AU628199B2 - Furnace for the electro-thermal atomization of samples for spectroscopical purposes - Google Patents

Description

WATERMARK PATENT TRADEMARK ATTORNEYS id1 0,q'_21 Renistered Patent Attornev i j coM~~w~~i~anus~n~:'~ 219~Form PATENTS ACT 19CZ-69 COMPLETE SPEC IFICATION

(ORIGINAL)

Class Int. Class Application Number: 59794/90 Lodged: 24th July 1990 Complete Specification Lodged: Accepted: R~ns Published: Priority ReltedAr Npme of Applicant t 4' Address of Applicant SActual lnventor: Address for Service BODENSEEWERK PERKIN-ELMER, GIIBH Postfach 1120, 7770 Uberlingen, Federal Republic of Germany ROLF TAMM and GUMMHER RODEL WATERMARK PATENT TRADEMARK TTORNEYS.

LOCKED BAG NO. 5, HAWTHORN, VICTORIA 3122, AUST RALIA Complete Specification for the invention entitled: FURNACE FOR THE ELECTRO-THERMAL ATOTMIZATION OF SAMPLES FORR SPECTROSCOPICAL PURPOSES The following statement is a full description of this invention, including the best method of performing it known to BS-3998 -1- FURNACE FOR THE ELECTRO-THERMAL ATOMIZATION OF SAMPLES FOR SPECTROSCOPICAL PURPOSES TECHNICAL FIELD The invention relates to a furnace for the electro-thermal atomization of samples for spectroscopical purposes which has a cavity for the accommodation of the sample.

A very sensitive, quantitative analyzing method for determining the amount of a certain looked for element in a sample is atomic absorption spectroscopy. In atomic absorption spectroscopy, a o.0 sample is atomized so that the individual components of the 0. sample are present in their atomic state and form an "atomic vapor". A measuring light beam is passed throughout this atomic Q0 0 vapor. This measuring light beam originates from line-emitting o o light source which emits the characteristic resonant lines of SOP the looked for element. Such a measuring light beam is only absorbed by the atoms of the looked for element. Therefore, the absorption of the measuring light beam in the atomic vapor provides a measure of the number of atoms of the looked for element in the path of rays of the measuring light beam, and 0 thus, after suitable calibration, a measure of the concentration of the looked for element in the sample.

For the atomization of the samples, furnaces usually made of graphite are used into which the sample solution is introduced 0e.: and which are heated by a strong electric current to a high temperature. Thereby, in the interior of the furnace, a "cloud of atoms" is generated throughout which the measuring light beam is passed through aligned openings of the furnace. This is designated as the "electro-thermal atomization'.

However, methods are also known wherein in such furnaces, where the sample is electro-thermally heated, a gas discharge is generated whereby the sample atoms are excited to emit characteristic line spectra.

The invention related to a furnace for such spectroscopical purposes and similar spectroscopical purposes.

B- 998 -2- The invention further relates to a method for producing such a furnace.

BACKGROUND ART From German patent application 24 20 546, it is known to coat furnaces which are made of a graphite tube with a layer of pyrocarbon in carrying out electro-thermal decomposition of samples. Thereby, in contrast to pure graphite, a non-porous surface is provided by such coating and the sample liquid is prevented from infiltrating the graphite. If such infiltration of sample liquid into the graphite tube were permitted, the atomization of elements of the sample is delayed. Thereby, the sensitivity and the accuracy of the measurement suffer.

Pyrocarbon is a carbon which is generated by thermal decomposition of carburent on the surface of a graphite element, a here a graphite tube. Different methods of supplying a 0 layer of pyrocarbon onto the surface of a graphite tube are known. Such a method is described in German patent application 24 20 546. Other methods work with gaseous carburents such as methane. In vacuo, where the elements which are to be coated are arranged, argon as a carrier gas carries methane over the surfaces which are to be coated, the methane being decomposed there generates the pyrocarbon coating.

oo In practice, it is often difficult to achieve uniform coating o° f graphite furnaces with pyrocarbon. This is particularly true for the interior of the cavity into which the sample for the atomization is introduced, the bore of a graphite tube. The thickness of the layer is difficult to determine.

Usually, the thickness of the layer being too small becomes obvious only in practical operation, namely by the early deterioration of the analytical results. The pyrocarbon layer wears out by use, so that, if a layer of pyrocarbon is too small, after relatively few analyses, the sample liquid, as described, will seep away in the material of the furnace which is no longer sufficiently coated.

The "graphite tube atomizer" in which the graphite furnace is formed by a graphite tube through which current flows in its longitudinal direction is described in German patent application 27 18 416.

BS-3998 -3- 311 761 shows a furnace for the electro-thermal atomization of samples with a tubular furnace body which is provided on opposite sides with longitudinal contact ribs which are, in turn, integral with cylindrical contact pieces. In the bore of the furnace body hollow, generally semi-cylindrical platforms extending through approximately 1800 are provided.

This platform is integral with the furnace body, it forms with the furnace body, with the contact ribs, and the contact pieces an integral element made of graphite. Opposite the platform, the furnace body has a sample inlet opening.

It is the purpose of the platform to delay the heating of the sample supplied to the platform to atomization temperature as compared to the heating of the wall of the f urnace so that there 0 is already a thermal equilibrium when the sample is f inally 0 atornized. This is achieved in that the sample on the platform is heated substantially indirectly by heat radiation from the 00 wall of the furnace.

From German utility model 89 01 529.0, a furnace similar to that described above is known in which the hollow, generally semi-cylindrical platform being integral with the furnace is 0 connected to the furnace body through a narrow web which is 0 arranged on the one side of the platform and only on one side of the longitudinal center plane of the platform.

When the furnaces are produced according to EP-A-0 311 761 or according to German utility model 89 01 529.0,, there is relatively much refuse when the integral platform is machined. In addition, very particular problems occur with the coating with, pyrocarbon.

of such furnaces having a complex structure.

DISCLOSURE OF THE INVENTION It is the object of the invention to design a furnace of the type mentioned above so that it is easy to manufacture.

i- 4 In particular, the refuse of furnace having an integral platform shall be reduced and the coating with pyrocarbon shall be facilitated.

According to the invention, this object is achieved in that the furnace comprises two halves forming a cavity which are joined along a separating plane intersecting the cavity.

The furnace can be made of graphite and can be provided with a coating, particularly a coating of pyrolytic graphite.

Conveniently, a platform for the accommodation of the sample can be integral with one of the two halves. The furnace can have a tubular furnace portion which on opposite sides is provided with contact pieces extending perpendicular to the axes of the furnace portion and through which an electric current can be circumferentially passed through the furnace portion being in one plane. Then the furnace is separated along this plane comprising the axes. The two halves of the furnace are preferably held together by rings which are slipped onto the contact pieces.

Trapezoidal contact ribs are preferably integrally provided between the substantially cylindrical contact pieces and the furnace portion. Conveniently, in the contact ribs around the contact pieces, grooves are provided, into which the cylindrical rings project.

A method for manufacturing a furnace of the type described above comprises the method steps: producing two blank parts which engage each other with planar surfaces, and o 00o machining the two blank parts in common so that a cavity o° intersected by ttie plane of the planar surfaces is generated and each of the blank parts forms one half of the furnace, and may conveniently include the steps: S 25 separating the two halves of the furnace which were produced in this way, o 0 0 00 o 0 00.

0 -L -r i -I ;il coating the halves of the furnace separately, the inner surfaces of the cavity forming outer surfaces of each of the two halves of the furnace, and assembling the halves thus coated in order to form the complete furnace.

In this way, the coating of the inner surfaces of the furnace is made while they are freely accessible, while they form outer surfaces. Thereby, a better and more uniform coating can be achieved.

Conveniently, in order to reduce the refuse of furnaces with an integrated platform, manufacturing can be made in the way that first joined pairs of blank parts are 1 0 machined such that, in the cavity of the each pair, two hollow, generally cylindrical platforms are formed, one of which is integral with the one half of the furnace, and the other one of which is integral with the other half of the furnace, second joined pairs of blank parts for forming halves of a furnace are machined so that the cavity of each pair forms a continuous bore without any platform being integral therewith. Conveniently, in 1 5 forming the furnace, each of the halves of a furnace produced from a blank part of the first pairs of blank parts and a half of the furnace produced from a blank part of a second pair of blank parts are joined.

The manufacturing of two halves of a furnace with an integral platform requires the same working steps as the manufacturing of a complete furnace with an o. 20 integral platform.

~When, with the machining of the platform, there is refuse in the blank parts, from which halves of a furnace having an integral platform shall be produced, this refuse normally results only one half of the furnace. The other half of the furnace can be 0 Qa used and can be combined with an other half of the furnace having no platform. Refuse elements having an integral platform can be reworked to haives of a furnace having no integral platform. Refuse elements having an integral platform can be reworked to halves of a furnace having no integral platform, V 0 0,0

C,

9 BS-3998 -6if required. According to the statistic refuse rate of the halves of a furnace having an integral platform, the halves of a furnace having no integral platform can be produced in a reduced number.

An embodiment of the invention will now be described in greater detail with reference to the accompanying drawings.

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 shows a plan view of a half of a transversely heated furnace having an integral platform.

o Fig. 2 shows a section taken along the line A-B of Fig. 1.

0 Fig. 3 shows a section taken along the line C-D of Fig. 1, S^ the upper half of the furnace having no integral 44: o0 platform being illustrated together with a ring for the connection of the halves of the furnace.

Fig. 4 is a view of the lower half of the furnace in the 'direction of the arrow of Fig. 2.

460 Fig. 5 shows in a section similar to Fig. 3 a furnace having no integral platform.

0 PREFERRED EMBODIMENT OF THE INVENTION In Figs. 1-4, a lower half of a furnace 10 is made of a graphite plate which has an upper planar surface 12 and a lower planar surface 14. On the lower side of the graphite plate, recesses 18 and 20 (Fig. 2) are provided symmetrically to a center plane 16, each of which is limited by a surface 22 and 24, respectively, extending parallel to the planar surface 14 and a convexcylindrical surface 30 and 32, respectively. The two convexcylindrical surfaces are matched to form a semi-cylindrical outer surface 36, the axis 34 of which is formed by the intersection of the planar surface 12 and the center plane 16.

BS-3998 -7- On the upper side of the plate, a cylindrical recess 38 is provided coaxially to the outer surface 36. In this way, a half tube 40 is formed which represents half of a tubular furnace body.

A hollow, generally cylindrical platform 42 is concentrically arranged within this half tube 40. The platform 42 is integral with the half tube 40. As can be seen from Figs. 1 and 3, the platform 42 is only connected to the half tube through a web 44. This web 44 is located on an axial projection 46 at one end of the platform 42 and is connected to the half tube 40 only on one side of the longitudinal center plane 16.

o Contact ribs 48 and 50 are provided on both sides adjacent to the half tube 40. In plan view, the contact ribs 48 and 50 are trapezoidal. Contact pieces 52 and 54, respectively, are integral with the contact ribs. The contact pieces are semi- Poo.

cylindrical. The aligned axes of the cylindrical outer surfaces j of the contact pieces are arranged in the planar surface 12 and extend perpendicular to the axis 34 of the half tube 40. Semicylindrical, axial grooves 56 and 58, respectively, are also provided in the planar surfaces of the semi-cylindrical contact pieces 52 and 54. The grooves 56 and 58 end in front of the "o outer surface 36 of the half tube 40 and intersect the recesses 18 and 20, respectively, in passage openings 60 and 62, respectively.

o Due to the recesses 18 and 20, the half tube 40 is connected along its edges by relatively thin bridges 64 and 66 to the thicker portions 68 and 70, respectively, of the contact ribs 48 and 50, respectively. The contact pieces 52 and 54 are provided on these thicker portions 68 and 70, the thickness of which corresponds to that of the plate from which the half of the furnace is made. Annular grooves 72 and 74, respectively, are provided in the thicker portions 68 and 70 of the contact ribs 48 and 50 around the contact piece 52.

An "upper" half 76 of the furnace is substantially identical with the described lower half of the furnace 10. However, the i BS-3998 -8upper half 76 has no integral platform 42. The half tube 78 (Fig. 3) has a continuously smooth cylindrical inner surface.

The upper half of the furnace 76 has a planar surface corresponding to the planar surface 12.

In order to form a furnace, a lower half of the furnace 10 and an upper half of the furnace 76 are joined with their planar surfaces 12 and 80. Cylindrical rings 82 and 84, respectively, are slipped onto the contact pieces 52 and 54. The cylindrical rings 82 and 84 project into the annular grooves 72 and 74.

Thereby, the two halves of the furnace are held in close contact i throughout a large portion of their lengths.

Fig. 5 shows, in an illustration similar to Fig. 3, a furnace which consists of two identical halves of the furnace 86 and 88 having no platform.

;The halves of the furnace are coated with pyrocarbon.

0 9 The production of the furnaces is achieved as follows: Two blank parts having the shape of the mentioned plates with the planar surfaces 12 and 80 are joined and are clamped to each other. Then the plates are machined together. However, in these pairs of plates, either both halves of the furnace or none of the halves of the furnace are provided with integral platforms 40. In practice, the manufacturing of one platform or of two platforms requires the same expenditure.

The halves of the furnaces obtained in this way are separated and coated with pyrocarbon according to a well-known method.

The coating of the halves of the furnaces, particularly in the critical areas of the platforms and the inner walls of the bores can, thanks to the separation, be achieved more easily than in the prior art furnaces, since the platforms and the inner walls in the halves of the furnaces represent outer surfaces which are easily accessible and the coating of which presents no difficulties. Each of the "lower" halves of the furnaces I BS-3998 -9having an integral platform 40 and an 'upper" half of the furnaces 76 are subsequently joined and are connected to each other by slipping on the rings 82 and 84.

Instead of a connection by the rings 82,84 also a connection by bonding can be provided. It is also possible that the halves of the furnaces remain separated and in operation are compressed by the contacts having the conical contact surfaces between which the furnace is held in the apparatus. This method can be used particularly in graphite tubes of the prior art type which are held with their end faces between annular contacts and through which current flows longitudinally. Also, such furnaces can advantageously be composed of two halves of a I furnace.

Soo oa I 0 4 1 t1 t( I

Claims (9)

1. A furnace for the electro-thermal atomization of samples for spectroscopical purposes comprising two halves forming a cavity which are joined along a separating plane intersecting the cavity.

2. A furnace, as set forth in claim 1, wherein the furnace is made of graphite and is provided with a coating.

3. A furnace, as set forth in claim 2, wherein each of the two halves of the furnace is provided with a coating of pyrolytic graphite.

4. A furnace, as set forth in claim 3, wherein a platform for the accommodation of the sample is an integral part of one of the two halves. A furnace, as set forth in claim 4, wherein the furnace iurther comprises a tubular furnace portion having contact pieces on opposite sides which extend perpendicular to an axis of the tubular furnace portion with the axes of the contact pieces and the furnace portion lying in one plane along which the two halves of the furnace are joined.

6. A furnace, as set forth in claim 5, wherein two halves of the furnace are held together by cylindrical rings which are slipped onto the contact pieces. I, S I C C S c CI L SS t T1" i _;1 11

7. A furnace, as set forth in claim 5 comprising, trapezoidal contact ribs integrally disposed between the cylindrical contact pieces and the furnace body, grooves formed within the contact ribs around the contact pieces into which grooves the cylindrical rings project.

8. A method for manufacturing the furnace of claim 1 comprising the steps of producing two blank parts which engage each other with planar surfaces, and machining the two blank parts in common, so that a cavity intersected by the plane of the planar surfaces is formed and each of the blank parts forms one half of the furnace.

9. A method, as set forth in claim 8, further comprising the steps of: 06., separating the two halves of the furnace so produced, 0 coating the halves of the furnace separately, the inner surfaces of the cavity forming outer surfaces of each of the two halves of the furnace, and assembling the thus coated two furnace halves in order to form the complete furnace. 0a *C arr e 00 c I i I Iir I~ a 4.O a a O La a a a a 'a0 7 1 A method, as set forth in claim 8, wherein said machining includes forming in the cavity of each pair of blank parts two hollow, generally cylindrical platforms, one of which is integral with one half of the furnace and one of which is integral with the other half of the furnace, and joining each of the blank parts to form the furnace.

11. A method, as set forth in claim 8, wherein said machining includes in the cavity of each pair of blank parts a continuous bore joining each of the blank parts to form the furnaces. DATED this 18th day of June 1992. BODENSEEWERK PERKIN-ELMER. GMBH WATERMARK PATENT TRADEMARK ATTORNEYS THE ATRIUM 290 BURWOOD ROAD HAWTHORN VICTORIA 3122 AUSTRALIA