SAX /WAX

BY
PRIYADHARSHINI N
ABBREVIATION OF SAXS AND WAXS

SAXS- Small Angle X-Ray Scattering

WAXS- Wide Angle X-Ray Scattering

INTRODUCTION:
Determine the micro and nano structure and phase
behaviour of multi component system.
Example: Cosmetics, Polymers, Detergents.
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SAX-Scattering angle lies between 0°- 10°
Used to study the structure of composites and polymers
WAX- Scattering angle lies between 10°-160°
Used to study fibers and polymers.
SMALL ANGLE X-RAY SCATTERING:
 SAXS is an instrument to be capable of delivering structural information about
partially or completely disordered system of macromolecules between 5 and
25nm.
 Gives information about macromolecular folding,unfolding,aggregation.
 Technique where elastic scattering of monochromatic x-rays are used .
Wavelength 0.1-0.2nm.
 Ultra-SAXS can resolve even large dimensions(150 nm). It is used to study
large colloidal structures.
SAXS INSTRUMENT :
 SAXS instrument a monochromatic beam of x-rays is brought to a sample from
which some of the x-rays scatter while most simple go through the sample
without interacting with it.
 The scattered x-rays form a scattering pattern which is then detected at a
detector which is typically a 2-dimensional flat x-ray detector situated behind
the sample perpendicular to the direction of the primary beam that initially
hit the sample.
 The scattering pattern contains the information on the structure of the
sample.
 The major problem of SAXS instrumentation is the separation of the weak
scattered intensity from the strong main beam.
 The smaller the desired angle is more difficult to become this scattering.
LABORATORY SAXS INSTRUMENT TYPE :
 Point Collimation Instrument
 Line Collimation Instrument
POINT COLLIMATION INSTRUMENT :
 Point collimation instruments have pinholes that shape the x-ray beam to a small
circular or elliptical spot that illuminates the sample.
 Thus the scattering is centro -symmetrically distributed around the primary x-ray
beam and the scattering pattern in the detection plane consists of cricles around the
primary beam.
 This measuring time is much larger that it takes in range of long hours or even a day

 It used to determine the anisotropic system .example : Fibres , Sheared liquid.

LINE COLLIMATION INSTRUMENT :
 Line Collimation Instruments restrict the beam only in one dimension.
 So that the beam cross section is a long but narrow line.
 The illuminated sample volume is much larger compared to point collimation
and the scattered intensity at the same flux density is proportionally large.
 Thus measuring times are much shorter compared to point collimation and
are in the range of minutes.
 It used to determine the isotropic nanostructured materials. Example:
proteins, surfactants, particle dispersion.
APPLICATION :

 Mesoporous materials
 Liquid crystal
 Micro emulsions
 Polymers
 Nano powder
 Nano composites
 Bio macro molecules
WAXD/WAXS:
 It commonly used to characterize crystalline structures of polymers and
fibers.
 The technique uses monochromatic x- ray radiation to generate a
transmission diffraction pattern of a specimens that does strongly absorb x-
rays such as organic or inorganic specimens containing light elements.
 Wide angle x-ray diffraction or scattering refers to x-ray diffraction with a
diffraction angle 2> 5.
WIDE ANGLE X-RAY DIFFRACTION:
 The incident x-ray beam is formed after x-rays pass through a monochromator
and a collimator.
 The highly monochromatic and parallel x-ray beam strikes a sample and
generates a diffracted beam at angle 2 with respect to the transmitted beam.
 The diffracted beams are recorded as an image on a film or by an area
detector that is placed at distance D from the specimen and perpendicular to
the incident beam direction.
 The beam stop is placed infront of the detector center to prevent beam from
striking the film or area detector directly.
 The WAXD is a photographic method, differing from the spectroscopic methods
of diffractrometry.
Ri is the distance between the transmitted beam and diffracted beam on the
recording film plane.
Θi is the incidence angle.
ORIENTATION OF POLYMER CRYSTAL:

 The main reason for using WAXD for polymer analysis is that crystalline
polymers are frequently presented in the form of fibers with preferential
crystal orientation with respect to the fibers axis.
 For example, a-b crystallographic plane is perpendicular to fiber axis that is
along a vertical direction.
WIDE ANGLE X-RAY SCATTERING:
 Wide angle x-ray scattering (WAXS) is considered to be an appropriate
technique for examining both crystalline and non crystalline materials.
 WAXS is particularly useful for polymers because a non crystalline
(amorphous) structure is the common characteristics of polymers, even for
crystalline polymers because they are no totally crystalline.
APPLICATION :
 Particle shape
 Specific surface area
 Pore size distribution
 Liquid crystalline phases
 Agglomeration behaviour of nano particles
 Particle structure
ADVANTAGES
 Non destructive method.
 SAXS over crystallography is that a crystalline sample is not needed.
 Accurate
 Quantitative
 Small sample size possible
DISADVANTAGES

 Complex / expensive instrumentation

 Complex data analysis
 Low information content
 High cost
REFERENCES :
 http://www.malvernpanalytical.com/en/products/technology/xray-scatterin
g/small-angle-x-ray-scattering
 http://biosaxs.com/technique.html
 http://www.slideshare.net/kalyannagaon/small-angle-x-ray-scattering-74903
532
 https://en.ppt-online.org/32598
 https://en.Wikipedia.org/wiki/wide-angle_X-ray_scattering