Condensation apparatus
10792694 ยท 2020-10-06
Assignee
Inventors
Cpc classification
B05C3/02
PERFORMING OPERATIONS; TRANSPORTING
Y10T137/6416
GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
B05C3/005
PERFORMING OPERATIONS; TRANSPORTING
B01D5/0027
PERFORMING OPERATIONS; TRANSPORTING
International classification
B05C3/00
PERFORMING OPERATIONS; TRANSPORTING
B05C3/02
PERFORMING OPERATIONS; TRANSPORTING
Abstract
Apparatuses for increasing the effective size of gas-entrained particles in a particle detector are disclosed. In one embodiment, an apparatus comprises an evaporation chamber, a condenser in fluid communication with the evaporation chamber, and an inlet in fluid communication with the condenser for receiving a stream of sample gas containing gas-entrained particles. The evaporation chamber includes a heating element and a porous support surrounding the heating element. The porous support carries thereon a working fluid, and the heating element vaporizes the working fluid to form vapor within the evaporation chamber. The porous support may include a portion which extends into a working fluid reservoir.
Claims
1. An apparatus for increasing the effective size of gas-entrained particles in a particle detector, the apparatus comprising: an evaporation chamber; a heating element and a porous support each of which is disposed within the evaporation chamber, the porous support carrying thereon a working fluid and the heating element configured to vaporize the working fluid to form vapor within the evaporation chamber; wherein the porous support surrounds the heating element; a working fluid reservoir disposed in the evaporation chamber, the working fluid reservoir being configured to hold a working fluid, wherein the porous support includes a portion which extends into the working fluid reservoir; a condenser in fluid communication with the evaporation chamber for receiving said vapor; the condenser having an outlet for connection to a panicle detector; and an inlet in fluid communication with the condenser for receiving a stream of sample gas containing gas-entrained particles; the apparatus being configured so that condensation of the vapor onto the gas-entrained particles in the sample gas takes place in the condenser to increase the size of the particles for detection by a particle detector.
2. The apparatus of claim 1, wherein the inlet is provided in fluid communication with evaporation chamber, wherein the inlet is configured such that the stream of sample gas is mixed with the vapor in the evaporation chamber and is transported through the condenser.
3. The apparatus of claim 1, comprising a temperature sensor disposed within the evaporation chamber.
4. The apparatus of claim 1, comprising a cooling means operationally connected to the condenser to provide cooling of a mixture of gases, vapor and particles in the condenser.
5. The apparatus of claim 1, wherein the condenser has a surface area to volume ratio greater than the surface area to volume ratio of a cylinder.
6. The apparatus of claim 1, comprising means for removing condensed substance from the interior walls of the condenser.
7. The apparatus of claim 1, comprising means for varying a temperature of the porous support and/or a temperature of the condenser or its parts.
8. The apparatus of claim 1, wherein the condenser comprises: a condenser body having a condenser inlet, the outlet, and a hollow interior which has an internal length, an internal width and an internal height; the condenser inlet providing fluid communication with the evaporation chamber; an inlet flow distributor tube connected to the condenser inlet and extending across the internal width of the condenser body; and an outlet flow distributor tube connected to the outlet and extending across the internal width of the condenser body; wherein the internal height of the condenser body is less than a corresponding internal height of each of the inlet and outlet flow distributor tube; inlet and outlet flow distributor tubes each being provided in the walls of the condenser with one or more slots or holes communicating with the hollow interior of the condenser body so as to provide a flow path from the inlet flow distributor tube through the hollow interior of the condenser and into the outlet flow distributor tube.
9. The apparatus of claim 8, wherein an internal cross sectional area of each flow distributor tube is greater than an internal cross sectional area of the condenser body, wherein the internal cross sectional area of the condenser body is defined as internal widthinternal height.
10. A condensation particle counter comprising the apparatus of claim 1.
11. An assembly comprising the apparatus of claim 1 connected to a particle detector.
12. An assembly comprising a plurality of apparatuses of claim 1 connected sequentially or in parallel.
13. The apparatus of claim 1, wherein the heating element comprises a rod portion and the porous support surrounds the rod portion.
14. The apparatus of claim 13, wherein the porous support is formed from a porous fabric and comprises a sleeve that fits over the rod portion of the heating element.
15. The apparatus of claim 13, wherein the rod portion of the heating element has a hollow interior within which is disposed a heater wire or heater probe and a thermocouple.
16. The apparatus of claim 15, wherein a thermally conductive filler is used to hold the heater wire or heater probe and the thermocouple in place.
17. The apparatus of claim 1, comprising a working fluid selected from dimethyl phthalate, dioctyl phthalate and dimethylsulphoxide.
18. The apparatus of claim 1, wherein the evaporation chamber is configured for receiving a stream of carrier gas for carrying vapor through to the condenser.
19. The apparatus of claim 18, wherein the carrier gas is provided by an additional inlet in fluid communication with the evaporation chamber.
20. The apparatus of claim 18, wherein the carrier gas and sample gas are provided by the inlet.
21. The apparatus of claim 1, wherein the heating element is in direct contact with the porous support.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1)
(2)
(3)
(4)
(5)
(6)
(7)
(8)
(9)
(10)
(11)
(12)
(13)
(14)
(15)
(16)
(17)
(18)
(19)
(20)
DETAILED DESCRIPTION OF THE INVENTION
(21) The invention will now be illustrated in greater detail by reference to the specific embodiments described in the following non-limiting examples.
(22)
(23) A stream of air containing small gas-entrained particles (e.g. airborne particles) is drawn into the chamber 1a via inlet 4a by means of a pump (not shown). As it passes through the evaporation chamber, the stream of air is heated and saturated with vapour formed by evaporation of the working fluid. The vapour-saturated stream of air then passes into the condenser where cooling of the air and condensation of the working fluid onto airborne particles takes place. As a result, the particles grow by condensation up to a readily detectable size of about 1 m.
(24) The enlarged particles pass out through the outlet 5a, and are directed to an optical particle counter where they are counted.
(25) The condensation apparatus illustrated in
(26) One major disadvantage is that the working fluid must be replaced on a regular and frequent basis.
(27) A further disadvantage is that the apparatus is very slow to warm up to an operating state. In the case of the TSI CPC 3007 described above, the apparatus has a 600 second warming up time before it can be used.
(28) Another disadvantage is that the layout of the apparatus does not readily lend itself to miniaturisation. Reducing the size of the apparatus would necessitate using a smaller working fluid cartridge which would therefore need to be refilled more frequently. Thus, miniaturisation would lead to a reduction in the period of time over which the apparatus could be used without refilling.
(29) A further disadvantage is that the abovementioned TSI CPC 3007 instrument cannot be used in an environment of elevated pressure and, according to its product specification, the instrument will only operate when held horizontally.
(30) The relatively rapid depletion of working fluid in the cartridge in the CPC shown in
(31) The condensation apparatus of the invention overcomes or at least alleviates the problems identified above with known CPCs.
(32) A condensation apparatus according to a first embodiment of the invention is shown in
(33) In use, a stream of clean carrier gas (e.g. air) which has been filtered through a filter (not shown) and which contains no (or negligible quantities of) detectable aerosol particles enters through inlet 1 into the evaporation chamber 2. In the evaporation chamber, heating element 3 is positioned to be in a good thermal contact with temperature sensor 4 and a predetermined temperature that is sufficient to evaporate working fluid and to generate conditions necessary to sustain condensation of the working fluid on particles of interest is controlled by temperature control device 5 which is linked to the temperature sensor. The working fluid is contained in a porous support that takes the form of a cover 6 that is placed on the heating element 3. In the case of a cylindrical heating element, the cover will be wrapped around its surface and soaked with the working fluid. As a result, the stream of clean air introduced via the inlet 1 is saturated with the vapour of the working fluid and moved towards the condenser/outlet 7. A gas (e.g. air) sample containing nano-particles of interest is introduced into the chamber through the second inlet 8. In the zone between the inlet 8 and the opening into the condenser 7, supersaturation of the working fluid vapours arises due to mixing of the hot saturated vapour and the unheated stream of sample gas containing the nano-particles of interest. Therefore, in this zone, heterogeneous nucleation of the working fluid on the particles of interest begins to occur. When the mixture of vapour and sample gas containing the nano-particles enters the condenser 7, additional supersaturation occurs due to cooling of the gases and vapour by the walls of the condenser/outlet. The excess of heat is removed from the surface of the condenser/outlet 7 by means of a cooling system 10. In
(34) As an example of the apparatus of shown in
(35) The temperature was controlled by a Digitron Temperature controller 5. It was found that the condensation apparatus thus constructed was able to enlarge nano-particles up to 1 to 2 m diameter. The condensation apparatus was used over a period of at least 2 months without refilling.
(36) Another embodiment of the present invention is shown in
(37) The mode of action of this embodiment is the same as for the embodiment of
(38) A further embodiment of the invention is illustrated in
(39) The shape of the condenser/outlet 7 can affect its performance. In the embodiment shown in
(40) The second inlet 8 can also have a rectangular or elongated oval cross sectional shape. In practice, the ratio of the height to the width of the rectangle can be from 1 to 100.
(41) In each of the embodiments shown in
(42) The cross sectional shape of the main body of the condensation chamber 2 can also be rectangular as can the cross sectional shape of the heating element 3. The heating element 3 is typically positioned and orientated so as to optimise the efficiency with which the stream of carrier gas entering the first inlet 1 is saturated with the working fluid vapour.
(43) If the width of the rectangular cross section condenser shown in
(44)
(45) It is advantageous to control the temperature of the liquid in the working fluid containers 16 to stabilise the temperature of the condenser. This can be done using an external cooling element (e.g. thermoelectric cooling element) as shown in
(46)
(47) The chambers 16 each have an additional outlet 18 and the two outlets are connected by a length of tubing. The inlets/outlets 17 are connected via lengths of tubing to a pump 19 and a temperature controller 20. Together, the inlets/outlets 17 and 18, the connecting tubing, the pump 19 and the temperature controller 20 form a circuit around which the working fluid can be pumped. The working fluid flowing around the circuit and through the fluid collection chambers 16 can be maintained at a constant pre-determined temperature by the temperature controller 20 and, in this way, the temperature of the internal surface of the condenser can be controlled.
(48) The circuit is provided with a valve (not shown) that enables a portion of the working fluid to be directed along tube 21 to a reservoir 12 of working fluid in the main body of the evaporation chamber 2 by means of an additional pump (not shown) or other liquid transporting means.
(49) The tubing connections shown in
(50) In addition, it should be appreciated that the left and the right fluid collection chambers 16 can be maintained at different temperatures. This generates extra supersaturation of the vapours of the working fluid in the condenser and enables the rate of growth of the droplets and the droplet size to be increased or decreased as required. In this case each chamber has its own temperature controlling cycle. The temperatures of liquid in the containers can be found experimentally by means of trial and error or calculated according to nucleation theory.
(51) Keeping two fluid collection chambers 16 at different temperatures has another important advantage. When supersaturation in the condenser is sufficiently high, nano-particles of different sizes can form droplets in different locations along their travel through the condenser and, therefore, droplets formed onto nano-particles of different sizes will grow to various sizes. For instance, 50 nm particles will produce 0.5 M droplets but 100 nm particles will generate 1 m droplets. This enables the size of the nano-particles to be obtained from the size of the droplets, a facility which can form the basis for methods of characterising aerosol size distributions.
(52) It should be also appreciated that the temperature of the internal surface of the condenser can be non-uniform, for instance, it can linearly decrease with the length of the condenser. This gradually increases supersaturation of the working fluid vapour along the length of the condenser and, therefore, increases the ability of the apparatus to grow nano-particles of different sizes up to droplets of different sizes. Larger nano-particles tend to form droplets earlier (at the beginning of the condenser) whereas smaller particles that require greater supersaturation tend to form droplets only later at the end of the condenser and consequently the smaller particles have less time to grow and therefore grow to smaller droplet sizes in comparison with larger nano-particles. This makes it possible to establish a one-to-one relationship between the size of droplets formed in the condensation chamber and the size of nano-particles. This relationship can be utilised to evaluate the size of nano-particles by analysing the size of the droplets.
(53) Supersaturation in the apparatus of the invention is controlled by the temperature of the walls, the dimensions of the component parts of the apparatus and the flow rates of the carrier gas and sample gas streams through the apparatus. Variation of these parameters enables a skilled person to select the supersaturation conditions. There is a well-known link between the supersaturation and the minimal size of nano-particles that can form droplets. Therefore, it is possible to change the lower detection limit of a condensation apparatus by changing one or several of these parameters, e.g. the temperature of a heating element 3. This is a powerful tool iii determining size distributions of nano-particles and the proportion of nano-particles in various size ranges. It also enables the development of a condensation apparatus with a predetermined lower detection limit, e.g. 100 nm, 30 nm, 10 nm or 3 nm or with a variable lower detection limit. This provides a platform for an aerosol particle sizing in order to obtain nano-particle size distributions.
(54) It also should be appreciated that a plurality of condensation apparatuses of the invention set up to give different supersaturation conditions can be connected to each other sequentially or in parallel. The sequential arrangement enables nano-particles of different sizes to grow up to different size droplets. If the first condensation chamber is set at lower supersaturation than the second then larger particles form droplets in the first chamber but smaller particles form droplets only in the second chamber whereas previously formed droplets are grown further and become distinctly larger in size. The same is true for the second and the third chambers. Thus, a plurality of chambers enables a plurality of droplet sizes to be formed. This allows the size distribution of nano-particles to be retrieved by analysing the size distribution of droplets, e.g. by using an optical particle counter.
(55) In the case of a parallel arrangement of condensation chambers, the stream of nano-particles of interest is divided into several parallel flows and the said flows are directed to different chambers. The chambers should be set to different values of supersaturation so as to have different lower size detection limits. This makes it possible to retrieve nano-particle number size distributions by analysing the numbers of droplets grown in these chambers.
(56) It will also be appreciated that it is possible to vary temperatures and other parameters of the condensation apparatus and therefore vary the supersaturation as well as the lower detection limit during a given measuring cycle. This enables a cumulative particle size distribution to be obtained.
(57) An apparatus according to a further embodiment of the invention is illustrated schematically in
(58) The embodiment of
(59) In order to reduce particle losses, both the nozzle 22 and the condenser 7 have cylindrical symmetry and the nozzle 22 is positioned along the axis of the condenser 7 in such a way that the end of the nozzle extends downstream beyond the second inlet 8. This enables the cooler sample gas stream to be formed around the vapour-containing carrier gas stream.
(60) An advantage of the condensation apparatus of the invention is that it provides reliable data and can be miniaturised to dimensions much smaller than those of known condensation counters
(61) A preferred working fluid in each of the embodiments of the invention is the semi-volatile dimethyl phthalate. A major advantage of using a semi-volatile compound is that it leads to a much lower consumption of working fluid. An apparatus of the invention has been found to work without requiring refilling for more than 10 months.
(62) The choice of flow rates, the temperature of the saturating chamber and the manner in which airborne particles of interest are introduced into the chamber will usually be made according to the nature of the particles and their concentration. The total flow out of the condenser outlet 11 is often in the range from 0.1 to 4 l/min. The clean carrier gas flow accounts for 10 to 90% of the total flow. For dimethyl phthalate, the temperature of the saturating chamber usually is in the range from 80 to 150 C.
(63) In order to reduce the power consumption of the heating element, a thin film heater can be used which has attached to it a porous medium which is wettable by the working fluid. It is advantageous for a part of the porous medium to be long enough to be in contact with working fluid at the bottom of the chamber 2.
(64) The evaporation chamber 2 and condenser 7 may be manufactured from a variety of materials including any metal, glass or ceramic or (in the case of the evaporation chamber) plastics such as PTFE, but it is preferred to use materials or surface treatments that are inert or resistant to oxidation in air or other carrier gases and which do not react chemically with the working fluid. Pyrex glass, quartz, ceramic and stainless steel were used for various modifications of the chambers and their elements.
(65) It will also be appreciated that the sample gas stream containing particles of interest can be introduced through inlet 1 and the clean air via inlet 8. This is preferable for temperature stable particles such as metal particles. However, aerosol particles formed from organic compounds can be affected the high temperatures generated by the heating element and should therefore be introduced via inlet 8.
(66) An apparatus according to another embodiment of the invention is illustrated in
(67) In this embodiment, a sample of aerosol of interest is directed into inlet 8 and a stream of clean air is introduced through inlet 23. The mixing chamber enables the stream of the aerosol sample of interest to be sandwiched between a central core stream of carrier gas containing working fluid vapour and a outer layer formed by the clean air from inlet 23. Using an apparatus of this type, it is found that the best results are obtained when the gas layers in the sandwich are cylindrically symmetrical.
(68) It is advantageous to prolong the working life of the apparatus without the need for frequent refilling with working fluid. A significantly longer operating life between refills can be achieved by means of a combination of two condensation units with means for collecting and recycling working fluid from droplets that have passed though the particle detector and which contain airborne particles. Such an assembly can comprise two condensing units and a system of aerosol flow manipulation with three way valves to redirect the flows. The condensation apparatus used with such an assembly is slightly different from the other specific embodiments described above and an example of a suitable condensation apparatus is shown in
(69) It should be understood from the above that the porous medium 26 should be positioned in such a way to form an airtight seal with the walls of the evaporation chamber so that all of the gas received through inlet 1 is filtered and all of the airborne particles are trapped. Droplets of working fluid collected on the porous support can be re-evaporated and released as vapour into the evaporation chamber on the downstream side of the porous support
(70) An assembly comprising two condensation apparatuses of the aforementioned type consumes negligible or no working fluid and therefore does not need to be refilled. Such an assembly is illustrated in
(71) The assembly shown in
(72) The assembly shown in
(73) Airflow containing nano-particles of interest is drawn via common inlet 35 into one condensation apparatus (e.g. apparatus 28) by appropriate adjustment of the three-way valve 30. Micro-droplets formed on the nano-particles in the apparatus are directed towards optical particle counter 29 by means of three-way valve 31 while valve 34 is closed. After being counted, micro-droplets are directed to the other apparatus 27 by three-way valve 32. In apparatus 27, micro-droplets are collected onto the porous medium and filtered clean air is released into the atmosphere through outlet 35 by opening valve 33. The evaporation chamber in apparatus 27 remains cold because there no voltage is applied to the heating element, and therefore the working fluid collected on the porous medium is stored.
(74) After an appropriate period of time, the apparatus 27 is heated, the valve positions are adjusted and apparatus 28 is allowed to cool so that it is able to collect droplets of working fluid. The previously idle apparatus 27 is then in working mode and the working fluid previously captured by the porous medium is heated and evaporated to form a vapour which is then mixed with a gas sample stream as described above.
(75) After passing through the condenser and particle counter, the stream of particle- and vapour-laden air is directed to apparatus 28 where the air is filtered and the working fluid collected as described above for apparatus 27. The cycle is then repeated.
(76) The time necessary to switch between the chambers can be determined empirically through trial and error. Normally it is only necessary to switch the valves after hundreds of hours of operations. Therefore, the system requires relatively little energy to operate and energy and can be easily implemented.
(77) If necessary, additional specialised gas filters can be attached to outlets 35 and 36 to trap working fluid vapour remaining in the gas stream after filtration by the porous support. However, by using a semi-volatile working fluid such as dimethyl phthalate, for the majority of applications there is no need to use additional filters because the vapour pressure of the semi-volatile compound is very low.
(78) In each of the foregoing embodiments, the condensation chamber can be equipped with a working fluid sensor, e.g. filled glass capillary or dew point type sensors (not shown in the Figures). A sensor placed e.g. inside the chamber enables the depletion of the working fluid to be monitored.
(79)
(80) By using a condenser of rectangular cross-section, the size of the condensation chamber can be reduced considerably. However, a potential problem with some rectangular condenser layouts, particularly where the inlet and outlet of the condenser are tubes of circular cross section, is that there may be non-uniformity of the flow velocity in the condenser. This can lead to some particles spending more time in the condenser than others meaning that there is non-uniform growth of the particles in the condenser. This in turn can give rise to inaccuracies in measurement of the numbers and sizes of the particles.
(81) Thus, as shown in
(82)
(83)
(84) The uniformity of the residence time is achieved by designing the flow distributors such that the internal area of the cross-sections of the flow distributors are sufficiently greater than the internal area of the cross-section of the condenser. As an example, if the cross-section of the flow distributors is a circle of the internal diameter Dt and the condenser internal height is Hc and the internal width Wc then Dt.sup.2>Hc*Wc. The ratio of Dt.sup.2/(Hc*Wc) should be more than 1.1 or preferably more than 2 or even more preferably the ratio should be more than 3.
(85) Fluid communication between the interiors of the flow distributors 102 and 104 and the interior of the rectangular condenser can be achieved by providing the walls of the flow distributors with elongate narrow slots or a linear array of holes that open into the condenser. It is advantageous to provide a narrow slot between the flow distributors 102 and 104 and the condenser 103. In
(86) In another embodiment, the flow distributor contains holes evenly distributed along the inlet and outlet of the rectangular condenser 103 instead of two slots. The number of holes Nh should be more than 1 or preferably more than 4 or even more preferably more than 10. The diameter of the holes Dh should be sufficiently small and can be evaluated from the expression: Dt.sup.2>Nh*Dh.sup.2. The ratio of Dt.sup.2/(Nh*Dh.sup.2) should be more than 1.1 or preferably more than 2 or even more preferably the ratio should be more than 3.
(87) In one embodiment of the condenser arrangement shown in
(88) It will also be appreciated that the shape of the cross-section of the distributor may be rectangular, triangular, ellipsoidal, polygonal or any combination of simple geometric shapes.
(89)
(90) The evaporation chamber shown in
(91) A heating element is mounted in one side of the PTFE body 200. The heating element has a mounting portion 206 removably secured in the wall of the PTFE body, and a rod portion 210 which extends into the chamber interior 216. A holder 204 holds the mounting portion 206 in place and an O-ring provides a seal between the mounting portion 206 and the wall of the chamber body. Another O-ring provides a seal between the mounting portion 206 and the rod 210.
(92) The rod portion 212 has a hollow interior within which are disposed a metal heating wire 222 and a thermocouple 224 (see
(93) The heating wire and thermocouple are connected to a controller (not shown).
(94) Beneath the heating element, the body of the evaporation chamber has a well 214/218 for holding a working liquid such as dimethyl lphthalate. The well 214/218 is connected via tube 218 (see
(95) As shown in
(96) In this embodiment, the heating element is in direct contact with the porous support thereby reducing the heat input required and time taken to evaporate the working fluid to form a saturated vapour within the chamber.
EXAMPLES
(97) Several examples of apparatus according to this invention have been built and tested and these are described below.
Example 1
(98) In one example constructed as shown in
Example 2
(99) A comparison was made between aerosol particle number concentrations (N) measured using an apparatus as illustrated in
(100) The results are shown in
(101) It was found that the apparatus of the invention enables nano-particles to be enlarged up to 1.2 m in diameter. The lower detection limit for the apparatus of the invention was estimated to be 3 nm. It is clear from
EQUIVALENTS
(102) It will readily be apparent that numerous modifications and alterations may be made to the specific embodiments of the invention described above without departing from the principles underlying the invention. All such modifications and alterations are intended to be embraced by this application.