ASTM E50-11(2016)

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E50 − 11 E50 − 11 (Reapproved 2016)
Standard Practices for
Apparatus, Reagents, and Safety Considerations for
Chemical Analysis of Metals, Ores, and Related Materials
This standard is issued under the fixed designation E50; the number immediately following the designation indicates the year of original
adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript
epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope
1.1 These practices cover laboratory apparatus and reagents that are required for the chemical analysis of metals, ores and
related materials by standard methods of ASTM. Detailed descriptions of recommended apparatus and detailed instructions for the
preparation of standard solutions and certain nonstandardized reagents will be found listed or specified in the individual methods
of analysis. Included here are general recommendations on the purity of reagents and protective measures for the use of hazardous
reagents.
1.2 These recommendations are intended to apply to the ASTM methods of chemical analysis of metals when definite reference
is made to these practices, as covered in Section 4.
1.3 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical
conversions to SI units that are provided for information only and are not considered standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of
regulatory limitations prior to use. Specific hazards are given in Section 8.
NOTE 1—The use of the verb “shall” (with its obligatory third person meaning) in this standard has been confined to those aspects of laboratory safety
where regulatory requirements are known to exist. Such regulations, however, are beyond the scope of these practices.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
E1 Specification for ASTM Liquid-in-Glass Thermometers
E77 Test Method for Inspection and Verification of Thermometers
E100 Specification for ASTM Hydrometers
E126 Test Method for Inspection, Calibration, and Verification of ASTM Hydrometers
E287 Specification for Laboratory Glass Graduated Burets
E288 Specification for Laboratory Glass Volumetric Flasks
E438 Specification for Glasses in Laboratory Apparatus
E542 Practice for Calibration of Laboratory Volumetric Apparatus
E694 Specification for Laboratory Glass Volumetric Apparatus
E969 Specification for Glass Volumetric (Transfer) Pipets
E1044 Specification for Glass Serological Pipets (General Purpose and Kahn)
E1621 Guide for Elemental Analysis by Wavelength Dispersive X-Ray Fluorescence Spectrometry
3. Terminology
3.1 For definitions of terms used in these practices, refer to Terminology E135.
These practices are under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and are the direct responsibility
of Subcommittee E01.20 on Fundamental Practices.
Current edition approved Oct. 15, 2011Aug. 1, 2016. Published November 2011August 2016. Originally approved in 1943. Last previous edition approved in 20052011
as E50–00 (2005). –11. DOI: 10.1520/E0050-11.10.1520/E0050-16.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E50 − 11 (2016)
4. Significance and Use
4.1 The inclusion of the following paragraph, or a suitable equivalent, in any standard (preferably after the section on Scope)
is due notification that the apparatus and reagents required in that standard are subject to the recommendations set forth in these
practices.
“Apparatus and Reagents—Apparatus and reagents required for each
determination are listed in separate sections preceding the procedure.
Apparatus, standard solutions, and certain other reagents shall conform to
the requirements prescribed in ASTM Practices E50, for Apparatus,
Reagents, and Safety Considerations for Chemical Analysis of Metals,
Ores, and Related Materials.”
4.2 It is assumed that the users of these practices will be trained analysts capable of performing common laboratory procedures
skillfully and safely. It is expected that work will be performed in a properly-equipped laboratory.
5. Purity of Water and Reagents
5.1 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Type I or II of Specification D1193. Type III or IV may be used if they effect no measurable change in the blank or sample.
5.2 Reagents—Unless otherwise indicated, it is intended that all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society when such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the
determination. In addition to this, it is desirable in many cases for the analyst to ensure the accuracy of his results by running blanks
or checking against a comparable sample of known composition.
6. Reagents
6.1 Concentrated Acids, Ammonium Hydroxide, and Hydrogen Peroxide—When acids, ammonium hydroxide, and hydrogen
peroxide are specified by name or chemical formula only, it is understood that concentrated reagents of the specific gravities or
concentrations shown in Table 2 are intended. The specific gravities or concentrations of all other concentrated acids are stated
wherever they are specified.
6.2 Diluted Acids and Ammonium Hydroxide—Concentrations of diluted acids and ammonium hydroxide, except when
standardized, are specified as a ratio stating the number of volumes of the concentrated reagent to be diluted with a given number
of volumes of water, as in the following example: HCl (5 + 95) means 5 volumes of concentrated HCl (sp gr 1.19) diluted with
95 volumes of water.
6.3 Standard Solutions—Concentrations of standard solutions are stated as molarities or normalities, expressed decimally; or the
equivalent of 1 mL of solution in terms of grams, milligrams, or micrograms of a given element expressed as “1 mL = x.xx—g,
mg, or μg of.”
6.4 NonstandardizedNonstandard Solutions—Composition of nonstandardizednonstandard solutions prepared by dissolving a
given mass of the solid reagent in a solvent are specified in grams of the salt as weighed per litre of solution, and it is understood
that water is the solvent unless otherwise specified. For example, to prepare barium chloride solution (100 g/L) dissolve 100 g of
barium chloride (BaCl ·2H O) in water and dilute to 1 L. In the case of certain reagents, the composition may be specified as a
2 2
weight mass fraction percent. For example, H O (3 %) means a solution containing 3 g of H O per 100 g of solution. Other
2 2 2 2
nonstandardizednonstandard solutions may be specified by name only and the designation of the composition of such solutions will
be governed by the instructions for their preparation.
4,5
7. Laboratory Ware (1,2)
7.1 Glassware—Unless otherwise stated all analytical methods are conducted in borosilicate glassware.
7.1.1 Tolerances—All glass apparatus and vessels used in analytical work must be carefully selected and calibrated to meet the
particular requirements for each operation. Standard volumetric flasks, burets, and pipets must be of Class A or B within the
tolerances established by the National Institute of Standards and Technology and ASTM.
7.1.2 Types—Glasses are available which include colored glass for the protection of solutions affected by light, alkali-resistant
glass, and high-silica glass having exceptional resistance to thermal shock. Standard-taper, interchangeable, ground-glass joints are
very useful in analytical work.
7.2 Plastic Labware:
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. DC, www.chemistry.org . For suggestions on the testing
of reagents not listed by the American Chemical Society, see the United States Pharmacopeia and 4.2 National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC),
Rockville, MD.MD, www.usp.org.
The boldface numbers in parentheses refer to the list of references at the end of these practices.
For further information the following ASTM Standards may be consulted: Volumetric Labware: Specifications E287, E288, and E438; Practice E542; and Specifications
E694, E969, and E1044. Thermometers: Specification E1 and Test Method E77. Hydrometers: Specification E100 and Test Method E126.
E50 − 11 (2016)
TABLE 1 Chemical Reagents Specified in ASTM Methods for Chemical Analysis of Metals
Name Formula
* Acetic acid CH COOH
Acetone CH COCH
3 3
Acetylacetone (2,4-pentanedione) CH COCH COCH
3 2 3
Alizarin-Red-S C H COC H-1,2-(OH) -3-SO NaCO
6 4 6 2 3
Aluminon (aurintricarboxylic acid-ammonium (4-HOC H -3-COONH ) C:C H-3-
6 3 4 2 6
salt) (COONH ):O
Aluminum metal (99.9 % min) Al
* Aluminum metal (sheet or rolled foil) Al
Aluminum ammonium sulfate Al (NH ) (SO ) ·24H O
2 4 2 4 4 2
Aluminum nitrate Al(NO ) ·9H O
3 3 2
Aluminum sulfate Al (SO ) ·18H O
2 4 3 2
Aluminum oxide, fused (Alundum)
1-Amino-2-naphthol-4-sulfonic acid NH C H (OH)SO H
2 10 5 3
Ammonium acetate CH COONH
3 4
Ammonium benzoate C H COONH
6 5 4
Ammonium bifluoride NH FHF
Ammonium bisulfate NH HSO
4 4
Ammonium bisulfite NH HSO
4 3
Ammonium carbonate (NH ) CO
4 2 3
* Ammonium chloride NH Cl
* Ammonium citrate CH (COONH )C(OH)(COOH)CH COONH
2 4 2 4
Ammonium fluoride NH F
A
* Ammonium hydroxide NH OH
Ammonium iodide NH I
Ammonium molybdate (NH ) MoO
4 2 4
* Ammonium heptamolybdate tetrahydrate (NH ) Mo O ·4H O
4 6 7 24 2
Ammonium nitrate NH NO
4 3
* Ammonium oxalate NH OCOCOONH ·H O
4 4 2
* Ammonium phosphate, dibasic (diammonium (NH ) HPO
4 2 4
acid phosphate)
* Ammonium persulfate (ammonium (NH ) S O
4 2 2 8
peroxydisulfate)
* Ammonium sulfate (NH ) SO
4 2 4
* Ammonium tartrate NH OCO(CHOH) COONH
4 2 4
Ammonium thiocyanate NH SCN
Ammonium vanadate NH VO
4 3
Antimony metal (powder) Sb
Antimony trichloride SbCl
* Arsenic trioxide As O
2 3
Asbestos (for use with Gooch crucible)
Barium Chloride BaCl ·2H O
2 2
Barium diphenylamine sulfonate (C H NHC H -4-SO ) Ba
6 5 6 4 3 2
* Benzoic acid C H COOH
6 5
α-Benzoin oxime (benzoin anti-oxime) C H CHOHC:NOHC H
6 5 6 5
Beryllium sulfate BeSO ·4H O
4 2
Bismuth metal (99.9 % min) Bi
Boric acid H BO
3 3
Bromocresol green (3',39,5',59-tetrabromo-m- C H SO OC(C H-3,5-Br -2-CH -4-OH)
6 4 2 6 2 3 2
cresolsulfonephthalein)
Bromocresol purple (5',59-Dibromo-o- C H SO OC(C H -3-CH -5-Br-4-OH)
6 4 2 6 2 3 2
cresolsulfonephthalein)
Bromine (liquid) Br
Bromophenol blue (3',39,5',59- C H SO OC(C H -3,5-Br -4-OH)
6 4 2 6 2 2 2
tetrabromophenolsulfonephthalein)
1-Butanol CH CH CH CH OH
3 2 2 2
Butyl acetate (normal) CH COOCH CH CH CH
3 2 2 2 3
* Cadmium chloride CdCl ·2 ⁄2 H O
2 2
Cadmium chloride, anhydrous CdCl
* † Calcium carbonate (low-boron) CaCO
Carbon dioxide (gas) CO
Carbon dioxide (solid) CO
Carbon tetrachloride CCl
Carminic acid 1,3,4-(HO) -2-C H O C COC H-5-COOH-6-
3 6 11 6 6 6
OH-8-CH CO
* Chloroform CHCl
Cinchonine C H N O
19 22 2
Citric acid HOC(COOH)(CH COOH)
2 2
Cobalt metal Co
Cobalt sulfate CoSO
Coke
Congo red test paper
Copper metal (99.9 % min) Cu
* Copper metal (powder or turnings) Cu
E50 − 11 (2016)
TABLE 1 Continued
Name Formula
Copper metal (P-free) Cu
Copper metal (Mn, Ni, and Co-free, less than Cu
0.001 % of each)
Copper-rare earth oxide mixture
m-Cresol purple (m-cresolsulfonephthalein) C H SO OC(C H -2-CH -4-OH)
6 4 2 6 3 3 2
Cupferron C H N(NO)ONH
6 5 4
Cupric chloride CuCl ·2H O
2 2
* Cupric nitrate Cu(NO ) ·3H O
3 2 2
* Cupric oxide (powder) CuO
Cupric potassium chloride CuCl ·2KCl·2H O
2 2
* Cupric sulfate CuSO ·5H O
4 2
Curcumin (2-CH OC H -1-OH-4-CH:CHCO) CH
3 6 3 2 2
Devarda’s alloy 50Cu-45Al-5Zn
Diethylenetriamine pentaacetic acid ((HOCOCH ) NCH CH ) NCH COOH
2 2 2 2 2 2
([[(carboxymethyl)imino]bis(ethylenenenitrilo)]
tetraacetic acid)
* Dimethylglyoxime CH C:NOHC:NOHCH
3 3
N,N' Diphenylbenzidine C H NHC H C H NHC H
6 5 6 4 6 4 6 5
Diphenylcarbazide (1,5-diphenylcarbohydrazide) C H NHNHCONHNHC H
6 5 6 5
* Disodium (ethylenedinitrilo) tetraacetate See (ethylenedinitrilo) tetraacetic acid
dihydrate disodium salt
Dithiol (toluene-3,4-dithiol) CH C H (SH)
3 6 3 2
Dithizone (diphenylthiocarbazone) C H NHNHCSN:NC H
6 5 6 5
Eriochrome black-T (1(1-hydroxy-2-naphthylazo)- 1-HOC H -2-N:N-1-C H -2-OH-4-SO Na-6-
10 6 10 4 3
6-nitro-2-naphthol-4-sulfonic acid sodium salt) NO
* EDTA (Disodium salt) See (ethylenedinitrilo) tetraacetic acid
disodium salt
* Ethanol C H OH
2 5
* Ethyl ether (diethyl ether) C H OC H
2 5 2 5
* (Ethylenedinitrilo) tetraacetic acid disodium salt HOCOCH (NaOCOCH )NCH N(CH COONa)CH COOH·2H O
2 2 2 2 2 2
Ethylene glycol monomethyl ether (2-methoxy- CH OCH CH OH
3 2 2
ethanol)
* Ferric chloride FeCl ·6H O
3 2
* Ferric nitrate Fe(NO ) ·9H O
3 3 2
Ferric sulfate Fe (SO ) ·nH O
2 4 3 2
* Ferrous ammonium sulfate Fe(NH ) (SO ) ·6H O
4 2 4 2 2
* Ferrous sulfate FeSO ·7H O
4 2
Fluoboric acid HBF
Fluoroboric acid HBF
Fluorescein, sodium salt 2NaOCOC H C:C H -3(:O)OC H -6-ONa
6 4 6 3 6 3
Formaldehyde HCHO
A
* Formic acid HCOOH
Gelatin
Graphite C
Glass wool
Glycerol CH OHCHOHCH OH
2 2
Hydrazine sulfate NH NH ·H SO
2 2 2 4
A
* Hydrobromic acid HBr
A
* Hydrochloric acid HCl
A
* Hydrofluoric acid HF
Hydrogen chloride gas HCl
* Hydrogen peroxide H O
2 2
Hydrogen sulfide gas H S
Hydroquinone 1,4-(OH) C H
2 6 4
* Hydroxylamine hydrochloride NH OH·HCl
B
* Hypophosphorus acid H PO
3 2
B
* Hypophosphorous acid H PO
3 2
Invert sugar
* Iodine I
Iron metal or wire (99.8 % min) Fe
Isopropyl ether (CH ) CHOCH(CH )
3 2 3 2
Lead metal Pb
* Lead acetate Pb(CH COO)
3 2
Lead chloride PbCl
* Lead nitrate Pb(NO )
3 2
Litmus
Lithium fluoride
...