Wednesday, 10 August 2016

Volume  and Density Determination  Methods Using Manual Laboratory Devices

PYCNOMETRY ( SPECIFIC GRAVITY BOTTLES):- A pycnometer is a vessel with a precisely known volume. Although  a pycnometer is used to determine density  ρ  or specific  gravity,  it measures  volume  V; a balance is used to determine mass  m.  Manual  pycnometers (glassware)  typically  are used to determine the density  or specific gravity  of liquids  by  filling the vessel, then weighing. Density  is  calculated by  ρ  =  m/V  and specific gravity  by  the same equation and dividing  both sides by  the density of water with reference to temperature. First the object containing  the void  is weighed empty. It  is then filled with a  liquid  of known density  and reweighed. The  weight difference  ∆m  is the weight of the liquid  and from  these data, volume  can be calculated by V =  ∆m/ρ. As  will be  explained,  this  process  is used to ‘calibrate’ sample cells used in  mercury porosimetry. Another pycnometer method is to place a quantity  of a dry,  pre-weighed solid sample  in the  pycnometer and fill the rest of the pycnometer with a liquid of known density (typically  water), the weight of  the  pycnometer filled only  with the liquid having  previously been  established. The density  of the sample can be  determined  from  the known density  of the water,  the  weight  of the pycnometer filled only with the liquid, the weight  of  the  pycnometer containing  both sample and  liquid,  and  the weight of the sample.  This is a common  method used in characterizing  soil samples.

HYDROSTATIC WEIGHING ( DISPLACEMENT METHOD):- By  this  method,  the volume  of a solid sample is determined  by  comparing  the weight of the sample in air to the weight  of  the  sample immersed in a liquid of known density. The volume  of the sample is equal to  the  difference in  the  two  weights divided by  the density  of the liquid.  Conversely, if the volume  of a solid object is accurately  known, the density  of the  liquid  can be  determined  by  the loss of weight of the immersed  object.This is the basis for the hydrometer method. If  the sample is porous, one must determine  if the pores are to be included  or  excluded  from the  volume.   If  they  are to be included or the sample will react with  the  displacement medium,  a  sealing  coating  can be applied. If  pore volume  is to be excluded, the liquid must displace the air and completely  fill the  pores. Various pretreatment methods are used including  evacuation and boiling. When  determining  volume  by  directly measuring  the displaced volume,  liquids,  fine particles  or gases can be used as the displacement medium. If  the  sample  material  is porous,  fine  particles will not penetrate into the smaller pores that water  can  enter.  Mercury, being  a non-wetting  liquid, also will not penetrate pores under ambient pressure  as  will wetting  liquids. Gases, Helium  in  particular, will penetrate readily  into very  fine pores.

HYDROMETERS:- A  hydrometer is  a  vertical  float that measures the density  or specific gravity  of  a liquid  or liquid/solid suspension (slurry). The hydrometer,  inscribed  with a graduated scale along  its length, sinks into the  liquid  until  it  has displaced  a volume  of liquid equal in weight to that of the float.  Specific  gravity  or  density  is read directly  from  the inscribed scale at the liquid  surface  after buoyancy  and gravitational forces equalize.

FLOAT-SINK OR SUSPENSION (BUOYANCY) METHOD:-This  method  requires  a liquid of known and adjustable  density  in which the sample is placed. The  density  of the liquid is adjusted until the sample  either  begins  to  sink  or float , or is suspended  at  neutral  density  in the liquid.The  density  of the object is then equated to that of the liquid. This method also is used  to separate materials by  their density.

DENSITY GRADIENT COLUMN:-  A density gradient  column  is a column  of liquid that varies in  density  with height.  A sample is placed in the liquid  and observed to determine at what vertical  level in the column  the sample is suspended.    The  density  of the liquid at that level  is  the density  of the sample, and that value is determined by  standards of known density.

TAP DENSITY AND VIBRATORY PACKING  DENSITY:- These are very  similar methods for  determining the bulk  density  of a collection of  particles under  specific  conditions  of packing.   In  the former case, packing  is achieved by  tapping  the container and in the latter by  vibrating  the container. The particles under test should  not break  up under test conditions.

BULK/ENVELOPE VOLUME BY COATING:- Coating the sample allows  determination of  bulk  volume or apparent volume  of solids while preventing absorption  or reaction with suspension liquids. Penetration of the coating  into the  open  pores  of the sample must be considered. Following  the referenced method  the  mass of the sample is obtained. The  sample  is  dipped into molten wax of known density. After withdrawal, any  air bubbles in the  wax  coating are pressed out, and the coated  sample  is weighed.  The difference in  weight  before  and after  coating  is  the weight of the wax, and dividing  this  number  by  the density  of the wax provides the volume  of  wax  composing  the coating.   The volume  of the coated sample  is determined by  hydrostatic weighing.    From  this volume, the volume  of wax (or other coating)  is subtracted, yielding  the bulk  (or  envelope) volume  of the sample.

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