ASTM D5185-09

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 Wavelengths^A

Element	Wavelength, 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

Element	Range, mg/kg	Repeatability, μg/gA
Aluminum	6–40	0.71 X0.41
Barium	0.5–4	0.24 X0.66
Boron	4–30	0.26 X
Calcium	40–9000	0.0020 X1.4
Chromium	1–40	0.17 X0.75
Copper	2–160	0.12 X0.91
Iron	2–140	0.13 X0.80
Lead	10–160	1.6 X0.32
Magnesium	5–1700	0.16 X0.86
Manganese	5–700	0.010 X1.3
Molybdenum	5–200	0.29 X0.70
Nickel	5–40	0.52 X0.49
Phosphorus	10–1000	1.3 X0.58
Potassium	40–1200	3.8 X0.33
Silicon	8–50	1.3 X0.26
Silver	0.5–50	0.15 X0.83
Sodium	7–70	0.49 X0.66
Sulfur	900–6000	0.49 X0.81
Tin	10–40	2.4 X0.17
Titanium	5–40	0.54 X0.37
Vanadium	1–50	0.061 X
Zinc	60–1600	0.15 X0.88

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

TABLE 3 Reproducibility

Element	Range, mg/kg	Reproducibility, μg/gA
Aluminum	6–40	3.8 X0.26
Barium	0.5–4	0.59 X0.92
Boron	4–30	13 X0.01
Calcium	40–9000	0.015 X1.3
Chromium	1–40	0.81 X0.61
Copper	2–160	0.24 X
Iron	2–140	0.52 X0.80
Lead	10–160	3.0 X0.36
Magnesium	5–1700	0.72 X0.77
Manganese	5–700	0.13 X1.2
Molybdenum	5–200	0.64 X0.71
Nickel	5–40	1.5 X0.50
Phosphorus	10–1000	4.3 X0.50
Potassium	40–1200	6.6 X0.29
Silicon	8–50	2.9 X0.39
Silver	0.5–50†	0.35 X
Sodium	7–70	1.1 X0.71
Sulfur	900–6000	1.2 X0.75
Tin	10–40	2.1 X0.62
Titanium	5–40	2.5 X0.47
Vanadium	1–50	0.28 X1.1
Zinc	60–1600	0.083 X1.1

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

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