microspheres for the treatment of irritable bowel syndrome and symptoms associated with it.  Irritable bowel syndrome (IBS) is a gastrointestinal disorder characterized by altered bowel habits without the presence of detectable structural abnormalities. IBS is fairly common and makes up 20-50% of visits to gastroenterologists.  Most commonly, patients have abdominal pain associated with altered bowel habits that consist of constipation, diarrhea, or both. The other group consists of patients with painless diarrhea.

    One embodiment disclosed herein includes a method of treating one or more symptoms of irritable bowel syndrome by  administering to the subject adsorbent carbon microspheres with a particle size of 0.01mm to about 2 mm to reduce the abdominal discomfort or pain. In one embodiment, the amount of the adsorbent carbon microspheres is sufficient to achieve at least about a 50% reduction in the number of days the subject experiences abdominal pain or discomfort.

    In some of the embodiments, the adsorbent carbon microspheres have a particle size of about 0.05mm to about 0.8 mm. In some of the above embodiments, the adsorbent carbon microspheres have a specific surface area of about 700 m.sup.2/g or more as determined by a BET method. In some of the above embodiments, the adsorbent carbon microspheres have a specific surface area of about 700 m.sup.2/g to about 2500 m.sup.2/g as determined by a BET method.

    Microsphere Manufacturing Process:

    First, a dicyclic or tricyclic aromatic compound or a mixture thereof having a boiling point of 200.degree. C. or more is added as an additive to a pitch such as a petroleum pitch or a coal pitch. The whole is heated and mixed, and then shaped to obtain a shaped pitch. Thereafter, the shaped pitch is dispersed and granulated in hot water at 70 to 180.degree. C., with stirring, to obtain a microspherical shaped pitch. The aromatic additive is extracted and removed from the shaped pitch by a solvent having a low solubility to the pitch but a high solubility to the additive. The resulting porous pitch is oxidized by an oxidizing agent to obtain a porous pitch subject to heat infusibility. The resulting infusible porous pitch is treated at 800 to 1000.degree. C. in a gas flow such as steam or carbon dioxide gas reactive with carbon to obtain a porous carbonaceous substance.

    The resulting porous carbonaceous substance is then oxidized in a temperature range of 300 to 800.degree. C., preferably 320 to 600.degree. C., in an atmosphere containing 0.1 to 50% by volume, preferably 1 to 30% by volume, particularly preferably 3 to 20% by volume, of oxygen. The substance is thereafter reduced in a temperature range of 800 to 1200.degree. C., preferably 800 to 1000.degree. C., in an atmosphere of a non-oxidizable gas to obtain the final product. More details of suitable production processes and suitable products may be found in U.S. Pat. Nos. 4,681,764 and 6,830,753 and U.S. Application Publication No. 2005/0112114, filed May 26, 2005, all of which are incorporated herein by reference in their entirety. Suitable adsorbent carbon microspheres are commercially available from Kureha Corp., and is sold in Japan under the trade name KREMEZIN.RTM. (also known as AST-120).

    Administration of the Microspheres to the Patient:

    For use as described herein, adsorbent carbon microspheres may be administered to the gut of a subject by any suitable means. In one embodiment, the carbon is administered orally. Formulations for oral administration may include, but are not limited to, free flowing microspheres, granules, tablets, sugar-coated tablets, capsules, suspensions, sticks, divided packages, or emulsions. In the case of capsules, gelatin capsules, or if necessary, enteric capsules may be used. The oral dosage administered to a subject may be any amount suitable to achieve the desired therapeutic result. In some embodiments, the oral dosage in the case of a human is about 1 to 20 g of the adsorbent per day.

  • Patent Review: Preparation of Swellable and Deformable Microspheres

    United States Patent number 7,794,755 was issued on September 14, 2010, describing the process for preparation of swellable and deformable microspheres. The patent is assigned to E.I. du Pont de Nemours and cites Figuly, Mahajan, and Schiffino as inventors.

    A process for producing microspheres was developed that provides microspheres with new combined properties of high density, low fracture, high swell capacity, rapid swell, and deformability following swell. The process is reliable and high yielding, and makes use of a low temperature azo initiator and a small molecule chlorinated solvent as the organic phase. The microsphere preparation made using the process is particularly useful in medical treatments such as embolization.

    The patent describes a need for microspheres with properties that are advantageous for many types of applications, including medical applications. Microspheres with high density, yet a large capacity to swell in an aqueous environment, would be useful for absorption applications such as small-scale spill control and for delivery applications in which they would carry and release active ingredients such as fertilizers, herbicides, pesticides, cosmetics, shampoos, and medications. Microspheres with additional properties of durability and deformability would provide a valuable material for introduction into animals, including humans, for applications such as tissue augmentation, void filling, wound treatment, and embolization. Tissue augmentation involves introduction of materials in a collapsed area to provide a filling function, such as the treatment of scars or wrinkles. Void filling involves introduction of materials into an empty space, such as one created by removal of a tissue mass. Wound treatment involves introduction of materials to stop bleeding, provide padding, deliver medication, and absorb fluids. Such materials are useful especially in emergency situations including accidents and military operations. Embolization treatment involves the introduction of a material into the vasculature in order to block the blood flow in a particular region, and may be used to treat non-cancerous tumors, such as uterine fibroids, and cancerous tumors, as well as to control bleeding caused by conditions such as stomach ulcers, aneurysms, and injury. Blockage may be desired in the case of arteriovenous malformation (AVM), where abnormal connections occur between arteries and veins. Additionally, blockage may be desired for pre-surgical control of blood flow.

    The patented process makes use of a water soluble, low temperature-active azo initiator in an aqueous solution of monomer, crosslinking agent, and emulsifier. A chlorinated organic medium is used in forming a suspension with the aqueous solution. The aqueous solution and organic medium both additionally include protecting colloids. The aqueous solution and organic medium, as well as the mixture of the two, are initially held below the initiation temperature of the azo initiator. The organic medium, which may comprise a chloroform and methylene chloride mixture, should have a high enough boiling temperature that the aqueous soluble azo initiator can be activated to cause polymerization producing microspheres.

    A prevalence of the microspheres are in the size range of about 25 to about 250 microns in diameter, as seen when analyzing a small sample size of microspheres. A heterogeneous size mixture of microspheres may be separated into microsphere samples of specific size ranges, if desired, for specific applications. Microspheres may be separated by methods such as fluidized bed separation and custom sieving, also called screen filtering.

    The swell capacity (amount of water uptake) of microspheres prepared by the described process may vary depending on the amount of crosslinking agent added to the first solution. For example, crosslinking agent may be added in such an amount as to impart a swell capacity to the microspheres of about 50 grams of water per gram of microspheres, an amount to impart a swell capacity of about 70 grams per gram of microspheres, and alternatively an amount to impart a swell capacity of about 100 grams per gram of microspheres.

    An additional attribute of the microspheres prepared by the present process is the capacity to deform following swell. When placed under pressure, the swelled microspheres do not maintain their substantially spherical shape, but compress in the axis of the pressure and expand in the axis that is perpendicular to the pressure. Thus environmental factors, such as pressure of a flowing medium or from the walls of an enclosing container, may cause deformation of the microspheres. In addition, pressure of individual microspheres next to each other may cause deformation. This ability to deform is thought to be imparted and enhanced through the closed cell void structure of the microspheres.

    This ability to deform allows the microspheres to take on a shape of a containing space, and to fill that space. Additionally, deformed microspheres have increased surface area contact with each other, as compared to the contact area between spherical beads. The increased surface area contact between the deformed microspheres provides a more compact structure than is achievable with non-deforming spherical microspheres. This compact structure provides high resistance to penetration. The deformability is highly desirable in some applications such as in embolization treatment, where the deformed, compact microspheres may provide strong blockage at target vascular sites.

  • Motivations for Using Biodegradable Microspheres in Drug Delivery

    In recent years there is significant interest in using biodegradable polymeric microspheres for drug delivery. Delivering drugs through biodegradable microspheres has numerous advantages compared to conventional delivery systems. While in conventional systems the drug is usually released shortly after delivery and stops working after a brief period of time, biodegradable polymer offers a way to provide sustained release over a longer time, thus eliminating the need for multiple doses and ensuring sustained and controlled drug delivery over weeks or months. Continue reading “Motivations for Using Biodegradable Microspheres in Drug Delivery” »

  • Chitosan microspheres prepared by spray drying

    Spray drying has been used in the production of fine powders from emulsions for many years, but it is not a process in which most people associate the production of microspheres.  This journal article shows how the authors were able to produce highly spherical microspheres in the 2-10um range by controlling the levels of Chitosan and crosslinking agents used.

    Chitosan MicrospheresThe key items I found of interest in this article were:

    The quality of the microspheres that were produced, as seen the the attached SEM micrograph.

    How the process variables did not affect the zeta potential of the microspheres produced (Table 4 below), and how the size can be varied by varying the concentrations of Chitosan or the Molecular weight (MW). Continue reading “Chitosan microspheres prepared by spray drying” »