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* GB785408 (A) Description: GB785408 (A) ? 1957-10-30 Improvements in or relating to luminescent materials Description of GB785408 (A) Translate this text into Tooltip [75][(1)__Select language] Translate this text into The EPO does not accept any responsibility for the accuracy of data and information originating from other authorities than the EPO; in particular, the EPO does not guarantee that they are complete, up-to-date or fit for specific purposes. PATENT SPECIFICATION Date of Application and filing Complete Specification: Dec 21, 1955. 785,408 No 36631/55. Application made in United States of America on Dec 27, 1954. Complete Specification Published: Oct 30, 1957. Index at acceptance:-Class 39 ( 1), 54 (C:E:F:H:P:Q). International Classification -CD 9 k. COMPLETE SPECIFICATION Improvements in or relating to Luminescent Materials We, WESTINGHOUSE ELE Cr RIC INTERNATIONAL COMPANY, of 40 Wall Street, New York 5, State of New York, United States of America, a Corporation organized and

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* GB785408 (A)

Description: GB785408 (A) ? 1957-10-30

Improvements in or relating to luminescent materials

Description of GB785408 (A) Translate this text into Tooltip

[75][(1)__Select language] Translate this text into

The EPO does not accept any responsibility for the accuracy of data and information originating from other authorities than the EPO; in particular, the EPO does not guarantee that they are complete, up-to-date or fit for specific purposes.

PATENT SPECIFICATION Date of Application and filing Complete Specification: Dec 21, 1955. 785,408 No 36631/55. Application made in United States of America on Dec 27, 1954. Complete Specification Published: Oct 30, 1957. Index at acceptance:-Class 39 ( 1), 54 (C:E:F:H:P:Q). International Classification -CD 9 k. COMPLETE SPECIFICATION Improvements in or relating to Luminescent Materials We, WESTINGHOUSE ELE Cr RIC INTERNATIONAL COMPANY, of 40 Wall Street, New York 5, State of New York, United States of America, a Corporation organized and existing under the Laws of the State of Delaware, in said United States of America, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement: - This invention relates to luminescent materials and, more particularly, to a process for improving the luminescent output of halophosphate-type luminescent materials. U.S Patent Specification No 2,691,601 discloses a method for increasing the brightness of halophosphate type phosphors wherein the phosphor is washed with a non-oxidizing acid or a base It is theorized

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that this removes impurities from the surface of the phosphor and thus increases the luminescent output An oxidizing acid, such as nitric acid, is specifically excluded in the teachings of this patent, for apparently it is felt that the oxidizing acid will deleteriously affect the luminescent output through interaction with the manganese activator. It is the general object of this invention to provide a process for further improving the luminescent output of halophosphate type luminescent materials. It is another object to provide specific washes for improving the luminescent output of halophosphate type luminescent materials. According to the invention, the aforesaid objects are achieved by providing an oxidizing acid washing process for halophosphate type luminescent materials, whereby the luminescent output is improved over the best non-oxidizing acid washes of the prior art. The invention will become more readily apparent from the following description of several exemplary embodiments thereof. Halophosphate luminescent materials are, lPrice 3/6 l in general, compounds more or less analogous to the natural mineral apatite and are supposed to be represented by a formula such as 3 M 3 (P 04)2 1 M'L 2 where L represents a mixture of halogen and M and M' 50 represent either different or identical bivalent metals or mixtures of such metals Commercially competitive halophosphate luminescent materials are normally activated by both manganese and antimony or by anti 55 mony alone and an example of a halophosphate luminescent material which is activated by antimony alone has the general formulation 3 Ca J(PO 4)2 Ca F 2: Sb Since competitive halophosphate phosphors are 60 activated by either manganese and antimony or antimony alone, the teachings of this invention, are as a practical matter, limited to such phosphors, although the teachings of the invention are equally applicable to halo 65 phosphates having other activators than manganese and antimony together, or antimony alone. In preparing a halophosphate luminescent material, the following raw-mix com 70 ponents may be mixed in the following proportions: calcium acid phosphate, 1,860 grams; calcium carbonate, 558 grams, calcium fluoride, 140 grams; manganese carbonate, 67 grams; antimony trioxide, 150 grams; and 75 ammonium chloride, 168 grams The foregoing raw-mix components are ball-milled with flint pebbles, for example, for a period of about 5 hours, for example The ballmilled raw-mix components are then fired at 80 a temperature of about 10850 C in a covered crucible for about 3 hours The fired phosphor is then hammer-milled If desired, the ball-milling and firing may be repeated, as is customary The foregoing method of pre 85 paring a halophosphate luminescent material is well known It is obvious that other

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halo'phosphate luminescent materials may be substituted for the foregoing specific example, and in addition various well-known modi 90 785,408 fications and techniques of preparation may also be incorporated in preparing the halophosphate. The foregoing method of preparation will produce a partially-crystalline, finelydivided, halophosphate luminescent material. In the practices of the prior art, this luminescent material would then be incorporated into a fluorescent lamp It has been found however, that an additional oxidizing-acid wash for the processed luminescent material will appreciably increase its output over the untreated luminescent materials of the prior art In addition, the oxidizing-acid wash of the processed luminescent material will improve the luminescent material lumen maintenance over the lumen maintenance of a luminescent material treated with a hydrochloric-acid wash, as described in the heretofore mentioned U S Patent Specification 2,691,601. In washing the processed luminescent material of this invention, the partiallycrystalline, finely-divided halophosphate luminescent material is placed in an aqueous solution of either of the well-known oxidizing acids, namely nitric or sulphuric As an example, 300 grams of the luminescent material may be placed in 1 liter of 0 05 N nitric or sulphuric acid and the solution mechanically agitated There is nothing particularly critical in the washing or agitation time as long as the finely-divided luminescent material is substantially completely wetted by the aqueous solution of the oxidizing-acid wash As an example, the luminescent material and aqueous solution of oxidizing acid may be mechanically agitated for two hours, but this washing period may be varied considerably without appreciably effecting the luminescent output of the luminescent material, provided the luminescent material is substantially completely wetted by the wash. After washing, the luminescent material may be separated from the aqueous solution of oxidizing acid by either straining or decanting In a decanting process, the luminescent material may be allowed to settle in the wash for one-half hour, for example, at which time the supernatant liquid will be crystal clear The supernatant liquid is then decanted and distilled water may be added to the original volume of the wash This is stirred for one-half hour, for example, and the luminescent material again allowed to settle, after which the supernatant liquid is again decanted The distilled water rinses may be repeated to a total of 3 or more times, if desired. Alternatively, it has been found that a mere filtering of the luminescent material from the aqueous solution of oxidizing acid will substantially separate the acid from the luminescent materials, so

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that the luminescent output of the washed luminescent material is substantially the same whether a filtering or a more elaborate decanting process is used In the filter procedure, the oxidizing-acid solution and luminescent 70 material may be separated by use of a filter type which will retain the finest precipitate, such as a number 5 "Whatman" filter, or equivalent It should be understood that coarser or finer filter paper may be used, if 75 desired, necessitating either repeated filterings or a longer filter period, and in addition any type of separating mechanism which will effectively separate the washed luminescent material from the washing solution may be 80 used. After separation from the washing solution, the washed luminescent material may be dried by any conventional drying means, for example, by drying in an oven at a tem 85 perature of J 11 OC for a period of 24 hours. In the foregoing example, the normality of the aqueous solution of oxidizing acid may vary between wide limits, for example between 0 01 N to 0 15 N and even these 90 limits are not particularly critical. In the foregoing specific example of the washing treatment of this invention, the relative amounts of washing solution and grams of luminescent material are not particularly 95 critical For example, 400 grams of luminescent material in 300 cubic centimeter of washing solution is suitable, although at this point the luminescent material, when evenly distributed throughout the washing mixture, 100 produces a relatively viscous mixture which is hard to handle Of course as much washing solution, with respect to the amount of luminescent material, may be used as desired, within the limits of economical 105 operation. The dried, acid-washed luminescent material is then suspended in solvent and a binder, for example, butyl acetate and nitrocellulose, to form a paint, as is well-known 110 in the fluorescent lamp art This paint is then applied to the inner surfaces of a fluorescent lamp envelope, the solvent volatilized and the lamp lehred (heated) to drive off the binder, as is standard practice in the 115 fluorescent lamp art. The fabrication of the final fluorescent lamp incorporating the treated luminescent material may then be completed, by techniques which are well-known in the art Such 120 lamps normally have alkaline-earth, oxidecoated, tungsten coiled-coil wire electrodes hermetically sealed into both tubular envelope ends, an envelope filling of argon gas at a pressure of 4 mm of mercury, for example, 125 and some mercury contained within the envelope. In testing the oxidizing-acid washing treatment of this invention, four groups of lamps were prepared using the same luminescent 130 785,408 material, but varying the treatment Group 1 consisted of unwashed ' luminescent material incorporated into 40 W T 12

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fluorescent lamps in accordance with the teachings of the prior art Group 2 consisted of 40 W T 12 lamps incorporating hydrochloric-acid washed luminescent material treated as disclosed in U S Patent 2,691,601 Group 3 consisted of 4 OW T 12 lamps incorporating nitric-acid washed luminescent material. Group 4 consisted of 40 W T 12 lamps incorporating sulphuric-acid washed luminescent material In the case of the oxidizing-acid washed luminescent material, a O 1 N acid solution was utilized In the case of hydro 15 chloric acid washed luminescent material, the teachings of the aforementioned patent were followed The test results are summarized in the following table. TABLE I Luminescent Material Treatment Lumens per watt at indicated life (Hours) 0 100 600 1000 2000 Group 1-control lamp 67 4 64 0 61 0 58 2 55 6 Group 2-HC 1 wash 68 4 65 9 63 1 60 8 57 4 Group 3-HNO 3 wash 68 5 66 0 63 4 61 1 58 6 Group 4-H 2 SO 4 wash 68 5 66 0 63 5 61 2 59 3 It can thus be seen that the initial himens per watt for all of the "acid-washed luminescent material lamps" were approximately 1 lumen per watt higher than the control lamps At 2000 hours life, however, the "hydrochloric-acid washed lamps" were 1 8 lumens per watt better than the control lamps, the "nitric-acid washed lamps" were 3 lumens per watt better than the control lamps, and the "sulphuric acid washed lamps" were 3 7 lumens per watt better than the control lamps. The explanation for the improvement of an acid-washed luminescent material over an unwashed material probably lies in the fact that milling or otherwise reducing a luminescent material to a finely-divided state converts some of the crystalline luminescent material to an amorphous state This has been verified by X-ray diffraction tests, in which tests the acid-washed luminescent material has been shown to be more crystalline than the unwashed luminescent material It also appears that the amorphous materials is much more soluble in the acid wash than the crystalline luminescent material so that the amorphous material is dissolved Why the oxidizing acids are more effective than the non-oxidizing acid is not clear, but it can be assumed that the oxidizing acids more effectively remove the amorphous material from the crystalline luminescent material It may thus be stated that halophosphate type luminescent materials which have been treated with an oxidizingacid wash are substantially crystalline having had substantially all amorphous material removed therefrom. The process of removing the amorphous material from the partially-crystalline luminescent material may be aptly described as an elutriation process In powder-metallurgy practices, elutriation is often used to describe separation of a coarse from a finer powder by washing and filtering or decanting In the broader sense, however,

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elutriation may be defined as purifying a powder by washing and then filtering or decanting, which is exactly the process as practiced in this in 75 vention, and is the sense in which the term is used in the claims. It will be recognised that the objects of the invention have been achieved by providing a process for improving the luminescent 80 output and lumen maintenance of halophosphate luminescent materials and in addition there have been provided specific oxidizing-acid washes for use in this process.

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* GB785409 (A)

Description: GB785409 (A) ? 1957-10-30

Improvements in sealing arrangements in vacuum apparatus

Description of GB785409 (A)

COMPLETE SPECIFICATION Improvements in Sealing Arrangements in Vacuum Apparatus We, GENERAL ELECTRIC COMPANY, a Corporation of the State of New York, United States of America, having its office at Schenectady 5, State of New York. United States of America, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement: This invention relates to vacuum apparatus comprising an enclosure evacuated or adapted to be evacuated and having a sealing arrangement for preventing appreciable leakage around a movable rod-like element extending through a wall of the enclosure of the vacuum apparatus.

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In the chemical, metallurgical and related arts an increasing use is being made of reaction and treatment apparatus involving vacuum or very low pressure chambers. One of the difficulties encountered with such apparatus is the provision of adequate seals about movable elements which extend through the vacuum chamber walls. These elements may have a variety of functions, but usually they must move freely with respect to the opening in the chamber wall. For example. such an element may have a rodlike configuration and may be used to manipulate apparatus or material within the chamber, may function as a drive shaft for mechanism within the chamber, may serve to conduct material to or from the chamber, or perform any other function which may require relative motion between the element and the container wall structure. Many of the previous seals for articulated or movable rod-like elements extending through a diaphragm or wall across which a pressure differential exists have depended upon either a deformable sealing element analogous to a gland and stuffing box or upon very closely machined surfaces, generally of a spherical or semi-spherical configuration. The firstmentioned means may be undesirable in any e I f l ~ particular environment for many reasons, one of which is that the sealing action obtained by deformation of a plastic material about the rod-like element nearly always results in an increase in friction and an attendant loss in the mobility of the element. Similarly, the second-mentioned means may be undesirable in any particular environment for a variety of reasons, but usually because of the difficulty in manufacturing and maintaining the high degree of accuracy necessary in the mating machined surfaces. In this respect this type of seal is particularly sensitive to mechanical attrition and temperature changes or differentials. A difficult problem has arisen in the continuous extraction of a continuously cast ingot or bar from a vacuum chamber containing a conventional continuous casting apparatus. Such a continuous casting apparatus usually consists of a conventional melting furnace to which material to be melted is charged by any suitable means. The molten material is continuously tapped from the crucible of the furnace into a tubular mould, the molten material solidifying in the upper portion of the mould and the solid bar thus formed being continuously extracted through the open bottom of the mould. The specific details of such continuous casting apparatus are well known and form no part of the present invention. This extracted bar or ingot is usually hot and frequently does not have a smooth surface. Where the material being continuously cast in this manner does not require melting in a vacuum such as, for example, brass or other similar alloys, the various operations may be carried out in the atmosphere without difficulty. However, certain molten metals and alloys react quite

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readily with gases of the atmosphere and are 'usually commercially produced in vacuum furnaces of the batch type in which it is sometimes necessary to maintain pressures of the order of 10-2 to 10or' mm. of mercury. One of the difficulties which has previously prevented the adaption of continuous casting apparatus to the vacuum furnace technique has been the difficulty of continuously extracting the hot cast bar or ingot from the vacuum chamber without contaminating the interior of the chamber with at- mospheric gases. Because the temperature of newly cast ingots of metals such as titanium, for example, may be of the order of 1000 C. or higher, a deformable seal of the gland and stuffing box type is unsuitable due to rapid destruction of the packing material. Further surface imperfections of such a bar prevents an efficient metal-to-metal contact between the bar and the wall structure. According to the present invention a vacuum apparatus comprises an enclosure evacuated or adapted to be evacuated having a sealing arrangement for the purpose set forth, namely, for reducing flow of gas into the enclosure by means of an aperture in the wall of the enclosure through which a rodlike element movable with respect to the apparatus extends, said sealing arrangement consisting of a tubular structure the internal surface of which closely surrounds the rodlike element for two or more successive lengths of said tubular structure so as to appreciably impede flow of gas between the rod-like element and said structure, but with a small clearance allowing the rod to be freely moved within the tubular structure, m combination with evacuating means connected with said tubular structure between adjacent ends of said lengths so as to extract a substantial portion of any gas flow- ing through said small clearance. Preferably the tubular structure includes one or more chambers situate between the adjacent ends of the closely surrounding lengths of said structure and in communication with said lengths, the evacuating means being connected to said chamber(s). By this means no physical contact exists between the rod-liLe element and the seal. While the seal of the invention is particularly suited for overcoming the problems involved in extracting a hot bar from a vacuum chamber, it is equally suitable for other and specifically different uses. For example, the seal of the invention is equally adaptable for inserting a rod-lilie element into a vacuum chamber. In this manner, material to be melted in a vacuum enclosed continuous casting apparatus may be continuously charged into the furnace crucible without loss of the vacuum by passing a rod-like element of the material through an appropriately located seal in a small of the vacuum chamber. Additionally in the event that a consumable electrode

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arc furnace is employed in such an apparatus. the rod-like element may constitute the consumable electrode. One embodiment of the invention will now be described by way of example with reference to the accompanying drawing, in which Fig. 1 is a fragmentary sectional view of a schematically represented vacuum chamber, rod-like element, and sealing means; and Fig. 2 is a section taken on line 2-2 of Fig. 1. With particular reference to Fig. 1, a portion of the wall structure of a vacuum container 1 is provided with an aperture '. Vacuum container 1 is provided with a vacuum source or pumping means of any suitable construction which has not been shown. A rod-like element 3 extends through aperture 2 into the vacuum chamber and is dimensioned so that it is slightly smaller than aperture 2. A tubular seal structure generally indicated by reference numeral 4 comprises a tubular member 5 comprising an impedance element concentrically arranged about element 3 and has an internal dimension with respect to element 3 approximately the same as aperture 2 i.e., there is formed between the element 3 and impedance element 5 an annular conduit or passage 6 through which a small volume of gas may flow. The impedance element 5 is secured to side wall 1 at the peripherv of aperture 2. As indicated in the figure; an annular bustle or pumping chamber 7 is secured to the lower end of impedance element 5. Extending beyond bustle 7 and connected thereto is another impedance element 8 which is similar in size and shape to impedance element 5 and co-operates with element 3 to provide a conduit 9 similar to conduit 6. Communicating with the interior of the pumping chamber or bustle 7 is a conduit 10 to a vacuum pump of any conventional design which is not shown. Attached to the outer end of impedance element 8 may be another bustle or pumping chamber ll, similar in all respects to pumping chamber 7, and provided with a conduit 12 to a vacuum source. Extending beyond and interconnected with bustle or chamber 11 is an impedance element 13 which is similar to impedance elements 5 and 8 and which provides a conduit 14 about the periphery of element 3 similar to conduits 6 and 9. Addi- tional bustles or pumping chambers similar to chambers 7 and 11 interconnected by itil- pedance elements similar to elements 5, 8 and 13 may be additionally provided if desired in the manner shown and discussed. The final or terminal pumping chamber or bustle its is provided with a vacuum pumping line or conduit x and has extending outwardly therefrom a terminal impedance element y which co-operates with the outer surface of rod element 3 to provide an annular conduit which is in communication through its outer end with the atmosphere. In practice, of course, the number of serially arranged bustles or pumping chambers and impedance elements to be used in a particular

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installation will depend upon several factors, namely, the pressure desired to be maintained within the vacuum container, the pumping capacity of the vacuum source of the container, the size of the annular conduit passages determined by the size of the rodlike element and the internal diameter of the impedance elements, the length of the conduits between the bustles and the chamber and the pumping capacities of the vacuum sources attached to the hustles. For purposes of this disclosure it will be assumed that the external pressure of the system is atmospheric, although it is to be noted that the invention is not necessarily limited to use in that pressure range. A sectional view of the relationship between rod 3 and a typical bustle chamber and impedance element is shown in Fig. 2. For purposes of illustration, element 3 has been shown as a right circular cylinder and the impedance elements 5, 8, 13 and y which, with bustle chamber 7, 11, and w, define the tubular seal structure the internal passage of which has a circular cross-section. It will be appreciated, however, that other lateral configurations of element 3 may be employed, such as, for example, a rectangular cross-section, provided, of course, that the shape of the tubular structure is altered to closely conform to the peripheral shape and dimension of the rod-like element. It is to be noted, with particular reference to Figs. 1 and 2, that while the minimum internal lateral dimensions of the various elements comprising the tubular seal structure closely approach the corresponding lateral dimension of the rod-like element 3, in every case they are a small but discrete amount greater. This has been illustrated in both figures as a series of annular conduits or passages identified by reference characters 6, 9, 14 and z. As indicated in Fig. 2, the outer periphery of rod-like element 3 closely approaches the inner surfaces of tubular elements 5, 8 13 and y but in each case is spaced a small but finite distance therefrom. The annular passages or conduits thus defined have a relatively small cross-sectional area compared to the cross-sectional area of element 3, and, consequently, gas passing through these conduits is in contact with a very large surface per unit volume of gas flow. Therefore, the frictional forces induced by the walls of the annular conduits and the surface of the rod is quite high in relation to the amount of gas flowing which serves to impede gas flow therethrough. From a theoretical standpoint, assume that a chamber is provided with a vacuum pump. Assume an aperture in a wall of the chamber is provided with an outwardly extending tubular element which contains a rod-like element of at least equal length, there being formed between the tubular element and the rod-like element an annular conduit which extends from

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the aperture throughout the length of the tubular element and provides a passageway between the interior of the chamber and the outside atmosphere. For a given cross-sectional area of the annular passageway or conduit there will be a finite length of passageway which will impose such a large frictional force upon gases flowing in the conduit that the vacuum pump serving the chamber can maintain the interior of the chamber at some pressure lower than atmospheric pressure. If a greater pressure differential between pressures outside and inside the chamber is desired, either the capacity of the pump must be increased, the cross-sectional area of the annular conduit must be decreased, the length of the conduit must be increased, or all of these changes may be made. In such an organization of elements, assume that the external pressure is atmospheric and the internal pressure within the chamber is maintained at a small fraction of an atmosphere. A quantity of gas at atmospheric pressure enters the outer end of the annular conduit and flows toward the evacuated chamber. As the gas progresses along the conduit, its free flow is impeded by frictional contact with the walls of the conduit. The ultimate result is that the number of gas molecules which pass a given point in the conduit in a given time becomes smaller as the distance the gas has travelled from the conduit entrance increases. This, of course, is manifested by a decrease in pressure. Unfortunately, for most industrial applications contemplated, it is not practical to utilize a vacuum seal which depends solely upon this flow impedance principal for sealing because the length of annular conduit is very large. In the present invention, each of the bustle chambers spaced along the annular conduit functions to replace long sections of conduit in that portions of the gas are abstracted from the flow path, giving the same net effect at subsequent points along the flow path as though the gas had passed through a long length of conduit. Otherwise stated, each bustle chamber reduces the number of gas molecules which may pass it along the annular conduit. In operation, assume a vacuum in chamber 1 is maintained by any suitable pumping means. Air at atmospheric pressure enters the annular conduit z at the outer end of the tubular passage and flows along the annular conduit z until it reaches bustle chamber w. The pressure of the air continuously decreases as it progresses along conduit z. When the air reaches the bustle chamber w. the pressure drops an additional amount as a portion of it is abstracted by the vacuum source operating through conduit x. The remaining air at reduced pressure then passes through succeeding annular conduits and intervening bustle chambers, the pressure and consequently the amount of air being correspondingly lowered at each

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bustle chamber. When the air has been reduced to a predetermined residual amount within the pumping capacity of the vacuum chamber, no further reduction in amount is needed and it may be permitted to enter the vacuum chamber to be subsequently removed during the normal pumping activity which maintains the pressure in that chamber. In certain installations it may be undesirable to permit any gas to flow into the vacuum chamber from the annular conduit. In this event, the number of bustle chambers, conduit cross-sectional area and bustle chamber pumping capacities may be selected so that the bustle chamber adjacent the vacuum chamber has a capacity that in normal operation supplements the main chamber's vacuum source and assists it in maintaining the pressure in the chamber. With reference to Fig. 1, in this embodiment, any gas in conduit 6 would flow from chamber 1 toward bustle chamber 7. The flow characteristics for any dimension of rod-like element and corresponding area of annular flow conduit may be determined for any given temperature, pressure range and bustle chamber pumping capacity by the application of well-known gas law equations and collision theory relationships. In the discussion above, it has been assumed that vacuum pumps of identical capacities are used for all the bustle chambers. However, higher efficiency and a corresponding fewer number of stages may be realized by increasing the pumping capacity of the higher pressure bustle chambers. From the foregoing, it may be seen that there is provided an efficient vacuum sealing apparatus whereby a movable rod-like element may be extended through a wall of a vacuum container and which co-operates with the container and the rod-like element to substantially prevent leakage of atmospheric gases around the movable rod-like element into the vacuum container. What we claim is : - 1. A vacuum apparatus comprising an enclosure evacuated or adapted to be evacuated and having a sealing arrangement for the purpose set forth consisting of a tubular structure the internal surface of which closely surrounds the rod-like element for two or more successive lengths of said tubular structure so as to appreciably impede flow of gas between the rod-like element and said structure, but with a small clearance allowing the rod to be freely moved within the tubular structure, in combination with evacuating means connected with said tubular structure between adjacent ends of said lengths so as to extract a substantial portion of any gas flowing through said small clearance. 2. A vacuum apparatus as claimed in Claim 1, in which the tubular structure includes one or more chambers situate between the adjacent ends of the closely surrounding lengths of said structure and in communication with said lengths, the

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evacuating means being connected to said chamber(s). 3. A vacuum apparatus having a sealing arrangement substantially as described with reference to the accompanying drawing.

* GB785410 (A)

Description: GB785410 (A) ? 1957-10-30

Improvements in and relating to substituted tetrahydronaphthalenes

Description of GB785410 (A) Translate this text into Tooltip

[75][(1)__Select language] Translate this text into

The EPO does not accept any responsibility for the accuracy of data and information originating from other authorities than the EPO; in particular, the EPO does not guarantee that they are complete, up-to-date or fit for specific purposes.

PATENT SPECIFICATION 785,410 Dote of Application and filing Complete Specification: Jan 3, 1956. No 168/56. I<Zgg// Application made in United States of America on Jan28, 1955. Complete Specification Published: Oct 30, 1957. Index at acceptance:-Class 2 ( 3), B 2, C 3 A 13 A 3 (A 2: B 3: F 3), C 3 A 14 A( 2 D: 8 A). International Classification:-CO 7 c. COMPLETE SPECIFICATION Improvements in and relating to Substituted Tetrahydronaphthalenes We, L GIV Au DAN & CIE S A, a Company organised under the laws of Switzerland, of Vernier, Geneva, Switzerland, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statementThis invention relates to novel chemical compounds, and more especially to acetyltetrahydronaphthalenes having musk like odours.

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Most of the known synthetic musk-like compounds fall into two classes: ( 1) nitrated aromatic hydrocarbons, such as musk xylene, and ( 2) macrocyclic ketones, lactones or esters, such as cyclopentadecanone, cyclopentadecanolide, and ethylene brassylate. While members in the first group are inexpensive to manufacture, they suffer from the disadvantage that they are not light-stable or alkali-stable, frequently causing discolouration in products such as soap Members of the second group, while reasonably stable to light and alkalies, are difficult to manufacture and are relatively costly. We have found that certain novel chemical compounds which we have synthesized have the desirable property of being musk-like in olfactory character and yet are extremely stable to light and alkalies, and, at the same time, are inexpensive to manufacture and hence not relatively costly. Our novel chemical compounds are 6acetyl-1,4,7-trimethyl-1-lower alkyl 1,2,3,4tetrahydronaphthalenes The term " lower alkyl" herein is intended to mean methyl and ethyl These substances are viscous, colourless oils, soluble in benzene, ethyl alcohol, ethylene dichloride, and similar solvents They possess musk-like odours per se or in solution and are light-stable and alkalistable. In general, our novel compounds are prepared by the sequence of reactions set forth below: lPrice 3 sl A&dj 3 Zl i' CH CHCH 2 CH 2 C CH 3 CHS Ofi 3-CH-CH 2 CH 2-Cs I{ Mg 3 OH ICH 3 H CH 3 CH, H 2504,J CH 3 1,4,7-trimethyl-1-R-1,2,3,4tetrahydronaphthalene CH 'H CH 3 C ( CH 2 Ai C 3 CH 3 e A CH 2 CH 3 R 6-acetyl-1,4,7-trimethyl-1-R1,2,3,4-tetrahydronaphthalene wherein R=CH, and C,2 H,. It will be readily apparent that our novel musk-like compounds can be employed in widely-varying formulations, depending upon the type of formulation, the odour effect desired, and the desires of the compounder of the formulation Consequently, we do not wish to confine ourselves to any particular formulation, but wish it to be understood that our products can be employed as musks in perfume containing formulations in general By the term "perfume-containing" we include, inter, alia, perfumes, cosmetics, soaps. The following examples are given to illustrate the invention. EXAMPLE 1. Preparation of 6-acetyl-1,1,4,7-tetramethyl1,Z,3,4-tetrahydronaphthalene. To a Grignard solution prepared from 20 g of magnesium, 116 g of methyl iodide and 300 ml of ether was added at reflux over 1 hour in a solution of 142 g of 5-p-tolylhexan-2-one in 200 ml of ether After refluxing 1 hour, the mixture was quenched with iced dilute

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hydrochloric acid The ether solution was washed neutral The ether was distilled off and the oil distilled over 2 g of soda ash There was obtained 141 g of 2-methyl-5-p-tolyl hexan-2-ol as a colourless oil of weak odour, B P 102 C ( 1 mm), d,,25 0.9466, n D 2 '1 5155. Sulphuric acid ( 93 %) ( 140 ml) was cooled to O C and 140 g of 2-methyl-5-p-tolyl2-hexanol, described above, was added with agitation over a period of 40 minutes, keeping the temperature at 00 C Stirring was continued 1 hour longer The solution was quenched on ice; the oil was taken up in benzene, washed with water, 5 % sodium hydroxide solution and water again until neutral The benzene was distilled off and the oil was vacuum-distilled over 2 g of soda ash There was obtained 113 g of 1,1,4,7-tetramethyl 1,2,3,4 tetrahydronaphthalene as a colourless oil, B P 86 ( 2 mm), d,525 0 9410, nj 20 1 5300. A mixture of 22 g of acetyl chloride and 47 g of 1,1,4,7-tetramethyl-1,2,3,4-tetrahydlronaphthalefne, described above, was added during 1 hour to a suspension of 38 g of aluminium chloride in 94 g of ethylene dichloride, stirring the mixture throughout the reaction period and cooling to maintain a temperature of 20-25 C. After the addition, stirring was continued for 1 hour The solution was quenched on ice The ethylene dichloride layer was separated and washed neutral The solvent was distilled off and the remaining oil distilled over 2 g of soda ash There was obtained a colourless oil ( 47 g) with strong musk odour, B P 1220 C ( 1 mm), d-,25 1.0060, n D'0 1 5452 The product is 6-acetyl1,1,4,7 tetramethyl 1,2,3,4 tetrahydronaphthalene. EXAMPLE 2. Preparation of 6-acetyl-1,4,7-trimethyl-1ethyl-1,2,3,4-tetrahydronaphthalene. In a similar manner to that described in Example 1 and using the Grignard reagent prepared from ethyl bromide, there was prepared -3 methyl 6 p tolyl heptan-3-ol, a colourless viscous liquid of mild odour, B P. 1060 C ( 1 mm), d&J 25 0 9472, n D 20 1 5151. The 3-methyl-6-p-tolyl heptan-3-ol, 139 g, was reacted with 139 ml of sulphuric acid ( 93 %) at O C with good agitation The reaction mixture was worked up as in Example 1 and there was obtained 113 g of 1,4,7trimethyl-l-ethyl-1,2,3,4 tetrahydronaphthalene as a colourless oil, B P 840 C ( 0 5 mm.), d,25, 0 9446, n D 20 1 5337. A mixture of 22 0 g of acetyl chloride and g of 1,4,7-trimethyl-1-ethyl-1,2,3,4-tetra 65 hydronaphthalene, as described above, was added during 1 hour to a suspension of 38 g. of aluminium chloride in 100 g of ethylene dichloride with agitation and cooling to maintain a temperature of 20-25 C After the 70 addition, agitation was continued for 1 hour. The solution was quenched on ice The oil layer was washed neutral and

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the solvent distilled from it The remaining oil was vacuumdistilled over 2 g of soda ash There was 75 obtained 47 g of 6-acetyl-1,4,7-trimethyl-1ethyl-1,2,3,4-tetrahydronaphthalene, a colourless oil, B P 125 " C ( 1 mm), d 252 '1 0066, n,,20 1 5468, having a musk-like odour. Anal Calc'd for C 17 H 04 O: C 83 54; H 990 80 Found: 83 53; 9 54

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* GB785411 (A)

Description: GB785411 (A) ? 1957-10-30

Improvements in and relating to injection nozzles for internal combustionengines

Description of GB785411 (A)

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PATENT SPECIFICATION

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Date of Application and filing Complete Specification: Jan 10, 1956. Application made in Switzerland on Feb 23, 1955. Complete Specification Published: Oct 30, 1957. 785,411 No 796156. Index at acceptance:-Class 7 ( 3), B 2 J( 1 B 6:15 19 A). International Classification:-FO 2 f. COMPLETE SPECIFICATION Improvements in and relating to Injection Nozzles for Internal Combustion Engines We, ADOLPH S AU Rm R LTD, of Arbon, Switzerland, a Swiss Company, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement:- This invention relates to injection nozzles of internal combustion engines. The present invention consists in an injection nozzle for internal combustion engines, with a valve member which under the action of the fuel pressure is displaced against the forces of two springs and at the same time releases in two stages the cross-sectional area of flow for the fuel to be injected in such a manner that the valve does not close between the two stages, characterised by the feature that the valve member in its closed position and during a first part of the stroke is influenced by a minor spring, the force of which amounts to 30 % to 70 % of a main spring which acts on it during a second part of the stroke, and that the minor spring is located between two movable abutments, one of the abutments being connected with the valve member and the other serving as an abutment for the main spring, so 30that at the start of the injection, during the first part of the stroke of valve member, at first only a small quantity of fuel leaves the nozzle at low pressure and, onlv after a considerable increase of the filel pressure, the valve member is further displaced to provide the increased crosssectional area of flow for the main injeetion. In the following description and with reference to the accompanying drawings the constructional forms of injection nozzles are described by way of example. Fig 1 is a diagram, in which the quantity injected related to unit time is shown; Fig 2 shows a diagram, in which the relation between fuel pressure and crosssectional area of flow is illustrated; Figs 3 to 5 show different constructional examples of injection nozzles 50 In Fig 1 the course of the quantity injected (M) related to the crank angle degrees (W) is shown in the case of a control method of a known kind and in the case of the invention by the two curves 40 55 and 41, the curve 40 showing the conditions in the known method and the curve 41 the conditions according to the invention As will be seen from the

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diagram, the invention operates with an actual pre-60 injection which is represented by the distance a-d-e and extends over the crank angle a-i The pre-injection starts at a. At d the cross-section required for the pre-injection is fuilly open It cannot be 65 exceeded before the point e The main injection starts at the point e, f corresponding to the point of the complete opening of the cross-section required for the main injection At g the closing by 70 the control member starts and at h the whole of the injection is ended. Fig 2 shows the relation between the fuel pressure (P) required for the opening process and the cross-sectional area of flow 75 (Q), the distance k to 1 corresponding to the cross-sectional area of flow required for the optimum smooth running of the engine, whilst the distance kc to m corresponds to the total cross-sectional area of 80 flow Point N corresponds to the squirting pressure (first opening pressure) of an ordinary nozzle BY the line 44 is represented the pressure difference (p minus n) required for opening an injection nozzle 85 of the hitherto usual type The curve 45 illustrates the pressure course according to the invention, required for causing the nozzle to open As will be seen from the diagram, the pressure difference (o minus 90 785,411 j is required for eausing the opening o P the cross-seetion necessary for the preinjection During this first pressure range the cross-sectional area of flow thus becomes larger Before the opening up of the main cross-sectional area of flow is initiated, the pressure must rise from o to q, the cross-sectional area of flow remaining constant during this second pressure range The very small pressure difference (r minus q) suffices for opening uip the main cross-sectional area of flow, during the third pressure range, during which the cross-sectional area of flow again becomes greater and during which the main portion of the fuel is injected under high pressure. In the example of the injection nozzle according to Fig 3 the nozzle body 1 has the bore 2 constructed as the spring space and the bore 4 which acts as a guide for the needle 3 In the bore 2 are housed the heavily pre-stressed main spring 5 and the additional spring 6 which is considerably weaker by comparison, the spring 5 seeking to force the plate 8 provided with the shank 7 against the upper end surface of the bush 9 The bush 9 encloses the spring 6 The latter bears at, one end against the plate 8 and at the other end presses by means of the ring 11 the needle o against its seating 13 The fuel is conveyed to the cavity 15 through the bore 16 and emerges through the injection holes 14 Between the needle 3 and the plate 8 and between the shank 7 and the upper end wall of the bore 2 are the distances of lift Xi and X 2 The bore 50 is the duct for leaking oil.

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The arrangement according to Fig:3 operates as follows: In the drawing the nozzle is shown in the closed position On fuel flowing through the duet 16 into the space 15, the needle 3 is lifted in opposition to the pressure of the spring 6, the spring force of which is 30 % to 70 % of the spring force of the spring 5, from its seating 13 and forced slightly upwards, until the needle 3, after travelling through the distance X 1, bears against the under side of the plate 8. During this first part of the injection and with a short distance of lift of the control member 3 only a small quantity of fuel flows at low pressure out of the injection holes 14 For overcoming the greater initial stressing force of the strong spring the fuel pressure in the space 15 must rise to such an extent that there will be a period of time, such as is required for obtaining a sufficiently long period of preinjection After this high fuel pressure has been exceeded, the nozzle needle 3 is displaced rapidly upwards Owing to the flat characteristic of the spring 5 a slight increase in pressure will suffice, until the shank 7 of the plate 8 after travellikji o through the distance -2, bears against tile upper end wall of the bore 2 Tliroghli this greater lift of the needle: the cross 70 sectional area of flow for the main injection is liberated, this taking-u place rapidly in consequence of the great pressure fall. Fig 4 shows a pilot pin nozzle, in which the needle 3 has the pin 17 lying ou Tside 75 the seating 13 and the fuel flows ou. through the injection holes 14 In the closed position shown the spring 6 presses the valve member 3 against its seating 1:, and there are the distances l X and X: 80 between the nozzle needle 3 and the plate 8 on the one hand and between the shankly 7 and the upper end wall of the bore 2 o i the other hand The plate 8 is pressed)v the spring 5 against the bush 9, whereby 85 the force of the spring 6 amounts to % e-70 % of the spring 3 The first lif t N 1 of the needle is made somewhlat snialler than the length / of the pin 17; it is also in a quite definite relation to the diameter go of the needle shank 3. The mode of operation is as follows on fuel flowing to the space 13, the needle 3 is raised until it has travelled through the distance X, Owing to the predetermined 95 relation between the diameter of the needle shank the cross-sectional area and therefore the amount of fuel flowing out will remain the same during the travel of the pin 17 through the distance X, The 100 increase in pressure in the space 15 and the opening of the main cross-seetional area of flow are correspondingly retarded. Ais, however, the distance of lift X, is somewhat smaller than the length 1 of the 105 pilot 17, the throttling required for the rise in pressure is obtained After the force of the strongly pre-stressed

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spring has been overcome, the needle 3 is pushed rapidly upwards, until the shank 7 after 1 lo passing through the distance X 2, comes to bear, wherebvy through the increased lift of the needle 3 the main portion of the fuel emerges under high pressure out of the injection holes 14 115 With the nozzle according to Fig there are provided in the bore 2 of the nozzle body 1 the bushes 24 and 25, between which the plate 26 is disposed. In the closed position of the nozzle this 120 plate is held by the strongly pre-stressed spring 27 against the lower end surface of the bush 24 The spring 28 bears against the upper side of the plate 26 The force of the spring 28 amounts to 30 cc G-70 %c or 125 the spring 27 It seeks by means of the bush 29 to hold the conical lower part 2 t 1 of the needle 30 against the seat 32 Tile needle 30 has in its downwardly directed part the grooves 33 When the nozzle is 130 785,411 in its closed position, there will be between the supporting plate 26 and the bush 29 on the one hand and between the plate 26 and the bush 25 on the other hand the distances of lift XI and X 2 The fuel is conveyed to the bore 2 through the duct 34. The nozzle shown in the closed position in Fig 5 operates as follows On fuel flowing through the duct 34 into the space 102, the needle 30 is displaced downwards after the small force of the spring 28 has been overcome, until the bush 29, after travelling through the stroke X 1, bears against the plate 26 In this part of the injection only a small quantity of fuel, corresponding to the small cross-section of the aperture, flows along the grooves 33 at low pressure out of the nozzle Through the following, considerable increase of the fuel pressure in the space 2 and in the grooves 33 the needle 30 will, after overcoming the force of the strongly prestressed spring 27 be rapidly displaced downwards, until the plate 26, after travelling through the distance X 2, bears against the bush 25 Through this enlargement of the cross-sectional area of the outlet the main portion of the fuel is ejected under high pressure.

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* GB785412 (A)

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Description: GB785412 (A) ? 1957-10-30

Improvements in or relating to vehicle seats

Description of GB785412 (A)

PATENT SPECIFICATION Date of Application and filing Complete Specification: Jan 12, 1956. 785,412 No 1061156. k Application made in United States of America on Jan18, 1955. Complete Specification Published: Oct 30, 1957. Index at acceptance:-Class 52 ( 2), Jl(AX:I). International Classification:-A 47,c. COMPLETE SPECIFICATION Improvements in or relating to Vehicle Seats We, GENERAL MOTORS CORPORATION, a Company Incorporated under the Laws of the State of Delaware in the United States of America, of Grand Boulevard in the City of Detroit, State of Michigan, in the United States of America (Assignees of JOHN HIMKA) do hereby declare the invention for which we pray that a patent may be granted to us and the method by which it is to be performed, to be particularly described in and by the following statement:- This invention relates to vehicle seats, and more particularly to vehicle front seats. The scope of the monopoly is defined by the appended claims; and how the invention can be carried into effect is hereinafter particularly described with reference to the accompanying drawings, in which:Fig 1 is a side elevational view, partly in section, of a vehicle seat embodying the invention, illustrating the form and arrangement of the parts when the seat is in the normal occupied position, certain parts being broken away to illustrate more clearly the details of construction; Fig 2 is a side elevational view, partly in section, similar to Fig 1, illustrating the, relationship of the parts when the seat is in a forwardly displaced position; Fig 3 is a skeleton plan view, with parts broken away, of the vehicle seat illustrated in Figs 1 and 2, showing the relationship of the parts when one of the seat backs is forwardly displaced; Fig 4 is an enlarged fragmentary plan view of the left side of the seat looking in the direction of arms 4-4 of Fig 2; Fig 5 is a fragmentary enlarged sectional front elevational view, partly in section, looking in the direction of arrows 5-5 of Fig

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1; and Fig 6 is an enlarged fragmentary sectional front elevational view looking in the direction of arrows 6-6 of Fig 1. Referring now to the drawings and partiI:cularly Figs 1 and 3, there is illustrated a vehicle front seat having a full width, normally transversely-extending seat bottom cushion 2 and a pair of tiltable seat backs 4 pivotally supported in side by side relation 50 at the rear edge of the cushion 2 Cushion 2 is mounted in a bottom frame 8 which extends thereunder and is provided with upturned side edges 10 Frame 8 is reinforced by means of a tubular skeleton 12 which forms 55 an integral part thereof At their lateral edges, seat backs 4 are provided with spaced, downwardly and forwardly extending arm portions 14 and 16 which are pivotally connected respectively, to spaced bracket mem 60 bers 18 and 20 Bracket members 18 and 20 are, in turn, rigidly secured in laterally spaced relation on tubular frame 12 and provide transversely aligned pivot axes for seat backs 4 ' 65 In order to support the seat bottom in the vehicle body and provide forward displacement thereof responsive to tilting of either seat back, a pair of longitudinally spaced parallel links 22 and 24 are interposed be 70 tween each end of seat bottom frame 8 and the vehicle floor As seen best in Fig 1, the rear legs 24 of each pair of links constitute integral continuations of outer seat back arms 14, while the forward links 22 are pivotally 75 connected to seat bottom frame 8 at 26. The lower ends 28 and 30 of forward and rearward links 22 and 24, respectively, are formed with modified socket portions 32 and 34 which are adapted for connection with 80 ball portions 36 and 38 (Fig 5) Ball portions 36, in turn, are rigidly connected respectively at the forward inner edges 40 of base members 42 while ball portions 38 are rigidly secured to depending portions 44 85 formed integrally at the outer rearward edges of members 42. As seen best in Figs 4 and 5, each base member 42 is connected by bolts 46 and 48 to one of two slidable, laterally spaced, ad 90 785,412 juster rails 50 Adjuster rails 50 are slidable on fixed rails 52 to permit fore and aft adjustment of the seat As seen in Figs 3 and 4, base members 42 are secured to upper ad6 juster rails 50 in a manner permitting horizontal angular movement of the members 42 about the axis of bolt connections 46 Thus, the forward ends 54 of slide members 42 may swing arcuately within the limits provided by transverse slots 56, the purpose of which will shortly become apparent. A description of the mode of operation will now be given As seen in Figs I and 5, when both seat backs 4 are in the normal, substantially vertically extending position, the downwardly extending arms 14 and legs 24, which form continuations thereof, are swingable arcuately about the fixed axis defined by ball member 38 Forward links 22, in

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turn, are swingable arcuately about the fixed axis defined by ball member 32 Since the intermediate portion of arm 14 is also pivotally connected to the seat frame at 18, it will be seen that forward tilting movement of either seat back 4 will cause forward swinging movement of leg 24 about the axis of ball portion 38 which, in turn, will cause the pivotal connection 18 to move forwardly in an arc described from the axis of ball portion 38 Since pivotal connection 18 is on the seat bottom frame 8, the rear part of the adjacent end of the seat frame and cushion will rise and move forwardly in a corresponding arc Simultaneously, the forward part of the same end of seat frame 8 and cushion 2 will rise and move forwardly in an arc defined by the link 22 about the axis of ball assembly 32. Since each seat back 4 may be tilted forvardly independently of the other, it will be apparent that forward movement of the cushion 2 and frame 8 will be imparted at one end only, since the opposite seat back will remain vertical and thereby retain the corresponding end of seat cushion 2 and frame 8 in the rearwardly disposed position Consequently, upon tilting of either seat back 4, the entire seat cushion 2 and frame 8 is displaced forwardly at the corresponding end so about an axis adjacent the rear pivotal connection 46 between base member 42 and adjuster rail 50 on the opposite side Since fore and aft adjuster rails 50 and 52 retain their fixed parallel relation, forward ends 54 of base members 42 must be capable of horizontal swinging movement to accommodate the displacement For that purpose transversely elongated slots 56 are provided at the forward ends 54 of each base member, so that when either side of the seat bottom is displaced forwardly the base members 42 can swing about their pivots 46 without imparting lateral stresses on fore and aft adjuster rails 50 and 52 It will also be seen that the planes of links 22 and 24 progressively change from an initial parallel relation with a line joining pivotal connections 36 and 38. However, because of the provision of limited universal action between ball members 36 and 38 and socket portions 32 and 34, no inter 70 ference is occasioned as a result of this change in parallelism when the seat backs 4 are tilted from the full rearward to the full forward position. It should also be noted that when the seat 75 structure is in the normal occupied position, links 22 and 24 are directed in a rearwardly and upwardly inclined path relative to the vehicle body floor 58 By virtue of this arrangement, the total weight of the seat and 8) the off-centre rearwardly displaced relation of the seat backs combine to produce a constant positive force maintaining the entire seat structure in the normal position shown in Fig 1 Hence considerable inertia must be 85 overcome to displace the seat forwardly, thus

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preventing inadvertent actuation, as from rapid deceleration of the vehicle To provide positive rearward limits for the normal occupied position of the seat bottom, links 22 are 9 i) formed with stops 62 which engage the upper surface 60 of slide rails 42 when the seat and seat backs have been actuated to the desired rearward position It will of course, be evident that stop 62 may be ad 95 justable to permit limited variation in the full rearward position of the seat assembly to accommodate individual preference in seat back inclination.

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