1、Designation: E32 15Standard Practices forSampling Ferroalloys and Steel Additives for Determinationof Chemical Composition1This standard is issued under the fixed designation E32; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the
2、 year of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These practices include procedures for the sampling ofthe various ferroalloys and steel additives, either bef
3、ore or aftershipment from the plants of the manufacturers. They aredesigned to give results representative of each lot that will becomparable with the manufacturers guaranteed analysis forthe same lot. For check analysis, the purchaser may use anysampling procedure he desires, but the analytical res
4、ultsobtained on such samples shall not be a basis for complaint orrejection, unless the procedure followed is of an accuracyequivalent to that prescribed in these methods.1.2 In sampling ferroalloys and steel additives, seriouserrors often occur from contamination of the samples by ironfrom the samp
5、ling appliances. Therefore, special precautionsshould be observed to avoid this source of error. Metallic ironmay be removed with a magnet from nonmagnetic alloys; itsestimation in other alloys requires special analytical procedures(Note 1). To avoid this error, parts of crushers and pulverizingequi
6、pment contacting the samples shall be of steel or othermaterial showing a high resistance to abrasion of the typeinvolved.NOTE 1Metallic iron in ferrochromium and ferrosilicon may bedetermined as follows: Transfer5gofthesample of alloy to a 150-mLbeaker, add 25 mL of HNO3(1 + 3), cover, boil 5 min,
7、filter into a 250-mLbeaker, and wash with hot water. Add NH4OH in slight excess, heat toboiling, filter, and wash with hot water. Dissolve the precipitate on thepaper with a minimum quantity of hot HCl (1 + 2), wash the filter with hotwater, and titrate the iron by a standard procedure such as that
8、describedin Test Method E354.1.3 The values stated in SI units are to be regarded as thestandard. The inch-pound values in parenthesis are given forinformation only.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of th
9、e 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 Documents2.1 ASTM Standards:2E11 Specification for Woven Wire Test Sieve Cloth and TestSievesE135 Terminology Relating to Analytical Che
10、mistry forMetals, Ores, and Related MaterialsE354 Test Methods for Chemical Analysis of High-Temperature, Electrical, Magnetic, and Other Similar Iron,Nickel, and Cobalt Alloys3. Terminology3.1 For definitions of terms used in these practices, refer toTerminology E135.4. Significance and Use4.1 Thes
11、e practices for the sampling of ferroalloys and steeladditives are primarily intended to test such materials forcompliance with compositional specifications. It is assumedthat all who use these methods will be trained samplers capableof performing common sampling procedures skillfully andsafely.5. A
12、pparatus for Preparing Samples5.1 The following equipment is required for the preparationof analytical samples of ferroalloys:5.1.1 CrusherA strongly built jaw crusher capable ofrapidly crushing 100-mm (4-in.) lumps to sizes 6.4 mm (14 in.)and smaller shall be used. The crushing plates of this machi
13、neshall be made of a hard and abrasion-resistant steel, such asmanganese steel or a properly hardened alloy or hypereutectoidcarbon steel.5.1.2 Roll CrusherA roll crusher, the rolls of which arefitted with tires of hardened and tempered chromium steel toavoid iron contamination of the sample, shall
14、be used to reduce1These practices are under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and are the directresponsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved Dec. 15, 2015. Published February 2016. O
15、riginallyapproved in 1939. Last previous edition approved in 2006 as E32 86 (2006)1.DOI: 10.1520/E0032-15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standa
16、rds Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1the 6.4-mm (14-in.) pieces to a particle size that will pass theNo. 10 (2.00-mm) sieve and be retained on the No. 20(850-m) sieve.5.1.3 Riffl
17、esRiffles, also designated as Jones dividers, areusually preferable to the use of hand methods for dividingsamples. Riffles with openings of 12.7 mm, 25.4 mm, 50.8 mm,and 76.2 mm (12 in., 1 in., 2 in., and 3 in.) should be available;the12-in. riffle to be used for samples containing particles upto 3
18、.2 mm (18 in.) in size, the 1-in. riffle for samples containingparticles up to 9.6 mm (38 in.), the 2-in. for samples containingparticles up to 19.1 mm (34 in.), and the 3-in. for samplescontaining particles up to 50.8 mm (2 in.) in size. Riffles shouldbe of the enclosed type to reduce dust losses.
19、The use ofmultiple riffles is not approved.5.1.4 Mortar and PestleThe mortar and pestle shall bothbe made of properly hardened alloy steel of a kind and gradedesigned to resist severe abrasive forces (Note 2). Suitabledimensions of the mortar are 79.4 mm (318 in.) in outsideheight, 76.2 mm (3 in.) i
20、n outside diameter, 39.7 mm (1916 in.)in inside diameter, and 60.3 mm (238 in.) in inside depth, thebottom 12.7 mm (12 in.) of which shall be rounded. The pestleshall be 152 mm (6 in.) in length, 38.1 mm (112 in.) indiameter, and rounded at the bottom. The upper part of thepestle should be slightly
21、softer than the remainder in order todecrease the tendency to shatter. Both the mortar and pestle,after hardening, shall be polished with abrasive paper toremove all scale. The narrow clearance between the pestle andthe sides of the mortar reduces the dust loss.NOTE 2For example: steel mortars and p
22、estles of the followingcomposition, after proper hardening and tempering treatments, have beenfound satisfactory:Carbon, % 0.60Manganese, % 0.25Phosphorus, % 0.02Sulfur, % 0.02Silicon, % 0.25Chromium, % 1.25Tungsten, % 2.20Vanadium, % 0.10After machining annealed steel of this grade to the usual for
23、m anddimensions, each part is heated to between 760 C and 800 C, quenchedin a light, mineral quenching oil and tempered at once. The pestle may betreated by quenching the lower portion only, the upper portion beingpermitted to air cool, and then tempering the quenched portion.NOTE 3Mechanically oper
24、ated pulverizing equipment such as a ringpulverizer may be substituted for the mortar and pestle, provided suitabletests show that the use of such equipment does not affect the compositionof a sample of any material obtained by these methods.5.1.5 SievesThe sieves shall conform to SpecificationE11.6
25、. Unit Quantities for Sampling and Analysis6.1 Each shipment, except as otherwise agreed upon by thepurchaser and the manufacturer, shall constitute a unit forsampling and analysis. It is recommended that shipments ofany alloy exceeding 450 Mg (500 tons) be divided into smallerlots for sampling acco
26、rding to some plan best adapted to thematerial and conditions, such as each cast, each carload, eachladleful, or each binful.6.2 Division of SamplesIn these methods the term “di-vide” is used to indicate a division of a sample into twoapproximately equal parts of similar composition as in riffling.7
27、. Sampling Spiegeleisen and 15 % Ferrosilicon7.1 Spiegeleisen is generally cast in pigs and shipped inbulk. Since this alloy is very hard and somewhat tough,sampling is most accurately and easily accomplished duringthe tapping of the metal from the furnace or during thepig-casting operation by takin
28、g small spoonfuls and pouringthe metal quickly into a test mold designed to solidify the metalquickly and give a clean test pig that is easily broken. Samplingof the metal in the solid state is difficult, and is best done duringthe loading or unloading, except when the material is loadedfrom bins or
29、 unloaded by dumping. The procedure, therefore,may be varied to suit the conditions but shall always conformto the following requirements:7.1.1 Sampling at FurnaceThe purchaser may arrangewith the manufacturer to have the sampling done at thefurnace. If so, each shipment or each cast may constitute
30、a unitsample for analyzing. The sample shall be obtained by collect-ing portions with a spoon from the runner as the metal flowsfrom the furnace, unless the metal is treated in the runner orladle to change its composition, in which event the portionsshall be taken as the metal flows from the ladle t
31、o the pigcasting machine. In any case, at least two spoonfuls of metalshall be taken from each ladle, one spoonful while the firstthird of a ladleful is flowing into or from the ladle and thesecond while the last third is flowing. Each spoonful shall betaken in a manner to avoid collecting dirt or s
32、lag, and the cleanmetal shall be immediately poured into a clean shallow mold toform a thin chill casting from which small pieces approxi-mately equal in size may be readily broken. When thespiegeleisen is cast in sand beds, the molten metal being runfrom the furnace directly to the casting floor, t
33、he samples shallbe taken by dipping skimmed molten metal from the runnertrough and pouring it into a small quartered cast-iron buttonmold. A sample shall be taken in this manner to represent themetal being cast in each pig bed. From the test castings thusobtained to represent a shipment, approximate
34、ly equal portionsshall be taken and combined to form the sample which shallhave a gross mass of not less than 200 g. The sample shall thenbe alternately crushed in a mortar and sieved until it all passesthrough a No. 80 (180-m) sieve. If the sample is to beanalyzed by more than one laboratory, it sh
35、all be mixed, coned,and quartered upon glazed paper (Note 4). The sample orsamples thus prepared shall be thoroughly mixed, dried for 1 hat 105 C to 110 C, and preserved for analysis in well-stoppered bottles properly labeled for full identification, in-cluding the name of the material, the manufact
36、urer, the date,the cast or lot number, etc.NOTE 4Finished samples are frequently divided into four portions:one for the purchaser, one for the manufacturer, one for an umpire ifnecessary, and one held in reserve.7.1.2 Sampling Solid FormsWhen the metal is in the solidstate, a gross sample shall firs
37、t be collected by selectingrandom pigs or pieces at regular intervals during the loading orunloading. Surface sampling of piles of the material will notE32152give a representative sample. When piles of the material mustbe sampled, the pieces shall be selected according to somefixed plan which assure
38、s the obtaining of pieces comprising thegross sample from uniformly distributed points throughout, acondition requiring the moving of all or many of the pieces inthe pile. For lots of 45 Mg (50 tons) or larger, 1 pig or pieceshall be taken for each 9 Mg (10 tons), and for small lots thenumber of pie
39、ces shall be proportionately increased to 10pieces for a 9-Mg (10-ton) lot, or 5 pieces for a 0.9-Mg (1-ton)lot. The various pigs thus collected shall be broken approxi-mately in half by any convenient means, and one of the halvesof each pig shall be reserved. From the fractured surface ofeach of th
40、ese half pigs, an approximately equal portion shall betaken by any suitable means (as by spalling with a heavyhammer), care being taken by the sampler to see that thesespalls are not all from the outer edges of the pigs but at leastsome are obtained from the central portion, and that nonecontains po
41、rtions of the outer surface which may be contami-nated with sand or other foreign material. The spallings fromeach half pig as collected shall be placed in separate envelopesand weighed to the nearest 1 g. Each portion so selected shallbe of approximately the same mass.7.1.2.1 The portions shall the
42、n be combined to form thesample and alternately crushed (preferably in a hardened-alloysteel mortar) and sieved until it passes a No. 6 (3.35-mm)sieve. Between 280 g and 420 g (10 oz and 15 oz) shall then beseparated from the crushed sample by riffling and this portionshall be pulverized to pass a N
43、o. 80 (180-m) sieve. Thepulverizing of over-sizes is best done with the hardened steelmortar and pestle, while sieving frequently to keep the sizeclose to 180 m and prevent loss of dust. The pulverizedsample shall be thoroughly mixed upon glazed paper, dividedif necessary, labeled, and dried prior t
44、o analysis, in accordancewith 7.1.1.8. Sampling Ferrosilicon, Standard Ferromanganese,Silicomanganese, Ferrophosphorus, and 12 % to 15 %Zirconium Alloy8.1 Alloys in this group are shipped in both lump andcrushed form, in bulk as well as in containers. Carload lots aregenerally shipped in bulk, excep
45、t the finely crushed sizeswhich are usually shipped in containers. Different proceduresare required for sampling the lump and the crushed alloy, andthe work of sampling is most conveniently done while loadingor unloading.8.2 Lump Alloy (above 50.8 mm (2 in.) in size)In samplingbulk shipments, lumps
46、of average size shall be set aside for thesample at regular intervals in the ratio of one lump fromapproximately each 270 kg (600 lb). The sample shall beaccumulated throughout the loading or unloading operation sothat all parts of the shipment will be equally represented. If thealloy is in containe
47、rs, every fifth container shall be dumped,and one representative lump shall be taken from each 55 kg(120 lb) of alloy which is equivalent to one lump per 270 kg(600 lb) for the lot. The sample shall also include a represen-tative amount of edge metal, small lumps, and any fines thatmay be present. F
48、rom each of the lumps in the sample, thereshall be broken three small pieces each about 19 mm (34 in.) insize, one from each of two opposite surfaces (top and bottom,if present) and one from the center, the three pieces constitutinga partial vertical cross-section of the lump. Alternatively, asingle
49、 piece constituting an entire vertical cross section of thelump may be taken.8.2.1 The pieces, together with a representative portion ofany fines present, shall be combined and crushed to pass a6.4-mm (14-in.) sieve. Not less than 9 kg (20 lb) shall beseparated from the crushed sample by riffling and at least aquarter portion of this shall be rolled to pass a No. 10(2.00-mm) sieve. A 170-g to 220-g (6-oz to 8-oz) portionobtained by riffling (a larger amount when more than onesample is required) of the 2.00-mm sample shall then bepulverized to pass
