Radiant energy – Ionic separation or analysis – Ion beam pulsing means with detector synchronizing means
Reexamination Certificate
2002-11-01
2004-09-07
Berman, Jack (Department: 2881)
Radiant energy
Ionic separation or analysis
Ion beam pulsing means with detector synchronizing means
C250S288000, C073S028040, C073S865500, C324S452000
Reexamination Certificate
active
06787763
ABSTRACT:
FIELD OF THE INVENTION
The invention relates to a method and apparatus for sizing and classifying charged particle or ions in a differential mobility analyzer.
BACKGROUND OF THE INVENTION
Differential mobility analyzers (DMAs) are the most powerful instruments available for sizing and classifying particles, especially in the diameter range below 100 nanometers. The most common DMA design involves two concentric cylindrical electrodes. The commercial versions of various instruments have served rather well the aerosol community's for several decades. A number of cylindrical designs have been studied, with different ratios between the electrode radii R
1
and R
2
and the axial distance L between inlet and outer slits for the aerosol flow. Other geometrical variations upstream the inlet or downstream the outlet slits have been tested for special purposes such as reducing the particle losses or the pressure drop, or for improving flow laminarity at moderate Reynolds number or to reach unusually high Reynolds numbers. As is well known to those skilled in the art, the Reynolds number is a dimensionless number which is equal to the density of a fluid times its velocity times a characteristic length, divided by the fluid's viscosity coefficient.
DMAs are used to separate small charged particles suspended in a gas according to their electrical mobility Z. They combine particle-free fluid flow (the sheath gas) and electric fields to drive charged particles introduced through a first narrow slit (the inlet or injection slit) located in a first electrode into a second narrow slit located in a second electrode. The space between these two slits and electrodes will be referred to as the “working section” of the DMA. Ideally, among the particles introduced through the injection slit, only those with mobilities contained within a relatively small range &Dgr;Z centered about a mean value Z are sampled through the outlet slit. The inverse of the ratio &Dgr;Z/Z is a measure of the DMA resolution. Traditionally, DMAs have been used for the separation of particles considerably larger than 5 nanometers. However, developments over the last decade have made these instruments suitable also for the separation of particles a few nanometers in diameter, and even smaller ions. Their use in the analysis of suspended ions and macroions is therefore of considerable practical interest. Such applications would benefit from the development of instruments of higher resolution and wider range than those that have been traditionally available. It should be noted that the term ion, as used in the instant application, refers not only to molecular ions, but also to charged clusters and in general to any charged particle.
The main obstacle limiting DMA resolution in the nanometer diameter range is Brownian motion. It is known that the associated peak broadening can be reduced considerably by two different means: (a) a geometrical design taking advantage of the existence of an optimal relative positioning between the two slits, and (b) increasing the Reynolds number (Re) of laminar operation of the sheath gas flow in the DMA to values as large as possible. Rosell-Llompart et al., Minimization of the diffusive broadening of ultrafine particles in differential mobility analyzers, in Synthesis and Characterization of Ultrafine Particles, pp. 109-114 (1993), the subject matter of which is herein incorporated by reference in its entirety, discloses high Reynolds number formulation accounting only for Brownian diffusion broadening in cylindrical DMAs. The relative full width &Dgr;Z/Z of the mobility peak associated to particles of fixed mobility Z can be written as
(&Dgr;
Z/Z
)
2
=16ln2
D
/(
L*U
)(
b
+1
/b
); (1)
b=L/L*; L*
2
=(
R
2
2
−R
1
2
)
2
/[2(
R
2
2
+R
1
2
)]. (2,3)
D is the diffusivity of the particles, related to their electrical mobility Z via
Z=De
/(
kT
), (4)
whore e is the elementary charge (the particles are taken to be singly charged), k Boltzmann's constant and T the absolute temperature. R
1
and R
2
are the radii of the inner and outer cylindrical electrodes. L is the axial distance between the
1
inlet and outlet slits, and U is the fluid velocity, taken to be independent of the radial coordinate r (plug flow). Suitable generalizations exist of these results for other velocity profiles, plane geometries, and even converging two-dimensional or axisymmetric situations. But equations (1-3) are representative of such broader cases, and suffice for the purposes of the present discussion. Since (b+1/b)≧2, it is clear that, at given radii R
1
and R
2
and fixed speed U, the resolution is maximized when the length L is equal to L*. The advantages of using DMAs of near-optimal length were first demonstrated experimentally by Rosell-Llompart et al. (1993).
The need to use very high Reynolds numbers follows also immediately from (1). L* coincides with the width &Dgr;=R
2
−R
1
of the working section in the limit of a small gap, &Dgr;<<R
2
(when R
1
tends to R
2
), and is reasonably close to it even if R
1
/R
2
differs substantially from unity (L*/&Dgr;=0.843 when R
1
/R
2
=0.222). Hence, the ratio D/(L*U) is fairly close to the Peclet number defined here as
Pe=D
/(&Dgr;
U
).
For the purposes of separating efficiently small species according to their mobility, it is desirable that &Dgr;Z/Z be as small as 1%, even for ions with diameters as small as 1 or 2 nanometers. Since (b+1/b)≧2, this requirement implies that L*U/D>2.22×10
5
. Note also that small ions in standard air have mobilities of 2 cm
2
/V/s, with associated diffusivities D=0.05 cm
2
/s. The dimensionless ratio between the kinematic viscosity of air v (=0.15 cm
2
/s) and D is therefore v/D=3, and the quantity UL*/v (close to the Reynolds number Re=U&Dgr;/v ) needs then to be as high as 0.74×10
5
. We shall see that, in order to cover a wide range of particle sizes, it is convenient to use DMAs with a distance L between the inlet and outlet slits as large as 3L* or even larger (b>3), in which case the resolution is reduced by a factor [(b+1/b)/2]
½
. To compensate for this effect calls for Reynolds numbers (Re) in excess of 10
5
.
The need for high Reynolds (or Peclet) numbers to moderate diffusion in convective diffusive flows is well known. However, the practical exploitation of this knowledge is made difficult by the natural tendency of high Reynolds number flows to become turbulent, as well as by the difficulties associated to the generation of the rather large flows required. For instance, Rosell, J., I. G. Loscertales D Bingham and J. Femández de la Mora “Sizing nanoparticles and ions with short differential mobility analyzer”, J. Aerosol Science, 27. 695-719, 1996, have demonstrated an ability to reach Reynolds numbers as large as 5000 in a variant of the widely used DMA disclosed by Winklmair, et al., A New Electro-mobility Spectrometer for the Measurement of Aerosol Size Distributions in the Size Range from 1 to 1,000 nanometers, J. Aersol Sci., Vol. 22, pp. 289-296 (1991), (commonly referred to as the “Vienna DMA”). But they needed flow rates of some 800 liters/minute, with associated pressure drops close to half an atmosphere. Under such conditions it would have been rather difficult to attain the desired range of Reynolds numbers up to 10
5
.
Some important aspects of the problem of achieving high Reynolds numbers, while avoiding turbulent transition, have been addressed in U.S. Pat. No. 5,869,831 and U.S. Pat. No. 5,936,242, both to de la Mora, et al., the subject matter of which are herein incorporated by reference in their entirety, following the method of greatly reducing the level of perturbations in the inlet sheath gas flow by means of several stages of laminarizing screens and filters followed by a large contraction which accelerates substantially the sheath gas prior to the working section. For brevity, this l
De La Mora Juan Fernandez
Labowsky Michael J.
Berman Jack
Carmody & Torrance LLP
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