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ASTM E1747-95(2011)

(Guide)

Standard Guide for Purity of Carbon Dioxide Used in Supercritical Fluid Applications

Standard Guide for Purity of Carbon Dioxide Used in Supercritical Fluid Applications

ABSTRACT
This guide defines purity standards for carbon dioxide to ensure the suitability of liquefied carbon dioxide gas for use in supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) applications. This guide defines quantitation, labeling, and statistical standards for impurities in carbon dioxide that are necessary for successful SFE or SFC laboratory work, and it suggests methods of analysis for quantifying these impurities. These contaminants are those components that either cause detector signals that interfere with those of the target analytes or physically impede the SFE or SFC experiment. Also, this guide is provided for use by specialty gas suppliers who manufacture carbon dioxide specifically for SFE or SFC applications. SFE or SFC CO2 products offered with a claim of adherence to this guide will meet certain absolute purity and contaminant detectability requirements matched to the needs of current SFE or SFC techniques.
SCOPE
1.1 This guide defines purity standards for carbon dioxide to ensure the suitability of liquefied carbon dioxide gas for use in SFE and SFC applications (see Guide E1449 for definitions of terms). This guide defines quantitation, labeling, and statistical standards for impurities in carbon dioxide that are necessary for successful SFE or SFC laboratory work, and it suggests methods of analysis for quantifying these impurities.
1.2 This guide is provided for use by specialty gas suppliers who manufacture carbon dioxide specifically for SFE or SFC applications. SFE or SFC carbon dioxide (CO2) products offered with a claim of adherence to this guide will meet certain absolute purity and contaminant detectability requirements matched to the needs of current SFE or SFC techniques. The use of this guide allows different SFE or SFC CO2 product offerings to be compared on an equal purity basis.
1.3 This guide considers contaminants to be those components that either cause detector signals that interfere with those of the target analytes or physically impede the SFE or SFC experiment.
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 limitations prior to use.

General Information

Status
Historical
Publication Date
31-Oct-2011
ICS
71.100.20 - Gases for industrial application
Technical Committee
E13 - Molecular Spectroscopy and Separation Science
Drafting Committee
E13.19 - Separation Science
Current Stage
Ref Project

Relations

Replaces
ASTM E1747-95(2005) - Standard Guide for Purity of Carbon Dioxide Used in Supercritical Fluid Applications
Effective Date
01-Nov-2011
Replaced By
ASTM E1747-95(2019) - Standard Guide for Purity of Carbon Dioxide Used in Supercritical Fluid Applications
Effective Date
01-Dec-2019

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ASTM E1747-95(2011) - Standard Guide for Purity of Carbon Dioxide Used in Supercritical Fluid ApplicationsASTM E1747-95(2011) - Standard Guide for Purity of Carbon Dioxide Used in Supercritical Fluid Applications
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ASTM E1747-95(2011) - Standard Guide for Purity of Carbon Dioxide Used in Supercritical Fluid Applications
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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: E1747 − 95 (Reapproved 2011)
Standard Guide for
Purity of Carbon Dioxide Used in Supercritical Fluid
1
Applications
This standard is issued under the fixed designation E1747; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
INTRODUCTION
Therapidcommercialdevelopmentofcarbondioxideforuseinsupercriticalfluidextraction(SFE)
and supercritical fluid chromatography (SFC) has hastened the need to establish common purity
standards to be specified by specialty gas suppliers. As a consequence of its isolation from
petrochemical side-streams or as a by-product of fermentation or ammonia synthesis, carbon dioxide
contains a wide range of impurities that can interfere with analytical quantification or instrument
operation.Thisguideisintendedtoserveasaguidetospecialtygassuppliersfortestingthesuitability
of carbon dioxide for use in SFC and SFE applications.
1. Scope responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.1 Thisguidedefinespuritystandardsforcarbondioxideto
bility of limitations prior to use.
ensure the suitability of liquefied carbon dioxide gas for use in
SFE and SFC applications (see Guide E1449 for definitions of
2. Referenced Documents
terms).This guide defines quantitation, labeling, and statistical
2
2.1 ASTM Standards:
standards for impurities in carbon dioxide that are necessary
D2504Test Method for Noncondensable Gases in C and
for successful SFE or SFC laboratory work, and it suggests
2
Lighter Hydrocarbon Products by Gas Chromatography
methods of analysis for quantifying these impurities.
D2820Test Method for C Through C Hydrocarbons in the
1.2 Thisguideisprovidedforusebyspecialtygassuppliers
3
Atmosphere by Gas Chromatography (Withdrawn 1993)
who manufacture carbon dioxide specifically for SFE or SFC
D3670Guide for Determination of Precision and Bias of
applications. SFE or SFC carbon dioxide (CO ) products
2
Methods of Committee D22
offered with a claim of adherence to this guide will meet
D3686Practice for Sampling Atmospheres to Collect Or-
certain absolute purity and contaminant detectability require-
ganic Compound Vapors (Activated Charcoal Tube Ad-
mentsmatchedtotheneedsofcurrentSFEorSFCtechniques.
sorption Method)
TheuseofthisguideallowsdifferentSFEorSFCCO product
2
D3687Practice for Analysis of Organic Compound Vapors
offerings to be compared on an equal purity basis.
Collected by the Activated Charcoal Tube Adsorption
1.3 This guide considers contaminants to be those compo-
Method
nentsthateithercausedetectorsignalsthatinterferewiththose
D4178Practice for Calibrating Moisture Analyzers
of the target analytes or physically impede the SFE or SFC
D4532Test Method for Respirable Dust in Workplace At-
experiment.
mospheres Using Cyclone Samplers
E260Practice for Packed Column Gas Chromatography
1.4 The values stated in SI units are to be regarded as
E355PracticeforGasChromatographyTermsandRelation-
standard. No other units of measurement are included in this
ships
standard.
E594Practice for Testing Flame Ionization Detectors Used
1.5 This standard does not purport to address all of the
in Gas or Supercritical Fluid Chromatography
safety concerns, if any, associated with its use. It is the
1 2
This guide is under the jurisdiction of ASTM Committee E13 on Molecular For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Spectroscopy and Separation Science and is the direct responsibility of Subcom- contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
mittee E13.19 on Separation Science. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Nov. 1, 2011. Published December 2011. Originally the ASTM website.
3
approved in 1995. Last previous edition approved in 2005 as E1747–95(2005). The last approved version of this historical standard is referenced on
DOI: 10.1520/E1747-95R11. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E1747 − 95 (2011)
E697Practice for Use of Electron-Capture Detectors in Gas 3.1.4 Nonvolatile—Materials that leave a nonvolatile (boil-
Chromatography ing point >250°C) residue following the vaporization of liquid
E1449Guidefor Supercritical FluidChromatographyTerms CO , such as small particles and high-boiling solutes, are
2
and Relationships detrimental to both SFE and SFC applications. Species repre-
E1510Practice for Installing Fused Silica Open Tubular sentati
...

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ASTM E1747-95(2019)(Guide)
Standard Guide for Purity of Carbon Dioxide Used in Supercritical Fluid Applications

ABSTRACT
This guide defines purity standards for carbon dioxide to ensure the suitability of liquefied carbon dioxide gas for use in supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) applications. This guide defines quantitation, labeling, and statistical standards for impurities in carbon dioxide that are necessary for successful SFE or SFC laboratory work, and it suggests methods of analysis for quantifying these impurities. These contaminants are those components that either cause detector signals that interfere with those of the target analytes or physically impede the SFE or SFC experiment. Also, this guide is provided for use by specialty gas suppliers who manufacture carbon dioxide specifically for SFE or SFC applications. SFE or SFC CO2 products offered with a claim of adherence to this guide will meet certain absolute purity and contaminant detectability requirements matched to the needs of current SFE or SFC techniques.
SCOPE
1.1 This guide defines purity standards for carbon dioxide to ensure the suitability of liquefied carbon dioxide gas for use in SFE and SFC applications (see Guide E1449 for definitions of terms). This guide defines quantitation, labeling, and statistical standards for impurities in carbon dioxide that are necessary for successful SFE or SFC laboratory work, and it suggests methods of analysis for quantifying these impurities.  
1.2 This guide is provided for use by specialty gas suppliers who manufacture carbon dioxide specifically for SFE or SFC applications. SFE or SFC carbon dioxide (CO2) products offered with a claim of adherence to this guide will meet certain absolute purity and contaminant detectability requirements matched to the needs of current SFE or SFC techniques. The use of this guide allows different SFE or SFC CO2 product offerings to be compared on an equal purity basis.  
1.3 This guide considers contaminants to be those components that either cause detector signals that interfere with those of the target analytes or physically impede the SFE or SFC experiment.  
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, health, and environmental practices and determine the applicability of 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.

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ASTM D8446-22(Test Method)
Standard Test Method for Water Vapor Content in Compressed Air Using Electronic Moisture Analyzers

SIGNIFICANCE AND USE
5.1 Water vapor is ubiquitous and a basic contaminant in compressed air. It cannot be eliminated but shall be controlled. Knowledge of the vapor content of compressed air is important for industrial processes to ensure that compressors that generate compressed air are functioning properly and equipment and systems that use the compressed air will function properly and maintain high reliability. This test method describes the measurement of water vapor using direct readout electronic instrumentation. Measurements are provided as dew point/frost point and calculations of related unitless quantities (ppm) are provided. Sampling techniques and warnings are provided to reduce false readings caused by contamination from the sampling method. Dry compressed air typically has a frost point between –80 °C and –40 °C (0.5 PPMV to 127 PPMV) at atmospheric pressure.  
5.2 Measurement of moisture in compressed air can be done after regulating the pressure down to ATM or measured at elevated pressure up to the full system pressure. When measurements are made of the actual dew point (for example, condensation) or the related property of vapor pressure, the value of the dew point (and vapor pressure) is directly affected by the sample pressure since the vapor pressure is a component of the total pressure. The relationship between vapor pressure and moisture content (and dew point) is well defined below 5 MPa, but at greater pressures, additional study needs to be done to define this relationship.  
5.3 Electronic moisture analyzers are also used for measuring moisture levels in other gases, including gaseous fuels. See Test Method D5454. In addition, tunable diode laser spectroscopy (TDLAS) is another technology that may be applicable to detecting moisture in compressed air. This technology is already being used in gases. See Test Method D7904.
SCOPE
1.1 This test method covers the determination of the water vapor content in compressed air using portable or in-situ electronic moisture analyzers. Such analyzers commonly use sensing cells based on phosphorus pentoxide, P2O5, aluminum oxide, Al2O3, or silicon piezoelectric-type cells or laser-based technologies.  
1.2 This test method is applicable for the range of condensation temperatures from –80 °C to 60 °C.  
1.3 Testing is often performed at reduced pressure from the full pressure of the system or source of compressed air depending on the capability of the specific analyzer. Testing above 2000 kPa may introduce additional uncertainty because of changes in the relationship between water vapor pressure and actual moisture content at elevated pressures.  
1.4 Units—The values stated in SI units are to be regarded as the 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.

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ASTM G114-21(Practice)
Standard Practices for Evaluating the Age Resistance of Polymeric Materials Used in Oxygen Service

SIGNIFICANCE AND USE
5.1 This practice allows the user to evaluate the effect of service or accelerating aging on the oxygen resistance of polymeric materials used in oxygen service.  
5.2 The use of this practice presupposes that the properties used to evaluate the effect of aging can be shown to relate to the intended use of the material, and are also sensitive to the effect of aging.  
5.3 Polymeric materials will, in general, be more susceptible than metals to aging effects as evidenced by irreversible property loss. Such property loss may lead to catastrophic component failure, including a secondary fire, before primary ignition or combustion of the polymeric material occurs.  
5.4 Polymers aged in the presence of oxygen-containing media may undergo many types of reversible and irreversible physical and chemical property change. The severity of the aging conditions determines the extent and type of changes that take place. Polymers are not necessarily degraded by aging, but may be unchanged or improved. For example, aging may drive off volatile materials, thus raising the ignition temperature without compromising mechanical properties. However, aging under prolonged or severe conditions (for example, elevated oxygen concentration) will usually cause a decrease in mechanical performance, while improving resistance to ignition and combustion.  
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1.1 These practices describe procedures that are used to determine the age resistance of plastic, thermosetting, elastomeric, and polymer matrix composite materials exposed to oxygen-containing media.  
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1.5.2 Procedure B: Accelerated Aging Comparative Oxygen Resistance—This procedure is suitable for evaluating materials that are used in ambient temperature service, or at a temperature that is otherwise lower than the aging temperature, and is useful for developing oxygen compatibility rankings on a laboratory comparison basis.  
1.5.3 Procedure C: Accelerated Aging Lifetime Prediction—This procedure is used to determine the relationship between aging temperature and a fixed level of property change, thereby allowing predictions to be made about the effect of prolonged service on oxidative degra...

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Standard Test Method for Minimum Ignition Energy and Quenching Distance in Gaseous Mixtures

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3.1 The minimum energies provide a basis for comparing the ease of ignition of gases. The flatplate ignition quenching distances provide an important verification of existing minimum ignition energy data and give approximate values of the propagation quenching distances of the various mixtures. It is emphasized that maximum safe experimental gaps, as from “flame-proof” or “explosion-proof” studies, are less than the flat-plate ignition quenching distances.
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1.1 This test method covers the determination of minimum energy for ignition (initiation of deflagration) and associated flat-plate ignition quenching distances.2 The complete description is specific to alkane or alkene fuels admixed with air at normal ambient temperature and pressure. This method is applicable to mixtures of the specified fuels with air, varying from the most easily ignitable mixture to mixtures near to, in theory, the limit-of-flammability compositions.
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1.3 This method is one of several being developed by Committee E27 for determining the hazards of chemicals, including their vapors in air or other oxidant atmospheres. The measurements are useful in assessing fuel ignitability hazards due to static or other electrical sparks. However, the quenching distance data must be used with great prudence since they are primarily applicable to the ignition stage and therefore, represent values for initial pressure and not the smaller values existing at higher pressures.  
1.4 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.  
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1.6 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 precautions are listed in Section 5.  
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3.1 The laboratory preparation of gas blends of known composition is required to provide primary standards for the calibration of chromatographic and other types of analytical instrumentation.
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1.1 This practice covers a laboratory procedure for the preparation of low-pressure multicomponent gas blends. The technique is applicable to the blending of components at percent levels and can be extended to lower concentrations by performing dilutions of a previously prepared base blend. The maximum blend pressure obtainable is dependent upon the range of the manometer used, but ordinarily is about 101 kPa (760 mm Hg). Components must not be condensable at the maximum blend pressure.  
1.2 The possible presence of small leaks in the manifold blending system will preclude applicability of the method to blends containing part per million concentrations of oxygen or nitrogen.  
1.3 This practice is restricted to those compounds that do not react with each other, the manifold, or the blend cylinder.  
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 D2779-92(2020)(Test Method)
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5.1 Knowledge of gas solubility is of extreme importance in the lubrication of gas compressors. It is believed to be a substantial factor in boundary lubrication, where the sudden release of dissolved gas may cause cavitation erosion, or even collapse of the fluid film. In hydraulic and seal oils, gas dissolved at high pressure can cause excessive foaming on release of the pressure. In aviation oils and fuels, the difference in pressure between take-off and cruise altitude can cause foaming out of the storage vessels and interrupt flow to the pumps.
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1.1 This test method covers the estimation of the equilibrium solubility of several common gases encountered in the aerospace industry in hydrocarbon liquids. These include petroleum fractions with densities in the range from 0.63 to 0.90 at 288 K (59°F). The solubilities can be estimated over the temperature range 228 K (−50°F) to 423 K (302°F).  
1.2 This test method is based on the Clausius-Clapeyron equation, Henry's law, and the perfect gas law, with empirically assigned constants for the variation with density and for each gas.  
1.3 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.  
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.  
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5.1 Oxygen gas transmission rate is an important determinant of the protection afforded by barrier materials. It is not, however, the sole determinant, and additional tests, based on experience, must be used to correlate package performance with O2GTR. This test method is suitable as a referee method of testing, provided that the user and source have agreed on sampling procedures, standardization procedures, test conditions, and acceptance criteria.
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1.1 This test method covers a procedure for the determination of the steady-state rate of transmission of oxygen gas into packages. More specifically, the method is applicable to packages that in normal use will enclose a dry environment.  
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5.1 Carbon dioxide gas transmission rate (CO2TR) is an important determinant of the packaging protection afforded by barrier materials. It is not, however, the sole determinant, and additional tests, based on experience, must be used to correlate packaging performance with CO2TR. It is suitable as a referee method of testing, provided that purchaser and seller have agreed on sampling procedures, standardization procedures, test conditions and acceptance criteria.
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1.1 This method covers a procedure for determination of the steady-state rate of transmission of carbon dioxide gas through plastics in the form of film, sheeting, laminates, coextrusions, or plastic-coated papers or fabrics. It provides for the determination of (1) carbon dioxide gas transmission rate (CO2TR), (2) the permeance of the film to carbon dioxide gas (PCO2), and (3) carbon dioxide permeability coefficient (P’CO2) in the case of homogeneous materials.  
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.  
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ASTM D2713-20(Test Method)
Standard Test Method for Dryness of Propane (Valve Freeze Method)

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5.1 This test is a functional test in which the water concentration in the product is related to product behavior characteristics in a pressure-reducing system of special design to arrive at a measure of product acceptability in common use applications. Experience has demonstrated that excessive water content (dissolved water) will cause freeze-up difficulties in pressure reducing systems.
SCOPE
1.1 This test method covers the measurement of the dryness of propane products that do not contain antifreeze agents such as, but not limited to, commercial propane and special duty propane (see Specification D1835).  
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ASTM B827-05(2020)(Practice)
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4.1 Mixed flowing gas (MFG) tests are used to simulate or amplify exposure to environmental conditions which electrical contacts or connectors can be expected to experience in various application environments (1, 2).4  
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4.5 The MFG exposures are generally used in conjunction with procedures which evaluate contact or connector electrical performance such as measurement of electrical contact resistance before and after MFG exposure.  
4.6 The MFG tests are useful for connector systems whose contact surfaces are plated or clad with gold or other precious metal finishes. For such surfaces, environmentally produced failures are often due to high resistance or intermittences caused by the formation of insulating contamination in the contact region. This contamination, in the form of films and hard particles, is generally the result of pore corrosion and corrosion product migration or tarnish creepage from pores in the precious metal coating and from unplated base metal boundaries, if present.  
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SCOPE
1.1 This practice provides procedures for conducting environmental tests involving exposures to controlled quantities of corrosive gas mixtures.  
1.2 This practice provides for the required equipment and methods for gas, temperature, and humidity control which enable tests to be conducted in a reproducible manner. Reproducibility is measured through the use of control coupons whose corrosion films are evaluated by mass gain, coulometry, or by various electron and X-ray beam analysis techniques. Reproducibility can also be measured by in situ corrosion rate monitors using electrical resistance or mass/frequency change methods.  
1.3 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 become familiar with all hazards including those identified in the appropriate Material Safety Data Sheet (MSDS) for this product/material as provided by the manufacturer, to establish appropriate safety, health, and environmental practices, and determine the applicability of regulatory limitations prior to use. See 5.1.2.4.  
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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