The present invention relates to a colour ink jet printing method, to a set of inks, to ink jet printer cartridges, to substrates printed using the method and to an ink jet printer.
Ink jet printing is a non-impact printing technique which involves ejecting, thermally or by action of an oscillating piezo crystal, droplets of ink from one or more fine nozzles directly onto a substrate. The ink may be aqueous, solvent or hot melt based.
The printing of textiles is conventionally carried out by screen or roller printing using gravure engraved cylinders. The design to be printed has to be engraved on to a cylinder and each individual colour in a design requires the application of a separate screen with a colour premixed to the required shade. This is a long and slow process and it can take many months for a textile design to appear as a printed textile. Consequently, there is a demand for a printing process which enables new designs to be printed onto a textile quickly for proofing purposes and for small production runs.
Ink jet printing of textiles offers the potential to transfer a design to a textile much faster than traditional textile printing methods. However, conventional colour ink jet printers operate with a colouring system which uses three subtractive primary colours (Cyan, Magenta and Yellow) together with black, hereinafter referred to as CMYK. This colouring system only provides a limited range of colours compared with conventional textile printing methods.
The limited colour range provided by conventional colour ink jet printers also limits their applicability in other imaging technologies, particularly where high resolution images are required from digital cameras or when printing images from the Internet. These xe2x80x9cphotorealisticxe2x80x9d applications require a wide range of colours to produce images of the same photographic quality as those prepared by conventional screen printing methods.
We have surprisingly found that the colour gamut of an ink jet printer is extended close to that obtained using conventional printing methods when a combination of inks containing dyes with specific calorimetric positions in colour space are used together with a CMYK colouring system in an ink jet printer.
According to a first aspect of the present invention there is provided a method for the coloration of a substrate comprising ink jet printing a first and second set of inks onto the substrate wherein:
(a) the first set of inks consists of one or more inks each of which independently contains a colorant selected from yellow, magenta, cyan and optionally black; and
(b) the second set of inks comprises one or more inks each of which independently contains a dye selected from:
a yellow dye of Formula (1) or salt thereof:
wherein:
X is a labile group or atom;
R1 is alkyl or xe2x80x94NH2;
A is xe2x80x94NR2R3, xe2x80x94OR2 or halogen;
R2 is H or optionally substituted alkyl; and
R3 is optionally substituted phenyl;
an orange dye of Formula (2) or salt thereof:
wherein:
R4 is H or optionally substituted alkyl;
X is as hereinbefore defined;
B is xe2x80x94NR5R6, xe2x80x94OR5 or halogen; and
R5 and R6 independently are H or optionally substituted alkyl;
a red dye of Formula (3) or salt thereof:
wherein:
X is as hereinbefore defined;
E is xe2x80x94NR7R8, xe2x80x94OR7 or halogen;
each R7 is independently H or alkyl; and
R8 is optionally substituted aryl;
and a blue dye of Formula (4) or salt thereof:
wherein:
each X independently is as hereinbefore defined;
each L independently is an optionally substituted alkylene group;
each W independently is halogen or a group of the formula xe2x80x94OR9 or xe2x80x94NR10R11;
R9 is H or alkyl, R10 is H or optionally substituted alkyl; and
R11 is an optionally substituted aryl group.
FIG. 1 compares the colour gamut obtained using a first set of inks alone (i.e. cyan, magenta and yellow) with that obtained using a first and second set of inks according to the present invention. In FIG. 1 the dots indicate the colour gamut from the first and second sets of inks. The crosses show the colour gamut from the first set of inks alone.
The coloration method of the present invention achieves a wide colour gamut by applying, in any combination, the inks from the hereinbefore defined first and second sets of inks to a substrate using an ink jet printer.
Preferably, the first set of inks consists of yellow, magenta and cyan inks and preferably also a black ink. Accordingly, in a preferred embodiment, the first set of inks consists of an ink containing a yellow colorant, an ink containing a magenta colorant, an ink containing a cyan colorant and an ink containing a black colorant.
The second set of inks comprises from one to four, preferably two to four and especially four inks each of which independently contains a dye selected from the hereinbefore defined dyes of the Formulae (1) to (4).
In a preferred embodiment, the second set of inks comprises an ink containing a dye of Formula (1), an ink containing a dye of Formula (2) an ink containing a dye of Formula (3) and an ink containing a dye of Formula (4).
In view of the above preferences, in an especially preferred embodiment of the present invention the first set of inks consists of an ink containing a yellow colorant, an ink containing a magenta colorant, an ink containing a cyan colorant and an ink containing a black colorant; and the second set of inks comprises an ink containing a dye of Formula (1), an ink containing a dye of Formula (2) an ink containing a dye of Formula (3) and an ink containing a dye of Formula (4).
As will be understood, the ink of the first set of inks which contains the yellow colorant is a different shade of yellow to that of the ink of the second set of inks which contains the yellow dye of Formula (1) so as to maximise the colour gamut available to the ink jet printer.
It is preferred that each of the inks in the first and second set of inks are a different colour.
The inks may be applied to the substrate in any combination, provided that at least one ink from each of the two sets is applied. The particular combination of inks selected from the first and second sets of inks will be chosen to achieve a desired colour at a specific position on the substrate. Therefore, a single ink from the first or second set of inks or any combination of inks from the first and second sets may be applied to a particular point on a substrate to achieve a specific colour at that point. By way of illustration, if a red corresponding to the colour of the red ink of the second set of inks was required at a particular point on the substrate, then that ink alone would be applied to that part of the substrate by the ink jet printer.
In the dyes of Formula (1), it is preferred that:
R1 is C1-4-alkyl or xe2x80x94NH2, more preferably methyl, ethyl or xe2x80x94NH2 and especially xe2x80x94NH2;
R2 is H or optionally substituted C1-6-alkyl, more preferably H or C1-4-alkyl and especially H, methyl and ethyl;
R3 is phenyl substituted by xe2x80x94COOH ,xe2x80x94SO3H or xe2x80x94OH, more preferably phenyl substituted by xe2x80x94SO3H; and
the group A is a group of the formula xe2x80x94NR2R3, xe2x80x94OR2 or Cl, more preferably xe2x80x94NR2R3.
The dyes of Formula (1) may be prepared by methods analogous to those described in the art for other similar azo dyes, for example as described in EP 559 331A1, page 5, wherein the compound of formula (4) has the formula H-A.
In the dyes of Formula (2), it is preferred that:
R4 is H or optionally substituted C1-4-alkyl, more preferably H, methyl or ethyl and especially methyl;
R5 and R6 are preferably each independently H or C1-4-alkyl, more preferably H; and
B is preferably xe2x80x94NR5R6, xe2x80x94OR6 or Cl, more preferably xe2x80x94NR5R6 and especially xe2x80x94NHR6.
The dyes of Formula (2) may be prepared by methods analogous to those described in the art for similar azo dyes, for example as described in GB 859,990, Example 1.
Preferred dyes of Formula (3) are those in which:
R7 is H or C1-4-alkyl, more preferably H, methyl or ethyl and especially H;
R8 is optionally substituted phenyl or naphthyl and especially phenyl optionally substituted by C1-4-alkyl; and
E is xe2x80x94NR7R8, xe2x80x94OR7 or Cl, more preferably xe2x80x94NR7R8 and especially xe2x80x94NHR8.
The dyes of Formula (3) may be prepared by methods analogous to those described in the art for other similar azo dyes, for example as described in GB 834,304, Example 3.
Preferred dyes of the Formula (4) are those in which:
R9 is H or C1-4-alkyl, especially H;
R10 is H or optionally substituted C1-6-alkyl, more preferably H or C1-4-alkyl and especially H or methyl;
R11 is an optionally substituted phenyl, more preferably phenyl substituted with carboxy, hydroxy or sulpho and especially phenyl substituted with one or preferably two sulpho groups;
each L independently is an optionally substituted C1-6-alkylene group, more preferably a C1-6-alkylene group and especially an alkylene group of the formula xe2x80x94CmH2mxe2x80x94,
wherein m is an integer from 1 to 6, preferably 2 or 3; and each W independently is xe2x80x94OR9, xe2x80x94NR10R11 or Cl, more preferably xe2x80x94NR10OR11 and especially xe2x80x94NHR11.
The dyes of Formula (4) may be prepared by methods analogous to those described in the prior art for similar triphenodioxazine dyes, for example as described in EP 576 123 Al on pages 6 to 8 and Example 1.
The cyan, yellow, magenta and black colorants present in the inks of the first set of inks may be selected from any of the colorants suitable for use in ink jet printers utilising the conventional CMYK colouring system for example, cyan, yellow, magenta and black pigments and dyes. Preferably the colorants present in the first set of inks are dyes, more preferably dyes which contain fibre reactive groups.
When any of the first set of inks contain a fibre reactive dye, any of the cyan, magenta, yellow and black reactive dyes listed in the Colour Index are suitable. Preferred reactive dyes comprise of one or more chromophores and one or more fibre reactive groups. Preferred fibre reactive groups are cellulose reactive groups, more preferably, vinylsulphone, sulphatoethylsulphone, halopyrimidine and holotriazine groups. Preferred halotriazine groups are fluoro and chlorotriazine groups, more preferably mono-chlorotriazine groups. Examples of suitable chromophores include azo, phthalocyanine, triphenodioxazine, anthraquinone and formazan chromophores. Especially preferred reactive dyes suitable for use in the first set of inks comprise one or more azo, phthalocyanine, triphenodioxazine, anthraquinone and formazan chromophore and one or more mono-chlorotriazine group. It is preferred that the reactive dye is water soluble.
Specific examples of reactive dyes suitable for use as colorants in the first set of inks include for example. Colour Index (C.I.) Reactive Red 31, C.I. Reactive Blue 71 and C.I. Reactive Black 8. These dyes are available from Zeneca Ltd.
In a preferred embodiment, the cyan colorant in the first set of inks is a dye of the Formula (5), or salt thereof
wherein:
Pc is a phthalocyanine nucleus;
Z is xe2x80x94NR12R13, xe2x80x94OR13 or halogen; wherein
R12 is H or optionally substituted alkyl;
R13 is H, optionally substituted alkyl or optionally substituted aryl;
X is as hereinbefore defined;
a is 1 to 3;
b is 1 to 3; and
(a+b)=4.
It is preferred that R12 is H or optionally substituted C1-4-alkyl, more preferably H or C1-4-alkyl and especially H.
Preferably R13 is H, optionally substituted C1-6-alkyl or optionally substituted phenyl, more preferably H or optionally substituted C1-4-alkyl and especially methyl or ethyl.
When Z is halogen it is preferably chloro.
Preferably Z is a group of the formula xe2x80x94NR12R13 or xe2x80x94OR13, more preferably xe2x80x94NHR13 or xe2x80x94OR13 and especially methoxy and ethoxy.
The dyes of Formula (5) may be prepared by methods analogous to those described in the art for similar phthalocyanine compounds. For example a suitable method is described in GB 805,562, Example 12.
In a preferred embodiment the yellow colorant present in the first set of inks is a dye of Formula (6) or salt thereof:
wherein:
Y is a halogen or a group of the formula xe2x80x94NR15R16 or xe2x80x94OR16, wherein R15 is H or optionally substituted C1-4-alkyl, and R16 is H optionally substituted alkyl or aryl;
R14 is H, optionally substituted alkyl or aryl; and
each X independently is as hereinbefore defined.
Preferably R14 is H or optionally substituted C1-4-alkyl, more preferably C1-4-alkyl and especially methyl or ethyl.
Preferably R15 is H or C1-4-alkyl, more preferably H, methyl or ethyl and especially H.
Preferably R16 is H, optionally substituted C1-4-alkyl or optionally substituted phenyl, more preferably H, C1-4-alkyl or phenyl and especially H, methyl and ethyl.
When Y is halogen it is preferably chloro.
It is preferred that Y is a group of the formula xe2x80x94NR15R16, more preferably xe2x80x94NHR16 and especially xe2x80x94NH2.
The dyes of Formula (6) may be prepared by methods analogous to those described in the art for similar azo dyes. For example a suitable method is described in GB 1,271,226, Examples 2 to 153.
In a preferred embodiment, the magenta colorant present in the first set of inks is a dye of the formula (7) or salt thereof:
wherein:
G is halogen or a group of the formula xe2x80x94NR17R18 or xe2x80x94OR17, wherein R17 is H or optionally substituted alkyl;
R18 is H, optionally substituted aryl or optionally substituted alkyl;
R19 and R20 are each independently C1-4-alkyl; and
X is as hereinbefore defined.
It is preferred that R17 is H or optionally substituted C1-4-alkyl, more preferably H or C1-4-alkyl and especially H or methyl.
Preferably R18 is H, optionally substituted phenyl or optionally substituted C1-6-alkyl, more preferably H, C1-6-alkyl or phenyl substituted by C1-4-alkyl, xe2x80x94COOH or xe2x80x94SO3H, especially C1-6-alkyl and phenyl substituted by methyl, ethyl or xe2x80x94SO3H and more especially phenyl substituted with xe2x80x94SO3H and methyl.
R19 and R20 are preferably independently methyl, ethyl or iso-propyl.
When G is halogen it is preferably chloro.
Preferably G is a group of the formula xe2x80x94NR17R18, more preferably xe2x80x94NHR18.
The dyes of Formula (7) may be prepared using methods analogous to those described in the art for other azo dyes. For example a suitable method is described in W094/22961.
A preferred black colorant present in the first set of inks is a 1:2 Chromium or Cobalt complex, or mixture thereof, of Formula (8) or salt thereof:
wherein:
T is halogen or a group of the formula xe2x80x94NR21R22 or xe2x80x94OR21, wherein
R21 is H or optionally substituted alkyl or optionally substituted aryl;
R22 is H or optionally substituted alkyl;
M is Cr or Co; and
X is as hereinbefore defined.
Preferably R21 is H, optionally substituted C1-6-alkyl or optionally substituted phenyl, more preferably H or C1-4-alkyl and especially H, methyl or ethyl.
Preferably R22 is H or C1-4-alkyl, more preferably H.
When T is halogen it is preferably chloro.
It is preferred that T is a group of the formula xe2x80x94NR21R22, more preferably xe2x80x94NHR21.
Preferably a mixture of Cobalt and Chromium complexes of the dyes of Formula (8) are present in the black ink. Preferred mixtures comprise the components:
(a) from 50 to 95, more preferably from 55 to 80 and especially from 60 to 75 parts of the 1:2 chromium complex; and
(b) from 5 to 50, more preferably 20 to 45 and especially 40 to 25 parts of the 1:2 cobalt complex, wherein all parts are by weight and the parts (a)+(b)=100.
The dye of Formula (8) and the complexes thereof may be prepared using methods analogous to those described in the art for similar azo dyes. For example, a suitable method is disclosed in GB 985,481, Examples 1 and 2.
A further preferred black colorant suitable for use in the first set of inks is a dye of the Formula (9) or a salt thereof.
wherein:
X is as hereinbefore defined; and
R23 and R24 are each independently H or optionally substituted alkyl.
Preferably R23 and R24 are each independently H or C1-6-alkyl optionally substituted by xe2x80x94OH or SO3H, more preferably H or C1-4-alkyl and especially H.
The sulpho group on the phenyl ring is preferably attached at the para position relative the second sulpho group on the ring.
It is preferred that the dye of Formula (9) is mixed with a small quantity of a yellow and/or a red dye to give a neutral black shade.
A preferred mixture of dye comprises:
(a) from 50 to 95, more preferably from 60 to 80 parts of the dye of Formula (9);
(b) from 5 to 20, more preferably from 5 to 15 parts of a yellow dye; and
(c) from 10 to 30, more preferably from 15 to 25 parts of a red dye;
wherein all parts are by weight and the sum of the parts (a), (b) and (c)=100. The red and yellow dyes which may be present in the mixture are preferably azo dyes, more preferably water-soluble azo dyes.
A preferred red dye is the dye of the hereinbefore defined Formula (3) wherein X is Cl and E is 2-methylphenylamino. A preferred yellow dye is the dye of the hereinbefore defined Formula (1) wherein X is Cl, A is 3-sulpho-N-methylaniline or 4-sulpho-N-methyl anilino and R1 is amino.
An especially preferred yellow dye is a 1:1 mixture of the dyes comprising:
(i) a dye of Formula (1) in which X is Cl, A is 3-sulpho-N-methylanilino and R1 is amino; and
(ii) a dye of Formula (1) in which X is Cl, A is 4-sulpho-N-methylanilino and R1 is amino.
In view of the foregoing preferences an especially preferred black colorant comprises:
(a) from 60 to 80 parts of the dye of Formula (10);
(b) from 15 to 25 parts of a 1:1 mixture of dyes of Formula (11); and
(c) from 5 to 15 parts of a red dye of Formula (12);
wherein all parts are by weight and the sum of the parts (a), (b) and (c)=100:
The dye of Formula (9) may be prepared using conventional methods for the preparation of azo dyes. For example a suitable method comprises:
(1) diazotising the aniline disulphonic acid of the formula:
(2) diazotising 2-amino-4-nitrobenzenesulphonic acid;
(3) coupling the product of stage (2) with 8-amino-1-naphthol-3,6-disulphonic acid under mildly alkaline conditions;
(4) coupling the product of stage (3) with the product of stage (1) under acidic conditions;
(5) reducing the nitro group on the product of stage (4), for example by hydrogenation over a palladium catalyst;
(6) condensing the product of stage (5) with the triazine compound of the formula:
and
(7) condensing the product of stage (5) with a compound of the formula NHR23R24
wherein X, R23 and R24 are as hereinbefore defined.
A further preferred magenta colorant suitable for use in the first set of inks is a dye of the Formula (13) or salt thereof:
wherein:
Q is halogen or a group of the formula xe2x80x94NR25R26 or xe2x80x94OR25, wherein
R25 is H or optionally substituted alkyl;
R26 is H, optionally substituted aryl or optionally substituted alkyl; and
X is as hereinbefore defined.
It is preferred that R25 is H or optionally substituted C1-4-alkyl, more preferably H or C1-4-alkyl and especially H or methyl.
Preferably R26 is H, optionally substituted phenyl or optionally substituted C1-6-alkyl, more preferably H, C1-6-alkyl or phenyl substituted by C1-4-alkyl, xe2x80x94COOH or xe2x80x94SO3H, especially C1-6-alkyl and phenyl substituted by methyl, ethyl or xe2x80x94SO3H and more especially phenyl substituted with xe2x80x94SO3H and xe2x80x94COOH.
When Q is halogen it is preferably chloro.
Preferably Q is a group of the formula xe2x80x94NR25R26, more preferably xe2x80x94NHR26.
The dyes of Formula (13) may be prepared using methods analogous to those described in the art for other azo dyes. For example a suitable method is described in GB 899,376.
Although Formulae (1) to (13) show the dyes in their free acid form, it is intended that salts of the dyes are included within the scope of the present invention. Thus the inks may contain dyes in their free acid and/or salt forms.
In view of the foregoing preferences for the colorants for the first set of inks, in a particularly preferred embodiment, the first set of inks comprises an ink containing a dye of Formula (5), an ink containing a dye of Formula (6) an ink containing a dye of Formula (7) and an ink containing a dye of Formula (8) or a dye of Formula (9); and the second set of inks comprises an ink containing a dye of Formula (1), an ink containing a dye of Formula (2) an ink containing a dye of Formula (3) and an ink containing a dye of Formula (4).
The labile group or atom represented by X in the dyes of Formulae (1) to (9) is a group or atom which is bound directly to the triazine nucleus and which is readily displaced therefrom in mildly alkaline conditions. Preferred labile groups include for example, a sulphonic acid group; a thiocyano group; a quaternary ammonium group, for example a trialkyl ammonium group or an optionally substituted pyridinium group, for example 3- or 4-caboxypyridinium; xe2x80x94OSO3H; or CH3COOxe2x80x94.
Preferred labile atoms include halogens, more preferably F, Cl or Br and especially Cl.
When the substituents on the dyes of Formulae (1) to (13) are optionally substituted, preferred substituents are selected from xe2x80x94OH, xe2x80x94SO3H, xe2x80x94COOH, xe2x80x94CN, xe2x80x94NO2, xe2x80x94PO3H2, halogen, especially Cl or Br, C1-4-alkyl and C1-4-alkoxy.
It is preferred that the colorants/dyes present in the inks are purified prior to incorporation into the ink by removing substantially all of the inorganic salts and other by products which may be present in the colorant/dye. Suitable purification processes include reverse osmosis and/or ultrafiltration.
The inks used in the first and second set of inks of the present invention comprise the relevant colorant or dye and a medium. The inks may comprise a mixture of two or more different colorants or dyes, or salts thereof, to provide an ink composition of the desired colour for use as an ink of the first or second set of inks of the present invention.
The medium for the ink compositions may be a liquid or a low melting point solid. Liquid media may be aqueous or solvent-based.
It is preferred that when dyes are used in the inks they are dissolved completely in the aqueous or solvent medium to form a solution.
Preferred inks are those comprising a dye, preferably a dye of the Formula (1) to (9) as hereinbefore defined and an aqueous medium.
The inks used in the method of the present invention preferably contain from 0.5% to 20%, more preferably from 0.5% to 15%, and especially from 2% to 12% by weight of the dye/colorant based on the total weight of the ink It is preferred that where the colorant is a dye, it has a solubility of around 10% or more to allow the preparation of concentrates which may be used to prepare more dilute inks and to minimise the chance of precipitation of the dye if evaporation of the liquid medium occurs during use of the ink.
Where the colorant is a dye its solubility can be enhanced by converting the sodium salt, in which form it is usually synthesised, either partially or wholly, into the lithium or ammonium salt Purification of the dye can be conveniently accomplished by use of membrane separation processes to separate unwanted by-products and inorganic materials from the solution or dispersion of the dye, followed by partial or complete exchange of the counter ion.
Where the liquid medium is aqueous based it is preferably water or a mixture of water and one or more water-soluble organic solvent. The weight ratio of water to organic solvent(s) is preferably from 99:1 to 1:99, more preferably from 95:1 to 50:50 and especially from 90:10 to 60:40.
The water-soluble organic solvent is preferably selected from C1-4-alkanols such as methanol, ethanol, n-propanol, isopropanol, n-butanol, sec-butanol, tert-butanol or isobutanol; amides such as dimethylformamide or dimethylacetamide; ketones or ketone-alcohols such as acetone or diacetone alcohol; ethers such as tetrahydrofuran or dioxane; oligo- or poly-alkylene glycols such as diethylene glycols, triethylene glycol, polyethylene glycol or polypropylene glycol; alkenyleneglycols or thioglycols containing a C2-C6-alkylene group such as ethylene glycol, propylene glycol, butylene glycol, pentylene glycol or hexylene glycol, thioglycol and thiodiglycol; polyols such as glycerol or 1,2,6-hexanetriol; C1-4-alkyl-ethers or polyhdric alcohols such as 2-methoxyethanol, 2-2-(2-methoxyethoxy)ethanol, 2-(2-ethoxyethoxy)-ethanol, 2-[2-(2-methoxyethoxy)ethoxy]ethanol, 2-[2-(2-ethoxyethoxy)-ethoxy]-ethanol; heterocyclic ketones, such as 2-pyrrolidone and N-methyl-2-pyrrolidone; or mixtures containing two or more of the aforementioned water-soluble organic solvents for example thiodiglycol and a second glycol or diethylene glycol and 2-pyrrolidone.
Preferred water-soluble organic solvents are 2-pyrrolidone; N-methylpyrrolidone; alkylene glycols and oligo-alkylene glycols, such as ethylene glycol, diethylene glycol, triethylene glycol; and lower alkyl ethers of polyhydric alcohols such as 2-methoxy-2-ethoxy-2-ethoxy-ethanol; polyethylene glycols with a molecular weight of up to 500; and thioglycols such as thiodiglycols. A preferred specific solvent mixture is a binary or ternary mixture of water and diethylene glycol and/or, 2-pyrrolidone or N-methylpyrrolidone in weight ratios 75-95:25-5 and 60-98:1-20:1-20 respectively. An especially preferred specific solvent mixture is a binary or tertiary mixture of water and thiodiglycol and/or 2-pyrrolidone or N-methylpyrrolidone in weight ratios 75-98:25-2 and 60-90:5-20:5-20 respectively.
Examples of suitable aqueous ink media are given in U.S. Pat. Nos. 4,963,189, 4,703,113, 4,626,284, EP 4,251,50A and U.S. Pat. No. 5,207,824.
When aqueous inks are used in the present invention, they preferably also contain a humectant to inhibit evaporation of water and a preservative to inhibit the growth of fungi, bacteria and/or algae in the solution. Examples of suitable humectants are, propan-1,2-diol, butan-1,2-diol, butan-2,3-diol and butan-1,3-diol. However, the presence of small amounts, up to about 10%, preferably not more than 5%, in total, of polyols having two or more primary hydroxy and/or primary alcohols is acceptable, although the ink is preferably free from such compounds
Where the liquid medium is solvent based the solvent is preferably selected from ketones, alkanols, aliphatic hydrocarbons, esters, ethers, amides or mixtures thereof. Where an aliphatic hydrocarbon is used as the solvent a polar solvent such as an alcohol, ester, ether or amide is preferably added. Preferred solvents include ketones, especially methyl ethyl ketone and alkanols especially ethanol and n-propanol.
Solvent based ink compositions are used where fast drying times are required and particularly when printing onto hydrophobic substrates such as plastics, metal or glass.
Where the medium for an ink composition is a low melting point solid the melting point of the solid is preferably in the range from 60xc2x0 C. to 125xc2x0 C. Suitable low melting point solids include long chain fatty acids or alcohols, preferably those with C18-24 chains, or sulphonamides. The dye or colorant may be dissolved in the low melting point solid or may be finely dispersed in it.
The inks may optionally contain other components conventionally used in inks for ink jet printing. For example, viscosity and surface tension modifiers, corrosion inhibitors, kogation reducing additives, surfactants and anti-cockle agents, for example those disclosed in U.S. Pat. No. 5,207,824, column 3, line 13 to column 4, line 21, which is included herein by reference thereto.
If desired, the inks may be buffered to a pH of from 5 to 8, more preferably from 6 to 7, with a suitable buffer such as the sodium salt of metanillic acid or an alkali metal phosphate.
Where the ink jet printing technique involves the charging and electrically-controlled deflection of drops, for example in a continuous ink jet printer, the inks preferably also contain a conducting material such as an ionised salt to enhance and stabilise the charge applied to the drops. Suitable salts for this purpose are alkali metal salts of mineral acids.
In view of the foregoing preferences, a particularly preferred ink composition is an aqueous ink comprising the components:
(a) 0.5 to 20 parts of the relevant dye;
(b) 50 to 98 parts water; and
(c) 2 to 50 parts water soluble organic solvent;
wherein all parts are parts by weight and the parts (a)+(b)+(c)=100. In addition to the components (a), (b) and (c), the ink may also contain further components as hereinbefore mentioned.
The ink jet printer used for the application of the inks to the substrate forms each ink into small droplets by ejection from a reservoir through a small orifice (the ink jet nozzle) so that the ink droplets are directed at the substrate during relative movement between the substrate and the reservoir. This process is commonly referred to as ink jet printing. The ink may be applied to the substrate using a xe2x80x9ccontinuousxe2x80x9d or a xe2x80x9cdrop on demandxe2x80x9d printer, both of which are well known in the art. Continuous ink jet printers produce a stream of ink from the ink jet nozzle which is formed into droplets and directed to the substrate via a suitable control means. Drop on demand printers eject individual droplets of ink from the ink jet nozzle in response to a control signal. Preferred drop on demand ink jet printers for use in the present invention are piezoelectric and thermal ink jet printers. In thermal ink jet printing, programmed pulses of heat are applied to the ink in the reservoir by means of a resistor adjacent to the ink jet nozzle. In piezo-electric printers ink droplets are ejected from the ink jet nozzle using a piezoelectric transducer. The transducer oscillates in response to an electrical control signal, thereby creating a pressure wave in the reservoir adjacent to the ink jet nozzle which ejects droplets of ink from the nozzle.
Ink jet printers suitable for use in the present invention apply at least one ink from the first set of inks and at least one ink from the second set of inks, wherein the first and second sets of inks are as hereinbefore defined.
Preferably the ink jet printer applies a first set of inks consisting of black, cyan, magenta and yellow inks and from one to four, preferably from two to four and especially four of the hereinbefore defined inks of the second set of inks.
Ink jet printers suitable for use in the present invention require a means to access each of the inks comprising the first and second sets of inks, for example from separate ink tanks containing each ink.
Preferably the inks comprising the first and second set of inks are contained in an ink cartridge suitable for use in an ink jet printer. The ink cartridge preferably comprises a container in which are held the first and second set of inks. Preferably the ink jet printer contains the ink cartridge, for example within a suitable housing in the printer.
It is preferred that the printer has a separate channel to direct each ink colour in the first and second set of inks to a nozzle, or array of nozzles, dedicated to that ink colour. The separate ink channels for each ink colour avoids cross contamination of inks in the ink jet head which could result in an undesirable colour on the printed substrate. Accordingly, preferred ink jet printers have from 5 to 8, more preferably from 6 to 8 and especially 8 ink channels. An example of an ink jet printer suitable for use in the present invention is described in EP 616 893 A2.
The substrate used in the ink-jet method of the present invention may be paper, plastics, textile, metal, ceramic or glass and is preferably paper, plastic or a textile material, especially a natural, semi-synthetic or synthetic material.
Examples of natural textile materials include wool, silk, hair and cellulosic materials, particularly cotton, jute, hemp, flax and linen.
Examples of synthetic and semi-synthetic materials include polyamides, polyesters, polyacrylonitriles and polyurethanes.
Preferred substrates include overhead projector slides paper and textile materials. Preferred papers include plain and treated papers. Preferred textile materials are cellulosic materials such as cotton. Especially preferred substrates are treated papers suitable for high resolution xe2x80x9cphoto-realisticxe2x80x9d image printing and cellulosic textile materials.
According to a second aspect of the present invention there is provided a set of ink jet printing inks comprising a first and second set of inks wherein:
(a) the first set of inks consists of a yellow ink, a magenta ink, a cyan ink and optionally a black ink; and
(b) the second set of inks comprises one or more inks selected from:
an ink containing a dye of Formula (1) or salt thereof;
an ink containing a dye of the Formula (2) or a salt thereof;
an ink containing a dye of Formula (3) or a salt thereof; and
an ink containing a dye of Formula (4) or a salt thereof;
wherein the dyes of Formulae (1), (2), (3) and (4) are as hereinbefore defined in the first aspect of the present invention.
Preferred inks in the set according to the second aspect of the present invention are as defined in the first aspect of the present invention.
Accordingly a preferred set of ink jet printing inks comprises:
(a) a first set of inks consisting of:
a cyan ink containing a dye of the Formula (5);
a yellow ink containing a dye of Formula (6);
a magenta ink containing a dye of the Formula (7) or Formula (13); and
a black ink containing a dye of the Formula (8) or Formula (9); and
(b) a second set of inks comprising from one to four, preferably from two to four and especially four inks selected from:
an ink containing a dye of Formula (1);
an ink containing a dye of Formula (2);
an ink containing a dye of Formula (3);and
an ink containing a dye of Formula (4).
According to a third aspect of the present invention there is provided a paper or an overhead projector slide, a metal, glass or ceramic substrate or textile material coloured by means of the method according to the first aspect of the present invention.
According to a fourth aspect of the present invention there is provided a process for the coloration of a textile material using ink-jet printing which comprises the steps:
i) applying to the textile material by ink-jet printing the inks from the first and second sets of ink in accordance with the method of the first aspect of the present invention; and
ii) heating the textile material at a temperature from 50xc2x0 C. to 250xc2x0 C. to fix the dyes and colorants on the material.
The process for coloration of a textile material by ink-jet printing preferably comprises a pre-treatment of the textile material with an aqueous pretreatment composition comprising a water-soluble base, a hydrotropic agent and a thickening agent followed by removing water from the pre-treated textile material to give a dry pre-treated textile material which is subjected to ink-jet printing in step i) above.
The pre-treatment composition preferably comprises a solution of the base and the hydrotropic agent in water containing the thickening agent.
The base is preferably an inorganic alkaline base, especially a salt of an alkali metal with a weak acid such as an alkali metal carbonate, bicarbonate or silicate or an alkali metal hydroxide. The amount of base may be varied within wide limits provided sufficient base is retained on the textile material after pre-treatment to promote the dyeing of the pre-treated textile material. Where the base is sodium bicarbonate it is convenient to use a concentration of from 1% to 5% by weight based on the total weight of the composition.
The hydrotropic agent is present to provide sufficient water to promote the fixation reaction between the dye and the textile material during the heat treatment, in step (ii) above, and any suitable hydrotropic agent may be employed. Preferred hydrotropic agents are urea, thiourea and dicyandiamide. The amount of hydrotropic agent depends to some extent on the type of heat treatment. If steam is used for the heat treatment generally less hydrotropic agent is required than if the heat treatment is dry, because the steam provides a humid environment. The amount of hydrotropic agent required is generally from 2.5% to 50% by weight of the total composition with from 2.5% to 10% being more suitable for a steam heat treatment and from 20% to 40% being more suitable for a dry heat treatment.
The thickening agent may be any thickening agent suitable for use in the preparation of print pastes for the conventional printing of cellulose reactive dyes. Suitable thickening agents include alginates, especially sodium alginate, xantham gums, monogalactam thickeners and cellulosic thickeners. The amount of the thickening agent can vary within wide limits depending on the relationship between concentration and viscosity. However, sufficient agent is preferred to give a viscosity from 10 to 1000 mPa.s, preferably from 10 to 100 mPa.s, (measured on a Brookfield RVF Viscometer). For an alginate thickener this range can be provided by using from 10% to 20% by weight based on the total weight of the pretreatment composition.
The remainder of the pre-treatment composition is preferably water, but other ingredients may be added to aid fixation of the dye to the textile material or to enhance the clarity of print by inhibiting the diffusion (migration) of dye from coloured areas to non-coloured areas before fixation.
Examples of fixation enhancing agents include cationic polymers and quaternary ammonium compounds. Suitable cationic polymers include for example, a 50% aqueous solution of a dicyanamide/phenol formaldehydelammonium chloride condensate e.g. MATEXIL FC-PN (available from ICI), which have a strong affinity for the textile material and the dye and thus increase the fixation of the dye on the textile material. Suitable quaternary ammonium compounds include for example those described in our EP 534 660 A1, incorporated herein by reference thereto, such as distearyl dimethylammonium chloride.
Examples of anti-migration agents are low molecular weight acrylic resins, e.g. polyacrylates, such as poly(acrylic acid) and poly(vinyl acrylate).
In the pre-treatment stage of the present process the pre-treatment composition is preferably evenly applied to the textile material. Where a deeply penetrated print or a deep shade is required the pretreatment composition is preferably applied by a padding or similar process so that it is evenly distributed throughout the material. However, where only a superficial print is required the pre-treatment composition can be applied to the surface of the textile material by a printing procedure, such as screen or roller printing, ink jet printing or bar application.
In the pre-treatment stage of the present process, water may be removed from the pre-treated textile material by any suitable drying procedure such as by exposure to hot air or direct heating, e.g. by infra-red radiation, or micro-wave radiation, preferably so that the temperature of the material does not exceed 100xc2x0 C.
The application of the ink composition to the textile material, stage (i) of the present process, is as hereinbefore defined for the coloration method of the first aspect of the present invention. It is preferred that each ink of the first set of inks contains a reactive dye.
After application of the ink, it is generally desirable to remove water from the printed textile material at relatively low temperatures ( less than 100xc2x0 C.) prior to the heat applied to fix the dye on the textile material as this has been found to minimise the diffusion of the dye from printed to non-printed regions. As with the pretreated textile material removal of water is preferably by heat, such as by exposure to hot air or to infra-red or micro-wave radiation.
In stage (ii) of the present process, the printed textile material is submitted to a short heat treatment, preferably after removal of water by low-temperature drying, at a temperature from 100xc2x0 C. to 200xc2x0 C. by exposure to dry or steam heat for a period of up to 20 minutes. If a steam (wet) heat treatment is used, the printed material is preferably maintained at 100-105xc2x0 C. for from 5 to 15 minutes whereas if a dry heat treatment is employed the printed material is preferably maintained at 140-160xc2x0 C. for from 2 to 8 minutes.
After allowing the textile material to cool, unfixed dye and other ingredients of the pretreatment and dye compositions may be removed from the textile material by a washing sequence, involving a series of hot and cold washes in water and aqueous detergent solutions before the textile material is dried.
According to a fifth aspect of the present invention there are provided textile materials, especially cellulosic textile materials, coloured by means of the process according to the fourth aspect of present invention.
According to a sixth aspect of the present invention there is provided a photorealistic print prepared using the coloration method according to the first aspect of the present invention.
A photorealistic print is a high resolution print which reproduces an image from digital data corresponding to that image. The photorealistic prints prepared in accordance with the present invention exhibit excellent colour yield and a wide colour gamut compared with images formed by conventional CMYK ink jet printers.
Examples of systems which prepare images in digitised form include digital cameras, images stored on a CD ROM system, images that have been digitised using an optical scanning device and computer graphics programs such as CAD/CAM systems.
The digital data corresponding to the image is used by a computer to control the discharge of inks selected from the first and second sets of ink from an ink jet printer in accordance with the coloration method of the first aspect of the present invention, thereby providing a photorealistic print corresponding to the digitised image on a substrate.
The substrate used in the preparation of photorealistic prints may be any of the hereinbefore mentioned substrates. However, preferred substrates are paper, more preferably coated paper. Examples of paper and coated paper substrates suitable for use in the preparation of photorealistic prints include Hewlett Packard coated papers such as HP 516347, HP Premium Coated Paper and HP Photopaper, Stylus Pro 720 dpi Coated Paper, Epson Photo Quality Glossy Film (available from Seiko Epson Corp.), Epson Photo Quality Glossy Paper (available from Seiko Epson Corp.) Canon HR 101 High Resolution Paper (available from Canon), Canon GP 201 Glossy Paper (available from Canon), and Canon HG 101 High Gloss Film (available from Canon).


1. Field of the Invention
The present invention relates to a photographic lens which can focus from infinity to a very close distance. In particular, the present invention is directed to such photographic lens which can be used at 1:1 magnification at maximum.
2. Description of the Prior Art
Lenses hitherto known useful for photography at a very short object distance are classified into two groups.
(1) Lenses of the type comprising a common photographic lens and a supplementary lens for close-up photography (so-called close-up lens) mounted on the common photographic lens; PA1 (2) Lenses of the type which are particularly designed for short distance photography. This type of lens is, when used, shifted forward as a unit from the film plane.
These known systems for photographing a very close object have the following disadvantages in any case:
In the case of the first mentioned system it is impossible to continuously change the magnification at which photography is carried out. For photography within a desired range of magnification, a number of supplementary lenses are required. In addition, exchange of such supplementary lenses is very troublesome to the user.
In the case of the latter mentioned system, it is possible to continuously change the magnification. However, a large and complicated mechanism is needed for shifting the lens. If portability is a consideration, the range of focusing movement available for the lens is limited. For the known system, the available photographic magnification is generally in the order of .times.0.5 at most.
Furthermore, it is desired that a close-up photographic lens satisfy various requirements at the same time. The lens should not only be able to take a photography approaching the object but also to take a photograph at a sufficiently large magnification while keeping a sufficiently large distance from the object to the lens (working distance). The lens should also be as small as possible in size. All of the lenses according to the prior art can not fully satisfy these requirements at the same time.


The detection of pathogenic microorganisms in biological fluids should be performed in the shortest possible time, in particular in the case of septicemia for which the mortality remains high in spite of the broad range of antibiotics which are available to doctors. The presence of biologically active agents such as a microorganism in a patient's body fluid, especially blood, is generally determined using blood culture bottles. A small quantity of blood is injected through an enclosing rubber septum into a sterile bottle containing a culture medium, and the bottle is then incubated at 37° C. and monitored for microorganism growth.
Instruments currently exist on the market in the U.S. that detect the growth of a microorganism in a biological sample. One such instrument is the BacT/ALERT® 3D instrument of the present assignee bioMérieux, Inc. The instrument receives a blood culture bottle containing a blood sample, e.g., from a human patient. The instrument incubates the bottle and periodically during incubation an optical detection unit in the incubator analyzes a colorimetric sensor incorporated into the bottle to detect whether microbial growth has occurred within the bottle. The optical detection unit, bottles and sensors are described in the patent literature, see U.S. Pat. Nos. 4,945,060; 5,094,955; 5,162,229; 5,164,796; 5,217,876; 5,795,773; and 5,856,175, the entire content of each of which is incorporated by reference herein. Other prior art of interest relating generally to the detection of microorganisms in a biological sample includes the following patents: U.S. Pat. Nos. 5,770,394, 5,518,923; 5,498,543, 5,432,061, 5,371,016, 5,397,709, 5,344,417 and its continuation U.S. Pat. Nos. 5,374,264, 6,709,857; and 7,211,430, the entire content of each of which is incorporated by reference herein.
Substantial, and potentially life saving, clinical benefits for a patient are possible if the time it takes for detection of a microbial agent in a blood sample and reporting the results to a clinician could be reduced. A system that meets this need has heretofore eluded the art. However, such rapid detection of a microbial agent in a biological sample such as a blood sample is made possible by apparatus described herein.
The disclosed system and methods combines a detection system operative to detect a container containing a test sample (e.g., a biological sample) as being positive for microbial agent presence. The systems and methods of this disclosure have the potential to: (a) reduce laboratory labor and user errors; (b) improve sample tracking, traceability and information management; (c) interface to laboratory automation systems; (d) improve work-flow and ergonomics; (e) deliver clinically relevant information; (f) faster results.
Many further advantages and benefits over the prior art will be explained below in the following detailed description.


1. Field of the Invention
The present invention relates to a hydraulic cylinder unit used as an actuator, and more particularly, to a simplified structural hydraulic cylinder providing simple maintenance and commonly used parts.
2. Description of the Related Art
The prior art shows a hydraulic cylinder unit 51 of a type, as shown in FIG. 4, in which oil is pumped from one end side of a cylinder to two oil chambers defined in the cylinder by a piston.
The hydraulic cylinder unit 51 comprises a cylinder body 52 including an outer cylinder 53, an inner cylinder 54, a lower cap 55 and an upper cap 56; and a piston 57 which is slidable in the inner cylinder 54. Oil is pumped from the side of the lower cap 55 to an upper chamber a and a lower chamber b (the piston 57 is at the maximum compression position, and b is indicated by a line) defined in the inner cylinder 54 by the piston 57.
That is, the lower cap 55 is provided with an upper chamber port 55a and a lower chamber port 55b. The upper chamber port 55a is communicated with an oil passage c formed between the outer and inner cylinders 53 and 54 through a first communication passage R.sub.1, and the oil passage c is in communication with the upper chamber a through a communication passage Q of the upper cap 56.
The lower chamber port 55b is in communication with the lower chamber b through a second communication passage R.sub.2.
In such a hydraulic cylinder unit 51, in order to move the piston 57 upward, a hydraulic oil is supplied from the lower chamber port 55b to increase the hydraulic pressure in the lower chamber b, and oil in the upper chamber a is discharged from the upper chamber port 55a, and in order to move the piston 57 downward on the contrary, hydraulic oil is supplied from the upper chamber port a, and oil in the lower chamber b is discharged from the lower chamber port 55b.
However, in this conventional structure, since the number of constituent parts of the cylinder body 52 is high, it takes much time to assemble the device. Further, since the upper chamber port 55a, the lower chamber port 55b, the first communication passage R.sub.1 and the second communication passage R.sub.2 are all integrally formed in the lower cap 55, there are problems due to complications in processing of the passages, the number of processing steps is high, the maintenance operation requires excessive time and labor, the cost is increased, and the lower cap is prone to be large in size.
Further, since a joint is threaded into the port portion, the port portion may be damaged if it is repeatedly attached and detached many times. In such a case, it is necessary to exchange the entire lower cap.
Furthermore, if it is necessary to vary a diameter of the inner cylinder, and to reduce a diameter of the piston, the entire inner cylinder must be integrally exchanged, and it is difficult to commonly use the parts.


Currently, hoppers and powered screw conveyors are used for delivering feed to animals. Such feed systems, however, have been known for being problematic and requiring periodic maintenance and attention in order to keep the feed flowing and the systems operating.


1. Field of the Invention
The present invention is directed generally to a cosmetic application system and method, and more particularly to a system and method for removing excess mascara from a mascara brush upon withdrawal from a container.
2. Description of the Related Art
Various techniques and structures have been used to reduce the amount of mascara on a mascara brush upon removal from a container. However, a number of disadvantages associated with these techniques and structures has inhibited their widespread use and manufacture.
In particular, U.S. Pat. Nos. 4,194,848, 4,332,494, 4,407,311, 4,609,300 and 4,705,053 are directed to mascara applicators having a complex structure for varying the amount of mascara remaining on a brush after removal from a container. A flexible member is disposed in the neck of the container to provide some degree of variation in the amount of mascara removed from a brush as it passes through an opening in the container. However, each of these patents is directed to a complex structure, which is difficult and costly to manufacture. Moreover, many of these structures do not facilitate continuous variation of the amount of mascara to be removed from a brush. In addition, because these structures apply an equal force against the brush during removal and re-insertion of the brush into the container, these systems unnecessarily impede a user's ability to reinsert the brush into the container after each use. In U.S. Pat. No. 5,397,193, an additional attempt was made to provide a system for removing excess mascara from an applicator brush. In this system, a plurality of internal flexible bristles are used to remove excess mascara from the applicator brush. As with the aforementioned patents, this system is also costly and difficult to manufacture, and does not facilitate continuous variation in the amount of force to be applied to the mascara brush upon removal from its container. In addition, this system also unnecessarily impedes a user's ability to reinsert the brush into the container after each use.
In addition, each of the aforementioned systems, because of their complicated internal structure, is particularly difficult to clean. Accordingly, these go systems do not lend themselves for use with any form of reusable or interchangeable mascara system.


The present disclosure pertains to controllers and particularly to controllers having network switches.


The invention relates to scintillator materials, to a manufacturing process for obtaining them and to the use of said materials, especially in gamma-ray and/or X-ray detectors.
Scintillator materials are widely used in detectors for gamma rays, X-rays, cosmic rays and particles having an energy of the order of 1 keV and also above this value.
A scintillator material is a material that is transparent in the scintillation wavelength range, which responds to incident radiation by emitting a light pulse.
It is possible to manufacture from such materials, which are generally single crystals, detectors in which the light emitted by the crystal that the detector contains is coupled to a light detection means and produces an electrical signal proportional to the number of light pulses received and to their intensity. Such detectors are used in particular in industry to measure thickness and grammage or coating weight, and in the fields of nuclear medicine, physics, chemistry and oil research.
One family of known scintillator crystals that is used is that of cerium-doped lutetium silicates. Cerium-doped Lu2SiO5 is disclosed in U.S. Pat. No. 4,958,080, and the U.S. Pat. No. 6,624,420 discloses Ce2x(Lu1-yYy)2(1-x)SiO5. Finally, U.S. Pat. No. 6,437,336 relates to compositions of the Lu2(1-x)M2xSi2O7 type, where M is at least partly cerium. These various scintillator compositions all have in common a high stopping power for high-energy radiation and give rise to intense light emission with very rapid light pulses.
A desirable additional property is to reduce the amount of light emitted after the incident radiation stops (i.e. delayed luminescence or afterglow). Physically, this phenomenon, well known to those skilled in the art, is explained by the presence of electron traps in the crystallographic structure of the material. The phenomenon of scintillation relies on the photoelectric effect, which creates an electron-hole pair in the scintillator material. Upon recombination on an active site (a Ce3+ site in the aforementioned scintillators), the electron emits photons via a process that generally takes place in much less than one microsecond. The aforementioned scintillators, which are particularly rapid, result in a pulse duration that decreases with a first-order exponential constant of around 40 ns. However, the trapped electrons do not generate light, but their detrapping by thermal excitation (including at room temperature) gives rise to photon emission—the afterglow—, which still remains measurable after times of greater than one second.
This phenomenon may be unacceptable in applications in which it is desired to isolate each pulse, using very short windowing. This is particularly the case with CT (computed tomography) applications (scanners) that are well known in the medical or industrial sectors. When the CT system is coupled to a PET (Positron Emission Tomography) scanner, which is becoming the standard in industry, the poorer resolution of the CT affects the performance of the entire system and therefore the capability of the clinician to interpret the result of the complete PET/CT system. Afterglow is known to be completely unacceptable for these applications.
Compositions of the lutetium silicates type, disclosed in U.S. Pat. No. 4,958,080 (of the LSO:Ce type, using the notation of those skilled in the art) and U.S. Pat. No. 6,624,420 (of the LYSO:Ce type) are known to generate a significant afterglow. In contrast, the compositions disclosed in U.S. Pat. No. 6,437,336 (of the LPS:Ce type) have the advantage of a much weaker afterglow. These results are given for example by L. Pidol, A. Kahn-Harari, B. Viana, B. Ferrand, P. Dorenbos, J. de Haas, C. W. E. van Eijk and E. Virey in “Scintillation properties of Lu2Si2O7:Ce3+, a fast and dense scintillator crystal”, Journal of Physics: Condensed Matter, 2003, 15, 2091-2102. The curve shown in FIG. 1 is extracted from this article and represents the amount of light detected in the form of the number of events (or counts) per mg of scintillator material as a function of time, under X-ray excitation for a few hours. The LPS:Ce composition gives a significantly better result in terms of afterglow.
The behavior of LYSO is very similar to that of LSO from this standpoint. The reduction in this afterglow forms the subject of the present application.
The afterglow property may be demonstrated more fundamentally by thermoluminescence (see S. W. S. McKeever “Thermoluminescence of solids”, Cambridge University Press (1985)). This characterization consists in thermally exciting a specimen after irradiation and measuring the light emission. A light peak close to room temperature at 300 K corresponds to an afterglow of greater or lesser magnitude depending on its intensity (detrapping). A peak at a higher temperature corresponds to the existence of traps that are deeper but less susceptible to thermal excitation at room temperature. This is illustrated in FIG. 2, extracted from the aforementioned article by L. Pidol et al., which shows, in another way, the advantage of a composition of the LPS type in terms of afterglow.
However, compositions of the LPS type have the drawback of a lower stopping power than those of the LSO or LYSO type. This situation stems simply from the average atomic number of the compound and from the density of the associated phase.


1. Field of the Art
The present invention relates to an electronic typewriter having a carriage which is automatically returned upon entering of predetermined carriage-return data such as space data or hyphen data through the corresponding key on a keyboard, if the carriage-return data is entered to be executed within a predetermined automatic-carriage-return zone which consists of a desired number of columns just before or up to the right-hand margin of a line of printing.
2. Related Art Statement
In making documents by means of an electronic typewriter, it is a common practice that a pair of successive space data are entered following period data at the end of a sentence in order to distinguish a space between sentences from a space between words of a sentence.
If the above typing method is used on an electronic typewriter having a function of executing an automatic carriage return, more specifically, if two sets of space data are entered in succession following period data as data to be executed within an automatic-carriage-return zone, the first space data causes the automatic carriage return operation. As a result, the second space data of the two is, against operator's will, executed to insert a space into the first column of a new line on a printing sheet of paper, whereby the beginnings of individual printed lines on the sheet of paper become uneven or indented unexpectedly.
To solve above problem, the existing electronic typewriters are designed not to execute the second space data if two sets of space data are entered in succession for execution within the automatic-carriage-return zone.
The above solution, however, has another problem which will occur when a certain number of space data are entered through a space key in order to insert the corresponding number of spaces at the beginning of a new line to open a paragraph. In other words, since space data is not executed when it is entered in the automatic-carriage-return mode, the number of space data which are executed at the beginning of a new line does not always correspond to the number of depressions of the space key. In order to open a new paragraph, therefore, it is required in the existing electronic typewriters that a desired number of space data be entered only after completion of the automatic carriage return operation. As a result, the existing electronic typewriters have a disadvantage of low typing speed.


String instruments include instruments such as the violin, viola, cello, double bass (sometimes called the contrabass), and harp. String instruments can be very challenging to learn and to teach, in part because mastery of string instruments requires knowledge of and experience with all of their interconnected components.
The violin, viola, cello, and double bass all consist of a body, a curved, hollow section made of wood where the sound resonates, and a neck, a straight piece that extends from the body with four strings stretched along it, attached to tuning pegs at the end. For example, FIG. 1 illustrates a diagram of violin and its component parts.
Part of learning to play these instruments involves learning how to string and tune each of the musical strings. A string is made from a core, and then layers of a synthetic material or metal compound is wrapped around the core to make the string. After the string is made, a “silking” is applied. This “silking” is comprised of a colored wrapping made out of fine fibers. These fibers are wrapped at the upper and lower ends of the strings. The silking can be used to identify the brand, and to make the upper portion of the string sturdy by absorbing tension as the string is initially threaded through the hole inside of each peg and wrapped in the peg box to a desired pitch.
Frequently, when strings are purchased in a set, there are no instructions as to how to differentiate one string from the next. An experienced musician would understand that he or she would have to separate all strings and then place them in order from thinnest to thickest in order to figure out where each string should be placed inside the peg box. However, the inexperienced musician would not know to do this without help.
Since each peg on a fretless instrument, such as a violin, receives a specific string, a string may break because a consumer may be unfamiliar of where to place a string inside the peg box. FIG. 2 illustrates an example peg box containing the four pegs used in violins, along with the corresponding strings. Each string is a specific length and width. For example, the G string on the violin is the thickest string. The D string on a violin is wider than an A string, but an E string on the violin is the thinnest string of all four strings. If a consumer does not know how to distinguish the differences between each string, he or she may place the strings in the wrong pegs. This will cause strings to pop or break prematurely.
Tuning the instrument can also be difficult, as a string may also break when a user turns the peg past its tension point when trying to tune the string. Even when a string does not break, tuning string instruments is a problem for novice instrumentalists and to those who have difficulty with pitch recognition.
Further complicating the learning process is the fact that fretless instruments are unlike most other instruments because each string contains a variation of intervals and overtones. For example, on a piano keyboard, the keys are spaced in intervals consisting of either whole steps or half steps. There is no interval lower than a half step. Unlike the piano, the strings on fretless instruments contain intervals that can be played lower than half steps. The reason is because each pitch on a string is relative to where an instrumentalist places his or her fingers on the fingerboard of the instrument. Without frets, there is no guarantee that an instrumentalist will place his or her finger on the fingerboard exactly one whole step or exactly one half step from the starting pitch.


Field of the Invention
The present invention relates to a circuit configuration for protecting a power MOSFET.
Circuit configurations for protecting power MOSFETs against overvoltage have long been known and are shown, for instance, in the Siemens Datenbuch [Siemens Databook] "Smart-SIPMOS", 1994/95, pages 2-7, FIG. 4. An overvoltage protection circuit configuration disclosed therein includes a Zener diode ZD2 and a diode D1.
A MOSFET semiconductor component with a voltage spike protection element which is also known from German Published, Non-Prosecuted Patent Application DE 41 22 347 A1, includes a transistor element with a gate electrode, a source electrode, and a drain electrode. In it, a Zener diode with a cathode electrode and an anode electrode is coupled to the drain electrode of the transistor element. A horizontal MOSFET element is also presented that has a gate electrode and a drain electrode. The drain electrode is coupled to the anode electrode of the Zener diode, and the source electrode of the MOSFET element is coupled to the gate electrode of the transistor element. A back-gate electrode which is also proposed therein is coupled to the source electrode of the transistor element.
The wiring of the MOSFET referred to at the outset may also be achieved by using an MOS diode which is realized by an MOS transistor having a gate terminal and a drain terminal that are short-circuited, instead of using the diode D1. FIG. 2 shows one such circuit, which is described in more detail below. In particular, such a protective circuit configuration is used in high-side switches with a charge pump. The MOS diode then takes on the task of blocking the high gate voltage from the supply in the normal operating state. In the event of overvoltage, that MOS diode is operated in the conducting direction, but the on-state voltage can assume undesirably high values under some circumstances.


Transmissions of small utility vehicles often utilize a dog-clutch assembly operable to adjust the configuration of the transaxle. To shift gears, a user adjusts the position of a dogged shifting gear within the transmission by actuating a shifter handle. Transmissions of this type can only shift into gear when the dogs of the shifting gear and the driving gear are properly aligned. If the dogs are misaligned (a state often referred to as dead-head), the shifting gear cannot move into engagement with the driving gear.
Conventional shifting systems utilizing dog-clutches suffer from a variety of limitations and disadvantages, such as those relating to shifting gears when the transmission is dead-headed. For example, when the dogs are not aligned, the user must continue to apply force to the shifter handle until the dogs become aligned. Once the dogs become aligned, the force provided by the user causes the shifting gear to move into engagement with the driving gear, and the user can stop applying force to the shifter handle. There is a need for the unique and inventive gear-shifting apparatuses, systems and methods disclosed herein.


A building's structure must withstand physical forces or displacements without danger of collapse or without loss of serviceability or function. The stresses on buildings are withstood by the buildings' structures.
Buildings five stories and less in height typically use a “bearing wall” structural system to manage dead and live load vertical forces. Vertical forces on the roof, floors, and walls of a structure are passed vertically from the roof to the walls to the foundation by evenly spreading the loads on the walls and by increasing the size and density of the framing or frame structure from upper floors progressively downward to lower floors, floor-to-floor. For ceilings and floor spans, trusses are used to support loads on the ceilings and floors and to transfer these loads to walls and columns.
Where vertical bearing elements are absent, for example at window and door openings, beams are used to transfer loads to columns or walls. In buildings taller than five stories, where the walls have limited capacity to support vertical loads, concrete and/or structural steel framing in the form of large beams and columns are used to support the structure.
Lateral forces (e.g., wind and seismic forces) acting on buildings are managed and transferred by bracing. A common method of constructing a braced wall line in buildings (typically 5 stories or less) is to create braced panels in the wall line using structural sheathing. A more traditional method is to use let-in diagonal bracing throughout the wall line, but this method is not viable for buildings with many openings for doors, windows, etc. The lateral forces in buildings taller than five stories are managed and transferred by heavy steel let-in bracing, or heavy steel and/or concrete panels, as well as structural core elements such as concrete or masonry stair towers and elevator hoistways.
There is a need for a panelized and modular system for constructing and assembling buildings without relying on concrete and/or structural steel framing, heavy steel let-in bracing, and heavy steel and/or concrete panels.


The present invention relates to triggering the production and introduction of shock waves into the body of a living being, such as a patient, in synchronism with the breathing of that patient.
German Printed Patent Application 3,146,628 (see also U.S. Pat. No. 4,745,920 and 4,685,461) describes the comminution of concrements by means of shock waves wherein the shock waves are triggered inter alia in response to the breathing of the patient. The purpose is the following. Breathing introduces, from an overall point of view, motion and displacement of organs and parts within the body of that person. This displacement is also effective on concrements such as kidney stones to be comminuted. Hence the location of the concrements varies periodically with the breathing of the person. On the other hand, focusing of shockwaves requires a definite point and locus into which shock waves are to be focused. Therefore the motion of the concrement on the one hand, and the focusing action on the other hand, have to be synchronized, which means that in the course of oscillatory displacement of the concrement on account of breathing, one can establish the locus for the concrement during a particular phase of the breathing cycle, by triggering shockwave generation during one of the next breathing cycles in the same phase point under the assumption that the concrement will have moved back to exactly the same position it had previously during a similar phase within a breathing cycle.
The following are references which refer broadly to this field of art and are of an exemplary nature only. Among thim is also the U.S. Pat. No. 4,539,989 which discloses a device for comminution of concrement in connection with a coupling cushion by means of which the device producing the shock wave is acoustically coupled to the body of the person.


1. Field
The invention relates to the field of computer configuration and, more particularly, to the storage of computer configuration signals.
2. Background Information
Computer systems may store configuration signals in a memory. A computer system is any device including a processor capable of executing one or more instructions to generate signals. Such signals typically take the form of sequences of binary signals known as bits. Examples of computer systems are personal computers, workstation computers, server computers, hand held computers, and set top boxes to name just a few examples. Configuration signals are signals that may determine various settings for the operation of the computer system. For example, configuration signals may determine whether various input/output (I/O) ports comprised by the system are enabled, and I/O addresses for these ports. Configuration signals may determine other computer system settings as well. Such computer configuration signals are well known in the art as “set up information”. On personal computers, setup information is also often stored in a memory known as a real time clock (RTC) complementary metal oxide silicon (CMOS).
Setup information may be applied prior to or during the booting of a program to control the computer system. Booting is the process of placing a sequence of instructions (a program) in control of various computer system resources. Resources include memory, interrupts, files, and I/O ports. An example of a program to boot is an operating system. An operating system is a program which controls various computer resources including those mentioned previously and further including typical I/O devices, such as a mouse and keyboard. Examples of operating systems are the Unix™ operating system and the Microsoft™ Windows™ operating system.
Setup information may be read, altered, and written back to a CMOS or other memory, where it is stored using a special program called a “setup program.” The setup program may be part of the sequence of instructions comprising the computer system's power-on self test (POST) program. Often, the POST executes prior to the basic input/output system (BIOS) program of the computer system in order to initialize settings.
The settings determined by setup information may vary among different computer makes and models. Furthermore, the location and lengths of the bit sequences that comprise the setup information in the memory in which they are stored may vary. Accordingly, it may be difficult to create one set up program to read, alter, and write back set up) information for various makes and models of computer systems. Instead, multiple set up programs may be called for different makes and models of computer system.
Existing setup programs typically employ a crude “textual” interface. Textual interfaces are well known in the art and may comprise an 80×25 matrix of character positions. The number, type, and position of characters in a textual interface is limited as are the number of colors in which such characters may be displayed. It is well known that such textual interfaces are more limited than modem “graphical user interfaces” (GUI) which provide individual control of the color and position on a per pixel basis on the computer system display. Typically, it is the operating system which implements a graphical user interface for the computer system. However, setup programs may execute before the operating system boots, and, therefore, the setup program may employ a less sophisticated textual interface instead of a GUI.
Thus, there is a continuing need for a setup program which may operate with various makes and models of computer systems and which may take advantage of graphical user interface features provided by an operating system.


Arrows have existed since before the dawn of history. The accurate placement and alignment of feathers on a shaft has long been a problem. Accordingly, numerous devices have been utilized over the centuries to apply feathers to a shaft. Some of the very recent devices have been patented.
For example, U.S. Pat. No. 1,896,563 to Belshaw relates to an arrow fletching machine in which horizontal movable bars operate in conjunction with an indexed wheel.
U.S. Pat. No. 2,286,574 to Rohde relates to a fletching jig adapted to high speed production of accurately feathered arrows.
U.S. Pat. No. 2,731,992 to Lozon relates to a fletching fixture containing a supporting structure for rotatably supporting the shaft of an arrow so that the shaft can be turned in a plurality of selective positions to have feathers applied thereto in circumferentially arranged positions.
U.S. Pat. No. 2,742,064 to Quist relates to a fletching device for holding the shaft of an arrow in position for receiving feathers and to another device for applying a feather to the shaft.
U.S. Pat. No. 2,836,208 to Hoyt relates to a universally adapted jig to accurately position and hold a plurality of either right or left wing feathers for either straight or spiral style fletching.
U.S. Pat. No. 2,884,034 to Portinga relates to a fletching jig which is adjustable to accomodate the fletching of feathers upon arrows in various degrees of spiralling in either a clockwise or counterwise direction about a shaft.
U.S. Pat. No. 2,918,097 to Thompson relates to a fletching jig for positioning the feathers on the shaft of arrows, either parallel with the shaft or an angle to the shaft.
U.S. Pat. No. 3,024,017 to Stanton relates to providing a rigid, nonadjustable fletching jig which permits the application of an adhesive directly to the arrow shaft through the use of a slim nozzle.
U.S. Pat. No. 3,015,483 to Martin relates to a fletching jig which allows fletches to be applied to the arrow shaft at desired angular locations.


1. Field of the Invention
The present invention pertains to a modified lignosulfonate composition; its method of preparation and its use as a dispersant, particularly in the manufacture of gypsum wallboard.
2. Description of Related Art
The use of lignosulfonate as a dispersing agent in the preparation of gypsum wallboard is disclosed, for example, in U.S. Pat. No. 2,856,304. In the manufacture of gypsum products such as wallboard, lath, plaster board, sheathing or other products, calcined gypsum is formed into a slurry with a suitable amount of water and, where customary, with other additives such as paper fiber, wood fiber, starch, rosin, etc.
In the preparation of wallboard or similar products, in particular, the slurry then is deposited between paper liners, pressed to the desired thickness by forming rolls, allowed to set and harden, cut to desired lengths, and passed through a dryer to remove excess moisture. A portion of the water used in making the slurry combines with the calcined gypsum, as water of crystallization, in forming the final set mass of interlaced crystals, but a large portion of the water must be removed in the dryer. Obviously, the drying process is more costly as the proportion of water to be removed from the formed board is higher.
It is known that using lignosulfonate as a dispersing agent reduces the amount of water required to provide a flowable gypsum slurry during the deposition and forming steps. Consequently, by using lignosulfonate, the amount of water to be removed during the final drying step can be reduced, resulting in a significant economy of operation, particularly as regards lower energy costs. An ancillary benefit also often observed is higher board strength. It also is known that lignosulfonate exhibiting improved dispersing ability is prepared by base exchange of the lignosulfonate with various metals, including iron, aluminum, chromium and copper, by alkaline treatment, by oxidation and the like. See, for example U.S. Pat. Nos. 2,935,504; 3,007,910; and 3,108,008.
Unfortunately, lignosulfonates also tend to retard the hardening or cure rate of the gypsum board, referred in the art as set retardation. While this does not present a problem with slower forming operations characteristic of the prior art, with the advent of faster processes, set retardation has matured into a significant concern. In fact, while hydrolysis and oxidation reactions tend to enhance the dispersing behavior of the lignosulfonate, such treatments tend to exacerbate set retarding characteristics.
In the prior art, the problem of set retardation has been dealt with primarily by adding various accelerating agents to the aqueous lignosulfonate-gypsum slurry. The prior art indicates that materials such as sodium chloride, aluminum sulfate, potassium sulfate, calcium sulfate dihydrate, and uncalcined or raw gypsum help to ameliorate set retardation.
Finally, in U.S. Pat. No. 2,856,304 it is taught that calcining raw gypsum containing a small amount of lignosulfonate helps reduce the setting time of the calcined gypsum product.
In accordance with the present invention, lignosulfonate is treated in a way which enhances its capability to disperse gypsum, while at the same time, avoids imparting to the lignosulfonate an undesirable increase in its set retardation characteristics. By using the modified lignosulfonate composition of the present invention, the amount of water needed to form a calcined gypsum slurry having the necessary plasticity is considerably reduced, and the production of gypsum shapes is simultaneously accelerated.


1. Field of the Invention
The field of the invention relates to the preparation of random linear injection moldable amide-imide copolymers which process comprises reacting fully or partially acylated aromatic diamines with aromatic tricarboxylic acid anhydrides or mixtures of aromatic tricarboxylic acid anhydrides and aromatic dicarboxylic acids and to novel polytrimellitic amide-imide copolymers and to molded objects and fibers prepared from these copolymers.
2. Background
Amide-imide and polyamide polymers and copolymers are a relatively new class of organic compounds known for their solubility in nitrogen containing solvents when in the polyamic acid form. The major application of these amide-imides has been as wire enamels and film formers. This is illustrated in U.S. Pat. Nos. 3,852,106 (1974), 3,817,942 (1974), 3,661,832 (1972), 3,454,890 (1970) and 3,347,942 (1967).
Polyimide and polyamide-imide polymers have also been found useful for molding applications as shown in U.S. Pat. Nos. 4,016,140 (1977), 3,654,227 (1972) and 3,573,260 (1971).
The general object of this invention is to provide injection moldable amorphous linear amide-imide copolymers. A more specific object of this invention is to provide a novel process for the manufacture of injection moldable amide-imide and amide copolymers by reacting fully or partially acylated aromatic diamines with aromatic tricarboxylic acid anhydrides or mixtures of aromatic dicarboxylic acids and aromatic tricarboxylic acid anhydrides. Another object is to provide novel polyamide-imide copolymers suitable for use as an engineering plastic particularly for and in injection molding. Other objects appear hereinafter.
We have discovered a novel melt condensation process in which fully or partially acylated aromatic diamines are reacted with aromatic tricarboxylic anhydrides or mixtures of aromatic tricarboxylic anhydrides with aromatic dicarboxylic acids to yield engineering plastics suitable for injection molding which feature very high tensile strength and heat distortion temperatures. Our novel process for the preparation of random linear injection moldable amide-imide and amide copolymers comprises reacting fully or partially acylated aromatic diamines with aromatic tricarboxylic acid anhydrides or mixtures of aromatic tricarboxylic acid anhydrides with aromatic dicarboxylic acids in a molar ratio of about 9:1 to about 1:9 at a temperature of about 450.degree. to 750.degree. F.
In the prior art, melt reaction of tricarboxylic acid anhydride compounds with aromatic diamines have produced products which are not suitable for injection molding application. The reason for this is not known, but it is specified that various side reactions occur. It has now been discovered that when fully or partially acylated diamines are reacted, injection molding grade polyamide-imide copolymers are produced. In our process we usually acylate more than half of the diamines utilized in the reaction. The preferred acylation is about 70 to 100 percent.
Evidence for linearity for our novel copolymer is demonstrated by the solubility of the polymer. Polymers produced from tricarboxylic acid anhydride compounds such as trimellitic acid anhydride and aromatic diamines via various melt polymerization methods show no solubility for products having inherent viscosity in excess of 0.5. The copolymer produced according to the novel process utilizing partially or fully acylated diamines is essentially soluble after curing with inherent viscosities in the range of 0.6 to 3.0. For the purpose of this invention, inherent viscosity is measured at 25.degree. C. and 0.5% w/v in 100% sulfuric acid or N-methylpyrrolidone.
The novel injection moldable amorphous random linear polyamide-imide copolymers of this invention comprise units of ##STR1## R comprises R.sub.1 and R.sub.2, R.sub.1 and R.sub.2 are divalent aromatic hydrocarbon radicals of from 6 to about 20 carbon atoms or two divalent hydrocarbon radicals of from 6 to 20 carbon atoms joined directly or by stable linkages selected from the group consisting of --O--, methylene, --CO--, --SO.sub.2 --, and --S-- radicals and wherein said R.sub.1 and R.sub.2 containing units run from about 10 mole percent R.sub.1 containing unit and about 90 mole percent R.sub.2 containing unit to about 90 mole percent R.sub.1 containing unit and about 10 mole percent R.sub.2 containing unit.
The novel injection moldable random linear copolymer may comprise structural Units A and B and also include Unit C of the following formula: ##STR2## wherein X is a divalent aromatic radical usually a divalent benzene radical and R.sub.3 comprises both R.sub.1 and R.sub.2 as defined above or is equal to R.sub.1. Furthermore, if structure C is present R of structural Units A and B can be equal to R.sub.1 or comprise both R.sub.1 and R.sub.2 as set forth above.
In the foregoing structural units Z is a trivalent aromatic radical. Z may be a trivalent radical of benzene, naphthalene, biphenyl, diphenyl ether, diphenyl sulfide, diphenyl sulfone, ditolyl ether, and the like.
Useful aromatic tricarboxylic acid anhydrides which contribute the trivalent radical moiety of Z include those compounds containing at least one pair of carboxyl groups in the ortho position with respect to each other or otherwise situated in a fashion which permits the formation of an anhydride structure, one other carboxyl group and from 9 to 21 carbon atoms. Within these limits, these compounds may contain one or more benzenoid rings such as, for instance, trimellitic anhydride and its isomers and multi-ring compounds such as the 1,8-anhydride of 1,3,8-tricarboxylnaphthalene. Usually these compounds contain up to three benzenoid rings.
The aromatic tricarboxylic acid anhydride used in the novel process to form the polyamide-imide polymers of this invention is of the formula: ##STR3## where Z is a trivalent aromatic radical defined as set forth hereinabove. The following aromatic tricarboxylic anhydrides are preferred: trimellitic acid anhydride; 2,3,6-naphthalene tricarboxylic anhydride; 1,5,6-naphthalene tricarboxylic anhydride, and the like; 2,6-dichloronaphthalene-4,5,7-tricarboxylic anhydride, and the like. One of the preferred aromatic tricarboxylic anhydrides is trimellitic anhydride since this compound is readily available and forms polymers having excellent physical properties of tensile strength and elongation and is resistant to high temperatures.
Suitable fully or partially acylated aromatic diamines useful in applicant's process include para- and meta-phenylenediamine, oxybis (aniline), thiobis (aniline), sulfonylbis (aniline), diaminobenzophenone, methylenebis (aniline), benzidine, 1,5-diaminonaphthalene, oxybis (2-methylaniline), thiobis (2-methylaniline), and the like. Examples of other useful aromatic primary diamines are set out in U.S. Pat. No. 3,494,890 (1970) and U.S. Pat. No. 4,016,140 (1977) both incorporated herein by reference.
Useful aromatic dicarboxylic acids include isophthalic acid and terephthalic acid. In applicant's process further preparation of injection moldable amide-imide and amide copolymers process can be conducted without utilizing a solvent or fluidizing agent though it is preferred to use agents such as N-methylpyrrolidone, dimethyl-acetamide, or acetic acid for the initial mixing of reactants. In general, since these polymers are linear, they may be easily cured in the melt using a twin screw extruder as the finishing reactor instead of a solid state polymerization. However, in some instances, it may be helpful to solid state polymerize the copolymers. The term "solid state polymerization" refers to chain extension of polymer particles under conditions where the polymer particles contain their solid form and do not become a fluid mass.
The solid state polymerizing can be carried out below the melting point of the copolymer and can be conducted in several ways. However, all the techniques require heating the ground or pelletized copolymer below the copolymer melting point, generally of about 400.degree. to 600.degree. F. while either sparging with an inert gas such as nitrogen or air or operating under vacuum.
Injection molding of the novel copolymer is accomplished by injecting the copolymer into a mold maintained at a temperature of about 350.degree.-500.degree. F. In this process a 0.1-2.0 minutes cycle is used with a barrel temperature of about 500.degree. F. to 700.degree. F. The injection molding conditions are given in Table I.
TABLE I ______________________________________ Mold Temperature 350-500.degree. F. Injection Pressure 2,000-40,000 psi and held for 0.5-20 seconds Back Pressure 0-400 psi Cycle Time 6-120 seconds Extruder: Nozzle Temperature 500.degree. F. to 700.degree. F. Barrels: Front heated to 500.degree. F. to 700.degree. F. Screw: 10-200 revolutions/minute ______________________________________
The mechanical properties of the polymers prepared in the Examples are given in Tables II, III, IV, V, VI and VII.
In applicant's process the acylated aromatic diamines need not be isolated or purified prior to their further reaction with the tricarboxylic acid anhydride compound or mixture of the tricarboxylic acid anhydride with dicarboxylic acid. Therefore, one can react one to two moles of acetic anhydride or acid or propionic anhydride or acid or any other C.sub.2 through C.sub.8 containing aliphatic anhydride or acid and one mole of the appropriate aromatic diamine or diamine mixture and use the resulting diacylated diamine solution in acetic acid or propionic acid to react with the tricarboxylic anhydride compound, or mixtures of the tricarboxylic anhydride compound with dicarboxylic acid.
In most cases, linear high molecular weight polyamide-imide polymers result after melt and/or solid state polymerization.


Technical Field
The present disclosure relates generally to the field of reposable or reusable surgical instruments. In particular, the disclosure relates to instruments having separable and replaceable components to provide clean, sterile or refurbished surfaces in each instance of use.
Background of Related Art
One type of surgical device is a linear clamping, cutting and stapling device. Such a device may be employed in a surgical procedure to resect a cancerous or anomalous tissue from a gastro-intestinal tract. Conventional linear clamping, cutting and stapling instruments include a pistol grip-styled structure having an elongated shaft and distal portion. The distal portion includes a pair of scissors-styled gripping elements, which clamp the open ends of the colon closed. In this device, one of the two scissors-styled gripping elements, such as the anvil portion, moves or pivots relative to the overall structure, whereas the other gripping element remains fixed relative to the overall structure. The actuation of this scissoring device (the pivoting of the anvil portion) is controlled by a grip trigger maintained in the handle.
In addition to the scissoring device, the distal portion also includes a stapling mechanism. The fixed gripping element of the scissoring mechanism includes a staple cartridge receiving region and a mechanism for driving the staples up through the clamped end of the tissue against the anvil portion, thereby sealing the previously opened end. The scissoring elements may be integrally formed with the shaft or may be detachable such that various scissoring and stapling elements may be interchangeable.
A number of surgical device manufacturers have developed product lines with proprietary drive systems for operating and/or manipulating such surgical device. In many instances, such surgical device further includes a handle assembly, which is reusable, and a disposable end effector or the like that is selectively connected to the handle assembly prior to use and then disconnected from the end effector following use in order to be disposed of or in some instances sterilized for re-use.
Surgical devices that are reposable, or reusable for multiple procedures, reduce the instrumentation costs per procedure. Providing a reusable surgical device, however, presents various challenges. For example, the complexity of a surgical device tends to result in fairly labor intensive cleaning procedures to prepare the surgical device for subsequent use. Improper cleaning may result in dangerous contamination being introduced into the surgical site. Also, some reusable surgical devices have removable and replaceable components to provide clean surfaces for each use. Many of these surgical devices require arduous disassembly and reassembly procedures that require extensive training, and may discourage use of the surgical device.