Sample Submission Guidelines

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The following information is requested for all samples submitted to Micromeritics Pharmaceutical Services (MPS) for analysis. A sample submission form is needed for all projects. Please include either a purchase order or credit card number for billing purposes. If you are a new customer and have not submitted samples previously, please also complete our on-line customer information sheet to set up your account.

The more information you can supply about your sample, the faster we can get the results back to you. We have to make critical decisions prior to analyzing your sample and the more information we have, the better our ability to choose correctly and obtain good results on the first try.

Samples submitted for gas adsorption or BET should also include degasing or preparation procedures. Samples submitted for particle size should also include information about how to properly disperse the sample. For chemisorption samples, we need to know the proper preparation procedure and analysis gas prior to analysis. Please contact us if you have any questions or to discuss options.

General Requirements:

Make sure the sample supplied is representative of the entire sample. MPS personnel can representatively divide the sample as needed for a given analysis.

Analysis method development usually requires at least three times the recommended minimum sample quantity and is not included in the list price for analysis.

Identify each sample and give chemical name if available. MPS personnel need to know what materials they are analyzing! Also, identify liquid and any additives for sample submitted as slurry or dilute dispersion.

Supply known hazards to personnel or instruments. Include Material Safety Data Sheet (MSDS) if available.

Give sample preparation/analysis procedures if known, or if trying to duplicate a previous analysis.

What is maximum temperature (specify °C or °F) to which a sample may be heated to prepare the sample?

What is maximum usable heating rate if it is critical?

For Absolute Volume and Density by Gas Pycnometry:*

Requires at least 0.1 cm3 true sample volume. Maximum sample size is right cylinder 46 mm OD x 61 mm L.

Liquid density determination requires at least 25 mL of a low-vapor-pressure liquid; for example, no higher than the vapor pressure of water at 25 ºC.

For density determination at a specific temperature within 10 to 50 °C range, specify temperature.

For determination of the open-cell content of rigid cellular plastic, supply enough material to cut two 25.4-mm (1-in) cubes, and give the density of the solid, unexpanded resin used to make the foam. Ideally, all six faces of the cubes should be cut by the same technique.

For Envelope Volume and Density by Dry-Powder Pycnometry:*

Smallest pieces (granules) usable are nominally 3 mm in shortest dimension, and the largest piece usable is a right cylinder 45 mm OD x 45 mm L. Sample should have at least 0.5 cm3 envelope volume for best results.

Supply absolute sample density if specific pore volume and percent porosity determinations are desired. The MPS can determine (at additional charge) the absolute sample density if unknown.

For Bulk Volume and Density by Mercury Displacement:

Largest usable piece is a right cylinder 25 mm OD x 25 mm L.

For (Transverse Axial Pressure) T.A.P.TM Density using GeoPyc 1360 Analyzer:*

Requires at least 250 cm3 sample volume before compaction. If result should compare with traditional "tap density," please supply measurement conditions and expected "tap density" and repeatability.

For Specific Surface Area by Physical Adsorption:*

Generally, for good precision (repeatability) with nitrogen adsorptive, there should be at least 10 m2 of total sample surface area available in the sample tube. Using the Gemini (balanced-tube) technique with nitrogen adsorptive, only 1 m2 of available sample surface area is needed for good precision. Good precision also is possible using krypton adsorptive with just 0.5 m2 of total sample surface area. Smaller total surface areas can be measured, but analyses are less precise. The smallest sample quantity (grams) needed for a good analysis is found by (recommended minimum total surface area available for analysis) ¸ (estimated specific surface area of the sample). If available, please supply at least five grams of sample. The largest usable sample piece for standard analyses should fit through a 9-mm bore.

For Meso- and Micro-Pore Volume / Size Distribution by Physical Adsorption:*

Follow the guidelines under "Specific Surface Area by Physical Adsorption" above. For a general guide to sample quantity, supply at least five grams of powder or four pieces which will fit through a 9-mm bore.

Also, provide approximate specific surface area and pore volume.

For Particle Size Distribution (PSD) by SediGraph 5100 Analyzer:

Requires at least 10 grams of powder or 500 mL of slurry. Identify slurry liquid and supply density and viscosity values at approximately 33 °C. Also identify any surfactants present.

Supply sample skeletal density if known. If sample skeletal density is not known, MPS personnel can use a handbook value or measure (at additional cost) the skeletal density.

For PSD using either Laser Light Scattering or Electrical Sensing Zone Technique:

Requires at least 1.5 grams of powder or 200 mL of slurry with low solids concentration, for example, process water. Smaller amounts of more concentrated slurries may be supplied.

If known, supply sample solubility for water, alcohols, and acetone.

For PSD by Optical Imaging using OptiSizer PSDA 5400:*

For most OptiSizer analyses where the largest particles are approximately 8 mm, at least 500 cm3 of sample is needed. To be representative, coarser samples require more and finer samples require less than the recommended 500 cm3 quantity.

For PSD of Dry Powder by Sieve Analysis:*

Sample quantity requirement is the same as for the OptiSizer PSDA 5400 analysis.

For Chemisorption Studies:

Typically requires at least three grams of sample.

Type of chemisorption needed? Pulse / Dynamic with AutoChem II 2920 or Static-Volumetric with ASAP 2020C?

Adsorptive to be used (H2, CO, N2O, NH3, O2, etc.)?

Is differential analysis required to determine strong chemisorption? Generally, yes for ASAP 2020C volumetric analysis.

Has sample been dried, calcined, activated, reduced, etc.?

What pretreatment is required (dry, reduce, calcine, unique activation, etc.)?

What active metals are present? Identify each metal with approximate loading (weight percent).

What is the support (alumina, silica, clay, zeolite, etc.)?

What is preferred analysis temperature? Please note that, unless specifically requested otherwise, room temperature analyses are performed at 35 °C for better temperature control.

For Macro- and Meso-Pore Volume / Size Distribution by Mercury Intrusion Porosimetry:

Supply at least 5 grams of powder or 4 solid pieces. The largest usable piece is a right cylinder 25-mm diameter x 25-mm long (1 inch OD x 1 inch L), or a rectangular solid piece 17.5 x 17.5 x 25 mm (0.71 inch square x 1 inch L).

Supply approximate specific pore volume or any two of skeletal density, bulk density, or percent porosity.

* Asterisk denotes non-destructive analysis, and samples may be returned intact.

GENERAL NOTE: IUPAC1 recommends the following pore size classification:

Macropores have opening widths (diameters) > 50 nm.

Mesopores have opening widths (diameters) between 2 and 50 nm.

Micropores have opening widths (diameters) < 2 nm.

For reference, 1 nm = 10 Å = 0.001 µm.

1) Pure & Applied Chemistry, Vol. 57, No. 4, pp. 603-619, 1984