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GB/T 37160-2019 English PDF (GBT37160-2019)

GB/T 37160-2019 English PDF (GBT37160-2019)

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GB/T 37160-2019: Standard test method for determination of trace metals in heavy distillate, residual oil and crude oil -- Inductively coupled plasma optical emission spectrometry (ICP-OES)

This Standard specifies using inductively coupled plasma optical emission spectrometry (ICP-OES) to determine the element contents such as aluminum, calcium, iron, potassium, magnesium, manganese, molybdenum, sodium, nickel, leak, vanadium and zinc in the heavy distillates, residual oils and crude oils.
GB/T 37160-2019
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 75.140
E 49
Standard Test Method for Determination of Trace
Metals in Heavy Distillate, Residual Oil and Crude Oil ?€?
Inductively Coupled Plasma Optical Emission
Spectrometry (ICP-OES)
ISSUED ON: MARCH 25, 2019
IMPLEMENTED ON: OCTOBER 01, 2019
Issued by: State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
Introduction ... 4
1 Scope ... 5
2 Normative References ... 5
3 Method Summaries ... 6
4 Apparatus ... 6
5 Reagents and Materials ... 7
6 Safety Events ... 7
7 Sampling and Specimen Processing ... 8
8 Preparation ... 8
9 Test Procedures ... 11
10 Calculation ... 12
11 Expression of Results ... 13
12 Precision and Deviation ... 13
Bibliography ... 15
Standard Test Method for Determination of Trace
Metals in Heavy Distillate, Residual Oil and Crude Oil ?€?
Inductively Coupled Plasma Optical Emission
Spectrometry (ICP-OES)
Warning: This Standard involves certain hazardous materials, operation and equipment; but is not intended to advise on all related safety issues. Therefore, users shall establish appropriate safety and protection measures and determine the applicability of the relevant regulatory restrictions before applying this Standard.
1 Scope
This Standard specifies using inductively coupled plasma optical emission spectrometry (ICP-OES) to determine the element contents such as aluminum, calcium, iron, potassium, magnesium, manganese, molybdenum, sodium, nickel, leak, vanadium and zinc in the heavy distillates, residual oils and crude oils. This Standard is applicable to the determination of trace metals in the heavy distillates, residual oils and crude oils; the Table 1 gives the measured concentration range and recommended wavelength of each element.
NOTE: Heavy distillates refer to the components distilled under reduced pressure, such as heavy diesel oil, wax oil, catalytic raw materials, vacuum gas oil, and the like. 2 Normative References
The following documents are essential to the application of this document. For the dated documents, only the versions with the dates indicated are applicable to this document; for the undated documents, only the latest version (including all the amendments) are applicable to this document.
GB/T 4756 Petroleum Liquids - Manual Sampling
GB/T 6682-2008 Water for Analytical Laboratory Use - Specification and Test Methods
4.14 Oven: The temperature can be controlled between 50??C and 60??C.
4.15 Water bath: The temperature can be controlled between 50??C and 100??C. 5 Reagents and Materials
5.1 Reagent purity: All reagents used in this Standard are of analytical grade or higher purity. If other grades of reagents are used, check the reagents for sufficient purity to ensure that the accuracy of the results is not affected.
5.2 Hydrochloric acid: The mass fraction is 36% ~ 38%.
Warning: Hydrochloric acid is corrosive acid that can cause burns.
5.3 Nitric acid: The mass fraction is 65%~68%.
Warning: Nitric acid is a corrosive acid that can cause burns.
5.4 Aqua regia: Nitric acid and hydrochloric acid shall be mixed in a volume ratio of 1:3; and it shall be prepared currently before each use.
Warning: Aqua regia is a corrosive acid that can cause burns.
5.5 Sulfuric acid: The mass fraction is 95%~98%.
Warning: Sulfuric acid is a corrosive acid that can cause burns.
5.6 Water: Deionized water; meet the requirements of Class-II water specified in GB/T 6682-2008.
5.7 Standard solution of internal standard element of scandium: The concentration is 1000mg/L; a commercially available standard solution can be used.
5.8 Standard solutions of metal elements: The concentration of aluminum, calcium, iron, potassium, magnesium, manganese, molybdenum, sodium, nickel, lead, vanadium and zinc is 1000mg/L, respectively; a commercially available standard solution can be used.
6 Safety Events
This Standard requires the use of high-pressure gas and corrosive acid. In the process of using nitric acid, hydrochloric acid, sulfuric acid, aqua regia, appropriate personal protective equipment shall be provided. Special tools shall be used to open high- pressure gas such as argon and compressed air.
8.3 Preparation of standard storage solution for metal element
8.3.1 Standard storage solution A for metal element: use pipette (4.7) to separately transfer 10mL of aluminum, calcium, iron, potassium, magnesium and manganese metal element standard solution (5.8) with concentration of 1000mg/L into 100mL volumetric flask (4.6); then use pipette to take 4mL of aqua regia (5.4) into the volumetric flask; use water (5.6) to dilute to the mark; then obtain the standard storage solution A for metal element with concentration of 100mg/L. This solution has a shelf life of one month.
8.3.2 Standard storage solution B for metal element: use pipette (4.7) to separately transfer 10mL of molybdenum, sodium, nickel, lead, vanadium and zinc metal element standard solution (5.8) with concentration of 1000mg/L into 100mL volumetric flask (4.6); then use pipette to take 4mL of aqua regia (5.4) into the volumetric flask; use water (5.6) to dilute to the mark; then obtain the standard storage solution B for metal elements with concentration of 100mg/L. This solution has a shelf life of one month. 8.4 Preparation of blank solution
Use pipette to transfer 1mL of standard storage solution for internal standard element of scandium (8.2.1) with concentration of 100mg/L into 100mL volumetric flask; use pipette to transfer 4mL of aqua regia into the volumetric flask; dilute with water to the mark; shake evenly; then obtain the standard blank solution. This solution has a shelf life of one month.
8.5 Preparation of 5mg/L standard working solution for metal element
Use pipette to separately transfer 1mL of standard storage solution for internal standard element of scandium (8.2.1) with concentration of 100mg/L, 5mL of standard storage solution A for metal element (8.3.1) with concentration of 100mg/L, 5mL of standard storage solution B for metal element (8.3.2) with concentration of 100mg/L, and 4mL of aqua regia into 100mL volumetric flask; use water to dilute to the mark; shake evenly. Then obtain the standard working solution for metal elements of aluminum, calcium, iron, potassium, magnesium, manganese, molybdenum, sodium, nickel, lead, vanadium, and zinc with concentration of 5mg/L. This solution has a shelf life of one month.
8.6 Preparation of 10mg/L standard working solution for metal element
Use pipette to separately transfer 1mL of standard storage solution for internal standard element of scandium (8.2.1) with concentration of 100mg/L, 10mL of standard storage solution A for metal element (8.3.1) with concentration of 100mg/L, 10mL of standard storage solution B for metal element (8.3.2) with concentration of 100mg/L, and 4mL of aqua regia into 100mL volumetric flask; use water to dilute to the mark; shake evenly. Then obtain the standard working solution for metal elements of aluminum, calcium, iron, potassium, magnesium, manganese, molybdenum, sodium, 8.7.7 Prepare the reagent blank as per the above procedures 8.7.2~8.7.6 for specimen preparation.
9 Test Procedures
9.1 Start the ICP-OES and ignite the plasma torch until the instrument is stable. Successively pipette the blank solution (8.4), 5mg/L standard working solution for metal element (8.5) and 10mg/L standard working solution for metal element (8.6); establish the standard working curve for each to-be-tested element. Table 1 lists the measured concentration ranges and the spectral line wavelengths of each to-be-tested element. Other wavelengths may also be used if the spectral line overlap occurs. The wavelength selection shall maintain sufficient sensitivity to achieve the necessary detection limits.
9.2 Successively pipette reagent blank (8.7.7) and the to-be-tested solution (8.7.6); determine the content of each element in the test solution; calculate the final results of each to-be-tested element in the specimen according to the specimen mass and constant volume.
9.3 If the concentration of one or more elements is outside the range of the calibration curve concentration, then use the blank solution (8.4) to dilute the test solution to the reading range of the calibration curve, and re-measure it.

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