GB/T 4336-2016 PDF English
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| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB/T 4336-2016 | English | 155 |
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Carbon and low-alloy steel - Determination of multielement contents - Spark discharge atomic emission spectrometric method (routine method)
| Valid |
| GB/T 4336-2002 | English | 359 |
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Standard test method for spark discharge atomic emission spectrometric analysis of carbon and low -- Alloy steel (routine method)
| Obsolete |
| GB/T 4336-1984 | English | 399 |
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Method for photoelectric emission spectroscopic analysis of carbon steel, medium and low alloy steel
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GB/T 4336-2016: Carbon and low-alloy steel - Determination of multielement contents - Spark discharge atomic emission spectrometric method (routine method)
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT4336-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S 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
No.1 Amendment List... 43
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.
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
chamber shall be able to replace the air in the optical path between the analysis gap
and the condenser and provide an argon atmosphere for the analysis gap.
4.5 Spectrometer
Generally, for the spectrometer, the reciprocal of the first-grade spectral line dispersion
of shall be less than 0.6 nm/mm, the focal length is 0.35 m ~ 1.0 m, the wavelength
range is 165.0 nm ~ 410.0 nm, the vacuum of the spectrometer shall work below 3 Pa,
or being filled with high-purity inert gas (the gas does not the absorb spectral line with
a wavelength less than 200 nm, and the purity is not less than 99.999 %).
4.6 Photometric system
The photometric system shall include a photoelectric conversion detector for receiving
a signal, an integrating capacitor capable of storing each of the output electrical signals,
a measuring unit for directly or indirectly recording the voltage or frequency on the
integrator, and a necessary switching circuit device provided for the desired timing.
5 Sampling and sample preparation
5.1 Sampling
The sampling and sample preparation is carried out according to the specifications of
GB/T 20066.When taking samples, it shall ensure that the analytical sample is taken
evenly, without shrinkages and cracks. When taking casting samples, the molten steel
shall be injected into the specified mold; when adopting aluminum deoxidation, the
deoxidizer content shall not exceed 0.35 %; when taking samples form steel products,
it shall select representative parts.
5.2 Sample preparation
Samples taken from the mold are usually cut in the height of 1/3 of the lower end. For
uncut samples, the surface shall be removed by 1 mm in thickness. The cutting
equipment used shall be the cutting machine with resin cutting blades, metal cutting
machines, etc.
6 Standard samples, standardization samples and
control samples
6.1 Standard samples
The standard sample is used to plot the calibration curve, its chemical properties and
organizational structure shall be similar to those of the analytical samples, and shall
cover the content range of the analytical elements and maintain the appropriate
gradient; the content of the analytical elements shall be determined with accurate and
reliable methods.
6.2 Standardization samples
The change in the state of the instrument may result in the deviation of the
measurement results, to directly use the original calibration curve to obtain accurate
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.
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.
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.
7.6 Photometric system
After being shut down and then restarted, generally adequate power time shall be
endured to make the photometric system work stably.
Select the appropriate pre-combustion time of the analytical element by making a pre-
combustion curve. The integration time is determined by the test basing on the
analytical accuracy.
8 Calibration
8.1 Calibration curve method
Under the selected working conditions, activate a series of standard samples; in
principle, use the standard samples of more than 5 levels, and activate at least 3 times
per sample; plot a curve indicating the relation between the luminous intensity (or
intensity ratio) and the content (or content ratio) of the analytical element as a
calibration curve. Use this calibration curve to measure the element content in the
sample.
8.2 Original calibration curve method
The original calibration curve method is to use the calibration curve method to plot the
calibration curve. When temperature, humidity, vibration and other factors lead to
displacement of the spectral line of the spectral instrument, or changes in luminous
intensity leads to the calibration curve drifts, use the standardization sample to correct
the drift of the calibration curve, to resume the strength of the corrected element to the
strength when the calibration curve is initially established.
8.3 Control sample method
Due to the difference in the smelting process and the organizational structure between
the analytical sample and the standard sample used to plot the calibration curve, the
calibration curve is often changed.
9 Analysis conditions and analysis procedures
9.1 Analysis conditions
The recommended analysis conditions of this Standard are as shown in Table 2, and
the analytical lines and internal marking lines are listed in Table 3.
9.2 Analysis procedures
9.2.1 Prepare the instrument in accordance with the requirements in 7.2 to 7.6.
9.2.2 Before the analysis work, activate a piece of sample 2 ~ 5 times, to confirm that
the instrument is in the best working condition.
9.2.3 Standardization of the calibration curve. under the selected working condition,
activate the standardization sample, and each sample is activated at least 3 times to
correct the calibration curve. When there are significant changes in the instrument or
the original calibration curve exceeds the calibration range due to the drift, the
calibration curve needs to be replotted.
9.2.6 Activate the analytical sample according to the working conditions selected by
Possible interference factorWavelength/nmElement
9.2.2, each sample is activated at least 2 times (the sample is activated once to obtain
an independent measurement result;
10 Calculation of analysis results
According to the relative strength (or absolute intensity) of the analytical line, obtain
the content of the analytical element from the calibration curve.
The analysis result of the elements to be measured shall be within the content range
of a series of standard sample used for the calibration curve.
11 Precision
The precision test of this Standard has been carried out by 15 laboratories to 11 to 22
levels of 14 elements in low-alloy steels in 2013, and by 12 laboratories to 18 to 36
levels of 5 elements in low-alloy steels in 2014.Under the repeatability condition as
specified in GB/T 6379.1, each laboratory shall measure the content of each level of
element 2 times.
12 Acceptability of measurement results and
determination of final report result
12.1 Under the repeatability conditions, if the absolute value of the difference between
two independent measurement results is not greater than r, the two measurement
results can be accepted. The final report result is the arithmetic mean of two
independent measurement results.
Element Content range (mass fraction)/m/% Repeatability r/% Reproducibility R/%
12.2 Under the repeatability conditions, if the absolute value of the difference between
two independent measurement results is greater than r, the laboratory shall measure
one or two more results.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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