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GB/T 4336-2016 English PDF (GBT4336-2016)

GB/T 4336-2016 English PDF (GBT4336-2016)

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GB/T 4336-2016: [Including 2017XG] Carbon and low-alloy steel -- Determination of multi-element contents -- Spark discharge atomic emission spectrometric method (routine method)

This Standard specifies the determination of carbon, silicon, manganese, phosphorus, sulfur, chromium, nickel, tungsten, molybdenum, vanadium, aluminum, titanium, copper, niobium, cobalt, boron, zirconium, arsenic and tin contents in carbon and low alloy steels by spark discharge atomic emission spectrometric method (routine method).
GB/T 4336-2016
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 77.080.20
H 11
Replacing GB/T 4336-2002
Carbon and low-alloy steel - Determination of multi-
element contents - Spark discharge atomic emission
spectrometric method (routine method)
ISSUED ON. FEBRUARY 24, 2016
IMPLEMENTED ON. NOVEMBER 1, 2016
Issued by. General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 6
3 Principle ... 6
4 Instruments ... 6
5 Sampling and sample preparation ... 7
6 Standard samples, standardization samples and control samples ... 8
7 Preparation of instruments ... 9
8 Calibration ... 10
9 Analysis conditions and analysis procedures ... 11
10 Calculation of analysis results ... 15
11 Precision ... 15
12 Acceptability of measurement results and determination of final report result ... 16
13 Determination of the accuracy of laboratory measurement results ... 19 14 Test report ... 19
Annex A (informative) Additional information of precision test ... 20
Annex B (informative) Precision-related data ... 33
Foreword
This Standard is drafted in accordance with the rules given in GB/T 1.1-2009. This Standard replaces GB/T 4336-2002 ?€?Carbon and low-alloy steel - Spark discharge atomic emission spectrometric method (routine method)?€?, compared with GB/T 4336- 2002, main technical content changes are as follows.
- The standard name is changed to ?€?Carbon and low-alloy steel - Determination of multi-element contents - Spark discharge atomic emission spectrometric method (routine method)?€?;
- MODIFY the measurement range of each element in Table 1;
- ADD the reference in ?€?2 Normative references?€?;
- MODIFY the description of the principle in ?€?3 Principle?€?;
- MODIFY the description of the excitation light source in 4.1;
- MODIFY the description of the spark room in 4.2;
- MODIFY the requirements for the purity of argon in 4.3, clearly specify the argon pressure and the instrument parts with constant flow;
- MODIFY the description of the electrode in 4.4;
- MODIFY the focal length and wavelength range in 4.5;
- MODIFY the description of the photometric system in 4.6;
- MODIFY ?€?6 Standard samples and recalibrated samples?€? TO ?€?6 Standard samples, standardization samples and control samples?€?; MODIFY the corresponding
description;
- ADD ?€?8 Calibration?€? and its description;
- MODIFY ?€?8 Analysis conditions and analysis procedures?€? TO ?€?9 Analysis conditions and analysis procedures?€?; MODIFY its description;
- MODIFY ?€?10 Precision?€? TO ?€?11 Precision?€?; re-calculate the repeatability limit and reproducibility limit formulas of each element according to the results of precision test;
- ADD ?€?12 Acceptability of measurement results and determination of final report result";
Carbon and low-alloy steel - Determination of multi-
element contents - Spark discharge atomic emission
spectrometric method (routine method)
1 Scope
This Standard specifies the determination of carbon, silicon, manganese, phosphorus, sulfur, chromium, nickel, tungsten, molybdenum, vanadium, aluminum, titanium, copper, niobium, cobalt, boron, zirconium, arsenic and tin contents in carbon and low alloy steels by spark discharge atomic emission spectrometric method (routine method).
This Standard applies to the sample analysis of casting or forging carbon and low-alloy steels by electric furnace, induction furnace, electroslag furnace, converter furnace, etc.; see Table 1 for the measurement range of each element.
Table 1 Determination range of each element
Element Measurement range (mass fraction)/%
2 Normative references
The following documents are indispensable for the application of this document. For dated references, only the dated edition applies to this document. For undated references, the latest edition (including all modifications) applies to this document. GB/T 6379.1 Accuracy (trueness and precision) of measurement methods and results - Part 1. General principles and definitions
GB/T 6379.2 Accuracy (trueness and precision) of measurement methods and results - Part 2. Basic method for the determination of repeatability and reproducibility of a standard measurement method
GB/T 20066 Steel and iron - Sampling and preparation of samples for the determination of chemical composition
3 Principle
Discharge is generated between the prepared bulk sample and the counter electrode under the action of the spark light source, and the plasma is generated in the high temperature and the inert atmosphere. When the atoms of the measured element are activated, the electrons are transitioned between different energy levels in the atom, and the characteristic spectrum is generated when the transition from the high-energy level to the low-energy level. Measure the spectral intensity of the characteristic spectrum of the selected analytical element and the internal standard element. According to the relation between the spectral intensity (or intensity ratio) and the concentration of the element to be measured in the sample, the content of the element to be measured is calculated by the calibration curve.
4 Instruments
The spark discharge atomic emission spectrometer consists mainly of the following units.
4.1 Excitation light source
The excitation light source shall be a stable spark excitation light source. 4.2 Spark room
The spark room is specially designed for use with argon, and the spark room is mounted directly on the spectrometer, with an argon flush spark bracket to place the flat sample and the rod-shaped counter electrode. The argon gas path in the spark results, 1 ~ 2 samples are used to standardize the instrument, these samples are called standardization samples. The sample shall be very uniform and have an appropriate content; the sample can be selected from standard samples or specially smelted. When using two-point standardization, the content is the content on each element calibration curve, respectively, near the upper and lower limits. The standardization sample is used to correct the deviation of the measured value of the instrument from the calibration curve due to various causes. The standardization sample shall be uniform and capable of obtaining a stable spectral line intensity. 6.3 Control samples
The control sample is the uniform sample with similar metallurgical process, organizational structure and chemical composition to those of the analytical sample, being used for correcting the measurement results of the analytical sample or for type standardization correction.
The control sample can be made by molding of molten metal or from metal products; when smelting the control sample, the content of each element shall be specified appropriately, so that the matrix composition of each sample is roughly equal; when assigning the control sample, attention shall be paid to the setting error of standard values and the traceability of data and methods.
7 Preparation of instruments
7.1 Storage of instruments
The spectrometer, as recommended by the equipment manufacturer, shall be placed in shock-proof and clean laboratories, usually the indoor temperature maintains at 15 ??C ~ 30 ??C and the relative humidity shall be less than 80 %. In the same standardization cycle, the indoor temperature change does not exceed 5 ??C. 7.2 Power supply
To ensure the stability of the instrument, the power supply voltage change shall be less than ?? 10 %, the frequency change shall be less than ?? 2 % and the AC power supply shall be the sine wave. According to the use requirements of the instrument, a dedicated ground line shall be equipped.
7.3 Excitation light source
In order to make the electrical part of the excitation light source work stably, before starting work, it shall be given the appropriate power time.
Use a voltage regulator or a voltage regulator device to adjust the power supply voltage to the desired value of the instrument.
7.4 Counter electrode
The electrode shall be regularly cleaned and replaced, the distance of the analysis gap shall be adjusted with the distance gauge, to keep it in normal working condition. 7.5 Optical system
The condenser shall be regularly cleaned and traced to correct the entrance slit position.
7.6 Photometric system
After being shut down and then restarted, generally adequate power time shall be endured to make the photometric sys...

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