ASTM D8130-17 (2024) 用电感耦合等离子体原子发射光谱法测定精对苯二甲酸（PTA）中金属的标准试验方法

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Designation: D8130 −17 (Reapproved 2024)
Standard Test Method for
Determination of Metals in Puriﬁed Terephthalic Acid (PTA)
by Inductively Coupled Plasma Atomic Emission
Spectrometric Method
1
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
1.1 This test method covers the determination of metal
elements in puriﬁed terephthalic acid (PTA) by inductively
coupled plasma atomic emission spectrometry (ICP-
AES). This method is applicable to PTA samples containing
sodium, chromium, cobalt, aluminum, titanium, potassium,
magnesium, manganese, iron, nickel, molybdenum, and cal-
cium over 0.055 mg/kg, respectively.
1.2 In determining the conformance of the test results using
this method to applicable speciﬁcation, results shall be rounded
off in accordance with the rounding-off method of Practice
E29.
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 establish appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
2
D1193 Speciﬁcation for Reagent Water
D4790 Terminology of Aromatic Hydrocarbons and Related
Chemicals
D6809 Guide for Quality Control and Quality Assurance
Procedures for Aromatic Hydrocarbons and Related Ma-
terials
D7111 Test Method for Determination of Trace Elements in
Middle Distillate Fuels by Inductively Coupled Plasma
Atomic Emission Spectrometry (ICP-AES)
E29 Practice for Using Signiﬁcant Digits in Test Data to
Determine Conformance with Speciﬁcations
E177 Practice for Use of the Terms Precision and Bias in
ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
2.2 ISO Document:
3
EN ISO 8213 Chemical products for industrial use—
Sampling techniques—Solid chemical products in the
form of particles varying from powders to coarse lumps
2.3 Other Document:
4
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
1910.1200
3. Summary of Test Method
3.1 A PTA sample is dissolved in ammonium hydroxide
solution. Calibration standards are prepared by mixing metallic
standard materials in ammonium hydroxide solution. An inter-
nal standard material is added to the calibration standards and
the sample solution to compensate for variations of test
specimen introduction efficiency. The calibration standards and
the sample solution are aspirated into the ICP-AES instrument.
The concentrations of the elements in the sample solution are
calculated by comparing emission intensity ratios of the sample
solution and calibration standards to the internal standard.
1
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
bility of Subcommittee D16.02 on Oxygenated Aromatics.
Current edition approved July 1, 2024. Published July 2024. Originally approved
in 2017. Last previous edition approved in 2017 as D8130 – 17. DOI: 10.1520/
D8130-17R24.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at www.astm.org/contact. For Annual Book of
ASTM Standards volume information, refer to the standard’s Document Summary
page on the ASTM website.
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org.
4
Available from U.S. Government Printing Office, Superintendent of
Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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.
1

4. Signiﬁcance and Use
4.1 The presence of metals in PTA used for the production
of polyester is undesirable because they may speed up or slow
down the reaction and be impurities in the ﬁnal product.
4.2 Determination of the metals in PTA is often required.
This test method is suitable for setting speciﬁcations and for
use as an internal quality control where these products are
produced or used.
4.3 This test method covers the determination of sodium,
chromium, cobalt, aluminum, titanium, potassium,
magnesium, manganese, iron, nickel, molybdenum, and cal-
cium.
5. Apparatus
5.1 Inductively-Coupled Plasma Atomic Emission
Spectrometer—Any commercial sequential or simultaneous
ICP-AES instrument capable of measuring emission intensities
of the elements of interest (listed in Table 1).
5.2 Analytical Balance, readable to 60.0001 g.
6. Reagents and Materials
6.1 Purity of Reagents—Unless otherwise indicated, it is
intended that all reagents shall conform to the reagent grade
speciﬁcation for analytical reagents of the American Chemical
Society,
5
where such speciﬁcations are available. Other grades
may be used, provided it is ﬁrst ascertained that the reagent is
of sufficiently high purity to permit its use without lessening
the performance or accuracy of the determination. Reagent
chemicals shall be used for all tests.
NOTE 1—Calibration and detection limits of this test method can be
biased by the purity of the reagents.
6.2 Argon Gas—99.99 % minimum purity. (Warning—
Argon is under high pressure.)
6.3 Nitrogen Gas—99.99 % minimum purity. (Warning—
Nitrogen is under high pressure.)
6.4 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean Type I reagent water
conforming or exceeding Speciﬁcation D1193. Freshly drawn
water should be used for preparation of all stock and working
standards, and sample solutions.
6.5 Ammonium Hydroxide—25 %(wt) to 28 %(wt).
NOTE 2—The metal impurities in ammonia hydroxide should be no
more than 10 µg/kg, and the non-metallic impurities should be no more
than 100 mg/kg. The reagent may be purchased.
6.6 Ammonium Hydroxide Solution—Pipette 13 mL of am-
monia hydroxide (6.5) to a 100 mL volumetric ﬂask, ﬁll the
volumetric ﬂask to the mark with water.
6.7 Internal Standard Stock Solution—1000 mg/L. The
single element chosen for the internal standard should not be a
component of the sample or calibration standard. Cadmium
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—100 mg/L. Pipette 10 mL of
Internal Standard stock solution (6.7) to a 100 mL volumetric
ﬂask, ﬁll the volumetric ﬂask to the mark with water.
6.9 Single Element Standard Stock Solution—1000 mg/L.
The test elements are listed in Table 1. The standards may be
purchased.
6.10 Single Element Standard Solution—100 mg/L. Pipette
10 mL of the single element standard stock solution (6.9) to a
100 mL volumetric ﬂask, ﬁll the volumetric ﬂask to the mark
with water.
6.11 Multi-element Mixed Standard Solution—1.0 mg/L.
Pipette 1 mL of each single element standard solution (6.10) to
a100 mL volumetric ﬂask, ﬁll the volumetric ﬂask to the
volume mark with water. Seal the volumetric ﬂask and mix
well. Prepare fresh multi-element mixed standard solution
daily when samples are to be analyzed.
6.12 Working Standards—The working standards are pre-
pared as follows: pipette 0 mL, 0.5 mL, 1.0 mL, 2.0 mL,
3.0 mL, and 5.0 mL of the multi-element mixed standard
solution (6.11) into six separate 100 mL volumetric ﬂasks. And
then pipette 0.2 mL of the internal standard (6.8) into each
volumetric ﬂask. Dilute to the mark with the ammonium
hydroxide solution (6.6). Seal the volumetric ﬂask and mix
well. The working standards will be 0.0 µg ⁄L, 5.0 µg ⁄L,
10.0 µg ⁄L, 20.0 µg ⁄L, 30.0 µg ⁄L, 50.0 µg/L of each element of
interest, and 200.0 µg/L of internal standard. Working stan-
dards are to be prepared daily when samples are to be analyzed.
7. Hazards
7.1 Consult current federal regulations, supplier’s Safety
Data Sheets, and local regulations for all materials used in this
test method.
8. Sampling and Test Specimens
8.1 Use only representative samples obtained as described
in EN ISO 8213, unless otherwise speciﬁed.
5
ACS Reagent Chemicals, Speciﬁcations and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
DC. For suggestions on the testing of reagents not listed by the American Chemical
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
copeial Convention, Inc. (USPC), Rockville, MD.
TABLE 1 Element and Recommended Wavelengths
A
Element Wavelength (nm)
Cobalt 228.616
Manganese 257.610
Iron 238.204
Chromium 267.716
Nickel 221.648
Sodium 589.592
Titanium 334.940
Molybdenum 202.033
Magnesium 285.231
Potassium 766.490
Calcium 317.933
Aluminum 396.153
Cadmium
B
228.802
Yttrium
B
371.029
A
These wavelengths are only suggested and do not represent all possible
choices. Other appropriate interference free wavelengths may also be used.
Consult instrument manufacture’s instructions or other ICP-AES references.
B
Cadmium and Yttrium are used as internal standards.
D8130 − 17 (2024)
2

9. Preparation of Apparatus
9.1 Prepare the ICP spectrometer according to the manufac-
turer’s instructions and parameter settings for the elements of
interest. Table 1 provides recommended element wavelengths
for PTA, other wavelengths may be used due to possible
instrument variations or spectral interferences from sample.
The optical path of ICP-AES can be purged with argon or
another high purity gas (for example, nitrogen) recommended
by the manufacturer. Before igniting the plasma, inspect the
quartz torch to make sure that it is clean. If carbon build-up is
observed, replace the torch and make the manufacturer’s
recommended adjustments for this problem. Warm up the
instrument while purging the optics for the time period
recommended by the ICP manufacturer.
10. Procedure
10.1 Calibration:
10.1.1 Aspirate ammonium hydroxide solution (6.6) and
zero the instrument. Analyze the working standards (6.12). A
calibration curve is constructed by plotting the concentrations
of each element of interest on the X-axis and the emission
intensity ratios of each element to the internal element on the
Y-axis. Most ICP spectrometers have software that automati-
cally performs the calculations to establish the calibration
curve when using an internal standard. The calibration curve
needs to be performed when a new batch of samples is to be
analyzed.
10.2 Analysis of Samples:
10.2.1 Weigh, to the nearest 0.0001 g, 7 g to 7.5 g of PTA
sample, and dissolved in ammonia hydroxide solution (6.6).
Quantitatively transfer dissolved sample into a 100 mL volu-
metric ﬂask, pipette 0.2 mL of the internal standard (6.8), and
dilute with ammonia hydroxide solution (6.6) to the mark. Seal
the volumetric ﬂask and mix well.
10.2.2 Aspirate ammonium hydroxide solution (6.6) and
zero the instrument. Analyze sample solution under the same
conditions that the working standards were run. The ICP
instrument software generates concentration values for each
element.
11. Calculation
11.1 Calculate the concentrations of element iin PTA as
follows:
X
i
5c
i
×v
w×1000 (1)
where:
X
i
= concentration of element iin PTA sample, mg/kg,
c
i
= concentration of element iin the sample solution, µg/L,
v= volume of volumetric ﬂask, mL, and
w= weight of PTA sample, g.
12. Report
12.1 Report the average value of metal content in mg/kg, to
the nearest 0.001 mg/kg. In condition of concentration of the
element of interest in PTA sample less than 0.055 mg/kg, the
results should be reported <0.055 mg/kg, respectively.
12.2 Report the following information in the report.
12.2.1 The complete identiﬁcation of the sample tested.
12.2.2 Any deviation from the procedure speciﬁed.
12.2.3 Results of the test.
12.2.4 Any abnormal situations observed during the test.
13. Precision and Bias
13.1 The precision of this test method is based on an
intra-laboratory study of Test Method D8130, Determination of
Metals in Puriﬁed Terephthalic Acid (PTA) by Inductively
Coupled Plasma Atomic Emission Spectrometric Method,
conducted in 2017. One laboratory tested one PTA sample for
metals. Every test result represents an individual determina-
tion. The laboratory reported 20 replicate results for each
analysis/material combination in order to estimate the repeat-
ability limits of the standard. Practice E691 was followed for
the design and analysis of the repeatability data; the details are
given in Research Report No. RR:D16-1062.
6
13.1.1 Repeatability Limit (r)—Two test results obtained
within one laboratory shall be judged not equivalent if they
differ by more than the “r” value for that material; “r” is the
interval representing the critical difference between two test
results for the same material, obtained by the same operator
using the same equipment on the same day in the same
laboratory.
13.1.1.1 Repeatability limits are listed in Table 2.
13.1.2 Bias—At the time of the study, the test specimens
chosen for analysis were not accepted reference materials
suitable for determining the bias for this test method, therefore
no statement on bias is being made.
6
Supporting data have been ﬁled at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D16-1062. Contact ASTM Customer
Service at www.astm.org/contact.
TABLE 2 Repeatability Limits (mg/kg)
Cobalt
mg/kg
Manganese
mg/kg
Iron
mg/kg
Chromium
mg/kg
Nickel
mg/kg
Sodium
mg/kg
AVERAGE 0.0346 0.5766 0.3306 0.1767 1.5794 0.2020
SD 0.0097 0.0125 0.0023 0.0015 0.0112 0.0069
r 0.0270 0.0351 0.0064 0.0042 0.0313 0.0193
Titanium
mg/kg
Molybdenum
mg/kg
Mangesium
mg/kg
Potassium
mg/kg
Calcium
mg/kg
Aluminum
mg/kg
AVERAGE 0.6037 0.4965 0.0406 0.1008 0.0509 0.0309
SD 0.0034 0.0119 0.0015 0.0039 0.0039 0.0026
r 0.0095 0.0334 0.0043 0.0110 0.0110 0.0073
D8130 − 17 (2024)
3

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标签： #电感耦合 #等离子体 #原子发射光谱法

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ASTM D8130-17 2024 Standard Test Method for Determination of Metals in Purified Terephthalic Acid (PTA) by Inductively Coupled Plasma Atomic Emission Spectrometric Method 用电感耦合等离子体原子发射光谱法测定精对苯二甲酸（PTA）中金属的标准试验方法

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ASTM D8130-17 (2024) 用电感耦合等离子体原子发射光谱法测定精对苯二甲酸（PTA）中金属的标准试验方法

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