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Analysis of the emission of volatile and condensable substances from vehicle interior materials by thermodesorptionPB VWL 709Page 1 of 24Issued : 2001-01-11Author:Approved:Replaces : 2000-07-19KanteDr.MunzFile: PBVWL709#2_engValid without signature if distributed electronically. Author has confirmation of approval.Circulation Plant 50 VWL Teams, VWKPlant 54 QWO Plant 67 QST1ObjectiveThe purpose of this analytical method is to determine emissions from materials used in vehicle interiors.2ScopeDaimlerChrysler, Mercedes-Benz product line3TermsEmissions, interior trim materials, vehicle interior air,thermodesorption analysis (TDSA), VOC value, Fog value.4ResponsibilitiesPWT/VWL, Organic Analysis Team5DescriptionVehicle interior materials are characterized according to the type and quantity of organic substances that can be stripped from them.Two cumulative values are determined to this end, from which the emission of volatile substances (VOC value) and the condensable content (fog value) can be estimated. Individual emission substances are also identified.During analysis the samples are thermally desorbed and the emissions separated out by gas chromatography and detected by mass spectroscopy.6Applicable documentsDBL 8585, List of MAC and BAT values (DFG)7AppendicesFile names1. Notes on weighed amounts and preparation of samples PBVWL709Anl1.doc2. Production of paint samples PBVWL709Anl2.doc3. Excel report templatePBVWL709Anl3.doc 4. Sketch of thermodesorption analysisPBVWL709Anl4.doc 5. Sample chromatogram for control test mixture PBVWL709Anl5.doc 6. Limiting/target valuesPBVWL709Anl6#2.docAnalysis of the emission of volatile and condensable substances from vehicle interior materials by thermodesorption PB VWL 709Page 2 of 2Contents1General notes, definitions and organization of contract___________________________31.1Materials to be tested, relevant vehicle interior area in relation to emissions_____________31.2Thermodesorption analysis______________________________________________________31.3VOC value (according to PB VWL 709)___________________________________________41.4Fog value_____________________________________________________________________41.5Evaluation of emitted substances_________________________________________________41.6When is VOC/fog analysis required?______________________________________________51.7Timing of sampling/preparation/dispatch__________________________________________61.8Presenting the results of the analysis______________________________________________6 2Analysis parameters________________________________________________________72.1Instrument system_____________________________________________________________72.2Device parameters for the VOC analysis run________________________________________82.3Device parameters for the fog analysis run_________________________________________9 3Method of analysis________________________________________________________103.1Cleaning the glass desorption tubes______________________________________________103.2Testing the system_____________________________________________________________103.3Calibration___________________________________________________________________123.4Sequence of sample analyses____________________________________________________16 4Validation characteristics___________________________________________________214.1Scattering of measured values for samples_________________________________________214.2Limit of determination/linearity_________________________________________________214.3Scattering and recovery of toluene_______________________________________________22 5Possibilities for error, known problems________________________________________235.1Sample preparation___________________________________________________________235.2Incorrect substance identification________________________________________________235.3Known Problems with the cold injection system (CIS, Gerstel)________________________245.4Samples with a high water content_______________________________________________24Analysis of the emission of volatile and condensable substances from vehicle interior materials by thermodesorption PB VWL 709Page 3 of 31 General notes, definitions and organization of contract1.1 Materials to be tested, relevant vehicle interior area in relation to emissions All materials that can contribute to emissions in the vehicle interior must be tested. Examples include emissions from textiles, carpets, adhesives, sealants, foams, plastic components, films, leather, interior paints and composite materials.The relevant vehicle interior area in relation to emissions comprises all areas that are linked to the passenger compartment either directly or by air contact. It also includes the luggage compartment, air-conditioning and heating systems, spaces behind trim, etc.If there is no difference in the composition of different samples of a material or if the difference in formulation is not expected to influence emissions, it is sufficient to examine representative samples of this component family.Responsibility for the accuracy of the assumption that emissions are identical lies with the supplier. In case of doubt he should contact his upstream supplier.For the first sample at least, a laboratory authorized by DaimlerChrysler must perform the VOC/fog analysis. The supplier must send the results to DaimlerChrysler (see section 3.4.5 ).1.2 Thermodesorption analysisIn thermodesorption analysis (TDSA) small quantities of material are heated in a glass tube under defined conditions, the volatile substances emitted during the process are transferred to a gas chromatograph in an inert gas stream, where they are first cryofocused at –150°C in the cryogenic trap (liner) of a temperature-programmable evaporator 1.At the end of the curing phase the liner is quickly heated to 280°C. The focused substances evaporate, are separated out in the gas chromatographic analytical column and then detected by mass spectroscopy.F Appendix 4 provides a schematic view of the thermodesorption analysis equipment.A semi-quantitative determination of the emissions, expressed as mass ppm 2, can be obtained by calibration with reference substances.Toluene and n-hexadecane are used as reference substances for VOC analysis and the fog value respectively. Unknown substance peaks can be identified from the mass spectra and the retention time.1 Here: = Cold injection system (CIS) = Temperature-programmable injector for gas chromatograph2ppm = parts per million = µg of substance per g of weighed portion that are stripped + detected under these conditions. It is not a measure of content.Analysis of the emission of volatile and condensable substances from vehicle interior materials by thermodesorption PB VWL 709Page 4 of 41.3 VOC value 3 (according to PB VWL 709)The VOC value is the sum of volatile to moderately volatile substances.It is calculated as toluene equivalent.In the method described here, substances in the boiling or elution range from pentane (C5) to eicosane (C20) or thereabouts are identified and evaluated.It is assumed that these substances can be detected from an analysis of the vehicle interior air.Determination is performed by curing the sample for 30 minutes at 90°C. The VOC value is measured as a double value.The higher of the two values is cited as the result.1.4 Fog valueFollowing VOC analysis the fog value is determined by leaving the second sample in the desorption tube and curing it for a further 60 minutes at 120°C.The fog value is the total of highly volatile substances that elute from n-hexadecane from the retention time onward. It is calculated as hexadecane equivalent.Substances with boiling points up to at least n-alkane C32 are detected.These substances can readily condense at room temperature and make a substantial contribution to the fogging coating on the windshield.The limits for the VOC and fog range have been established by convention. They have been derived empirically from numerous analyses of vehicle fogging condensates. According to these analyses, fogging consists primarily of substances that boil above around 280°C (boiling point of n-hexadecane = 286°C).1.5 Evaluation of emitted substancesReference is made to the latest list of MAC values4 and to DBL 8585 in order to evaluate the toxicity of the substances identified. Substances listed in the following categories should be rated as critical:Category ClassificationCarcinogenic K1, K2, K3 A, K3 BPregnancy A, BMutagenic1, 2, 3 A, 3 BAllergic effect H,S3VOC value = volatile organic compoundsThis VOC value refers exclusively to the method described here and is not comparablewith VOC values obtained using other methods.4List of MAC and BAT values, Issued by: Deutsche Forschungsgemeinschaft, Wiley-VCH-VerlagAnalysis of the emission of volatile and condensable substances from vehicle interior materials by thermodesorption PB VWL 709Page 5 of 5If substances of this type are detected, they must be explicitly identified in the analysis report.Substances that are assumed or known to be potentially harmful due to their physiological properties (e.g. odor, irritation to mucous membranes) must also be rated as critical.The same applies to substances that can be regarded as precursors of other critical compounds or that are known allergens, e.g. carcinogenic nitrosamines can form from aliphatic secondary amines.Limiting values for VOC, fog and individual substances are set out in Appendix 6.1.6 When is VOC/fog analysis required?1.6.1 Sample approval/developmentThe relevant supply specifications state whether material testing is necessary along with any requirements that exist.Generally speaking, the results of the thermodesorption analysis must be submitted together with the first sample test report for first and new sample approvals.For coordination purposes the supplier must submit a VOC/fog result from the Institut Fresenius5 for the first sample test report.For the sample approval of materials comprising various components, analyses already arranged by upstream suppliers can be submitted.In the context of the preliminary development of materials, a decision can be made by agreement with the team responsible for the material regarding the stage of development beyond which an analysis is reasonable.1.6.2 Standard monitoringIn the context of standard monitoring of approved products, a simple determination of the overall VOC and fog value, in other words no analysis of individual peaks, is all that is required. This must be arranged by the supplier at appropriate test intervals and documented. A visual comparison with the approved chromatogram is sufficient to check for any substantial changes, e.g. additional new substances.5 Address: Institut Fresenius, Chemische und Biologische Laboratorien GmbHDr. KrügerHauert 944227 DortmundGermanyTel. +49 (0)231/758960Analysis of the emission of volatile and condensable substances from vehicle interior materials by thermodesorption PB VWL 709Page 6 of 61.6.3 Formulation changesNew sample approval is required under all circumstances in the event of changes to the formulation that could worsen emissions.1.6.4 ComplaintsIn the event of complaints about materials relating to the question of emissions, thermodesorption analysis may help to identify the cause.Details of a complaint analysis should be agreed with the DaimlerChrysler team in charge.1.7 Timing of sampling/preparation/dispatchThe time at which a sample is taken for analysis must be chosen such that the age of the material corresponds to the shortest possible delivery time for the component to the DC final assembly plant.Example:A foamed material is generally delivered to the car plant within 2 to 12 days after foaming. Analysis must therefore be performed on a foam sample that has been allowed to evaporate for a maximum of 2 days.The worst-case scenario must always be assumed.A representative sample of size DIN A5 or thereabouts is taken for analysis. It must not become contaminated. Each sample is completely wrapped in an airtight package comprising two layers of thick aluminum foil (30 µm), the edges of which are folded several times. The sample is also sealed in a polythene bag and can then be sent to the laboratory. It is then stored at a maximum of –18°C until it is analyzed.Further details of the handling of the material for analysis and the preparation of the sample are provided in Appendices 1 + 2.Appendix 1: Determining the weighed amount of different material samples.Appendix 2: Specifications for the production of paint films.1.8 Presenting the results of the analysisThe contracted laboratory prepares a written analysis report containing the VOC and fog value together with a list of the substances detected. The substances are quantified and compared with the current MAC list.The component supplier sends DaimlerChrysler the written laboratory report, comprising the GC report, chromatograms for the VOC and fog analysis, and all raw data from the analysis (on CD-ROM), for inspection.Analysis of the emission of volatile and condensable substances from vehicle interior materials by thermodesorption PB VWL 709Page 7 of 72 Analysis parameters2.1 Instrument systemThe analytical method described in this report was performed with the following instrument system:Instrument Model/manufacturerThermodesorption system TDSA (with auto sampler), Gerstel,glass desorption tube, external diameter= 6 mm, internal diameter = 4 mm Gas chromatograph (GC)HP6890 with electronic pressure regulation,Agilent (Hewlett Packard)Cryogenic trap Cold injection system KAS 3, Gerstel,glass liner: smooth type, filled withdeactivated quartz wadding (cat. no. 842010) Mass spectrometry detector (MSD)HP5972A, Agilent (Hewlett Packard)Evaluation software Chemstation G1701BAMS Excel 97,Wiley275/Nist MS spectra libraryNotes:AttentionTransferability of results cannot be assumed if different thermodesorption/GC systems are used. It must be checked in each case.In some circumstances the quantity emitted is substantially dependent on the constructional features of the individual analytical instrument system. For example, the geometry of the sample chamber, the length of the heated zone, the length of the transfer line, the type of pneumatic regulation or different flow conditions, may influence the result.Analysis of the emission of volatile and condensable substances from vehicle interior materials by thermodesorption PB VWL 709Page 8 of 82.2 Device parameters for the VOC analysis run2.2.1 Thermodesorption unit (TDSA) parameters for the VOC analysis runSample mode Sample removalFlow mode Splitless6Initial temp.20°CDelay time 1 minute1st rate60 K/min.1st final temp.90°C1st final time30 minutesTransfer line to CIS280°CGC run time67 minutes2.2.2 Cryogenic trap (cold injection system, KAS 3) parameters for the VOC analysisrunFlow mode Split 1:30Initial temp. -150 °C1st rate 12 K/ sec1st final temp. 280°C1st final time 5 minutesEquilibration time 1 minute2.2.3 Gas chromatograph (GC) device parameters for the VOC analysis runTransfer line to MSD280°CCarrier gas Helium 5.0, post-purifiedFlow rate 1.3 ml/min.Pneumatics (EPS)Constant flow modeAnalytical column50 m x 0.32 mm, 0.52 µm5% phenylmethyl siloxanesHP Ultra 2 (19091B-115)Oven temperature program: 40°C, 2 min. isothermal,3 K/min. to 92°C5 K/min. to 160°C10 K/min. to 280°C,(Total run time: approx. 59 minutes)10 min. isothermal2.2.4 Mass spectrometer settings (MSD) for the VOC analysis runStart of data recording After 3.0 minutesCalibration of mass axis Standard spectra autotune(measured at oven temp. of 100°C) Scan mode (low/high mass)29-280 amu, at 3.1 scans/sMS threshold100Note: The chromatographic integration conditions must be selected so that 1 ppm peaks can be detected reliably.6 For technical reasons a forced split flow of approx. 3 ml/min nevertheless occurs here.Analysis of the emission of volatile and condensable substances from vehicle interior materials by thermodesorption PB VWL 709Page 9 of 92.3 Device parameters for the fog analysis run2.3.1 Thermodesorption unit (TDSA) parameters for the fog analysis runSample mode Sample removalFlow mode SplitlessInitial temp.20°CDelay time 1 minute1st rate60 K/min.1st final temp.120°C1st final time60 minutesTransfer line280°CGC run time57 minutes2.3.2 Cryogenic trap (cold injection system KAS 3) parameters for the fog analysis runFlow mode Split 1:30Initial temp. -150 °C1st rate 12 K/ sec1st final temp. 280°C1st final time 5 minutesEquilibration time 1 minute2.3.3 Gas chromatograph (GC) device parameters for the fog analysis runTransfer line to MSD280°CCarrier gas Helium 5.0, post-purifiedFlow rate 1.3 ml/min.Pneumatics (EPS)Constant flow modeAnalytical column50 m x 0.32 mm, 0.52 µm5% phenylmethyl siloxanesHP Ultra 2 (19091B-115)Oven temperature program: 50°C, 2 min. isothermal,25 K/min. to 160°C10 K/min. to 280°C,(Total run time approx. 48 minutes)30 minutes isothermal2.3.4 Mass spectrometer settings for the fog analysis runStart of data recording After 12.5 minutesCalibration of mass axis Standard spectra autotune(at oven temp. of 100°C)Scan mode (low/high mass)29-370 amu, at 2.3 scans/sMS threshold100The chromatographic integration conditions must be selected so that 1 ppm peaks can be detected reliably.Analysis of the emission of volatile and condensable substances from vehicle interior materials by thermodesorption PB VWL 709Page 10 of 103 M ethod of analysis3.1 Cleaning the glass desorption tubesOnly glass tubes that are completely free from contamination may be used. Even brand-new desorption tubes must be thoroughly cleaned before being used for the first time. The tubes must be cleaned by storing them for several hours, ideally overnight, in an alkaline cleaning solution7.They must then be rinsed thoroughly, first under hot running water for at least one minute, then with demineralized water.The tubes are then dried in a drying oven (approx. 45 minutes at 105°C) and stored free from contamination (wrapped in aluminum foil in an airtight package) until use.3.2 Testing the systemThe function of the instrument system is tested by analyzing a standard control solution within the sample series (see 3.2.1).The standard control solution contains non-polar, polar basic and acid components that would display a noticeable peak tailing even with low adsorption effects.This process can also be used to check for substance losses due to leaks.Peaks occurring in close succession, such as o-xylene and n-nonane, can be used to check the separation efficiency of the chromatographic column. These two substance peaks must be virtually baseline-separated under the chosen chromatographic conditions.The performance of the mass spectroscopy detector is checked by means of mass and sensitivity tuning (standard spectra autotune in the case of HP instruments), and the specifications required by the manufacturer must be achieved. An air/water check must also be performed to test the integrity of the entire system.All substances in the control mixture must be clearly identified in the mass spectra library (e.g. Wiley 275) during the search run.The TDSA/GC system must also be checked for possible memory effects by performing a dummy run with an empty desorption tube at least before every sample series.If negative effects such as severe peak tailing, disruptive dummy run peaks or significant loss of substance occur, the system must be cleaned. The GC column, CIS liner, transfer line or seals may need to be replaced.We recommend documenting the results of the control run for each sample series as part of quality control procedures (control card). The peak area ratios, concentrations as toluene equivalents and retention times can be used as control quantities.3.2.1 Preparing the control solution7 The alkaline laboratory glass cleaner SODOSIL RA8 (Riedel-deHa?n) has proven effective.Analysis of the emission of volatile and condensable substances from vehicle interior materials by thermodesorption PB VWL 709Page 11 of 11The following substances dissolved in methanol have proven to be suitable for use as the system control (listed in elution sequence under VOC conditions):Table 1 Control mixturebenzene2-ethylhexanol-1n-heptane n-undecanetoluene2,6 dimethylphenoln-octane n-dodecanen-butyl acetate n-tridecanep-xylene n-tetradecaneo-xylene dicyclohexylaminen-nonane n-pentadecanen-decane n-hexadecane220 ± 20 mg of each component are weighed into a glass vessel (e.g. 5 ml roll-edged glass) to an accuracy of 0.1 mg. Approx. 100 mg of this mixture are transferred to a 50 ml measuring flask and weighed (weighing accuracy ± 0.1 mg). Methanol (p.a.) is then added to just below the calibration mark on the measuring flask, the flask is closed and carefully shaken until all solvent droplets have fully dissolved in the methanol. The measuring flask is then filled up to the calibration mark and shaken again.4 µl of this solution are then injected into a Tenax desorption tube for the control run (as described in section 3.3.2).This means that the desorption tube contains approx. 0.45 ± 0.05 µg of each substance. The retention times for the n-alkanes present in this mixture are a suitable reference point for determining the retention index of unknown substance peaks and can therefore be used as an additional check for MS identification during the sample runs.3.2.2 Stability of the control solutionApart from the n-butyl acetate component, the control solution can be kept for several weeks if stored correctly (refrigerated at 8°C maximum). Butyl acetate hydrolyzes noticeably within a few days, however. An additional butanol and acetic acid peak occurs in the chromatogram and the butyl acetate peak becomes correspondingly smaller. In this case the control solution must be repeated with a fresh batch in order to evaluate the butyl acetate peak.Analysis of the emission of volatile and condensable substances from vehicle interior materials by thermodesorption PB VWL 709Page 12 of 123.3 CalibrationCalibration is performed using the external standards method.This method involves charging separate desorption tubes containing Tenax TA with the individual calibration solutions.3.3.1 Calibration solutionsTwo calibration solutions are required:1. For the VOC analysis approx. 0.5 µg/µl toluene (p.a.) in methanol (p.a.)2. For the fog analysis approx. 0.5 µg/µl n-hexadecane (p.a.) in methanol (p.a.)Approx. 25 mg (accuracy to ± 0.1 mg) of toluene or n-hexadecane are weighed into a 50 ml measuring flask, the measuring flask is filled with methanol to just below the calibration mark, closed and shaken well. The flask is then topped up with methanol to the calibration mark and shaken again.The calibration solutions can be stored in a cool place for up to 3 months. Guaranteeing the accuracy of the concentration is part of the laboratory’s quality control procedure.Analysis of the emission of volatile and condensable substances from vehicle interior materials bythermodesorption PB VWL 709Page 13 of 133.3.2 Charging the calibration or control solution onto TenaxA desorption tube filled with Tenax TA is connected to an injection device guaranteeing a controlled flow of inert gas (helium 5.0) through the tube while the calibration solution is being added.Models consisting of septum screw fittings from worn-out GC injectors or a cold injection head fitted with an adaptor and no septum (Gerstel) have proven effective. The advantage of the latter design is that the dead volumes are relatively low, so fewer losses can occur.A simple adjustable flowmeter should be connected upstream of the injection device to control the helium flow.A gas meter for controlling the overall volume passing through the injection device and for checking the integrity of the system must be connected downstream of the injection device.The flow rate should be set to approx. 0.7 ± 0.3 l/min, and the total flow quantity should be around 2.5 – 3 liters. The methanol matrix fed into the system is largely removed, whereas toluene or hexadecane remain on the Tenax.Fig. 1 Equipment for charging the calibration solutionAnalysis of the emission of volatile and condensable substances from vehicle interior materials bythermodesorptionPB VWL 709Page 14 of 143.3.2.1 Tenax desorption tube:The Tenax packing must be inserted into the tube in such a way that it can be completely covered by the heating zone of the desorption oven.For the tubes in the Gerstel TDSA instrument the Tenax packing should be around 5-6cm in length.A gap of approx. 3 cm must be left between the Tenax packing and the end of the tube on the transfer line side to prevent the transfer line from protruding into the packing. A plug of deactivated (silanized) glass wadding measuring approx. 1 cm in length, into which the calibration solution is injected, is placed on top of the Tenax layer.Fig. 2 Tenax packing in the desorption tubeAfter bringing the calibration solution up to room temperature, 4 µl are drawn up with a 10µl GC syringe, ensuring that the solution is free from bubbles, and slowly (over approx.15 seconds) injected into the plug of glass wadding. The inert gas flow is switched on during this process.Notes:1. To avoid losses it is advisable to inject the calibration solution directly into the glass waddingplug. Otherwise sizeable fluctuations in the measured values are likely .2. Tenax can alter over time depending on usage. The quality of the Tenax tubes must bechecked by suitable means (e.g. visual check + dummy run). If necessary the packing should be replaced.GC carrier gas flowAnalysis of the emission of volatile and condensable substances from vehicle interior materials by thermodesorption PB VWL 709Page 15 of 153.3.3 Analysis parameters for the calibration and control solution3.3.3.1 Thermodesorption unit (TDSA) parameters for the calibration runSample mode Sample removalFlow mode SplitlessInitial temp.20°CDelay time 1 minute1st rate60 K/min1st final temp.280°C1st final time 5 minutesTransfer line to CIS280°C3.3.3.2 Cryogenic trap (cold injection system, KAS 3) parameters for thecalibration runFlow mode Split 1:30Initial temp. -150 °C1st rate 12 K/sec1st final temp. 280°C1st final time 5 minutesEquilibration time 1 minute3.3.3.3 Gas chromatograph parameters for the calibration and control runThe same parameters are used for toluene calibration and analysis of the control mixture as for the VOC sample run. Only data recording begins later, after approx. 5.5 minutes, in order to mask the methanol peak.Hexadecane calibration is performed under the same GC conditions as the fog analysis run.The GC runs can be shortened relative to the sample runs by interrupting the oven temperature program following elution of the calibration substances.。
STANDARD TEST METHODS CHEMICAL COATED FABRICS AND FILMCompiled and Issued By:2000_______________FOR BETTER PRODUCTS . . .America’s leading manufacturers and consumers - use products from Chemical Fabrics and Film members for a myriad of uses.AIRCRAFT Seat backs, upholstery, wall panels and compartments.ATHLETIC & Bowling bags, exercise mats, golf bags, gym and workout bags, SPORTING GOODS tennis bags.AUTOMOTIVE & Camper topping, convertible topping, door and console TRANSPORTATION coverings, instrument panel coverings, landau tops, securityshades, upholstery.EXTERIOR FILMS & Awnings and canopies, backlit awnings and signage, banners, LAMINATES outdoor decking, outdoor furniture, pond and pit liners, roofing,swimming pool l iners, tents and tarpaulins.& Belts, jackets, protective clothing, rainwear, shoe uppers, sock FOOTWEARGARMENTS linings.GRAPHIC ARTS & Bookbinding coverstock, checkbooks, coin purses, etc., hand CASE COVERINGS bags and accessories, luggage and briefcases.HOME & CONTRACT Ceiling tile facings, commercial seating, commercialFURNISHINGS wallcoverings, folding doors, laminating films for wood, metaland wallboard, matting, residential upholstery, residentialwallcovering, window shades and blinds.Convertible topping, decking, upholstery and bolsters.MARINEMISCELLANEOUS Children safety seats, industrial tapes, juvenile furniture, mattresscovers, strip doors, tank lining, toys.______________FOREWORDThis, the Eighth Edition of the Standard Test Methods (STM) Pamphlet, has been prepared by the Technical Committee of the Chemical Fabrics & Film Association. These test methods are used by the industry and its customers to determine the physical properties of chemical coated fabrics and films, to facilitate quality control and to assure customer satisfaction.Section I covers test procedures for the coated fabrics; Section II covers test procedures for films. These tests include adhesion of coating, weight, resistance to cold and flame, blocking, aging, abrasion resistance, hydrolytic stability, volatility, tensile, and tearing strength and many more. The purpose of each test is explained in non-technical terms and the tests are referenced to comparable standard test methods of the American Society for Testing and Materials, Federal Test Methods and Specifications, Textile Test Methods, and the American Association of Textile Chemists and Colorists.Section III includes terminology and customs in the Industry. Also in this section are suggestions on how to remove common stains. Additional information in Section III includes a statement on fitness for use, the chronological history of fabric coating and information about the Chemical Fabrics & Film Association.Every effort has been made to assure the accuracy of the information in this Pamphlet and the avoidance of excessive risks in the tests. However, the Association and those responsible for the preparation of Association publications make no representation or warranty, or assume or accept any responsibility or liability, with respect thereto.In test methods where a specific material, apparatus, and/or supplier is listed, please note that such a listing is for the convenience of users of the Standard Test Methods. Any equipment from any supplier which produces comparable results under the testing procedure is acceptable.TABLE OF CONTENTSSubject Page Section I---Tests for Chemical Coated FabricsStandard Conditions of Test (6)CFFA-1 Abrasion Resistance (6)MethodWyzenbeeka.AbraserTaberb.CFFA-2 Accelerated Light Aging (7)Fadeometera.Weatherometerb.c. QUV Accelerated WeatheringCFFA-3 Adhesion of Coating to Fabric (10)Resistance (11)CFFA-300 BacterialCFFA-4 Blocking (11)CFFA-5 Button Pull-Through Resistance.................................................................Deleted CFFA-6 Cold Crack Resistance.. (12)Methoda.RollerMandrelMethodb.Resistance (13)CFFA-7 CrockingDrya.Wetb.CFFA-700 Dimensions of Coated Fabric (13)Widtha.Lengthb.Thicknessc.Massd.Cleanability (14)CFFA-8 DryCFFA-9 Flame and Smoke Resistance (15)Resistance (15)CFFA-10 FlexCFFA-11 HydrolyticStability (15)CFFA-12 Lacquer or Varnish Lifting (16)Resistance (17)CFFA-120 MildewCFFA-13 OilResistance (17)CFFA-130 Scrubbability (18)Strength (19)CFFA-14 SeamCFFA-140 Shrinkage (19)Resistance (19)CFFA-141 StainCFFA-15 Stretch and Set (21)Strength (22)CFFA-16 TearingMethodElmendorfa.Methodb.TongueMethodc.TrapezoidCFFA-17 Tensile Strength and Elongation - Grab Method (24)CFFA-18 Volatility (25)CFFA-180 Washability (26)CFFA-19 Water Vapor Transmission (26)CFFA-20 Weight of Coating and Fabric (28)Section II -- Tests for Chemical FilmsResistance (29)CFFA-200 Abrasiona. Wyzenbeek MethodAbraserTaberb.CFFA-201 Blocking (29) (29)CFFA-21 DensityCFFA-22 Dimensional Changes at Elevated Temperatures (30)CFFA-220 Dimensions of Film (31)a.WidthLengthb.c.ThicknessMassd.CFFA-23 Low Temperature Impact Resistance (31)CFFA-24 Permeability to Air.....................................................................................Deleted CFFA-25 Soapy Water Extraction (31)Strength (32)CFFA-26 TearingMethoda.GravesMethodb.ElmendorfCFFA-27 Tensile Strength and Elongation (33)CFFA-270 Volatility (34)CFFA-28 Snap Back Testing for Pool Liner Films (34)Section IIITerminology and Customs in the Industry (35)Cleaning and Care Instructions (36)Fitness for Use (37)Information About the Products and the Chemical Fabrics & Film Association (38)NOTE:Test methods are listed alphabetically. Single and double digit numbers used to reference the test methods contained herein have not been changed from the previous editions. Three-digit numbers indicate test methods added to the Seventh Edition._______________SECTION ITests for Chemical Coated FabricsSTANDARD CONDITIONS OF TESTReference: ASTM D751-98 - Test Methods for Coated FabricsPhysical tests may be made under prevailing atmospheric conditions except in the settlement of disputes. Unless otherwise specified, tests shall then be made upon material in standard conditions, i.e., the condition reached when the material is in moisture equilibrium with an atmosphere having a relative humidity of 65% and temperature of 70°F (21°C). A tolerance of + 2% is permitted in relative humidity and + 2°F (1°C) in temperature. Material shall be considered to be in equilibrium when it shows no progressive change in weight after free exposure to moving air.Because of the labor involved in determining whether equilibrium has been reached, it is customary to condition the material for a minimum period of 15 hours at the temperature and relative humidity previously mentioned.NOTE: These conditions are standard and will be used unless the test method requires special environmental conditioning._______________CFFA - 1 ABRASION RESISTANCEa. WyzenbeekMethodPurpose: To determine the abrasion resistance of chemical coated fabrics under service conditions Reference:ASTM D4157-92 - Abrasion Resistance of Textile Fabrics (Oscillatory Cylinder Method) Apparatus: Oscillatory Cylinder Type*To determine abrasion resistance of chemical coated fabrics, one specimen of each sample approximately 2 x 8 inches (5 x 20 cm) in size shall be cut with the long dimension parallel to the machine direction and tested for resistance to abrasion, using the Wyzenbeek abrasion wear tester, operating under the following conditions: Pressure on Specimen 2 lbs.Tension on Specimen (with scalebar in horizontal position) 6 lbs.Abradant #8 Cotton Duck, #220 Grit Silicon Carbide Sheet,Stainless Steel Screen (Surface Screen 50 x 70 Mesh,Support Screen 14-18 Mesh) or Abradants as specified Speed, Double Rubs/Hour 5000Temperature of Room 70° - 90°F (21° - 32°C)On stretchable fabrics such as knit, masking tape shall be used to reinforce backing to prevent elongation.*Available from J.K. Technologies, Inc., 2524 S. 8000 West Road, Kankakee, IL 60901b. Taber Abraser MethodPurpose: To determine the abrasion resistance of chemical coated fabrics and filmsusing a rotary platform double head testerReference: ASTM D3389-94 - Method for Testing Coated Fabrics AbrasionResistance Rotary Platform, Double Head AbraderApparatus: Rotary Platform Double Head Abraser*To determine the abrasion resistance of a chemical coated fabric or film, one specimen of each sample shall be cut in a 4-1/8" circle and mounted on a S-16 Specimen Plate*. This specimen plate shall then be mounted on the Taber platform. Abrasion resistance is tested by the Taber platform turning on a vertical axis, against the sliding rotation of two rubber-base abrading wheels. Various hardness abrasive wheels, test weights, and test cycles can be used in the Taber test. These are specified depending on the type of material beingtested and the expected service requirements of the finished coated fabrics or film.After exposing the specimen to the required number of test cycles using the specified abrasive wheel and weight, the sample should be examined for signs of visual wear or loss of embossing detail.*Available from Taber Industries, 455 Bryant Street, North Tonawanda, NY 14120._______________CFFA - 2 ACCELERATED LIGHT AGINGPlastic materials that are used for exterior applications are subject to attack typically by ultraviolet light, oxygen, and water. No single light exposure apparatus can exactly simulate natural exposure, as climatic conditions will vary with respect to geography and topography.Listed are the commonly used methods within the coated fabrics and film industries. They have been found to be useful tools in predicting the behavior of plastics under outdoor exposure conditions, only after a history of their use has been established.After exposure, the specimens are examined for any signs of stiffness, tack, crazing, color change, or any other deviation. Acceptable degree of change in color can be an agreed upon visual variation or measured by an agreed upon spectrophotometer, values expressed in Delta E units, in CIELAB, or CMC systems.a. FadeometersArc1. XenonReference:ASTM G26-96 Method C - Operating Light Exposure Apparatus (Xenon-Arc Type) With and Without Water for Exposure of Non-Metallic MaterialsApparatus:Xenon Weathering Unit*Xenon-ArcWatercooledBorosilicate inner and outer optical filters (or for automotive, Quartz inner and Type SBorosilicate outer filter as per SAE J-1885).Using the apparatus, two specimens from each sample are exposed under the following conditions:Wattage settings are dependent upon the age of the burner tubes. Adjust the wattage to the Xenon lamp so that it provides 20 AATCC Fading Units in 15-20 clock hours. Black panel shall be adjusted to + 37°F (63° + 3°C). Relative humidity set to 86º + 41ºF (30º + 5ºC).145°Arc2. CarbonReference:ASTM G23- 96 Method 3 - Operating Light Exposure Apparatus (Carbon-ArcType) With and Without Water for Exposure of Non-Metallic Materials Apparatus:Carbon Arc Fadeometer*Using the apparatus, two specimens from each sample are exposed under the following conditions: Set current to 15-17 amps with 120-145 volts across the arc. Black panel shall be adjusted to + 37°F (63° + 3°C).145°b. WeatherometerArc1. XenonReference:ASTM G26-96 Method A - Operating Light Exposure Apparatus (Xenon-Arc Type) With and Without Water for Exposure of Non-Metallic Materials.Apparatus:Xenon Weathering Unit*Xenon-ArccooledWaterBorosilicate inner and outer optical filtersUsing the apparatus, two specimens from each sample are exposed under the following conditions: Wattage settings are dependent upon the age of the burner tubes. Water shall be delivered in a finespray. Water temperature shall be 77º + 41ºF (25° + 5°C), contain less than 1 ppm solids, and have a pH of 6.0 - 8.0. It must leave no deposits or stain on the specimen after continuedexposure.The test cycle shall consist of 102 minutes of light followed by 18 minutes of light plus water spray. Black panel shall be adjusted to 145° + 37°F (63° + 3°C) attained during the light onlyportion of the cycle.2. CarbonArcReference:ASTM G23-96 - Method 1 - Operating Light Exposure Apparatus (Carbon-ArcType) With and Without Water for Exposure of Non-Metallic Materials.Apparatus:Carbon Arc Weatherometer*Using the apparatus, two specimens from each sample are exposed under the following conditions: Set current to approximately 16 amps and 140 volts across the arc. Water shall be delivered to a fine spray through a series of four vertical nozzles delivered on a 3 inch (8 cm) width section of thespecimen at an approximate rate of 0.20 pint (100 cc) per minute. Water pressure to be maintained at 12-18 psi. Water temperature shall be near ambient temperature 77º + 41ºF (25º + 5ºC), and containless than 1 ppm solids and have a pH of 6.0 - 8.0. It must leave no deposits or stain on the specimenafter continued exposure. The test cycle shall consist of 102 minutes of light followed by 18 minutes of light plus water spray. Black panel shall be adjusted to 145° + 37°F (63° + 3°C) attained during thelight only portion of the cycle.c. QUV Accelerated Weathering1. Fluorescent UV With Irradiance MonitorReference:ASTM D4329-99 - Standard Practice for Fluorescent UV Exposure of Plastics.Apparatus:Fluorescent UV/Condensation Device equipped with irradiance monitoring and control (preferred).Employs the use of an irradiance controlled UV/Condensation Device in order to set the tester’s irradiance to a level equal to 1.75 x greater than older style UV/Condensation Devices, thus accelerating results. Irradiance controlled devices also reduce variability caused by fluctuating light intensities by fixing the irradiance level.Exposure Cycle: 8 hours of UV at 140ºF (60 + 3°C).4 hours of condensing humidity at 122ºF (50 + 3°C).Lamp Type: UVA-340 with a peak emission of 340 nm.Irradiance Setpoint: 1.35 W/m2 as measured at 340 nm.Lamp Rotation: None required.2. Fluorescent UV Without Irradiance MonitorReference:ASTM D4329-99 - Standard Practice for Fluorescent UV Exposure of PlasticsApparatus:Fluorescent UV/Condensation Device without irradiance monitoring and control.Employs a Fluorescent UV-Condensation Apparatus without irradiance monitoring and control. At any given time, the light intensity will fall within certain range of irradiance, depending on the lamp ages, the laboratory temperature, and the UV exposure temperature.Exposure Cycle: 8 hours of UV at 60 (+ 3)°C.4 hours of condensing humidity at 50 (+ 3)°C.Lamp Type: UVA-340 with a peak emission of 340 nm.Irradiance Level: Not controlled. 0.77 W/m2 + 10%.Irradiance can be measured by using the method outlined inAppendix B of SAE J2020.Lamp Rotation: Every 400 hours.NOTE: An earlier light source, the 313 bulb, used in the QUV is not recommended, as it generates UV radiation that does not normally exist in natural sunlight and, therefore, is not properly indicative of conditions relative to outdoor exposure.*Available from Atlas Electric Devices Co., 4114 North Ravenswood Avenue, Chicago, IL 60613._______________CFFA - 3 ADHESION OF COATING TO FABRICPurpose: To determine the force or pull necessary to separate chemical coating from its fabric backing. Reference: ASTM D751-98 - Test Methods for Coated FabricsApparatus:Testing machine consisting of straining mechanism, holding clamps, and load recordingmechanism.Specimens 2 inches (5 cm) in width and 8 inches (20 cm) in length shall be cut from the coated fabric. Two sets of two specimens each will be required, one set for adhesion in the machine direction having the longer dimension parallel to the machine direction of the fabric, and the other set for adhesion in the cross machine direction having the longer dimension parallel to the cross machine direction of the fabric. The specimens shall be prepared for test as follows:a. When the strength of the coating film exceeds the adhesive bond to the fabric, as with thick films, thespecimen shall be prepared for test by carefully cutting the coating through to the fabric on two parallel cuts A and B, 1 inch (2.5 cm) apart running lengthwise of the specimen with one cut 1 inch (2.5 cm)longer than the other as shown in the drawing.The ends of cuts A and B shall be joined together with a diagonal cut C which shall also be carefully cut through the coating to the fabric. The edge of a knife shall be worked under the strip separatedfrom the backing for a distance of 2 inches (5 cm) from that point.b. With thin films or in cases where the coating is not sufficiently strong to be stripped from the fabric asdescribed in Paragraph (a), two specimens of the coated fabric shall be cemented together face to face with an adhesive suitable for adhering the type of coating being evaluated. Care should be taken not to alter the coating/fabric adhesion. The cuts shown in the above drawing shall then be made from one side being careful to penetrate only through one layer of fabric and not to injure the other fabric layer.The fabric from one side shall then be stripped down for a distance of 2 inches (5 cm). This will allow the backing fabric to be inserted in one jaw of the machine. The force required to separate the coating and the backing fabric can then be measured.NOTE:In case the fabric is too weak to be tested in a 1 inch (2.5 cm) width, the specimen may be cut 3 inches (7.5 cm) in width and the strip for evaluation cut 2 inches (5 cm) in width. The results shall then be recorded as pounds pull per 2 inch (5 cm) strip.Clamp the separated portion of the 1 inch (2.5 cm) strip in the moveable jaw of the testing machine and end D of the specimen in the fixed jaw so that the movement of the moveable jaw will separate the coating from the backing. The rate of travel of the moveable jaw shall be either 2 inches (5 cm) per min. or 12 inches (30 cm) per min., as specified. The distance of the separation of the coating or plies shall be a minimum of 3 inches (7.5 cm).The report shall include the following:1. Type of testing machine and the rate of travel of the moveable jaw, and2. The average test value for at least two specimens cut in the longitudinal direction and two specimenscut in the transverse direction. The averages of the five high peaks shall be used to determine the pull in pounds for reporting the adhesion of the coating or plies.______________CFFA - 300 BACTERIAL RESISTANCEPurpose: To determine the degree of bacteriostatic activity of chemical coated fabrics and films. Reference: AATCC* Test Method 147-1998Principle: Specimens of the test material are placed in contact with the AATCC Bacteriostastis agar** which has been streaked with:Staphylococcus aureus American Type Culture Collection6538***No.Klebsiella pneumoniae American Type Culture CollectionNo.4352***Salmonella choleraesuis American Type Culture Collection10708***No.Pseudomonas aeruginosa American Type Culture Collection13388***No.After incubation at 99°F (37°C) for 18 to 24 hours, the incubated plates are examined for interruption of growth along the streaks of inoculum beneath the fabric and for a clear zone of inhibition beyond the specimen edge. Reports of results will include an observation of zones of inhibition and growth under the specimen if present. The customer (or supplier) will establish the final criteria for a pass or fail judgment based on observations of the results.*Available from American Association of Textile Chemists and Colorists, P. O. Box 12215, ResearchTriangle Park, NC 27709.**Available from Difco Laboratories, 920 Henry Street, Detroit, MI 48201.***Available from American Type Culture Collection, 10801 University Boulevard, Manassas, VA20110-2209._______________CFFA - 4 BLOCKINGPurpose: To determine the development of surface tack at an elevated temperatureReference: Federal Standard No. 191A - Method 5872Apparatus:Forced Air Laboratory OvenThree specimens 2 x 2 inches (5 x 5 cm) shall be placed face to face between two glass plates 2-1/2 x 2-1/2 inches (6.4 x 6.4 cm), weighted with a one pound (454 gms) weight and exposed to 180° + 2°F (82o + 1°C) for a period of thirty minutes. Specimens shall be removed from the oven, taken from between the glass plates, and allowed to condition (at room temperature) for at least fifteen minutes before making observations. Specimen shall be rated according to the following scale:No. 1---No blocking; No adhesion.No. 2---No blocking; Slight adhesion.No. 3---Slight blocking; coating must be peeled to be separated.No. 4---Blocking; coating cannot be separated intact.Where specified, both sides of double coated material shall be tested._______________CFFA - 6 COLD CRACK RESISTANCEPurpose: To determine the temperature at which cracks may appear if chemical coated fabrics are left in the cold and then folded sharplyApparatus: Low Temperature ApparatusMethoda. RollerReference: Federal Standard No. 191A - Method 5874 - Low Temperature Effect of Coated Cloth Four 2 x 6 inch (5 x 15 cm) specimens are cut, two in the machine direction and two in the cross machine direction, one set each to be tested on both sides.The two narrow ends of each specimen are brought together and stapled to a card so as to form a smooth loop at the unstapled end. The specimens shall be exposed for 2 hours at the specified temperature.A 5 pound (2.2 Kg.) roller shall be used on light materials (up to 15 oz/yd2 or 500 g./m2) and a 10 pound (4.5 Kg.) roller on heavier materials. The roller shall be rolled lengthwise from the stapled end toward the loop with no pressure exerted other than the weight of the roller on the specimen. The specimen shall be evaluated in one of two ways:1. Serious cracking will be visible to the naked eye.2. Fine cracking may be detected by examination under a magnifying glass.NOTE: Cracks caused by obvious defects in the fabric are to be discarded and the test re-run.Methodb. MandrelFour specimens 2 x 8 inches (5 x 20 cm) are cut, two in the machine direction and two in the cross machine direction, one set each to be tested on both sides. A ½ inch (12 mm) mandrel shall be conditioned at the specified temperature for a minimum of 30 minutes before testing. After conditioning and without removal from the test conditions, the specimen shall be bent quickly 180 degrees around the mandrel and the specimen shall meet at not more than 1/4 inch (6 mm) behind the mandrel. The specimen is then evaluated visually for cracks._______________CFFA - 7 CROCKING RESISTANCEPurpose: To determine the resistance to transfer of color from chemical coating to another surface byactionrubbingReference: Federal Standard No. 191A - Method 5651-68 - Colorfastness to CrockingApparatus: Crockmeter*a. DryThe specimen to be tested shall be rubbed with an unstarched, 96 x 100 (80 x 80) Gcotton print cloth with a Crockmeter or similar device. The essential features are that the white cloth be firmly held over the flat end of a cylindrical "finger" 5/8 inch (1.5 cm) in diameter which presses with a weight of 32 ounces/force upon the coated surface to be tested. The finger shall be moved across the specimen twenty times at the approximate rate of 1/2 second per stroke, four inches (10 cm) long. The test is made with dry cloth and test piece.b. WetThe wet crocking test is conducted in the same manner as dry crocking except the crock cloth is saturated with destilled or deionized water and squeezed or wrung to removed excess water to a moisture pickup of 65 + 5% based on the weight of dry crock cloth. The crocking test shall be performed immediately thereafter .Evaluating Scale:Using a sample of the original material compared with the material tested when white crock cloth is required.Excellent: No perceptible staining of the white crock cloth.Good: Slight staining of the white crock cloth.Fair: Appreciable, but not objectionable, staining of the white crock cloth.Poor: Objectionable staining of white crock.*Available from Atlas Electric, 4141 Ravenswood Avenue, Chicago, IL 60613, (773) 327-4520, Fax (773) 327-5787._______________CFFA - 700 DIMENSIONS OF COATED FABRICPurpose: To determine the dimensions of a chemical coated fabricReference: ASTM D751-98 - Test Methods for Coated Fabricsa. WidthMeasure the width of the chemical coated fabric laid out smooth on a horizontal surface without tension in either direction. Report the average of at least five different measurements uniformly distributed along the full length of the roll or piece as the average and minimum width of the roll or piece.b. LengthLay the chemical coated fabric out smooth, without tension, on a horizontal surface and measure the length parallel to the selvage; or, measure successive portions, each at least 4.5 yards (5 m) in length, under the same conditions.c. ThicknessApparatus: The gauge used for the measurement of thickness shall be of the deadweight typeequipped with a dial graduated to read directly to 0.001 in. (0.025 mm). The presserfoot shall be circular with a diameter of 0.375 + 0.001 inches (9.52 + 0.03 mm). Thepresser foot and moving parts connected therewith shall be weighted so as to apply atotal force of 6 + 0.1 oz. (1.7 + 0.1 N) equivalent to a pressure of 23.5 + 0.5 kPa (3.4psi) to the specimen. The presser foot and anvil surfaces shall be plane to within0.0001 inches (0.0025 mm) and parallel to each other within 0.0001 inches (0.0025mm). The gage shall be calibrated for the actual load exerted by the presser foot bymeans of any device so arranged as to measure the total vertical force exerted by thepresser foot at the several gage readings or presser foot levels selected for calibration.The presser foot shall be brought to each calibration level from a higher one.Place the coated fabric upon the anvil of the gage smooth, but without tension. Lower the presser foot upon the material gradually (without impact), allow it to rest upon it 10 seconds, and then observe the reading of the dial. Make similar measurements at no less than five different places uniformly distributed over the surface of the coated fabrics exclusive of the area adjacent to either selvage and within one tenth the width of the fabric or within 100 inches (2.5 m) of either end of a roll of piece. Report the average of the five or more measurements as the average thickness.d. MassMethod Applicable to a Piece, Cut, or Roll - Weigh the full piece, cut, or roll on a calibrated scale accurate to 0.25%, measure the length and width of the coated fabric, and calculate the mass, reporting it in grams per square meter (ounces per square yard) to the nearest 2 g (0.1 oz).Method Applicable to a Sample - Cut a specimen having an area of at least 125 cm2 (20 in.2), or a number of specimens not less than 50 mm (2 in.) square and having a total area of at least 125 cm2 (20 in.2) from the coated fabric, weigh on a calibrated scale accurate to 0.25%, and calculate the mass, reporting it in grams per square meter (ounces per square yard). Unless a specimen the full width of the fabric is used, take no specimen nearer the selvage than one-tenth the width of the fabric.NOTE 3: This test method is intended for use when a small sample of coated fabric is sent to the laboratory for test. The result is considered to be applicable to the sample, but not to the piece or lot of goods from which the sample was taken unless the number of samples and method of sampling are specified and agreed upon by those concerned. If this is done, each sample should be tested in accordance with 8.2 and the results averaged to obtain the average mass in grams per square meter (or ounces per square yard)._______________CFFA - 8 DRY CLEANABILITYPurpose: To determine the resistance of chemical coated fabrics to dry cleaningReference: International Fabricare Institute, 12251 Tech Road, Silver Springs, MD 20904, 301-622-1900。
测定mgf2薄膜的复折射率光谱的英文The Characterization of the Refractive Index Spectrum of MgF2 Thin FilmsThe optical properties of thin-film materials have become increasingly important in various technological applications, ranging from optoelectronic devices to optical coatings. Among the numerous thin-film materials, magnesium fluoride (MgF2) has gained significant attention due to its unique optical characteristics, such as a wide transparent spectral range, low refractive index, and excellent chemical stability. Accurate determination of the refractive index spectrum of MgF2 thin films is crucial for the design and optimization of optical components and systems.In this study, we aim to present a comprehensive characterization of the refractive index spectrum of MgF2 thin films. The refractive index of a material is a fundamental optical property that describes the speed of light propagation within the material. The refractive index can be wavelength-dependent, leading to a refractive index spectrum, which is essential for understanding the optical behavior of thin-film materials.To achieve this goal, we employed a combination of experimental techniques and theoretical analysis. The MgF2 thin films were deposited on glass substrates using a well-established deposition method, such as thermal evaporation or sputtering. The thickness of the films was carefully controlled to ensure the accuracy of the refractive index measurements.The refractive index spectrum of the MgF2 thin films was determined using a spectroscopic ellipsometry technique. Ellipsometry is a non-destructive optical characterization method that measures the change in the polarization state of light upon reflection from the sample surface. By analyzing the ellipsometric data, the refractive index and other optical properties of the thin films can be accurately determined.The measurement process involved placing the MgF2 thin-film sample in the ellipsometer and collecting the ellipsometric data over a wide range of wavelengths, typically from the ultraviolet to the near-infrared region of the electromagnetic spectrum. The collected data were then analyzed using appropriate optical models and numerical algorithms to extract the refractive index spectrum of the MgF2 thin films.To ensure the reliability and accuracy of the refractive index data, several factors were considered during the measurement andanalysis processes. These factors include the surface roughness of the thin films, the potential presence of anisotropy, and the influence of the underlying substrate. Appropriate mathematical models were employed to account for these factors and obtain a accurate refractive index spectrum.The results of the study revealed the detailed refractive index spectrum of the MgF2 thin films over the measured wavelength range. The refractive index was found to exhibit a strong wavelength dependence, with the value decreasing as the wavelength increased. This behavior is consistent with the dispersion characteristics ofMgF2, which is known to have a low refractive index and high transparency in the visible and near-infrared regions.Furthermore, the study also investigated the potential effects of film thickness and deposition conditions on the refractive index spectrum. By varying these parameters, the researchers were able to understand the relationship between the thin-film properties and the resulting optical characteristics. This knowledge can be valuable for tailoring the optical performance of MgF2 thin films for specific applications.The findings of this study contribute to the existing understanding of the optical properties of MgF2 thin films and provide a reliable reference for the refractive index spectrum. This information is crucialfor the design and optimization of various optical components and devices that utilize MgF2 as a key material, such as antireflective coatings, optical filters, and optical waveguides.In conclusion, this comprehensive study on the refractive index spectrum of MgF2 thin films offers valuable insights for researchers and engineers working in the field of optical thin-film technology. The accurate characterization of the refractive index spectrum presented here can facilitate the development of advanced optical systems and devices that harness the unique optical properties of MgF2.。
利多卡因外用膜的制备刘秀青廖丹红(广西中医药大学,广西南宁,530001)摘要:[目的]掌握小量制备膜剂的方法。
熟悉常用成膜材料的性质和特点.[方法]采用手工刮板法制备利多卡因外用膜剂制备。
[结果]膜剂外观完整光洁,厚度一致,色泽均匀,无明显气泡。
[结论]膜剂除主药和成膜材料,还需加入增塑剂(如甘油,山梨醇等)。
质量好的膜剂是外观光洁,厚度一致,没有明显的气泡。
关键词:膜剂,利多卡因,成膜材料Lidocaine topical membrane preparationLiuxiu Qing, Liao Danhong(Guangxi University of Traditional Chinese Medicine, Nanning, Guangxi, 530001) Abstract: Objective To know the small amount of film former method of preparation.Familiar with the nature of the material used and the characteristics of film. . Methods Preparation of homogenate made film preparation of lidocaine topical film former..Results cover film appearance of a complete smooth, uniform thickness, uniform color, no air bubbles. Conclusion In addition to the main film former drug and film materials, need to add plasticizers (such as glycerol, sorbitol, etc.)Key words: Film former, Lidocaine,Film-forming material利多卡因是医用临床常用的局部麻药,1963年用于治疗心率失常,是目前防治急性心肌梗死及各种心脏病并发快速室性心律失常药物,是急性心肌梗死的室性早搏,室性心动过速及室性震颤的首选药。
第47卷第1期2010年1月真空VACUUMVol.47,No.1Jan.2010收稿日期:2009-07-08作者简介:徐小玉(1979-),女,江苏省常州市人,硕士。
联系人:黄之德,副教授。
磁控溅射法制备铁氧体薄膜的界面结合强度研究徐小玉,黄之德(常州轻工职业技术学院,江苏常州213164)摘要:利用磁控溅射法在单硅晶基底和玻璃基底上沉积铁氧体薄膜,采用AFM 观察薄膜的微观形貌,采用划痕法测试薄膜的界面结合强度,测试结果表明:由于两种不同材质上沉积的薄膜粗糙度缘故,硅晶/铁氧体薄膜的临界载荷为19.7N ,其划痕形貌为裂纹状扩展,玻璃/铁氧体薄膜的临界载荷为5.3N ,其划痕形貌为剥落状。
关键词:铁氧体薄膜;界面结合强度;划痕法中图分类号:TB43;O484文献标识码:A文章编号:1002-0322(2010)01-0043-03Study on interfacial adhesion strength of ferrite film deposited by magnetron sputteringXU Xiao-yu ,HUANG Zhi-de(Changzhou Institute of Light Industry Technology,Changzhou 213164,China)Abstract:The ferrite thin films were deposited on monocrystalline silicon and glass substrates by magnetron sputtering.Theirmorphologies were observed by AFM with the interfacial adhesion strength between film and substrate tested by scratch test.The results showed that because of the different surface roughnesses of the two types of substrates,the scratched crack propagates on ferrite film deposited on silicon substrate when the critical load is 19.7N,but the film deposited on glass substrate is spalled from the substrate during the scratch test when the critical load is 5.3N.Key words:ferrite film;interfacial adhesion strength;scratch test由于电子器件的微型化、小型化发展趋势,薄膜器件的应用范围也不断扩大。
射线法金属薄膜厚度英文回答:X-ray diffraction (XRD) is a versatile non-destructive technique for characterizing the structure and properties of materials, including the thickness of metal films. XRD works by directing a beam of X-rays at the sample and measuring the intensity and pattern of the diffracted X-rays. The thickness of the metal film can be determined by analyzing the intensity of the diffracted X-rays at specific angles.The basic principle behind XRD is Bragg's law, which states that when X-rays interact with a crystalline material, they are diffracted at specific angles that are determined by the wavelength of the X-rays and the spacing between the atoms in the crystal. In the case of a thin metal film, the diffracted X-rays will interfere with each other, producing a pattern of peaks and valleys in the intensity of the diffracted X-rays.The thickness of the metal film can be determined by measuring the distance between the peaks in the diffraction pattern. The distance between the peaks is related to the spacing between the atoms in the metal film, which in turn is related to the thickness of the film.XRD is a highly accurate and precise technique for measuring the thickness of metal films. It is non-destructive, so it does not damage the sample, and it can be used to measure the thickness of films on a variety of substrates.中文回答:射线法测量金属薄膜厚度。
Chemlok® 6411 Adhesive Technical Data SheetChemlok® 6411 adhesive is a covercoat adhesive that bonds rubber compounds to metal. It is composed of a mixtureof polymers and heat-reactive components dissolved or dispersed in an organic solvent system.For general use, Chemlok 6411 adhesive should be used as a covercoat adhesive over Chemlok 205 or 207 primer. In some applications, it may be used as a one-coat adhesive. Features and Benefits:Versatile – can be used as a one-coat adhesive; bonds a wide variety of elastomer compounds to rigid substrates when used in combination with Chemlok 205 or 207 primer. Use of Chemlok 205 or 207 primer helps to ensure environmental resistance of the bonded assembly and adhesion to the substrate.Easy to Apply – applies easily by spray, dip, brush or roll coat methods.Environmentally Resistant – provides good resistance to heat, oil and corrosive-type conditions. Elastomers:• Natural Rubber (NR) • Polybutadiene (BR)• Polyisoprene (IR) • Polychloroprene (CR)• Styrene-butadiene (SBR) • Nitrile (NBR)• EPDM Polymers• Chlorinated Polyethylene (CPE)• Chlorosulfonated Polyethylene (CSM)Application:Surface Preparation – Thoroughly clean metal surfaces prior to primer application. Remove protective oils, cutting oils and greases by solvent degreasing or alkaline cleaning. Remove rust, scale or oxide coatings by suitable chemical or mechanical cleaning methods.Allow primer to thoroughly dry before applying Chemlok 6411 adhesive.For further detailed information on surface preparation of specific substrates, refer to Chemlok Adhesives application guide.Mixing – Thoroughly stir adhesive before use, and agitate sufficiently during use to keep dispersed solids uniformly suspended. If dilution is needed, use xylene or toluene. Note proper dilution for the various application methods is best achieved by experience. Give careful attention to agitation since dilution will accelerate settling.Applying – Apply adhesive by brush, roll coat, dip, spray or any other method that gives a uniform coating and avoids excessive runs and tears.Regardless of application method, the dry film thickness of Chemlok 6411 adhesive should be 12.7-25.4 micron (0.5-1.0 mil).Drying/Curing – Allow the applied adhesive to dry until visual examination of the film has shown that all solvent has evaporated. This will take approximately 30 minutes at room temperature. Drying time can be shortened by using hot airdrying ovens or tunnels up to 90°C (194°F).Parker LORDEngineered Materials Group 111 LORD DriveCary, NC 27511-7923USAphone +1 877 ASK LORD (275 5673)Values stated in this document represent typical values as not all tests are run on each lot of material produced. For formalized product specifications for specific product end uses, contact the Customer Support Center.Information provided herein is based upon tests believed to be reliable. In as much as Parker LORD has no control over the manner in which others may use this information, it does not guarantee the results to be obtained. In addition, Parker LORD does not guarantee the performance of the product or the results obtained from the use of the product or this information where the product has been repackaged by any third party, including but not limited to any product end-user. Nor does the company make any express or implied warranty of merchantability or fitness for a particular purpose concerning the effects or results of such use.WARNING — USER RESPONSIBILITY . FAILURE OR IMPROPER SELECTION OR IMPROPER USE OF THE PRODUCTS DESCRIBED HEREIN OR RELATED ITEMS CAN CAUSE DEATH, PERSONAL INJURY AND PROPERTY DAMAGE.This document and other information from Parker-Hannifin Corporation, its subsidiaries and authorized distributors provide product or system options for further investigation by users having technical expertise.The user, through its own analysis and testing, is solely responsible for making the final selection of the system and components and assuring that all performance, endurance, maintenance, safety and warning requirements of the application are met. The user must analyze all aspects of the application, follow applicable industry standards, and follow the information concerning the product in the current product catalog and in any other materials provided from Parker or its subsidiaries or authorized distributors.To the extent that Parker or its subsidiaries or authorized distributors provide component or system options based upon data or specifications provided by the user, the user is responsible for determining that such data and specifications are suitable and sufficient for all applications and reasonably foreseeable uses of the components or systems.©2020 Parker Hannifin - All Rights ReservedInformation and specifications subject to change without notice and without liability therefor. Trademarks used herein are the property of their respective owners.Chemlok 6411 Adhesive — Technical Data SheetOD DS4008 11/20 Rev.7Shelf Life/Storage:Shelf life is one year from date of shipment when stored by the recipient below 25°C (77°F) in original, unopened container.Cautionary Information:Before using this or any Parker LORD product, refer to the Safety Data Sheet (SDS) and label for safe use and handling instructions.For industrial/commercial use only. Must be applied by trained personnel only. Not to be used in household applications. Not for consumer use.。
DuPont FEP Film FLUOROCARBON FILMDescriptionDuPont FEP fluorocarbon film offers the outstanding properties of FEP fluoropolymer in a convenient, easy-to-use form. It can be heat-sealed, thermoformed, welded, metalized, and laminated to many other materials or serve as a hot melt adhesive.This combination of unique properties and easy-to-use form offers design and fabrication opportunities for a wide variety of end uses.FEP Is Unique Among Plastics• Most chemically inert of all plastics• Withstands both high- and low-temperature extremes• Superior anti-stick/low friction properties• Outstanding weather resistance• Excellent optical characteristics• Superior electrical properties• Free of plasticizers or additives• Excellent processibility with conventional thermoplastic methodsDuPont FEP Film Is Offered• In thicknesses from 12.5–500 µm (0.5–20 mil)• In custom slit widths up to 1.2–1.6 m (46–63 in) depending on thickness• In various size rolls wound on 7.6 cm or 15.2 cm(3 in or 6 in) cores DuPont FEP film affords the engineer/designer a wide range of opportunities to take advantage of these properties with minimal and convenient fabrication techniques. The ability of DuPont FEP film to be easily cut, thermoformed, heat sealed, and welded permits ready application as diaphragms, gaskets, protective linings, or thermoformed pouches or containers, wherever high temperature and/or chemical resistance is required.The excellent optical properties and resistance to weathering and ultraviolet degradation have led to the use of DuPont FEP film in such varied applications as environmental growth chambers, solar energy collectors, and radome windows.Its superior dielectric properties have been used in flexible, flat cable insulation, printed circuits, and electronic components for computers and aircraft.The nonstick properties of DuPont FEP film have found use in conveyor belts, process roll covers, and as mold release films.A complete listing of FEP film grades and their availability in different thicknesses is given in Table 1.In addition to FEP, DuPont offers films of PFA, for use at temperatures up to 260°C (500°F), and Tefzel® ETFE fluoropolymer for increased toughness and resistance to tear propagation.DuPont FEP film offers unique properties in a convenient form requiring minimal fabrication. Consider it for your next project. For additional information, call (800) 283-2493.Information BulletinTypes and GuagesNote: Each roll of DuPont film is clearly identified as to resin type, film thickness, and film type.FEP 500 CResin type Film thickness, 500 gauge, 5 mil Film type, cementable one sideMechanical and Thermal PropertiesDuPont FEP films perform well over a wide range oftemperatures. DuPont FEP film has a continuous servicetemperature range from –240 to 205°C (–400 to 400°F), and itcan be used in intermittent service at temperatures as high as260°C (500°F). See Tables 2 and 3.Tensile PropertiesFigures 1–3 show how tensile properties of DuPont FEP film varywith temperature. FEP films retain useful mechanical propertiesover a wide range from cryogenic to high temperatures.Dimensional StabilityThere are three components to the property of dimensionalstability—hygroscopic expansion, residual shrinkage, andthermal expansion.Hygroscopic ExpansionBecause the moisture absorption of DuPont FEP fluorocarbonfilm is less than 0.01% when totally immersed in water, changesin relative humidity have little effect on the film.Figure 1: Tensile Stress vs. Elongation of DuPont FEP FilmFigure 2: Tensile Properties of DuPont FEP Film vs. TemperatureFigure 3: Tensile Stress vs. Elongation of DuPont FEP Film*200 gauge unless otherwise noted **100 gauge film***Temperature at which film supports a load of 0.14 MPa (20 psi) for 5 secResidual ShrinkageStresses set up in the film during manufacturing or converting can cause shrinkage in unrestrained film when exposed to high temperatures. Exposure of film to an elevated temperature, and the attendant shrinkage, will relieve this stress, and no further shrinkage will occur at lower temperatures.Thermal ExpansionAfter residual shrinkage has been removed, DuPont FEP film will expand and contract according to its normal coefficient of thermal expansion (see Figures 4 and 5). Note that this coefficient increases with temperature.Figure 4: Shrinkage of DuPont FEP 100A Film vs. Temperature*Samples melted in arc did not trackFigure 6: Dielectric Strength vs. Film Thickness of DuPont FEP Film Dielectric Constant Figure 7: Dielectric Constant vs. Temperature of DuPont FEP Film at 1 kHz and 100 kHzFigure 5: Thermal Expansion of DuPont FEP Film Electrical PropertiesFEP fluorocarbon films exhibit excellent electrical properties overa wide range of frequencies and temperatures. Table 4 showshow initial properties are retained even after long-term exposureto extreme environmental conditions.Dielectric StrengthFigure 6 shows how the dielectric strength of DuPont FEP film isa function of film thickness; thinner films exhibit greaterdielectric strength.For DuPont FEP film, dielectric constant is independent of filmthickness. There is no difference between Type A and Type C films.At a constant frequency, the dielectric constant of DuPont FEPfilm decreases with rise in temperature due to thermal expansion(see Figure 7). At a constant temperature, the dielectric constantfalls slightly with an increase in frequency above 107 Hz (seeFigure 8).The consistently low value of the dissipation factor over a broadrange of temperature and frequency makes FEP fluorocarbonfilm ideal in applications where electrical losses must beminimized (see Figure 9).At a constant temperature, this dissipation factor of FEP filmsvaries as noted in Figure 10. Absolute values remain low incomparison with many other dielectric materials.Figure 9: Dissipation Factor vs. Temperature of DuPont FEP FilmFigure 10: Dissipation Factor vs. Frequency of DuPont FEP FilmVolume ResistivityVolume resistivity of DuPont FEP film decreases slightly as thefilm thickness increases (see Figure 11).Even at 200°C (392°F), the insulation resistance of DuPont FEPfilm (65,000 megohm-microfarad) is higher than most conventionaldielectric materials at room temperature (see Figure 12).Figure 12: Insulation Resistance vs. Temperature (125 µm/0.5 milDuPont FEP film)Figure 11: Volume Resistivity vs. Thickness (at 175°C [347°F])Insulation ResistanceFigure 8: Dielectric Constant vs. FrequencyAbietic acidAcetic acidAcetic anhydride Acetone Acetophenone Acrylic anhydride Allyl acetateAllyl methacrylate Aluminum chloride Ammonia, liquid Ammonium chloride Aniline Benzonitrile Benzoyl chloride Benzyl alcohol BoraxBoric acid Brominen-Butyl amine Butyl acetateButyl methacrylate Calcium chloride Carbon disulfide CetaneChlorine Chloroform Chlorosulfonic acid Chromic acid CyclohexaneCyclohexanoneDibutyl phthalateDibutyl sebacateDiethyl carbonateDiethyl etherDimethyl formamideDi-isobutyl adipateDimethylformamideDimethylhydrazine,unsymmetricalDioxaneEthyl acetateEthyl alcoholEthyl etherEthyl hexoateEthylene bromideEthylene glycolFerric chlorideFerric phosphateFluoronaphthaleneFluoronitrobenzeneFormaldehydeFormic acidFuraneGasolineHexachlorethaneHexane HydrazineHydrochloric acidHydrofluoric acidHydrogen peroxideLeadMagnesium chlorideMercuryMethyl ethyl ketoneMethacrylic acidMethanolMethyl methacrylateNaphthaleneNaphtholsNitric acidNitrobenzene2-Nitro-butanolNitromethaneNitrogen tetroxide2-Nitro-2-methyl propanoln-Octadecyl alcoholOils, animal and vegetableOzonePerchlorethylenePentachlorobenzamidePerfluoroxylenePhenolPhosphoric acidPhosphorus pentachloridePhthalic acidPinenePiperidenePolyacrylonitrilePotassium acetatePotassium hydroxidePotassium permanganatePyridineSoap and detergentsSodium hydroxideSodium hypochloriteSodium peroxideSolvents, aliphatic andaromatic**Stannous chlorideSulfurSulfuric acidTetrabromoethaneTetrachlorethyleneTrichloracetic acidTrichlorethyleneTricresyl phosphateTriethanolamineVinyl methacrylateWaterXyleneZinc chlorideChemical PropertiesDuPont FEP fluorocarbon film is chemically inert and solvent resistant to virtually all chemicals except molten alkali metals, fluorine at elevated temperatures, and certain complex halogenated compounds such as chlorine trifluoride at elevated temperatures and pressures.In circumstances where end-use temperatures are close to the upper service limit of 205°C (400°F), 80% sodium hydroxide, metal hydrides, aluminum chloride, ammonia, and certain amines (R-NH2) may attack the film in a manner similar to molten alkali metals. Special testing is required when such extreme reducing or oxidizing conditions are evident. With these exceptions noted, DuPont FEP fluorocarbon films exhibit a very broad range of chemical and thermal serviceability.Due to the many complex aspects of performance in severe environments, final selection should be based on functional evaluations or experience under actual end-use conditions. The chemical substances listed in Table 5 are representative of those with which DuPont FEP film has been found to be nonreactive.Table 5 - Typical Chemicals with Which DuPont FEP Film is Nonreactive** Based on experiments conducted up to the boiling points of the liquids listed. FEP resins have normal service temperatures up to 205°C (400°F). Absence of a specific chemical does not mean that it is reactive with FEP film.** Some halogenated solvents may cause moderate swelling.AbsorptionAlmost all plastics absorb small quantities of certain materials with which they come in contact. Submicroscopic voids between polymer molecules provide space for the material absorbed without chemical reaction. This phenomenon is usually marked by a slight weight increase and sometimes by discoloration.DuPont FEP fluorocarbon films have unusually low absorption compared with other thermoplastics. They absorb practically no common acids or bases at temperatures as high as 200°C(392°F) and exposures of up to one year. Even the absorption of solvents is extremely small. Weight increases are generally less than 1% when exposed at elevated temperatures for longperiods. In general, aqueous solutions are absorbed very little by DuPont FEP film. Moisture absorption is typically less than 0.01% at ambient temperature and pressure.PermeabilityMany gases and vapors permeate FEP films at a much lower rate than for other thermoplastics (see Figure 13). In general, permeation increases with temperature, pressure, and surface contact area and decreases with increased film thickness. Table 6 lists rates at which various gases are transmittedthrough DuPont FEP fluorocarbon film, while Table 7 lists rates of vapor permeability for some representative substances. Note that the pressure for each material is its vapor pressureat the indicated temperature.*To convert to cm 3/(100 in2.24 h.atm), multiply by 0.0645.Figure 13: Water Vapor Transmission Rate of DuPont FEP Film at 40°C (104°F) per ASTM E-96 (Modified)Note: Values are averages only and not for specificationpurposes. To convert the permeation values for 100 in 2 to those for 1 m 2, multiply by 15.5.Optical PropertiesDuPont FEP films transmit a high percentage of ultraviolet and visible light and are much more transparent to the infrared spectrum than glass (see Figures 14–16). Other optical properties of FEP films of interest are:FEP Solar Transmission (ASTM E-424) 96%Refractive Index (ASTM D-542)1.341–1.347Figure 14: Transmission Spectrum for DuPont FEP FilmMiscellaneous PropertiesCryogenic ServiceFEP has performed satisfactorily in cryogenic service attemperatures below that of liquid nitrogen. DuPont FEP fluorocarbon film is normally inert to liquid oxygen (LOX) when the film is free of contamination, pigmentation, or fillers for dew (Fungus) ResistanceFEP has been shown to be completely resistant to mildew growth by testing both in humidity chamber exposure inoculated with a mixed spore suspension and a soil burial test for three months.WeatherabilityIn contrast to most other clear thermoplastic films, DuPont FEP film remains essentially unchanged after 20 years of outdoor exposure (see Figure 17). There is no evidence of discoloration, ultraviolet degradation, or strength loss. This outstandingperformance is due to the structure of the polymer molecule and is not the result of chemical additives.Types C and C-20 DuPont FEP film are not recommended for outdoor applications because ultraviolet radiation may adversely affect the treated surface.Figure 17: The Effects of Florida Weathering on DuPont FEP FilmFigure 15: Transmittance at Normal Incidence of Solar Radiation through DuPont FEP Films for Various ThicknessesFigure 16: Transmittance of Solar Radiation through 25 µm (1 mil) DuPont FEP Film for Various Angles of IncidenceSafety and HandlingUnheated FEP fluorocarbon is essentially inert. Animal tests indicate that FEP is non-irritating and non-sensitizing to the skin. Dust generated by cutting, grinding, or machining the unheated film should be avoided, as with any other nuisance dusts that are regulated by OSHA at 15 mg/m 3 in air (29 CFR 1910:1000).Care should be taken to avoid contamination of smoking tobacco or cigarettes with fluorocarbon resins.DuPont FEP film can be processed and used at elevated temperatures without hazard if proper ventilation is used. Ventilation should be provided at processing temperatures of275°C (525°F) or above. Additional details on safety in handling and use are available in the “Guide to the Safe Handling of Fluoropolymer Resins” latest edition, published by theFluoropolymers Division of the Society of Plastics Industry (SPI).Other related literature available from DuPont:BulletinTitleE-80413-2 DuPont PFA Film—Specification Bulletin (T62-3)H-55003-2 DuPont FEP Film—Specification Bulletin (T62-1)H-55008-3DuPont FEP Film—Properties BulletinH55007-3 (09/10)For more information call (302) DuPont Fluoroproducts P.O. Box 80713Wilmington, DE 19880-0713EuropeDuPont de Nemours Int’l SA DuPont Fluoroproducts 2, chemin du Pavillon P .O. Box 50CH-1218 Le Grand-Saconnex Geneva, SwitzerlandJapanDuPont Kabushiki Katsha Arco Tower8-1, Shimomeguro 1-chome Meguro-ku, Tokyo 153 Japan81-3-5434-6139Asia PacificDuPont China Holding Co. Ltd.Bldg. 11, 399 Keyuan Road Zhangjiang Hi-Tech Park Pudong New District Shanghai, 201203, China Tel: +86 400 88 51 888CanadaDuPont Canada, Inc.DuPont Fluoroproducts P .O. Box 2200, Streetsville 7070 Mississauga RoadMississauga, Ontario, Canada L5M 2H3(800) 207-0756South AmericaDuPont do Brasil S/A FluoropolymersAlameda Itapecuru, 50606454-080 - Alphaville P .O. Box 263Barueri, Sao Paulo, Brazil 0800-171715Produtos.Brazil@。
专利名称:Method for Producing a Film Element发明人:Ludwig Brehm,Haymo Katschorek,NorbertLaus申请号:US15259620申请日:20160908公开号:US20160375714A1公开日:20161229专利内容由知识产权出版社提供专利附图:摘要:The invention concerns a process for producing a film element having mutually registered metallic layers () and a film element which can be produced by such a process.A first metallic layer () provided on a first surface of a flexible single-layer or multi-layercarrier film () and a masking layer () provided on the second surface of the carrier film (), opposite to the first surface, are structured in accurate register relationship with each other by means of mutually synchronised structuring procedures. After structuring of the first metallic layer () and the masking layer () one or more further layers are applied to the first metallic layer (). Applied to the one or more further layers () is a second metallic layer () to which a first photoactivatable layer () is applied. The first photoactivatable layer () is structured by means of trans-exposure through the masking layer (), the first metallic layer, the one or more further layers and the second metallic layer () from the side of the masking layer () by means of electromagnetic radiation of a wavelength to which the first photoactivatable layer () is sensitive, or the first photoactivatable layer is exposed controlledly through the masking layer from the side of the film body that is opposite to the masking layer.申请人:LEONHARD KURZ Stiftung & Co. KG地址:Furth DE国籍:DE更多信息请下载全文后查看。
专利名称:METHOD OF PRODUCTION OF A FILM 发明人:AULNETTE, Cécile,CAYREFOURCQ,Ian,MAZURE, Carlos申请号:EP06809161.0申请日:20060706公开号:EP1911085B1公开日:20111012专利内容由知识产权出版社提供摘要:The invention relates to a method of producing a film intended for applications in electronics, optics or optronics starting from an initial wafer, which includes a step of implanting atomic species through one of the faces of the wafer, which method comprises the following stages: (a) formation of a step of determined height around the periphery of the wafer, the mean thickness of the wafer at the step being less than the mean thickness of the rest of the wafer; (b) protection of said step against the implantation of atomic species; and (c) implantation of atomic species through that face of the wafer having said step, so as to form an implanted zone at a determined implant depth, said film being determined, on one side, by the implanted face of the wafer and, on the other side, by the implanted zone. The invention also relates to a wafer obtained by said method.申请人:SOITEC SILICON ON INSULATOR地址:FR国籍:FR代理机构:Bomer, Françoise Marie更多信息请下载全文后查看。
专利名称:X-RAY MASK发明人:ARAKAWA TOMIYUKI,荒川 富行,OKUYAMAHIROSHI,奥山 浩申请号:JP特願平4-47661申请日:19920204公开号:JP特開平5-217864A公开日:19930827专利内容由知识产权出版社提供专利附图:摘要:PURPOSE:To control distortion of a pattern position generated after an X-ray mask for X-ray lithography is irradiated with the X-ray and abosorbs it by dividing a mask supporting film into four regions of equal area with two line segments crossing orthogonally with each other and covering each region with a particular absorbingmaterial pattern. CONSTITUTION:A SiN film is formed on a Si film by the chemical vaporphase growth method under the reduced pressure and Ta is formed in various areas and shapes thereon by the sputtering method. Thereafter, Si is back-etched to form, for example, a square window having a side of 26mm in view of completing a sample. The exposure region (square window having a side of 26mm) is divided into 16 small regions and distortion of position after irradiation with the X-ray in such a case that such smaller regions are covered with Ta in various combinations is measured. As a result, reduction of distortion becomes distinctive in the case that an absorbing material coverage rate of each region is 50% or higher. Thereby, a pattern position distortion on the mask can be controlled.申请人:SOLTEC:KK,株式会社ソルテック地址:東京都文京区湯島3丁目31番1号国籍:JP代理人:吉原 省三 (外1名)更多信息请下载全文后查看。
专利名称:Method of controlling the film thickness of blown and axially, preferably biaxiallystretched tubular films发明人:FEISTKORN, WERNER, DR. DIPL.-ING.,VOSS, KLAUS-PETER, DIPL.-ING.申请号:EP90120516.1申请日:19901025公开号:EP0432423A1公开日:19910619专利内容由知识产权出版社提供摘要:For the axial, preferably biaxial stretching of tubular films laid flat after their production on a blown film extruder line, the said films are inflated again to form a tubular film bubble (4) or are expanded to form a film tube. In the inflated or expanded state, these then run through an oven (11), from which they are drawn off, with renewed flattening (12), at a rate which is increased with respect to the running-in rate by an amount corresponding to the desired stretching ratio. In order to ensure that the stretched tubular films have a substantially equal thickness distribution over their circumference, the film thickness of the stretched tubular film emerging from the oven (11) is measured over its circumference before or after its flattening (12) and the thickness distribution over the circumferential profile of the tubular film produced on the blown film extruder line is set according to the measured thicknesses of the circumferential profile in such a way as to compensate substantially for deviations from the average film thickness brought about in the oven during stretching on account of uneven heating and possibly other disturbing influences.申请人:WINDMOELLER & HOELSCHER地址:MUENSTERSTRASSE 50; W-4540 LENGERICH,Münsterstrasse 50 D-49525 Lengerich DE国籍:DE代理机构:Gossel, Hans K., Dipl.-Ing.更多信息请下载全文后查看。
专利名称:Ductile film and method of designing ductilefilm发明人:飯島 佑介申请号:JP2018224674申请日:20181130公开号:JP2020083850A公开日:20200604专利内容由知识产权出版社提供专利附图:摘要:PROBLEM TO BE SOLVED: To provide a film in which the influence of variations in film shape on film characteristics is minimized, and a method for designing the film. Aductile film has a summit of a length of a first slope portion, a length of a top portion anda length of a second slope portion in a predetermined direction as L, and a top portion and a bottom surface in a direction orthogonal to the predetermined direction. When the distance between the parts is H and the sum of the length of the first slope, the length of the top, the length of the bottom and the length of the second slope in the predetermined direction is P, the value of U/L is 0. It becomes 19 or more and 0.83 or less, the value of L/P becomes 0.51 or more and 0.70 or less, and the value of H/L becomes 0.28 or more and 0.67 or less. [Selection diagram] Figure 1申请人:凸版印刷株式会社地址:東京都台東区台東1丁目5番1号国籍:JP代理人:特許業務法人第一国際特許事務所更多信息请下载全文后查看。
专利名称:HIGHLY ORIENTED FILM BY COLD DRAWING AND ITS PRODUCTION发明人:YOSHIMURA ISAO,HATAKE HIDEO,KANEKO KOUJI申请号:JP6387378申请日:19780530公开号:JPS54155272A公开日:19791207专利内容由知识产权出版社提供摘要:PURPOSE:To obtain a highly oriented flushing film suitable for agricultural and packaging materials, having high strength, by extruding a composition consisting of ethylene-vinyl acetate copolymer, alpha-olefin copolymer, and polyamide, from a die, followed by orientation. CONSTITUTION:A composition consisting of A) ethylene-vinyl acetate copolymer, B) a thermoplastic elastomer made of alpha-olefin copolymer, and C) polyamide is mixed to give a molten blend. The blend is extruded from a die, guenched by a liquid refrigerant, and set to make a raw film, which is heated up to not more than 100 deg.C and oriented in a cold state at 20-100 deg.C at an area draw ratio of 5-30:1 and at a cross direction draw ratio of 2-7:1 to have a reflectance of diffused reflection not less than 30%. A copolymer of A having less than 30 wt. % of vinyl acetate group degrades orientation in a cold state, film strength, and thermal shrinkage, and a copolymer of A having not less than 30 wt. of vinyl acetate group reduces stretchability.申请人:ASAHI DOW LTD更多信息请下载全文后查看。
专利名称:Unwinder for a film with a base unit and adispenser unit发明人:SCHARF, PETER申请号:EP14166481.3申请日:20140429公开号:EP2805906A3公开日:20141231专利内容由知识产权出版社提供专利附图:摘要:the invention relates to a klebefilmabroller 1 with a sockeleinheit 2 and acassette compartment 3 for a klebefilm, whereby the cassette compartment toaccommodate a klebefilmrolle and a knife to cut the klebefilms 13 or 16. thesockeleinheit has a base to establish or positioning on a substrate and a recording on the cassette compartment.the cassette compartment 3 is for use as a handabroller from the inclusion of the sockeleinheit 2 is delivered and for use as a standabroller in the inclusion of the sockeleinheit arranged and \/ or the cassette compartment is the inclusion of the sockeleinheit rotatable between a first job. onsstellung,in the klebefilm 13 by a user of the klebefilmrolle deductible and the knife 16 separable, and a second funktionsstellung, in the klebefilm and knife 16 from the surroundings and the user are covered.申请人:SENATOR GMBH & CO. KGAA地址:Bahnhofstrasse 57 64401 Gross-Bieberau DE国籍:DE代理机构:Leonhard, Frank Reimund更多信息请下载全文后查看。
专利名称:MANUFACTURE OF FILM发明人:SUENAGA JUNICHI,SHINONOME OSAMI,KISHIDA MINORU,FUJITAEIJI,KINUGAWA MASAYUKI申请号:JP10563690申请日:19900419公开号:JPH044126A公开日:19920108专利内容由知识产权出版社提供摘要:PURPOSE:To obtain a film of a liquid crystalline polymer which possesses well-balanced high power and high elasticity in a crosswise direction and high uniformity, by a method wherein a specific thermotropic liquid crystalline polymer is oriented biaxially by an inflation method. CONSTITUTION:A liquid crystalline polymer to be used follows a measurement method ASTIM D-648 and a difference between thermal deformation temperatures measured under loads of 18.6 kg/cm<2> and 4.6 kg/cm<2> is within a range of 15 deg.C. As the liquid crystalline polymer which falls under this category and capable of performing melting and molding, a matter, which is a copolymer, for example, of p-hydroxybenzoic acid and polyethylene terephthalate and having a mol ratio of50/50-70/30, can be mentioned. Although the same is made into a film by an inflation method, at the time of extrusion of a molten material through an annular slit die, a tubular film is expanded by applying external force to the inside of the tubular film to be obtained and the film is oriented by applying draft to also a receiving direction of the film. Then a draw ratio in the direction meeting at right angles with the receiving direction is made normally at least two times, preferably at least three times.申请人:UNITIKA LTD 更多信息请下载全文后查看。
Asian Journal of Pharmaceutical Sciences14(2019)313–320Available online at journal homepage:/locate/AJPSOriginal Research PaperFormulation of a film-coated dutasteride tabletbioequivalent to a soft gelatin capsule(Avodart®):Effect ofγ-cyclodextrin and solubilizersMi-Hong Min a,b,Jin-Hyong Park b,Mi-Ran Choi b,Jong-Hyun Hur b,Byung-Nak Ahn b,Dae-Duk Kim a,∗a College of Pharmacy and Research Institute of Pharmaceutical Sciences,Seoul National University,Seoul08826,Republic of Koreab Central Research Institute,Whanin Pharmaceutical Company,4F,GBSA,107Gwanggyo-ro,Yeongtong-gu,Suwon16229,Republic of Koreaa r t i c l e i n f oArticle history:Received25April2018Revised26August2018Accepted30August2018Available online5October2018Keywords:DutasterideTabletCyclodextrinComplexFormulationa b s t r a c tThe aim of this study was to optimize a tablet formulation of dutasteride that is bioequiva-lent to a commercially available soft gelatin capsule(Avodart®).The effect of cyclodextrin onenhancing the aqueous solubility of dutasteride was investigated,after which the formula-tion was further optimized with solubilizing polymer and surfactant.Among the cyclodex-trins tested,the highest solubility was observed when dutasteride was complexed withγ-cyclodextrin.Moreover,the addition of polyvinylpyrrolidone and Gelucire/TPGS furtherenhanced the solubility of dutasteride.Differential scanning calorimetry(DSC)and powderX-ray diffraction(pXRD)studies demonstrated that dutasteride existed in the amorphousform in the complex.Optimized dutasteride complexes were selected after a pharmacoki-netic study in rats,and film-coated tablets were prepared by the direct compression method.In vitro dissolution profiles for the tablets of dutasteride complexes were similar to those ofthe reference.Moreover,pharmacokinetic parameters including the C m ax and AUC valuesafter oral administration in beagle dogs were not significantly different from those of thereference with a relative bioavailability of92.4%.These results suggest the feasibility of de-veloping a tablet formulation of dutasteride using cyclodextrin complex in addition to asolubilizing polymer and surfactant.©2018Shenyang Pharmaceutical University.Published by Elsevier B.V.This is an open access article under the CC BY-NC-ND license.(h ttp:///licenses/by-nc-nd/4.0/)∗Corresponding author.College of Pharmacy and Research Institute of Pharmaceutical Sciences,Seoul National University,1Gwanak-ro,Gwanak-gu,Seoul08826,Republic of Korea.Tel.:+8228807870.E-mail address:ddkim@snu.ac.kr(D.D.Kim).Peer review under responsibility of Shenyang Pharmaceutical University.https:///10.1016/j.ajps.2018.08.0071818-0876/©2018Shenyang Pharmaceutical University.Published by Elsevier B.V.This is an open access article under the CC BY-NC-ND license.(h ttp:///licenses/by-nc-nd/4.0/)314Asian Journal of Pharmaceutical Sciences14(2019)313–3201.IntroductionDutasteride is a competitive inhibitor of type I and type II5-α-reductases and is used to treat benign prostatic hyperplasia (BPH)and hair loss[1].Studies have revealed that dutasteride can reduce fetal adrenal and prostate weight and can increase fetal ovarian and testis weight.It has been classified as preg-nancy category X by the FDA;thus,women who are preg-nant or may become pregnant must avoid taking and handling dutasteride.Dutasteride is classified as Biopharmaceutics Classifica-tion System(BCS)class II and is commercially available in the market only as a soft gelatin capsule formulation due to its low aqueous solubility[1].However,the physical strength of the gelatin shell could become weaker under high tempera-ture,which might break the seam-line or deform the shape of the capsule.Additionally,the active ingredient could mi-grate into the gelatin shell[2].Because dutasteride is readily absorbed through the skin,these issues can lead to various health problems.Therefore,developing a tablet form of du-tasteride is required to enhance the safety of the drug.Ad-ditionally,improved patient compliance is expected with a smaller solid tablet than a soft gelatin capsule.Moreover,be-cause dutasteride is commonly co-prescribed with other BPH medicines such as tamsulosin,it would be more convenient to formulate solid dosage forms for fixed-dose combinations with other drugs.Previous studies on solubilization of dutasteride have been mainly focused on self-emulsifying drug delivery system (SMEDDS)technology[3–5],which is an oil formulation suit-able for soft capsule.To increase the bioavailability of various hydrophobic and poorly water-soluble drugs,the drugs can be formulated to form a complex with cyclodextrin(CD)as a solid dosage form,thereby enhancing their solubility and/or dissolution rate[6–12].Because no covalent bonds are in-volved in the drug-CD complex formation,the complex can be easily dissociated in aqueous solution[13].Moreover,diverse approaches have been attempted to further enhance the complexation efficacy,which include the addition of polymers [14],organic salts[15],and buffer[16]to the complexation me-dia.Addition of a small amount of a water-soluble polymer to an aqueous complexation medium increases the complexa-tion efficiency,which consequently can decrease the formu-lation bulk by reducing the amount of CD required[13].More-over,water-soluble polymers form complexes with various compounds and stabilize micelles and other types of aggre-gates in aqueous solutions[13,17].They are additionally capa-ble of increasing the aqueous solubility of cyclodextrins with-out decreasing their complexing abilities[18].Pharmaceutical polymers such as methylcellulose,hydroxypropylmethylcel-lulose and polyvinylpyrrolidone have traditionally been used to prevent drug nucleation and crystal growth by creating a polymeric network around growing crystals[19].Thus,their addition leads to a decrease in drug crystallization and gener-ates a synergetic effect on the solubilizing effect of CDs[8].Additionally,we assume that the addition of surfactants would further enhance the solubilization of free drug dis-sociated from the drug-CD complex.The objective of this study was to investigate the effect of the CD complex on enhancing the aqueous solubility and dissolution of dutas-teride,after which the formulation was further optimized with diverse polymers and/or surfactants.After a film-coated tablet formulation was finalized,its pharmacokinetics in bea-gle dogs was compared to that of Avodart®soft capsule.2.Materials and methods2.1.MaterialsDutasteride was purchased from Cipla Ltd(Mumbai,India).α-Cyclodextrin(α-CD),β-cyclodextrin(β-CD),γ-cyclodextrin (γ-CD)and hydroxypropyl-β-cyclodextrin(HP-β-CD)were obtained from Wacker Chemie AG(München,Germany). Polyvinylpyrrolidone K30(PVP)(BASF,Germany),d-α-tocopheryl polyethylene glycol1000succinate(TPGS) (Isochem,France),stearoyl polyoxylglycerides(Gelucire50/13) (Gattefosse,France),polyethyleneglycol(PEG400)(Yakuri Pure Chem,Japan)and polyethyleneoxide-polypropylene oxide copolymer(Poloxamer407)(BASF,Germany)were used as ctose(SuperTab11SD)(DFE pharma, Japan),microcrystalline cellulose(Avicel PH102)(FMC,USA), crospovidone(Polyplasone XL)(Ashland,Netherland),mag-nesium stearate(Faci,Italy),Opadry®(Colorcon,Singapore) and ethylcellulose(Ethocel10)(Colorcon,Korea)were used as excipients for the tablets.Avodart®soft capsules(Glaxo-SmithKline,United Kingdom)were purchased from a local pharmacy.2.2.Preparation of dutasteride-cyclodextrin complex and solubility studyDutasteride-loaded CD complexes were prepared by the oven-drying method.Briefly,dutasteride was first dissolved in ethanol at2mg/ml concentration.Various types of cyclodex-trins(α-CD,β-CD,γ-CD,HP-β-CD)were separately dissolved in distilled water(DW)at a concentration of100mg/ml.The dutasteride solution and CD solution were homogeneously mixed at a1:1volume ratio,followed by drying in an oven at 60°C(SANYO,Japan),to determine the aqueous solubility of dutasteride complexed with various CDs at a1:50weight ra-tio.Dried dutasteride-cyclodextrin(DuCD)complexes(equiva-lent to approximately0.5mg of dutasteride)were dispersed in 1.0ml of DW.After gentle stirring for1h,undissolved dutas-teride was removed through filtration(0.45-μm PVDF filter), followed by appropriate dilution with a mixture of acetoni-trile and water(60/40,v/v).The concentration of dutasteride was analyzed using high-performance liquid chromatography (HPLC),equipped with a reverse phase C18column(Zorbax SB-phenyl,150mm×3mm,3.5um,Agilent)and UV detector at 240nm.The mobile phase was a mixture of acetonitrile and water(55/45,v/v)at a flow rate of0.5ml/min.The injection volume was50μl[20].Because theγ-CD complex exhibited the highest solubility among the complexes tested,complexes were prepared at var-ious weight ratios(1:10–1:70)of dutasteride toγ-CD(DuγCD) to optimize the solubility of dutasteride.Next,a0.4or1.0 weight ratio of polymer and/or surfactant was added to theAsian Journal of Pharmaceutical Sciences14(2019)313–320315dutasteride-γ-cyclodextrin complex(DuγCD-PS)as a solubil-ity auxiliary additive to further enhance the aqueous solubil-ity of dutasteride.The aqueous solubility of dutasteride in theDuγCD and DuγCD-PS solutions was determined after filtra-tion as described above.2.3.Pharmacokinetics after oral administrationof DuγCD-PS complex in ratsThe pharmacokinetics of dutasteride after oral administrationof diverse DuγCD-PS complexes was compared with that ofthe reference(Avodart®,GlaxoSmithKline)in rats.The animalstudies were approved by the WhanIn Pharmaceutical Com-pany Animal Ethics Committee.Male Sprague-Dawley rats(8weeks old,230–270g)were purchased from DBL Co.,Ltd(Chungcheongbuk-do,Korea).All rats were habituated for1week before the experiment and randomly divided into groupsof4–6animals each.The rats were subjected to fasting12hprior to the study,and the carotid arteries were cannulatedwith polyethylene tubing PE-50under isoflurane(I-FRAN LIQ-UID,Hana Pharm Co.,Ltd.,Seoul,Korea).Each group of ani-mals was administered either the reference drug(interior oilcontent of Avodart®soft capsule)or DuγCD-PS complex(sus-pended in DW)via oral gavage at a dose of2.39mg/kg of du-tasteride,and each rat was orally administered10ml/kg of DW.Blood samples(approximately0.3ml)were collected from thecarotid artery into heparinized tubes at0,0.5,1,2,4,8,and24h after the administration.The plasma was obtained bycentrifuging the samples at13,000rpm for5min and storedat−70°C until analysis.The concentration of dutasteride in the plasma sampleswas analyzed using LC/MS/MS,as previously described[21].Briefly,100μl of plasma samples was vortex mixed with900μlof acetonitrile containing finasteride(10ng/ml)as an internalstandard and centrifuged at13000rpm.Next,5μl of super-natant was injected into the LC/MS/MS system.LC separationwas performed by an Acquity H class UPLC(Waters,USA),and the mass spectrometric detection was performed on aTQ Detector(Waters,USA)using MRM.A turbo electrosprayinterface was used in positive ionization mode.The majorworking parameters of LC and the mass spectrometer aresummarized in Supplement Table S1.The pharmacokineticparameters(T m ax,C m ax,and AUC0–24h)of dutasteride wereanalyzed using WinNonlin®(ver.6.2,Pharsight)based on thelinear trapezoidal rule.The relative bioavailability(BA)of theDuγCD-PS complexes was calculated as follows:Relative BA(%)=AU C t estAU C re ference×100%2.4.Characterization of dutasteride andγ-cyclodextrin complexesThe surface morphology was observed using field emis-sion scanning electron microscope(FESEM)(JSM-6700F,JEOL, Japan)at an accelerating voltage of5kV.Samples were spread onto carbon tabs(double-adhesive carbon-coated tape)ad-hered to aluminum stubs,which were then coated with a thin layer of platinum.Thermal analysis of DuγCD and DuγCD-PS complexes were conducted by using a differential scanning calorimeter(DSC200F3Mala,Netzsch).Analyses were per-formed in an aluminum pan under a heating rate of10°C/min over a temperature range of20–280°C.XRD Ultima III(Rigaku) was used to perform the powder X-ray diffraction(pXRD)anal-yses.The measurement conditions were as follows:scanning speed of3°/min and step width of0.02°.FTIR was observed using Nicolet IR Spectrometer(iS50,Thermo,USA).2.5.Preparation of dutasteride tabletsTablets of DuγCD-PS complexes(F4and F5)were prepared by the compression method.Briefly,the DuγCD-PS complexes were granulated using the fluid-bed granulator(WBF-II,Enger, Taiwan)with a mixture of lactose(Super Tab11SD)and micro-crystalline cellulose(Avicel PH102)as a powder bed.The for-mulation was designed for each tablet(240mg total weight) to contain0.5mg of dutasteride.Carr’s index for the granules before tablet compression was18,indicating fair flowability. The granules were compressed on a rotary tablet compressor using an8.5-mm round shape punch,and the hardness of the tablet was adjusted between12and13kp.Next,the tablet was film-coated with HPMC-based Opadry®.The dimension of the film-coated tablet after3%weight coating(diameter8.5mm, thickness4.2mm,round shape)was smaller compared with the marketed soft gelatin capsule Avodart®(length19mm, thickness6.7mm,rod shape).(Fig.S1).2.6.Dissolution test of the dutasteride tabletIn vitro dissolution profiles of dutasteride from the DuγCD-PS complex tablet were evaluated by the USP dissolution method (Tier I and Tier II)and compared with that of the reference (Avodart®).In the Tier I method,the dissolution rates of dutas-teride were measured using apparatus2in which the dissolu-tion medium was900ml of0.1N HCl solution with2%(w/v) sodium lauryl sulfate(SLS)at37°C and stirred at50rpm.In the Tier II method,the dissolution medium was450ml of0.1N HCl solution with pepsin(1.6g/l,label activity1:3000)for the first25min,followed by the addition of450ml of0.1N HCl so-lution with SLS(4%,w/v)for the remaining dissolution test. The samples(5ml)were obtained at fixed time intervals and were analyzed by HPLC with a UV detector,as described above, after filtering through a0.45μm PVDF filter.2.7.Pharmacokinetic study of the dutasteride tabletin beagle dogsAn in vivo cross-over pharmacokinetic study of dutasteride was performed after oral administration of the DuγCD-PS complex tablet or the reference(Avodart®)in beagle dogs. The animal studies were approved by the Institutional Ani-mal Care and Use Committee of Korea Animal Medical Sci-ence Institute.Six male beagle dogs(10kg,10months old) were subjected to fasting overnight before the experiment. Each dog was administered either one capsule of the ref-erence(Avodart®,0.5mg as dutasteride)or one tablet of DuγCD-PS(F5)(0.5mg as dutasteride),followed by10ml of water.Blood samples were taken from the cephalic vein and collected(3ml)into heparinized tubes at0,0.5,1,2,4,8,12,24, and48h after the administration.The plasma was obtained316Asian Journal of Pharmaceutical Sciences14(2019)313–320Table1–Aqueous solubility of dutasteride complexed with various cyclodextrins at a1:50weight ratio and the average binding affinity as obtained by the computer docking simulation tool Glide(Schrödinger,New York,USA).Cyclodextrin Solubility(μg/m l)∗Average binding affinity( G bind)(kcal/mol)α-cyclodextrin 1.3±0.3−55.14β-cyclodextrin23.8±1.8−89.58γ-cyclodextrin61.8±3.1−98.69HP-β-cyclodextrin25.5±2.0NDND:not determined.∗Each value is the mean±SD(n=3).Table2–Effect of the weight ratio of dutasteride:γ-cyclodextrin(DuγCD)on the aqueous solubility of dutas-teride.Weight Ratio(Dutasteride:γ-Cyclodextrin)Solubility(μg/m l)∗1:10 5.5±1.21:3024.7±2.01:5061.8±3.11:7093.9±2.2∗Each value is the mean±SD(n=3).by centrifuging the samples at3000rpm for5min and stored at−70°C until analysis.The wash-out period between treat-ments was4weeks.The treatment of the plasma samples and the LC/MS/MS analysis conditions were the same as that used above for the rat study.The C m ax and T m ax were determined from the experimental data.The calculated dutasteride con-centrations were used to obtain the area under the plasma concentration-time profile from time zero to the last concen-tration time point(A UC0-t)by the linear trapezoidal method. Statistical analysis was performed with the unpaired t-test where appropriate.Significance was set at P<0.05.All data were presented as mean±standard deviation.3.Results and discussion3.1.Effect of cyclodextrin complex on the aqueous solubility of dutasterideTable1presents the aqueous solubility of dutasteride when complexed with various cyclodextrins at a1:50weight ratio, together with their binding affinity obtained by the computer docking simulation tool Glide(Schrödinger,New York,USA). Among the CDs tested,theγ-CD complex resulted in the high-est aqueous solubility of dutasteride and showed the lowest binding affinity value,indicating stable complex formation. Thus,γ-CD complexes with various weight ratios(1:10–1:70) of DuγCD were prepared,and the aqueous solubility of du-tasteride was determined.The aqueous solubility of dutas-teride increased up to a1:70weight ratio(T able2),and this value was thus selected for further evaluation.It is interest-ing to note that the solubility of dutasteride synergistically increased with the addition of a solubilizing polymer at a0.4 weight ratio(i.e.,PVP and PEG)and a surfactant(i.e.,Gelu-cire,TPGS and Poloxamer)to the DuγCD complex(dutasteride:Table3–Effect of the solubilizing polymer and surfactant on the aqueous solubility of dutasteride(μg/m l)added to the DuγCD(1:70)complex at weight ratios of0.4and1.0, respectively.Complex Polymer Surfactant Solubility(μg/m l)∗DuγCD(1:70)––93.9±2.2PVP–118.4±3.3Gelucire147.0±4.0TPGS138.7±1.2Poloxamer134.1±1.7PEG–109.6±2.2Gelucire127.0±3.7TPGS118.6±0.9Poloxamer139.7±2.0∗Each value is the mean±SD(n=3).γ-cyclodextrin=1:70)(T able3).The highest solubility of du-tasteride achieved with the addition of the0.4weight ratio of PVP and Gelucire was147μg/ml,which is1.5times higher than the solubility of DuγCD(1:70)(93μg/ml).In a previous re-port,the highest solubility of dutasteride was only47.1μg/ml when dutasteride was complexed with HP-β-CD and HPMC at a weight ratio of1:26.6:13.3[22].Moreover,the study prepared the complex by the supercritical fluid manufacturing method, which is environmentally friendly but not widely equipped in pharmaceutical companies.Thus,it is notable that DuγCD-PS prepared by the simple drying method achieved an aque-ous solubility of dutasteride that was higher than the reported solubility.Based on the preliminary solubility study,DuγCD-PS com-plexes were further optimized by changing the weight ra-tio of dutasteride toγ-CD(1:10–1:70)and surfactant.Table4 presents the composition of DuγCD-PS complexes selected for further evaluation and the aqueous solubility of du-tasteride.When the0.4weight ratio of PVP was selected as a solubilizing polymer,the solubility of dutasteride in-creased up to170μg/ml as the content of the surfactant(Gelu-cire:TPGS=1:1)increased to2weight ratio(F5).These results are consistent with previous reports that the addition of a water-soluble polymer synergistically enhances the solubiliz-ing effect of CDs by preventing drug nucleation and/or crys-tal growth[8].Moreover,it is notable that the surfactant fur-ther increased the solubility of dutasteride,which supports our assumption that surfactants would further enhance theAsian Journal of Pharmaceutical Sciences 14 (2019) 313–320317Fig. 1 –Mean plasma concentration-time profiles of dutasteride after oral administration of the Du γCD-PS complex at a dose of 2.39 mg/kg of dutasteride in rats ( n = 4–6). Each point and vertical bar represent the mean and standard deviation, respectively.Table 4 –Composition of Du γCD-PS complexes and the aqueous solubility of dutasteride.Rx Composition (weight ratio)Solubility( μg / m l ) ∗Dutasteride γ- CD Polymer a SurfactantF1 110 0.4 0.4 b 33.8 ±1.5 F2 1 30 0.4 0.4 b 97.3 ±3.1 F3 1 50 0.4 0.4 b 104.5 ±3.0 F4 1 50 0.4 2 c 118.9 ±3.4 F51700.42 c170.6 ±4.9a Polymer: PVP bGelucire c Gelucire/TPGS (1:1) ∗Each value is the mean ±SD (n = 3).drug solubility by solubilizing the free drug dissociated from the drug-CD complex.3.2. Pharmacokinetic study of Du γCD-PS complex in ratsThe plasma concentration profiles of dutasteride after oral ad-ministration of Avodart ®or the Du γCD-PS complex at a doseof 2.39 mg/kg of dutasteride in rats are presented in Fig. 1 , and the pharmacokinetic parameters are summarized in Table 5 . Du γCD-PS complexes (F1) with 10 and 0.4 weight ratios of γCD and surfactant, respectively, resulted in only 29.6% relative BAcompared to that of the reference (Avodart ®). However, whenthe weight ratio of γCD increased to 30 and 50 (F2 and F3, respectively), the relative BA of dutasteride increased up to 74% of the reference. Moreover, the addition of surfactant at a weight ratio of 2 (F4 and F5) further increased the relative BA up to 93.6% of the reference.For BCS class II drugs including dutasteride, improving the aqueous solubility is the most practical strategy to increase itsoral bioavailability by enhancing the dissolution of the drugin the gastrointestinal (GI) tract [23] . As the solubility of du- tasteride increased by increasing the drug to γ-CD weight ra- tio and by adding surfactant ( T able 4 ), the relative BA of du- tasteride increased proportionally ( T able 5 ). In addition to the solubilizing effect of γ-CD, surfactant appears to synergisti- cally enhance the bioavailability (F3 vs . F4) by inhibiting pre- cipitation and solubilizing the free drug dissociated from the CD complex, as we assumed. However, it is interesting to note that the increase in the γ-CD weight ratio up to 70 (F5) could not further increase the relative BA of dutasteride, despite its higher solubility than F4 formulation. It is known that γ-CD solubilizes poorly water-soluble drugs by inclusion of insol- uble drug into its hydrophobic cavity and formation of γ-CD aggregates [15] . However, the drug could additionally be em- bedded among γ-CD aggregates at a high CD ratio, resulting in supersaturation of the drug. The drug is easily released by the dissociation of γ-CD aggregates (by dilution in the gastroin- testinal fluid and/or by the ring opening of γ-CD with the at- tack of digestive enzyme), after which the drug may be precip- itated. Surfactant might not be able to sufficiently inhibit the precipitation of supersaturated dutasteride in F5 in vivo ; thus, the higher solubility of dutasteride compared to F4 could not proportionally increase the bioavailability.3.3. Characterization of dutasteride and γ-cyclodextrin complexesSurface morphology of dutasteride observed by the FESEM was irregular in shape, while γCD was a parallelogram shape. However, the morphology of complexes was similar to an aggregate (Fig. S2). In FTIR study, characteristic peaks ofdutasteride in the range of 1650–1700 cm−1 (carbonyl stretch- ing), 1600 cm −1 (N –H bend) were markedly decreased in γ- C Dcomplexes (Fig. S3). DSC and pXRD are useful techniques to318Asian Journal of Pharmaceutical Sciences 14 (2019) 313–320Table 5 –Pharmacokinetic parameters of dutasteride after oral administration of the reference (Avodart ®) or Du γCD-PScomplex at a dose of 2.39 mg/kg of dutasteride in rats.RxT m ax (h) C m ax (ng/ml) AUC 0-24h (ng ·h/ml) Relative BA% (to the reference) Reference (Avodart ®) 10.4 ±7.8 253.4 ±22.84336.9 ±497.4–F1 12.0 ±8.0 63.7 ±23.5 1282.4 ±334.9 29.6 F2 8.9 ±9.0 148.8 ±31.9 3147.3 ±689.1 72.6 F3 10.4 ±7.8 170.6 ±43.4 3228.2 ±459.9 74.4 F4 3.0 ±1.2 215.2 ±51.3 4061.1 ±588.9 93.6 F511.0 ±8.9195.8 ±21.34060.2 ±295.393.6Each value is the mean ±SD (n = 4–6).Fig. 2 –DSC thermograms of the (A) Du γCD complexes and (B) Du γCD-PS complexes.Fig. 3 –Powder X-ray diffraction pattern of the Du γCD-PS complexes.determine the occurrence of inclusion of drug crystals. The thermograms of dutasteride and the complexes are presented in Fig. 2 A . Dutasteride showed a very sharp endothermic peak at 251 °C, which corresponds to its melting temperature. It is notable that the endothermic peak of dutasteride was almost negligible when the weight ratio of γCD was higher than 1:30 in the Du γCD complexes. Moreover, as shown in Fig. 2 B , the endothermic peak of dutasteride completely disappeared in Du γCD-PS complexes (F3, F4 and F5) containing solubilizing polymer ( i .e ., PVP) and surfactant ( i .e ., Gelucire and TPGS), indicating that dutasteride is present in an amorphous form in Du γCD-PS complexes. Moreover, the pXRD results of the Du γCD-PS complexes were consistent with those of DSC and did not exhibit the specific pattern for dutasteride crystal ( F ig. 3 ). Because both F4 and F5 formulations could achievehigh bioavailability (93.6%) compared to the reference, theywere selected for preparing the tablet formulation.3.4. Dissolution study of Du γCD-PS tabletFig. 4 presents the in vitro dissolution profiles of dutasteridefrom the tablets of Du γCD-PS complexes (F4 and F5) coatedwith HPMC-based Opadry®, which were compared with that of the reference (Avodart®, soft gelatin capsule). In the Tier I method ( F ig. 4 A ), dissolution of F5 was more rapid than that of F4 and the reference for the first 15 min. However, both F4 and F5 tablets showed a complete release of dutasteride within 45 min, which is similar to the reference. Notably, du- tasteride was not dissolved for the first 25 min until SLS was added in the Tier II method ( F ig. 4 B ), indicating the importanceAsian Journal of Pharmaceutical Sciences 14 (2019) 313–320319Fig. 4 –In vitro dissolution profiles of dutasteride from the reference soft gelatin capsule (Avodart®) and the film-coated tablets of Du γCD-PS complexes determined following the USP dissolution method (A) Tier I and (B) Tier II by using apparatus 2. Each point and vertical bar represent the mean and standard deviation, respectively ( n = 3).Table 6 –Pharmacokinetic parameters of the reference or F5 tablet after oral administration in beagle dogs ( n = 6, crossover study).Composition T m ax (h) C m ax (ng/ml) AUC 0–24 h (ng ·h/ml) Relative BA% (to the reference) Reference 1.7 ±0.567.3 ±17.9 1964.7 ±546.1 –F5 1.2 ±0.7 61.2 ±16.9 1815.6 ±532.4 92.4 P -valueN/A0.59900.5593–N/A: Not assessedof surfactants in the release medium to mimic the physiologi- cal condition. Moreover, it was previously reported that poorly water-soluble drugs can be solubilized in the gastrointestinal tract by endogenous surfactants including bile acids, bile salts and lecithin [24] .Dutasteride is classified as a BCS class II drug, which im- plies that it is highly membrane permeable and lipophilic with a log P value of 5.09. Its terminal elimination half-life is known to be very long (3–5 weeks) at steady-state in humans [21] . Thus, rapid initial dissolution of dutasteride from the tablet followed by gastrointestinal absorption would be critical to achieve a similar pharmacokinetic profile after oral adminis- tration. Based on the in vitro dissolution study ( F ig. 4 A ), the F5 tablet was selected for the in vivo animal study.3.5. Pharmacokinetic study of Du γCD-PS tablet in beagledogsFig. 5 shows the plasma concentration profiles of dutasterideafter oral administration of Avodart ®or the tablet of Du γCD-PS complexes (F5) in beagle dogs. Their pharmacokinetic pa- rameters summarized in Table 6 indicate that the C m ax and AUC t values were not significantly different ( P > 0.05). Notably, the T m ax value of F5 was shorter than that of the reference, which is consistent with the in vitro dissolution study ( F ig. 4 ). Moreover, the relative bioavailability of F5 was 92.4% of that of the reference. Thus, further investigation would be necessaryFig. 5 –Mean plasma concentration-time profiles ofdutasteride after oral administration of the reference softgelatin capsule (Avodart®) or the F5 tablet in beagle dogs ( n = 6, crossover). Each point and vertical bar represent the mean and standard deviation, respectively.with a larger number of animals and/or humans to evaluate the bioequivalence of the F5 tablet to the reference soft cap- sule, considering the highly variable plasma concentration of dutasteride (CV = 47%) [25] .。