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ASTM E1172-87(2011)

(Practice)

Standard Practice for Describing and Specifying a Wavelength-Dispersive X-Ray Spectrometer

Standard Practice for Describing and Specifying a Wavelength-Dispersive X-Ray Spectrometer

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.

General Information

Status
Historical
Publication Date
14-Nov-2011
ICS
17.180.30 - Optical measuring instruments
Technical Committee
E01 - Analytical Chemistry for Metals, Ores, and Related Materials
Drafting Committee
E01.20 - Fundamental Practices
Current Stage
Ref Project

Relations

Replaces
ASTM E1172-87(2003) - Standard Practice for Describing and Specifying a Wavelength-Dispersive X-Ray Spectrometer
Effective Date
15-Nov-2011
Referred By
ASTM D7085-04(2018) - Standard Guide for Determination of Chemical Elements in Fluid Catalytic Cracking Catalysts by X-ray Fluorescence Spectrometry (XRF)
Effective Date
15-Nov-2011
Referred By
ASTM E539-19 - Standard Test Method for Analysis of Titanium Alloys by Wavelength Dispersive X-Ray Fluorescence Spectrometry
Effective Date
15-Nov-2011
Referred By
ASTM F2063-18 - Standard Specification for Wrought Nickel-Titanium Shape Memory Alloys for Medical Devices and Surgical Implants
Effective Date
15-Nov-2011

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ASTM E1172-87(2011) - Standard Practice for Describing and Specifying a Wavelength-Dispersive X-Ray SpectrometerASTM E1172-87(2011) - Standard Practice for Describing and Specifying a Wavelength-Dispersive X-Ray Spectrometer
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ASTM E1172-87(2011) - Standard Practice for Describing and Specifying a Wavelength-Dispersive X-Ray Spectrometer
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E1172 − 87(Reapproved 2011)
Standard Practice for
Describing and Specifying a Wavelength-Dispersive X-Ray
1
Spectrometer
This standard is issued under the fixed designation E1172; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
6
1. Scope trochemical Laboratory (Withdrawn 2005)
E876 Practice for Use of Statistics in the Evaluation of
1.1 This practice covers the components of a wavelength-
6
Spectrometric Data (Withdrawn 2003)
dispersive X-ray spectrometer that are basic to its operation
and to the quality of its performance. It is not the intent of this
3. Terminology
practice to specify component tolerances or performance
3.1 For terminology relating to X-ray spectrometry, refer to
criteria, as these are unique for each instrument. The document
Terminology E135.
does, however, attempt to identify which of these are critical
and thus which should be specified.
4. Significance and Use
1.2 This standard does not purport to address all of the
4.1 This practice describes the essential components of a
safety concerns, if any, associated with its use. It is the
wavelength-dispersive X-ray spectrometer. This description is
responsibility of the user of this standard to establish appro-
presented so that the user or potential user may gain a cursory
priate safety and health practices and determine the applica-
understanding of the structure of an X-ray spectrometer sys-
bility of regulatory limitations prior to use. Specific safety
tem. It also provides a means for comparing and evaluating
hazard statements are given in 5.3.1.2 and 5.3.2.4, and in
different systems as well as understanding the capabilities and
Section 7.
limitations of each instrument.
1.3 There are several books and publications from the
2
National Institute of Standards and Technology and the U.S.
5. Description of Equipment
3,4
Government Printing Office which deal with the subject of
5
5.1 Types of Spectrometers—X-ray spectrometers can be
X-ray safety. Refer also to Practice E416.
classified as sequential, simultaneous, or a combination of
2. Referenced Documents these two (hybrid).
5.1.1 Sequential Spectrometers—The sequential spectrom-
5
2.1 ASTM Standards:
eter disperses and detects secondary X rays by means of an
E135 Terminology Relating to Analytical Chemistry for
adjustable monochromator called a goniometer. In flat-crystal
Metals, Ores, and Related Materials
instruments, secondary X rays are emitted from the specimen
E416 Practice for Planning and Safe Operation of a Spec-
and nonparallel X rays are eliminated by means of a Soller slit
(collimator). The parallel beam of X rays strikes a flat
analyzing crystal which disperses the X rays according to their
1
This practice is under the jurisdiction of ASTM Committee E01 on Analytical
wavelengths. The dispersed X rays are then measured by
Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.20 on Fundamental Practices. suitable detectors. Adjusting the goniometer varies the angle
Current edition approved Nov. 15, 2011. Published June 2012. Originally
between the specimen, crystal, and detector, permitting the
approved in 1987. Last previous edition approved in 2003 as E1172 – 87(2003).
measurement of different wavelengths and therefore different
DOI: 10.1520/E1172-87R11.
2
elements. Sequential instruments containing curved-crystal
NBS Handbook, X-Ray Protection, HB76, and NBS Handbook 111, ANSI
N43.2-1971, available from National Institute of Standards and Technology,
optics are less common. This design substitutes curved for flat
Gaithersburg, MD 20899.
crystals and entrance and exit slits for collimators.
3
Radiation Safety Recommendations for X-Ray Diffraction and Spectrographic
5.1.2 Simultaneous Spectrometers—Simultaneous spec-
Equipment, No. MORP 68-14, 1968, available from U.S. Department of Health,
Education, and Welfare, Rockville, MD 20850. trometers use separate monochromators to measure each ele-
4
U.S. Government Handbook 93, Safety Standards for Non-Medical X-Ray and
ment. These instruments are for the most part of fixed
Sealed Gamma-Ray Sources, Part 1, General, Superintendent of Documents,
configuration, although some simultaneous instruments have a
available from U.S. Government Printing Office, Washington, DC 22025.
5
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced o
...

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ASTM E1172-22(Practice)
Standard Practice for Describing and Specifying a Wavelength Dispersive X-Ray Spectrometer

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.  
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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.  
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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.
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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.  
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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.  
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ASTM D7726-11(2023)(Guide)
Standard Guide for The Use of Various Turbidimeter Technologies for Measurement of Turbidity in Water

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5.1 Turbidity is a measure of scattered light that results from the interaction between a beam of light and particulate material in a liquid sample. Particulate material is typically undesirable in water from a health perspective and its removal is often required when the water is intended for consumption. Thus, turbidity has been used as a key indicator for water quality to assess the health and quality of environmental water sources. Higher turbidity values are typically associated with poorer water quality.  
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5.1 Cryo-TEM is a technique used to record high resolution images of samples that are frozen and embedded in a thin layer of vitrified, amorphous ice (2-5). Because vitrification occurs so rapidly, the resultant specimen is almost instantly frozen, yielding a very accurate representation of the specimen at the moment of freezing, without the distortions typically associated with air drying delicate wet samples. Once frozen, images of the specimen are recorded at low temperature using a specially designed electron microscope equipped with a cryo-holder capable of operating under low dose conditions in order to prevent beam induced structural damage to the specimen. The cryo-TEM technique is the consensus choice to directly observe, analyze and accurately measure liposomes suspended in aqueous solutions. Fig. 1 illustrates this by comparing an electron micrograph from an air-dried negatively stained liposomal preparation with an electron micrograph of the same solution imaged by cryo-TEM.
FIG. 1 Left—An Electron Micrograph of an Air-Dried Liposomal Preparation that has been Negatively Stained with 2 % Uranyl Acetate for Contrast; Right—An Electron Micrograph of the Same Liposomal Preparation Prepared as a Frozen Vitrified Specimen for Cryo-TEM
Note 1: Both images are shown to the same scale; scale bar is 200 nm.  
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ASTM D3321-19(2023)(Test Method)
Standard Test Method for Use of the Refractometer for Field Test Determination of the Freezing Point of Aqueous Engine Coolants

SIGNIFICANCE AND USE
4.1 This practice is commonly used by vehicle service personnel to determine the freezing point, in degrees Celsius or Fahrenheit, of aqueous solutions of commercial ethylene and propylene glycol-based coolant. A durable hand-held refractometer is available that reads the freezing point, directly, in degrees Celsius or Fahrenheit, when a few drops of engine coolant are properly placed on the temperature-compensated prism surface of the refractometer. This refractometer is for glycol and water solutions, and is not suitable for other coolant solutions.  
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1.1 This test method covers the use of a portable refractometer for determining the approximate freezing protection provided by ethylene and propylene glycol-based coolant solutions as used in engine cooling systems and special applications.  
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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.

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ASTM E520-08(2023)(Practice)
Standard Practice for Describing Photomultiplier Detectors in Emission and Absorption Spectrometry

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.

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Standard Guide for Relative Intensity Correction of Raman Spectrometers

SIGNIFICANCE AND USE
4.1 Generally, Raman spectra measured using grating-based dispersive or Fourier transform Raman spectrometers have not been corrected for the instrumental response (spectral responsivity of the detection system). Raman spectra obtained with different instruments may show significant variations in the measured relative peak intensities of a sample compound. This is mainly as a result of differences in their wavelength-dependent optical transmission and detector efficiencies. These variations can be particularly large when widely different laser excitation wavelengths are used, but can occur when the same laser excitation is used and spectra of the same compound are compared between instruments. This is illustrated in Fig. 1, which shows the uncorrected luminescence spectrum of SRM 2241, acquired upon four different commercially available Raman spectrometers operating with 785 nm laser excitation. Instrumental response variations can also occur on the same instrument after a component change or service work has been performed. Each spectrometer, due to its unique combination of filters, grating, collection optics and detector response, has a very unique spectral response. The spectrometer dependent spectral response will of course also affect the shape of Raman spectra acquired upon these systems. The shape of this response is not to be construed as either “good or bad” but is the result of design considerations by the spectrometer manufacturer. For instance, as shown in Fig. 1, spectral coverage can vary considerably between spectrometer systems. This is typically a deliberate tradeoff in spectrometer design, where spectral coverage is sacrificed for enhanced spectral resolution.
FIG. 1 SRM 2241 Measured on Four Commercial Raman Spectrometers Utilizing 785 nm Excitation  
4.2 Variations in spectral peak intensities can be mostly corrected through calibration of the Raman intensity (y) axis. The conventional method of calibration of the spectral response of a Raman...
SCOPE
1.1 This guide is designed to enable the user to correct a Raman spectrometer for its relative spectral-intensity response function using NIST Standard Reference Materials2 in the 224X series (currently SRMs 2241, 2242, 2243, 2244, 2245, 2246), or a calibrated irradiance source. This relative intensity correction procedure will enable the intercomparison of Raman spectra acquired from differing instruments, excitation wavelengths, and laboratories.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 Because of the significant dangers associated with the use of lasers, ANSI Z136.1 or suitable regional standards should be followed in conjunction with this practice.  
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.

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ASTM E388-04(2023)(Test Method)
Standard Test Method for Wavelength Accuracy and Spectral Bandwidth of Fluorescence Spectrometers

ABSTRACT
This test method covers the testing of the spectral bandwidth and wavelength accuracy of fluorescence spectrometers that use a monochromator for emission wavelength selection and photomultiplier tube detection. The method can be applied to instruments that use multi-element detectors, such as diode arrays, but results must be interpreted carefully. Atomic lines between 250 nm and 1000 nm are used in the method. The difference between the apparent wavelength and the known wavelength for a series of atomic emission lines is used as a test for wavelength accuracy. The apparent width of some of these lines is used as a test for spectral bandwidth.
SCOPE
1.1 This test method covers the testing of the spectral bandwidth and wavelength accuracy of fluorescence spectrometers that use a monochromator for emission wavelength selection and photomultiplier tube detection. This test method can be applied to instruments that use multi-element detectors, such as diode arrays, but results must be interpreted carefully. This test method uses atomic lines between 250 nm and 1000 nm.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.

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