GB/T 17476-1998 Standard test method for determination of additive elements, wear metals and contaminants in used lubricating oils and of certain elements in base oils (inductively coupled plasma atomic emission spectrometry)

Summary page. This page is a compiled excerpt/summary of the standard — it is not the full standard text and does not replace it. Verify every value against the official standard and the product certificate before use.

Evidence note: this page is an unofficial method study card for the historical 1998 edition, not the full text of the standard or an operating procedure; the edition has been withdrawn and technical review is pending. The original held lacks its cover, the original technical doubts are retained, and the controlled standard and product certificate should be checked before use.

1. Edition and reading boundaries: Original PDF pages 1-3; two official status records (checked 2026-10-05). This card covers only the method for elemental analysis of used lubricating oils in GB/T 17476-1998. The historical issue date is 1998-08-20 and the implementation date 1999-01-01. The official standards public system marks it as withdrawn; the National Standards Information Public Service Platform records a withdrawal date of 2023-09-01 and full replacement by GB/T 17476-2023. Only the version relationship is stated here; the technical conditions of the 2023 edition are not imported. An older web page routed the 1998 entry as the 2023 edition studied and used the 2023 title; the present round completes the study content from the 1998 original. The 11 pages held begin with the foreword and lack the cover; page 3 of the PDF is the 1998 body title, continuing to clause 16.3. The index field "complete" must not be taken to mean the file has been checked page by page against the official controlled copy.

2. Scope and limits of the results: PDF page 3, clause 1. This edition uses ICP-AES to measure additive elements, wear metals and contaminants in used lubricating oils and certain elements in base oils. The 22 elements are Al, Ba, B, Ca, Cr, Cu, Fe, Pb, Mg, Mn, Mo, Ni, P, K, Na, Si, Ag, S, Sn, Ti, V and Zn. The method addresses oil-soluble metals and cannot serve as a quantitative method for insoluble particulate matter. Particles larger than a few micrometres may give low results; a low metal result does not mean there is no particulate wear. High concentrations may be diluted further, but the measured value must lie within the linear range of the working curve. Sulphur measurement requires a vacuum or inert-gas purged optical path; some instruments are limited by wavelength range and cannot be assumed to measure sodium or potassium. Most lower limits in Tables 2 and 4 are estimated as 10 times the standard deviation of repeatability, while the calcium, sulphur and zinc limits are the actual lowest concentrations of the cooperative study and must not be treated directly as detection limits for any instrument.

3. Principle and premises for interpretation: PDF page 4, clauses 3-5. A homogeneous oil sample is diluted by mass with mixed xylene or another suitable solvent, and the standard solutions are treated in the same way; the solution is nebulized into the ICP, the emission intensity is compared with the calibration curve, and the element concentration in the original oil sample is obtained by means of the dilution factor. An internal standard may optionally be used to reduce differences in transport effects. Changes in additives, wear metals or coolant contamination must be interpreted together with the initial concentration of the oil, the equipment history and the product specification. This card gives no fault-diagnosis thresholds, oil-change or acceptance conclusions.

4. Apparatus and consumables conditions: PDF page 6, clause 7 and Table 1. An ICP-AES with a quartz torch and an RF excitation source is required; both sequential scanning and simultaneous measurement are described in the original. Sulphur measurement requires measurement capability near 180 nm. A Babington-type high-salt nebulizer and a peristaltic pump are the configuration recommended in this edition, which does not confirm the suitability of any specific product. The pump delivery rate range is 0.5 to 3 mL/min; the sample tubing must retain its performance in the organic solvent used for at least 6 h. The original lists Viton tubing for hydrocarbon solvents and PVC tubing for MIBK, but the actual material compatibility still requires verification. Containers are 30 to 120 mL screw-cap plastic bottles; a bath-type or probe-type ultrasonic bath or a vortex mixer may be used for homogenization, and the balance readability is 0.001 g. The table below has been checked line by line against original Table 1; units are nm. These are recommended wavelengths only, not an exhaustive selection or fixed measurement parameters. | Element | Recommended wavelength (nm) | | --- | --- | | Al | 308.22, 396.15, 309.27 | | Ba | 233.53, 455.40, 493.41 | | B | 249.77 | | Ca | 315.89, 317.93, 364.44, 422.67 | | Cr | 205.55, 267.72 | | Cu | 324.75 | | Fe | 259.94, 238.20 | | Pb | 220.35 | | Mg | 279.08, 279.55, 285.21 | | Mn | 257.61, 293.31, 293.93 | | Mo | 202.03, 281.62 | | Ni | 231.60, 277.02, 221.65 | | P | 177.51, 178.29, 213.62, 214.91, 253.40 | | K | 766.49 | | Na | 589.59 | | Si | 288.16, 251.61 | | Ag | 328.07 | | S | 180.73, 182.04, 182.62 | | Sn | 189.99, 242.95 | | Ti | 337.28, 350.50, 334.94 | | V | 292.40, 309.31, 310.23, 311.07 | | Zn | 202.55, 206.20, 313.86, 334.58, 481.05 |

5. Reagents, standards and internal standard: PDF pages 6-7, clauses 8-9. The original uses analytical-grade reagents; other grades must be shown not to affect accuracy. The base oil/light white oil should contain none of the elements to be determined, and viscosity matching should be considered; the standard diluent for sulphur analysis uses sulphur-free white oil. The multi-element organometallic standard is listed in the original at 0.0500% (m/m) per element, and the mixture must be homogeneous. Sulphur requires a separate standard; the original lists NIST SRM 1622C or dibenzyl disulphide of 99.99% (m/m) purity, together with the dependence on sulphur analysis according to SH/T 0172. The potassium standard is listed at 0.0500% (m/m). These are records of a historical method and do not indicate confirmation of current product models, certificates or supply. The diluents listed in the original are mixed xylene, o-xylene, kerosene, petroleum spirit, tetralin, decalin or MIBK, provided they contain none of the analytes and are suitable for the instrument. The list must not be read as unconditional interchangeability. Oil-soluble calcium, cobalt or yttrium, among others, may be considered as internal standards, but the sample as received must not already contain that element. The original preparation example is 20 g of a 0.500% (m/m) organometallic material made up to volume in a 1 L volumetric flask with solvent, prepared fresh at least weekly; the 100 µg/mL stated on the original page is not mandatory, but at least 100 times the detection limit of the internal standard must be reached. The internal standard concentration must be the same in samples and working standards.

6. Sampling and homogenization: PDF page 7, clause 10. Sampling refers to GB/T 4756. The full text of the referenced standard is not reproduced here. Used oil must be thoroughly homogenized before weighing; for viscous samples the original specifies heating to 60 °C, then homogenizing, sampling and weighing. Particle settling, the homogenization method, the representativeness of the sample and the suitability of the heat treatment must be implemented in a controlled laboratory procedure; this study card alone is not sufficient to arrange the operation.

7. Preparation of blanks and working standards: PDF pages 7-8, clause 11. The blank is diluted by mass with base oil or white oil. Absolute concentration example: 2 g of 0.0500% (m/m) multi-element standard, 8 g base oil and 90 g solvent; the original working-standard heading says 10 µg/mL, while the preparation is by mass and the density/unit conversion is not set out, so this card does not silently convert it into an equivalent figure. Relative concentration example: 2 g of 100 µg/g multi-element standard oil, 18 g base oil and 200 g solvent, stated as oil:solvent = 1:10 (m/m). The concentration series of the standards should cover the samples and lie within the linear range; the sulphur series uses sulphur-free white oil. Two portions of homogenized oil are weighed independently for each sample; clauses 11.4/11.5 specify oil:solvent = 1:10 (m/m), shaken and sealed. Clause 11.6, the internal standard route, in turn requires a concentration of 10% (m/m) for the diluted working standard/sample; a 1:10 oil/solvent ratio and a final 10% are not the same statement, and the difference in the original wording is retained [to be verified] rather than silently recalculated in place of the original.

8. Interference correction and symbols: PDF page 5, clause 6, equations (1) to (8). For spectral interference, a suitable wavelength and on-peak or off-peak background correction are considered first; where necessary the interference coefficient is determined with high-purity single-element solutions. The coefficients must be established under conditions matching the sample and are not guaranteed to be reusable from day to day; coefficients derived from off-peak background may be negative. Rearranged from the original equations: cₐ = Iₐ/Hₐ; cᵢ = Iᵢ/Hᵢ; Kᵢₐ = Hᵢ/Hₐ = Iᵢ/(cᵢ·Hₐ). Iₐ is the background-corrected net intensity of the analytical line, Hₐ the sensitivity, and Iᵢ the contribution of the interfering line to the analytical line. Approximate concentration = (Iₐ+Iᵢ)/Hₐ = cₐ + Iᵢ/Hₐ; corrected concentration cₐ = cₐ(approximate) − Kᵢₐ·cᵢ. For multiple interferences, K₁ₐ·c₁, K₂ₐ·c₂ and so on are subtracted term by term as in original equation (8). This is only a restatement of the original formulae; the specific signal definitions and the software calculation still require the original manual and independent review. Differences in viscosity change the transport rate; a pump, an internal standard, or both, can reduce the effect, and in severe cases the original specifies increasing the dilution from 10-fold to 20-fold while keeping the internal standard concentration constant. Blockage by particles gives low results, and spectral correction cannot replace particle handling.

9. Instrument preparation and parameter boundaries: PDF page 8, clause 12. This edition makes clear that there are no unified fixed operating conditions for different instruments, solvents and wavelengths, and that organic-sample conditions should be established from the instrument manual. Check the nebulizer mounting, leak-tightness, waste drainage and liquid seal; inspect the pump tubing before every start, replacing it where necessary and checking the uptake rate. The original requires the plasma to be ignited and warmed up for at least 30 min before analysis, and the diluent sprayed afterwards to check for carbon build-up; adjustments of power and gas flow for organic compared with aqueous samples depend on the instrument, and specific RF power or flow rates are not guessed from this card. Profile scanning follows the manual; parameters include element, wavelength, background correction, interference coefficients, integration and internal standard. Integration is generally 5 to 10 s, 4 to 10 times, as described in this edition and not as a mandatory configuration for all models.

10. Calibration and quality control: PDF pages 8-9, clauses 13 and 14.2. The linear range of each element is established with the blank and the standard series. The blank and working standard are checked at the start of each analysis group; sample analysis proceeds only if the target concentration error is within 5%, otherwise recalibration is required. A standard is checked again after every 5 samples, and a deviation beyond 5% requires calibration and re-running of the samples. Internal standard equation (9): I(Re) = [I(e) − I(Be)]/I(is), being the element intensity, the element blank intensity and the internal standard intensity respectively. The correction factor is established from the intensity ratio; the software definition and calculation of the internal standard must not be assumed to agree on the basis of an interface label.

11. Measurement and reporting: PDF page 9, clauses 14-15. Samples and check standards must have the same integration time, background correction and plasma conditions. The diluting solvent is sprayed for 60 s before each injection, and the concentration in the original sample is calculated using the actual dilution factor; the internal standard route gives the concentration from the intensity ratio. Ca, Mg, Zn, Ba, P and S are reported to three significant figures; the other elements, Al, B, Cr, Cu, Fe, Pb, Mn, Mo, Ni, K, Na, Si, Ag, Sn, Ti and V, to two significant figures. The original result unit is µg/g; the OCR reading "8/g" must not be copied, nor may the reporting clause be imported directly from the 2023 edition as mg/kg.

12. Expression and range of precision: PDF pages 9-10, Tables 2 and 4, clauses 16.1-16.2. The original gives interlaboratory statistical results at the 95% confidence level, covering xylene/kerosene and the nebulizer, pump and background-correction configurations of some laboratories. r compares repeat determinations of the same sample on the same instrument; R compares independent results from different laboratories. X is the mean concentration in µg/g; ^ in the table below denotes a power, and the coefficients and exponents are confirmed separately from the scanned page. The lower concentration limits for r and R differ for silver and are retained as 0.5 and 5, not covered by a single value. Precision is not a sample acceptance limit, nor is it the measurement uncertainty of any instrument. | Element | Concentration range (µg/g) | r (µg/g) | R (µg/g) | | --- | --- | --- | --- | | Al | 6-40 | 0.71X^0.41 | 3.8X^0.26 | | Ba | 0.5-4 | 0.24X^0.66 | 0.59X^0.92 | | B | 4-30 | 0.26X | 13X^0.01 | | Ca | 40-9000 | 0.0020X^1.4 | 0.015X^1.3 | | Cr | 1-40 | 0.17X^0.75 | 0.81X^0.61 | | Cu | 2-160 | 0.12X^0.91 | 0.24X | | Fe | 2-140 | 0.13X^0.80 | 0.52X^0.80 | | Pb | 10-160 | 1.6X^0.32 | 3.0X^0.36 | | Mg | 5-1700 | 0.16X^0.86 | 0.72X^0.77 | | Mn | 5-700 | 0.010X^1.3 | 0.13X^1.2 | | Mo | 5-200 | 0.29X^0.70 | 0.64X^0.71 | | Ni | 5-40 | 0.52X^0.49 | 1.5X^0.50 | | P | 10-1000 | 1.3X^0.58 | 4.3X^0.50 | | K | 40-1200 | 3.8X^0.33 | 6.6X^0.29 | | Si | 8-50 | 1.3X^0.26 | 2.9X^0.39 | | Ag | 0.5-50 (r); 5-50 (R) | 0.15X^0.83 | 0.35X | | Na | 7-70 | 0.49X^0.66 | 1.1X^0.71 | | S | 900-6000 | 0.49X^0.81 | 1.2X^0.75 | | Sn | 10-40 | 2.4X^0.17 | 2.1X^0.62 | | Ti | 5-40 | 0.54X^0.37 | 2.5X^0.47 | | V | 1-50 | 0.061X | 0.28X^1.1 | | Zn | 60-1600 | 0.15X^0.88 | 0.083X^1.1 |

13. Selected-concentration examples from the original tables and bias: PDF pages 10-11, Tables 3 and 5, clause 16.3. Below, at concentrations of 1/10/100/1000 µg/g, original Tables 3 and 5 are set out as four values for r and four for R respectively; a dash means the original table gives no value, not zero. The example values in the original tables have not been recalculated from the equations to overwrite them. The original tables contain examples where the values and the ranges are inconsistent; for example Ba gives R = 0.6 at concentration 1, and Ag gives R = 0.4 at concentration 1 although the range in Table 4 starts at 5. These facts of the original are retained and must not be used to widen the applicability of the precision; they require review against the controlled standard and by technical staff. The bias discussion concerns diluted oil-soluble metals and excludes insoluble particles. The statement in clause 16.3 that for certain elements the difference between the expected value and the mean does not exceed the repeatability is subject to premises such as the absence of significant interference, and must not be generalized into an accuracy guarantee for all elements. | Element | r at 1 | r at 10 | r at 100 | r at 1000 | R at 1 | R at 10 | R at 100 | R at 1000 | | --- | --- | --- | --- | --- | --- | --- | --- | --- | | Al | — | 1.8 | — | — | — | 6.8 | — | — | | Ba | — | — | — | — | 0.6 | — | — | — | | B | — | 2.6 | — | — | — | 1.3 | — | — | | Ca | — | — | 1 | 32 | — | — | 6 | 120 | | Cr | 0.2 | 1.0 | — | — | 0.8 | 3.3 | — | — | | Cu | — | 1.0 | 8 | — | — | 2.4 | 24 | — | | Fe | — | 0.8 | 5 | — | — | 3.3 | 21 | — | | Pb | — | 3.3 | 7 | — | — | 6.9 | 16 | — | | Mg | — | 1.2 | 8 | 61 | — | 4.2 | 25 | 150 | | Mn | — | 0.2 | 4 | — | — | 2.1 | 33 | — | | Mo | — | 1.5 | 7 | — | — | 3.3 | 17 | — | | Ni | — | 1.6 | — | — | — | 4.7 | — | — | | P | — | 4.9 | 19 | 71 | — | 14 | 43 | 140 | | K | — | — | 17 | 37 | — | — | 25 | 49 | | Si | — | 2.4 | — | — | — | 7.1 | — | — | | Ag | 0.2 | 1.0 | — | — | 0.4 | 3.5 | — | — | | Na | — | 2.2 | — | — | — | 5.6 | — | — | | S | — | — | — | 130 | — | — | — | 210 | | Sn | — | 3.5 | — | — | — | 8.8 | — | — | | Ti | — | 1.3 | — | — | — | 7.4 | — | — | | V | 0.1 | 0.6 | — | — | 0.3 | 3.5 | — | — | | Zn | — | — | 8 | 65 | — | — | 13 | 170 |

14. Reference dependencies, missing items and questions: Verification record for original PDF pages 1-11. The reference dependencies include GB/T 4756 for sampling and SH/T 0172 for sulphur determination; the versions of the referenced documents and their procedures were not re-verified in this round. The foreword lists the historical adoption relationship with ASTM D5185-95, which does not mean that other versions are currently equivalent. The 11 pages held, equations (1) to (9), Tables 1 to 5 and the reporting units have been checked visually page by page; the cover is missing, the file has not been collated page by page against the official controlled copy, and independent technical review is pending. The differences in dilution ratio/final percentage, mass preparation/volume units and precision examples in the original are all retained; they are not silently changed and are not filled in from the 2023 edition. Can it measure total particulate metal? This edition is not a quantitative method for insoluble particles. Can product suitability or a certificate be confirmed? No. The page retains only the original public catalogue query entry; the absence of related stock does not mean the company has no corresponding product. Can it be operated directly? No, this is an unofficial study card for a historical edition; the effective controlled document, safety measures and actual equipment conditions should be checked.

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