GB/T 34099-2017 Determination of aluminum, silicon, vanadium, nickel, iron, sodium, calcium, zinc, and phosphorus content in residual fuel oils — Inductively coupled plasma emission spectrometric method

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Card type: Test method

1. Method number / full title / English title / replacement relationship

• Standard number: GB/T 34099—2017
• Chinese title: Determination of aluminum, silicon, vanadium, nickel, iron, sodium, calcium, zinc, and phosphorus content in residual fuel oils — Inductively coupled plasma emission spectrometric method
• English title: Determination of aluminium, silicon, vanadium, nickel, iron, sodium, calcium, zinc and phosphorus in residual fuel oil — Inductively coupled plasma emission spectrometry method
• Replacement relationship: not provided in the available source (the foreword only states that it was drafted in accordance with GB/T 1.1—2009, and does not mention any replaced standard)
• Publication/implementation: published on 2017-07-31, implemented on 2018-02-01
• Custodian: National Technical Committee for Standardization of Petroleum Products and Lubricants (SAC/TC 280)
• Drafting organization: Sinopec Research Institute of Petroleum Processing
• Main drafters: Yan Jingjie, Xue Yan

2. Scope of application and non-applicability

• Applicable to the determination of aluminum, silicon, vanadium, iron, nickel, sodium, calcium, zinc, and phosphorus content in residual fuel oils (Chapter 1).
• The determination range for each element is given in Table 1 (mass fraction, mg/kg):
  • Al: 5~150
  • Si: 10~250
  • V: 1~400
  • Ni: 1~100
  • Fe: 2~60
  • Na: 1~100
  • Ca: 3~100
  • Zn: 1~70
  • P: 1~60
• If the sulfur mass fraction in the residual fuel oil is greater than 0.3%, sulfur does not need to be added as an ashing aid during sample pretreatment; the precision data in Chapter 10 were obtained from fuel oils with a sulfur mass fraction greater than 0.3%.
• There is a certain correlation between the aluminum and silicon contents in residual fuel oils, and the catalyst powder content can be estimated from the aluminum or silicon content or from the contents of both elements.
• Non-applicable scope: not provided in the available source.

3. Method principle

A test portion of known mass is heated, ignited, and burned to obtain a carbonaceous residue; the residue is burned in a muffle furnace to remove residual carbon and obtain ash. The ash is fused with a lithium tetraborate-lithium fluoride flux, and the molten mixture is then dissolved in a tartaric acid-hydrochloric acid mixed solution, and finally diluted with water to a certain volume. The resulting aqueous solution is measured with an inductively coupled plasma emission spectrometer. By comparing the emission intensity of the resonance line of the element to be determined in the sample test solution with that in the standard solution, the concentration of each element to be determined is obtained, and the content of each element in the sample is then calculated (Chapter 3).

4. Reagents and materials (purity / preparation)

• 5.1 General: All reagents used are analytical grade or higher purity; the water used for testing meets at least the Grade 3 water requirements of GB/T 6682—2008.
• 5.2 Potassium bisulfate (KHSO₄): solid (the source text writes KHSOA, requires confirmation against the source standard (source-text extraction)).
• 5.3 Ashing aid: sulfur, purity better than mass fraction 99.9%.
• 5.4 Isopropanol.
• 5.5 Toluene.
• 5.6 Toluene-isopropanol mixture: volume ratio of toluene to isopropanol is 1:1.
• 5.7 Hydrochloric acid: mass fraction 36%.
• 5.8 Hydrochloric acid solution (1:1): volume ratio of hydrochloric acid (5.7) to water is 1:1.
• 5.9 Hydrochloric acid solution (1:2): volume ratio of hydrochloric acid (5.7) to water is 1:2.
• 5.10 Lithium tetraborate.
• 5.11 Lithium fluoride.
• 5.12 Flux: a mixture of mass fraction 90% lithium tetraborate (5.10) and mass fraction 10% lithium fluoride (5.11).
• 5.13 Tartaric acid.
• 5.14 Tartaric acid-hydrochloric acid mixed solution: dissolve about 5 g tartaric acid (5.13) in about 500 mL water acidified with 40 mL hydrochloric acid (5.7), then dilute with water to 1000 mL.
• 5.15 Nitric acid: mass fraction 70%.
• 5.16 Nitric acid solution (1+1): volume ratio of nitric acid (5.15) to water is 1:1.
• 5.17 Preparation of standard solutions:
  • 5.17.1 Aluminum standard solution: either a commercially available 1000 mg/L aluminum standard solution may be used, or it may be prepared according to 5.17.2.
  • 5.17.2 Preparation of aluminum standard solution: weigh 1.000 g±0.001 g aluminum metal wire (mass fraction > 99.9%) into a 400 mL beaker (4.13), add 50 mL concentrated hydrochloric acid (5.7), and heat to dissolve; after cooling, transfer to a 1000 mL volumetric flask (4.9), dilute to the mark with water, and obtain a 1000 mg/L aluminum standard solution.
  • 5.17.3 Silicon standard solution: either a commercially available 1000 mg/L silicon standard solution may be used, or it may be prepared according to 5.17.4.
  • 5.17.4 Preparation of silicon standard solution: weigh 2.140 g±0.001 g silicon dioxide of purity better than 99.99% and 8 g sodium hydroxide into a sealed zirconium crucible (4.4) and fuse; during heating, control the electric furnace heating wire to a dark red color until the melt becomes a clear liquid; after cooling, place the solid melt into a 400 mL beaker, add 100 mL hydrochloric acid solution (5.9) to dissolve; after cooling, transfer to a 1000 mL volumetric flask (4.9), dilute to the mark with water to obtain a 1000 mg/L silicon standard solution, and immediately transfer to a 1000 mL plastic bottle (4.15) for long-term storage.
  • 5.17.5 Vanadium standard solution: either a commercially available 1000 mg/L vanadium standard solution may be used, or it may be prepared according to 5.17.6.
  • 5.17.6 Preparation of vanadium standard solution: weigh 1.000 g±0.001 g vanadium metal (mass fraction > 99.9%) into a 400 mL beaker (4.13), add 40 mL nitric acid solution (5.16), and slowly heat to dissolve; after cooling, transfer to a 1000 mL volumetric flask (4.9), dilute to the mark with water, and obtain a 1000 mg/L vanadium standard solution.
  • 5.17.7 Nickel standard solution: either a commercially available 1000 mg/L nickel standard solution may be used, or it may be prepared according to 5.17.8.
  • 5.17.8 Preparation of nickel standard solution: weigh 1.000 g±0.001 g nickel metal (mass fraction > 99.9%) into a 400 mL beaker (4.13), add 40 mL nitric acid solution (5.16), and slowly heat to dissolve; after cooling, transfer to a 1000 mL volumetric flask (4.9), dilute to the mark with water, and obtain a 1000 mg/L nickel standard solution.
  • 5.17.9 Iron standard solution: either a commercially available 1000 mg/L iron standard solution may be used, or it may be prepared according to 5.17.10.
  • 5.17.10 Preparation of iron standard solution: weigh 1.000 g±0.001 g iron metal (mass fraction > 99.9%) into a 400 mL beaker (4.13), add 40 mL hydrochloric acid solution (5.8), and slowly heat to dissolve; after cooling, transfer to a 1000 mL volumetric flask (4.9), dilute to the mark with water, and obtain a 1000 mg/L iron standard solution.
  • 5.17.11 Sodium standard solution: either a commercially available 1000 mg/L sodium standard solution may be used, or it may be prepared according to 5.17.12.
  • 5.17.12 Preparation of sodium standard solution: weigh 2.542 g±0.001 g sodium chloride (NaCl) into a 400 mL beaker (4.13), dissolve with water; transfer to a 1000 mL volumetric flask (4.9), dilute to the mark with water, and obtain a 1000 mg/L sodium standard solution.
  • 5.17.13 Calcium standard solution: either a commercially available 1000 mg/L calcium standard solution may be used, or it may be prepared according to 5.17.14.
  • 5.17.14 Preparation of calcium standard solution: weigh 2.498 g±0.001 g calcium carbonate (CaCO₃) into a 400 mL beaker (4.13), add 100 mL water and add dropwise 10 mL hydrochloric acid solution (5.8) to dissolve; transfer to a 1000 mL volumetric flask (4.9), dilute to the mark with water, and obtain a 1000 mg/L calcium standard solution.
  • 5.17.15 Zinc standard solution: either a commercially available 1000 mg/L zinc standard solution may be used, or it may be prepared according to 5.17.16.
  • 5.17.16 Preparation of zinc standard solution: weigh 1.000 g±0.001 g zinc metal (mass fraction > 99.9%) into a 400 mL beaker (4.13), dissolve with a small amount of hydrochloric acid solution (5.8); transfer to a 1000 mL volumetric flask (4.9), dilute to the mark with water, and obtain a 1000 mg/L zinc standard solution.
  • 5.17.17 Phosphorus standard solution: either a commercially available 1000 mg/L phosphorus standard solution may be used, or it may be prepared according to 5.17.18.
  • 5.17.18 Preparation of phosphorus standard solution: weigh 4.264 g±0.001 g of diammonium hydrogen phosphate [(NH₄)₂HPO₄, the source text has source-text extraction as NHA, HPO., requires confirmation against the source standard (source-text extraction)] into a 400 mL beaker (4.13), dissolve with water; transfer to a 1000 mL volumetric flask (4.9), dilute to the mark with water, to obtain a 1000 mg/L phosphorus standard solution.

5. Apparatus and equipment

• 4.1 General: all platinum dishes and glass containers are required to be sodium-free, and before use must be carefully cleaned with hot hydrochloric acid solution (5.8), then thoroughly rinsed with deionized water.
• 4.2 Inductively coupled plasma optical emission spectrometer: any sequential scanning or simultaneous full-spectrum inductively coupled plasma optical emission spectrometer may be used.
• 4.3 Platinum crucible: capacity 100 mL, inner diameter not less than 70 mm, cleaned with molten potassium hydrogen sulfate (5.2). Recommended cleaning method: place 5 g of potassium hydrogen sulfate in the platinum crucible, heat in a muffle furnace to 525 ℃±25 ℃ or heat on a Bunsen burner for 5 min; after cooling, thoroughly rinse with deionized water, dry and set aside for use.
• 4.4 Zirconium crucible: capacity 30 mL~50 mL, with a lid of the same material.
• 4.5 Stirrer: non-aerating high-speed shear type.
• 4.6 Oven: capable of controlling the temperature at 50 ℃~60 ℃.
• 4.7 Muffle furnace: capable of achieving constant temperature 525 ℃±25 ℃ and 925 ℃±25 ℃; the front and back of the furnace preferably have small holes to allow dry air to pass slowly; ensure the refractory walls are intact and free of loose particles.
• 4.8 Electric heating plate: with or without magnetic stirring function.
• 4.9 Volumetric flask: 100 mL and 1000 mL, meeting the GB/T 12806—2011 A grade requirements.
• 4.10 Pipette: 1 mL, 2 mL, 5 mL, 10 mL, 20 mL and 25 mL, meeting the GB/T 12808—2015 A grade requirements.
• 4.11 Pipette: 1 mL and 2 mL, graduation value 0.1 mL, meeting the GB/T 12807—1991 requirements.
• 4.12 Graduated cylinder: 10 mL, 25 mL, 50 mL and 100 mL, meeting the GB/T 12804—2011 requirements.
• 4.13 Beaker: 400 mL, meeting the GB/T 15724—2008 requirements.
• 4.14 Filter paper: ashless quantitative filter paper, maximum ash mass fraction not exceeding 0.01%.
• 4.15 Plastic bottle: 100 mL and 1000 mL, suitable for long-term storage of dilute acid solutions.
• 4.16 Analytical balance: readability 0.2 mg.

6. Recommended operating conditions

• 7.5.1 General: operate the ICP emission spectrometer according to the instrument manual, and set the instrument operating parameters. Because different instruments differ in design, ICP excitation source and selected analytical wavelengths, it is rather difficult to specify in detail the required operating conditions; the wavelengths in Table 2 are for the user's reference only, and the user may investigate and select other suitable wavelengths according to the instrument used and the sample situation.
• Table 2 Element wavelengths (nm):
  • Al: recommended 396.15; others 167.01, 394.40 (the source text has source-text extraction as 393.36/422.67, requires confirmation against the source standard (source-text extraction))
  • Si: recommended 251.61; others 288.15
  • Na: recommended 589.59; others 588.99
  • V: recommended 292.40; others 209.88/292.46/309.31/311.07
  • Ni: recommended 231.60; others 221.68/232.00
  • Fe: recommended 259.94; others 213.86
  • Ca: recommended 317.93; others 214.91
  • Zn: recommended 213.61/178.22 (the correspondence between the Zn row and the P row in Table 2 of the source text requires confirmation against the source standard (source-text extraction))
  • P: recommended 213.61/178.22 (the correspondence between the Zn row and the P row in Table 2 of the source text requires confirmation against the source standard (source-text extraction))
• 7.5.2 Peristaltic pump: if a peristaltic pump is used, check the pump tubing before starting up each day to see whether it needs replacement; verify the solution aspiration rate and adjust it to an appropriate value.
• 7.5.3 ICP excitation source: before analysis, the ICP excitation source should be stabilized for more than 30 min; during the warm-up period, introduce distilled water or deionized water into the plasma torch (some manufacturers may recommend a longer warm-up time).
• 7.5.4 Element spectra: under normal instrument operating conditions, determine the spectra of the elements to be measured as required.
• 7.5.5 Operating parameters: in order to determine the required elements, appropriate operating parameters need to be set for the instrument, mainly including: element, wavelength, background correction point, internal standard element correction point, integration time and three consecutive replicate integrations.
• 7.5.6 Calibration curve: before testing each batch of samples, establish a five-point working curve using the blank solution and standard working solutions. When using this test method for the first time, the linearity of the instrument needs to be checked using the blank solution and standard working solutions; if the instrument is linear over the entire working curve range, two-point calibration may be used (blank and highest concentration); or three-point calibration may be used (blank, middle concentration and highest concentration); if the linearity is poor, multi-point calibration may be used.
• 7.5.7 Analysis of the solution to be tested: analyze the solution to be tested under the same conditions as the standard solutions (such as the same integration time, background correction, plasma conditions, etc.); after each sample analysis, spray distilled water or deionized water to rinse the torch for at least 10 s. If the concentration of some elements in the sample solution exceeds the mass concentration range of the standard calibration solutions, it needs to be diluted with the blank solution (7.3) so that the concentration of the sample solution is within the mass concentration range of the standard calibration solutions. After every 5 samples analyzed, calibration must be performed once with a standard calibration solution (any one); if the mass concentration of a certain element is found to exceed the known value by 5%, necessary adjustments must be made to the instrument, and then recalibration must be performed.

7. Sampling and sample preparation

• 6.1 Unless otherwise specified, all laboratory samples shall be collected according to the GB/T 4756 or GB/T 27867 method.
• 6.2 Thoroughly mix the laboratory sample uniformly in the original container before taking the test portion. Mixing method: place the sample container in an oven (4.6) at a temperature of 50 ℃~60 ℃ and heat until the sample is completely liquefied and reaches a uniform viscosity; insert the rod of the stirrer (4.5) into the sample container, with the insertion depth such that the rod head is about 5 mm from the bottom of the container, and stir the sample for about 5 min. Note: if the sample is not homogenized according to this procedure, the results obtained will be invalid.
• 7.1 Sample amount: weigh 20 g–50 g of the thoroughly mixed sample (6.2) as the test portion, so as to obtain an ash content of preferably 5 mg–50 mg; the sample amount depends on the ash content. If the content of any of the elements to be determined exceeds the concentration range of the working curve, the test solution should be diluted and the content of that element re-determined; volumetric flasks (4.9) and pipettes (4.10 or 4.11) may be selected according to the dilution factor.
• 7.2 Preparation of the sample solution:
  • 7.2.1 After the laboratory sample is thoroughly mixed, immediately transfer the test portion into a weighed platinum crucible (4.3), then weigh the total weight of the crucible and test portion, to the nearest 0.1 g, to obtain the mass of the test portion to be tested.
  • 7.2.2 If the sulfur mass fraction in the sample is lower than 0.3%, add 0.3 g of the ashing aid sulfur (5.3) to the platinum crucible, and sprinkle the sulfur as evenly as possible over the upper part of the test portion. If only aluminum, silicon and iron are to be determined, or if it is known that the ashing aid has little effect on the sample blank, the 7.5 step may be carried out directly; if the effect of the ashing aid on the blank value is unclear, or if vanadium, nickel, sodium, calcium, zinc and phosphorus are to be determined, then the ashing aid must be tested as a blank sample.
  • 7.2.3 Place the platinum crucible containing the sample on an electric furnace and heat slowly until the test portion ignites; maintain the heating temperature so that all combustible components in the test portion are burned off, leaving only residual carbon and ash. Note: if the test portion contains a large amount of water, partial loss of the sample may occur during carbonization due to bubbling. If bubbling occurs, the test portion should be discarded, a new test portion taken, and 1 mL~2 mL of isopropanol (5.4) added to the new test portion before heating again; if the bubbling still does not disappear, add 10 mL of toluene-isopropanol mixture (5.6) to the test portion and mix uniformly, then place some strips of ashless filter paper (4.14) in the mixture and heat slowly. Note: when the paper strips begin to burn, most of the water has already been removed.
  • 7.2.4 Place the carbonized platinum crucible into a muffle furnace (4.7) at 525 ℃±25 ℃, ensuring that the ash in the crucible is not contaminated by refractory materials from the inner wall of the muffle furnace, because such contamination will affect the determination result of silicon; heat at constant temperature until the carbon is burned off, leaving only ash. Note: this step may take overnight.
  • 7.2.5 Remove the platinum crucible and cool to room temperature, add 0.4 g of flux (5.12) and mix with the ash; then place the platinum crucible into a muffle furnace preheated to 925 ℃±25 ℃ for 5 min; remove it, ensure that the flux and ash have fully contacted, then place the platinum crucible into the muffle furnace and heat at 925 ℃±25 ℃ for 10 min.
  • 7.2.6 Take out the platinum crucible; after the melt has cooled to room temperature, add 50 mL tartaric acid-hydrochloric acid mixed solution (5.14), place the platinum crucible on a hot plate (4.8), and heat slowly while ensuring it does not boil until the melt is completely dissolved. Note 1: Excessive evaporation of the solution may produce a sparingly soluble silicon precipitate. Note 2: To completely dissolve the melt, the heating time needs to be extended; a magnetic stirrer or shaking may be used to accelerate the dissolution process.
  • 7.2.7 After the solution has cooled, transfer it to a 100 mL volumetric flask (4.9), rinse the platinum crucible several times with deionized water to ensure the entire sample is transferred, then dilute to the mark with water, and transfer the made-up solution to a 100 mL plastic bottle (4.15). Note: Because the dilute acid solution contains tetrafluoroboric acid (from the flux), the solution needs to be transferred to a plastic bottle; however, storage tests show that within one week the solution has no corrosive effect on glassware, and the mass concentration of free fluoride ions contained in the solution is less than 5 mg/L.
• 7.3 Preparation of the blank solution: In a 100 mL volumetric flask, add 0.4 g flux (5.12) and 50 mL tartaric acid-hydrochloric acid mixed solution (5.14), dilute to 100 mL with water, mix well, and immediately transfer to a 100 mL plastic bottle (4.15).
• 7.4 Preparation of standard calibration solutions:
  • 7.4.1 Standard calibration solutions for aluminum, silicon, vanadium, nickel, iron, sodium, calcium, zinc, and phosphorus: Take 25 mL standard solutions with mass concentration 1000 mg/L (5.17.1, 5.17.3, 5.17.5, 5.17.7, 5.17.9, 5.17.11, 5.17.13, 5.17.15, and 5.17.17) into a 100 mL volumetric flask, dilute to the mark with water, and obtain a standard solution with mass concentration 250 mg/L. Then take 36 clean 100 mL volumetric flasks, respectively add 0.4 g flux (5.12) and 50 mL tartaric acid-hydrochloric acid mixed solution (5.14); to 4 of these volumetric flasks respectively add 2 mL, 4 mL, 10 mL, and 20 mL aluminum standard solution with mass concentration 250 mg/L, and dilute to the mark with water to obtain four aluminum standard calibration solutions, with mass concentrations respectively 5 mg/L, 10 mg/L, 25 mg/L, and 50 mg/L; to another 4 volumetric flasks respectively add 2 mL, 4 mL, 10 mL, and 20 mL silicon standard solution with mass concentration 250 mg/L, and dilute to the mark with water to obtain four silicon standard calibration solutions. Using the same method, obtain standard calibration solutions for the other elements (vanadium, nickel, iron, sodium, calcium, zinc, and phosphorus). Note: The mass concentrations of the series of standard solutions for each element (aluminum, silicon, vanadium, nickel, iron, sodium, calcium, zinc, and phosphorus, 9 in total) all include 5 mg/L, 10 mg/L, 25 mg/L, and 50 mg/L.
  • 7.4.2 Storage: Transfer all standard calibration solutions to 100 mL plastic bottles (4.15) for storage. When aluminum, silicon, vanadium, nickel, iron, sodium, calcium, zinc, and phosphorus elements are determined simultaneously, the standard calibration solutions for each element from 5 mg/L to 50 mg/L may be used in combination, provided that it is ensured that there is no mismatch of reagents used among the standard solutions prepared in 5.17.1~5.17.18, or that other elements within a certain concentration range can cause only blank-level interference with the element being determined.

8. Analysis steps

• See 7.2 preparation of the sample solution, 7.3 preparation of the blank solution, 7.4 preparation of standard calibration solutions, 7.5 spectrometer operating conditions.
• 7.5.7 Analysis of the solution to be tested: Analyze the solution to be tested under the same conditions as the standard solutions; after each sample analysis, spray-rinse the torch tube with distilled water or deionized water for at least 10 s; if the concentration exceeds the range of the standard calibration solutions, dilute with blank solution (7.3); after every 5 samples analyzed, calibrate once with a standard calibration solution (any one); if the mass concentration of a certain element exceeds 5% of the known value, necessary adjustments to the instrument are required, and then recalibrate.

9. Qualitative and quantitative determination and calculation formula

• Use formula (1) to calculate the content E (mg/kg) of various elements (aluminum, silicon, vanadium, nickel, iron, sodium, calcium, zinc, and phosphorus) in the sample:
  • E = 100cd / m₂ (the original text source-text extraction writes “E=100cd”; the correspondence between denominator m₂ and 100 requires confirmation against the source standard (source-text extraction))
  • Where:
    • c: mass concentration of each element to be determined in the sample solution, obtained from the calibration curve or read directly, in milligrams per liter (mg/L);
    • d: dilution factor, the volume multiple by which the sample solution needs to be diluted so that its mass concentration falls within the concentration range of the calibration solutions;
    • m₂: mass of the sample weighed, in grams (g);
    • 100: dilution volume.
• The determination results of the content of various elements shall be accurate to 1 mg/kg.

10. Precision

• 9.1 Overview: Judge the reliability of test results according to the following provisions (95% confidence level). In 9.2 and 9.3, the precision data for elements other than aluminum and silicon were obtained through IP 367 statistics, and the precision data for aluminum and silicon were obtained from IP 377.
• 9.2 Repeatability: For the same operator, in the same laboratory, using the same instrument, determining the same sample, the difference between two consecutive replicate determination results obtained shall not be greater than the repeatability value in Table 3.
• 9.3 Reproducibility: For different operators, in different laboratories, using different instruments, correctly operating the same sample according to the test method, the difference between two single independent test results obtained shall not be greater than the reproducibility value in Table 3.
• Table 3 Precision table (z is the average of the two test results being compared, unit mg/kg):
  • Al: Repeatability 0.066 0z (the original text source-text extraction writes 0.066 0z, requires confirmation against the source standard (source-text extraction)); Reproducibility 0.337 2z (the original text source-text extraction writes 0.3372, requires confirmation against the source standard (source-text extraction))
  • Si: Repeatability 0.064 3z; Reproducibility 0.332z
  • V: Repeatability 0.654 9z^0.26 (the original text source-text extraction writes 0.654 9z26, requires confirmation against the source standard (source-text extraction)); Reproducibility 1.679 9z^0.26 (the original text source-text extraction writes 1.679 9z26, requires confirmation against the source standard (source-text extraction))
  • Ni: Repeatability 0.815 3z^0.55 (the original text source-text extraction writes 0.815 3z0.55, requires confirmation against the source standard (source-text extraction)); Reproducibility 1.681 4z^0.55 (the original text source-text extraction writes 1.681 4z0.55, requires confirmation against the source standard (source-text extraction))
  • Fe: Repeatability 0.635 8z^0.55 (the original text source-text extraction writes 0.635 8z0.55, requires confirmation against the source standard (source-text extraction)); Reproducibility 0.937 6z^0.55 (the original text source-text extraction writes 0.937 6z0.55, requires confirmation against the source standard (source-text extraction))
  • Na: Repeatability 0.537 4z^0.55 (the original text source-text extraction writes 0.537 4×055, requires confirmation against the source standard (source-text extraction)); Reproducibility 1.066 7z^0.35 (the original text source-text extraction writes 1.066 720.35, requires confirmation against the source standard (source-text extraction))
  • Ca: Repeatability 0.373 4z^0.65 (the original text source-text extraction writes 0.373 420.65, requires confirmation against the source standard (source-text extraction)); Reproducibility 0.644 0z^0.65 (the original text source-text extraction writes 0.644 0.z0.65, requires confirmation against the source standard (source-text extraction))
  • Zn: Repeatability 0.329 5z^0.7 (the original text source-text extraction writes 0.329 5z07, requires confirmation against the source standard (source-text extraction)); Reproducibility 0.508 2z^0.7 (the original text source-text extraction writes 0.508 2z7, requires confirmation against the source standard (source-text extraction))
  • P: Repeatability 0.600 8z^0.55 (the original text source-text extraction writes 0.600 8z0.55, requires confirmation against the source standard (source-text extraction)); Reproducibility 1.276 5z^0.55 (the original text source-text extraction writes 1.276 5z9.55, requires confirmation against the source standard (source-text extraction))
• Table 4 Typical precision values: the original text source-text extraction table structure is disordered, and the correspondence among elements, content, repeatability, and reproducibility cannot be reliably reconstructed, requires confirmation against the source standard (source-text extraction). The content points visible in the original text include 1, 10, 50, 100, 200, 300, 400 mg/kg, involving elements Ni, Fe, Na, Ca, Zn, P, V, etc.; the specific values require confirmation against the source standard (source-text extraction).

11. Report

The test report shall include the following contents (Chapter 10):

• a) cite this standard;
• b) detailed description of the product tested;
• c) test results (see Chapter 8);
• d) test date.

12. Referenced documents

• GB/T 4756 Petroleum liquids — Manual sampling
• GB/T 6682—2008 Water for analytical laboratory use — Specification and test methods
• GB/T 12804—2011 Laboratory glassware — Graduated cylinders
• GB/T 12806—2011 Laboratory glassware — One-mark volumetric flasks
• GB/T 12807—1991 Laboratory glassware — Graduated pipettes
• GB/T 12808—2015 Laboratory glassware — One-mark pipettes
• GB/T 15724—2008 Laboratory glassware — Beakers
• GB/T 27867 Automatic sampling method for petroleum liquids in pipelines
• References:
  • [1] IP 367 Petroleum products—Determination and application of precision data in relation to methods of test
  • [2] IP 377 Petroleum products—Determination of aluminium and silicon in fuel oils—Inductively coupled plasma emission and atomic absorption spectroscopy methods

13. Source and verification

This page is an AI translation of the available Chinese method card. Human verification is pending. It is not an official translation of the standard. Check the source standard and product certificate before use.

14. Quick Q&A Reference