ASTM D5185-09 - 15.4.2009
 
Significance and Use

This test method covers the rapid determination of 22 elements in used lubricating oils and in base oils, and it provides rapid screening of used oils for indications of wear. Test times approximate a few minutes per test specimen, and detectability for most elements is in the low mg/kg range. In addition, this test method covers a wide variety of metals in virgin and re-refined base oils. Twenty-two elements can be determined rapidly, with test times approximating several minutes per test specimen.

When the predominant source of additive elements in used lubricating oils is the additive package, significant differences between the concentrations of the additive elements and their respective specifications can indicate that the incorrect oil is being used. The concentrations of wear metals can be indicative of abnormal wear if there are baseline concentration data for comparison. A marked increase in boron, sodium, or potassium levels can be indicative of contamination as a result of coolant leakage in the equipment. This test method can be used to monitor equipment condition and define when corrective actions are needed.

The concentrations of metals in re-refined base oils can be indicative of the efficiency of the re-refining process. This test method can be used to determine if the base oil meets specifications with respect to metal content.

 
1. Scope

1.1 This test method covers the determination of additive elements, wear metals, and contaminants in used lubricating oils by inductively coupled plasma atomic emission spectrometry (ICP-AES). The specific elements are listed in Table 1.

1.2 This test method covers the determination of selected elements, listed in Table 1, in re-refined and virgin base oils.

1.3 For analysis of any element using wavelengths below 190 nm, a vacuum or inert-gas optical path is required. The determination of sodium and potassium is not possible on some instruments having a limited spectral range.

1.4 This test method uses oil-soluble metals for calibration and does not purport to quantitatively determine insoluble particulates. Analytical results are particle size dependent, and low results are obtained for particles larger than a few micrometers.

1.5 Elements present at concentrations above the upper limit of the calibration curves can be determined with additional, appropriate dilutions and with no degradation of precision.

1.6 For elements other than calcium, sulfur, and zinc, the low limits listed in Table 2 and Table 3 were estimated to be ten times the repeatability standard deviation. For calcium, sulfur, and zinc, the low limits represent the lowest concentrations tested in the interlaboratory study.

1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

1.8 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 6.1, 8.2, and 8.4.

TABLE 1 Elements Determined and Suggested WavelengthsA

ElementWavelength, nm

Aluminum

308.22, 396.15, 309.27

Barium

233.53, 455.40, 493.41

Boron

249.77

Calcium

315.89, 317.93, 364.44, 422.67

Chromium

205.55, 267.72

Copper

324.75

Iron

259.94, 238.20

Lead

220.35

Magnesium

279.08, 279.55, 285.21

Manganese

257.61, 293.31, 293.93

Molybdenum

202.03, 281.62

Nickel

231.60, 227.02, 221.65

Phosphorus

177.51, 178.29, 213.62, 214.91, 253.40

Potassium

766.49

Sodium

589.59

Silicon

288.16, 251.61

Silver

328.07

Sulfur

180.73, 182.04, 182.62

Tin

189.99, 242.95

Titanium

337.28, 350.50, 334.94

Vanadium

292.40, 309.31, 310.23, 311.07

Zinc

202.55, 206.20, 213.86, 334.58, 481.05

A These wavelengths are only suggested and do not represent all possible choices.

TABLE 2 Repeatability

ElementRange, mg/kgRepeatability, μg/gA

Aluminum

640

0.71 X0.41

Barium

0.54

0.24 X0.66

Boron

430

0.26 X

Calcium

409000

0.0020 X1.4

Chromium

140

0.17 X0.75

Copper

2160

0.12 X0.91

Iron

2140

0.13 X0.80

Lead

10160

1.6 X0.32

Magnesium

51700

0.16 X0.86

Manganese

5700

0.010 X1.3

Molybdenum

5200

0.29 X0.70

Nickel

540

0.52 X0.49

Phosphorus

101000

1.3 X0.58

Potassium

401200

3.8 X0.33

Silicon

850

1.3 X0.26

Silver

0.550

0.15 X0.83

Sodium

770

0.49 X0.66

Sulfur

9006000

0.49 X0.81

Tin

1040

2.4 X0.17

Titanium

540

0.54 X0.37

Vanadium

150

0.061 X

Zinc

601600

0.15 X0.88

A where: X = mean concentration, μg/g.

TABLE 3 Reproducibility

ElementRange, mg/kgReproducibility, μg/gA

Aluminum

640

3.8 X0.26

Barium

0.54

0.59 X0.92

Boron

430

13 X0.01

Calcium

409000

0.015 X1.3

Chromium

140

0.81 X0.61

Copper

2160

0.24 X

Iron

2140

0.52 X0.80

Lead

10160

3.0 X0.36

Magnesium

51700

0.72 X0.77

Manganese

5700

0.13 X1.2

Molybdenum

5200

0.64 X0.71

Nickel

540

1.5 X0.50

Phosphorus

101000

4.3 X0.50

Potassium

401200

6.6 X0.29

Silicon

850

2.9 X0.39

Silver

0.550

0.35 X

Sodium

770

1.1 X0.71

Sulfur

9006000

1.2 X0.75

Tin

1040

2.1 X0.62

Titanium

540

2.5 X0.47

Vanadium

150

0.28 X1.1

Zinc

601600

0.083 X1.1

A where: X = mean concentration, μg/g.

 
2. Referenced Documents

C1109-23

Standard Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic Emission Spectroscopy

D1552-23

Standard Test Method for Sulfur in Petroleum Products by High Temperature Combustion and Infrared (IR) Detection or Thermal Conductivity Detection (TCD)

E135-26a

Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials (Includes all amendments and changes 8/6/2026).

D7260-25

Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants

D4951-14(2019)

Standard Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry

D4927-26

Standard Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy

D4628-23

Standard Test Method for Analysis of Barium, Calcium, Magnesium, and Zinc in Unused Lubricating Oils by Atomic Absorption Spectrometry

D4057-22

Standard Practice for Manual Sampling of Petroleum and Petroleum Products

D4307-17(2021)

Standard Practice for Preparation of Liquid Blends for Use as Analytical Standards