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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

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 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

Element Range, mg/kg Reproducibility, 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.

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04/15/2009
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