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ANSIC78-21-1 IEC 灯具外形标准

ANSIC78-21-1 IEC 灯具外形标准

ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplements American National StandardApproved October 30, 2003 Secretariat: ANSLG - National Electrical Manufacturers AssociationFor Electric Lamps—PAR and R Shapes An American National Standard implies a consensus of those substantially concerned with its scope and provisions. It is intended as a guide to aid the manufacturer, the consumer, and the general public. The existence of an American National Standard does not in any respect preclude anyone, whether he has approved the standard or not, from manufacturing, marketing, purchasing, or using products, processes, or procedures not conforming to the standards. Users are cautioned to obtain the latest editions.The American National Standards Institute does not develop standards and will in no circumstances give an interpretation of any American National Standard. Moreover, no person shall have the right or authority to issue an interpretation of an American National Standard in the name of the American National Standards Institute.CAUTION NOTICE: This American National Standard may be revised or withdrawn at any time. The procedures of the American National Standards Institute require that action be taken periodically to reaffirm, revise, or withdraw this standard. Purchasers of American National Standards may receive current information on all standards by calling or writing the American National Standards Institute.Copyright © 2003 by American National Standard Lighting Group—NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 22209ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplementsi i AmericanNationalStandardApproval of an American National Standard requires verification by ANSI thatthe requirements for due process, consensus, and other criteria for approvalhave been met by the standards developer. An American National Standardimplies a consensus of those substantially concerned with its scope andprovisions. Consensus is established when, in the judgment of the ANSIBoard of Standards Review, substantial agreement has been reached bydirectly, and materially affected interests. Substantial agreement meansmuch more than a simple majority, but not necessarily unanimity.Consensus requires that all views and objections be considered, and that aconcerted effort be made toward their resolution.The existence of an American National Standard does not in any respectpreclude anyone, whether s/he has approved the standard or not, frommanufacturing, marketing, purchasing, or using products, processes, orprocedures not conforming to the standards. It is intended as a guide to aidthe manufacturer, the consumer, and the general public.The American National Standards Institute does not develop standards andwill in no circumstances give an interpretation of any American NationalStandard. Moreover, no person shall have the right or authority to issue aninterpretation of an American National Standard in the name of the AmericanNational Standards Institute. Requests for interpretations should beaddressed to the secretariat or sponsor whose name appears on this titlepage.CAUTION NOTICE: This American National Standard may be revised orwithdrawn at any time. The procedures of the American National StandardsInstitute require that action be taken periodically to reaffirm, revise, orwithdraw this standard. Purchasers of American National Standards mayreceive current information on all standards by calling or writing the AmericanNational Standards Institute.Printed and distributed by:Information Handling Services/Global Engineering Documents15 Inverness Way East, Englewood, CO 80112-5776Under Contract with National Electrical Manufacturers Association Copyright Ó 2003 by American National Standard Lighting Group In Affiliation with National Electrical Manufacturers AssociationAll rights reserved.No part of this publication may be reproduced in any form,in an electronic retrieval system or otherwise, withoutprior written permission of the publisher.Printed in the United States of AmericaCopyright © 2003 by American National Standard Lighting Group- NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 22209ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplementsiiiTable of ContentsForeword………………………………………………………………………………………………………ivPart I General Information11 Scope……………………………………………………………………………………………12 Normative References………………………………………………………………………..13 Definitions and abbreviations.……………………………………………….………………24 Lamp designations……………………………………………………………………………25 Bulb designations………………………………………………………………………………26 Bulb finish………………………………………………………………………………………37 Beam photometry and classification…………………………………………………………38 Lamp drawings……………………………………………………….………………………...39 Electrical characteristics……………………………………………………………………..410 Requirements…………………………………………………………………………………..411 Information on luminaire design.…………………………………………………………….4Part II Lamp Classes7 Table 1 Standard Lamp Classes with PAR and R Bulbs……………………………………………9Part III Lamp Space Drawings15 Part IV Product Drawings35 Annexes41 Annex AInformative References………………………………..………………………………………43Copyright © 2003 by National Electrical Manufacturers Association 1300 North 17th Street, Suite 1847, Rosslyn VA 22209Second Edition(Date)ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplementsForeword(This Foreword is not part of ANSI C78.21-2003.)Suggestions for improvement of this standard should be submitted to the Secretariat C78, American National Standard Lighting Group, 1300 North 17th Street, Suite 1847, Rosslyn VA 22209.This standard was processed and approved by Accredited Standards Committee on Electric Lamps, C78, and its Working Group, C78 WG-1 for Incandescent, Photo, and Stage-Studio Lamps. Committee approval of the standard does not necessarily imply that all committee members voted for that approval.i vCopyright © 2003 by American National Standard Lighting Group- NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 22209ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplements American National StandardPART I General Information1 ScopeThis standard provides physical and electrical characteristics of the group of incandescent lamps that have PAR and R bulb shapes. Lamps with clear, frosted, and lens end bulbs and with clear and prescription lenses and with various reflector coatings are covered. Lamps covered in this standard may contain either of two basic types of light sources; an incandescent filament or a tungsten halogen inner bulb. Sunlamps and heat lamps of the R type are included. Lamps with discharge arc tubes are not included.Other groups of incandescent lamps are covered in the following associated standards:ANSI C78.20-2003, American National Standard for Incandescent Lamps - A, G, PS and Similar Shapes with E26 Medium Screw BasesANSI C78.22-1995, American National Standard for Incandescent Lamps - A, G, PS and Similar Shapes with E39 Mogul Screw BasesANSI C78.23-1995, American National Standard for Incandescent Lamps - Miscellaneous TypesAt the time of issuance of this standard there was no comparable standard published by the International Electrotechnical Commission (IEC).2 Normative referencesThe following standards contain provisions, which through reference in this text constitute provisions of this American National Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this American National Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below.ANSI C78.30-1997, Procedure for Use in Preparation of Incandescent Lamp Space DrawingsANSI/IEC C78.60360-2002, Standard Method of Measurement of Lamp Cap Temperature Rise ANSI/IEC C78.60432:1-2002, Incandescent Lamps - Safety Specifications - Tungsten Filament Lamps for Domestic and Similar General Lighting Purposes - Part 1ANSI/IEC C78.60432:2-2002, Incandescent Lamps - Safety Specifications - Tungsten Halogen Lamps for Domestic and Similar General Lighting Purposes - Part 2ANSI C78.379-1994, Method for the Classification of the Beam Patterns of Reflector LampsANSI C79.1-2002, Nomenclature for Glass Bulbs Intended for Use with Electric LampsANSI C81.61-1990 (R1996), Electrical Lamp BasesANSI C81.63-1991 (R1996), Gauges for Electrical Bases and Lampholders1 Copyright © 2003 by American National Standard Lighting Group – NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 22209ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplementsIESNA LM-20-1994, IESNA Approved Method for Photometric Testing of Reflector-type LampsIESNA LM-45-2000, IESNA Approved Method for Electrical and Photometric Measurements of General Service Incandescent Filament LampsIESNA LM-54-1999, IES Guide to Lamp SeasoningDrawings contained herein are not drawn to scale3 Definitions and abbreviationsIn addition to bulb and base codes that are defined in the referenced standards, some terms common to the industry are utilized in this standard and used in Table 1.3.1 MOL (Maximum Overall Length): Distance along the lamp axis from eyelet solder to top or face of bulb.3.2 LCL (Light Center Length): Distance from the reference plane (eyelet solder for screw bases) to the center of the light-emitting filament of the lamp.3.3 Class: A grouping of like lamps having the same rated wattage, bulb shape, base, MOL, and bulb finish, including two or more voltage ratings within a voltage range. Each line item in Table 1 is a class.3.4 Voltage range: A series of rated voltages related to commonly available supply lines. A footnote to Table 1 lists several common voltage ranges that apply to classes of lamps in this standard.3.5 Rated wattage: Wattage marked on lamp. See IESNA LM-45 for measurement of wattage.3.6 Rated voltage: The voltage marked on the lamp. If lamps are marked with a range voltage it shall be interpreted that they are appropriate for use on any line voltage within that range. Consult manufacturer’s catalog to determine design voltage.3.7 Base temperature rise: The surface temperature rise above ambient temperature of a standard test lampholder fitted to the lamp, when measured according to the standard method. Maximum base temperature rise limits apply to base-up burn position at which maximum temperature rise occurs unless lamps are restricted to other burn positions by their manufacturers. See ANSI/IEC C78.60360 for method of measurement.3.8 Service: The field of most common application for a given lighting source. Service indicated in this standard is not necessarily the only application. “Spotlight" and "floodlight” are generic terms only used to describe either spot or flood light service.4 Lamp designationsThis standard does not place any control over lamp designations. Incandescent reflector lamps are generally designated by wattage, bulb type, and voltage ratings. Additional codes may be applied by lamp manufacturers. See lamp manufacturers’ catalogs for more detailed information.5 Bulb designationsBulb designations used in this standard are defined in ANSI C79.1 and used in Table 1. Since the traditional eighth-inch sizes have long been utilized in some lamp designations, they are so used in this standard. The metric equivalents are shown in parentheses.2Copyright © 2003 by American National Standard Lighting Group - NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 22209ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplements Certain bulbs are noted in Table 1 with "BR" and “ER” designations, which are used by most manufacturers. These are the same as "RB" and "RE" bulb designations in ANSI C79.1.PAR is a designation that means “parabolic aluminized reflector” mostly applied to pressed hard glass, two-part (lens and reflector) reflector lamps. Some R-lamps are also made with hard glass, so noted in Table 1. PAR16 compact reflector lamps made with ceramic enclosures are also listed. Other R-lamps are made with soft glass, and soft glass is implied unless otherwise noted.Bulb finish6.1 ReflectorBulbs used in PAR and R lamps usually have an internal metallic coating on the reflector section of the bulb for directing a light beam out through the lens. Sometimes dichroic coatings are used in the reflector section of the bulb, for selective transmission of infrared energy through that area.6.2 LensOnly those R lamps with clear, inside-frosted, and lens end lens sections are considered in this standard unless otherwise noted. Similarly, PAR lamps with clear lenses, stippled patterns, or molded prescriptions are considered. Colored coatings are not covered unless specifically noted. Beam photometry and classificationSee IESNA LM-20 for method of photometry testing of reflector lamps. See ANSI C78.379 for information on classification of beam patterns.Lamp Drawings8.1 Lamp space drawings in Part IIIFor each bulb-base-MOL category, lamp space drawings in Part III of this standard show the maximum limits of the space that may be occupied by any part of the bulb. A typical bulb shape is shown as a dashed line within that maximum space. The space shown shall accommodate the longest and shortest lamps with maximum bowl and neck diameters and maximum bulb eccentricity. These drawings were prepared in accordance with the lamp space drawing procedures in ANSI C78.30.The following general conditions apply to the construction of these space drawings:a. Straight lines are used as much as possible to simplify the space outlines. All compromiseswith the actual space are in excess of the actual space required.b. All excursions of a lamp bulb are shown relative to a fixed-position base.c. Bulb eccentricity with respect to the base axis is a combination of allowances for angular tilt (skewness) and lateral displacement (true eccentricity). An eccentricity angle of 3 degrees applies generally to incandescent lamps unless special applications require tighter limits.d. The base contact-making gauge for each type of base controls the space near the rim of the base in the base-to-neck transition zone.e. All dimensions are in millimeters unless otherwise specified.3 Copyright © 2003 by American National Standard Lighting Group – NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 22209ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplementsf. Most figure numbers shown in the figures and in Table 1 relate directly to old American National Standards for that category. For instance, Figure C78.21-254 is derived from the superseded Standard, ANSI C78.254-1966.8.2 Product drawings in Part IVA different situation occurs with those lamps that are not held in place by the base to lampholder fit. These rim-mounted PAR lamps are held in place at a seating plane on the bulb, and the terminals provide only electrical continuity, not mechanical stability for the entire lamp. Drawings of such lamps are product drawings and not lamp space drawings. They define the dimensions of finished lamps. Their positions and space requirements are determined by the rim-holding devices of their luminaires.9 Electrical characteristicsThe values of lamp voltage, current, and wattage shown in Part II are those nominal values that apply after the lamps have been seasoned. See IESNA LM-54 for guidelines on lamp seasoning.10 Requirements10.1 Screw bases and special gauges shall be as described in ANSI C81.61 and C81.63.10.2 Individual lamps shall satisfy limits for MOL that apply to their class as shown in Table 1.10.3 All finished lamps shall have controlled dimensions, bulb size, and eccentricity such that they occupy a space within dimensions shown in the appropriate lamp space drawing in Part III.10.4 Finished lamps of the rim-mounted type shall comply with the dimensions shown in the product drawings in Part IV.10.5 The average base temperature rise of samples of a lamp of any specific rated voltage shall not be greater than the limit shown for the lamp class in Table 1.10.6 See ANSI/IEC C78.60432:1 for other safety requirements for tungsten filament reflector lamps, and see ANSI/IEC C78.60432:2 for other safety requirements for tungsten halogen reflector lamps.11 Information for luminaire designCertain lamp types listed in Table 1 have characteristics, which restrict their applications. In addition, lamp manufacturers may have issued caution notices or instructions that indicate restrictions in the application of PAR and R lamps. Observe the following information and the manufacturers' notices.11.1 Burning positionCertain incandescent lamps are designed for operating only in specific burning positions, and misapplication could cause overheating.11.2 Lampholder temperatureSome of the lamps specified in Table 1 can exhibit base temperatures that are high enough to cause deterioration or damage to some lampholder materials. Those lamps should be used only in lampholders or connectors designed to withstand higher temperatures.4Copyright © 2003 by American National Standard Lighting Group - NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 22209ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplements 11.3 Base temperatureThe lamp manufacturers may provide information that some lamps specified in Table 1, when used in certain luminaires, could generate enough heat to weaken the lamps’ basing cement, even when the lampholders can withstand the heat. Those lamps shall be used only in luminaires designed to maintain the proper temperature of the bases.11.4 Bulb temperatureSome lamps covered by this standard operate at such high bulb temperatures that contact between the bulb and a foreign object could shatter the bulb. Avoid such contacts.11.5 Heat in beamSome lamps covered by this standard emit sufficient heat in their beam patterns to damage materials close by that are flammable or susceptible to heat damage. Avoid lamp operation near such materials.11.6 Moist conditionsMetal parts of certain PAR and R lamps may become a shock hazard when moisture is present. De-energize the circuits before touching these lamps.11.7 Protective screenUse of a protective screen to protect persons may be advisable for some lamps.11.8 ShieldingTungsten halogen inner bulbs operate at high temperature and internal gas pressure above atmospheric pressure. Consequently, a bulb could shatter. Certain lamps may also emit some amount of ultraviolet radiation. Therefore, a suitable protective shield, screening technique, or both shall be used with the luminaire to protect people and surroundings from both hazards.An integral outer envelope, surrounding a tungsten halogen inner bulb, may satisfy this shielding requirement. See the lamp manufacturers instructions.11.9 Accessory equipmentCertain lamps may not perform satisfactorily if accessory equipment or parts of a luminaire are attached to or touch them.11.10 Exposure limitationDue to the amount of energy emitted by certain lamps, such as sunlamps, the times of exposure of persons working near them may have to be limited.11.11 ProtectionMany of the lamps covered in this standard have hard glass bulbs and can withstand the outdoor environment. Others, due to higher wattage input and hotter bulb temperature, cannot be used outdoors without additional protection provided by an appropriate luminaire.11.12 Special luminairesLamps of the cool-beam type are suitable for use only in luminaires specifically designed for those lamps.5 Copyright © 2003 by American National Standard Lighting Group – NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 22209ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplementsTHIS PAGEINTENTIONALLYLEFT BLANK 6Copyright © 2003 by American National Standard Lighting Group - NEMA 1300 North 17th Street, Suite 1847, Rosslyn VA 22209ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplementsPART II - Lamp Classes7 Copyright © 2003 by American National Standard Lighting Group – NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 22209ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplementsTHIS PAGEINTENTIONALLYLEFT BLANK 8Copyright © 2003 by American National Standard Lighting Group - NEMA 1300 North 17th Street, Suite 1847, Rosslyn VA 22209ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplementsPART III - Lamp Space Drawings15 Copyright © 2003 by American National Standard Lighting Group - NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 22209ANSI C78.21-2003Revision of ANSI C78.21-1995 with all supplementsTHIS PAGEINTENTIONALLYLEFT BLANK 16Copyright © 2003 by American National Standard Lighting Group - NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 22209Bulb: R40(R127)Base: Special Skirted Medium Screw, E26/53x39Overall Length: 187.3 (7-3/8 in.) max171.5 (6-3/4 in.) minEccentricity: 3O maximumAll dimensions are millimeters unless otherwise specified.Figure C78.21-23617 Copyright © 2003 by American National Standard Lighting Group - NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 22209Bulb: BR40(R127) Base: Medium Screw, E26/24Overall Length: 166.7 (6-9/16 in.) max150.8 (5-15/16 in.) min Eccentricity: 3O maximumAll dimensions are in millimeters unless otherwise specified.Figure C78.21-23718Copyright © 2003 by American National Standard Lighting Group - NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 2220919Copyright © 2003 by American National Standard Lighting Group - NEMA 1300 North 17th Street, Suite 1847, Rosslyn VA 22209Bulb: PAR38 (PAR121) Base: Skirted Medium Screw, E26/50x39 Overall Length: 135.0 (5-5/16 in.) max127.8 (5-1/32 in.) min Eccentricity: 3OMaximumAll dimensions are millimeters unless otherwise specified.Figure C78.21-238Bulb: R20(R63) Base: Medium Screw, E26/24Overall Length: 100.0 (3 15/16 in.) max90.5 (3-9/16 in.) min Eccentricity: 3O MaximumAll dimensions are millimeters unless otherwise specified.Figure C78.21-254 20Copyright © 2003 by American National Standard Lighting Group - NEMA 1300 North 17th Street, Suite 1847, Rosslyn VA 22209Bulb: R40(R127)Base: Mogul Screw, E39/41Overall Length: 184.2 (7 1/4 in.) max168.3 (6-5/8 in.) minEccentricity: 3O MaximumAll dimensions are millimeters unless otherwise specified.Figure C78.21-25521 Copyright © 2003 by American National Standard Lighting Group - NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 2220922Copyright © 2003 by American National Standard Lighting Group - NEMA 1300 North 17th Street, Suite 1847, Rosslyn VA 22209Bulb: BR40 (BR127) Base: Medium Screw, E26/24 Overall Length: 174.6 (6-7/8 in.) max158.8 (6-1/4 in.) min Eccentricity: 3OMaximumAll dimensions are millimeters unless otherwise specified.Figure C78.21-256Bulb: R40(R127)Base: Special Skirted Medium Screw, E26/53x39Overall Length: 193.7 (7-5/8 in.) max177.8 (7 in.) minEccentricity: 3O MaximumAll dimensions are millimeters unless otherwise specified.Figure C78.21-25723 Copyright © 2003 by American National Standard Lighting Group - NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 2220924Copyright © 2003 by American National Standard Lighting Group - NEMA 1300 North 17th Street, Suite 1847, Rosslyn VA 22209Bulb: R14 (R44) Base: Intermediate Screw, E17/20 Overall Length: 65.1 (2-9/16 in.) max59.0 (2-5/16 in.) min Eccentricity: 3OMaximumAll dimensions are millimeters unless otherwise specified.Figure C78.21-26525Copyright © 2003 by American National Standard Lighting Group - NEMA 1300 North 17th Street, Suite 1847, Rosslyn VA 22209Bulb: BR30 (BR95) Base: Medium Screw, E26/24 Overall Length: 136.5 (5-3/8 in.) max123.8 (4-7/8 in.) min Eccentricity: 3OMaximumAll dimensions are millimeters unless otherwise specified.Figure C78.21-266Bulb: ER30(R95) Base: Medium Screw, E26/24Overall Length: 161.9 (6-3/8 in.) max149.2 (5-7/8 in.) minEccentricity: 3O MaximumAll dimensions are millimeters unless otherwise specified.Figure C78.21-26726Copyright © 2003 by American National Standard Lighting Group - NEMA1300 North 17th Street, Suite 1847, Rosslyn VA 22209Bulb: ER40(R127) Base: Medium Screw, E26/53x39Overall Length: 187.3 (7-3/8 in.) max171.5 (6-3/4 in.) minEccentricity: 3O maximumAll dimensions are millimeters unless otherwise specified.Figure C78.21-268Base: Mogul Screw, E39/41Overall Length: 196.9 (7 3/4 in.) max168.3 (6-5/8 in.) min without protrusion Eccentricity: 3O MaximumNOTES1 This lamp does not have to include an extra dimple on top of the bulb2 All dimensions are millimeters unless otherwise specified.Figure C78.21-269Bulb PAR30 (PAR95) long neckBase E26/24 medium screwMaximum overall length 120.7 (4-3/4 in.)Minimum overall length 109.2 (4-5/16 in.)Eccentricity 3ºmaximum All dimensions are millimeters unless otherwise notedFigure C78.21-275Bulb PAR30 (PAR95) short neck Base E26/24 medium screw Maximum overall length 92.1 (3-5/8 in.)Minimum overall length 82.0 (3-1/4 in.)Eccentricity 3ºmaximum All dimensions are millimeters unless otherwise specified.Figure C78.21-276(PAR63) Bulb PAR20Base E26/24 medium screwMaximum overall length 88.9 (3-1/2 in.)Minimum overall length 73.0 (2-7/8 in.)maximum Eccentricity 3ºAll dimensions are millimeters unless otherwise specified.Figure C78.21-277(BRL121) Bulb BRL38Base E26/24 medium screwMaximum overall length 147.6 (5-13/16 in.)Minimum overall length 134.9 (5-5/16 in.)maximum Eccentricity 3ºAll dimensions are millimeters unless otherwise specified.Figure C78.21-278(PAR51) Bulb PAR16Base E26/24 medium screwMaximum overall length 84.0 (3-5/16 in.)Minimum overall length 69.9 (2-3/4 in.)maximum Eccentricity 3ºNotes: Dimensions are in millimeters unless otherwise notedFigure C78.21-279THIS PAGE INTENTIONALLY LEFT BLANKPART IV - Product DrawingsTHIS PAGE INTENTIONALLY LEFT BLANKBulb: PAR46(PAR146) Base: G12.7 Medium Side ProngMax. Overall Length: 101.6mm (4.0 in)Figure 78.21 – 258Bulb: PAR56(PAR178)End-ProngMogulBase: GX16d/12Max. Overall Length: 127.0mm (5.0 in.)Figure C78.21 - 259(PAR203)Bulb: PAR64End-ProngMogulExtendedBase: GX16d/31Overall Length: 152.4mm (6.0 in.) max.Figure C78.21-263(PAR114) Bulb: PAR36Terminals Base: ScrewMax. Overall Length: 69.9mm (2.75 in)Figure C78.21-264ANNEXESTHIS PAGE INTENTIONALLY LEFT BLANKAnnex AInformative ReferencesANSI C81.62-1991, Lampholders for Electric LampsANSI/NEMA WD 6-1988, Wiring Devices - Dimensional RequirementsANSI/UL 153-2002, Underwriters Laboratories Inc. Standard for Safety - Portable Electric Luminaires UL 496-1996, Underwriters Laboratories Inc. Standard for Safety - Edison Base LampholdersUL 817-2001, Underwriters Laboratories Inc. Standard for Safety - Cord Sets and Power Supply Cords UL 1598-2000, Underwriters Laboratories Inc. Standard for Safety - Luminaires。

英文文献-溶胶-凝胶法制备LiFePO4改进其电化学性能

英文文献-溶胶-凝胶法制备LiFePO4改进其电化学性能

Electrochimica Acta 92 (2013) 248–256Contents lists available at SciVerse ScienceDirectElectrochimicaActaj o u r n a l h o m e p a g e :w w w.e l s e v i e r.c o m /l o c a t e /e l e c t a c taGel-combustion synthesis of LiFePO 4/C composite with improved capacity retention in aerated aqueous electrolyte solutionMilica Vujkovi´c a ,Ivana Stojkovi´c a ,Nikola Cvjeti´canin a ,Slavko Mentus a ,b ,∗,1a University of Belgrade,Faculty of Physical Chemistry,P.O.Box 137,Studentski trg 12-16,11158Belgrade,Serbia bThe Serbian Academy of Sciences and Arts,Kenz Mihajlova 35,11158Belgrade,Serbiaa r t i c l ei n f oArticle history:Received 2October 2012Received in revised form 3January 2013Accepted 5January 2013Available online 11 January 2013Keywords:Aqueous rechargeable Li-ion battery Galvanostatic cycling Gel-combustion Olivine LiFePO 4LiFePeO 4/C compositea b s t r a c tThe LiFePO 4/C composite containing 13.4wt.%of carbon was synthesized by combustion of a metal salt–(glycine +malonic acid)gel,followed by an isothermal heat-treatment of combustion product at 750◦C in reducing atmosphere.By a brief test in 1M LiClO 4–propylene carbonate solution at a rate of C/10,the discharge capacity was proven to be equal to the theoretical one.In aqueous LiNO 3solu-tion equilibrated with air,at a rate C/3,initial discharge capacity of 106mAh g −1was measured,being among the highest ones observed for various Li-ion intercalation materials in aqueous solutions.In addition,significant prolongation of cycle life was achieved,illustrated by the fact that upon 120charg-ing/discharging cycles at various rates,the capacity remained as high as 80%of initial value.The chemical diffusion coefficient of lithium in this composite was measured by cyclic voltammetry.The obtained val-ues were compared to the existing literature data,and the reasons of high scatter of reported values were considered.© 2013 Elsevier Ltd. All rights reserved.1.IntroductionThanks to its high theoretical Coulombic capacity (170mAh g −1)and environmental friendliness,LiFePO 4olivine became a desir-able cathodic material of Li-ion batteries [1,2],competitive to other commercially used cathodic materials (LiMnO 4,LiCoO 2).As evidenced in non-aqueous electrolyte solutions,a small vol-ume change (6.81%)that accompanies the phase transition LiFePO 4 FePO 4enables Li +ion insertion/deinsertion reactions to be quite reversible [1–3].The problem of low rate capability,caused by low electronic conductivity [4,5],was shown to be solv-able to some extent by reduction of mean particle size [6].Further improvements in both conductivity and electrochemical perform-ances were achieved by forming composite LiFePO 4/C,where in situ produced carbon served as an electronically conducting con-stituent [5,7–27].Ordinarily,both in situ formed carbon and carbon black additive,became unavoidable constituent of the LiFePO 4-based electrode materials [28–37].Zhao et al.[27]reported that Fe 2P may arise as an undesirable product during the synthesis of LiFePO 4/C composite under reducing conditions,however,other authors found later that this compound may contribute positively∗Corresponding author at:University of Belgrade,Faculty of Physical Chemistry,P.O.Box 137,Studentski trg 12-16,11158Belgrade,Serbia.Tel.:+381112187133;fax:+381112187133.E-mail address:slavko@ffh.bg.ac.rs (S.Mentus).1ISE member.to the electronic conductivity and improve the electrochemical per-formance of the composite [28–30].Severe improvement in rate capability and capacity retention was achieved by partial replace-ment of iron by metals supervalent relative to lithium [31–37].Thus one may conclude that the main aspects of practical applica-bility of LiFePO 4in Li-ion batteries with organic electrolytes were successively resolved.After the pioneering studies by Li and Dahn [38,39],recharge-able Li-ion batteries with aqueous electrolytes (ARLB)attracted considerable attention [40–50].The first versions of ARLB’s,suf-fered of very low Coulombic utilization and significantly more pronounced capacity fade relative to the batteries with organic electrolyte,regardless on the type of electrode materials [43].For the first time,LiFePO 4was considered as a cathode material in ARLB’s by Manickam et al.in 2006[44].He et al.[46],in an aqueous 0.5M Li 2SO 4solution,found that LiFePO 4displayed both a surprisingly high initial capacity of 140mAh g −1at a rate 1C and recognizable voltage plateau at a rate as high as 20C,which was superior relative to the other electrode materials in ARLB’s.Recently,the same authors reported a high capacity decay in aer-ated electrolyte solution,amounting to 37%after only 10cycles [48].In the same study,they demonstrated qualitatively by a brief cyclovoltammetric test,that a carbon layer deposited from a vapor phase over LiFePO 4particles,suppressed the capacity fade [48].Inspired by the recent discoveries about excellent rate capa-bility [46]but short cycle life [48]of LiFePO 4in aerated aqueous solution,we attempted to prolong the cycle life by means of protecting carbon layer over the LiFePO 4particles.Therefore we0013-4686/$–see front matter © 2013 Elsevier Ltd. All rights reserved./10.1016/j.electacta.2013.01.030M.Vujkovi´c et al./Electrochimica Acta92 (2013) 248–256249synthesized LiFePO4/C composite by a fast and simple glycine-nitrate gel-combustion technique.This method,although simpler than a classic solid state reaction method combined with ball milling[44,48],was rarely used for LiFePO4synthesis[19,27].It yielded a porous,foamy LiFePO4/C composite,easily accessible to the electrolyte.Upon the fair charging/discharging performance was confirmed by a brief test in organic electrolyte,we examined in detail the electrochemical behavior of this material in aqueous electrolyte,by cyclic voltammetry,complex impedance and cyclic galvanostatic charging/discharging methods.In comparison to pure LiFePO4studied in Ref.[48],this composite displayed markedly longer cycle life in aerated aqueous solutions.The chemical dif-fusion coefficient of lithium was also determined,and the reasons of its remarkable scatter in the existing literature were considered.2.ExperimentalThe LiFePO4/C composite was synthesized using lithium nitrate, ammonium dihydrogen phosphate(Merck)and iron(II)oxalate dihydrate(synthesized according to the procedure described else-where[51])as raw materials.Our group acquired the experience in this synthesis technique on the examples of spinels LiMn2O4 [52]and LiCr0.15Mn1.85O4[53],where glycine served as both fuel and complexing/gelling agent to the metal ions.A stoichiometric amount of each material was dissolved in deionized water and mixed at80◦C using a magnetic stirrer.Then,first glycine was added into the reaction mixture to provide the mole ratio of glycine: nitrate of2:1,and additionally,malonic acid(Merck)was added in an amount of60wt.%of the expected mass of LiFePO4.The role of malonic acid was to decelerate combustion and provide con-trollable excess of carbon[14].After removing majority of water by evaporation,the gelled precursor was heated to initiate the auto-combustion,resulting in aflocculent product.The combustion product was heated in a quartz tube furnacefirst at400◦C for3h in Ar stream,and then at750◦C for6h,under a stream of5vol.%H2in Ar.This treatment consolidated the olivine structure and enabled to complete the carbonization of residual organic matter.The VO2powder prepared by hydrothermal method was used as an active component of the counter electrode in the galvanostatic experiments in aqueous electrolyte solution.The details of the syn-thesis and electrochemical behavior of VO2are described elsewhere [54,55].The considerable stoichiometric excess of VO2was used,to provide that the LiFePO4/C composite only presents the main resis-tive element,i.e.,determines the behavior of the assembled cell on the whole.The XRD experiment was performed using Philips1050diffrac-tometer.The Cu K␣1,2radiation in15–70◦2Ârange,with0.05◦C step and2s exposition time was used.The carbon content in the composite was determined by its com-bustion in theflowing air atmosphere,by means of thermobalance TA SDT Model2090,at a heating rate of10◦C min−1.The morphology of the synthesized compounds was observed using the scanning electron microscope JSM-6610LV.For electrochemical investigations,the working electrode was made from LiFePO4/C composite(75%),carbon black-Vulcan XC72 (Cabot Corp.)(20%),poly(vinylidenefluoride)(PVDF)binder(5%) and a N-methyl-2-pyrrolidone solvent.The resulting suspension was homogenized in an ultrasonic bath and deposited on electron-ically conducting support.The electrode was dried at120◦C for 4h.Somewhat modified weight ratio,85:10:5,and the same drying procedure,were used to prepare VO2electrode.The non-aqueous electrolyte was1M LiClO4(Lithium Corpo-ration of America)dissolved in propylene carbonate(PC)(Fluka). Before than dissolved,LiClO4was dried over night at140◦C under vacuum.The aqueous electrolyte solution was saturated LiNO3solution.The cyclic voltammetry and complex impedance experiments were carried out only for aqueous electrolyte solutions,by means of the device Gamry PCI4/300Potentiostat/Galvanostat.The three electrode cell consisted of a working electrode,a wide platinum foil as a counter electrode,and a saturated calomel electrode(SCE) as a reference one.The experiments were carried out in air atmo-sphere.The impedance was measured in open-circuit conditions, at various stages of charging and discharging,within the frequency range10−2−105Hz,with7points per decade.Galvanostatic charging/discharging experiments were carried out in a two-electrode arrangement,by means of the battery testing device Arbin BT-2042,with two-terminal connectors only.In the galvanostatic tests in non-aqueous solution,working electrode was a2×2cm2platinum foil carrying2.3mg of compos-ite electrode material(1.5mg of olivine),while counter electrode was a2×2cm2lithium foil.The cell was assembled in an argon-filled glove box and cycled galvanostatically within a voltage range 2.1–4.2V.The galvanostatic tests in the aqueous electrolyte solution were carried out in a two-electrode arrangement,involving3mg of cathodic material,as a working electrode,and VO2in a multi-ple stoichiometric excess,as a counter electrode.According to its reversible potential of lithiation/delithiation reaction[55],VO2per-formed as an anode in this cell.The4cm2stainless steel plates were used as the current collectors for both positive and negative electrode.The cell was assembled in room atmosphere,and cycled within the voltage window between0.01and1.4V.3.Result and discussion3.1.The XRD,SEM and TG analysis of the LiFePO4/C compositeFig.1shows the XRD patterns of the composite LiFePO4/C pre-pared according to the procedure described in the Experimental Section.As visible,the diffractogram agrees completely with the one of pure LiFePO4olivine,found in the JCPDS card No.725-19. The narrow diffraction lines indicate complete crystallization and relatively large particle dimensions.On the basis of absence of diffraction lines of carbon,we may conclude that the carbonized product was amorphous one.Fig.2shows the SEM images of the LiFePO4/C composite at two different magnifications.Theflaky agglomerates,Fig.2left,with apparently smooth surface and low tap density,are due to a partial liquefaction and evolution of gas bubbles during gel-combustion procedure.These agglomerates consist of small LiFePO4/CFig.1.XRD patterns of LiFePO4/C composite in comparison to standard crystallo-graphic data.250M.Vujkovi´c et al./Electrochimica Acta 92 (2013) 248–256Fig.2.SEM images of LiFePO 4/C composite at two different magnification,20000×and 100000×.composite particles visible better at higher magnification,Fig.2,ly at the magnification of 100,000×,one may see that the size of majority of composite particles was in the range 50–100nm.The mean particle diameter,2r,as per SEM microphotograph amounted to 75nm.This analysis evidences that the gel-combustion method may provide nanodisprsed particles,desirable from the point of view of rate capability.For instance,Fey et al.[16]demonstrated that particle size reduction from 476to 205nm improved the rate capa-bility of LiFePO 4/C composite in organic electrolyte,illustrated by the increase of discharge capacity from 80mAh g −1to 140mAh g −1at discharging rate 1C.Also,carbon matrix prevented particles from agglomeration providing narrow size distribution,contrary to often used solid state reaction method of synthesis,when sintering of ini-tially nanometer sized particles caused the appearance of micron sized agglomerates [22].The SEM microphotograph (Fig.2)alone did not permit to rec-ognize carbon constituent of the LiFePO 4/C composite.However,carbonized product was evidenced,and its content measured,by means of thermogravimetry,as described elsewhere [9].The dia-gram of simultaneous thermogravimetry and differential thermal analysis (TG/DTA)of the LiFePO 4/C composite performed in air is presented in Fig.3.The process of moisture release,causing a slight mass loss of 1%,terminated at 150◦C.In the temperature range 350–500◦C carbon combustion took place,visible as a drop of the TG curve and an accompanying exothermic peak of the DTA curve.However,the early stage of olivine oxidation merged to some extent with the late stage of carbon combustion,and therefore,the minimum of the TG curve,appearing at nearly 500◦C,was not so low as to enable to read directly the carbon content.Fortunately,as proven by XRD analysis,the oxidation of LiFePO 4at tempera-ture exceeding 600◦C,yielded only Li 3Fe 2(PO 4)3and Fe 2O 3,whatFig.3.TGA/DTA curve of LiFePO 4/C under air flow at heating rate of 10C min−1.corresponded to the relative gain in mass of exactly 5.07%[9].Therefore,the weight percentage of carbonaceous fraction in the LiFePO 4/C composite was determined as equal to the difference between the TG plateaus at temperatures 300and 650◦C,aug-mented for 5.07%.According to this calculation the carbon fraction amounted to 13.4wt.%,and by means of this value,the electro-chemical parameters discussed in the next sections were correlated to pure LiFePO 4.Specific surface area of LiFePO 4,required for the measurement of diffusion constant,was determined from SEM image (Fig.2).Assuming a spherical particle shape and accepting mean particle radius r =37.5nm,the specific surface area was estimated on the basis of equation [17,22,45,46]:S =3rd(1)where the bulk density d =3.6g cm −3was used .This calculation resulted in the value S =22.2m 2g −1.In this calculation the contri-bution of carbon to the mean particle radius was ignored,however the error introduced in such way is more acceptable than the error which may arise if standard BET method were applied to the com-posite with significant carbon ly,due to a usually very developed surface area of carbon,the measured specific sur-face may exceed many times the actual surface area of LiFePO 4.3.2.Electrochemical measurements3.2.1.Non-aqueous electrolyte solutionIn order to compare the behavior of the synthesized LiFePO 4/C composite to the existing literature data,available predominantly for non-aqueous solutions,a brief test was performed in non-aqueous 1M LiClO 4+propylene carbonate solution by galvano-static experiments only.The results for the rates C/10,C/3and C,within the voltage limits 2.1–4.2V,were presented in Fig.4.The polarizability of the lithium electrode was estimated on the basis of the study by Churikov [56–67],who measured the current–voltage curves of pure lithium electrode in LiClO 4/propylene carbon-ate solutions at various temperatures.To the highest rate of 1C =170mA g −1in nonaqueous electrolyte,the corresponding cur-rent amounted to 0.25mA,which was equal to the current density of 0.064mA cm −2through the Li counter electrode.According to Fig.2in Ref.[67],for room temperature,the corresponding over-voltage amounted to only 6mV.Since lithium electrode is thus practically non-polarizable in this system,the voltages presented on the ordinate of the left diagram are the potentials of the olivine electrode expressed versus Li/Li +reference electrode.The clear charge and discharge plateaus at about 3.49V and 3.40V,respec-tively,correspond to the LiFePO 4 FePO 4phase equilibria [5].At discharging rate of C/10,the initial discharge capacity,within the limits of experimental error,was close to a full theoreticalM.Vujkovi´c et al./Electrochimica Acta 92 (2013) 248–256251Fig.4.The initial charge/discharge curves (a)and cyclic performance (b)of LiFePO 4/C composite in 1M LiClO 4+PC at different rates within a common cut-off voltage of2.1–4.2V.Fig.5.Charge/discharge profile and corresponding cyclic behavior of LiFePO 4/C in 1M LiClO 4+PC at the rate of 1C.capacity of LiFePO 4(170mAh g −1).This value is higher than that for LiFePO 4/C composite obtained by glycine [19],malonic acid [14]and adipic acid/ball milling [15]assisted methods.As usual,the discharge capacity decreased with increasing discharging rate (Fig.4b),and amounted to 127mAh g −1at C/3,and 109mAh g −1at 1C.For practical application of Li-ion batteries,a satisfactory rate capability and long cycle life are of primary importance.The charge/discharge profiles and dependence of capacity on the cycle number at the rate 1C are presented in Fig.5.The capacity was almost independent on the number of cycles,similarly to theearlier reports by Fey et al.[37–39].For comparison,Kalaiselvi et al.[19],by a glycine assisted gel-combustion procedure,with an additional amount (2wt.%)of carbon black,produced a similar nanoporous LiFePO 4/C composite displaying somewhat poorer per-formance,i.e.,smaller discharge capacity of 160mAh g −1at smaller discharging rate of C/20.On the other hand,better rate capability of LiFePO 4/C com-posite,containing only 1.1–1.8wt.%of carbon,in a non-aqueous solution,was reported by Liu et al.[21].For instance they mea-sured 160mAh g −1at the rate 1C,and 110at even 30C [21].This may be due to a thinner carbon layer around the LiFePO 4olivine particles.However the advantage of here applied thicker carbon layer exposed itself in aqueous electrolyte solutions,as described in the next section.3.2.2.Aqueous electrolyte solution3.2.2.1.Cyclic voltammetry.By the cyclic voltammetry method (CV)the electrochemical behavior of LiFePO 4/C composite in satu-rated aqueous LiNO 3solution was preliminary tested in the voltage range 0.4–1V versus SCE.The cyclic voltammograms are pre-sented in Fig.6.The highest scan rate of 100mV s −1,tolerated by this material,was much higher than the ones (0.01–5mV s −1)used in previous studies in both organic [13,24,25]and aqueous electrolyte solutions [47,48].Since one deals here with the thin layer solid redox electrode,limited in both charge consumption and diffusion length,the voltammogram is more complicated for interpretation comparing with the classic case of electroactive species in a liquid solution.A sharp,almost linear rise of current upon achieving reversible potential,with overlapped rising parts at various scan rates,similar to ones reported elsewhere [21,25],resembles closely the voltammogram of anodic dissolution ofaFig.6.Cyclic voltammograms of LiFePO 4/C in saturated LiNO 3aqueous electrolyte with a scan rate of 1mV s −1(left)and at various scan rates in the range 1–100mV s −1.252M.Vujkovi´c et al./Electrochimica Acta 92 (2013) 248–256Fig.7.Anodic and cathodic peak current versus square root of scan rate forLiFePO 4/C composite in aqueous LiNO 3electrolyte solution.thin metal layer [56],which proceeds under constant reactant activity.Since the solid/solid phase transitions LiFePO 4 FePO 4accompanies the redox processes in this system [5,8,57,58],the positive scan of the voltammograms depict the phase transition of LiFePO 4to FePO 4,while the negative scan depicts the phase transi-tion FePO 4to LiFePO 4.As shown by Srinivasan et al.[5],LiFePO 4may be exhausted by Li not more than 5mol.%before to trans-form into FePO 4,while FePO 4may consume no more than 5%Li before to transform into LiFePO 4,i.e.cyclic voltammetry exper-iments proceeds under condition of almost constant activity of the electroactive species.Although these aspects of the Li inser-tion/deinsertion process do not fit the processes at metal/liquid electrolyte boundary implied by Randles–Sevcik equation:i p =0.4463F RT1/2C v 1/2AD 1/2(2)this equation was frequently used to estimate apparent diffusion coefficient in Li insertion processes [5,17,21,46,59].To obtain peak current,i p ,in amperes,the concentration of lithium,C =C Li ,should be in mol cm −3,the real surface area exposed to the electrolyte in cm 2,chemical diffusion coefficient of lithium through the solid phase,D =D Li ,in cm 2s −1,and sweep rate,v ,in V s −1.The Eq.(2)pre-dicts the dependence of the peak height on the square root of sweep rate to be linear,as found often in Li-ion intercalation processes [17,21,25,59,60].This condition is fulfilled in this case too,as shown in Fig.7.The average value of C Li may be estimated as a reciprocal value of molar volume of LiFePO 4(V M =44.11cm 3mol −1),hence C Li =2.27×10−2mol cm −3.The determination of the actual surface area of olivine is a more difficult task,due to the presence of carbon in the LiFePO 4/C ly,classical BET method of sur-face area measurement may lead to a significantly overestimated value,since carbon surface may be very developed and participate predominantly in the measured value [15].Thus the authors in this field usually calculated specific surface area by means of Eq.(1),using mean particle radius determined by means of electron microscopy [17,22,45,46].Using S =22.2m 2g −1determined by means of Eq.(1),and an actual mass of the electroactive substance applied to the elec-trode surface (0.001305g),the actual electrode surface area was calculated to amount to A =290cm 2.This value introduced in Randles–Sevcik equation yielded D Li ∼0.8×10−14cm 2s −1.From the aspect of capacity retention,the insolubility of olivine in aqueous solutions is advantageous compared to the vanadia-based Li-ion intercalation materials,such as Li 1.2V 3O 8[61],LiV 3O 8[62]and V 2O 5[63],the solubility of which in LiNO 3solution was perceivable through the yellowish solutioncoloration.Fig.8.The Nyquist plots of LiFePO 4/C composite in aqueous LiNO 3solution at var-ious stages of delithiation;inset:enlarged high-frequency region.3.2.2.2.Impedance measurements.Figs.8and 9present the Nyquist plots of the LiFePO 4/C composite in aqueous LiNO 3solution at various open circuit potentials (OCV),during delithiation (anodic sweep,Fig.8)and during lithiation (cathodic sweep,Fig.9).The delithiated phase,observed at OCV =1V,as well as the lithi-ated phase,observed at OCV =0V,in the low-frequency region (f <100Hz)tend to behave like a capacitor,characteristic of a surface thin-layered redox material with reflective phase bound-ary conditions [64].At the OCV not too far from the reversible one (0.42V during delithiation,0.308V during lithiation),where both LiFePO 4and FePO 4phase may be present,within the whole 10−2–105Hz frequency range,the reaction behaves as a reversible one (i.e.shows the impedance of almost purely Warburg type).The insets in Figs.8and 9present the enlarged parts of the impedance diagram in the region of high frequencies,where one may observe a semicircle,the diameter of which corresponds theoretically to the charge transfer resistance.As visible,the change of open circuit potential between 0and 1V,in spite of the phase transition,does not cause significant change in charge transfer resistance.The small charge transfer resistance obtained with the carbon participation of 13.4%,being less than 1 ,is the smallest one reported thus far for olivine based materials.This finding agrees with the trend found by Zhao et al.[27],that the charge transfer resistance scaleddownFig.9.The Nyquist plots of LiFePO 4/C composite in aqueous LiNO 3solution at var-ious stages of lithiation;inset:enlarged high-frequency region.M.Vujkovi´c et al./Electrochimica Acta 92 (2013) 248–256253Fig.10.The dependence Z Re vs.ω−1/2during lithiation at 0.308V (top)and delithi-ation at 0.42V (down)in the frequency range 72–2.68Hz.to 1000,400and 150 when the amount of in situ formed carbon in the LiFePO 4/C composite increased in the range 1,2.8and 4.8%.For OCV corresponding to the cathodic (0.42V)and anodic (0.308V)peak maxima,the Warburg constant W was calculated from the dependence [21]:Z Re =R e +R ct + W ω−1/2(3)In the frequency range 2.7–72Hz,almost purely Warburg impedance was found to hold (i.e.the slope of the Nyquist plot very close to 45degrees was found).At the potential of cathodic current maximum (0.42V),from Fig.10, W was determined to amount to 7.96 s −1/2.At the potential of anodic maxima,0.308V, W was determined to amount to 9.07 s −1/2.In the published literature,for the determination of diffusion coefficient on the basis of impedance measurements,the following equation was often used [66,68,69]:D =0.5V M AF W ıE ıx2(4)where V M is molar volume of olivine,44.1cm 3, W is Warburg con-stant and ıE /ıx is the slope of the dependence of electrode potential on the molar fraction of Li (x )for given value of x .However,the potentials of CV maxima in the here studied case correspond to the x range of two-phase equilibrium,where for an accurate deter-mination of ıE /ıx a strong control of perturbed region of sample particles is required [69],and thus the determination of diffusion coefficients was omitted.3.2.2.3.Galvanostatic measurements.The galvanostatic measure-ments of LiFePO 4/C in saturated LiNO 3aqueous solution were performed in a two-electrode arrangement using hydrother-mally synthesized VO 2[55]as the active material of thecounterFig.11.Capacity versus cycle number and charge/discharge profiles (inset)for thecell consisting of LiFePO 4/C composite as cathode,and VO 2in large excess as anode,in saturated LiNO 3aqueous electrolyte observed at rate C/3.electrode.Preliminary cyclovoltammetric tests of VO 2in saturated LiNO 3solution at the sweep rate 10mV s −1,evidenced excellent cyclability and stable capacity of about 160mAh g −1during at least 50cycles.The voltage applied to the two-electrode cell was cycled within the limits 0and 1.4V.Due to a significant stoichiometric excess of VO 2over LiFePO 4/C composite (5:1)the actual voltage may be considered to be the potential versus reference VO 2/Li x VO 2electrode.Fig.11shows the dependence of the discharging Coulombic capacity of the LiFePO 4/C composite on the number of galvano-static cycles at discharging rate C/3,as well as (in the inset)the voltage vs.charging/discharging degree for 1st,2nd and 50th cycle.The charge/discharge curves do not change substantially in shape upon cycling,indicating stable capacity.For an aqueous solution,a surprisingly high initial discharge capacity of 106mAh g −1and low capacity fade of only 6%after 50charge/discharge cycles were evidenced.This behavior is admirable in comparison to other elec-trode materials in aqueous media reported in literature (LiTi 2(PO 4)3[42],LiV 3O 8[57]),and probably enabled by a higher thermody-namic stability of olivine structure [1].Fig.12presents the results of cyclic galvanostatic investigations of LiFePO 4/C composite in aqueous LiNO 3solution at various dis-charging rates.The charging/discharging rate was initially C/3for 80cycles and then was increased stepwise up to 3C.ThecapacityFig.12.Cyclic performance of LiFePO 4/C in saturated LiNO 3aqueous electrolyte at different charging/discharging rates.。

G34 Standard Test Method(EXCO Test) 腐蚀标准

G34 Standard Test Method(EXCO Test) 腐蚀标准

Designation:G34−01(Reapproved2013)Standard Test Method forExfoliation Corrosion Susceptibility in2XXX and7XXX Series Aluminum Alloys(EXCO Test)1This standard is issued under thefixed designation G34;the number immediately following the designation indicates the year of original adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.A superscript epsilon(´)indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1.Scope1.1This test method covers a procedure for constant im-mersion exfoliation corrosion(EXCO)testing of high-strength 2XXX and7XXX series aluminum alloys.N OTE1—This test method was originally developed for research and development purposes;however,it is referenced,in specific material specifications,as applicable for evaluating production material(refer to Section14on Precision and Bias).1.2This test method applies to all wrought products such as sheet,plate,extrusions,and forgings produced from conven-tional ingot metallurgy process.1.3This test method can be used with any form of specimen or part that can be immersed in the test solution.1.4This standard does not purport to address all of the safety concerns,if any,associated with its use.It is the responsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1ASTM Standards:2D1193Specification for Reagent WaterE3Guide for Preparation of Metallographic SpecimensG15Terminology Relating to Corrosion and Corrosion Test-ing(Withdrawn2010)3G112Guide for Conducting Exfoliation Corrosion Tests in Aluminum Alloys2.2ASTM Adjuncts:Illustrations(Enlarged Glossy Prints)43.Terminology3.1Definitions:3.1.1exfoliation—corrosion that proceeds laterally from the sites of initiation along planes parallel to the surface,generally at grain boundaries,forming corrosion products that force metal away from the body of the material giving rise to a layered appearance(Terminology G15).4.Summary of Test Method4.1This test method provides an accelerated exfoliation corrosion test for2XXX and7XXX series aluminum alloys that involves the continuous immersion of test materials in a solution containing4M sodium chloride,0.5M potassium nitrate,and0.1M nitric acid at2563°C(7765°F).The susceptibility to exfoliation is determined by visual examination,with performance ratings established by refer-ence to standard photographs.5.Significance and Use5.1This test method was originally developed for research and development purposes;however,it is referenced,in specific material specifications,as applicable for evaluating production material(refer to Section14on Precision and Bias).5.2Use of this test method provides a useful prediction of the exfoliation corrosion behavior of these alloys in various types of outdoor service,especially in marine and industrial environments.5The test solution is very corrosive and repre-sents the more severe types of environmental service, excluding,of course,unusual chemicals not likely to be encountered in natural environments.1This test method is under the jurisdiction of ASTM Committee G01on Corrosion of Metals and is the direct responsibility of Subcommittee G01.05on Laboratory Corrosion Tests.Current edition approved May1,2013.Published July2013.Originally approved st previous edition approved in2007as G34–01(2007).DOI:10.1520/G0034-01R13.2For referenced ASTM standards,visit the ASTM website,,or contact ASTM Customer Service at service@.For Annual Book of ASTM Standards volume information,refer to the standard’s Document Summary page on the ASTM website.3The last approved version of this historical standard is referenced on .4Available from ASTM International Headquarters.Order Adjunct No. ADJG003402.Original adjunct produced in1980.5Ketcham,S.J.,and Jeffrey,P.W.,“Exfoliation Corrosion Testing of7178and 7075Aluminum Alloys”(Report of ASTM G01.05Interlaboratory Testing Program in Cooperation with the Aluminum Association);and Sprowls,D.O.,Walsh,J.D., and Shumaker,M. B.,“Simplified Exfoliation Testing of Aluminum Alloys,”Localized Corrosion—Cause of Metal Failure,ASTM STP516,ASTM,1972.Copyright©ASTM International,100Barr Harbor Drive,PO Box C700,West Conshohocken,PA19428-2959.United States5.3The exfoliation ratings were arbitrarily chosen to illus-trate a wide range in resistance to exfoliation in this test.However,it remains to be determined whether correlations can be established between EXCO test ratings and realistic service conditions for a given alloy.It is an ongoing activity of the Task Group on Exfoliation Corrosion of Aluminum Alloys (G01.05.02.08)to maintain outdoor exposure tests for this purpose.For example,it has been reported 6that samples of Al-Zn-Mg-Cu alloys rated EA or P in a 48-h EXCO test did not develop more than a slight amount of incipient exfoliation (EA)during six-to nine-year exposures to seacoast atmospheres,whereas,ED rated materials in most cases developed severe exfoliation within a year in the seacoast atmosphere.It is anticipated that additional comparisons will become available as the outdoor tests are extended.6.Apparatus6.1Any suitable glass,plastic,or similarly inert container can be used to contain the solution and specimens during the period of test.Depending upon the shape and size of the specimens,rods or racks of glass,plastic,or any inert sub-stance shall be used to support the specimen above the bottom of the container.The container should be fitted with a loose-fitting cover to reduce evaporation.7.Reagents7.1Purity of Reagents—The test solution shall be prepared with reagent grade sodium chloride (NaCl),potassium nitrate (KNO 3),and nitric acid (HNO 3).7.2Purity of Water—Distilled or deionized water shall be used to prepare test solution.The water purity must conform to Specification D1193,Type IV reagent water,except that for this method,the values of chloride and sodium can be disregarded.7.3A test solution of the following composition shall be used:NaCl (4.0M )KNO 3(0.5M )HNO 3(0.1M )Dissolve 234g of NaCl,50g of KNO 3in water,and add 6.3mL of concentrated HNO 3(70weight %).Dilute to 1L.This solution has an apparent pH of 0.4.7.4The solution shall be maintained at a temperature of 2563°C (7765°F).8.Sampling8.1Sampling procedures are not considered applicable to this test method,as they are often covered by product specifi-cations.It is assumed that the test specimens are removed from representative samples of materials.9.Test Specimens9.1Specimens may be of any practical size or shape.Nevertheless,for the results to be of most significance a specimen size of at least 50by 100mm (2by 4in.),or the equivalent,is recommended.9.2The edges of sawed specimens need not be machined,but specimens obtained by blanking or shearing shall have edges dressed by machining or filling to a depth equal to the thickness of the specimen to remove cold-worked metal.9.3Remove the cladding of alclad sheet by machining the test surface;remove or mask the cladding on the back side (non-test surface)also.9.4When removing test specimens from extrusions and forgings,take care to avoid specimen locations underneath flanges,ribs,etc.,where the grain structure is usually variable.10.Standardization10.1To provide an indication when some inadvertent de-viation from the correct test conditions occurs,it is necessary to expose to the test at regular intervals a control specimen of a material with known resistance.This control should exhibit the same degree of exfoliation each time it is included in the test.10.2The control may be any material of the alloy type included in the scope of this test method,preferably one with an intermediate degree of susceptibility (Fig.1and Fig.2).11.Procedure11.1Degrease the specimens with a suitable solvent.11.2Mask the back surfaces of the specimens to minimize corrosion of non-test areas.Protective coatings must have good adherence to avoid crevice corrosion beneath the coating;also,they should not contain leachable ions or protective oils that will influence the corrosion of the test surface.(See Figs.1-6.)411.3Use the solution in sufficient quantity to provide a volume-to-metal surface area ratio of 10to 30mL/cm 2(65to 200mL/in.2).Include all exposed metal area in the determina-tion of total surface area.11.4Use fresh solution at the start of each test.Do not change the solution even though the pH increases during the test.It is normal for the pH to increase from the initial apparent value of 0.4to about 3during the first several hours depending upon the amount of corrosion that occurs.11.5Immerse the specimens in the solution using rods or racks of inert material to support the specimens above the bottom of the container.Place the test surface upward in a horizontal position to prevent loss of exfoliated metal from the surface of the specimen.Do not concurrently immerse in the same container alloys containing less than 0.25%copper with those containing greater amounts of copper.11.6The following maximum periods of exposure are recommended for testing the alloy types indicated:2XXX Series 96h 7XXX Series48h6Sprowls,D.O.,Summerson,T.J.,and Loftin,F.E.,“Exfoliation Corrosion Testing of 7075and 7178Aluminum Alloys—Interim Report on Atmospheric Exposure Tests”(Report of ASTM G01.05.02Interlaboratory Testing Program in Cooperation with the Aluminum Association);and Lifka,B.W.and Sprowls,D.O.,“Relationship of Accelerated Test Methods for Exfoliation Resistance in 7XXX Series Aluminum Alloys With Exposure to a Seacoast Atmosphere,”Corrosion in Natural Environments,ASTM STP 558,ASTM,1974.Undermining pitting that may form the surface give the appearance of incipient exfoliation(Keller’s Etch;100×).FIG.1Examples of Pitting CorrosionThe length of time to develop exfoliation in material of a given alloy and temper may vary with the mill product form,with some materials developing severe exfoliation in much shorter periods than those listed.Therefore,inspect test speci-mens in place and rate in accordance with Section 12at periods such as 5,24,48,and 72h,and discontinue the exposure of a specimen when it has developed the most severe exfoliation rating (Fig.6).11.7Rate the performance of test specimens in accordance with Section 12immediately after discontinuation of the exposure while the specimens are still wet or moist,taking into account all loose products of exfoliation lying on the test specimen or on the bottom of the container.11.8Clean exposed test specimens,if desired,by rinsing in water and soaking in concentrated nitric acid after the speci-mens have been inspected and rated.12.Interpretation of Results12.1The following codes and classifications shall be used when reporting the visual rating of corroded specimens:Classification Code No appreciable attack N Pitting PExfoliationEA through ED12.2Descriptions of the various classifications,which are illustrated in Figs.1-6,4are asfollows:Exfoliation resulting from rapid lateral attack of selective boundaries or strata forming wedges of corrosion product that force layers of metal upward giving rise to alayered appearance (Keller’s Etch;100×).FIG.2Four Degrees of Severity of ExfoliationCorrosion12.2.1N—No appreciable attack:Surface may be discol-ored or etched,but no evidence of pitting or exfoliation.12.2.2P—Pitting:Discrete pits,sometimes with a tendency for undermining and slight lifting of metal at the pit edges (Fig.1).12.2.3EA through ED—Exfoliation (Figs.1-6):12.2.3.1Visible separation of the metal into layers mani-fested in various forms,such as blisters,slivers,flakes,fairly continuous sheets,and sometimes granular particles resulting from disintegration of thin layers,depending upon the grain morphology of the sample.Various degrees of exfoliation with increasing penetration and loss of metal are illustrated in Fig.2.Additional examples of the various ratings are shown in Figs.3-6.12.2.3.2The formation of tiny pit-blisters or the dislodge-ment of an extremely thin surface layer of metal after only a few hours of exposure may resemble superficial exfoliation (EA),but can in fact result from undermining pitting.If continued exposure to the recommended periods in 11.6produces more corrosion but no evidence of advancing delamination,metallographic examination (see Guide E3)will be required to determine whether the initial effect wastrulyFIG.3Examples of Exfoliation Rating EA (Superficial):Tiny Blisters,Thin Slivers,Flakes or Powder,with only Slight Separation ofMetalFIG.4Example of Exfoliation Rating EB (Moderate);Notable Layering and Penetration into theMetalexfoliation (Fig.2)or undermining pitting (Fig.1);in the latter case the rating should be P.12.2.3.3When exfoliation occurs in isolated sites,rate the worst localized condition observed.12.3The visual ratings are intended to be finite indications of the resistance to exfoliation,and care should be taken when rating a series of test specimens to compare them with the photographs and captions in Figs.1-6rather than with each other.The final rating of a specimen shall be determined by the poorest classification observed during the exposure.12.3.1When it is difficult to classify a specimen,it is advisable to place it in the category of greater susceptibility.N OTE 2—Enlarged glossy prints of Figs.1-6are available from ASTM International.4These prints are more convenient to use and are of better quality than the reproductions in the printed standard.The user is urged to obtain and use these prints.13.Report13.1The report should contain the following essentialinformation:FIG.5Examples of Exfoliation Rating EC (Severe):Penetration to a Considerable Depth into theMetalFIG.6Examples of Exfoliation Rating ED (Very Severe)(Similar to EC Except for Much Greater Penetration and Loss ofMetal)13.1.1Alloy and temper of the material tested,13.1.2Mill product,section thickness,and the surface tested,including reference to applicable product specification, 13.1.3Sampling procedure if other than that specified in referenced product specification,13.1.4A rating of the test specimens using the codes and classifications in Section12,and13.1.5Notation of any deviation in test procedure from that set forth in preceding paragraphs.13.2Other information that may be desirable for certain types of reports includes:13.2.1Size,type,and number of replicate specimens; method of edge preparation,and13.2.2V olume to surface ratio.14.Precision and Bias14.1Precision:14.1.1The precision of the data from this test method was evaluated by way of an interlaboratory test program using two non-commercial tempers of Alloy7075with different levels of exfoliation corrosion susceptibility.Seven laboratories,includ-ing experienced and inexperienced users,participated in the round robin.The laboratories received rough machined panels, which theyfinish machined,exposed according to the proce-dure in this test method,and rated visually according to the photographs included in this test method.14.1.2The raw data from laboratories is listed in Table1 and plotted in Fig.7.All seven laboratories rated the more susceptible T6X material as having severe or very severe exfoliation corrosion as designated by the ratings EC and ED. However,for the more resistant T7X temper there was no agreement as the visual ratings ranged from pitting only to very severe exfoliation as designated by the ratings P to ED.Fig.7 shows that there was no clustering of the ratings either,they seem to follow a uniform distribution.14.1.2.1The data in Table1show the ratings were repeat-able within laboratories.In each case the same rating was obtained for both panels tested by the individual laboratory.14.1.2.2The reproducibility of ratings among different laboratories is shown most clearly in Fig.7.In addition to the visual ratings,one of the laboratories measured the depth of corrosion using an ultrasonic technique(the laboratories re-ported original panel thickness)and the data showed not only that the two tempers had different amounts of exfoliation,but that there was good consistency within each temper as plotted in Fig.8.Thus the laboratory to laboratory variation in ratings for the T7X material resulted from individual rater’s interpre-tation of the photographs and wording used to define the visual rating system.Samples with resistance,that is,intermediate between highly susceptible and highly resistant samples can be the most difficult to rate visually,which is confirmed by these results.One of the reasons for this is corrosion debris that does not result from exfoliation corrosion as discussed in Guide G112.14.1.2.3Based on the results from this interlaboratory test program,the visual rating system gives consistent ratings for highly susceptible samples,but produces a large amount of laboratory-to-laboratory variaition for tempers with intermedi-ate levels of resistance.Experience indicates that the visual ratings will produce more consistent results for highly resistant samples,such as7075–T73X products,than it does for samples with intermediate resistance,such as T7X tested in this interlaboratry test program.14.2Bias—The procedure in Test Method G34has no bias because the exfoliation rating is defined only in terms of this test method.TABLE1Visual Ratings from Interlaboratory Test of Alloy7075 Plate in Two Noncommercial TempersLaboratoryT6X T7XSpecimen1Specimen2Specimen1Specimen2A ED ED EB EBB EC EC ED EDC EC EC EA EAD EC-ED EC-ED EC ECE ED ED ED EDF EC EC EB EBG EC EC PP FIG.7Histogram of Visual Exfoliation Ratings by Seven Labora-tories for Two Tempers of7075Plate Tested at the T/4Plane FIG.8Histogram of Average Corrosion Depths as Measured by Ultrasonic Inspection for Two Tempers of7075Plate at the T/4Plane15.Keywords15.1exfoliation corrosion;heat treatable aluminum alloys;immersion corrosion test;2XXX aluminum alloys;7XXXaluminum alloysASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this ers of this standard are expressly advised that determination of the validity of any such patent rights,and the riskof infringement of such rights,are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyfive years and if not revised,either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of theresponsible technical committee,which you may attend.If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards,at the address shown below.This standard is copyrighted by ASTM International,100Barr Harbor Drive,PO Box C700,West Conshohocken,PA19428-2959, United States.Individual reprints(single or multiple copies)of this standard may be obtained by contacting ASTM at the aboveaddress or at610-832-9585(phone),610-832-9555(fax),or service@(e-mail);or through the ASTM website().Permission rights to photocopy the standard may also be secured from the ASTM website(/COPYRIGHT/).。

Masoneilan Control Valve Sizing Handbook

Masoneilan Control Valve Sizing Handbook
© 2000 Dresser Industries, Inc. All rights reserved.
Masoneilan
DRESSER
VALVE
DIVISION
2
Foreword
This handbook on control valve sizing is based on the use of nomenclature and sizing equations from ISA Standard S75.01 and IEC Standard 534-2. Additional explanations and supportive information are provided beyond the content of the standards. The sizing equations are based on equations for predicting the flow of compressible and incompressible fluids through control valves. The equations are not intended for use when dense slurries, dry solids or non-Newtonian liquids are encountered. Original equations and methods developed by Masoneilan are included for two-phase flow, multistage flow, and supercritical fluids. Values of numerical factors are included for commonly encountered systems of units. These are United States customary units and metric units for both kilopascal and bar usage. The principal use of the equations is to aid in the selection of an appropriate valve size for a specific application. In this procedure, the numbers in the equations consist of values for the fluid and flow conditions and known values for the selected valve at rated opening. With these factors in the equation, the unknown (or product of the unknowns, e.g., Fp Cv) can be computed. Although these computed numbers are often suitable for selecting a valve from a series of discrete sizes, they do not represent a true operating condition. Some of the factors are for the valve at rated travel, while others relating to the operating conditions are for the partially open valve. Once a valve size has been selected, the remaining unknowns, such as Fp, can be computed and a judgement can be made as to whether the valve size is adequate. It is not usually necessary to carry the calculations further to predict the exact opening. To do this, all the pertinent sizing factors must be known at fractional valve openings. A computer sizing program having this information in a database can perform this Cv

JCR分区

JCR分区

小类名称(英文小类分区大类名称大类分区刊名简称刊名全称ISSN小类名称(中文)PLOS PATHOG P LoS Pathogens1553-7366病毒学VIROLOGY1生物1 REV MED VIRO REVIEWS IN MEDIC1052-9276病毒学VIROLOGY1医学1 ADV VIRUS RE ADVANCES IN VIRU0065-3527病毒学VIROLOGY2医学2 AIDS AIDS0269-9370病毒学VIROLOGY2医学2 ANTIVIR THER ANTIVIRAL THERAP1359-6535病毒学VIROLOGY2医学2J VIROL JOURNAL OF VIROL0022-538X病毒学VIROLOGY2医学2 RETROVIROLOG Retrovirology 1742-4690病毒学VIROLOGY2医学2 ANTIVIR RES A NTIVIRAL RESEAR0166-3542病毒学VIROLOGY3医学2 INFLUENZA OT Influenza and Ot1750-2640病毒学VIROLOGY3医学3INT J MED MI INTERNATIONAL JO1438-4221病毒学VIROLOGY3医学3J CLIN VIROL JOURNAL OF CLINI1386-6532病毒学VIROLOGY3医学2J GEN VIROL J OURNAL OF GENER0022-1317病毒学VIROLOGY3医学3J MED VIROL J OURNAL OF MEDIC0146-6615病毒学VIROLOGY3医学3J VIRAL HEPA JOURNAL OF VIRAL1352-0504病毒学VIROLOGY3医学3 MICROBES INF MICROBES AND INF1286-4579病毒学VIROLOGY3医学3 VIROLOGY VIROLOGY0042-6822病毒学VIROLOGY3医学3 ACTA VIROLACTA VIROLOGICA0001-723X病毒学VIROLOGY4医学4 AIDS RES HUM AIDS RESEARCH AN0889-2229病毒学VIROLOGY4医学4 ARCH VIROLARCHIVES OF VIRO0304-8608病毒学VIROLOGY4医学4 CURR HIV RES CURRENT HIV RESE1570-162X病毒学VIROLOGY4医学3 FOOD ENVIRON Food and Environ1867-0334病毒学VIROLOGY4医学4 FUTURE VIROL Future Virology1746-0794病毒学VIROLOGY4医学4 INDIAN J VIR Indian Journal o0970-2822病毒学VIROLOGY4医学4 INTERVIROLOG INTERVIROLOGY0300-5526病毒学VIROLOGY4医学4J NEUROVIROL JOURNAL OF NEURO1355-0284病毒学VIROLOGY4医学3J VIROL METH JOURNAL OF VIROL0166-0934病毒学VIROLOGY4医学3S AFR J HIV SOUTHERN AFRICAN1608-9693病毒学VIROLOGY4医学4 VIRAL IMMUNO VIRAL IMMUNOLOGY0882-8245病毒学VIROLOGY4医学4 VIROL J Virology Journal1743-422X病毒学VIROLOGY4医学3 VIROLOGIE VIROLOGIE1267-8694病毒学VIROLOGY4医学4 VIRUS GENES V IRUS GENES0920-8569病毒学VIROLOGY4医学4 VIRUS RES VIRUS RESEARCH0168-1702病毒学VIROLOGY4医学3 VIRUSES-BASE Viruses-Basel1999-4915病毒学VIROLOGY4医学4 ACTA NEUROPA ACTA NEUROPATHOL0001-6322病理学PATHOLOGY1医学1AM J PATHOL A MERICAN JOURNAL0002-9440病理学PATHOLOGY1医学2 ANNU REV PAT Annual Review of1553-4006病理学PATHOLOGY1医学1J PATHOL JOURNAL OF PATHO0022-3417病理学PATHOLOGY1医学1AM J SURG PA AMERICAN 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SCIENC4工程技术4 MATERIALWISS MATERIALWISSENSC0933-5137材料科学:综合MATERIALS SCIENC4工程技术4 MATH MECH SO MATHEMATICS AND 1081-2865材料科学:综合MATERIALS SCIENC4工程技术4 MET MATER IN METALS AND MATER1598-9623材料科学:综合MATERIALS SCIENC4工程技术3 METALL MATER METALLURGICAL AN1073-5615材料科学:综合MATERIALS SCIENC4工程技术4 METALLOFIZ N METALLOFIZIKA I 1024-1809材料科学:综合MATERIALS SCIENC4工程技术4 MICRO NANO L Micro & Nano Let1750-0443材料科学:综合MATERIALS SCIENC4工程技术4 MICROELECTRO MICROELECTRONICS1356-5362材料科学:综合MATERIALS SCIENC4工程技术4。

ASTM D 1209-05 S透明液体色度的试验方法(铂钴标度)(英文版)

ASTM D 1209-05 S透明液体色度的试验方法(铂钴标度)(英文版)

Designation:D1209–05Standard Test Method forColor of Clear Liquids(Platinum-Cobalt Scale)1This standard is issued under thefixed designation D1209;the number immediately following the designation indicates the year of original adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.A superscript epsilon(e)indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1.Scope*1.1This test method describes a procedure for the visual measurement of the color of essentially light colored liquids (Note1).It is applicable only to materials in which the color-producing bodies present have light absorption charac-teristics nearly identical with those of the platinum-cobalt color standards used.N OTE1—A procedure for estimating color of darker liquids,described for soluble nitrocellulose base solutions,is given in Guide D365.1.2The values stated in SI units are to be regarded as standard.No other units of measurement are included in this standard.1.3For purposes of determining conformance of an ob-served or a calculated value using this test method to relevant specifications,test result(s)shall be rounded off“to the nearest unit”in the last right-hand digit used in expressing the specification limit,in accordance with the rounding-off method of Practice E29.1.4This standard does not purport to address all of the safety concerns,if any,associated with its use.It is the responsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.For specific hazard statements see Section6.1.5For specific hazard information,see the Material Safety Data Sheet.2.Referenced Documents2.1ASTM Standards:2D156Test Method for Saybolt Color of Petroleum Prod-ucts(Saybolt Chromometer Method)D365Guide for Soluble Nitrocellulose Base SolutionsD1193Specification for Reagent WaterE29Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE202Test Methods for Analysis of Ethylene Glycols and Propylene GlycolsE346Test Methods for Analysis of Methanol3.Significance and Use3.1The property of color of a solvent varies in importance with the application for which it is intended,the amount of color that can be tolerated being dependent on the color characteristics of the material in which it is used.The paint, varnish,and lacquer solvents,or diluents commercially avail-able on today’s market normally have little or no color.The presence or absence of color in such material is an indication of the degree of refinement to which the solvent has been subjected or of the cleanliness of the shipping or storage container in which it is handled,or both.3.2For a number of years the term“water-white”was considered sufficient as a measurement of solvent color. Several expressions for defining“water-white”gradually ap-peared and it became evident that a more precise color standard was needed.This was accomplished in1952with the adoption of Test Method D1209using the platinum-cobalt scale.This test method is similar to the description given in Standard Methods for the Examination of Water and Waste Water3and is referred to by many as“APHA Color.”The preparation of these platinum-cobalt color standards was originally described by A. Hazen in the American Chemical Journal4in which he assigned the number5(parts per ten thousand)to his platinum-cobalt stock solution.Subsequently,in theirfirst edition(1905) of Standard Methods for the Examination of Water,the American Public Health Association,using exactly the same concentration of reagents,assigned the color designation500 (parts per million)which is the same ratio.The parts per million nomenclature is not used since color is not referred directly to a weight relationship.It is therefore recommended that the incorrect term“Hazen Color”should not be used.Also, because it refers primarily to water,the term“APHA Color”is1This test method is under the jurisdiction of ASTM Committee D01on Paint and Related Coatings,Materials,and Applications and is the direct responsibility of Subcommittee D01.35on Solvents,Plasticizers,and Chemical Intermediates.Current edition approved May15,2005.Published May2005.Originally approved st previous edition approved in2000as D1209–00.2For referenced ASTM standards,visit the ASTM website,,or contact ASTM Customer Service at service@.For Annual Book of ASTM Standards volume information,refer to the standard’s Document Summary page on the ASTM website.3Standard Methods for the Examination of Water and Waste Water,M.Franson, Ed.,American Public Health Assoc.,14th ed.,1975,p.65.4Hazen,A.,“New Color Standard for Natural Waters,”American Chemical Journal,V ol XIV,1892,p.300–310.*A Summary of Changes section appears at the end of this standard. Copyright©ASTM International,100Barr Harbor Drive,PO Box C700,West Conshohocken,PA19428-2959,United States.undesirable.The recommended nomenclature for referring to the color of organic liquids is “Platinum-Cobalt Color,Test Method D 1209.”3.3The petroleum industry uses the Saybolt colorimeter Test Method D 156for measuring and defining the color of hydrocarbon solvents;however,this system of color measure-ment is not commonly employed outside of the petroleum industry.It has been reported by various sources that a Saybolt color of +25is equivalent to 25in the platinum-cobalt system or to colors produced by masses of potassium dichromate ranging between4.8and5.6mg dissolved in 1L of distilled water.Because of the differences in the spectral characteristics of the several color systems being compared and the subjective manner in which the measurements are made,exact equivalen-cies are difficult to obtain.4.Apparatus4.1Spectrophotometer ,equipped for liquid samples and for measurements in the visible region.N OTE 2—The spectrophotometer used must be clean and in first-class operating condition.The instrument should be calibrated in accordance with the instructions given in the Standards for Checking the Calibration of Spectrophotometers (200to 1000nm).54.2Spectrophotometer Cells ,matched having a 10-mm light path.4.3Color Comparison Tubes —Matched 100-mL,tall-form Nessler tubes,provided with ground-on,optically clear,glass caps.Tubes should be selected so that the height of the 100-mL graduation mark is 275to 295mm above the bottom of the tube.4.4Color Comparator —A color comparator constructed to permit visual comparison of light transmitted through tall-form,100-mL Nessler tubes in the direction of their longitu-dinal axes.The comparator should be constructed so that white light is passed through or reflected off a white glass plate and directed with equal intensity through the tubes,and should be shielded so that no light enters the tubes from the side.65.Reagents5.1Purity of Reagents —Reagent grade chemicals shall be used in all tests.Unless otherwise indicated,it is intended that all reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.7Other grades may be used,provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.5.2Purity of Water —Unless otherwise indicated,references to water shall be understood to mean reagent water conforming to Type IV of Specification D 1193.5.3Cobalt Chloride (CoCl 2·6H 2O).5.4Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-chloric acid (HCl).5.5Potassium Chloroplatinate (K 2PtCl 6).6.Platinum-Cobalt Reference Standards6.1Platinum-Cobalt Stock Solution —Dissolve 1.245g of potassium chloroplatinate (K 2PtCl 6)and 1.00g of cobalt chloride (CoCl 2·6H 2O)in water.Carefully add 100mL of hydrochloric acid (HCl,sp gr 1.19)and dilute to 1L with water.The absorbance of the 500platinum-cobalt stock solu-tion in a cell having a 10-mm light path,with reagent water in a matched cell as the reference solution,8must fall within the limits given in Table 1.N OTE 3—This stock solution is commercially available from reputable chemical suppliers.6.2Platinum-Cobalt Standards —From the stock solution,prepare color standards in accordance with Table 2by diluting the required volumes to 100mL with water in the Nessler5See NIST Letter Circular LC-1017.6The sole source of supply of the unit known to the committee at this time is Scientific Glass and Instruments,Inc.,P.O.Box 6,Houston,TX 77001.If you are aware of alternative suppliers,please provide this information to ASTM Interna-tional Headquarters.Your comments will receive careful consideration at a meeting of the responsible technical committee,1which you may attend.7Reagent Chemicals,American Chemical Society Specifications ,American Chemical Society,Washington,DC.For suggestions on the testing of reagents not listed by the American Chemical Society,see Analar Standards for Laboratory Chemicals ,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeia and National Formulary ,U.S.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.8See the manufacturer’s instruction manual for complete details for operating the spectrophotometer.TABLE 1Absorbance Tolerance Limits For No.500Platinum-Cobalt Stock SolutionWavelength,nmAbsorbance 4300.110to 0.1204550.130to 0.1454800.105to 0.1205100.055to 0.065TABLE 2Platinum-Cobalt Color StandardsColor StandardNumberStock Solution,mLColor StandardNumberStock Solution,mL517014102100201531503020420040255250503063006035735070408400805010450906012500100AAThis is platinum-cobalt color No.10in Guide D 365.TABLE 3Platinum-Cobalt Color Standards for Very Light ColorsColor StandardNumberStock Solution,mLColor StandardNumberStock Solution,mL10.209 1.8020.4010 2.0030.6011 2.2040.8012 2.405 1.0013 2.606 1.2014 2.807 1.40153.0081.60tubes.Cap the tubes and seal the caps with shellac or a waterproof cement.When properly sealed and stored,these standards are stable for at least 1year and do not degrade markedly for 2years.96.2.1For a more precise measurement of light colors below 15platinum-cobalt,prepare color standards from the stock solution in accordance with Table 3by diluting the required volumes to 100mL with water in the Nessler e a semi-microburet for measuring the required amount of stock solution.7.Procedure7.1Introduce 100mL of specimen into a Nessler tube,passing the specimen through a filter if it has any visible turbidity.Cap the tube,place in the comparator,and compare with the standards.8.Report8.1Report as the color the number of the standard that most nearly matches the specimen.In the event that the color lies midway between two standards,report the darker of the two.8.2If,owing to differences in hue between the specimen and the standards,a definite match cannot be obtained,report the range over which an apparent match is obtained,and report the material as “off-hue.”9.Precision9.1Color Samples with Pt-Co Color Greater than 2510:9.1.1These precision statements are based upon an inter-laboratory study in which six platinum-cobalt standards having values of 25,75,170,265,385,and 475were prepared in accordance with the instructions given in Section 6of this test method and were given coded labels.These solutions were tested by one analyst in each of ten different laboratories making a single observation on one day and then repeating theobservation on a second day.The analysts were requested to estimate the color to the nearest one unit for solutions below 40platinum-cobalt,to the nearest five units for solutions between 40and 100platinum-cobalt and to the nearest ten units for solutions above 100platinum-cobalt.Based on the results of this interlaboratory study,the following criteria,calculated according to RR-D02-1007,should be used for judging the acceptability of results at the 95%confidence level when the results are obtained under optimum conditions where the hue of the sample matches exactly the hue of the standards.Poor precision will be obtained in varying degrees as the hue of the sample departs from that of the standards.9.1.1.1Repeatability —Two results,obtained by the same analyst should be considered suspect if they differ by more than:r =0.027(X +92)platinum-cobalt unitswhere X is the average of the two results.9.1.1.2Reproducibility —Two results,obtained by analysts in different laboratories,should be considered suspect if they differ by more than:R =0.087(X +92)platinum-cobalt units where X is the average of the two results.9.1.1.3Table 4shows precision values for samples with Pt-Co Color of greater than 25.9.2Color Samples with Pt-Co Color Less than 2511:9.2.1The results of two interlaboratory studies were pooled to give precision values calculated according to RR-D02-1007.One study of glycols included 4samples and 7laboratories;the other study included 5samples and 6laboratories.Based on the pooled repeatability and reproducibility standard deviations,the following criteria should be used for judging,at the 95%confidence level,the acceptability of results obtained on samples with less than 25Pt-Co Color.9.2.1.1Reapeatability —Two results,each the mean of du-plicates,obtained by the same operator on different days should be considered suspect if they differ by more than two platinum-colbalt units.9.2.1.2Reproducibility —Two results,each the mean of duplicates,obtained by operators in different laboratories,should be considered suspect of they differ by more than seven platinum-cobalt units.9.3Bias —The test procedure has no bias because the value of the test result is defined only in terms of the test method.10.Keywords10.1clear liquids;color;platinum-cobalt color scale9Scharf,W.W.,Ferber,K.H.,and White,R.G.,“Stability of Platinum-Cobalt Color Standards,”Materials Research and Standards ,V ol 6,No.6,June 1966,pp.302–304.10Supporting data are available from ASTM International Headquarters.Request RR:D01-1024and RR:D02-1007.11These precision statements are based on interlaboratory studies conducted by Committee E-15on Industrial Chemicals on samples of ethylene glycol and methanol as reported in Test Methods E 202,E 346,and research reports RR:E15-28,and D01-1108.TABLE 4Precision Values for Greater than 25Pt-Co ColorColor (Pt-Co units)Repeatability,rReproducibility,R2531075515165722265103138513414751649SUMMARY OF CHANGESCommittee D01.35has identified the location of selected changes to this standard since the last issue (D1209–00)that may impact the use of this standard.(1)Added reference to Practice E29in1.3of the Scope section.(2)Added Practice E29to list of Referenced Documents.(3)Removed self-reference in Section2.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this ers of this standard are expressly advised that determination of the validity of any such patent rights,and the risk of infringement of such rights,are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyfive years and if not revised,either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsible technical committee,which you may attend.If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards,at the address shown below.This standard is copyrighted by ASTM International,100Barr Harbor Drive,PO Box C700,West Conshohocken,PA19428-2959, United States.Individual reprints(single or multiple copies)of this standard may be obtained by contacting ASTM at the above address or at610-832-9585(phone),610-832-9555(fax),or service@(e-mail);or through the ASTM website ().。

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AND SYSTEM SCI0022-0000 2007JCRN670POLYM ENG SCI POLYMER ENGINEERING AND SCIENCE0032-38880142-727X 2007JCRN671INT J HEAT FLUID FL INTERNATIONAL JOURNAL OF HEAT AND1086-4415 2007JCRN672INT J ELECTRON COMM INTERNATIONAL JOURNAL OF ELECTRONI2007JCRN673ENERG CONVERS MANAGE ENERGY CONVERSION AND MANAGEMENT0196-8904 2007JCRN674COMP MATER SCI COMPUTATIONAL MATERIALS SCIENCE0927-02560164-0925 2007JCRN675ACM T PROGR LANG SYS ACM TRANSACTIONS ON PROGRAMMING LA2007JCRN676HYDROMETALLURGY HYDROMETALLURGY0304-386X 2007JCRN677J WATER RES PL-ASCE JOURNAL OF WATER RESOURCES PLANNIN0733-94961521-3323 2007JCRN678IEEE T ADV PACKAGING IEEE TRANSACTIONS ON ADVANCED PACK1226-086X 2007JCRN679J IND ENG CHEM JOURNAL OF INDUSTRIAL AND ENGINEER2007JCRN680COAST ENG COASTAL ENGINEERING0378-3839 2007JCRN681ADAPT BEHAV ADAPTIVE BEHAVIOR1059-71230268-2575 2007JCRN682J CHEM TECHNOL BIOT JOURNAL OF CHEMICAL TECHNOLOGY AND2007JCRN683COMPUT EDUC COMPUTERS & EDUCATION0360-13150965-8564 2007JCRN684TRANSPORT RES A-POL TRANSPORTATION RESEARCH PART A-POL0924-1868 2007JCRN685USER MODEL USER-ADAP USER MODELING AND USER-ADAPTED INT2007JCRN686COMPUT AIDED GEOM D COMPUTER AIDED GEOMETRIC DESIGN0167-8396 2007JCRN687DISTRIB COMPUT DISTRIBUTED COMPUTING0178-2770 2007JCRN688TRIBOL LETT TRIBOLOGY LETTERS1023-8883 2007JCRN689OXID MET OXIDATION OF METALS0030-770X 2007JCRN690J POLYM ENVIRON JOURNAL OF POLYMERS AND THE ENVIRO1566-25431537-1646 2007JCRN691J MICROLITH MICROFAB JOURNAL OF MICROLITHOGRAPHY MICROF2007JCRN692IEEE T CIRCUITS-I IEEE TRANSACTIONS ON CIRCUITS AND1549-8328 2007JCRN693MEAS SCI TECHNOL MEASUREMENT SCIENCE & TECHNOLOGY0957-0233 2007JCRN694J MECH DESIGN JOURNAL OF MECHANICAL DESIGN1050-0472 2007JCRN695COMPUT BIOL MED COMPUTERS IN BIOLOGY AND MEDICINE0010-4825 2007JCRN696DATA KNOWL ENG DATA & KNOWLEDGE ENGINEERING0169-023X 2007JCRN697IEEE T ROBOT IEEE Transactions on Robotics1552-30981468-6996 2007JCRN698SCI TECHNOL ADV MAT SCIENCE AND TECHNOLOGY OF ADVANCED2007JCRN699POWDER TECHNOL POWDER TECHNOLOGY0032-5910 2007JCRN700IMAGE VISION COMPUT IMAGE AND VISION COMPUTING0262-8856 2007JCRN701APPL SOFT COMPUT APPLIED SOFT COMPUTING1568-49461089-3954 2007JCRN702MICROSCALE THERM ENG MICROSCALE THERMOPHYSICAL ENGINEER2007JCRN703ANIM BIOTECHNOL ANIMAL BIOTECHNOLOGY1049-5398 2007JCRN704IEEE SENS J IEEE SENSORS JOURNAL1530-437X2007JCRN705APPL BIOCHEM BIOTECH APPLIED BIOCHEMISTRY AND BIOTECHNO0273-2289 2007JCRN706IEEE T BROADCAST IEEE TRANSACTIONS ON BROADCASTING0018-93160885-8993 2007JCRN707IEEE T POWER ELECTR IEEE TRANSACTIONS ON POWER ELECTRO2007JCRN708INFORMS J COMPUT INFORMS JOURNAL ON COMPUTING1091-98560928-0707 2007JCRN709J SOL-GEL SCI TECHN JOURNAL OF SOL-GEL SCIENCE AND TEC1063-6536 2007JCRN710IEEE T CONTR SYST T IEEE TRANSACTIONS ON CONTROL SYSTE2007JCRN711PROPELL EXPLOS PYROT PROPELLANTS EXPLOSIVES PYROTECHNIC0721-3115 2007JCRN712J FUNCT PROGRAM JOURNAL OF FUNCTIONAL PROGRAMMING0956-79681134-3060 2007JCRN713ARCH COMPUT METHOD E ARCHIVES OF COMPUTATIONAL METHODS0022-3697 2007JCRN714J PHYS CHEM SOLIDS JOURNAL OF PHYSICS AND CHEMISTRY O2007JCRN715BIOTECHNOL LETT BIOTECHNOLOGY LETTERS0141-54920023-432X 2007JCRN716KOVOVE MATER KOVOVE MATERIALY-METALLIC MATERIAL0255-2701 2007JCRN717CHEM ENG PROCESS CHEMICAL ENGINEERING AND PROCESSIN0888-613X 2007JCRN718INT J APPROX REASON INTERNATIONAL JOURNAL OF APPROXIMA2007JCRN719EXP FLUIDS EXPERIMENTS IN FLUIDS0723-48640926-8782 2007JCRN720DISTRIB PARALLEL DAT DISTRIBUTED AND PARALLEL DATABASES1545-598X 2007JCRN721IEEE GEOSCI REMOTE S IEEE Geoscience and Remote Sensing1438-2377 2007JCRN722EUR FOOD RES TECHNOL EUROPEAN FOOD RESEARCH AND TECHNOL2007JCRN723TRANSPORT SCI TRANSPORTATION SCIENCE0041-16551546-2218 2007JCRN724CMC-COMPUT MATER CON CMC-Computers Materials & Continua2007JCRN725J HYDROL ENG JOURNAL OF HYDROLOGIC ENGINEERING1084-06990143-7496 2007JCRN726INT J ADHES ADHES INTERNATIONAL JOURNAL OF ADHESION2007JCRN727J COMPLEXITY JOURNAL OF COMPLEXITY0885-064X1349-4198 2007JCRN728INT J INNOV COMPUT I International Journal of Innovativ2007JCRN729COMBUST THEOR MODEL COMBUSTION THEORY AND MODELLING1364-7830 2007JCRN730B EARTHQ ENG Bulletin of Earthquake Engineering1570-761X 2007JCRN731EXPERT SYST APPL EXPERT SYSTEMS WITH APPLICATIONS0957-41740890-6955 2007JCRN732INT J MACH TOOL MANU INTERNATIONAL JOURNAL OF MACHINE T2007JCRN733J THERM SPRAY TECHN JOURNAL OF THERMAL SPRAY TECHNOLOG1059-9630 2007JCRN734CEREAL CHEM CEREAL CHEMISTRY0009-0352 2007JCRN735ETRI J ETRI JOURNAL1225-6463 2007JCRN736J MICROENCAPSUL JOURNAL OF MICROENCAPSULATION0265-20480278-0046 2007JCRN737IEEE T IND ELECTRON IEEE TRANSACTIONS ON INDUSTRIAL EL1094-3420 2007JCRN738INT J HIGH PERFORM C INTERNATIONAL JOURNAL OF HIGH PERF0888-3270 2007JCRN739MECH SYST SIGNAL PR MECHANICAL SYSTEMS AND SIGNAL PROC1051-8223 2007JCRN740IEEE T APPL SUPERCON IEEE TRANSACTIONS ON APPLIED SUPER2007JCRN741COGN SYST RES Cognitive Systems Research1389-0417 2007JCRN742EARTHQ SPECTRA EARTHQUAKE SPECTRA8755-29300022-5142 2007JCRN743J SCI FOOD AGR JOURNAL OF THE SCIENCE OF FOOD AND2007JCRN744ENERG J ENERGY JOURNAL0195-6574 2007JCRN745INT J FATIGUE INTERNATIONAL JOURNAL OF FATIGUE0142-1123 2007JCRN746FOOD REV INT FOOD REVIEWS INTERNATIONAL8755-9129 2007JCRN747FOOD TECHNOL-CHICAGO FOOD TECHNOLOGY0015-6639 2007JCRN748SENS LETT Sensor Letters1546-198X 2007JCRN749DRY TECHNOL DRYING TECHNOLOGY0737-39370218-8430 2007JCRN750INT J COOP INF SYST INTERNATIONAL JOURNAL OF COOPERATI2007JCRN751J FOOD SCI JOURNAL OF FOOD SCIENCE0022-1147。

USP 通用章节目录

USP29-通用章节指导目录(附录)Guide to General Chapters 通用章节指导目录中此颜色并且带有“***”的为新增内容。

General Requirements for Test and Assays检查与含量分析的一般要求<1>INJECTIONS……2455注射剂<11>USP REFERENCE STANDARDS……2458USP对照品Apparatus for Test and Assays用于检查与含量分析的器具<16>AUTOMATED METHODS OF ANAL YSIS……2491自动化分析方法<21>THERMOMETERS……2497温度计<31>VOLUMETRIC APPARATUS……2497容量器具<41>WEIGHTS AND BALANCES……2499砝码与天平Microbiological Tests 微生物检查法<51>ANTIMICROBIAL EFFECTIVENESS TESTING……2499抗菌剂有效性检查法<55>BIOLOGICAL INDICATORS—RESISTANCE PERFORMANCE TESTS (2501)生物指示剂-耐药性实验<61>MICROBIAL LIMIT TESTS……2503微生物限度检查法<71>STERILITY TESTS……2508无菌检查法Biological tests and assays生物检查法与测定法<81>ANTIBIOTICS—MICROBIAL ASSAYS……2513抗生素-微生物测定<85>BACTERIAL ENDOTOXINS TEST……2521细菌内毒素检查法<87>BIOLOGICAL REACTIVITY TESTS, IN VITRO……2525体外的生物反应性检查法<88>BIOLOGICAL REACTIVITY TESTS, IN VIVO……2526体内的生物反应性检查法<91>CALCIUM PANTOTHENATE ASSAY……2530泛酸钙测定法<111>DESIGN AND ANAL YSIS OF BIOLOGICAL ASSAYS……2531 生物测定法的设计与分析<115>DEXPANTHENOL ASSAY……2543右泛醇(拟胆碱药)测定法<121>INSULIN ASSAYS……2544胰岛素测定法<141>PROTEIN—BIOLOGICAL ADEQUACY TEST……2546蛋白质-生物适应性试验<151>PYROGEN TEST……2546热原检查法<161>TRANSFUSION AND INFUSION ASSEMBLIES AND SIMILAR MEDICAL DEVICES (2547)输血输液用具以及相类似的医疗器械<171>VITAMIN B12 ACTIVITY ASSAY……2548维生素B12活性测定法Chemical Tests and assays化学实验与测定法<181>IDENTIFICATION—ORGANIC NITROGENOUS BASES (2549)鉴别-有机氮碱?<191>IDENTIFICATION TESTS—GENERAL……2550鉴别实验-通用<193>IDENTIFICATION—TETRACYCLINES……2551鉴别-四环素<197>SPECTROPHOTOMETRIC IDENTIFICATION TESTS......2552分光光度计鉴别实验<201>THIN-LAYER CHROMATOGRAPHIC IDENTIFICATION TEST.. (2553)薄层色谱鉴别实验Limit Test 限度检查法<206>ALUMINUM……2554铝<211>ARSENIC……2554砷<221>CHLORIDE AND SULFATE……2555氯和硫<223>DIMETHYLANILINE……2555二甲基苯胺<226>4-EPIANHYDRO-TETRACYCLINE……25564-?-四环素<231>HEA VY METALS……2556重金属<241>IRON……2557铁<251>LEAD……2558铅<261>MERCURY……2558汞<271>READIL Y CARBONIZABLE SUBSTANCES TEST……2560易碳化物检查法<281>RESIDUE ON IGNITION……2560灼烧残渣<291>SELENIUM……2560硒Other Tests and Assays 其它检查法与测定法<301>ACID-NEUTRALIZING CAPACITY……2561酸中和容量<311>ALGINATES ASSAY……2562藻酸盐测定法<331>AMPHETAMINE ASSAY……2562苯丙胺测定法<341> ANTIMICROBIAL AGENTS—CONTENT……2563 抗菌剂-含量<345> Assay for Citric Acid/Citrate and Phosphate……2565 柠檬酸/柠檬酸盐和磷酸盐的测定<351>ASSAY FOR STEROIDS……2565类固醇(甾类化合物)测定法<361> BARBITURATE ASSAY……2565 巴比妥类药物测定法<371>COBALAMIN RADIOTRACER ASSAY……2566钴铵素放射性跟踪剂测定法<381>ELASTOMERIC CLOSURES FOR INJECTIONS……2567 注射剂的弹性密封件<391>EPINEPHRINE ASSAY……2567肾上腺测定法<401>FATS AND FIXED OILS……2568脂肪与混合油<411>FOLIC ACID ASSAY……2571叶酸测定法<425>IODOMETRIC ASSAY—ANTIBIOTICS……2572碘量检查法-抗生素<429>LIGHT DIFFRACTION MEASUREMENT OF PARTICLE SIZE (2572)粒子尺寸的光衍射测量<431>METHOXY DETERMINA TION……2575甲氧基测定法<441>NIACIN OR NIACINAMIDE ASSAY……2576烟酰或烟酰胺测定法<451>NITRITE TITRATION……2578亚硝酸盐滴定<461>NITROGEN DETERMINA TION……2578氮测定法<466>ORDINARY IMPURITIES……2579一般杂质<467>ORGANIC VOLATILE IMPURITIES……2580有机的易挥发杂质<471>OXYGEN FLASK COMBUSTION……2590氧瓶燃烧法<481>RIBOFLAVIN ASSAY……2590核黄素测定法<501>SALTS OF ORGANIC NITROGENOUS BASES……2591有机氮盐<511>SINGLE-STEROID ASSAY……2591单一的类固醇测定法<521>SULFONAMIDES……2592磺胺制剂<531>THIAMINE ASSAY……2593硫胺素测定法<541>TITRIMETRY……2593滴定法<551>ALPHA TOCOPHEROL ASSAY……2596α-维生素E测定法<561>ARTICLES OF BOTANICAL ORIGIN……2596植物起源的药品<563>IDENTIFICATION OF ARTICLES OF BOTANICAL ORIGIN……2603植物药品的鉴别<565>BOTANICAL EXTRACTS……2609植物提取<571>VITAMIN A ASSAY……2611维生素A的测定法<581>VITAMIN D ASSAY……2612维生素D的测定法<591>ZINC DETERMINATION……2616锌的测定法Physical Test and Determinations物理检查与测定法INHALERS, AND DRY POWDER <601>AEROSOLS, NASAL SPRAYS,USP28METERED-DOSEINHALERS……2617气溶胶,鼻用喷雾剂,定量吸入器与干粉吸入器<611>ALCOHOL DETERMINATION……2637乙醇测定法<616>BULK DENSITY AND TAPPED DENSITY……2638堆密度与拍实密度<621>CHROMATOGRAPHY…….2639色谱法<631>COLOR AND ACHROMICITY……2651呈色与消色<641>COMPLETENESS OF SOLUTION……2652完全溶解<643>TOTAL ORGANIC CARBON……2652总有机碳<645>WA TER CONDUCTIVITY……2653水电导率<651>CONGEALING TEMPERA TURE……2654凝点温度<661>CONTAINERS……2655容器<671>CONTAINERS—PERMEATION……2663容器-渗透<691>COTTON……2664棉花<695>CRYSTALLINITY……2665结晶性<696>Crystallinity Determination By Solution Calorimetry……2666 通过溶液量热学测定结晶性<698>DELIVERABLE VOLUME……2667可转移的体积<699>DENSITY OF SOLIDS……2669固体密度<701>DISINTEGRATION……2670崩解时限***<701>Disintegration (Harmonized Chapter, Official April 1,2006)………..2671崩解时限(协调的章节,法定日期,2006.4.1)<711>DISSOLUTION……2673 溶出度***<711>Dissolution (Harmonized Chapter, Official April 1,2006)………..2675 溶出度(协调的章节,法定日期,2006.4.1)<721>DISTILLING RANGE……2682馏程<724>DRUG RELEASE……2682药物释放度***<724>Drug releasee (Harmonized Chapter, Official April 1,2006)………..2690药物释放度(协调的章节,法定日期,2006.4.1)<726>ELECTROPHORESIS……2694电泳<727>CAPILLARY ELECTROPHORESIS……2696毛细管电泳法***<730>Plasma Spectrochemistry….2700 血浆光谱化学<731>LOSS ON DRYING……2704干燥失重<733>LOSS ON IGNITION……2704灼烧失重<736>MASS SPECTROMETRY……2705 质谱<741>MELTING RANGE OR TEMPERATURE……2708熔距或熔点<751>METAL PARTICLES IN OPHTHALMIC OINTMENTS……2709眼用软膏中的金属粒子<755>MINIMUM FILL……2710最低装填量<761>NUCLEAR MAGNETIC RESONANCE……2710核磁共振<771>OPHTHALMIC OINTMENTS……2715眼用软膏<776>OPTICAL MICROSCOPY……2716光学显微镜<781>OPTICAL ROTATION……2718旋光<785>OSMOLALITY AND OSMOLARITY……2718同渗重摩与同渗容摩<786>PARTICLE SIZE DISTRIBUTION ESTIMATION BY ANAL YTICAL SIEVING (2720)通过筛分法估算粒子分布<788>PARTICULATE MATTER IN INJECTIONS……2722注射剂中的颗粒<789>PARTICULATE MATTER IN OPHTHALMIC SOLUTIONS……2729眼用溶液中的颗粒<791>pH (2730)<795>PHARMACEUTICAL COMPOUNDING—NONSTERILE PREPARATIONS (2731)药物混合-非无菌制剂<797>PHARMACEUTICAL COMPOUNDING—STERILE PREPARATIONS (2735)药物混合-无菌制剂<801>POLAROGRAPHY……2752极谱法<811>POWDER FINENESS……2754粉剂细度<821>RADIOACTIVITY……2755放射性<823>RADIOPHARMACEUTICALS FOR POSITRON EMISSION TOMOGRAPHY —COMPOUNDING……2763用于正电子发射断层摄影术的放射性药物<831>REFRACTIVE INDEX……2766折光率<841>SPECIFIC GRA VITY……2766比重<846>SPECIFIC SURFACE AREA……2767 比表面积<851>SPECTROPHOTOMETRY AND LIGHT-SCA TTERING……2770分光光度计与光散射<861>SUTURES—DIAMETER…2775缝线-直径<871>SUTURES—NEEDLE ATTACHMENT……2775缝线-穿孔实验<881>TENSILE STRENGTH…..2776张力<891>THERMAL ANAL YSIS……2776热分析<905>UNIFORMITY OF DOSAGE UNITS……2778制剂单位的含量均匀度<905>UNIFORMITY OF DOSAGE UNITS (Harmonized Chapter, Official April 1,2006)……2780制剂单位的含量均匀度(协调的章节2006.4.1)<911>VISCOSITY……2785粘度<921>WA TER DETERMINA TION……2785水测定法<941>X-RAY DIFFRACTION……2788X光衍射General Information通用信息<1010>ANAL YTICAL DATA—INTERPRETA TION AND TREATMENT (2790)分析数据-解释与处理<1015>AUTOMA TED RADIOCHEMICAL SYNTHESIS APPARATUS (2801)放射性自动合成装置<1031>THE BIOCOMPATIBILITY OF MATERIALS USED IN DRUG CONTAINERS, MEDICAL DEVICES, AND IMPLANTS (2802)用于药物容器、医疗设施和植入剂的材料的生物相容性<1035>BIOLOGICAL INDICATORS FOR STERILIZATION……2811灭菌用生物指示剂<1041>BIOLOGICS……2814生物制剂***<1043>Ancillary Material for Cell, Gene, and Tissue-Engineered Products…….2814 细胞,基因与组织设计产品的辅助材料<1045>BIOTECHNOLOGY-DERIVED ARTICLES……2821生物技术提取产品<1046>CELL AND GENE THERAPY PRODUCTS……2831细胞与基因治疗产品<1047>BIOTECHNOLOGY-DERIVED ARTICLES—TESTS……2858生物技术产品-检查法<1048>QUALITY OF BIOTECHNOLOGICAL PRODUCTS: ANAL YSIS OF THE EXPRESSION CONSTRUCT IN CELLS USED FOR PRODUCTION OF r-DNA DERIVED PROTEIN PRODUCTS1 (2883)生物产品质量:从蛋白质产品中提取的r-DNA产品在细胞中表达结构的分析<1049>QUALITY OF BIOTECHNOLOGICAL PRODUCTS: STABILITY TESTING OF BIOTECHNOLOGICAL/BIOLOGICAL PRODUCTS1 (2884)生物技术产品的质量:生物技术/生物产品的稳定性实验<1050>VIRAL SAFETY EV ALUA TION OF BIOTECHNOLOGY PRODUCTS DERIVED FROM CELL LINES OF HUMAN OR ANIMAL ORIGIN (2887)从人或动物细胞中提取的生物技术产品的病毒安全性评估<1051>CLEANING GLASS APPARATUS……2896玻璃容器的清洗<1061>COLOR—INSTRUMENTAL MEASUREMENT……2896显色-仪器测量***<1065>Ion Chromatography………2898 离子色谱法<1074>EXCIPIENT BIOLOGICAL SAFETY EV ALUA TION GUIDELINES (2900)赋形剂(辅料)生物安全性评估指导<1075>GOOD COMPOUNDING PRACTICES……2903好的混合操作<1078>GOOD MANUFACTURING PRACTICES FOR BULK PHARMACEUTICAL EXCIPIENTS (2906)批药品赋形剂的生产管理规范***<1079>Good Storage and Shipping Practices……2915 良好的贮存与船运规范<1081>GEL STRENGTH OF GELATIN……2920白凝胶的凝胶强度<1086>IMPURITIES IN OFFICIAL ARTICLES……2920药典物品中的杂质<1087>INTRINSIC DISSOLUTION……2923内部的溶出度<1088>IN VITRO AND IN VIVO EV ALUA TION OF DOSAGE FORMS (2924)体内与体外的剂型的评估<1090>IN VIVO BIOEQUIV ALENCE GUIDANCES……29291体内生物等效性指导<1091>LABELING OF INACTIVE INGREDIENTS……2968非活性成分的标示<1101>MEDICINE DROPPER……2969医用滴管<1111>MICROBIOLOGICAL ATTRIBUTES OF NONSTERILE PHARMACEUTICAL PRODUCTS (2969)非无菌药品中的微生物分布<1116>MICROBIOLOGICAL EV ALUA TION OF CLEAN ROOMS AND OTHER CONTROLLED ENVIRONMENTS……2969洁净的房间与其它可控环境的微生物评估<1118>MONITORING DEVICES—TIME, TEMPERATURE, AND HUMIDITY (2976)监控装置-时间、温度与湿度<1119>NEAR-INFRARED SPECTROPHOTOMETRY……2979近红外分光光度测定法***<1120>Raman Spectrophotometry……..2983 Raman分光光度测定法<1121>NOMENCLATURE……2988命名***<1136>Packaging-Unit-of-Use……2989包装-单元使用<1146>PACKAGING PRACTICE—REPACKAGING A SINGLE SOLID ORAL DRUG PRODUCT INTO A UNIT-DOSE CONTAINER……2990 包装操作-将单一固体口服药品产品再包装成单元剂量<1150>PHARMACEUTICAL STABILITY……2994药物稳定性<1151>PHARMACEUTICAL DOSAGE FORMS……2996药物剂型<1160>PHARMACEUTICAL CALCULATIONS IN PRESCRIPTION COMPOUNDING (3006)按处方混合的药物的计算<1171>PHASE-SOLUBILITY ANAL YSIS……3016相溶解分析***<1174>Powder Flow….3017 粉末流动性<1176>PRESCRIPTION BALANCES AND VOLUMETRIC APPARATUS….3020 处方天平与容量器具***<1177>Good Packaging Practices….3021 良好的包装操作***<1178>Good Repackaging Practices….3023 良好的再包装操作<1181>SCANNING ELECTRON MICROSCOPY……3025扫描电子显微镜<1191>STABILITY CONSIDERATIONS IN DISPENSING PRACTICE……3029 分装操作中稳定性考察<1196>PHARMACOPEIAL HARMONIZATION……3031药典的一致性<1207>STERILE PRODUCT PACKAGING—INTEGRITY EV ALUATION (3035)无菌产品包装-完整性评估<1208>STERILITY TESTING—V ALIDATION OF ISOLATOR SYSTEMS (3037)无菌实验-隔离系统的验证<1209>STERILIZATION—CHEMICAL AND PHYSICOCHEMICAL INDICATORS AND INTEGRATORS……3040灭菌-化学与物理化学的指示剂以及二者的综合<1211>STERILIZATION AND STERILITY ASSURANCE OF COMPENDIAL ARTICLES (3041)药典物品中的灭菌与灭菌保证<1216>TABLET FRIABILITY……3046片剂的脆碎度<1221>TEASPOON……3047茶匙<1222>TERMINALL Y STERILIZED PHARMACEUTICAL PRODUCTS—PARAMETRIC RELEASE……3047最终灭菌产品-放行参数<1225>V ALIDATION OF COMPENDIAL METHODS……3050药典方法的验证<1227>V ALIDATION OF MICROBIAL RECOVERY FROM PHARMACOPEIAL ARTICLES (3053)从药物中回收微生物的验证<1230>W ATER FOR HEALTH APPLICATIONS……3055健康用水<1231>W ATER FOR PHARMACEUTICAL PURPOSES……3056制药用水<1241>W ATER–SOLID INTERACTIONS IN PHARMACEUTICAL SYSTEMS (3074)在药物系统中水与固体的相互作用<1251>WEIGHING ON AN ANAL YTICAL BALANCE……3076关于分析天平的称重***<1265>Written Prescription Drug Information-Guidelines……….3078 书面的处方药信息-指南Dietary Supplements营养补充剂General Tests and Assays 一般检查法与测定法<2021>MICROBIAL ENUMERATION TESTS—NUTRITIONAL AND DIETARY SUPPLEMENTS (3080)微生物数量实验-营养与食品添加剂<2022>MICROBIOLOGICAL PROCEDURES FOR ABSENCE OF SPECIFIED MICROORGANISMS—NUTRITIONAL AND DIETARY SUPPLEMENTS (3083)不得检出特定微生物的程序-营养与营养补充剂<2023>MICROBIOLOGICAL A TTRIBUTES OF NONSTERILE NUTRITIONAL AND DIETARY SUPPLEMENTS……3087非无菌的营养与食品添加剂中的微生物分布<2040>DISINTEGRATION AND DISSOLUTION OF DIETARY SUPPLEMENTS (3089)食品添加剂的崩解与溶出<2091>WEIGHT VARIATION OF DIETARY SUPPLEMENTS……3092食品添加剂的重量差异<2750>MANUFACTURING PRACTICES FOR DIETARY SUPPLEMENTS (3093)食品添加剂的生产操作。

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Elektrotehniˇskivestnik68(4):225–230,2001ElectrotechnicalReview,Ljubljana,Slovenija

MethodsofReadingLiquid-in-GlassThermometersValentinBatagelj,JovanBojkovski,JankoDrnovˇsek,IgorPuˇsnikUniversityofLjubljana,FacultyofElectricalEngineering,LaboratoryofMetrologyandQuality,Trˇzaˇska25,1000Ljubljana,Slovenija

E-mail:valentin.batagelj@fe.uni-lj.si,jovan.bojkovski@fe.uni-lj.si

Abstract.TheobjectiveofthispaperistoanalysethedifferentmethodsofreadingLiquid-in-GlassThermometers(LiGTs).TheaimistominimiseuncertaintycontributionsincalibrationsofLiGTsandmakethemeasiertouse.TheinherentproblemoftheLiGTsistheobjectivityofreadingandhencetheresultinguncertaintycontribution.Mostcommonly,LiGTsarereadwiththenakedeyeorbyusingamagnifyingglass.Theseareclassifiedassubjectivemethods.Majorimprovementscouldbeachievedbyusingspeciallydesignedstereoscopes.AstereoscopeandstandardplatinumresistancethermometertogetherrepresentthereferencestandardincalibrationofpreciseLiGTs.Theentireprocedureisconsideredasthereferencemethod.Asanewmethod,aCCDcamerawithspeciallydevelopedimageprocessingsoftwareisintroduced.ItcombinestheobjectivityofthestereoscopereadingsandautomationofLiGTmeasurementsandcalibrations.

Keywords:readingofanalogueinstruments,LiGT,calibration,temperature,uncertaintyofreading

Metodeodˇcitavanjatekoˇcinskihtermometrov

Povzetek.Ciljtegaˇclankajeanaliziratirazliˇcnemetodeodˇcitavanjatekoˇcinskihtermometrovzaminimiziranjeprispevkanegotovostiprikalibracijitekoˇcinskihtermometrovinpoenostavitinjihovouporabo.Inherentniproblemtekoˇcinskihtermometrovjesubjektivnostodˇcitavanjainiznjeizvirajoˇcanegotovostodˇcitavanja.Ponavadisetekoˇcinskitermometriodˇcitavajosprostimoˇcesomalispomoˇcjopoveˇcevalnegastekla.Tostasubjektivnimetodi.Bistvenoizboljˇsanjepomeniuporabaposebejmodificiranegastereoskopa,kipredstavljareferenˇcnistandard,celotnipostopekpajereferenˇcnametoda.KotnovametodajepredstavljenoodˇcitavanjesCCDkameroinposebejrazvitoprogramskoopremozaobdelavoslike.Tametodazdruˇzujeobjektivnostodˇcitkovsstereoskopominmoˇznostavtomatizacijeodˇcitavanjatekoˇcinskihtermometrov.

Kljuˇcnebesede:odˇcitavanjeanalognihinstrumentov,tekoˇcinskitermometri,kalibracija,temperatura,negotovostodˇcitavanja

1IntroductionLiquid-in-glassthermometers(LiGTs)areanaloguemea-suringinstruments,wheretheheightoftheliquidcolumninsideaglassstemisproportionaltotheexposedtemper-ature.LiGTsareoneoftheearliestformsofthermome-ters,[1].Theyhavebeendevelopedfortheuseintherangefrom-190oCupto600oC,includingthemeasure-mentoftemperaturedifferenceswitharesolutiondowntoamilikelvin.LiGTsarestillverypopularbecauseofthechemicalinertnessofglass,goodlong-termstability

Received6March2001Accepted1October2001

atthesameuncertaintylevelandreasonableprice.ThemaindisadvantageofLiGTs,aswithmostanaloguemea-suringinstruments,isthelackofanycommunicationin-terfacewithacomputerandthusthelackofpossibilitiestoautomatethemeasurement.LiGTscanbecalibratedwithuncertaintiesfromafewmilikelvinsuptoafewdegreescentigrade,mostlyde-pendingonthescaledivisionandthusreadingofaLiGT,[2,3].Thereadingisusuallydonewiththenakedeyeorwiththehelpofamagnifyingglass.Othermethodsin-cludespeciallydesignedstereoscopesanduseofcamerastogetherwithimageprocessingalgorithms.Inthispa-perweassumethatallotheruncertaintysourcesarewellknownandwehighlightonlyaproblemrelatedtotheun-certaintythatiscausedbythereadingofaLiGT.Aspecialemphasisisalsogiventotheobjectivityofreadingwiththedifferentmethods.

2ReadingWiththeNakedEyeThebasicmethodofreadingLiGTsisreadingwiththenakedeye.IfonetriestoreadatemperatureofaLiGT(Fig.1)withthenakedeyeaspreciselyaspossible,with-outanyadditionalhelp,thereadingsaredispersed.Anobservermightreadtoonethirdofthescaledivision,whileanotherjustonequarteroreventoonefifthofthescaledivision.Thesightabilityisanobjectivereasonofinfluenceonreadingsbydifferentobservers.Ifonewantstoremainrealisticinmakingapre-226Batagelj,Bojkovski,Drnovˇsek,PuˇsnikFigure1.ReadingofaLiGTwiththenakedeyecisereadingwithouttryingtooverestimatethereading,aLiGTcanbereadwiththenakedeyeuptoonethirdofthescaledivision.

3ReadingWithaMagnifyingGlassApossibleimprovementinreadingLiGTsistheuseofamagnifyingglass.Withahelpofamagnifyingglassonecanestimateareadingwithinonequarteruptoonetenthofascaledivision,dependingonamagnifyingfactoranddistancebetweenscalemarkings.Butthosereadingsaremostlybiasedandverydependentontheonewhoreadsthetemperature.Forexample,ifaliquidcolumnissome-wherebetween22,12oCand22,14oC,asshowninFig.2,anobservercanread22,13oCwhileanotherobservercanread22,135oC.Evenskilledobserversarenotcon-sistent.Theytendtofavourcertainnumbersinmakingestimates.

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