ASTM E50-00(2005)
(Practice)Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
SIGNIFICANCE AND USE
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. The apparatus, standard solutions, and certain other reagents used in more than one procedure are referred to by number and shall conform to the requirements prescribed in ASTM Practices E 50, for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials.”
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.
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 are included. An identifying number has been assigned each apparatus (see Section 8) and reagent (see Section 25) for convenience of reference in the analytical methods. Included also are general recommendations on the purity of reagents and protective measures for the use of hazardous reagents.
1.2 The aim of these recommendations is to present descriptions of such apparatus and reagents as are common to several ASTM methods, and thus avoid needless repetition. No attempt has been made to provide a description of every apparatus and reagent prescribed in ASTM methods for the chemical analysis of metals. Other apparatus and reagents that are required will be found listed or specified in the individual methods of analysis.
1.3 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 .
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.5 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 7 and Note 2.
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.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E50 – 00 (Reapproved 2005)
Standard Practices for
Apparatus, Reagents, and Safety Considerations for
Chemical Analysis of Metals, Ores, and Related Materials
ThisstandardisissuedunderthefixeddesignationE50;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginal
adoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscript
epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
meaning) in this standard has been confined to those aspects of laboratory
1. Scope
safety where regulatory requirements are known to exist. Such regula-
1.1 These practices cover laboratory apparatus and reagents
tions, however, are beyond the scope of these practices.
that are required for the chemical analysis of metals, ores and
related materials by standard methods of ASTM. Detailed 2. Referenced Documents
descriptions of recommended apparatus and detailed instruc- 2
2.1 ASTM Standards:
tions for the preparation of standard solutions and certain
D1100 Specification for Filter Paper for Use in Chemical
nonstandardized reagents are included.An identifying number 3
Analysis
has been assigned each apparatus (see Section 8) and reagent
D1193 Specification for Reagent Water
(see Section 25) for convenience of reference in the analytical
E1 Specification for ASTM Liquid-in-Glass Thermometers
methods. Included also are general recommendations on the
E70 Test Method for pH of Aqueous Solutions With the
purity of reagents and protective measures for the use of
Glass Electrode
hazardous reagents.
E77 Test Method for Inspection and Verification of Ther-
1.2 Theaimoftheserecommendationsistopresentdescrip-
mometers
tions of such apparatus and reagents as are common to several
E100 Specification for ASTM Hydrometers
ASTMmethods,andthusavoidneedlessrepetition.Noattempt
E126 Test Method for Inspection, Calibration, andVerifica-
has been made to provide a description of every apparatus and
tion of ASTM Hydrometers
reagentprescribedinASTMmethodsforthechemicalanalysis
E128 Test Method for Maximum Pore Diameter and Per-
of metals. Other apparatus and reagents that are required will
meability of Rigid Porous Filters for Laboratory Use
be found listed or specified in the individual methods of
E145 Specification for Gravity-Convection and Forced-
analysis.
Ventilation Ovens
1.3 These recommendations are intended to apply to the
E147 SpecificationforApparatusforMicrodeterminationof
ASTM methods of chemical analysis of metals when definite
Nitrogen by Kjeldahl Method
reference is made to these practices, as covered in Section 3.
E287 Specification for Laboratory Glass Graduated Burets
1.4 Thevaluesstatedininch-poundunitsaretoberegarded
E288 Specification for Laboratory Glass Volumetric Flasks
as standard. The values given in parentheses are mathematical
E319 Practice for the Evaluation of Single-Pan Mechanical
conversions to SI units that are provided for information only
Balances
and are not considered standard.
E438 Specification for Glasses in Laboratory Apparatus
1.5 This standard does not purport to address all of the
E542 Practice for Calibration of Laboratory Volumetric
safety concerns, if any, associated with its use. It is the
Apparatus
responsibility of whoever uses this standard to consult and
E617 Specification for Laboratory Weights and Precision
establish appropriate safety and health practices and deter-
Mass Standards
mine the applicability of regulatory limitations prior to use.
E675 SpecificationforInterchangeableTaper-GroundStop-
Specific hazards are given in Section 7 and Note 2.
cocks And Stoppers
E676 Specification for Interchangeable Taper-Ground
NOTE 1—The use of the verb “shall” (with its obligatory third person
Joints
These practices are under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct 2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
responsibilityofSubcommitteeE01.20onFundamentalPracticesandMeasurement
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Traceability.
Standards volume information, refer to the standard’s Document Summary page on
Current edition approved May 1, 2005. Published June 2005. Originally
the ASTM website.
approved in 1943. Last previous edition approved in 2000 as E50–00. DOI: 3
Withdrawn. The last approved version of this historical standard is referenced
10.1520/E0050-00R05.
on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E50 – 00 (2005)
E694 Specification for Laboratory Glass Volumetric Appa- 5. Reagents
ratus
5.1 Concentrated Acids, Ammonium Hydroxide, and Hydro-
E969 Specification for Glass Volumetric (Transfer) Pipets
gen Peroxide—Whenacids,ammoniumhydroxide,andhydro-
E1044 Specification for Glass Serological Pipets (General
gen peroxide are specified by name or chemical formula only,
Purpose and Kahn)
it is understood that concentrated reagents of the specific
E1621 Guide for X-Ray Emission Spectrometric Analysis
gravities or concentrations shown in Table 1 are intended. The
specific gravities or concentrations of all other concentrated
3. Significance and Use
acids are stated wherever they are specified.
3.1 The inclusion of the following paragraph, or a suitable
5.2 Diluted Acids and Ammonium Hydroxide—
equivalent, in any standard (preferably after the section on
Concentrations of diluted acids and ammonium hydroxide,
Scope) is due notification that the apparatus and reagents
except when standardized, are specified as a ratio stating the
required in that standard are subject to the recommendations
number of volumes of the concentrated reagent to be diluted
set forth in these practices.
with a given number of volumes of water, as in the following
“Apparatus and Reagents—Apparatus and reagents required for each de-
example: HCl (5+95) means 5 volumes of concentrated HCl
termination are listed in separate sections preceding the procedure. The
(sp gr 1.19) diluted with 95 volumes of water.
apparatus, standard solutions, and certain other reagents used in more
5.3 Standard Solutions—Concentrations of standard solu-
than one procedure are referred to by number and shall conform to the
requirements prescribed in ASTM Practices E50, for Apparatus, Reagents,
tions are stated as molarities or normalities, expressed deci-
and Safety Considerations for Chemical Analysis of Metals, Ores, and Re-
mally; or the equivalent of 1 mLof solution in terms of grams,
lated Materials.”
milligrams, or micrograms of a given element expressed as “1
3.2 It is assumed that the users of these practices will be
mL=x.xx—g, mg, or µg of.”
trained analysts capable of performing common laboratory
5.4 Nonstandardized Solutions—Concentrations of non-
proceduresskillfullyandsafely.Itisexpectedthatworkwillbe
standardized solutions prepared by dissolving a given weight
performed in a properly-equipped laboratory.
of the solid reagent in a solvent are specified in grams of the
salt as weighed out per litre of solution, and it is understood
4. Purity of Water and Reagents
that water is the solvent unless otherwise specified. For
4.1 Water—Unless otherwise indicated, references to water
example, to prepare barium chloride solution (100 g/L) dis-
are understood to mean reagent water of Type II grade, as
solve 100 g of barium chloride (BaCl ·2H O) in water and
2 2
defined by Specification D1193.
dilute to 1 L. In the case of certain reagents, the concentration
4.2 Reagents—Unless otherwise indicated, it is intended
maybespecifiedasaweightpercent.Forexample,H O (3%)
2 2
thatallreagentsconformtothespecificationsoftheCommittee
means a solution containing3gofH O per 100 g of solution.
2 2
on Analytical Reagents of the American Chemical Society
Other nonstandardized solutions may be specified by name
when such specifications are available. Other grades may be
only and the designation of the concentration of such solutions
used, provided it is first ascertained that the reagent is of
will be governed by the instructions for their preparation.
sufficiently high purity to permit its use without lessening the
,
accuracyofthedetermination.Inadditiontothis,itisdesirable
6. Laboratory Ware (1,2)
in many cases for the analyst to ensure the accuracy of his
6.1 Glassware—Unlessotherwisestatedallanalyticalmeth-
results by running blanks or checking against a comparable
ods are carried out in borosilicate glassware.
sample of known composition.
Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof
4 these practices.
Reagent Chemicals, American Chemical Society Specifications, American
For further information the following ASTM Standards may be consulted:
Chemical Society, Washington, DC, www.chemistry.org. For suggestions on the
Volumetric Labware: Specifications E287, E288, and E438; Practice E542; and
testing of reagents not listed by the American Chemical Society, see the United
Specifications E694, E969, and E1044. Thermometers: Specification E1 and Test
States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention,
Method E77. Hydrometers: Specification E100 and Test Method E126.
Inc. (USPC), Rockville, MD, http://www.usp.org.
TABLE 1 Concentration of Acids, Ammonium Hydroxide, and Hydrogen Peroxide
Specific
Reagent, Weight %
Name Formula Gravity,
Nominal Min Max
Approximate
Acetic acid CH COOH 1.05 . 99.5 .
Formic acid HCOOH 1.20 . 88.0 .
Hydrobromic acid HBr 1.49 48 47.0 49.0
Hydrochloric acid HCl 1.19 . 35.0 38.0
Hydrofluoric acid HF 1.15 . 48.0 51.0
Nitric acid HNO 1.42 . 69.0 71.0
Perchloric acid HClO 1.67 . 70.0 72.0
Phosphoric acid H PO 1.69 . 85.0 .
3 4
Sulfuric acid H SO 1.84 . 95.0 98.0
2 4
Sulfurous acid H SO 1.03 . 6.0(SO ) .
2 3 2
Ammonium hydroxide NH OH 0.90 . 27.0(NH ) 30.0 (NH )
4 3 3
Hydrogen peroxide H O 1.10 30 28.0 .
2 2
E50 – 00 (2005)
6.1.1 Tolerances—All glass apparatus and vessels used in Plastic labware may crack from interaction of a “stress
analytical work must be carefully selected and calibrated to cracking agent” (present, possibly in the solution to be ana-
meet the particular requirements for each operation. Standard lyzed) with molded-in stresses. This is, however, a long-time
volumetric flasks, burets, and pipets must be of Class A or B phenomenon and is normally not a factor in analytical work
within the tolerances established by the National Institute of because contact times usually are limited and the labware is
Standards and Technology and ASTM. washed regularly.
6.1.2 Types—Glasses are available which include colored 6.2.3.3 Some plastics may contain small concentrations of
glass for the protection of solutions affected by light, alkali- metals used as catalysts during manufacture. Such metals may
resistant glass, and high-silica glass having exceptional resis- dissolve in the analytical reagent system and cause interfer-
tance to thermal shock. Standard-taper, interchangeable, ence, particularly when small amounts of metals are to be
ground-glass joints are very useful in analytical work. determined.
6.2 Plastic Labware: 6.2.3.4 A general indication of the effect of individual
6.2.1 Tolerances—All plastic apparatus and vessels used in reagents can often be obtained from manufacturers’ publica-
analytical work must be calibrated to meet the particular tions.Itisimportant,ofcourse,toconsiderthatexposuretime,
requirements for each operation. Standard volumetric flasks, temperature, concentration, and other reagents in the system
burets, and pipets must be of precision grade within the may alter the effects of a given reagent on a given plastic.
tolerances established by the National Institute of Standards Because of these factors, the plastic labware must be thor-
and Technology for the corresponding types of glassware (see oughly tested under the conditions of the method. The type of
6.2.4). plastic labware (see footnote B of Table 2) will be found
6.2.2 Physical Properties—There are a number of physical specified in the method as well as any special precautions for
properties which influence the usefulness of plastic labware its use.
(Table 2). 6.2.4 Precautions—Most plastic labware must not be used
6.2.3 Compatibility—Manyreagentscanaffectthestrength, with strong oxidants at elevated temperatures; or exposed to
flexibility, surface appearance, color, dimensions, or weight of localized or general temperature above the limits in Table 2.
plastics. The two basic modes of interaction that can cause With proper precaution polytetrafluoroethylene labware may
these changes are described in 6.2.3.1-6.2.3.4. be used with strong oxidizing agents at elevated temperatures
6.2.3.1 Chemical—The analytical reagents can react with (see Table 2). For the best performance new volumetric ware
thepolymerchainbyoxidation,byattackonfunctionalgroups should be rinsed with a mild detergent according to the
in or on the polymer molecule, or by depolymerization with a directions of the manufacturer before using. Plastic volumetric
resultant deterioration in physical properties. ware shrinks slightly as it ages; therefore, it must be recali-
6.2.3.2 Physical—Absorption of solvents in the plastic can bratedperiodically.Interiorsurfacesofvolumetricwareshould
result in softening, swelling, and permeation of the solvent not be cleaned by abrasive action.
through the plastic. No room temperature solvents are known
7. Hazards (3-8)
forthepolyolefins,however,itisbetternottousethemtostore
reagents.ReagentssuchasNH,Br,H S,andnitrogenoxides
7.1 General Requirements—Nearly all procedures carried
3 2 2
may be absorbed from reagent solutions by the plastic and
out in the chemical laboratory are potentially hazardous. Each
becomeasourceoferrorbysubsequentreleasewhenthevessel
oftheproceduresusedinthesemethodsofchemicalanalysisof
is used for a different analysis. Atmospheric contaminants
metals has been safely performed many times in a number of
may diffuse through the plastic and spoil contained reagents or
laboratories. Specific warnings are given in the methods when
samples. Other polymer types may dissolve in some solvents.
Specialcareshouldbeusedwithfluorinatedmaterials,becauseattemperatures
around 250°C traces of possibly hazardous vapors may be emitted. Heat in a hood
From the publications of the Nalgene Labware Div., Nalge Sybron Corp.
or well-ventilated area.
Theobald, L. S., Analyst, Vol 84, 1959, p. 570.
A
TABLE 2 Physical Properties of Plastic Labware
Brittleness
B
Plastic Temperature Limit,° C Specific Gravity Water Absorption, % Fl
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.