E01.20 - Fundamental Practices
Fundamental Practices
General Information
ABSTRACT
This practice describes the photomultiplier properties that are essential to their judicious selection and use of in emission and absorption spectrometry. The properties covered here include structural features, electrical properties, and characteristics involved in precautions and problems. The structural features covered are envelope configurations, window materials, electrical connections, and housing for the external structure, and the photocathode, dynodes and anode, and rigidness of structural components for the internal structure. Electrical properties, on the other hand, incorporate the following: optical-electronic characteristics of the photocathode including spectral response; current amplification including gain per stage, overall gain, gain control (voltage-divider bridge), linearity of response, and anode saturation; signal nature; dark current including cathode size, internal aperture, and refrigeration effects; noise nature including additivity of noise power, signal-to-noise ratio, equivalent noise input; and photomultiplier properties as a component in an electrical circuit including output impedance, response time, and signal gating and integration possibilities. Finally, the characteristics involved in precautions and problems cover fatigue and hysteresis effects, illumination of photocathode, and gas leakage.
SCOPE
1.1 This practice covers photomultiplier properties that are essential to their judicious selection and use in emission and absorption spectrometry. Descriptions of these properties can be found in the following sections:
Section
Structural Features
4
General
4.1
External Structure
4.2
Internal Structure
4.3
Electrical Properties
5
General
5.1
Optical-Electronic Characteristics of the Photocathode
5.2
Current Amplification
5.3
Signal Nature
5.4
Dark Current
5.5
Noise Nature
5.6
Photomultiplier as a Component in an Electrical Circuit
5.7
Precautions and Problems
6
General
6.1
Fatigue and Hysteresis Effects
6.2
Illumination of Photocathode
6.3
Gas Leakage
6.4
Recommendations on Important Selection Criteria
7
1.2 Radiation in the frequency range common to analytical emission and absorption spectrometry is detected by photomultipliers presently to the exclusion of most other transducers. Detection limits, analytical sensitivity, and accuracy depend on the characteristics of these current-amplifying detectors as well as other factors in the system.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 The chemical measurement processes covered by this guide are used for determination of Carbon, Sulfur, Nitrogen, Oxygen and Hydrogen in metals, ores and related materials. A test method utilizing this guidance is used to test such materials, and also form the basis for quality assurance of these materials. Thus, it is economically and scientifically critical that these instruments be understood by the laboratories that use them.
5.2 It is assumed that all who use this guide will be trained analysts, capable of performing common laboratory procedures skillfully, and safely. It is expected that any work will be performed in a properly equipped laboratory.
5.3 It is expected that the laboratory will prepare their own work procedures for any of the information described in this guide.
5.4 This guide contains numerous references to “manufacturer’s recommendations”. The user of this guide is expected to refer to the instrument operation manual for the specific instrument being used or consult directly with the manufacturer to obtain instructions or recommendations.
5.5 This guide stresses the conservation of certified reference materials (CRMs). CRMs should not be used for drift checks or conditioning measurments. Other materials should be developed and used for these operations.
SCOPE
1.1 This guide covers information for using Combustion, Inert Gas Fusion and Hot Extraction instruments to determine the mass fraction of the non-metallic elements Carbon, Sulfur, Nitrogen, Oxygen and Hydrogen in metals, ores and related materials.
1.2 This guide does not specify all the operating conditions because of the differences among different manufacturer’s instruments. Laboratories should follow instructions provided by the manufacturer of the instrument.
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 The information in this guide is contained in the sections indicated as follows:
Sections
Carbon/Sulfur by Combustion/Infrared Detection
14 – 19
Nitrogen/Oxygen by Inert Gas Fusion/Thermal Conductivity and Infrared Detection
20 – 25
Hydrogen by Inert Gas Fusion Instrumental Measurement and Hot Extraction/Various Detection Cell Technology
26 – 31
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Guide10 pagesEnglish language
SIGNIFICANCE AND USE
4.1 This practice describes the essential components of a wavelength dispersive X-ray spectrometer. This description is presented so that the user may gain a general understanding of the structure of an X-ray spectrometer system. It also provides a means for comparing and evaluating different systems as well as understanding the capabilities and limitations of each instrument.
4.2 A laboratory may implement this practice or an X-ray fluorescence method in partnership with a manufacturer of the analytical instrumentation. If a laboratory chooses to consult with an instrument manufacturer, then the following should be considered. The laboratory should know the alloy matrices to be analyzed, elements and mass fraction ranges to be determined, and the expected performance requirements for each of these elements. The laboratory should inform the instrument manufacturer of these requirements so an analytical method may be developed which meets the laboratory’s expectations. Typically, instrument manufacturers customize the instrument configuration to satisfy the end-user’s requirements for elemental coverage, elemental precision, and detection limits. Instrument manufacturer developed analytical methods may include specific parameters for sample excitation, wavelengths, inter-element interference corrections, calibration and regression, equipment configuration/installation, and sample preparation requirements. Laboratories should have a basic understanding of the parameters derived by the manufacturer.
SCOPE
1.1 This practice covers the components of a wavelength dispersive X-ray spectrometer that are basic to its operation and to the quality of its performance. It is not the intent of this practice to specify component tolerances or performance criteria, as these are unique for each instrument. However, the practice does attempt to identify which tolerances are critical and thus which should be specified.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific safety hazard statements are given in Section 7.
1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard5 pagesEnglish language
- Standard5 pagesEnglish language
SIGNIFICANCE AND USE
5.1 This sampling practice is useful for converting material taken from ingots or other solid materials into a homogeneous solid sample suitable for direct excitation on a spark atomic emission or X-ray fluorescence spectrometer. The resultant button may itself be chipped to provide specimens for test methods requiring solutions or chips.
5.2 This practice has been used extensively for the preparation of zirconium, zirconium alloy, titanium, and titanium alloy materials, and is applicable to other reactive, refractory, ferrous and nonferrous alloys, such as cobalt, cobalt alloys, niobium, nickel, nickel alloys, cast irons, steels, stainless steels, tantalum, tool steels, and tungsten.
SCOPE
1.1 This practice covers the preparation of solid samples of reactive and refractory metals and alloys by electric arc remelting. The samples for melting may be in the form of drillings, chunks, chips, turnings, wire, sponge, powder briquettes, and powdered metals.
1.1.1 This practice is also suitable for preparation of solid samples of other metals, such as cast irons, steels, stainless steels, tool steels, nickel, nickel alloys, cobalt, and cobalt alloys.
1.2 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 9.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard7 pagesEnglish language
- Standard7 pagesEnglish language
SIGNIFICANCE AND USE
5.1 X-ray fluorescence spectrometry can provide an accurate determination of metallic and many non-metallic elements in a wide variety of solid and liquid materials. This guide covers the information that should be included in an X-ray spectrometric analytical method and provides direction to the user for determining the optimum conditions needed to achieve acceptable accuracy.
5.2 The accuracy of a determination is a function of the calibration algorithm, the sample preparation, and the sample homogeneity. Close attention to all aspects of these areas is necessary to achieve acceptable results.
5.3 All concepts discussed in this guide are explored in detail in a number of published texts and in the scientific literature.
SCOPE
1.1 This standard provides guidelines for developing and describing analytical procedures using a wavelength dispersive X-ray spectrometer for elemental analysis of solid metals, ores, and related materials. Material forms discussed herein include solids, powders, and solid forms prepared by chemical and physical processes such as borate fusion and pressing of briquettes.
1.2 Liquids are not discussed in this guide because they are much less frequently encountered in metals and mining laboratories. However, aqueous liquids can be processed by borate fusion to create solid specimens, and X-ray spectrometers can be equipped to handle liquids directly.
1.3 Some provisions of this guide may be applicable to the use of an energy dispersive X-ray spectrometer.
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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 the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Guide9 pagesEnglish language
- Guide9 pagesEnglish language
ABSTRACT
This practice covers general recommendations for photoelectric photometers and spectrometers and for photometric practice for chemical analysis of metals, ores, and related materials. However, this practice does not include a description of every apparatus nor does it present recommendations on every detail of practice in photometric or spectrophotometric methods of chemical analysis of metals. To improve photoelectric photometers and spectrophotometers, some suggestions related to their components are mentioned, in particular, the radiation source (illuminant), filters, monochromators, absorption cells, photosensitive tubes, and current-measuring devices. In addition, prior to using photometric methods in the chemical analysis of metals, ores, and related materials, it is recommended that a complete photometric investigation of the reaction be performed. The investigation shall involve the study of the specificity of the reagent used to produce absorption; validity of Beer's law; effects of salts, solvent, pH, temperature, concentration of reagents, and the order of adding reagents; time required for absorption development and the stability of the absorption; absorption curve of the reagent and the absorbing substances; and optimum concentration range for quantitative analysis.
SCOPE
1.1 This practice covers general recommendations for photoelectric photometers and spectrophotometers and for photometric practice prescribed in ASTM methods for chemical analysis of metals, sufficient to supplement adequately the ASTM methods. A summary of the fundamental theory and practice of photometry is given. No attempt has been made, however, to include in this practice a description of every apparatus or to present recommendations on every detail of practice in ASTM photometric or spectrophotometric methods of chemical analysis of metals.2
1.2 These recommendations are intended to apply to the ASTM photometric and spectrophotometric methods for chemical analysis of metals when such standards make definite reference to this practice, as covered in Section 4.
1.3 In this practice, the terms “photometric” and “photometry” encompass both filter photometers and spectrophotometers, while “spectrophotometry” is reserved for spectrophotometers alone.
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 the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard8 pagesEnglish language
SIGNIFICANCE AND USE
4.1 This guide is intended to assist those writing or revising compositional specifications, sampling practices, and test methods for ferrous and non-ferrous metals, ores, and related materials. It is directed toward those areas that must be addressed to properly coordinate compositional specification, sampling practice, and test methods. Its use will help ensure that compositional requirements are clearly defined and that sampling practices and test methods are available to meet product specifications.
4.2 This guide does not attempt to define which elements should be controlled, where samples should be taken, or how they should be analyzed. These items are addressed in standards such as Specification A276, Test Methods and Practices A751, Test Method E34, Practice E255, Test Method E342, and Test Methods E350.
4.3 A primary purpose for ASTM sampling practices and test methods is to provide widely-accepted and tested methodology for use in meeting ASTM product specifications. Although it is recognized that individual laboratories are free to use other methods, the availability of ASTM approved methodology is essential for referee purposes and to demonstrate that properly equipped laboratories can make the required measurements.
4.4 Sampling practices and test methods to be recommended for use in testing a given product are most easily selected cooperatively by the specification-writing and the methods-writing committees that have jurisdiction over the product. When existing sampling or test methods do not meet the needs of the new product specification standard, the specification-writing committee should request that the methods-writing committee develop the required standards. ASTM Committee E01 is responsible for test methods and practices covering the sampling and analysis of most metals, ores, and related materials.
SCOPE
1.1 This guide covers procedures for specifying compositional requirements and identifying appropriate sampling and quantitative analysis test methods to be referenced in product specification standards for metals, ores, and related materials. It is not intended to replace or conflict with either individual product specifications or standards covering broad classifications of products such as Test Methods and Practices A751.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Guide3 pagesEnglish language
- Guide3 pagesEnglish language
SIGNIFICANCE AND USE
4.1 This practice is intended for users who are attempting to establish GF-AAS procedures. It should be helpful for establishing a complete atomic absorption analysis program.
SCOPE
1.1 This practice covers a procedure for the determination of microgram per milliliter (μg/mL) or lower concentrations of elements in solution using a graphite furnace attached to an atomic absorption spectrometer. A general description of the equipment is provided. Recommendations are made for preparing the instrument for measurements, establishing optimum temperature conditions and other criteria which should result in determining a useful calibration concentration range, and measuring and calculating the test solution analyte concentration.
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific safety hazard statements are given in Section 9.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard9 pagesEnglish language
- Standard9 pagesEnglish language
SIGNIFICANCE AND USE
5.1 This practice is intended to provide fundamental direction for the calibration, drift correction, and periodic control of the analytical curves for spark atomic emission spectrometers.
5.2 It is assumed that this practice will be used by trained operators capable of performing the procedures described herein.
SCOPE
1.1 This practice provides direction for establishing and controlling spark atomic emission spectrochemical analytical curves. The generation of analytical curves and their control are considered as separate though interrelated operations. This practice is applicable to spark atomic emission spectrometers.
Note 1: X-ray fluorescence spectrometric applications are no longer covered by this practice. See Guides E1361 and E1621 for discussion of this technique.
1.1.1 Since software programs are readily available to compute multiple linear regressions that can be used to generate analytical curves and since most instruments include this feature, this practice does not address this procedure. However, some recommendations are given to evaluate the equations that are generated.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard4 pagesEnglish language
- Standard4 pagesEnglish language
SIGNIFICANCE AND USE
4.1 Accuracy in quantitative X-ray spectrometric analysis depends upon adequate accounting for interelement effects either through sample preparation or through mathematical correction procedures, or both. This guide is intended to serve as an introduction to users of X-ray fluorescence correction methods. For this reason, only selected mathematical models for correcting interelement effects are presented. The reader is referred to several texts for a more comprehensive treatment of the subject (2-7).
SCOPE
1.1 This guide is an introduction to mathematical procedures for correction of interelement (matrix) effects in quantitative X-ray spectrometric analysis.
1.1.1 The procedures described correct only for the interelement effect(s) arising from a homogeneous chemical composition of the specimen. Effects related to either particle size, or mineralogical or metallurgical phases in a specimen are not treated.
1.1.2 These procedures apply to both wavelength and energy-dispersive X-ray spectrometry where the specimen is considered to be infinitely thick, flat, and homogeneous with respect to the depth of penetration of the exciting X-rays (1).2
1.2 This document is not intended to be a comprehensive treatment of the many different techniques employed to compensate for interelement effects. Consult Refs (2-5) for descriptions of other commonly used techniques such as standard addition, internal standardization, etc.
1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Guide12 pagesEnglish language
SIGNIFICANCE AND USE
4.1 Equipment and procedures described in this guide are comparative methods and are intended for identification or segregation, or both, of pieces or lots of metals that were mixed or lost their identity during certain manufacturing operations. It is presumed that all pieces or lots of metal have been previously checked and did meet applicable specifications.
4.2 The equipment and procedures described in this guide may also be suitable for identifying or segregating, or both, scrap metals.
SCOPE
1.1 This guide covers the identification or segregation, or both, of mixed metal lots under plant conditions using trained plant personnel.
1.2 The identification is not intended to have the accuracy and reliability of procedures performed in a laboratory using laboratory equipment under optimum conditions, and performed by trained chemists or technicians. The identification is not intended to establish whether a given piece or lot of metal meets specifications.
1.3 Segregation of certain metal combinations is not always possible with procedures provided in this guide and can be subject to errors.
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 the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Guide3 pagesEnglish language
SIGNIFICANCE AND USE
4.1 An increasing number of atomic emission spectrometers are equipped with enclosed excitation stands and plasmas which call for atmospheres other than ambient air. This practice is intended for users of such equipment.
SCOPE
1.1 This practice covers general recommendations relative to the use of gas shielding during and immediately prior to specimen excitation in atomic emission spectrochemical analysis. It describes the concept of excitation shielding, the means of introducing gases, and the variables involved with handling gases.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard4 pagesEnglish language
- Standard4 pagesEnglish language
SIGNIFICANCE AND USE
4.1 This practice is for optimizing the parameters used in the determination of trace elements in metals and alloys by the graphite furnace atomic absorption spectrometric method. It also describes the practice for checking the spectrometer performance. The work is expected to be performed in a properly equipped laboratory by trained operators and appropriate disposal procedures are to be followed.
SCOPE
1.1 This practice covers the optimization of graphite furnace atomic absorption spectrometers and the checking of spectrometer performance criteria.
1.2 The values stated in SI units are to be regarded as the standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard5 pagesEnglish language
- Standard5 pagesEnglish language
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.”
TABLE 1 Chemical Reagents Specified in ASTM Methods for Chemical Analysis of Metals
Name
Formula
* Acetic acid
CH3COOH
Acetone
CH3COCH3
Acetylacetone (2,4-pentanedione)
CH3COCH2COCH3
Alizarin-Red-S
C6H4COC6H-1,2-(OH)2-3-SO3NaCO
Aluminon (aurintricarboxylic acid-ammonium salt)
(4-HOC6H3-3-COONH4)2C:C6H-3-(COONH4):O
Aluminum metal (99.9 % min)
Al
* Aluminum metal (sheet or rolled foil)
Al
Aluminum ammonium sulfate
Al2(NH4)2(SO4)4·24H2O
Aluminum nitrate
Al(NO3)3·9H2O
Aluminum sulfate
Al2(SO4)3·18H2O
Aluminum oxide, fused (Alundum)
1-Amino-2-naphthol-4-sulfonic acid
NH2C10H5(OH)SO3H
Ammonium acetate
CH3COONH4
Ammonium benzoate
C6H5COONH4
Ammonium bifluoride
NH4FHF
Ammonium bisulfate
NH4HSO4
Ammonium bisulfite
NH4HSO3
Ammonium carbonate
(NH4)2CO3
* Ammonium chloride
NH4Cl
* Ammonium citrate
CH2(COONH4)C(OH)(COOH)CH2COONH4
Ammonium fluoride
NH4F
* Ammonium hydroxideA
NH4OH
Ammonium iodide
NH4I
Ammonium molybdate
(NH4)2MoO4
* Ammonium heptamolybdate tetrahydrate
(NH4)6Mo7O24·4H2O
Ammonium nitrate
NH4NO3
* Ammonium oxalate
NH4OCOCOONH4·H2O
* Ammonium phosphate, dibasic (diammonium acid phosphate)
(NH4)2HPO4
* Ammo...
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 the user of this standard to establish appropriate safety, health, and environmental 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.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard12 pagesEnglish language
- Standard12 pagesEnglish language
SIGNIFICANCE AND USE
4.1 This practice describes the essential components of the DCP spectrometer. This description allows the user or potential user to gain a basic understanding of this system. It also provides a means of comparing and evaluating this system with similar systems, as well as understanding the capabilities and limitations of each instrument.
SCOPE
1.1 This practice describes the components of a direct current plasma (DCP) atomic emission spectrometer. This practice does not attempt to specify component tolerances or performance criteria. This practice does, however, attempt to identify critical factors affecting bias, precision, and sensitivity. Before placing an order a prospective user should consult with the manufacturer to design a testing protocol for demonstrating that the instrument meets all anticipated needs.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are give in Section 9.
1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 Analyses using DCP-AES require proper preparation of test solutions, accurate calibration, and control of analytical procedures. ASTM test methods that refer to this guide shall provide specifics on test solutions, calibration, and procedures.
5.2 DCP-AES analysis is primarily concerned with testing materials for compliance with specifications, but may range from qualitative estimations to umpire analysis. These may involve measuring major and minor constituents or trace impurities, or both. This guide suggests some approaches to these different analytical needs.
5.3 This guide assists analysts in developing new methods.
5.4 It is assumed that the users of this guide will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that the work will be performed in a properly equipped laboratory.
5.5 This guide does not purport to define all of the quality assurance parameters necessary for DCP-AES analysis. Analysts should ensure that proper quality assurance procedures are followed, especially those defined by the test method. Refer to Guide E882.
SCOPE
1.1 This guide covers procedures for using a Direct Current Plasma Atomic Emission Spectrometer (DCP-AES) to determine the concentration of elements in solution. Recommendations are provided for preparing and calibrating the instrument, assessing instrument performance, diagnosing and correcting for interferences, measuring test solutions, and calculating results. A method to correct for instrument drift is included.
1.2 This guide does not specify all the operating conditions for a DCP-AES because of the differences between models of these instruments. Analysts should follow instructions provided by the manufacturer of the particular instrument.
1.3 This guide does not attempt to specify in detail all of the hardware components and computer software of the instrument. It is assumed that the instrument, whether commercially available, modified, or custom built, will be capable of performing the analyses for which it is intended, and that the analyst has verified this before performing the analysis.
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 the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 7.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Guide8 pagesEnglish language
SIGNIFICANCE AND USE
5.1 This practice describes the essential components of an ICP-AES. The components include excitation/radio-frequency generators, sample introduction systems, spectrometers, detectors, and signal processing and displays. This description allows the user or potential user to gain a cursory understanding of an ICP-AES system. This practice also provides a means for comparing and evaluating various systems, as well as understanding the capabilities and limitations of each instrument.
5.2 Training—The manufacturer should provide training in safety, basic theory of ICP-AES analysis, operations of hardware and software, and routine maintenance for at least one operator. Training ideally should consist of the basic operation of the instrument at the time of installation, followed by an in-depth course one or two months later. Advanced courses are also offered at several of the important spectroscopy meetings that occur throughout the year as well as by independent training institutes. Several independent consultants are available who can provide training, sometimes at the user's site.
SCOPE
1.1 This practice describes the components of an inductively coupled plasma atomic emission spectrometer (ICP-AES) that are basic to its operation and to the quality of its performance. This practice identifies critical factors affecting accuracy, precision, and sensitivity. It is not the intent of this practice to specify component tolerances or performance criteria, since these are unique for each instrument. A prospective user should consult with the manufacturer before placing an order, to design a testing protocol that demonstrates the instrument meets all anticipated needs.
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific safety hazard statements are given in Section 13.
- Standard15 pagesEnglish language
- Standard15 pagesEnglish language
SIGNIFICANCE AND USE
4.1 The grinding materials used for the preparation of the surfaces of specimens prior to analysis by spark atomic emission or X-ray fluorescence spectrometry can contaminate the surface and thus produce erroneous results. This guide provides examples of the effects of these contaminations and recommendations for evaluating grinding materials to eliminate or reduce these effects in spectrochemical analysis.
4.2 The examples given in this guide are not the only contaminations that can occur. Especially in X-ray spectrometry, all phases of the surface preparation should be examined for potential contamination effects.
4.3 Analytical significance of the contaminations observed depends on the needs of the analyst for the particular application at a given composition.
SCOPE
1.1 This guide covers recommendations for the evaluation of various grinding materials used to prepare the surfaces of specimens to be analyzed by spark atomic emission or X-ray fluorescence spectrometry.
1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Guide5 pagesEnglish language
- Guide5 pagesEnglish language
ABSTRACT
This practice describes the photomultiplier properties that are essential to their judicious selection and use of in emission and absorption spectrometry. The properties covered here include structural features, electrical properties, and characteristics involved in precautions and problems. The structural features covered are envelope configurations, window materials, electrical connections, and housing for the external structure, and the photocathode, dynodes and anode, and rigidness of structural components for the internal structure. Electrical properties, on the other hand, incorporate the following: optical-electronic characteristics of the photocathode including spectral response; current amplification including gain per stage, overall gain, gain control (voltage-divider bridge), linearity of response, and anode saturation; signal nature; dark current including cathode size, internal aperture, and refrigeration effects; noise nature including additivity of noise power, signal-to-noise ratio, equivalent noise input; and photomultiplier properties as a component in an electrical circuit including output impedance, response time, and signal gating and integration possibilities. Finally, the characteristics involved in precautions and problems cover fatigue and hysteresis effects, illumination of photocathode, and gas leakage.
SCOPE
1.1 This practice covers photomultiplier properties that are essential to their judicious selection and use in emission and absorption spectrometry. Descriptions of these properties can be found in the following sections:
Section
Structural Features
4
General
4.1
External Structure
4.2
Internal Structure
4.3
Electrical Properties
5
General
5.1
Optical-Electronic Characteristics of the Photocathode
5.2
Current Amplification
5.3
Signal Nature
5.4
Dark Current
5.5
Noise Nature
5.6
Photomultiplier as a Component in an Electrical Circuit
5.7
Precautions and Problems
6
General
6.1
Fatigue and Hysteresis Effects
6.2
Illumination of Photocathode
6.3
Gas Leakage
6.4
Recommendations on Important Selection Criteria
7
1.2 Radiation in the frequency range common to analytical emission and absorption spectrometry is detected by photomultipliers presently to the exclusion of most other transducers. Detection limits, analytical sensitivity, and accuracy depend on the characteristics of these current-amplifying detectors as well as other factors in the system.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
5.1 X-ray fluorescence spectrometry can provide an accurate determination of metallic and many non-metallic elements in a wide variety of solid and liquid materials. This guide covers the information that should be included in an X-ray spectrometric analytical method and provides direction to the analyst for determining the optimum conditions needed to achieve acceptable accuracy.
5.2 The accuracy of a determination is a function of the calibration scheme, the sample preparation, and the sample homogeneity. Close attention to all aspects of these areas is necessary to achieve acceptable results.
5.3 All concepts discussed in this guide are explored in detail in a number of published texts and in the scientific literature.
SCOPE
1.1 This guide provides guidelines for developing and describing analytical procedures using a wavelength dispersive X-ray spectrometer for elemental analysis of solid metals, ores, and related materials. Material forms discussed herein include solids, powders, and solid forms prepared by chemical and physical processes such as borate fusion and pressing of briquettes.
1.2 Liquids are not discussed in this guide because they are much less frequently encountered in metals and mining laboratories. However, aqueous liquids can be processed by borate fusion to create solid specimens, and X-ray spectrometers can be equipped to handle liquids directly.
1.3 Some provisions of this guide may be applicable to the use of an energy dispersive X-ray spectrometer.
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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 the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Guide9 pagesEnglish language
- Guide9 pagesEnglish language
SIGNIFICANCE AND USE
5.1 This sampling practice is useful for converting material taken from ingots or other solid materials into a homogeneous solid sample suitable for direct excitation on a spark atomic emission or X-ray fluorescence spectrometer. The resultant button may itself be chipped to provide specimens for test methods requiring solutions or chips.
5.2 This practice has been used extensively for the preparation of zirconium, zirconium alloy, titanium, and titanium alloy materials, and is applicable to other reactive, refractory, ferrous and nonferrous alloys, such as cobalt, cobalt alloys, niobium, nickel, nickel alloys, steels, stainless steels, tantalum, tool steels, and tungsten.
SCOPE
1.1 This practice covers the preparation of solid samples of reactive and refractory metals and alloys by electric arc remelting. The samples for melting may be in the form of chips, turnings, wires, sponge and powdered metals.
1.1.1 This practice is also suitable for preparation of solid samples of other metals, such as steels, stainless steels, tool steels, nickel, nickel alloys, cobalt, and cobalt alloys.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 9.
1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
- Standard3 pagesEnglish language
- Standard3 pagesEnglish language
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.”
(A) * Reagent on which ACS specifications exist.
† ACS specification exists but does not cover all requirements.
For concentration of laboratory reagent, see Table 2.(B) Contains at least 50 % H3PO2.
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.
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.
- Standard12 pagesEnglish language
- Standard12 pagesEnglish language
ABSTRACT
This practice covers general recommendations for photoelectric photometers and spectrometers and for photometric practice for chemical analysis of metals, ores, and related materials. However, this practice does not include a description of every apparatus nor does it present recommendations on every detail of practice in photometric or spectrophotometric methods of chemical analysis of metals. To improve photoelectric photometers and spectrophotometers, some suggestions related to their components are mentioned, in particular, the radiation source (illuminant), filters, monochromators, absorption cells, photosensitive tubes, and current-measuring devices. In addition, prior to using photometric methods in the chemical analysis of metals, ores, and related materials, it is recommended that a complete photometric investigation of the reaction be performed. The investigation shall involve the study of the specificity of the reagent used to produce absorption; validity of Beer's law; effects of salts, solvent, pH, temperature, concentration of reagents, and the order of adding reagents; time required for absorption development and the stability of the absorption; absorption curve of the reagent and the absorbing substances; and optimum concentration range for quantitative analysis.
SCOPE
1.1 This practice covers general recommendations for photoelectric photometers and spectrophotometers and for photometric practice prescribed in ASTM methods for chemical analysis of metals, sufficient to supplement adequately the ASTM methods. A summary of the fundamental theory and practice of photometry is given. No attempt has been made, however, to include in this practice a description of every apparatus or to present recommendations on every detail of practice in ASTM photometric or spectrophotometric methods of chemical analysis of metals.2
1.2 These recommendations are intended to apply to the ASTM photometric and spectrophotometric methods for chemical analysis of metals when such standards make definite reference to this practice, as covered in Section 4.
1.3 In this practice, the terms “photometric” and “photometry” encompass both filter photometers and spectrophotometers, while “spectrophotometry” is reserved for spectrophotometers alone.
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 the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard8 pagesEnglish language
- Standard8 pagesEnglish language
SIGNIFICANCE AND USE
4.1 This guide is intended to assist those writing or revising compositional specifications, sampling practices, and test methods for ferrous and non-ferrous metals, ores, and related materials. It is directed toward those areas that must be addressed to properly coordinate compositional specification, sampling practice, and test methods. Its use will help ensure that compositional requirements are clearly defined and that sampling practices and test methods are available to meet product specifications.
4.2 This guide does not attempt to define which elements should be controlled, where samples should be taken, or how they should be analyzed. These items are addressed in standards such as Specification A276, Methods, Practices and Terminology A751, Test Method E34, Practice E255, Test Method E342, and Test Methods E350.
4.3 A primary purpose for ASTM sampling practices and test methods is to provide widely-accepted and tested methodology for use in meeting ASTM product specifications. Although it is recognized that individual laboratories are free to use other methods, the availability of ASTM approved methodology is essential for referee purposes and to demonstrate that properly equipped laboratories can make the required measurements.
4.4 Sampling practices and test methods to be recommended for use in testing a given product are most easily selected cooperatively by the specification-writing and the methods-writing committees that have jurisdiction over the product. When existing sampling or test methods do not meet the needs of the new product specification standard, the specification-writing committee should request that the methods-writing committee develop the required standards. ASTM Committee E01 is responsible for test methods and practices covering the sampling and analysis of most metals, ores, and related materials.
SCOPE
1.1 This guide covers procedures for specifying compositional requirements and identifying appropriate sampling and quantitative analysis test methods to be referenced in product specification standards for metals, ores, and related materials. It is not intended to replace or conflict with either individual product specifications or standards covering broad classifications of products such as Test Methods A751.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Guide3 pagesEnglish language
- Guide3 pagesEnglish language
SIGNIFICANCE AND USE
4.1 This practice describes the essential components of a wavelength dispersive X-ray spectrometer. This description is presented so that the user or potential user may gain a cursory understanding of the structure of an X-ray spectrometer system. It also provides a means for comparing and evaluating different systems as well as understanding the capabilities and limitations of each instrument.
4.2 It is understood that a laboratory may implement this practice or an X-ray fluorescence method in partnership with a manufacturer of the analytical instrumentation. If a laboratory chooses to consult with an instrument manufacturer, then the following should be considered. The laboratory should have an idea of the alloy matrices to be analyzed, elements and mass fraction ranges to be determined, and the expected performance requirements for each of these elements. The laboratory should inform the instrument manufacturer of these requirements so they may develop an analytical method which meets the laboratory’s expectations. Typically, instrument manufacturers customize the instrument configuration to satisfy the end-user’s requirements for elemental coverage, elemental precision, and detection limits. Instrument manufacturer developed analytical methods may include specific parameters for sample excitation, wavelengths, inter-element interference corrections, calibration and regression, equipment configuration/installation, and sample preparation requirements. Laboratories should have a basic understanding of the parameters derived by the manufacturer.
SCOPE
1.1 This practice covers the components of a wavelength dispersive X-ray spectrometer that are basic to its operation and to the quality of its performance. It is not the intent of this practice to specify component tolerances or performance criteria, as these are unique for each instrument. However, the practice does attempt to identify which tolerances are critical and thus which should be specified.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use. Specific safety hazard statements are given in 5.3.1.2 and 5.3.2.4, and in Section 7.
- Standard5 pagesEnglish language
- Standard5 pagesEnglish language
SIGNIFICANCE AND USE
4.1 This practice is intended for users who are attempting to establish GF-AAS procedures. It should be helpful for establishing a complete atomic absorption analysis program.
SCOPE
1.1 This practice covers a procedure for the determination of microgram per millilitre (μg/mL) or lower concentrations of elements in solution using a graphite furnace attached to an atomic absorption spectrometer. A general description of the equipment is provided. Recommendations are made for preparing the instrument for measurements, establishing optimum temperature conditions and other criteria which should result in determining a useful calibration concentration range, and measuring and calculating the test solution analyte concentration.
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific safety hazard statements are given in Section 9.
- Standard9 pagesEnglish language
- Standard9 pagesEnglish language
ABSTRACT
This practice describes the photomultiplier properties that are essential to their judicious selection and use of in emission and absorption spectrometry. The properties covered here include structural features, electrical properties, and characteristics involved in precautions and problems. The structural features covered are envelope configurations, window materials, electrical connections, and housing for the external structure, and the photocathode, dynodes and anode, and rigidness of structural components for the internal structure. Electrical properties, on the other hand, incorporate the following: optical-electronic characteristics of the photocathode including spectral response; current amplification including gain per stage, overall gain, gain control (voltage-divider bridge), linearity of response, and anode saturation; signal nature; dark current including cathode size, internal aperture, and refrigeration effects; noise nature including additivity of noise power, signal-to-noise ratio, equivalent noise input; and photomultiplier properties as a component in an electrical circuit including output impedance, response time, and signal gating and integration possibilities. Finally, the characteristics involved in precautions and problems cover fatigue and hysteresis effects, illumination of photocathode, and gas leakage.
SCOPE
1.1 This practice covers photomultiplier properties that are essential to their judicious selection and use in emission and absorption spectrometry. Descriptions of these properties can be found in the following sections:
Section
Structural Features
4
General
4.1
External Structure
4.2
Internal Structure
4.3
Electrical Properties
5
General
5.1
Optical-Electronic Characteristics of the Photocathode
5.2
Current Amplification
5.3
Signal Nature
5.4
Dark Current
5.5
Noise Nature
5.6
Photomultiplier as a Component in an Electrical Circuit
5.7
Precautions and Problems
6
General
6.1
Fatigue and Hysteresis Effects
6.2
Illumination of Photocathode
6.3
Gas Leakage
6.4
Recommendations on Important Selection Criteria
7
1.2 Radiation in the frequency range common to analytical emission and absorption spectrometry is detected by photomultipliers presently to the exclusion of most other transducers. Detection limits, analytical sensitivity, and accuracy depend on the characteristics of these current-amplifying detectors as well as other factors in the system.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
4.1 This practice is for optimizing the parameters used in the determination of trace elements in metals and alloys by the electrothermal atomic absorption spectrometric method. It also describes the practice for checking the spectrometer performance. The work is expected to be performed in a properly equipped laboratory by trained operators and appropriate disposal procedures are to be followed.
SCOPE
1.1 This practice covers the optimization of electrothermal atomic absorption spectrometers and the checking of spectrometer performance criteria.
1.2 The values stated in SI units are to be regarded as the standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard5 pagesEnglish language
- Standard5 pagesEnglish language
SIGNIFICANCE AND USE
4.1 Accuracy in quantitative X-ray spectrometric analysis depends upon adequate accounting for interelement effects either through sample preparation or through mathematical correction procedures, or both. This guide is intended to serve as an introduction to users of X-ray fluorescence correction methods. For this reason, only selected mathematical models for correcting interelement effects are presented. The reader is referred to several texts for a more comprehensive treatment of the subject (2-7).
SCOPE
1.1 This guide is an introduction to mathematical procedures for correction of interelement (matrix) effects in quantitative X-ray spectrometric analysis.
1.1.1 The procedures described correct only for the interelement effect(s) arising from a homogeneous chemical composition of the specimen. Effects related to either particle size, or mineralogical or metallurgical phases in a specimen are not treated.
1.1.2 These procedures apply to both wavelength and energy-dispersive X-ray spectrometry where the specimen is considered to be infinitely thick, flat, and homogeneous with respect to the depth of penetration of the exciting X-rays (1).2
1.2 This document is not intended to be a comprehensive treatment of the many different techniques employed to compensate for interelement effects. Consult Refs (2-5) for descriptions of other commonly used techniques such as standard addition, internal standardization, etc.
- Guide12 pagesEnglish language
- Guide12 pagesEnglish language
SIGNIFICANCE AND USE
5.1 X-ray fluorescence spectrometry can provide an accurate and precise determination of metallic and many non-metallic elements in a wide variety of solid and liquid materials. This guide covers the information that should be included in an X-ray spectrometric analytical method and provides direction to the analyst for determining the optimum conditions needed to achieve acceptable accuracy.
5.2 The accuracy of a determination is a function of the calibration scheme, the sample preparation, and the sample homogeneity. Close attention to all aspects of these areas is necessary to achieve acceptable results.
5.3 All concepts discussed in this guide are explored in detail in a number of published texts and in the scientific literature.
SCOPE
1.1 This guide provides guidelines for developing and describing analytical procedures using a wavelength dispersive X-ray spectrometer for elemental analysis of solid metals, ores, and related materials. Material forms discussed herein include solids, powders, and solid forms prepared by chemical and physical processes such as borate fusion and pressing of briquettes.
1.2 Liquids are not discussed in this guide because they are much less frequently encountered in metals and mining laboratories. However, aqueous liquids can be processed by borate fusion to create solids specimens, and X-ray spectrometers can be equipped to handle liquids directly.
1.3 Some provisions of this guide may be applicable to the use of an energy dispersive X-ray spectrometer.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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 the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Guide9 pagesEnglish language
- Guide9 pagesEnglish language
SIGNIFICANCE AND USE
5.1 This practice is intended as a fundamental guide for the calibration, standardization, and daily control of the analytical curves for atomic emission spectrometers.
5.2 It is assumed that this practice will be used by trained operators capable of performing the procedures described herein.
SCOPE
1.1 This practice covers guidance for establishing and controlling atomic emission spectrochemical analytical curves. The generation of analytical curves and their routine control are considered as separate although interrelated operations. This practice is applicable to atomic emission spectrometers.Note 1—X-ray emission spectrometric applications are no longer covered by this practice. See Guides E1361 and E1621 for discussion of this technique.
1.1.1 Since computer programs are readily available to run multiple linear regressions that can be used to generate analytical curves and since most instruments include this feature, this practice does not go into detail on the procedure. However, some recommendations are given on evaluating the equations that are generated.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard4 pagesEnglish language
- Standard4 pagesEnglish language
SIGNIFICANCE AND USE
4.1 This practice describes the essential components of the DCP spectrometer. This description allows the user or potential user to gain a basic understanding of this system. It also provides a means of comparing and evaluating this system with similar systems, as well as understanding the capabilities and limitations of each instrument.
SCOPE
1.1 This practice describes the components of a direct current plasma (DCP) atomic emission spectrometer. This practice does not attempt to specify component tolerances or performance criteria. This practice does, however, attempt to identify critical factors affecting bias, precision, and sensitivity. A prospective user should consult with the vendor before placing an order to design a testing protocol for demonstrating that the instrument meets all anticipated needs.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are give in Section 9.
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
4.1 An increasing number of optical emission spectrometers are equipped with enclosed excitation stands and plasmas which call for atmospheres other than ambient air. This practice is intended for users of such equipment.
SCOPE
1.1 This practice covers general recommendations relative to the use of gas shielding during and immediately prior to specimen excitation in optical emission spectrochemical analysis. It describes the concept of excitation shielding, the means of introducing gases, and the variables involved with handling gases.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard4 pagesEnglish language
SIGNIFICANCE AND USE
Analyses using DCP-AES require proper preparation of test solutions, accurate calibration, and control of analytical procedures. ASTM test methods that refer to this guide shall provide specifics on test solutions, calibration, and procedures.
DCP-AES analysis is primarily concerned with testing materials for compliance with specifications, but may range from qualitative estimations to umpire analysis. These may involve measuring major and minor constituents or trace impurities, or both. This guide suggests some approaches to these different analytical needs.
This guide assists analysts in developing new methods.
It is assumed that the users of this guide will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that the work will be performed in a properly equipped laboratory.
This guide does not purport to define all of the quality assurance parameters necessary for DCP-AES analysis. Analysts should ensure that proper quality assurance procedures are followed, especially those defined by the test method. Refer to Guide E882.
SCOPE
1.1 This guide covers procedures for using a Direct Current Plasma atomic emission spectrometer (DCP-AES) to determine the concentration of elements in solution. Recommendations are provided for preparing and calibrating the instrument, assessing instrument performance, diagnosing and correcting for interferences, measuring test solutions, and calculating results. A method to correct for instrument drift is included.
1.2 This guide does not specify all the operating conditions for a DCP-AES because of the differences between models of these instruments. Analysts should follow instructions provided by the manufacturer of the particular instrument.
1.3 This guide does not attempt to specify in detail all of the hardware components and computer software of the instrument. It is assumed that the instrument, whether commercially available, modified, or custom built, will be capable of performing the analyses for which it is intended, and that the analyst has verified this before performing the analysis.
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 the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 7.
- Guide8 pagesEnglish language
- Guide8 pagesEnglish language
SIGNIFICANCE AND USE
This practice describes the essential components of a wavelength-dispersive X-ray spectrometer. This description is presented so that the user or potential user may gain a cursory understanding of the structure of an X-ray spectrometer system. It also provides a means for comparing and evaluating different systems as well as understanding the capabilities and limitations of each instrument.
SCOPE
1.1 This practice covers the components of a wavelength-dispersive X-ray spectrometer that are basic to its operation and to the quality of its performance. It is not the intent of this practice to specify component tolerances or performance criteria, as these are unique for each instrument. The document does, however, attempt to identify which of these are critical and thus which should be specified.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific safety hazard statements are given in 5.3.1.2 and 5.3.2.4, and in Section 7.
1.3 There are several books and publications from the National Institute of Standards and Technology and the U.S. Government Printing Office , which deal with the subject of X-ray safety. Refer also to Practice E416.
- Standard5 pagesEnglish language
SIGNIFICANCE AND USE
This practice describes the essential components of an inductively-coupled plasma atomic emission spectrometer (ICP-AES). The components include excitation/radio-frequency generators, sample introduction systems, spectrometers, detectors, and signal processing and displays. This description allows the user or potential user to gain a cursory understanding of an ICP-AES system. This practice also provides a means for comparing and evaluating various systems, as well as understanding the capabilities and limitations of each instrument.
Training—The vendor should provide training in safety, basic theory of ICP spectrochemical analysis, operations of hardware and software, and routine maintenance for at least one operator. Training ideally should consist of the basic operation of the instrument at the time of installation, followed by an in-depth course one or two months later. Advanced courses are also offered at several of the important spectroscopy meetings that occur throughout the year as well as by independent training institutes. Furthermore, several independent consultants are available who can provide training, in most cases at the user's site.
SCOPE
1.1 This practice describes the components of an inductively-coupled plasma atomic emission spectrometer (ICP-AES) that are basic to its operation and to the quality of its performance. This practice identifies critical factors affecting accuracy, precision, and sensitivity. It is not the intent of this practice to specify component tolerances or performance criteria, since these are unique for each instrument. A prospective user should consult with the vendor before placing an order, to design a testing protocol to demonstrate that the instrument meets all anticipated needs.
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific safety hazard statements are given in Section 13.
- Standard14 pagesEnglish language
SIGNIFICANCE AND USE
This sampling practice is useful for converting chips, turnings, and wires taken from ingots or other solid materials into a homogeneous solid sample suitable for direct excitation on an optical emission or X-ray fluorescence spectrometer. The resultant button may itself be chipped to provide samples for plasma emission, atomic absorption, and wet chemical analysis.
This practice has been used extensively for the preparation of zirconium, zirconium alloy, titanium, and titanium alloy materials, and is applicable to other reactive, refractory, ferrous and nonferrous alloys, such as cobalt, cobalt alloys, columbium (niobium), nickel, nickel alloys, stainless steels, tantalum, tool steels, and tungsten.
SCOPE
1.1 This practice covers the preparation of solid samples of reactive and refractory metals and alloys by electric arc remelting. The samples for melting may be in the form of chips, turnings, wires, and sponge. Powdered metals need to be compacted before melting.
1.1.1 This practice is also suitable for preparation of solid samples of other metals, such as steels, stainless steels, tool steels, nickel, nickel alloys, cobalt, and cobalt alloys by electric arc remelting.
This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 9.
- Standard3 pagesEnglish language
- Standard3 pagesEnglish language
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 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.
- Standard12 pagesEnglish language
- Standard12 pagesEnglish language
SIGNIFICANCE AND USE
Equipment and procedures described in this guide are comparative methods and are intended for identification or segregation, or both, of pieces or lots of metals that were mixed or lost their identity during certain manufacturing operations. It is presumed that all pieces or lots of metal have been previously checked and did meet applicable specifications.
The equipment and procedures described in this guide may also be suitable for identifying or segregating, or both, scrap metals.
SCOPE
1.1 This guide covers the identification or segregation, or both, of mixed metal lots under plant conditions using trained plant personnel.
1.2 The identification is not intended to have the accuracy and reliability of procedures performed in a laboratory using laboratory equipment under optimum conditions, and performed by trained chemists or technicians. The identification is not intended to establish whether a given piece or lot of metal meets specifications.
1.3 Segregation of certain metal combinations is not always possible with procedures provided in this guide and can be subject to errors.
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 the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Guide3 pagesEnglish language
- Guide3 pagesEnglish language
ABSTRACT
This practice covers general recommendations for photoelectric photometers and spectrometers and for photometric practice for chemical analysis of metals, ores, and related materials. However, this practice does not include a description of every apparatus nor does it present recommendations on every detail of practice in photometric or spectrophotometric methods of chemical analysis of metals. To improve photoelectric photometers and spectrophotometers, some suggestions related to their components are mentioned, in particular, the radiation source (illuminant), filters, monochromators, absorption cells, photosensitive tubes, and current-measuring devices. In addition, prior to using photometric methods in the chemical analysis of metals, ores, and related materials, it is recommended that a complete photometric investigation of the reaction be performed. The investigation shall involve the study of the specificity of the reagent used to produce absorption; validity of Beer's law; effects of salts, solvent, pH, temperature, concentration of reagents, and the order of adding reagents; time required for absorption development and the stability of the absorption; absorption curve of the reagent and the absorbing substances; and optimum concentration range for quantitative analysis.
SCOPE
1.1 This practice covers general recommendations for photoelectric photometers and spectrophotometers and for photometric practice prescribed in ASTM methods for chemical analysis of metals, sufficient to supplement adequately the ASTM methods. A summary of the fundamental theory and practice of photometry is given. No attempt has been made, however, to include in this practice a description of every apparatus or to present recommendations on every detail of practice in ASTM photometric or spectrophotometric methods of chemical analysis of metals.
1.2 These recommendations are intended to apply to the ASTM photometric and spectrophotometric methods for chemical analysis of metals when such standards make definite reference to this practice, as covered in Section 4.
1.3 In this practice, the terms “photometric” and “photometry” encompass both filter photometers and spectrophotometers, while “spectrophotometry” is reserved for spectrophotometers alone.
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 the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard8 pagesEnglish language
- Standard8 pagesEnglish language
SIGNIFICANCE AND USE
This guide is intended to assist those writing or revising compositional specifications, sampling practices, and test methods for ferrous and non-ferrous metals, ores, and related materials. It is directed toward those areas that must be addressed to properly coordinate compositional specification, sampling practice, and test methods. Its use will help ensure that compositional requirements are clearly defined and that sampling practices and test methods are available to meet product specifications.
This guide does not attempt to define which elements should be controlled, where samples should be taken, or how they should be analyzed. These items are addressed in standards such as Specification A276, Methods, Practices and Terminology A751, Test Method E34, Practice E255, Test Method E342, and Test Methods E350.
A primary purpose for ASTM sampling practices and test methods is to provide widely-accepted and tested methodology for use in meeting ASTM product specifications. Although it is recognized that individual laboratories are free to use other methods, the availability of ASTM approved methodology is essential for referee purposes and to demonstrate that properly equipped laboratories can make the required measurements.
Sampling practices and test methods to be recommended for use in testing a given product are most easily selected cooperatively by the specification-writing and the methods-writing committees that have jurisdiction over the product. When existing sampling or test methods do not meet the needs of the new product specification standard, the specification-writing committee should request that the methods-writing committee develop the required standards. ASTM Committee E01 is responsible for test methods and practices covering the sampling and analysis of most metals, ores, and related materials.
SCOPE
1.1 This guide covers procedures for specifying compositional requirements and identifying appropriate sampling and quantitative analysis methodologies to be referenced in product specification standards for metals, ores, and related materials. It is not intended to replace or conflict with either individual product specifications or standards covering broad classifications of products such as Test Methods A751.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Guide3 pagesEnglish language
- Guide3 pagesEnglish language
SIGNIFICANCE AND USE
This practice is intended for users who are attempting to establish GF-AAS procedures. It should be helpful for establishing a complete atomic absorption analysis program.
SCOPE
1.1 This practice covers a procedure for the determination of microgram per millilitre (μg/mL) or lower concentrations of elements in solution using a graphite furnace attached to an atomic absorption spectrometer. A general description of the equipment is provided. Recommendations are made for preparing the instrument for measurements, establishing optimum temperature conditions and other criteria which should result in determining a useful calibration concentration range, and measuring and calculating the test solution analyte concentration.
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific safety hazard statements are given in Section 9.
- Standard9 pagesEnglish language
- Standard9 pagesEnglish language
SIGNIFICANCE AND USE
The grinding materials used for the preparation of the surfaces of specimens prior to analysis by optical emission or X-ray emission spectroscopy can contaminate the surface and thus produce erroneous results. This guide provides examples of the effects of these contaminations and recommendations for evaluating grinding materials to eliminate or reduce these effects in spectrochemical analysis.
The examples given in this guide are not the only contaminations which can occur. Especially in X-ray spectrometry, all phases of the surface preparation should be examined for potential contamination effects.
Analytical significance of the contaminations observed depends on the needs of the analyst for the particular application at a given concentration level.
SCOPE
1.1 This guide covers recommendations for the evaluation of various grinding materials used to prepare the surfaces of specimens to be analyzed by optical emission or X-ray emission spectroscopy.
1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Guide5 pagesEnglish language
- Guide5 pagesEnglish language
SIGNIFICANCE AND USE
An increasing number of optical emission spectrometers are equipped with enclosed excitation stands and plasmas which call for atmospheres other than ambient air. This practice is intended for users of such equipment.
SCOPE
1.1 This practice covers general recommendations relative to the use of gas shielding during and immediately prior to specimen excitation in optical emission spectrochemical analysis. It describes the concept of excitation shielding, the means of introducing gases, and the variables involved with handling gases.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard4 pagesEnglish language
SIGNIFICANCE AND USE
This practice describes the essential components of the DCP spectrometer. This description allows the user or potential user to gain a basic understanding of this system. It also provides a means of comparing and evaluating this system with similar systems, as well as understanding the capabilities and limitations of each instrument.
SCOPE
1.1 This practice describes the components of a direct current plasma (DCP) atomic emission spectrometer. This practice does not attempt to specify component tolerances or performance criteria. This practice does, however, attempt to identify critical factors affecting bias, precision, and sensitivity. A prospective user should consult with the vendor before placing an order to design a testing protocol for demonstrating that the instrument meets all anticipated needs.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are give in Section 9.
WITHDRAWN RATIONALE
This practice describes the components of a direct current plasma (DCP) atomic emission spectrometer.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, this practice was withdrawn in October 2004 because it is no longer in practice.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
ABSTRACT
This practice describes the photomultiplier properties that are essential to their judicious selection and use of in emission and absorption spectrometry. The properties covered here include structural features, electrical properties, and characteristics involved in precautions and problems. The structural features covered are envelope configurations, window materials, electrical connections, and housing for the external structure, and the photocathode, dynodes and anode, and rigidness of structural components for the internal structure. Electrical properties, on the other hand, incorporate the following: optical-electronic characteristics of the photocathode including spectral response; current amplification including gain per stage, overall gain, gain control (voltage-divider bridge), linearity of response, and anode saturation; signal nature; dark current including cathode size, internal aperture, and refrigeration effects; noise nature including additivity of noise power, signal-to-noise ratio, equivalent noise input; and photomultiplier properties as a component in an electrical circuit including output impedance, response time, and signal gating and integration possibilities. Finally, the characteristics involved in precautions and problems cover fatigue and hysteresis effects, illumination of photocathode, and gas leakage.
SCOPE
1.1 This practice covers photomultiplier properties that are essential to their judicious selection and use of photomultipliers in emission and absorption spectrometry. Descriptions of these properties can be found in the following sections:
Section Structural Features4 General4.1 External Structure4.2 Internal Structure4.3 Electrical Properties5 General5.1 Optical-Electronic Characteristics of the Photocathode5.2 Current Amplification5.3 Signal Nature5.4 Dark Current5.5 Noise Nature5.6 Photomultiplier as a Component in an Electrical Circuit5.7 Precautions and Problems6 General6.1 Fatigue and Hysteresis Effects6.2 Illumination of Photocathode6.3 Gas Leakage6.4 Recommendations on Important Selection Criteria7
1.2 Radiation in the frequency range common to analytical emission and absorption spectrometry is detected by photomultipliers presently to the exclusion of most other transducers. Detection limits, analytical sensitivity, and accuracy depend on the characteristics of these current-amplifying detectors as well as other factors in the system.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard6 pagesEnglish language
- Standard6 pagesEnglish language
SIGNIFICANCE AND USE
Analyses using DCP-AES require proper preparation of test solutions, accurate calibration, and control of analytical procedures. ASTM test methods that refer to this guide shall provide specifics on test solutions, calibration, and procedures.
DCP-AES analysis is primarily concerned with testing materials for compliance with specifications, but may range from qualitative estimations to umpire analysis. These may involve measuring major and minor constituents or trace impurities, or both. This guide suggests some approaches to these different analytical needs.
This guide assists analysts in developing new methods.
It is assumed that the users of this guide will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that the work will be performed in a properly equipped laboratory.
This guide does not purport to define all of the quality assurance parameters necessary for DCP-AES analysis. Analysts should ensure that proper quality assurance procedures are followed, especially those defined by the test method. Refer to Guide E 882.
SCOPE
1.1 This guide covers procedures for using a direct current plasma-atomic emission spectrometer (DCP-AES) to determine the concentration of elements in solution. Recommendations are provided for preparing and calibrating the instrument, assessing instrument performance, diagnosing and correcting for interferences, measuring test solutions, and calculating results. A method to correct for instrument drift is included.
1.2 This guide does not specify all the operating conditions for a DCP-AES because of the differences between models of these instruments. Analysts should follow instructions provided by the manufacturer of the particular instrument.
1.3 This guide does not attempt to specify in detail all of the hardware components and computer software of the instrument. It is assumed that the instrument, whether commercially available, modified, or custom built, will be capable of performing the analyses for which it is intended, and that the analyst has verified this before performing the analysis.
This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 7.
- Guide8 pagesEnglish language
- Guide8 pagesEnglish language
SIGNIFICANCE AND USE
This practice is intended as a fundamental guide for the calibration, standardization, and daily control of the analytical curves for atomic emission spectrometers.
It is assumed that this practice will be used by trained operators capable of performing the procedures described herein.
SCOPE
1.1 This practice provides guidance for establishing and controlling atomic emission spectrochemical analytical curves. The generation of analytical curves and their routine control are considered as separate although interrelated operations. This practice is applicable to atomic emission spectrometers.Note 1
X-ray emission spectrometric applications are no longer covered by this practice. See Guides E 1361 and E 1621 for discussion of this technique.
1.1.1 Since computer programs are readily available to run multiple linear regressions that can be used to generate analytical curves and since most instruments include this feature, this practice does not go into detail on the procedure. However, some recommendations are given on evaluating the equations that are generated.
This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
- Standard4 pagesEnglish language
SIGNIFICANCE AND USE
This sampling practice is useful for converting chips, turnings, and wires taken from ingots or other solid materials into a homogeneous solid sample suitable for direct excitation on an optical emission or X-ray fluorescence spectrometer. The resultant button may itself be chipped to provide samples for plasma emission, atomic absorption, and wet chemical analysis.
This practice has been used extensively for the preparation of zirconium, zirconium alloy, titanium, and titanium alloy materials, and is applicable to other reactive, refractory, ferrous and nonferrous alloys, such as cobalt, cobalt alloys, columbium (niobium), nickel, nickel alloys, stainless steels, tantalum, tool steels, and tungsten.
SCOPE
1.1 This practice covers the preparation of solid samples of reactive and refractory metals and alloys by electric arc remelting. The samples for melting may be in the form of chips, turnings, wires, and sponge. Powdered metals need to be compacted before melting.
1.1.1 This practice is also suitable for preparation of solid samples of other metals, such as steels, stainless steels, tool steels, nickel, nickel alloys, cobalt, and cobalt alloys by electric arc remelting.
This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 9.
- Standard3 pagesEnglish language
SIGNIFICANCE AND USE
Accuracy in quantitative X-ray spectrometric analysis depends upon adequate accounting for interelement effects either through sample preparation or through mathematical correction procedures, or both. This guide is intended to serve as an introduction to users of X-ray fluorescence correction methods. For this reason, only selected mathematical models for correcting interelement effects are presented. The reader is referred to several texts for a more comprehensive treatment of the subject (2-7).
SCOPE
1.1 This guide is an introduction to mathematical procedures for correction of interelement (matrix) effects in quantitative X-ray spectrometric analysis.
1.1.1 The procedures described correct only for the interelement effect(s) arising from a homogeneous chemical composition of the specimen. Effects related to either particle size, or mineralogical or metallurgical phases in a specimen are not treated.
1.1.2 These procedures apply to both wavelength and energy-dispersive X-ray spectrometry where the specimen is considered to be infinitely thick, flat, and homogeneous with respect to the depth of penetration of the exciting X rays (2-5).
1.2 This document is not intended to be a comprehensive treatment of the many different techniques employed to compensate for interelement effects. Consult Refs () for descriptions of other commonly used techniques such as standard addition, internal standardization, etc.
- Guide12 pagesEnglish language
Frequently Asked Questions
E01.20 is a Technical Committee within ASTM International. It is named "Fundamental Practices". This committee has published 112 standards.
E01.20 develops ASTM standards in the area of Information technology. Currently, there are 112 published standards from this technical committee.
ASTM is a standardization organization that develops and publishes standards to support industry, commerce, and regulatory requirements.
A Technical Committee (TC) in ASTM is a group of experts responsible for developing international standards in a specific technical area. TCs are composed of national member body delegates and work through consensus to create standards that meet global industry needs. Each TC may have subcommittees (SCs) and working groups (WGs) for specialized topics.