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    PM Standarts

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    Eren Tekin

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    © All Rights Reserved
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    1995 EDITION Vis aes Sy FEDERATION a7 QW a PR wre Prof. Dr. Remzi VAROL $0.0. Mak, Moh. BOI. Standard Test Methods for Metal Powders and Powder Metallurgy Products Standard Test Methods for Metal Powders and Powder Metallurgy Products Introduction The Metal Powder Industries Federation ‘The Metal Powder Industries Federation (MPIF) ig a voluntary-membership, not-for-profit trade association formed by the members of the P/M industry to promote the advancement of the metal powder producing and consuming industries and the practice of powder metallurgy technology. MPIF is a federation of six trade associations, each of which is concerned with some Egpect of powder metallurgy or metal powders: the Powder Metallurgy Parts Association (PMPA), Metal Powder Producers ‘Aseociation (MPPA), Refractory Metals Association (RMA), Powder Metallurgy Equipment Association (PMEA), Metal Powder ‘Technology Association (MPTA), and the Metal Injection Molding Association (MMA). MPIF Standards MPIF standards cover five categories: 1. P/M Nomenciature 2. Powder Testing Standards 3, P/M and MIM Materials Standards 4, Material Testing Standards 5, Safety Standards (ANSIMPIF) Certain trade associations within MPIF have established standards committees composed of technical people who are responsible for developing standards within their area of expertise and proposing them to the MPIF membership. Before ‘a standard can be issued as an official MPIF standard, It must be approved by the MPIF membership as a whole. The standards Contained in this book have all been adopted under this procedure. Purpose and Use MPIF standards are intended to present and clarity P/M technology so as to aid in the conduct of business. P/M materials specifications and test standards relate to those activities that concern designers and users of P/M parts as well as the manufacturer. “The use of any MPIF standard is entirely voluntary. Existence of an MPIF standard does not in any respect preclude any member of MPIF or non-member from manufacturing or selling products not included in this standard. Suppliers are at liberty to supply products or to use procedures other than those identified in any standard, Disclaimers Neither MPIF nor any of its federated trade association members assumes or accepts any liability resulting from use of non-use of any MPIF standard. In addition, neither MPIF nor any of Its federated trade associations accepts any liability OF responsibility for the compliance of any product with any standard or for the results of any testing or other procedure ‘undertaken in accordance with any standard, ‘By publication of these standards, no position is taken with respect to the validity of any patent rights in connection therewith, ‘and the Metal Powder Industries Federation does not undertake to insure anyone utlizing the standards against liability for infringement of any Letters Patent nor assume any such liability. Availabilty 'MPIF standards may be revised at any time by the group responsible for their creation. Users are cautioned to refer to the latest edition. Comments from any source concerning the standards or MPIF's standards programs are welcome. [No part of this publication may be repro- (duced, stored in a retlval systom, or Published by transmitted, In any form or by any means, ‘Metal Powder Industries Federation ‘electronic, mechanical, photocopying, 105 College Road East recording, of otherwise, without the prior Princeton, New Jersey 08540-6692 U.S.A. ‘permission of the publisher. ‘TEL: (609) 452-7700 © Copyright 1995 FAX: (609) 987-8523 ISBN No, 1878954555 LMPIF Standard Test Methods General Information | Table of Contents GENERAL INFORMATION ‘Test Methods - Standards Classification Subject (Key Word) Index. Sources of Specialized Equipment P/M-Metric Conversion Table. STANDARD TITLE, ISSUE/REVISION DATE ‘Sampling Finished Lots of Metal Powders (86). Loss of Weight in Hydrogen for Metal Powders (Hydrogen Loss), Determination of (86)... Flow Rate of Free-Flowing Metal Powders Using the Hall Apparatus, Determination of (85)... Apparent Density of Free-Flowing Metal Powders Using the Hall Apparatus, Determination of (92) Sieve Analysis of Metal Powders, Determination of (92)... ‘Acid Insoluble Matter in Iron and Copper Powders, Determination of (88). Iron Content and Iron Oxide Content of Iron Powder, Determination of (90)... Terms Used in Powder Metallurgy, Definition of (84) . Preparing and Evaluating Tensile Specimens of Powder Metallurgy Materials, Method for (93) Green Sirength of Compacted Metal Powder Specimens, Determination of (90)... [Apparent Density of Non-Free-Flowing Metal Powders Using the Camey Apparatus, Determination of (92) ‘Terms for Metal Powder Compacting Presses & Tooling, Definition of (82). ‘Average Particle Size of Metal Powders Using the Fisher ‘Subsieve Sizer, Determination of (90)... Properties of Sintered Bronze P/M Filter Powders, Determination of (83). Impact Energy of Unnotched Powder Metalurgy Test Specimens, Determination of (83).. ‘Tranverse Rupture Strength of Powder Metallurgy Materials, Determination of (91)... o Density of Compacted or Sintered Metal Powder Products, Determination of (86). Hardness of Powder Metallurgy Products, Determination of (91). Dimensional Change from Die Size of Sintered Metal Powder Specimens, Determination of (86). Compressibilty of Metal Powders, Determination of (94). ‘Tap Density of Metal Powders, Determination of (82)... Apparent Density of Metal Powders Using the Amold ‘Meter, Determination of (94) Copper-Base Infitrating Powders, Testing (94)... Preparing and Evaluating Metal Injection Molded Debound and Sintered Tension Test Specimens, Methods for (91). Microhardness of Powder Metallurgy Materials, Determination of (84). Effective Case Depth of Powder Metallurgy Products, Determination of (84)... “Measuring the Volume of Apparent Density Cup Used in the Hall or ‘Camey Apparatus (Standards 04 and 28), Method for (92) [MPIF Standard Test Methods 0 Mw v v ‘STANDARD NUMBER ot 02 03 on oe General Information Il Test Methods — Standards Classification STANDARD NUMBER Testing of Metal Powders 01 Sampling Finished Lots of Metal Powders (02 Loss of Weight in Hydrogen for Metal Powders (Hydrogen Loss) (03 Flow Rate of Free-Flowing Metal Powders Using the Hall Apparatus (04 Apparent Density of Free-Flowing Metal Powders Using the Hall Apparatus 28 Apparent Density of Non-Free Flowing Metal Powders Using the Carney Apparatus 48 Apparent Density of Metal Powders Using the Amold Meter 05 Sieve Analysis of Metal Powders 32 Average Particle Size of Metal Powders Using the Fisher Subsieve Sizer (06 Acid Insoluble Matter in Iron and Copper Powders 07 _ tron Content and Iron Oxide Content of Iron Powder, 39 Properties of Sintered Bronze P/M Filter Powders 45. Compressibllty of Metal Powders. 46 Tap Density of Metal Powders 49 Testing Copper Base Inftrating Powders Testing of P/M Products 40 Tensile Specimens of Powder Metallurgy Materials 15 Green Strength of Compacted Metal Powder Specimens 40 Impact Energy of Unnotched Powder Metallurgy Test Specimens 41 Transverse Rupture Strength of Powder Metallurgy Materials, 42. Density of Compacted or Sintered Metal Powder Products 43 Hardness of Powder Metallurgy Products 44 Dimensional Change from Die Size of Sintered Metal Powder Specimens 50 Metal Injection Molded Debound and Sintered Tension Test Specimens 51 Microhardness of Powder Metallurgy Materials 52. Effective Case Depth of Powder Metallurgy Products Other Testing 53 Volume of the Apparent Density Cup—Hall/Camey Apparatus MPIF Standard Test Methods General Information _ Ill Subject (Key Words) Index — Standard Number Apparent Density ‘Amold meter, 48 Camey apparatus, 28, Hall apparatus, 04 Case depth (effective), 52 Compressibility, 45 Definitions ‘Compacting presses and tooling, 31 Powder metallurgy terms, 09 Density determination, 42 Dimensional change, 44 Filter powders (bronze), 39 Flow rate (Hall apparatus), 03 Green strength, 15 Hardness determination, 43 Hydrogen loss, 02 MPIF Standard Test Methods Impact energy, 40 Infitrating powders (copper base), 49 Insoluble matter, 06 Iron content, 07 Microhardness, 51 Patticle size (Fisher subsieve sizer), 32 ‘Sampling metal powders, 01 Sieve analysis, 05 Tap density, 46 Tensile test specimens Injection Molded, 50 Powder Metallurgy, 10 ‘Transverse rupture strength, 41 Volume ‘Apparent density cup, 53 General Information IV ‘Sources* of Specialized Equipment Noted in Standard Test Methods for Metal Powders and Powder Metallurgy Products Std, No. 01 — Sampling Keystone Sampling Thief and Sample Splitter Gilson Co, Inc. P.O. Box 677 ‘Worthington, OH 43085 (800) 444-1508, ‘Seedburo Equipment Co. 1022 West Jackson Boulevard Chicago, IL 60607 (800) 284-5779 ‘Sepor, Inc. P.O, Box 578 Wilmington, CA 90748 (800) 753-6463, Stds. No. 3— Flow Rate Nos. 04 and 28 — Apparent Density Hall Flowmeter, Carey Funnel and ‘Standard Powder Alcan Powders & Pigments ‘904 Lehigh Avenue Union, NJ 07083 (908) 851-4590 Std. No. 05 — Sieve Analysis ‘Sieve Shaker Fisher Scientific Co, (major US. cities) (200) 768-7000 Gilson Co., Inc. P.O. Box 677 ‘Worthington, OH 43085, (800) 444-1508 W.S. Tylor, Inc. P.O. Box 8900 Gastonia, NC 28053 (800) 238-9537 ‘Stds. No. 10 and 50 — Tension Test Strength No. 15 — Green Strength No. 41 — Transverse Rupture Strength No. 44 — Dimensional Change ‘Compacting Dies, Transverse Rupture Strength Fixture and Green Strength Tester Major Gauge & Tool Co. 12953 Farmington Road Livonia, MI 48150 (318) 425-5165 Plymouth Tool Div. Federal-Mogul Co. 45700 Mast Street Plymouth, Ml 48170 (313) 453-3628, Green strength tester engineering drawings available from: ‘Alcan Powders & Pigments ‘901 Lehigh Avenue Union, NJ 07083 (908) 851-4500 x544 Std. No. 32— Average Particle Size Fisher Subsieve Sizer Fisher Scientific Co. (major US. cities) (800) 766-7000 ‘Std. No. 46 — Tap Density Tap Density Tester Quantachrome Corp. 1900 Corporate Drive Boynton Beach, FL 33426 (407) 731-4999, Vankel Industries, nc. 36 Meridian Road Edison, NJ 08820 (908) 548-3616 ‘Std, No. 48 — Apparent Density ‘Amold Meter ‘Amold Engineering 648 Cedar Road St. Marys, PA 15857 (814) 834-3952 ‘Other — Apparent Density ‘Scott Paint Pigment Volumeter WR Scientific (major U.S. cities) (800) 992-5000 Note: Other soures for this equipment may exist LMPIF Standard Test Methods General Information V Metric Units for P/M P/M TERMS Approx. Conversion Quantity Designation Customary Unit _ Preferred Working Unit Symbol___to Metric Particle Size S microns (obs) __micrometre am - Specific Surface - mq square metre per gram m/g : Apparent Density a fom? ‘gram per cubic centimetre gfe - Flow Time : 8/509 second per 60 grams 8/509 : Powder Mass : ound (Ibm) kilogram kg x 0.454 ton megagram Mg x 0.907 ton metric ton t x0.907 Bulk Density : lbmvtts ‘gram per cubic centimetre gfom Xo016 "omv/gat ‘gram per cubic centimetre gfe xo.120 ‘Tap Density a ‘g/m? g/em® : Compacting Pressure S tsi rewton per square millimetre N/mm? x 1379 Green Density 2% g/oms ‘gram per cubic centimetre g/ems 5 Green Strength - si newton per square millimetre N/mm? x0.007 ‘Atmosphere Flow - fe/min ‘cubic centimetre per second cm/s x4720 FH cubic centimetre per second omi/s x7.868 Belt Speed - pm millimetre per minute mm/min -X 25.40 Sintered Density a gfoms ‘gram per cubic centimetre fem? - ‘Surface Finish - rmicroinches mmicrometre am x 0.025 Heating Rate - °F ieee degree Celsius per second °Cls X 0556 Crush Strength kK 10 psi newton per square millimetre N/mm? X 6.895 Yiold Strength - 10% psi newton per square millimetre N/mm? 6.895 Tensile Strength - 10% psi newton per square millimetre N/mm? X 6.895 ‘Transverse Rupture Strength = 10% psi newton per square millimetre N/mm? 6.895 Impact Energy : feb joule J X 1956 ‘Young's Modulus - 108 psi newton per square millimetre N/mm? 6,895, Force - ound force (Ibf) newton N 4448 MPIF Standard Test Methods METAL POWDER INDUSTRIES FEDERATION Method for Sampling Finished Lots of Metal Powders MPIF Standard 01 Issued 1945, Adopted 1948, Revised 1961, 1973, 1981 Reapproved 1986 1. SCOPE 4. TEST SPECIMEN Ths tandacd coon two ethos Tor wiewing © ET Method A ea ed sett cames LA Atleast thre increments shall be taken for cach Son tene fot of powder, The aust umber Jepnds on he LLL ee is rd Bomdecs in the a of being size of the lot and the powder involved and shall packaged from blenders or storage tank ‘be agreed upon by the parties involved. Ce re et ee ee ores aaa a M 12 ‘This standard may involve hazardous materials, operations, and 421 See Table 2 ened yl fr mar pr od Pro te psy sro ik ee oer sa marten ere oe ‘egultory lntations prior se ————_—_______—_— No. of Containers No. of Containers to 2. DEFINITIONS in the Lot be Sampled 21 The following terms are defined: 15 All 21.1 Lot—A definite quantity of powder processed or 615 3 produced under uniform conditions. Teas A 2.1.2 Increment—A quantity of powder obtained by a eae H sampling device at one time from a single lot ae 5 2.1.3 Gross sample—A quantity of powder consisting of + all of the increments taken from a single lot. 100-149 10 2.14 Composite sample—The blended entire gross sample 130-199 rn ff a representative part thereof. 200.299 2 2.15 Test sample—A quantity of powder taken from the 300-399 B composite sample for determining a single property ‘More than 400 13+ 1 per 100 or for preparing the test pieces. It should normally additional containers be taken by splitting the composite sample. 2.1.6 Test portion (Test specimen}—A defined quantity of powder actually drawn from the test sample on which the testis actually performed. 3. APPARATUS 3.1 Method A’ 3.1.1 Rectangular receptacle capable of being moved completely across the stream of flowing powder at ‘constant speed and havingalength and width greater than the stream of powder, It must be large enough that there is no overflow when collecting the sample, 3.1.2 Small blender 3.13 Sample splitter (Fig. 1) 32° Method B 3.21 Keystone Sampler (Fig. 2) 3.22 Sample splitter NOTE I—Names of manufacturers of this apparatus are listed in General Information IV. MPIF Standard Test Methods _ 5. PROCEDURE 5.1 Method A S.L1 The rectangular receptacle is passed completely through the stream of flowing powder at a constant speed. If the entire contents of one lot of powder is being packed in a single container, increments shall be taken when the container is %, 4 and % filled, If several containers are to be filled by one lot of powder, the first increment shall be taken when the first container is % filled, the second inerement shall be taken in the middle of the run, ‘and the third increment taken near the end of the run, Additional increments may be agreed upon by the parties concerned. The total of all increments shall be at least $000 g. age 2012) ee ‘A gross sample composed of at least five thousand ‘grams shall be blended in a small blender for 10- 15 revolutions. ‘The blended gross sample or composite sample shall then be passed through a sample splitter to form ‘a number of test samples depending on the design of the splitter. These test samples are then used to supply the test portions for subsequent testing. 532 Method B ‘The Keystone Sampler in the closed position shall be inserted into the powder through a point 70% of the distance from the center of the cross section to the periphery and straight down to the bottom of the container, The sampler is then twisted to the ‘open position to allow powder to flow into the sampler tube. When filled, the sampler is once again closed, then removed from the container, and the contents emptied into a suitable container. When a suitable number of increments have been taken they shall be blended for 10-15 revolutions to obtain a composite sample. ‘The composite sample shall be passed through a sample splitter to obtain the test samples. ‘The test portion shall be obtained from the test sam- ple by use of a micro sample splitter or by quartering. APPENDIX ‘AL COMPARABLE STANDARDS, ASTM B25 TSO 3954 FIGURE 1 Sample Spttor By pilccion of ese nas 0 pion tke with repo he vai of any ule isn crmeson thet td te Nl Powder nur Feet os teat one aye iinet scr nast aiy or engemest ‘fay eters Put ee an soc aly. (MEME snr aoe ihe pb et odes imi isa ettaangs tte tenor nd he paca ta to ws th eh ‘Scag atsnng be proper stra for spar roar Exerc fa ‘Munctctrng sing pose ot lied in san or om wy pos ‘dieser eget ran thwe ed a is Snare “Te gare rem sve re wed it sana re acorhoe ie [Bute provid ASTM ESSOSK Sant Pras fr Us of the tard ‘yen of Uns The Modemied Mee Sater), planed ye Amara Sosy Fos ad Mens 1916 Rac Suet Pdf PA 1913 FIGURE2: Keystone Sampler ‘This Standard, propared bythe Metal Powder Industries Federations aubjoct 0 periodic revision. Suggestions for revision should be addressed to the Metal Ponder Indusiies Federation, 105 College Road East, Princaton, NJ, 08540-8602. Users of Standards are cautioned to secure the latet editions, Complete edo of standards may be obtained from 1 Federation atthe above adress, MPIF Standard Test Methods METAL POWDER INDUSTRIES FEDERATION Method for Determination of Loss of Weight in Hydrogen for Metal Powders (Hydrogen Loss) MPIF Standard 02 Issued 1948, Revised 1964, 1977, 1986 ———<—ui 4. SCOPE Ll This standard describes a method for determining the approximate oxygen content of some metal powders by measuring weight loss after hes reducing gas LI Only oxygen from oxides which are reducible by hydrogen under the test conditions is measured. The test will not measure oxygen from oxides such as, SiO:, AlOs, MgO, CaO, BeO, TiO:. 1.1.2 The measured oxygen content is lower than the total oxygen since standard conditions of the test do not always allow complete reduction. Maintaining stand- ard conditions is mandatory. 1.1.3 The weight loss can also include carbon, sulfur and other impurities that may react with hydrogen or products of reaction, Compensation must be made. 1.14 The weight loss may include loss of elements such 1s cadmium and zine due to evaporation. 1.1.5 The weight loss may include oxygen from oxides reduced by carbon if present. LL6 The weight loss may include the weight gain from some components of the powder being oxidized or hydrided during the test. 1.1.7 The weight loss may include moisture and absorbed or adsorbed gases. 1.2 This standard may involve hazardous materials, operations, and equipment. This standard docs not purport 10 eddress all of the polenial safety problems associated with ls use It is the ‘responsibilty ofthe wer ofthis standard to establish appropriate ‘afety and health proctices and to determine the appicabily of regulatory limitations prior to we. —<———{$$—$——— 2. APPARATUS 21 Furnace capable of operating at the recommended temperature. 22 Temperature control capable of maintaining temperatures to + 25° F (+ 15° Q. 23. Gas-tght ceramic or metallic combustion tube. 24 — Flow meter to measure flow of reducing gas. 25 — Quartz or alundum combustion boats. 26 Balance suitable for weighing to the nearest 0.001 g. 27 Reagents 27.1 Nitrogen having an oxygen content of less than 20 ppm and a dew point less than -40° F (-40° C). MPIF Standard Test Methods 2.72 Reducing gaseither hydrogen having an oxygen content of less than 20 ppm and a dew point lower than 40° F (-40° C), or dissociated ammonia having 1 dew point better than ~40° F (-40° C). 3. TEST SPECIMEN 3.1 The test specimen of metal powder, obtained in ac- cordance with MPIF Standard 01, Sampling of Finished Lots of Metal Powders, shall be approximately 5 g (410 6 g) weighed to the nearest 0.001 g. 4. PROCEDURE ‘Caution - Certain mixtures of hydrogen or dissociated am- ‘monia and air can explode when ignited. Proper purging with nitrogen can reduce the risk of explosions. 4.1 Method A 4.1.1 The furnace with combustion tube inserted shall be adjusted to bring the inside of the combustion tube to the temperature indicated forthe metal being tested, See Table 1. 4.12 The test specimen shall be spread to a uniform depth in a combustion boat which has been preconditioned to.aconstant weight and weighed to the nearest 0.001 The depth of powder inthe boat should be approxi ‘mately 1/8 in. (3 mm). The boat and specimen shall then be weighed to the nearest 0.001 g. 4.13 Nitrogen shall be passed through the combustion tube for a period of at least one minute prior to insertion fof the boat, which shall be placed at the center of the zone of uniform temperature of the furnace. 4.14 Theflow of reducing gas shall be started, the nitrogen stopped, and the time when the reducing gas is introduced shall be recorded. 4.15 A positive flow of reducing gas through the system shall be maintained for the time of reduction during which the temperature inside the combustion tube ‘must be held within + 25° F (t 15° C). 4.1.6 At the end of the prescribed time, from Table 1, the flow of reducing gas shall be discontinued, and nitrogen shall be introduced into the tube. 4.1.7 After nitrogen has been flowing through the combustion tube for at least one minute, the tube shall be opened, and the boat withdrawn under nitrogen atmosphere to the cooler part of the ‘combustion tube. 4.1.8 The specimen shall be allowed to cool in the nitrogen atmosphere until there is no danger from reoxidation (normally 15 to 30 min.) after which it shall be removed from the tube and permitted to cool to room temperature in a desiccator. 4.1.9 When the boat has cooled to room temperature, it, shall be reweighed to the nearest 0.001 g. 42 Alternate Method. The following alternate method. ‘may be employed satisfactorily ifthe use of nitrogen is impractical. 42.1 The furnace with the combustion tube inserted shall be adjusted to bring the inside of the combustion tube to the temperature indicated for the metal being tested. See Table | 42.2 The test specimen shall be placed into the combustion boat, which is weighed to the nearest 0.001 g, and spread to a uniform depth throughout the boat. The depth of powder in the boat should be approximately 1/8 in, (3 mm). The boat and specimen shall then be weighed to the nearest 0.001 g. 42.3. The boat containing the specimen shall be placed in ‘the combustion tube through which dry reduction, ‘gas is flowing, The boat is inserted through the reducing gas discharge end of the tube which is open to the atmosphere and at which hydrogen is burning. ‘The boat shall be placed within and at the center of the zone of uniform temperature of the furnace, and the time of insertion shall be recorded. 424 A positive flow of reduction gas through the system shall be maintained for the time of reduction, during which the temperature inside the combustion tube ‘ust be held within + 25° F(t 15° ©). 425 At the end of this period, the entire combustion tube with reducing gas still flowing through it shall be Tablet Metal Powder Time Temperature Boat Cobalt 60min. 2050°F (1120°C) Alundum Copper 30" 1600°F (875°C) Quartz Coppersin 30° 1425°F (775°C) Quartz Lead 30" 1020°F (550°C) Alundum Lead-tin 30" 1020°F ($50°C) Alundum Tron & Steel 60" 2050°F (1120°C)Alundum Nickel 0" = 2080°F (120°C) Alundum Tin 30" 1020°F (550°C) Alundum Tungsten 60" __—_—2050°F(1120°C) Quartz withdrawn from the furnace and set on a rack until the specimen has cooled to a point at which it can be removed from the reducing gas atmosphere without danger of reoxidation. This is normally 15 to 30 min, Then the specimen shall be removed from the tube and permitted to cool to room temperature in a desiccator. 42.6 When the specimen has cooled to room temperature, it shall be reweighed in the boat to the nearest 0.001 g. 5. CALCULATIONS 5.1 Calculate the hydrogen loss as follows: Hydrogen loss (Hs Loss), AB x 100 Hy Loss, where: A = original weight of boat and specimen in grams B = weight of boat and specimen after reduc- tion in grams C = original weight of specimen in grams 6. REPORT 6.1 Results shall be reported as percent hydrogen loss to the nearest .01 percent. Duplicate results within £ 5% of the amount present shall be considered satisfactory. APPENDIX ‘Al, COMPARABLE STANDARDS ASTM E 159 1S0 4491/2 Dacainer By picion ose ds ops tk with eect oh aly fay ein evi eel ove Fen St STN tr ope he a we ep ciate ‘Sicing nd cing oper mac en pra pos xser of a ‘i stn des ot any esp: peta any DUP man ar no mere at Imunacrng ong posit led sandal alisng pss. (Sree tran owed isda “Tienes sem comenine car wed ik snd we serine wih he [lllncepawsed io ASTM E5009 Stun ree for Ue of We eran Shem of Unt The Masons Mei Sse, ped by the Arve Socety for oringané Maal 96 Race Smt Pini, P1918, ‘Tis Standard, prepared by the Metal Powder Indusies Federation, is subject to period revision, Suggestions for revision should be addressed 10 ‘ndust the Metal Pow Federation, 105 Collage Road East, Princeton, N.J. 08540-6692. Users of Standards are cautioned to secure the latest edtone. Compete action o standards may be obained trom the Federation at the above adress MPIF Standard Test Methods Prof. Dr. Remsi VAROL ‘5.0.0. Mak: Moh. BO. METAL POWDER INDUSTRIES FEDERATION q Method for Determination of Flow Rate of Free-Flowing Metal Powders Using the Hall Apparatus MPIF Standard 03 Issued 1945, Revised 1972, 1980, 1985 ——_— 4. SCOPE 11 This standard describes a method for determining the rate of flow of metal powders and is only suitable for those powders which will low unaided through the specified Hall flowmeter funnel. 1.2 This standard may involve hazardous meters, operations, and quipment. Ths standard doesnot purport 0 adaress all ofthe poten! sfety probleme asvocated with tis use It the Pespontbiy ofthe user ofthis standard oesablsk appropriate Snjery and heath practice and to determine the applicability of regulatory lations prior se — APPARATUS 21 Hall Flowmeter Funnel: A standard flowmeter funnel (Fig. 1) having a calibrated orifice of 0.10” (2.54 mm) in diameter, 22 Stand: A support Fig. 2)to hold the flowmeter funnel, 23 Stopwatch 24 Base: A vibrat assembly 25 Balance: A balance having a capacity of at east 100 gand a sensitivity of 0.1 g. NOTE I—Names of manufacturers of this apparatus are listed in General Information IV. n-free table to support the flowmeter —_—_—$——$——— 3. TEST SPECIMEN 3.1 The test specimen shall consist of a mass of $0 + 0.1 g of metal powder obtained in accordance with MPIF Standard 01, Sampling Finished Lots of Metal Powders. 3.2 Thetestspecimens shall be tested as sampled. Itshould be noted, however, that moisture and additives such as oils, lubricants, graphite, etc. may alter the flow characteristics. —_—— $$ 4, PROCEDURE 41 The test specimen shall be carefully loaded into the flowmeter funnel while keeping the discharge orifice at the bottom of the funnel closed by placing a dry finger under it, Care should be taken to make certain the short stem of the funnel is filled. MPIF Standard Test Methods 42 The stopwatch shall be started simultaneously with the removal of the finger from the discharge orifice ‘and stopped at the instant the last of the powder leaves the funnel. The elapsed time in seconds shall be recorded. 5, CALCULATIONS 51 Calculate the flow rate by multiplying the elapsed time by the correction factor which has been ‘determined as indicated in the Appendix AL. 6. REPORT 61 Report the flow rate in 5/50 g to the nearest second. APPENDIXES Al. CALIBRATION OF HALL FLOWMETER FUNNEL. ‘The manufacturer supplies the funnel calibrated as follows: Using the procedure described in Section 4, the flow rate of standard 150 mesh Turkish emery is determined. The average of five determinations (the extremes of which shall not differ by more than (04 8) is stamped on the bottom of the funnel. The correction factor of the unused funnel is 40.0 divided by this number. It is recommended that the factor be periodically verified by the user by determining, by the above method, the flow rate of the standard 150 mesh (<106 ym) Turkish emery. If the flow rate hhas changed from that stamped on the instrument, the new correction factor will be 40.0 divided by this new flow rate. Before adopting the new correction factor, however, itis recommended that the cause of the change be investigated. If the flow rate has increased, itis probable that repeated use has burnished the orifice, and the new correction factor may be used. ‘A decrease in flow rate may indicate a plating of soft powder upon the orifice. This should be carefully removed with the aid of a pipe cleaner, and the calibration test rerun, the new correction factor being, calculated if required. It is recommended that the use cof a funnel be discontinued after the flow rate of the standard sample has increased, such that the time of flow is less than 37 s, The manufacturer's experience (WPIF Standard No. 03 — page 201 2) ee indicates that under conditions of almost continuous daily use, a decrease in time of flow of 3 s should ‘be expected after 5 years of service NOTE 2—Standardized no, 150 emery grit is no longer being sold, In those instances where the user desires to verify the correction factor and does not possess the no. 150 emery grit, the funnel may be returned to Alcan Powders and Pigments, 901 Lehigh Avenue, Union, N.J, 07083, for re-calibration and re-certification. It is recommended that verification be done at least annually depending on frequency of use. 2. REPORTON PRECISION OF MPIF STANDARD NO. 03 A21 A planned testing program was carried out among ‘users of the Hall flowmeter apparatus to obtain data to determine the precision of this method. The complete report on this work is availabe inthe offices ‘of the Metal Powder Industries Federation. A2.2 It was found that the different reaction times of individual analysts only has a minor influence upon the coefficient of variability, (V). If it were a major factor, V would increase directly with flow rate. However, the fastest flowing metal powder, nickel, did have the lowest coefficient of variability 3.0% while the slowest flowing, aluminum, had the highest, 5.8%. 0325" (22 mm) 010" (254 mm) FIGURE 1: Hall Flowmeter Funnel FIGURE 2 Stand A23. This method yields more precise flow rates when testing smooth surface powders than rough nodular powders. Compare the smooth emery, V = 20%, nickel V = 3.0%, with the rough iron, V = 5.5%, aluminum V= 5.8%. A24 MPIF Standard No. 03 is operable, under conditions of calibrating with standard emery powder, with precision of V = 2.0%. A2S MPIF Standard No. 03 is operable, in the testing of free-flowing metal powders with a precision of V = 66. 3, COMPARABLE STANDARDS ASTM B23 1S0 4490, yin te in niin ne win po be ai ‘EStonkstate totes spon ung the sara ny oe ingest ‘any Ltrs cat or soe ny ue ay STA ropes tn pt cn i ‘String ting te proper tea fos price ree. Exe ‘Mou snr does ot nay Rope psa ty tPF emer ono marber oe Imantacring ling proc cae stro om lig pose hes oreqlpnet et ban hos lel ns adr "Tie mare yom snverion to: wed Ss sada a crane he [Polslocs pied sy AST ESDODI Sana! Petes for Un fe fermen Smo Unt The Modemine Met Syste passed bythe Amen Sock) {oc ening to ern 116 Rae Sac, Plan PA 1910 FIGURE’: Assembly {Tis Standard prepared by the Metal Powder Indusvies Federation ls subject to periodic revision. Suggestions for revision should be addressed to the Metal Ponder Industries Federation, 105 Collage Road Easi, Princeton, N.J. 08540-6892. Users of Standards are cautioned to secure the latest edons. Complete edon of standards may be obtained ftom the Federation atthe above address, LMPIF Standard Test Methods METAL POWDER INDUSTRIES FEDERATION Method for Determination of Apparent Density of Free-Flowing Metal Powders U: Hall Apparatus MPIF Standard 04 Issued 1945, Adopted 1948, Revised 1972, 1980, 1985, ————_— $$ 1, SCOPE 1:1 This standard deseribes a method for determining the apparent density of free-flowing metal powders and is only suitable for those powders which will flow unaided through the specified Hall flowmeter funnel, See MPIF Standard No. 28 for apparent density of non-free-flowing metal powders. This stondord may involve hazardous materials, operations, and Cauipment Tis standard doesnot purport to address al of the pote safety problems astolaed wih it ge. Ii he respons Dy ofthe er ofthis standard to extablish appropriate safety {nd heath practices and to determin the applicability of ela. ‘yliitions prior tose. —<— $< ___ 2. APPARATUS Hall Flowmeter Funnel: A standard flowmeter funnel Fig. 1) having an orifice 0.100 inch (2.54 mm) in diameter. 22 Density Cup: A cylindrical cup (Fig. 2) having & capacity of 25 + 0.03 cm* with an inside diameter of 2805 mm, 23 Stand: A support (Fig. 3) to hold the flowmeter fun- rel concentric with the density cup so that the bottom of the orifice is approx. 1.0 inch (25 mm) above the top ofthe density cup when assembled (Fig. 4). 24 Base: A vibration-free table to support the flowmeter assembly. 25 Balance: A balance having a capacity of atleast 200 g and a sensitivity of 0.01 g. NOTE 1—Names of manufacturers of this apparatus are list- cd in General Information IV. 3. TEST SPECIMEN 3.1 The test specimen shall consist of a volume of approximately 30 to 40 cm* of metal powder, obtained in accordance with MPIF Standard 01, ‘Sampling Finished Lots of Metal Powders, 3.2 The test specimens shall be tested as sampled. It should be noted however, that moisture, temperature and additives such as ols, lubricants, graphite, etc ray alter the apparent defy MPIF Standard Test Methods nN g The 1992 0) 4. PROCEDURE 1 The entire test specimen shall be carefully loaded into the flowmeter funnel and permitted to flow through the discharge orifice into the center of the density coup. The testing apparatus should not be moved dur- ing the filling When the powder completely fills and overflows the periphery of the density cup, the funnel shall be rotated approximately 90° in a horizontal plane so thatthe remaining powder falls away from the cup. Using @ non-magnetic spatula with the blade held perpendicular to the top of the cup, the powder shall be leveled off flush with the top of the density cup. Care must be taken to avoid jarring the apparatus at any time, After the leveling operation, the density cup should be lightly tapped on the side to settle the powder to avoid spilling in transfer. ‘The powder shall be transferred to the balance and weighed to the nearest 0.1g, This isthe mass M. 5. CALCULATIONS 5.1 Calculate the apparent density as follows: ‘Apparent Density, (,) =A PP oo=-¥ where: ‘M =mass of powder from the density cup in grams the volume of the cup (as determined by the procedure in ‘Standard 53) NOTE 2—If the measured volume is 25 + 0.03 cm? itis permissible to use 25 em’ for V. 6. REPORT 61 Report the resulls as apparent density to the nearest 0.01 gfem’ APPENDIXES ‘Al, _ REPORT ON PRECISION OF MPIF STANDARD NO. 04. (MPIF Standard No. 06 — page 2of2) AL. A planned testing program was carried out among the users of the Hall flowmeter apparatus to obtain data to determine the precision of this method. The complete report on this work is available in the offices of the Metal Powder Industries Federation. AL2 The report concludes that MPIF Standard No. 04 is ‘operable in the testing of free-flowing metal powder, With a coefficient of variation equal to 2.1%. 42, COMPARABLE STANDARDS ASTM B 212 1S0 3923/1 (a Ye 16 microinch (4x 10° m) finish or beter 0.125 + 0.005 @18£013mm) aie 0.100: 0009" (254=0.08 mm) FIGURE 1: Hall Flowmeter Funne! FIGURE 2: Densty Cup (25+ 0.03 em) ‘This Standard, prepared by the Metal Powder Indusios Federation, is subject to periodic revision. Suggestions for esi rh gl owe Fron ecu eng eit ee i hs Sr oom ae Pee ier Tesing an terns Te ace See Pasig, PAISIOR FIGURE 4; Assembly the Metal Powder Industiae Faderation, 105 College Road East, Princeton, N-J. 08540-6682. Users of Standards are cautioned to secure the latest eons, Complete edition of standards may be obtained from tho Federation at the above adress. PIF Standard Test Methods METAL POWDER INDUSTRIES FEDERATION Method for Determination of Sieve Analysis of Metal Powders MPIF Standard 05 Issued 1945, Revised 1949, Adopted 1949, Revised 1962, 1973, 1985, 1992 4, SCOPE T__ This standard describes a method for determining the dry sieve analysis of granular metal powders. This standard may imlve hasardows materals, operations and ‘auipment. Thi tandord does not purport to adress all of the Potential afer problems associated with suse. Is the respons ‘lyf he azer ofthis standard to establish propriate sfety nd health practices and determine the appicbliny of epuato Fy lintatons rir tse 2. APPARATUS 21 Sloves: A set of calibrated sieves should be selected based upon the mesh size of powders being evaluated. ‘The sieves shall be 8 in. (200 mm) in diameter and either 1 of 2 in, (25 or 50 mm) in depth and fited with brass, bronze, stainless steel, or other suitable wire, The new U.S. Series standard sieves are the pre= ferred series to use. NOTE 1—For more detailed information, refer to ASTM Standard E 11. NOTE 2—The new U.S. Series was adopted in 1970. The old USS. Series standard sieves and equipment sieves manu- factured by other companies, such as Tyler, may also bbe used if the new U.S. Series is not available. Care should be taken to make sure that sieve opening sizes are correct when performing standardization work, Table 1_ Testing Sieves According to the U.S. Standard Series and Tyler Standard Screen Scale Sieve Series. Mesh —____Sieve Opening (am) _ Designation NewUS. OWUS. Tyler Number Series _Series Series 20 350 S41 333 35 = = 47 40 05 420 = 60 250 250 295 80 180, 7 15 100 130 149 137 140 106 105, = 150 = = 104 200 5 4 74 230 6 3 = 250 = = 8 225 4 4 4 -MPIF Standard Test Methods ‘Sieve Shaker: A mechanically operated single eccen- tric sieve shaker which imparts to the nest of sieves a rotary motion of 285 + 15 rpm and a tapping action of. 150 = 10 taps per minute. The sieve shaker shall be fitted with a plug to receive the impact of the tapping. device, The entire apparatus shall be mounted rigidly, and preferably shall be provided with a time switch to insure accuracy of duration of the test. 3—Names of manufacturers of this apparatus are list- ‘ed in General Information IV. AA balance having a capacity of at least 150 g and a sensitivity of 0.01 g, NOTE 4—Use of a sound-proof enclosure is recommended. 3. TEST SPECIMEN 3.1 The test specimen, obtained in accordance with MPIF Standard OL and having en apparent density greater than 1.5 gem’ as determined by MPIF Standards 04 ‘of 28, shall be 90-110 g. Ifthe apparent density of the powder is less than 1.50 gem’, a 40-60 g sample shall be used, 4. PROCEDURE an “The group of sieves selected shall be assembled in consecutive order based on size of openings. The sieve having the largest opening shall be placed atthe top, and the assembly completed by a solid collecting pan placed below the bottom sieve. The test specimen shall be placed on the top sieve, and this sieve closed with a solid cover. The sieve assembly shall then be fastened securely in a suitable mechanical sieve shak- ing device and operated for 15 minutes. ‘The sieved fractions shall be removed from the nest of sieves by removing the coarsest sieve from the rest, gently tapping its contents to one side and pour- ing them on a glazed paper. Any material adhering to the bottom of the sieve and frame shall be brushed with a soft brush into the next finer sieve. The sieve just removed then shall be tapped upside down, on the paper containing the portion that had been retained on it. This fraction shall be weighed to with- in 0.1 g. This process shall be repeated for each sieve in the nest, and the fraction collected in pan shall also be removed and weighed. The sum of the masses of all the fractions shall be recorded. The difference (MPIF Standard No. 05 — page 2 012) between the sum and the total sample mass shall be added to the mass ofthe fraction collected in the pan, provided the sum of all the fractions is not less than 99% of the original sample mass NOTE 5—If the sum is less than 99%, check for weighing terrors, pin holes, etc. and repeat the test. 5. REPORT SI The masses of the fractions retained on each sieve and the mass of the fraction collected in the pan shall bbe expressed as percentages of the test specimen mass to the nearest 0.1%. Powder specimen whose mass fraction is less than 0.1%, shall be reported as “trace” If fraction is absent, it shall be reported as "0.0". 5.2. Form for reporting test data of a typical 100 mesh powder. ‘Table 2 New U.S, Standard Series —_—_—_—_—_—_——— APPENDIX KI, Certified Sieves — Master Set Sieves conforming to ASTM Standard E 11 can be obtained from the sieve manufacturers, and arrange- ‘ments can be made through them to have the sieves, certified to NIST Standards. If used continually, the sieves will, after a period of time, become less accurate and might no longer be acceptable as certified sieves. The common practice, which would be considered acceptable according to this standard, ‘would be to use the certified sieves as a master set for checking and calibrating other working sets of sieves. 2, Matched Sieves The use of a matched set of sieves, established through use of a standard powder is recommended when closer correlation of tests between supplier and ‘consumer is desired. a3. Particle Size Meth Designation Percentage By Table 5 Suggested Sieve Series (New U.S.) for Metal wm) No, Mass Powders > 180 + 80 Pers ae ‘Nominal Powder S180 > 150 oe Mesh Size 20 40 60 100 140 200 325 $150> 106 = 100+ 140 sare <106> 75 ~ 140+ 200 S 75> 45 ~ 2004325 New US. a vt vt7 < 45 ~ 325 si 301 Lie Zz fim Wa Wa AA Table} Old US. Standard Series Series 14d ATT bol zt 7[vtvtvTvt7 Particle Size Mesh Designation Percentage By ee Se —m_ No Mass. bast _tv[vlv iv lvl 7 eat] + 8 ra PAPAPAPAPARA S177> 149 = 80+ 100 51495105 = 100+ 140, ‘Ad, Report on Precision and Accuracy of MPIF Standard S105> 74 - 140+ 200 05 S4> 4 200435 Ad.L_ A testing program is being carried out among Iabora- < 44 05 tories employing this method to determine precision and accuracy, ‘AS. Comparable Standards ‘Tabled Tyler Standard Sereen Scale Sieve Series ASTM B 214 Particle Size Mesh Designation Percentage By aad (um) No. Mass: Disclaimer > 175 + 80 put nghs a comcion ari oe te Mel Power out Penton it 1753149 — 804100 [Snes ing esi ot ly gr S149> 106-1004 150, "SAF standards we ape th pues ad ae designed i ein mien ele sscctng a sening pop onl fr pre pac Exntce of S 74> 44 ~ 2004325 Ma srd doesnt in ay eapct presse ay MIE ere oon member om = 44 Ths Mamta orcoy pect bead sar Rom ele ps 5.3 Interpretation of this report should be made with ref- ‘erence to dimensional tolerance of the standard sieves as specified in ASTME 11, {delies provided in ASTM ESHD I; Standard Pace for Use ofthe Inratoal jt of ns Tne Mourad Maric Sem) passed by he Ameren Soy [er Toning sn ue fe Rae St Pindip, Pa 191 ‘This Standard, prepared by the Metal Powder Industries Federation, a aubjec a porlode revision. Suggestions for vision should be addressed 10 the Metal Powder Indusiiee Federation, 105 College Road East, Princoton, NJ. 08580-6692. Usors ot Standards are cautioned to secure MPIF Standard Test Methods METAL POWDER INDUSTRIES FEDERATION Method for Determination of Acid Insoluble Matter in Iron and Copper Powders MPIF Standard 06 Issued 1948, Revised 1954, 1964, 1974, 1983, 1988 4. SCOPE pes pas S; 4, PROCEDURE 1 2 This standard describes an analytical method for determination of the acid insolubles content of ele ‘mental jron and copper metal powders. “The acid insolubles referred to are non-base elemen- tal materials which are not completely soluble in ordinary mineral acids. These are generally consid- cred to be silica and silicates, carbides, alumina, clays or other refractory oxides and some dificutly solu- ble iron oxides which may be present in the raw ‘material from which the powders are made or intro- ‘duced in their manufacturing processes. This method. ‘excludes insoluble material that is volatile or com- bbustible at the specified ignition temperature. This standard may involve hazardous materials, operations, and guipment. Til standard does not purport to adres al of he Dotenal safety probloms associated wih use. IIs the Fesponsbliy ofthe se of this sondard fo establh appropiate Syfery ond health practices and fo determin the appeabilty of Tegulatory lintations prior we 2, APPARATUS Hot Plate Mull furnace capable of operating at 1800°F (980 250 and 750 ml. casserole or beaker. Glass funnel Quartz or porcelain crucible, Desiceator. ‘Analytical Balance having a sensitivity of 0.1 mg. Fine filter paper (ashless grade), Whatman #41 or equivalent, Reagents for use with Iron Powder. HCI- 1+ Hel- 1425. HINO, - I+1. ‘Reagents for use with Copper Powder. HHNOs - 141 NH ——_—_——————————— 3. TEST SPECIMEN 31 MIF ‘The test specimen shall be 5 g of metal powder, obtained in accordance with MPIF Standard 01 “Sampling Finished Lots of Metal Powders,” weighed to the nearest 0.001 g. Standard Test Methods 41 alt 42 42 421 422 NOTE Iron Powder Place the 5 g sample in @ 750 mL casserole. Add 100 mL of HCI (1+1) with caution and cover with watch glass. Allow the solution to stand at room temperature until reaction is complete, Place casserole ‘on hot plate. Heat to boiling point and hold until reaction ceases. Add 150 mL of distilled water and reheat to boiling point. Filter using a fine paper and ‘wash the residue on the filter paper alternately with hot distilled water and hot HCl (1+25) (a total of six times) to insure that all iron salts are dissolved, 1 — If it is desired to exclude carbides as part of the insoluble matter, add 20 mL of concentrated HINOs to the HCl (i+1) and proceed as indicated above. This will prevent the inclusion of combined carbon with the insoluble matter being determined. ‘Weigh a crucible to the nearest 0.0001 g and place the filter paper and residue in it, Dry and place in muffle furnace at 1800° F (980° C). Burn off the paper for one hour. Cool in the desiccator. Re-weigh crucible and ash to the nearest 0.0001 g. Copper Powder Place the 5 g sample in a 250 mL casserole. Add 100 mL. of HNO: (I++1) and cover with watch glass. Allow the solution to stand at room temperature until the reaction is complete. Place casserole on hot plate. Heat to boiling point. Boil to half volume. Add distilled water to bring volume to approximately 100 mL. Heat solution to boiling point and filter using. fine paper. Wash filter with hot distiled water until all traces of blue color disappear. Weigh the crucible to the nearest 0.0001 g and place the filter paper and precipitate in it. Dry and place in muffle furnace at 1800°F (980°C) for one hour. Cool in the desiccator. Weigh crucible and ash to the nearest 0.0001 g. The difference in weight is the insoluble matter. 2 — If the ignited residue is suspected to contain tin oxide, add 5 g of NHL to the crucible and heat in a furnace at 425-475° F (220-250° ©) for 15 minutes. After the fumes have disappeared, remove the crucible and cool. Add 2 to 3 mL. of HNOs, ‘evaporate to dryness, ignite, and weigh. Repeat the treatment with NHL and HNO; until constant weight is obtained. The loss in weight represents tin oxide. (MPIF Standard No. 06 — page 20f2) 5. CALCULATIONS 5.1 Calculate the percentage of total insoluble matter as follows: Total insoluble matter, % where: A= weight of crucible and ash after ignition, in ‘grams, ‘weight of crucible, in grams, and ‘grams of sample used. B c 6. REPORT 6.1 Report the total insoluble matter as a percentage to the nearest 0.01%. APPENDIXES ‘Al. REPORT ON PRECISION OF MPIF STANDARD 06 A.L1 A planned testing program was carried out among laboratories employing this method to determine precision. A complete report on this work is available in the offices of the Metal Powder Industries Federation. A.L2. This report concludes that this method is operable with the following average precision, A121 Iron Powder - +12.6% A.1.22 Copper Powder - £11.69 42. COMPARABLE STANDARDS ASTM E 194 180 4496 yin he iin en th. he iy a ‘any ses Pus ar tame yah aby. Sh trod ii et ep tins in ‘Sting re otung the prope mural fore presar ‘Pi tad dns oy apt pret y PE man cr on mer om ‘erie oe pot ced nr fing pe [Boles provid in ASTM E380 Standard Proce for Use ofthe Inematina Syacm of Unis The Mountz Metis Syston, pte! bythe Amen Sse [er oning sd Mule Race Set, Pla PA 1108. ‘This Standard, prepared by the Metal Powder Induces Federation, is subject to periodic revision, Suggestions for revision should be addressed to the Motal Powder Indust Federation, 105 College Road Easi, Princeton, N-J. 08540-6692. Users of Standards are cautioned to secure the latest exitons, Complete edton of standards may be obtained fem the Federation atthe above address. MPIF Standard Test Methods METAL POWDER INDUSTRIES FEDERATION Method for Determination of Iron Content and Iron Oxide Content of Iron Powder MPIF Standard 07 ————um— 4. SCOPE 1 12 ‘These methods cover procedures for the chemical analysis of granular iron powder to determine: Total Tron Content (4), Metallic Iron Content (5), and Ferric and Ferrous Oxide Content (6). The following methods have been established to provide simple and direct procedures for determin- ing the total and metalic iron content and iron oxide content of iron powder such as that used in powder ‘metallurgical applications. The precision ofthis Stand- ard when carefully used is shown in the Appendix. This standard may involve hazardous materials, operations, and Gquipmont. This standard does not purport to addrese all of the potenial safty problems associated with ts use. It the ‘esponsibility ofthe tae of ths standard 0 establish opproprite tery and health practices and to determine the applicability ‘of regulatory lmlatons prior to use. ——$———————— 2. APPARATUS ‘The following apparatus is required. Fume hood suitable for use with perchloric acid, Titrating apparatus, Filtering apparatus. Source of carbon dioxide or nitrogen. Tank nitrogen ‘or CO» is the most convenient source although CO: ‘may be satisfactorily generated in a simple glass gas ‘generator by adding H:SO« drop by drop toa solution of sodium carbonate, (Not required to determine Total Iron Content) ——_—_—_—_—_——— 3. TEST SPECIMEN 3.1 The test specimen for each of the procedures which follows is obtained in accordance with MPIF Standard O1, Sampling of Finished Lots of Metal Powders, and shall be 0.500 g weighed to the nearest 0.001 g. NOTE 1—Special precautions should be followed for the disposal of the solutions involved because of the use cof mercury and strong acids in these procedures. —_—eee—e—— 4, PROCEDURE FOR DETERMINATION OF TOTAL IRON CONTENT IN IRON POWDER 41 4d Reagents erchloric acid (70 percent). Perehlorc acid can be used safely as specified in the procedure, It should not, however, be brought in contact with finely divided ‘luminusn, silicon or organic matter. MPIF Standard Tost Methods 412 413 414 415 416 ald 418 419 4110 41 424 422 423 Issued 1949, Adopted 1954, Revised 1961, 1977, 1365, 190 = SepeSpas Stannous chloride solution — fully dissolve 12.5 g of SnCly-2H.0 in 25 mL of HCI and dilute to 250 mL. Keep stoppered. Mercuri chloride solution (saturated). ‘Titration solution — add 15 mL of HS0« and 15 mL of HPO, and 10 mi. of distilled water. Standard potassium dichromate solution (0.05 N). Sodium diphenylamine sulfonate solution—add 0.32 ‘oflbarium diphenylamine sulfonate to 100 mL of NasSO« (10 percent) and filter from residue Ferric sulfate solution (100 g per 1000 mL). ure electrolytic iron wire or powder. Certified analy- sis samples may be obtained from the National Bureau of Standards, Washington, D.C. [Nitric acd (concentrated). Nitric acd (I part HNO) + 1 part HO). Hydrochloric acid (2 parts HCI + I part H:0), Procedure Procedure 42.1 is recommended for the usual com- ‘mercial iron powders and where it is undesirable to use perchloric acid. Procedure 4.2.2, which uses perchloric acid, is an alternate procedure, Procedure 422 is recommended for use on iron powders high in chromium and other elements that may be difficult to dissolve by procedure 42.1 ‘Non-perchloric acid method: Weigh 0.500 g of sample into 600 mL beaker. Add 15 mL of HCl (+1), cover and heat gently until action ceases. Add cautiously 5 mL of concentrated HNOs. Place a glass rod in the beaker, cover and evaporate slowly to about 5 mL, ‘Add 15 mL of HCI (2+1) and heat gently to redissolve ‘any precipitate formed. Wash down the cover glass and. sides ofthe beaker and proceed as in 4.23 except omit the 3 mL of HC. Perchloric acid method: Weigh 0.500 g of sample into {600 ml. beaker. Add 2 mL. of water, 10 mL of HNO, (11) and 10 mL of HCI @+1). Cover and heat gently until ation ceases. Place glass rod in the beaker during heating so that any condensate will strike the rod and prevent loss of solution due to spattering. Add 10 mL ‘of HCI, (70 percent) and evaporate slowly in the fame hhood to dense fumes of HCIO,. Cool slightly. Wash down cover and sides of beaker with about 10 mL ‘of water and repeat evaporation in the fume hood to dense fumes. A second evaporation is not necessary if all dark particles are in olution. Proceed as in 42.3. Cool, make up to $00 mL. in volumetric flask and take 100 mL. with a pipette back into the original beaker. (MPIF Standard No. 07 — page 2 of 3) E = grams of sample in aliquot. Add 3 mL of HCI and boil several minutes to expel 5.1.5 Ferric sulfate solution (100 g per 1000 mL). fiee chlorine, Then add SnCk solution drop by drop 5.1.6 Pare electrolytic iron wire or powder. to the boiling solution to reduce the iron to the ferrous 5.2 Procedure ‘state, as indicated by a change from bright yellow to 5.2.1 Weigh 0.500 g of sample into a dry 500 mL Erlenmeyer colores, Provide an exces of one, but not more than flask and shake to distribute the sample evenly over two drops of Sn. solution. Cool to approximately the bottom, Provide the flask with a bunsen valve TPF GPC), Add 10 mL of HgCh solution. Str well and displace the air with CO: or nitrogen, Add 150 and allow to stand for about three minutes, mL of HgCh solution to the flask and. heat. Boi 424 Dilute to about 300 mL with cold, recently boiled gently for five minutes dist water. Add 25 mL of the titrating solution and 52.2 Cool to approximately 77°F (25°C) but do not allow 2 raL-of sodium diphenylamine sulfonate as indicator sir-to be drawn into the flask during the cooling “Titrate with standard 0.05 N’KxCnO; solution to a Period. Fitter the cooled solution into a 300 mL. volue permanent purple coor Inetric flask, washing the flask and: paper well with 43° Blank determination water, Dilute to the mark and mix thoroughly. To make a blank determination, follow the same 52.3 Take 100 mL of the solution with a pipet and procedure and use the same amounts of reagents. transfer to 600 ml. beaker. Dilute to about 300 ml. Immediately before titration, add I mL. of Fes SO); with cold, recently boiled disled water. Add 25 mL. solution. Standardie the 005 N K:CnOy against pure of the titrating solution and 2 mL of sodium iron wire or high purity electrolytic iron powder. diphenylamine sulfonate as indicator and titrate with 44 Caleuations standard 0.05 NKsCa0r solution to @ permanent 44.1 Caleulate the factor forthe standard K:Cn0; trating purple color. solution as follows: 53. Blank determination To make a blank determination, follow the same B procedure and use the same amounts of reagents Factor A= Immediately before titration, add I mL. of FeSO.) nee cD solution. Standardize the 00S N KsCrO> against pure A etison per miL of standard KsCrs0r, ee ee purity electrolytic iron powder. grams of pure electrolytic iron used 10 stan- $4.1 Calealate factor (C for titrating solution in the dardize the K:ChO> solution, tranne indie inthe, previous deemnaton C = mL of K:Cx0; solution required to trate the for total iron content under “Calculations.” pure iron, and. late jercentage of metallic iron as follo D = tal of RCO solution required to titrate the "42 Callulate the percentage of metallic ies blank. C(AB) 442 Caeulate the peroentage of total iron a follows: Metalic Iron, F A(C-D) Total Iron, % ="; 100 where: < A~ mL of K:Cn0; solution required to titrate the where: sample, [A= factor fr titrating solution = grams of iron per B= mL of K:CnOy solution required to titrate the rm of K:Ct0; solution, blank, : ele aan cicor sake ee tea = factor for titrating solution - grams of iron per sample, mL of KiCr0> solution, and D = mL-of K:Ci0; solution required to titrate the D = grams of sample in aliquot blank, and 6. PROCEDURE FOR DETERMINATION OF FERRIC AND FERROUS OXIDE CONTENTS IN IRON POWDER 5. PROCEDURE FOR DETERMINATION OF METALLIC IRON IN IRON POWDER 6.1 Reagents 51 Reagents: 6.1L Sulfuric acid (I+4) - mix 15 mL. of H:80. with 60 Si. Mereutie chloride solution - add 7 g of HgCh to iL of water. about 150 mL of recently boiled distilled water and 6.1.2 Titrating mixture - add 15 mL of H:SO« and 15 mL. heat to dissolve. of H;PO, to 70 mL. of distilled water. 5.12 Titrating solution - add 15 mL of H:SO. and 15 6.1.3 Sodium diphenylamine sulfonate solution-add 0.32 mL of HsPO« to 70 mL of distilled water. of barium diphenylamine sulfonate to 100 mL of 5.13 Standard potassium dichromate solution (0.05 N). 'NasSOs (10 percent) and filter from residue 5.14 Sodium diphenylamine sulfonate solution—add 6.14 Standard potassium bichromate solution (0.05 N). 0.32 g of barium diphenylamine sulfonate to 100 ml. 6.1.5 _ Ferric sulfate solution (100 g per 1000 mL) cof Na:SO (10 percent) and filter from residue. 6.16 Pure electrolytic iron wire or powder. MPIF Standard Test Methods (PIF standard No. o7 — page 8 of 3) 622 623 63 64 641 642 643 644 Procedure ‘Weigh 0,500 g of sample into a dry 500 ml. Erlenmeyer flask and shake to distribute the sample evenly over the bottom. Provide the flask with a bunsen valve ‘and displace the air with CO; or nitrogen. Add 60 mL of H:S0: (I+4), Heat to about 120 to 140°F (50 to 60° C) until sample is completely dissolved, then increase the heat and boil for 1 to 2 minutes. Cool solution to approximately 77°F (25°C). Transfer the entire sample to a S00 mL. volumetric flask, fill to the mark and mix thoroughly. Measure out 100 ‘mL of the solution with a pipette and transfer to a 600 ml. beaker. Dilute to about 300 mL with cold, recently boiled distilled water. Add 25 ml of the titrating solution and 2 mL of sodium diphenylamine sulfonate as indicator. Titrate with standards 0.05 N K.CriO; solution to a permanent purple color. ‘This titration gives both metallic iron and iron present as FeO. Blank-Determination To make a blank determination, follow the same procedure and use the same amounts of reagents Immediately before titration, add 1 mL of Fes (SO.)s solution, Standardize the 0.05 N KsCr,0r against pure iron wire or high purity electrolytic iron powder. Calculations Calculate the factor (C) for the titrating solution in the same matter as indicated in the first determination for total iron content under “Calculations.” Calculate the percentage of iron present as metallic igon and FeO as follows: ce Iron as Fe and FeO, % =" DX 100 where: (A= mL of K:ChO; solution required to titrate the sample, ‘mL of K:Cr0> solution required to titrate the blank, C = factot for titrating solution - grams of iron per ml of KsCn0; solution, and D = grams of sample in aliquot. Calculate the percentage of FeO as follows: where: G = percent total iron as determined in previous analysis for total iron content in iron powder, and E= percent iron as Fe and FeO calculated in 6.4.2 —_—_—_——— APPENDIX AL. Report on Precision of MPIF Standard 07. ‘ALI. A round robin test on three iron powders was conducted by eight laboratories. A complete report is available in the offices of the Metal Powder Industries Federation. 12, Summary of results of determination of total iron in iron powder: FeO, % 2865 (E - where: percent iron as Fe and FeO calculated in 6.4.2. percent metallic iron as determined in previous Analysis for metalic iron content in iron powder. Calculate percentage FexOs as follows: Fei0s, 96 = 1.4298 (G-E) Iron Powder Total Iron Contents, % Sample NX R ° v A 21 9735-102 05330548 B 25° 9799 «152 0.368 0.376 c 25° «9783-181 «0495—(0.508. A13. Summary of results of determination of Metallic iron in iron powder. Iron Powder ‘Total Metallic Iron Content, 9 Sample Ne R o ‘A 22 9484 +166 (0.620 ~—«0.654 B 29521169 OS1S OSA c 209345 «2.930839 0898 where: N= total number of analyses made on each sample by agiven procedure, X = average or arithmetic mean on N test results, R= range which is the difference between the largest and smallest of N test results, 9 = standard deviation defined as the square root of the averages of the squares of the deviation ‘of the numbers from their average, X, and, V = coefficient of variation defined as the standard deviation, 0, expressed as a percentage of the average, X 2. COMPARABLE STANDARDS None Distance aon of tse sana ops tte wh epee vali fy ant rcton here ad ie el Powder nes Peden Set, rare etic nse enone ig the manasa! Ee or gee "ue secs aon th pc et a oe se init iso= 1 een neat nde cher to site phe SSeS tinge proper mera obispo. Exc of wt ptr Str destin ay eet eo any MPF ener ener oo incre er allng ese ot loess or om ane P= ‘hes or eget tran hme ted nt tnd ies orca ott nw iain Senda __ Titec js ast tool Stunde or Ue of Imai Siecwrar Unis The Mournaré Meri Sse, psd bye Ariesean Sot ‘eToung set Mans face Suet, Pcp PA 1910 ‘Tis Standaré, propared by the Metal Powder Industies Federation, the Metal Powder Industries Federation, 105 College Road East, Ts saben fo povodc revision, Suggestions fr revision should be adéressad to ‘princeton, NJ. 08840-6602. Users of Standards are cautloned to secure the latest eatons. Complete editon of standards may Be obtained from the Federation atthe above adress, METAL POWDER INDUSTRIES FEDERATION Definition of Terms Used in Powder Metallurgy MPIF Standard 09 Issued 1950, as tentative, Adopted 1953 and Revised in 1962, 1971, 1985, 1990, 1992, 1994 1. SCOPE 1 This standard includes definitions of those terms that are necessary for the interpretation and application ‘of powder metallurgy and other related standards that are not adequately defined in common language, to ‘ensure consistency of usage, proper understanding, and precise interpretation. ‘Absolute Pore Sie — The maximum pore opening of a porous material, such as a filter through which no larger particle will pass. Synonymous with maximum Pore Size. ‘Acicular Powder — Needle shaped particles. ‘Activated Sintering — A process by which the rate of sinter- ing is significant increased by means other than changing time or temperature, eg. addition of a constituent to the powder, or the atmosphere, or thermal cycling. Agglomerate — Several particles adhering together. Air Classification — The separation of powder into particle size fractions by means of an air stream of controlled velocity. Alloy Powder — See Pre-alloy Powder. Angle of Repose — The basal angle of a pile formed by 1 powder when freely poured under specified conditions conto @ horizontal surface Apparent Density — The weight of a unit volume of powder, usually expressed as grams per cubic centimeter, deter- ‘ined by a specified method. ‘Apparent Hardness — The value obtained by testing a sin- ‘ered material with standard indentation hardness equip- ment. Since the reading is a composite of pores and solid material, itis usually lower than that of solid material of the same composition and condition. Not to be confused with particle hardness. Atomization — The dispersion of a molten metal into parti- cles by a rapidly moving gas or liquid stream or by ‘mechanical means. Atomized Metal Powder — Metal powder produced by the dispersion of a molten metal by a rapidly moving gas or liquid stream, or by mechanical means. Binder — A cementing medium; either a material added to the powder to increase the green strength of the ‘compact, and which is expelled during sintering; or a ‘material (usually of relatively lower melting point) added toa powder mixture for the specific purpose of cementing together powder particles which alone would not sinter into a strong body. LMPIF Standard Test Methods Spee m [Ss Blank — A. pressed, presintered or fully sintered compact, usually in the unfinished condition, requiring cutting, machining, or some other operation to give it its final shape, See Preforming. Blending — The thorough intermingling of powders of the ‘same nominal composition (not to be confused with mixing). Bridging — The formation of arched cavities in a powder Briquet — See Compact. Bulk Density — The density of a powder under non-specitied conditions, for example in a shipping container. ‘Burn Off — That stage of a sintering cycle referring to the time and temperature necessary to remove ingredients used to assist the forming of a powder metallurgy part, such as binders or die lubricants. Cake — A coalesced mass of unpressed metal powder. Carbonyl Powder — A metal powder prepared by the thermal ‘decomposition of a metal carbonyl. Cemented Carbides — A solid and coherent mass made by pressing and sintering a mixture of powders of one or more ‘metalic carbides and a much smaller amount of a metal, such as cobalt, to serve as a binder. Chemically Precipitated Metal Powder — Powder produced by the replacement of one metal from a solution of its salts by the addition of another element higher in the electro chemical series, or by other reducing agent. (Classification — Separation of a powder into fractions according to particle size. Closed Pore — A pore not communicating with the surface. Coining — The pressing of a sintered compact to obtain a definite surface configuration (not to be confused with Repressing or Sizing) Cold Pressing — The forming ofa compact at room temperature. Cold Welding — Cohesion between two surfaces of metal, ‘generally under the influence of externally applied pres- sure at room temperature. Comminuted Powder — A powder produced by mechanical disintegration of solid metal ‘Communicating Pores — See Interconnected Porosity ‘Compact — An object produced by the compression of metal powder, generally while confined in a die, with or without the inclusion of nonmetallic constituents. Synonymous with Briquet. (PIF starard No. 09 —pago 2016) ‘Compactibility — The capacity of a metal powder to be pressed into a desired shape which maintains its integrity uring subsequent processing. Compactbilty isa function of both compressibility and green strength, ‘Compacting Tool Set — See Die. Composite Compact — A metal powder compact consisting of two or more adhering layers, rings, or other shapes of different metals or alloys with each layer retaining its original identity. Composite Powder — A powder in which each particle consists of two or more separate materials. ‘Compound Compact — A metal powder compact consisting of mixed metals, the particles of which are joined by pressing or sintering or both, with each metal particle retaining substantially its original composition. Compressibility — The capacity of a metal powder to be densified under a uniaxially applied pressure in a closed die. Compressibility is measured in accordance with (MPIF Standard 45 and may be expressed numerically as, the pressure to reach a required density or, altematively, the density ata given pressure, Compression Ratio — The ratio of the volume of the loose powder to the volume of the compact made from it Synonymous with Fill Ratio. Continuous Sintering — Presintering, or sintering, in such ‘manner that the objects are advanced through the furnace at a fixed rate by manual or mechanical means. Core Rod — The separate member of the compacting tool set or die that forms a hole in the compact. Cracked Ammonia — See Dissociated Ammonia. (Cut — See Fraction. Dendritic Powder — Particles, usually of electrolytic origin, ‘having the typical pine tree structure, Density (Dry) — The weight per unit volume of an unim- pregnated P/M part Density (Wet) — The weight per unit volume of a P/M part, impregnated with oil or other nonmetallic materials. Density Ratio — The ratio of the determined density of @ compact to the absolute density of metal of the same composition, usually expressed as a percentage. Syn- ‘onymous with % Theoretical Density. Die — The part or parts making up the confining form in which a powder is pressed. The parts of the die may be some or all of the following: Die body, punches, and core rods. Synonymous with Mold and Compacting Tool Set. Die Body — The stationary or fixed part of a die. Die Insert — A removable liner or part of a die body or punch. Synonymous with Die Liner. Die Lubricant — A lubricant mixed with the powder or applied to the walls of the die and punches to facilitate the pressing and ejection of the compact. Die Set — The parts of a press that hold and locate the die in proper relation to the punches. Dimensional Change — See Growth; See Shrinkage. Dispersion-Strengthened Material — A material consisting of a metal and a finely dispersed, substantially insoluble, ‘metallic or nonmetallic phase. Dissociated Ammonia — A reducing gas produced by the thermal decomposition of anhydrous ammonia over a catalyst, resulting in a gas of 75% hydrogen and 259% nitrogen. Synonymous with Cracked Ammonia Double-Action Pressing — A method by which @ powder is pressed between opposing punches both moving relative to the die. Electrolytic Powder — Powder produced by electrolytic ‘deposition or the puverization ofan electrodepost. Endothermic Atmosphere (Gas) — A reducing gas atmo- sphere used in sintering and produced by the reaction of 4 hydrocarbon fuel gas and air over a catalyst with the aid of an external heat source. Its low in carbon dioxide and water vapor with relatively large percentages of hydrogen and carbon monoxide, Maximum combustibles approximately 60% Equi-axed Powder — See Granular Powder. Exothermic Atmosphere (Gas) — A reducing gas atmosphere used in sintering and produced by partial or complete combustion of a hydrocarbon fuel gas and ai. Maximum combustibles approximately 25% Exudation — The action by which all or a portion of the Jow melting constituent of compact isforced to the surface during sintering, Sometimes referred to as “bleed out”. Synonymous with Sweating, Ferrite — In the field of magnetics, substances having the general formula: MO, Mo™“0s the trivalent metal often being iron Fill Ratio — See Compression Ratio. Fines — The portion of @ powder composed of particles Which are smaller than a specified size, currently less than 44 micrometres. See also Superfines. Flake Powder — Flat or scale-like particles whose thickness is small compared with the other dimensions. Flow Rate — The time required for a powder sample of standard weight to low through an orifice in a standard instrument according toa specitied procedure. Fluid Permeability — See Permeability (Fu). Fraction — That portion of a powder sample which lies between two stated particle sizes, Synonymous with Cut MPIF Standard Test Methods (PIF Standard No. 09 — page 3 of 6) dea eee eee el Gas Classification — The separation of powder into particle size fractions by means of a gas stream of controlled velocity Granular Powder — Particles having approximately equi- dimensional non-spherical shapes. Granulation — A general term for the production of coarse smetal powiders using methods such as: a. Pouring the molten metal through a sereen into water Ghotting), b. Violent agitation of the molten metal while solidifying, ¢. Agglomeration of smaller particles. Green — Unsintered (not sintered); for example: Green compact, green density, green strength Green Expansion — The increase in dimensions ofa compact relative tothe die dimensions after being ejected from die, measured at right angles tothe direction of pressing. Growth — An increase in dimensions of a compact occurring

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