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1.1 This test method covers the determination of a number of metals such as aluminum, antimony, barium, calcium, iron, lithium, magnesium, molybdenum, phosphorus, silicon, sodium, sulfur, and zinc in unused lubricating greases by inductively coupled plasma atomic emission spectrometry (ICP-AES) technique.

1.1.1 The range of applicability for this test method, based on the interlaboratory study conducted in 2005, is aluminum (10600), antimony (102300), barium (50800), calcium (2050 000), iron (10360), lithium (3003200), magnesium (3010 000), molybdenum (5022 000), phosphorus (502000), silicon (1015 000), sodium (301500), sulfur (160028 000), and zinc (3002200), all in mg/kg. Lower levels of elements may be determined by using larger sample weights, and higher levels of elements may be determined by using smaller amounts of sample or by using a larger dilution factor after sample dissolution. However, the test precision in such cases has not been determined, and may be different than the ones given in Table 1.

1.1.2 It may also be possible to determine additional metals such as bismuth, boron, cadmium, chromium, copper, lead, manganese, potassium, titanium, etc. by this technique. However, not enough data is available to specify the precision for these latter determinations. These metals may originate into greases through contamination or as additive elements.

1.1.3 During sample preparation, the grease samples are decomposed with a variety of acid mixture(s). It is beyond the scope of this test method to specify appropriate acid mixtures for all possible combination of metals present in the sample. But if the ash dissolution results in any visible insoluble material, the test method may not be applicable for the type of grease being analyzed, assuming the insoluble material contains some of the analytes of interest.

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

1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.

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 appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in Sections 8 and 10.

TABLE 1 Precision of Grease Analysis

Note – X is the mean concentration in mg/kg.

Element Range,
mg/kg
Repeatability Reproducibility
Aluminum 10600 0.2163 X0.9 6.8156 X0.9
Antimony 102300 0.3051 X0.8191 4.6809 X0.8191
Barium 50800 0.3165 X0.7528 2.9503 X0.7528
Calcium 2050 000 2.2853 X0.7067 3.0571 X0.7067
Iron 10360 0.8808 X0.7475 2.5737 X0.7475
Lithium 3003200 0.0720 X1.0352 0.1476 X1.0352
Magnesium 3010 000 0.6620 X0.6813 2.6155 X0.6813
Molybdenum 5022 000 0.1731 X0.9474 0.4717 X0.9474
Phosphorus 502000 1.2465 X0.6740 4.0758 X0.6740
Silicon 1015 000 1.3859 X0.9935 4.8099 X0.9935
Sodium 301500 6.5760 X0.5 11.571 X0.5
Sulfur 160028 000 1.0507 X0.8588 1.5743 X0.8588
Zinc 3002200 0.1904 X0.8607 0.5912 X0.8607

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