ASTM D6130-24 用电感耦合等离子－原子发射分光仪测定发动机冷却液中硅及其它元素的标准试验方法

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Designation: D6130 −24
Standard Test Method for
Determination of Silicon and Other Elements in Engine
Coolant by Inductively Coupled Plasma-Atomic Emission
Spectroscopy
1
This standard is issued under the ﬁxed designation D6130; 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 silicon in
engine coolant by inductively coupled plasma-atomic emission
spectroscopy (ICP-AES). Silicon can be determined as low as
the range of 5 ppm by this test method. Other elements also
found in engine coolant can be determined by this method.
This test method is applicable to the determination of dissolved
or dispersed elements.
1.2 This test method is applicable to both new and used
engine coolant.
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
D1176 Practice for Sampling and Preparing Aqueous Solu-
tions of Engine Coolants or Antirusts for Testing Purposes
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 U.S. EPA Standards:
3
Method 6010, Inductively Coupled Plasma Method, SW-
846, Test Methods for Evaluating Solid Waste
Method 200.7, Inductively Coupled Plasma - Atomic Emis-
sion Spectrometric Method for Trace Element Analysis of
Water And Wastes, EPA-600/4-79-020, revised 1984
3. Summary of Test Method
3.1 Elements in solution are determined, either sequentially
or simultaneously, by ICP-AES. New or used engine coolants
are prepared by dilution. Samples and standards are introduced
to the nebulizer using a peristaltic pump and the aerosol is
injected into an argon-supported inductively coupled plasma.
The high temperature of the plasma atomizes the sample and
produces atomic emission intensities at wavelengths associated
with the desired elements. Emission intensity is proportional to
concentration. Elemental determinations are made by compar-
ing standard and sample emission intensities.
4. Signiﬁcance and Use
4.1 Some engine coolants are formulated with silicon con-
taining additives. This test method provides a means of
determining the concentration of dissolved or dispersed ele-
ments which give an indication of this additive content in the
engine coolant.
5. Interferences
5.1 Interferences may be categorized as follows:
5.1.1 Spectral—Light emission from spectral sources other
than the element of interest may contribute to apparent net
signal intensity. Sources of spectral interference include direct
spectral line overlaps, broadened wings of intense spectral
lines, ion-atom recombination continuum emission, molecular
band emission and stray (scattered) light from the emission of
1
This test method is under the jurisdiction of ASTM Committee D15 on Engine
Coolants and Related Fluids and is the direct responsibility of Subcommittee
D15.04 on Chemical Properties.
Current edition approved June 1, 2024. Published June 2024. Originally
approved in 1997. Last previous edition approved in 2018 as D6130 – 11 (2018).
DOI: 10.1520/D6130-24.
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 U.S. Environmental Protection Agency, Environmental Moni-
toring and Support Laboratory, Cincinnati, OH 45268.
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

elements at high concentrations. Avoid overlaps by selecting

alternate analytical wavelengths.

5.1.2 Physical—Physical interferences are effects associated

with sample nebulization and transport processes such as

viscosity and particulate contamination.

5.1.3 Background—High background effects from scattered

light, etc., can be compensated for by background correction

adjacent to the analyte line.

5.1.4 Chemical—Chemical interferences are caused by mo-

lecular compound formation, ionization effects, and thermo-

chemical effects associated with sample vaporization and

atomization in the plasma. Normally these effects are not

pronounced and can be minimized by careful selection of

operating conditions (incident power, plasma observation

position, etc.).

6. Apparatus

6.1 Spectrometer—An inductively coupled plasma emission

spectrometer of the simultaneous or sequential type including

RF generator, torch, nebulizer, spray chamber, recommended

peristaltic pump and host computer.

7. Reagents and Materials

7.1 Purity of Chemicals—Reagent grade or better chemicals

shall be used for preparation of all standards and samples.

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 accuracy of the determination.

7.2 Purity of Water—References to water shall be under-

stood to mean deionized water.

7.3 Standard Stock Solutions—Certiﬁed solutions may be

purchased or prepared from high purity grade chemicals or

metals (See Method 6010, SW-846, Method 200.7). Standards

contain 1000 mg/L of the element of interest. Salts should be

dried as indicated.

7.4 Calibration Standards—Prepare the standards in volu-

metric ﬂasks using appropriate volumes of each stock solution

to cover the expected concentration range of the samples.

Elements in multielement standards should be shown to be

compatible and stable. Compensate for differences in standard/

sample matrix by using an appropriate amount of ethylene

glycol or an internal standard, or both. Suggested combinations

and analytical lines are in Table 1. Validate calibration stan-

dards. Monitor stability.

8. Sampling

8.1 Collect sample in accordance with Practice D1176.

9. Calibration and Standardization

9.1 Set the up instrument according to the manufacturer’s

instructions. Warm it up at least 20 min.

9.2 Proﬁle and calibrate the instrument according to manu-

facturer’s recommended procedures with the blank and

standards, aspirating the standard for at least 30 s to allow the

instrument to equilibrate prior to signal integration. Water

should be run for an additional 60 s after standards containing

boron. Calibration should be validated and stability of stan-

dards should be monitored.

10. Sample Preparation

10.1 Dilute the sample with deionized water so the concen-

tration of the element(s) of interest is in the linear detection

range of the instrument. Generally a

⁄

dilution for

prediluted engine coolant and a

⁄

100

dilution for engine coolant

concentrate are sufficient. Samples may be prepared by weight

to volume or by volume to volume. Be certain when preparing

dilutions by volume that the entire sample aliquot is trans-

ferred. Filter or centrifuge samples that contain particulate.

11. Procedure

11.1 Aspirate the prepared samples into the calibrated

instrument using the same conditions established for the

calibration procedure. Rinse sufficiently to prevent carryover.

Run water an additional 60 s between samples containing

boron.

11.2 Run a blank and an instrument check standard (a

calibration standard, calibration veriﬁcation or standard engine

coolant) every ten samples or as established to be necessary for

the instrument. Analyze a blank and check standard at the end

of each run. The concentration shall be within 65 % of the

expected value. If the concentration is out of range, correct the

problem, recalibrate the instrument and rerun the samples in

question.

11.3 Matrix spikes and duplicates may be performed as

quality control procedures if sample concentrations are suspect

due to contamination, spectral interferences or trace levels of

the element of interest.

11.4 Perform the corrections and calculations, including

dilution factors, using the instrument host computer.

12. Report

12.1 Samples prepared by weight to volume dilution may be

reported in ppm by weight or % by weight depending on the

concentration of the element of interest. Samples prepared by

volume may be reported as g/L, mg/L, µg/mL, etc. These units

may be converted to ppm weight or % by weight using the

density of the sample:

TABLE 1 Analytical Wavelengths for ICP-AES Determination of

Elements in Engine Coolant

Element Wavelength, nm

Mixed Standard 1

Silicon 251.612, 288.158, 252.851, 252.411

Molybdenum 202.030, 204.598

Boron 249.773

Phosphorus 214.914, 178.29

Mixed Standard 2

Aluminum 308.215, 394.401, 369.152

Lead 220.353

Zinc 213.856

Iron 259.94, 259.837, 238.204

Copper 324.754, 219.226

Magnesium 279.079, 280.270, 279.553

Calcium 317.933, 393.37, 396.847, 315.887

Sodium 588.995, 589.592

Potassium 766.491

D6130 − 24

concentration

ppm by wt

5concentration

µg/mL

density

g/mL

(1)

13. Precision and Bias

13.1 The precision of this test method is based on an

interlaboratory study conducted in 2009. A total of nine

laboratories participated in this study, testing samples of six

different coolants for their metals content. Every test result

represents an individual determination, and all participants

were asked to report four replicate test results for each

metal/coolant combination. Practice E691 was followed for the

design and analysis of the data; the details are given in

RR:D15-1030.

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 rvalue for that material; ris 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 Tables 2-12.

13.1.2 Reproducibility limit, R—Two test results shall be

judged not equivalent if they differ by more than the Rvalue

for that material; Ris the interval representing the critical

difference between two test results for the same material,

obtained by different operators using different equipment in

different laboratories.

13.1.2.1 Reproducibility limits are listed in Tables 2-12.

13.1.3 The above terms (repeatability limit and reproduc-

ibility limit) are used as speciﬁed in Practice E177.

13.1.4 Any judgment in accordance with statements 13.1.1

and 13.1.2 would have an approximate 95 % probability of

being correct.

13.2 Bias—At the time of the study, there was no accepted

reference material suitable for determining the bias for this test

method, therefore no statement on bias is being made.

13.3 The precision statement was determined through sta-

tistical examination of 864 test results, submitted by six

laboratories, on twelve metals, in six coolants.

13.3.1 The six coolant types were described as follows:

Coolant A

Coolant B

Coolant C

Coolant D

Coolant E

Coolant F

13.4 To judge the equivalency of two test results, it is

recommended to choose the coolant material that is closest in

characteristics to the test material.

14. Keywords

14.1 engine coolant; inductively coupled plasma-atomic

emission spectroscopy; silicon

Supporting data have been ﬁled at ASTM International Headquarters and may

be obtained by requesting RR:D15-1030.

TABLE 2 Boron (µg/mL)

Material Average

χ¯

Repeatability

Standard

Deviation, S

Reproducibility

Standard

Deviation, S

Repeatability

Limit, r

Reproducibility

Limit, R

Sample A 222.12 3.60 18.74 10.08 52.46

Sample B 436.66 4.60 30.75 12.88 86.11

Sample C 440.44 7.52 33.22 21.04 93.01

Sample D 872.63 2.73 55.30 7.64 154.84

Sample E 315.75 5.06 23.76 14.17 66.53

Sample F 205.20 6.76 14.19 18.93 39.72

The average of the laboratories’ calculated averages.

D6130 − 24

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标签： #电感耦合等离子 #原子发射分光仪 #发动机冷却液

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ASTM D6130-2024 Standard Test Method for Determination of Silicon and Other Elements in Engine Coolant by Inductively Coupled Plasma-Atomic Emission Spectroscopy 用电感耦合等离子－原子发射分光仪测定发动机冷却液中硅及其它元素的标准试验方法

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ASTM D6130-24 用电感耦合等离子－原子发射分光仪测定发动机冷却液中硅及其它元素的标准试验方法

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