ASTM D4864-14

Standard Test Method for Determination of Traces of Methanol in Propylene Concentrates by Gas Chromatography (Withdrawn 2016)

SIGNIFICANCE AND USE
5.1 Methanol is a common impurity in propylene concentrate. It can have a deleterious effect on various processes that use propylene concentrate as a feedstock.
SCOPE
1.1 This test method covers the determination of methanol in propylene concentrates in the range of approximately 4 mg/kg to 40 mg/kg (parts-per-million by mass).  
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
Note 1: There is no direct acceptable SI equivalent for screw threads.  
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 warning statements are given in 11.1.1, 11.2.1, and 12.11.
WITHDRAWN RATIONALE
This test method covered the determination of methanol in propylene concentrates in the range of approximately 4 mg/kg to 40 mg/kg (parts-per-million by mass).
Formerly under the jurisdiction of Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants, this test method was withdrawn in December 2016. This standard is being withdrawn without replacement because of the availability of more reliable methods with better precision.

General Information

• Status: Withdrawn
• Publication Date: 14-Jul-2014
• Withdrawal Date: 12-Dec-2016
• ICS: 71.080.10 - Aliphatic hydrocarbons
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.D0.03 - Propylene

Relations

• Referred By: ASTM D5273-18 - Standard Guide for Analysis of Propylene Concentrates
• Effective Date: 15-Jul-2014
• Referred By: ASTM D5274-00(2019) - Standard Guide for Analysis of 1,3–Butadiene Product
• Effective Date: 15-Jul-2014

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4864 − 14
Standard Test Method for
Determination of Traces of Methanol in Propylene
1
Concentrates by Gas Chromatography
This standard is issued under the fixed designation D4864; 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.
1. Scope* 3.2.1.1 Discussion—Typicallytheoutagetubeisdesignedto
allow a ullage or vapor space of 15 % to 20 % of the volume
1.1 This test method covers the determination of methanol
of the sample cylinder.
in propylene concentrates in the range of approximately
4 mg⁄kg to 40 mg/kg (parts-per-million by mass).
4. Summary of Test Method
1.2 The values stated in SI units are to be regarded as
4.1 A known mass of water is pressured into a sample
standard. The values given in parentheses are for information
cylinder containing a known amount of liquified propylene
only.
concentrate. The contents in the cylinder are shaken and the
NOTE 1—There is no direct acceptable SI equivalent for screw threads.
water/methanol phase is withdrawn.Areproducible volume of
1.3 This standard does not purport to address all of the the extract is then injected into the analytical column of a gas
safety concerns, if any, associated with its use. It is the
chromatograph (GC) equipped with either a thermal conduc-
responsibility of the user of this standard to establish appro- tivity or a flame ionization detector. The methanol concentra-
priate safety and health practices and determine the applica-
tion is calculated from the area of the methanol peak using
bility of regulatory limitations prior to use. Specific warning calibration and extraction factors obtained from synthetic
statements are given in 11.1.1, 11.2.1, and 12.11.
blends of known methanol content.
2. Referenced Documents
5. Significance and Use
2
2.1 ASTM Standards:
5.1 Methanol is a common impurity in propylene concen-
D4307 Practice for Preparation of Liquid Blends for Use as
trate. It can have a deleterious effect on various processes that
Analytical Standards
use propylene concentrate as a feedstock.
E260 Practice for Packed Column Gas Chromatography
6. Interferences
3. Terminology
6.1 There are no known interferences using the GC columns
3.1 Definitions:
referenced in this test method. However, any water-soluble
3.1.1 propylene concentrate—concentrate containing more
component that co-elutes with methanol on any other GC
than 90 % propylene.
column used would interfere.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 outage tube—a length of tubing, usually metal, at- 7. Apparatus
tached to the inside of a valve on a high pressure sampling
7.1 Gas Chromatograph—Any GC equipped with either
cylinder such that a fixed percentage of liquid may be expelled
flame ionization or thermal conductivity detectors with an
from the cylinder to create a specified ullage or vapor space for
overall sensitivity sufficient to detect at least 4 mg/kg of
safety in storage, handling, and transportation.
methanol.
7.2 Column—Any GC column that separates methanol from
1
water, other alcohols, and any co-extracted hydrocarbons.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
NOTE 2—See Table 1 for a suitable list of columns and Fig. 1 and Fig.
Subcommittee D02.D0.03 on Propylene.
2 for examples of chromatograms.Also, refer to Practice E260 for typical
Current edition approved July 15, 2014. Published August 2014. Originally
instructions in preparing such columns. Alternatively, columns can be
approved in 1988. Last previous edition approved in 2013 as D4864 – 90 (2013).
purchased from commercial sources.
DOI: 10.1520/D4864-14.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
7.3 Data Handling System—Any commercially available
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
GC integrator or GC computer system capable of accurately
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. integrating the area of the methanol peak is satisfactory.
*A Summary of Changes section appears at the end of this standard
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D4864 − 14
A
TABLE 1 Suitable Gas Chromatographic Columns and Temperatures
Column Oven Temperature,°
Column Size, m × mm Tubing Type Packing Coating, µm Thickness
Number C
1 1.22 × 6.35 O.D. SS 15 % Carbowax 1540 on . 90
60/80 Chromosorb W AW
2 3.05 × 4.76 O.D. SS 80/100 mes
...