ASTM D8130-17

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.
Designation:D8130 −17
Standard Test Method for
Determination of Metals in Purified Terephthalic Acid (PTA)
by Inductively Coupled Plasma Atomic Emission
Spectrometric Method
This standard is issued under the fixed designation D8130; 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 D6809 Guide for Quality Control and Quality Assurance
Procedures for Aromatic Hydrocarbons and Related Ma-
1.1 This test method covers the determination of metal
terials
elements in purified terephthalic acid (PTA) by inductively
D7111 Test Method for Determination of Trace Elements in
coupled plasma atomic emission spectrometry (ICP-AES).This
Middle Distillate Fuels by Inductively Coupled Plasma
method is applicable to PTA samples containing sodium,
Atomic Emission Spectrometry (ICP-AES)
chromium, cobalt, aluminum, titanium, potassium,
E29 Practice for Using Significant Digits in Test Data to
magnesium, manganese, iron, nickel, molybdenum and cal-
Determine Conformance with Specifications
cium over 0.055 mg/kg, respectively.
E177 Practice for Use of the Terms Precision and Bias in
1.2 In determining the conformance of the test results using
ASTM Test Methods
thismethodtoapplicablespecification,resultsshallberounded
E691 Practice for Conducting an Interlaboratory Study to
off in accordance with the rounding-off method of Practice
Determine the Precision of a Test Method
E29.
2.2 ISO Document:
EN ISO 8213 Chemical products for industrial use—
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this Sampling techniques—Solid chemical products in the
form of particles varying from powders to coarse lumps
standard.
2.3 Other Document:
1.4 This standard does not purport to address all of the
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
safety concerns, if any, associated with its use. It is the
1910.1200
responsibility of the user of this standard to establish appro-
priate safety, health and environmental practices and deter-
3. Summary of Test Method
mine the applicability of regulatory limitations prior to use.
3.1 A PTA sample is dissolved in ammonium hydroxide
1.5 This international standard was developed in accor-
solution.Calibrationstandardsarepreparedbymixingmetallic
dance with internationally recognized principles on standard-
standard materials in ammonium hydroxide solution.An inter-
ization established in the Decision on Principles for the
nal standard material is added to the calibration standards and
Development of International Standards, Guides and Recom-
the sample solution to compensate for variations of test
mendations issued by the World Trade Organization Technical
specimenintroductionefficiency.Thecalibrationstandardsand
Barriers to Trade (TBT) Committee.
the sample solution are aspirated into the ICP-AES instrument.
2. Referenced Documents
The concentrations of the elements in the sample solution are
calculatedbycomparingemissionintensityratiosofthesample
2.1 ASTM Standards:
solution and calibration standards to the internal standard.
D1193 Specification for Reagent Water
D4790 Terminology ofAromatic Hydrocarbons and Related
4. Significance and Use
Chemicals
4.1 The presence of metals in PTA used for the production
1 of polyester is undesirable because they may speed up or slow
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
down the reaction and be impurities in the final product.
bility of Subcommittee D16.02 on Oxygenated Aromatics.
Current edition approved Aug. 1, 2017. Published September 2017. DOI:
10.1520/D8130-17. Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 4th Floor, New York, NY 10036, http://www.ansi.org.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Available from U.S. Government Printing Office, Superintendent of
Standards volume information, refer to the standard’s Document Summary page on Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
the ASTM website. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D8130−17
A
TABLE 1 Element and Recommended Wavelengths
6.4 Purity of Water—Unless otherwise indicated, references
Element Wavelength (nm)
to water shall be understood to mean Type I reagent water
Cobalt 228.616
conforming or exceeding Specification D1193. Freshly drawn
Manganese 257.610
water should be used for preparation of all stock and working
Iron 238.204
standards, and sample solutions.
Chromium 267.716
Nickel 221.648
6.5 Ammonium Hydroxide—25 to 28 %(wt).
Sodium 589.592
NOTE 2—The metal impurities in ammonia hydroxide should be no
Titanium 334.940
Molybdenum 202.033 more than 10 µg/kg, and the non-metallic impurities should be no more
Magnesium 285.231
than 100 mg/kg. The reagent may be purchased.
Potassium 766.490
6.6 Ammonium Hydroxide Solution—Pipette 13 mL of am-
Calcium 317.933
Aluminum 396.153
monia hydroxide (6.5) to a 100 mL volumetric flask, fill the
B
Cadmium 228.802
volumetric flask to the mark with water.
B
Yttrium 371.029
A
6.7 Internal Standard Stock Solution—1000 mg/L. The
These wavelengths are only suggested and do not represent all possible
choices. Other appropriate interference free wavelengths may also be used.
single element chosen for the internal standard should not be a
Consult instrument manufacture’s instructions or other ICP-AES references.
component of the sample or calibration standard. Cadmium
B
Cadmium and Yttrium are used as internal standards.
and yttrium were found to perform well as an internal standard
for this test method and are recommended. The standard may
be purchased.
6.8 Internal Standard Solution—100mg/L.Pipette10mLof
4.2 Determination of the metals in PTA is often required.
Internal Standard stock solution (6.7) to a 100 mL volumetric
This test method is suitable for setting specifications and for
flask, fill the volumetric flask to the mark with water.
use as an internal quality control where these products are
6.9 Single Element Standard Stock Solution—1000 mg/L.
produced or used.
The test elements are listed in Table 1. The standards may be
4.3 This test method covers the determination of sodium,
purchased.
chromium, cobalt, aluminum, titanium, potassium,
magnesium, manganese, iron, nickel, molybdenum and cal- 6.10 Single Element Standard Solution—100 mg/L. Pipette
cium. 10 mL of the single element standard stock solution (6.9)toa
100 mL volumetric flask, fill the volumetric flask to the mark
5. Apparatus with water.
5.1 Inductively-Coupled Plasma Atomic Emission
6.11 Multi-element Mixed Standard Solution—1.0 mg/L.
Spectrometer—Any commercial sequential or simultaneous Pipette 1 mLof each single element standard solution (6.10)to
ICP-AES instrument capable of measuring emission intensities
a 100 mL volumetric flask, fill the volumetric flask to the
of the elements of interest (listed in Table 1). volume mark with water. Seal the volumetric flask and mix
well. Prepare fresh multi-element mixed standard solution
5.2 Analytical Balance, readable to 60.0001 g.
daily when samples are to be analyzed.
6. Reagents and Materials
6.12 Working Standards—The working standards are pre-
pared as follows: pipette 0, 0.5, 1.0, 2.0, 3.0 and 5.0 mLof the
6.1 Purity of Reagents—Unless otherwise indicated, it is
multi-element mixed standard solution (6.11) into six separate
intended that all reagents shall conform to the reagent grade
100 mL volumetric flasks. And then pipette 0.2 mL of the
specification for analytical reagents of theAmerican Chemical
internal standard (6.8) into each volumetric flask. Dilute to the
Society, where such specifications are available. Other grades
mark with the ammonium hydroxide solution (6.6). Seal the
may be used, provided it is first ascertained
...