1、Designation: E50 11Standard Practices forApparatus, Reagents, and Safety Considerations forChemical Analysis of Metals, Ores, and Related Materials1This standard is issued under the fixed designation E50; the number immediately following the designation indicates the year of originaladoption or, in
2、the case of revision, the 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 The
3、se practices cover laboratory apparatus and reagentsthat are required for the chemical analysis of metals, ores andrelated materials by standard methods of ASTM. Detaileddescriptions of recommended apparatus and detailed instruc-tions for the preparation of standard solutions and certainnonstandardi
4、zed reagents will be found listed or specified inthe individual methods of analysis. Included here are generalrecommendations on the purity of reagents and protectivemeasures for the use of hazardous reagents.1.2 These recommendations are intended to apply to theASTM methods of chemical analysis of
5、metals when definitereference is made to these practices, as covered in Section 4.1.3 The values stated in inch-pound units are to be regardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered standard.1.4
6、 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of whoever uses this standard to consult andestablish appropriate safety and health practices and deter-mine the applicability of regulatory limitations prior to use.Specifi
7、c hazards are given in Section 8.NOTE 1The use of the verb “shall” (with its obligatory third personmeaning) in this standard has been confined to those aspects of laboratorysafety where regulatory requirements are known to exist. Such regula-tions, however, are beyond the scope of these practices.2
8、. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE1 Specification for ASTM Liquid-in-Glass ThermometersE77 Test Method for Inspection and Verification of Ther-mometersE100 Specification for ASTM HydrometersE126 Test Method for Inspection, Calibration, and Verifica-tion
9、of ASTM HydrometersE287 Specification for Laboratory Glass Graduated BuretsE288 Specification for Laboratory Glass Volumetric FlasksE438 Specification for Glasses in Laboratory ApparatusE542 Practice for Calibration of Laboratory VolumetricApparatusE694 Specification for Laboratory Glass Volumetric
10、Appa-ratusE969 Specification for Glass Volumetric (Transfer) PipetsE1044 Specification for Glass Serological Pipets (GeneralPurpose and Kahn)E1621 Guide for X-Ray Emission Spectrometric Analysis3. Terminology3.1 For definitions of terms used in these practices, refer toTerminology E135.4. Significan
11、ce and Use4.1 The inclusion of the following paragraph, or a suitableequivalent, in any standard (preferably after the section onScope) is due notification that the apparatus and reagentsrequired in that standard are subject to the recommendationsset forth in these practices.“Apparatus and ReagentsA
12、pparatus and reagents required for each de-termination are listed in separate sections preceding the procedure. Appa-ratus, standard solutions, and certain other reagents shall conform to therequirements prescribed in ASTM Practices E50, for Apparatus, Reagents,and Safety Considerations for Chemical
13、 Analysis of Metals, Ores, and Re-lated Materials.”4.2 It is assumed that the users of these practices will betrained analysts capable of performing common laboratoryprocedures skillfully and safely. It is expected that work will beperformed in a properly-equipped laboratory.1These practices are und
14、er the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and are the directresponsibility of Subcommittee E01.20 on Fundamental Practices.Current edition approved Oct. 15, 2011. Published November 2011. Originallyapproved in 1943. Last previous edition
15、 approved in 2005 as E5000 (2005). DOI:10.1520/E0050-11.2For 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 standards Document Summary page onthe ASTM website.1Copy
16、right ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.TABLE 1 Chemical Reagents Specified in ASTM Methods for Chemical Analysis of MetalsName Formula* Acetic acid CH3COOHAcetone CH3COCH3Acetylacetone (2,4-pentanedione) CH3COCH2COCH3Alizarin-Red
17、-S C6H4COC6H-1,2-(OH)2-3-SO3NaCOAluminon (aurintricarboxylic acid-ammoniumsalt)(4-HOC6H3-3-COONH4)2C:C6H-3-(COONH4):OAluminum metal (99.9 % min) Al* Aluminum metal (sheet or rolled foil) AlAluminum ammonium sulfate Al2(NH4)2(SO4)424H2OAluminum nitrate Al(NO3)39H2OAluminum sulfate Al2(SO4)318H2OAlumi
18、num oxide, fused (Alundum)1-Amino-2-naphthol-4-sulfonic acid NH2C10H5(OH)SO3HAmmonium acetate CH3COONH4Ammonium benzoate C6H5COONH4Ammonium bifluoride NH4FHFAmmonium bisulfate NH4HSO4Ammonium bisulfite NH4HSO3Ammonium carbonate (NH4)2CO3* Ammonium chloride NH4Cl* Ammonium citrate CH2(COONH4)C(OH)(CO
19、OH)CH2COONH4Ammonium fluoride NH4F* Ammonium hydroxideANH4OHAmmonium iodide NH4IAmmonium molybdate (NH4)2MoO4* Ammonium heptamolybdate tetrahydrate (NH4)6Mo7O244H2OAmmonium nitrate NH4NO3* Ammonium oxalate NH4OCOCOONH4H2O* Ammonium phosphate, dibasic (diammoniumacid phosphate)(NH4)2HPO4* Ammonium pe
20、rsulfate (ammoniumperoxydisulfate)(NH4)2S2O8* Ammonium sulfate (NH4)2SO4* Ammonium tartrate NH4OCO(CHOH)2COONH4Ammonium thiocyanate NH4SCNAmmonium vanadate NH4VO3Antimony metal (powder) SbAntimony trichloride SbCl3* Arsenic trioxide As2O3Asbestos (for use with Gooch crucible)Barium Chloride BaCl22H2
21、OBarium diphenylamine sulfonate (C6H5NHC6H4-4-SO3)2Ba* Benzoic acid C6H5COOHa-Benzoin oxime (benzoin anti-oxime) C6H5CHOHC:NOHC6H5Beryllium sulfate BeSO44H2OBismuth metal (99.9 % min) BiBoric acid H3BO3Bromocresol green (38,39,58,59-tetrabromo-m-cresolsulfonephthalein)C6H4SO2OC(C6H-3,5-Br2-2-CH3-4-O
22、H)2Bromocresol purple (58,59-Dibromo-o-cresolsulfonephthalein)C6H4SO2OC(C6H2-3-CH3-5-Br-4-OH)2Bromine (liquid) Br2Bromophenol blue (38,39,58,59-tetrabromophenolsulfonephthalein)C6H4SO2OC(C6H2-3,5-Br2-4-OH)21-Butanol CH3CH2CH2CH2OHButyl acetate (normal) CH3COOCH2CH2CH2CH3* Cadmium chloride CdCl2212 H
23、2OCadmium chloride, anhydrous CdCl2* Calcium carbonate (low-boron) CaCO3Carbon dioxide (gas) CO2Carbon dioxide (solid) CO2Carbon tetrachloride CCl4Carminic acid 1,3,4-(HO)3-2-C6H11O6C6COC6H-5-COOH-6-OH-8-CH3CO* Chloroform CHCl3Cinchonine C19H22N2OCitric acid HOC(COOH)(CH2COOH)2Cobalt metal CoCobalt
24、sulfate CoSO4CokeCongo red test paperCopper metal (99.9 % min) CuE50112TABLE 1 ContinuedName Formula* Copper metal (powder or turnings) CuCopper metal (P-free) CuCopper metal (Mn, Ni, and Co-free, less than0.001 % of each)CuCopper-rare earth oxide mixturem-Cresol purple (m-cresolsulfonephthalein) C6
25、H4SO2OC(C6H3-2-CH3-4-OH)2Cupferron C6H5N(NO)ONH4Cupric chloride CuCl22H2O* Cupric nitrate Cu(NO3)23H2O* Cupric oxide (powder) CuOCupric potassium chloride CuCl22KCl2H2O* Cupric sulfate CuSO45H2OCurcumin (2-CH3OC6H3-1-OH-4-CH:CHCO)2CH2Devardas alloy 50Cu-45Al-5ZnDiethylenetriamine pentaacetic acid(ca
26、rboxymethyl)iminobis(ethylenenenitrilo)tetraacetic acid)(HOCOCH2)2NCH2CH2)2NCH2COOH* Dimethylglyoxime CH3C:NOHC:NOHCH3N,N8 Diphenylbenzidine C6H5NHC6H4C6H4NHC6H5Diphenylcarbazide (1,5-diphenylcarbohydrazide) C6H5NHNHCONHNHC6H5* Disodium (ethylenedinitrilo) tetraacetatedihydrateSee (ethylenedinitrilo
27、) tetraacetic aciddisodium saltDithiol (toluene-3,4-dithiol) CH3C6H3(SH)2Dithizone (diphenylthiocarbazone) C6H5NHNHCSN:NC6H5Eriochrome black-T (1(1-hydroxy-2-naphthylazo)-6-nitro-2-naphthol-4-sulfonic acid sodium salt)1-HOC10H6-2-N:N-1-C10H4-2-OH-4-SO3Na-6-NO2* EDTA (Disodium salt) See (ethylenedini
28、trilo) tetraacetic aciddisodium salt* Ethanol C2H5OH* Ethyl ether (diethyl ether) C2H5OC2H5* (Ethylenedinitrilo) tetraacetic acid disodium salt HOCOCH2(NaOCOCH2)NCH2N(CH2COONa)CH2COOH2H2OEthylene glycol monomethyl ether (2-methoxy-ethanol)CH3OCH2CH2OH* Ferric chloride FeCl36H2O* Ferric nitrate Fe(NO
29、3)39H2OFerric sulfate Fe2(SO4)3nH2O* Ferrous ammonium sulfate Fe(NH4)2(SO4)26H2O* Ferrous sulfate FeSO47H2OFluoboric acid HBF4Fluorescein, sodium salt 2NaOCOC6H4C:C6H3-3(:O)OC6H3-6-ONaFormaldehyde HCHO* Formic acidAHCOOHGelatinGraphite CGlass woolGlycerol CH2OHCHOHCH2OHHydrazine sulfate NH2NH2H2SO4*
30、 Hydrobromic acidAHBr* Hydrochloric acidAHCl* Hydrofluoric acidAHFHydrogen chloride gas HCl* Hydrogen peroxide H2O2Hydrogen sulfide gas H2SHydroquinone 1,4-(OH)2C6H4* Hydroxylamine hydrochloride NH2OHHCl* Hypophosphorus acidBH3PO2Invert sugar* Iodine I2Iron metal or wire (99.8 % min) FeIsopropyl eth
31、er (CH3)2CHOCH(CH3)2Lead metal Pb* Lead acetate Pb(CH3COO)2Lead chloride PbCl2* Lead nitrate Pb(NO3)2LitmusLithium fluoride LiFE50113TABLE 1 ContinuedName FormulaMagnesium metal (Sn-free) MgMagnesium perchlorate, anhydrous Mg(ClO4)2* Magnesium sulfate MgSO47H2OManganese metal (99.8 % min) MnManganou
32、s nitrate Mn(NO3)2Manganous sulfate MnSO4H2OMannitol CH2OH(CHOH)4CH2OHMarble chips* Mercuric chloride HgCl2* Mercury Hg* Methanol CH3OHMethyl isobutyl ketone (4-methyl-2-pentanone) CH3COCH2CH(CH3)2* Methyl orange (pp-dimethylamino)phenylazobenzenesulfonic acidsodium salt)4-NaOSO2C6H4N:NC6H4-4-N(CH3)
33、2Methyl purple formula unknown, patented* Methyl red (o-(p-dimethylamino)phenylazobenzoic acid)4-(CH3)2NC6H4N:NC6H4-2-COOHMolybdenum metal (99.8 % min) MoMolybdic acid, anhydride (molybdenum trioxide) MoO3Molybdic acid (ammonium paramolybdate) Assay: as MoO385 %Morin, anhydrous (28,3,48,7-pentahydro
34、xyflavone)5,7-(HO)2C6H2OC(C6H3-2,4-(OH)2):C(OH)COb-Naphthoquinoline (5,6-benzoquinoline) C10H6CH:CHCH:NNeocuproine (2,9-dimethyl-1,10-phenanthroline) (CH3)2C12H6N212H2ONickel metal (99.8 % min) NiNickel metal (sheet) NiNickelous nitrate Ni(NO3)26H2ONickelous sulfate NiSO46H2O* Nitric acidAHNO3Nitrog
35、en gas (oxygen-free) N2Nitrogen, liquid N2m-Nitrophenol NO2C6H4OH1-Nitroso-2-naphthol(a-nitroso-b-naphthol) NOC10H6OHNitroso-R-salt (1-nitroso-2-naphthol-3,6-disulfonicacid disodium salt)1-NOC10H4-2-(OH)-3,6-(SO3Na)2Osmium tetraoxide OsO4Oxalic acid (COOH)2Oxygen gas O2* Perchloric acidAHClO41,10-Ph
36、enanthroline (o-phenanthroline) CH:CHCH:NC:CCH:CHC:CN:CHCH:CHH2O* Phenolphthalein C6H4COOC(C6H4-4-OH)2* Phosphoric acid H3PO4Piperidine NH(CH2)4CH2Platinized quartzPlatinized silica gelPlatinum gauze Pt* Potassium biphthalate 1-KOCOC6H4-2-COOHPotassium bisulfate KHSO4* Potassium bromate KBrO3* Potas
37、sium bromide KBr* Potassium chlorate KClO3* Potassium chloride KCl* Potassium chromate K2CrO4Potassium columbate 4K2O3Cb2O516H2O* Potassium cyanide KCN* Potassium dichromate K2Cr2O7* Potassium ferricyanide K3Fe(CN)6Potassium ferrocyanide K4Fe(CN)63H2O* Potassium fluoride KF2H2O* Potassium hydroxide
38、KOH* Potassium iodate KIO3* Potassium iodide KIPotassium iodide starch paper* Potassium nitrate KNO3* Potassium m-periodate KIO4* Potassium permanganate KMnO4Potassium persulfate K2S2O8Potassium phosphate, monobasic KH2PO4* Potassium pyrosulfate K2S2O7* Potassium sulfate K2SO4E50114TABLE 1 Continued
39、Name FormulaPotassium tantalum fluoride K2TaFPotassium thiocarbonate K2CS3* Potassium thiocyanate KSCNPyrogallic acid (pyrogallol) C6H3-1,3-(OH)3Quinine sulfate (C20H24N2O2)2H2SO42H2O8-Quinolinol (8-hydroxyquinoline) HOC6H3N:CHCH:CHSebacic acid HOCO(CH2)8COOHSelenium (powder) SeSilicon dioxide (sili
40、ca) SiO2* Silver nitrate AgNO3Soda-limeSoda-mica mineral (CO2absorbent)Sodium acetate CH3COONaSodium arsenite NaAsO2Sodium azide NaN3* Sodium bicarbonate NaHCO3* Sodium bismuthate NaBiO3Sodium bisulfate see sodium hydrogen sulfate* Sodium bisulfate, fused see sodium hydrogen sulfate, fusedSodium bis
41、ulfite NaHSO3* Sodium borate Na2B4O710H2O* Sodium carbonate, anhydrous Na2CO3Sodium chlorate NaClO3Sodium chloride NaClSodium citrate HOC(COONa)(CH2COONa)22H2OSodium cyanide NaCNSodium diethyldithiocarbamate (C2H5)2NCSSNa3H2OSodium dimethylglyoximate CH3C(:NONa)C(:NONa)CH38H2OSodium diphenylamine su
42、lfonate C6H5NHC6H4-4-SO3NaSodium dithionite (hydrosulfite) Na2S2O4* Sodium fluoride NaFSodium hydrogen sulfate NaHSO4Sodium hydrogen sulfate, fused A mixture of Na2S2O7and NaHSO4* Sodium hydroxide NaOHSodium hypophosphite NaH2PO2H2OSodium molybdate Na2MoO42H2OSodium nitrate NaNO3Sodium nitrite NaNO2
43、Sodium oxalate NaOCOCOONaSodium perchlorate NaClO4Sodium peroxide Na2O2Sodium phosphate, dibasic, anhydrous Na2HPO4Sodium pyrophosphate Na4P2O710H2OSodium pyrosulfate Na2S2O7Sodium sulfate, anhydrous Na2SO4Sodium sulfide Na2S9H2OSodium sulfite Na2SO37H2OSodium sulfite, anhydrous Na2SO3Sodium thiocya
44、nate NaSCN* Sodium thiosulfate Na2S2O35H2O* Sodium tungstate Na2WO42H2O* Stannous chloride SnCl22H2O* Starch (C6H10O5)xSuccinic acid HOCOCH2CH2COOHSulfamic acid NH2SO3HSulfatoceric acid (ceric sulfate) H4Ce(SO4)45-Sulfosalicylic acid 2-HOC6H3-1-COOH-5-SO3H2H2OSulfur dioxide gas SO2* Sulfuric acidAH2
45、SO4* Sulfurous acidAH2SO3Talc* Tartaric acid HOCO(CHOH)2COOHTest lead PbTetrapropylammonium hydroxide (CH3CH2CH2)4NOHThioglycollic acid (mercaptoacetic acid) CH2SHCOOHThiourea NH2CSNH2Tin metal (99.9 %min) SnTitanium dioxide TiO2Titanium metal (low Sn) TiTriethanolamine (2,28,29-nitrilotriethanol) (
46、CH2OHCH2)3NE501155. Purity of Water and Reagents5.1 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Type I or II of Specification D1193. Type III or IV may beused if they effect no measurable change in the blank orsample.5.2 Reagen
47、tsUnless otherwise indicated, it is intendedthat all reagents conform to the specifications of the Committeeon Analytical Reagents of the American Chemical Societywhen such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high
48、 purity to permit its use without lessening theaccuracy of the determination. In addition to this, it is desirablein many cases for the analyst to ensure the accuracy of hisresults by running blanks or checking against a comparablesample of known composition.6. Reagents6.1 Concentrated Acids, Ammoni
49、um Hydroxide, and Hydro-gen PeroxideWhen acids, ammonium hydroxide, and hydro-gen peroxide are specified by name or chemical formula only,it is understood that concentrated reagents of the specificgravities or concentrations shown in Table 2 are intended. Thespecific gravities or concentrations of all other concentratedacids are stated wherever they are specified.6.2 Diluted Acids and Ammonium HydroxideConcentrations of diluted acids and ammonium hydroxide,except when standardized, are specified as a ratio stati
