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ASTM D5399-04

(Test Method)

Standard Test Method for Boiling Point Distribution of Hydrocarbon Solvents by Gas Chromatography

Standard Test Method for Boiling Point Distribution of Hydrocarbon Solvents by Gas Chromatography

SIGNIFICANCE AND USE
The gas chromatographic determination of the boiling point distribution of hydrocarbon solvents can be used as an alternative to conventional distillation methods for control of solvents quality during manufacture, and specification testing.
Boiling point distribution data can be used to monitor the presence of product contaminants and compositional variation during the manufacture of hydrocarbon solvents.
Boiling point distribution data obtained by this test method are not equivalent to those obtained by Test Methods D 86, D 850, D 1078, D 2887, D 2892, and D 3710.
SCOPE
1.1 This test method covers the determination of the boiling point distribution of hydrocarbon solvents by capillary gas chromatography. This test method is limited to samples having a minimum initial boiling point of 37°C (99°F), a maximum final boiling point of 285°C (545°F), and a boiling range of 5 to 150°C (9 to 270°F) as measured by this test method.
1.2 The values stated in SI units are standard. The values given in parentheses are for information purposes only.
1.3 For purposes of determining conformance of an observed or calculated value using this test method to relevant specifications, test result(s) shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E 29.
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.

General Information

Status
Historical
Publication Date
31-May-2004
ICS
71.040.50 - Physicochemical methods of analysis
Technical Committee
D01 - Paint and Related Coatings, Materials, and Applications
Drafting Committee
D01.35 - Solvents, Plasticizers, and Chemical Intermediates
Current Stage
Ref Project

Relations

Replaces
ASTM D5399-95(2000) - Standard Test Method for Boiling Point Distribution of Hydrocarbon Solvents by Gas Chromatography
Effective Date
01-Jun-2004
Replaced By
ASTM D5399-04(2009) - Standard Test Method for Boiling Point Distribution of Hydrocarbon Solvents by Gas Chromatography
Effective Date
01-Jun-2009

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ASTM D5399-04 - Standard Test Method for Boiling Point Distribution of Hydrocarbon Solvents by Gas ChromatographyASTM D5399-04 - Standard Test Method for Boiling Point Distribution of Hydrocarbon Solvents by Gas Chromatography
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ASTM D5399-04 - Standard Test Method for Boiling Point Distribution of Hydrocarbon Solvents by Gas Chromatography
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D5399–04
Standard Test Method for
Boiling Point Distribution of Hydrocarbon Solvents by Gas
1
Chromatography
This standard is issued under the fixed designation D 5399; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope* D 2892 Test Method for Distillation of Crude Petroleum
(15-Theoretical Plate Column)
1.1 This test method covers the determination of the boiling
D 3710 Test Method for Boiling Range Distribution of
point distribution of hydrocarbon solvents by capillary gas
Gasoline and Gasoline Fractions by Gas Chromatography
chromatography. This test method is limited to samples having
E 29 Practice for Using Significant Digits in Test Data to
a minimum initial boiling point of 37°C (99°F), a maximum
Determine Conformance with Specifications
final boiling point of 285°C (545°F), and a boiling range of 5
E 691 Practice for Conducting an Interlaboratory Study to
to 150°C (9 to 270°F) as measured by this test method.
Determine the Precision of a Test Method
1.2 The values stated in SI units are standard. The values
given in parentheses are for information purposes only.
3. Terminology
1.3 For purposes of determining conformance of an ob-
3.1 Definitions:
served or calculated value using this test method to relevant
3.1.1 initial boiling point (IBP)—the point at which a
specifications, test result(s) shall be rounded off “to the nearest
cumulativeareacountequalto0.5 %ofthetotalareaunderthe
unit” in the last right-hand digit used in expressing the
chromatogram is obtained.
specification limit, in accordance with the rounding-off method
3.1.2 final boiling point (FBP)—the point at which a cumu-
of Practice E 29.
lative area count equal to 99.5 % of the total area under the
1.4 This standard does not purport to address all of the
chromatogram is obtained.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 The sample is introduced into a capillary gas chromato-
bility of regulatory limitations prior to use.
graphic column that separates hydrocarbons in the order of
2. Referenced Documents increasing boiling point. The column temperature is raised at a
2 reproducible rate and the area under the chromatogram is
2.1 ASTM Standards:
recorded throughout the run. Boiling points are assigned from
D 86 Test Method for Distillation of Petroleum Products at
a calibration curve obtained under the same conditions by
Atmospheric Pressure
running a known mixture of hydrocarbons covering the boiling
D 850 Test Method for Distillation of Industrial Aromatic
range expected in the sample. From these data, the boiling
Hydrocarbons and Related Materials
point distribution of the sample is obtained.
D 1078 Test Method for Distillation Range of Volatile
Organic Liquids
5. Significance and Use
D 2887 Test Method for Boiling Range Distribution of
5.1 The gas chromatographic determination of the boiling
Petroleum Fractions by Gas Chromatography
point distribution of hydrocarbon solvents can be used as an
alternative to conventional distillation methods for control of
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
solvents quality during manufacture, and specification testing.
and Related Coatings, Materials, andApplications and is the direct responsibility of
5.2 Boiling point distribution data can be used to monitor
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
the presence of product contaminants and compositional varia-
Current edition approved June 1, 2004. Published June 2004. Originally
approved in 1993. Last previous edition approved in 1995 as D 5399 – 95 (2000). tion during the manufacture of hydrocarbon solvents.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.3 Boiling point distribution data obtained by this test
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
method are not equivalent to those obtained by Test Methods
Standards volume information, refer to the standard’s Document Summary page on
D 86, D 850, D 1078, D 2887, D 2892, and D 3710.
the ASTM website.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D5399–04
TABLE 1 Calibration Mixture
6. Apparatus
Peak Number Compound Identification Normal Boiling Point, °C
6.1 Chromatograph—Any gas
...

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Standard Test Method for Boiling Point Distribution of Hydrocarbon Solvents by Gas Chromatography

SIGNIFICANCE AND USE
5.1 The gas chromatographic determination of the boiling point distribution of hydrocarbon solvents can be used as an alternative to conventional distillation methods for control of solvents quality during manufacture, and specification testing.  
5.2 Boiling point distribution data can be used to monitor the presence of product contaminants and compositional variation during the manufacture of hydrocarbon solvents.  
5.3 Boiling point distribution data obtained by this test method are not equivalent to those obtained by Test Methods D86, D850, D1078, D2887, D2892, and D3710.
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1.1 This test method covers the determination of the boiling point distribution of hydrocarbon solvents by capillary gas chromatography. This test method is limited to samples having a minimum initial boiling point of 37 °C (99 °F), a maximum final boiling point of 285 °C (545 °F), and a boiling range of 5 °C to 150 °C (9 °F to 270 °F) as measured by this test method.  
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5.1 Many coating properties are markedly affected by the film thickness of the dry film such as adhesion, flexibility, wear, durability, chemical resistance, and hardness. To be able to compare results obtained by different operators, it is essential to measure film thickness carefully.  
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5.5 Multilayered coatings have many interfaces and the instrument will measure to the interface separating the two most acoustically different materials. Some instruments have the ability to detect and measure the individual layer thicknesses in a multi-layer system.  
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SCOPE
1.1 This test method describes the use of ultrasonic film thickness gages to measure accurately and nondestructively the dry film thickness of organic coatings applied over a substrate of dissimilar material. Measurements may be made on field structures, on commercially manufactured products, or on laboratory test specimens. These types of gages can accurately measure the dry film thickness of organic coatings on a variety of substrates such as concrete, wood, wallboard, plastic, fiber composites and metal.  
1.2 This test method is not applicable to coatings that will be readily deformable under load of the measuring instrument as the instrument probe is placed directly on the coating surface to take a reading.  
1.3 The effective range of instruments using the principle of ultrasonics is limited by gage design. A thickness range of 8 μm to 7.60 mm (0.3 to 300 mils) has been demonstrated.  
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3.1 It is important to monitor the anion concentrations and anion contaminants in electrocoat baths. Wet chemical methods are long, tedious, and of questionable accuracy in the ppm range. Ion chromatography offers a fast, convenient and accurate alternative. Since IC analysis of electrocoat bath samples is difficult, the permeates are often analyzed for contaminants. This guide addresses some important considerations for such analyses.
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3.1 The procedure described in this practice is designed to provide a method by which the coating weight of chromium treatments on metal substrates may be determined.  
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4.1 This test method is similar to Test Method D4367 with the exception that capillary columns are used and intended for trace level of benzene in hydrocarbon solvents. The need for trace benzene analysis in hydrocarbon solvents arose because of the increase of more stringent regulation of benzene level in these materials.
SCOPE
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4.1 This test method determines the purity of isophorone, as well as the concentration of various potential impurities, several of which are critical in the application of these solvents.
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Standard Test Method for Determination of the Weight Percent Individual Volatile Organic Compounds in Waterborne Air-Dry Coatings by Gas Chromatography

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5.1 In using Practice D3960 to measure the volatile organic compound content of waterborne coatings, precision can be poor for low volatile organic compound content air-dry coatings if the volatile organic weight percent is determined indirectly. The present method directly identifies and then quantifies the weight percent of individual volatile organic compounds in air-dry coatings (Note 6). The total volatile organic weight percent can be obtained by adding the individual weight percent values (Note 7).
Note 6: The present method may be used to speciate solvent-borne air-dry coatings. However, since these normally contain high, and often complex, quantities of solvent, precision tends to be better using other methods contained in Practice D3960, where the volatile fraction is determined by a direct weight loss determination.
Note 7: Detectable compounds may result from thermal decomposition in a hot injection port or from reaction with the extraction solvent. If it can be shown that a material is a decomposition product, or is the result of a reaction with the extraction solvent, then results for that compound should be discounted from the volatile measured by Test Method D6886.
SCOPE
1.1 This test method is for the determination of the weight percent of individual volatile organic compounds in waterborne air-dry coatings (Note 1).  
1.2 This method may be used for the analysis of coatings containing silanes, siloxanes, and silane-siloxane blends.  
1.3 This method is not suitable for the analysis of coatings that cure by chemical reaction (this includes two-component coatings and coatings which cure when heated) because the dilution herein required will impede the chemical reaction required for these types of coatings.  
1.4 Precision statistics for this method have been determined for waterborne coatings in which the volatile organic compound weight percent is below 5 percent. The method has been used successfully with higher organic content waterborne coatings and with solventborne coatings (Note 2).  
1.5 This method may also be used to measure the exempt volatile organic compound content (for example, acetone, methyl acetate, t-butyl acetate and p-chlorobenzotrifluoride) of waterborne and solvent-borne coatings. Check local regulations for a list of exempt compounds. The methodology is virtually identical to that used in Test Method D6133 which, as written, is specific for only exempt volatile compounds.  
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1.7 Volatile organic compound content of a coating can be calculated using data from Test Method D6886 but requires other data (see Appendix X2.)
Note 1: Data from this method will not always provide the volatile organic compound content of a paint film equivalent to EPA Method 24. Some compounds and some semi-volatile compounds may be considered volatile using the GC conditions specified but will not fully volatilize during the one hour at 110°C conditions of EPA Method 24. Some or all of these materials remain in the paint film and therefore are not considered volatile organic compounds according to EPA Method 24. In addition, some compounds may decompose at the high inlet temperature of the GC. However, note the EPA Method 24 has poor precision and accuracy at low levels of volatile organic compounds.
Note 2: This method measures volatile organic compound weight of air-dry coatings directly as opposed to other methods in Practice D3960 which measure the volatile organic compound weight percent indirectly. A direct measurement of the weight percent particularly in low volatile organic compound content waterborne coatings, generally gives better precision. California Polytechnic State University carried out an extensive study for the California Air Resources Board comparing the precision of the direct method...

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Standard Guide for Forensic Analysis of Geological Materials by Powder X-Ray Diffraction

SIGNIFICANCE AND USE
5.1 The overarching goals of the forensic analysis of geological materials include (A) identification of an unknown material (see 11.3), (B) analysis of soils, sediments, or rocks to restrict their possible geographic origins as part of a provenance analysis (see 11.4), and (C) comparison of two or more samples to assess if they could have originated from the same source or to exclude a common source based on observation of exclusionary differences (see 11.5). XRD is only one analytical method that can be applied to the evidentiary samples in service of these distinct goals. Guidance for the analysis of forensic geological materials can be found in Refs (2-4).  
5.2 Within the analytical scheme of geological materials, XRD analysis is used to: identify the crystalline components within a sample; identify the crystalline components separated from a mixture, typically clay-sized material (see 8.8), or a selected particle class for which additional analysis is needed (see 8.11); or compare two or more samples based on the identified crystalline phases or diffraction patterns (see 11.5).  
5.2.1 Non-destructive XRD analysis can be performed in situ on geological material adhering to a substrate (see 8.12.3).  
5.2.2 The most common forensic applications of XRD to geological materials are (A) identification or confirmation of a selected phase or fraction of a sample (see 8.12), (B) identification of minerals in the clay-sized fractions of soils (see 8.8), and (C) identification of the phases of the hydrated cement component of concrete or mortar.  
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1.1 This guide covers techniques and procedures for the use of powder X-ray diffraction (XRD) in the forensic analysis of geological materials (to include soils, rocks, sediments, and materials derived from them such as concrete), to enable non-consumptive identification of solid crystalline materials present as single components or multi-component mixtures.  
1.2 This guide makes recommendations for the preparation of geological materials for powder XRD analysis with adaptations for samples of limited quantity, instrumental configuration to generate high-quality XRD data, identification of crystalline materials by comparison to published diffraction data, and forensic comparison of XRD patterns from two or more samples of geological materials to support criminal investigations.  
1.3 Units—The values stated in SI units are to be regarded as standard. Other units are avoided, in general, but there is a long-standing tradition of expressing X-ray wavelengths and lattice spacing in units of Ångströms (Å). One Ångström = 10–10 meter (m) = 0.1 nanometer (nm).  
1.4 This standard is intended for use by competent forensic science practitioners with the requisite formal education, discipline-specific training (see Practice E2917), and demonstrated proficiency to perform forensic casework.  
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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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