GB/T 11170-2008 PDF in English
GB/T 11170-2008 (GB/T11170-2008, GBT 11170-2008, GBT11170-2008)
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GB/T 11170-2008 | English | 190 |
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Stainless steel -- Determination of multi-element contents -- Spark discharge atomic emission spectrometric method (Routine method)
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GB/T 11170-1989 | English | 279 |
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Method for photoelectric emission spectroscopic analysis of stainless steel
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Standards related to (historical): GB/T 11170-2008
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GB/T 11170-2008: PDF in English (GBT 11170-2008) GB/T 11170-2008
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.080.20
H 11
Replacing GB/T 11170-1989
Stainless steel - Determination of multi-element contents -
Spark discharge atomic emission spectrometric method
(Routine method)
ISSUED ON: SEPTEMBER 11, 2008
IMPLEMENTED ON: MAY 01, 2009
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
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 equipment ... 7
6 Standard samples, standardized samples and control samples ... 8
7 Preparation of instruments ... 8
8 Analysis conditions and steps ... 9
9 Calculation of analysis results ... 13
10 Precision ... 13
11 Test report ... 14
Stainless steel - Determination of multi-element contents -
Spark discharge atomic emission spectrometric method
(Routine method)
1 Scope
This Standard specifies the analysis for the determination of carbon, silicon, manganese,
phosphorus, sulfur, chromium, nickel, molybdenum, aluminum, copper, tungsten,
titanium, niobium, vanadium, cobalt, boron, arsenic, tin and lead contents by spark
discharge atomic emission spectrometric method.
This Standard applies to the determination of carbon, silicon, manganese, phosphorus,
sulfur, chromium, nickel, molybdenum, aluminum, copper, tungsten, titanium, niobium,
vanadium, cobalt, boron, arsenic, tin and lead contents in stainless steel. The
determination range of each element is shown in Table 1.
2 Normative references
The terms in the following documents become the terms of this Standard by reference
to this Standard. For dated references, all subsequent amendments (not including errata
content) or revisions do not apply to this Standard. However, parties to agreements that
are based on this Standard are encouraged to study whether the latest versions of these
standards can be used. For undated references, the latest edition applies to this Standard.
GB/T 6379.1, Accuracy (trueness and precision) of measurement methods and
results - Part 1: General principles and definitions (GB/T 6379.1-2004, ISO 5725-
1:1994, IDT)
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 6379.2-2004, ISO 5725-
2:1994, IDT)
GB/T 20066, Steel and iron - Sampling and preparation of samples for the
determination of chemical composition (GB/T 20066-2006, ISO 14284:1996, IDT)
3 Principle
Use the prepared block sample as an electrode; use a light source generator to excite
and emit light between the sample and the counter electrode; introduce the beam into
the spectrometer. After the light beam is dispersed by the dispersion element, measure
the intensity of the selected internal standard line and analytical line. According to the
calibration curve of standard samples, obtain the content of the to-be-measured element
in the analyzed sample.
4 Instruments
The spark discharge atomic emission spectrometer – vacuum type or gas-filled type –
is mainly composed of the following units.
4.1 Excitation light source
The excitation light source shall be a stable spark discharge light source.
4.2 Spark chamber
The spark chamber shall be specially designed for the use of argon gas. The spark
chamber shall be mounted directly on the spectrometer, and shall have an argon-flushed
spark stand, to accommodate the flat sample and the rod-shaped counter electrode. The
argon gas circuit of the spark chamber shall be able to replace the air in the optical path
between the analytical gap and the condenser, and provide an argon atmosphere for the
analytical gap.
4.3 Argon gas system
The argon gas system mainly includes an argon gas container, a two-stage pressure
regulator, a gas flow meter and a timing control part that can automatically change the
argon gas flow rate according to the analysis conditions.
Since the purity and flow rate of argon gas have a great influence on the analysis and
measurement value, it shall be ensured that the purity of argon gas is not less than
99.996%; otherwise, an argon gas purification device must be used, and the pressure
and flow rate of argon gas in the spark chamber must be kept constant.
4.4 Counter electrode
Different counter electrodes shall be used for equipment of different models. Generally,
a conical tungsten rod with a diameter of 4 mm ~ 7 mm and a top processing of 30° ~
120° shall be used; also, a flat tungsten electrode with a diameter of 1 mm can be used.
Each laboratory determines the time to replace the counter electrode according to the
specific situation.
4.5 Spectrometer
In general, the reciprocal of the first-order spectral line dispersion of a spectrometer
shall be less than 0.6 nm/mm, the focal length shall be 0.5 m ~ 1.0 m, and the
wavelength range shall be 120.0 nm ~ 623.0 nm. The vacuum degree of the
spectrometer shall work below 3 Pa, or be filled with high-purity nitrogen or argon gas
(the gas does not absorb spectral lines with wavelengths less than 200 nm, and the purity
is not lower than 99.999%).
4.6 Photometric system
The photometric system shall include a photomultiplier tube (or other photoelectric
conversion device) for receiving signals, an integrating capacitor capable of storing
each output electrical signal, a measuring unit for directly or indirectly recording the
voltage on the capacitor, and a necessary switching circuitry provided for the required
timing.
5 Sampling and sample preparation equipment
5.1 Sampling and sample preparation
Sampling and sample preparation shall be carried out in accordance with the
requirements of GB/T 20066. The surface of the sample taken shall ensure that two
points can be excited without overlapping, the recommended thickness is not less than
3 mm, and there is no physical defect.
5.2 Sample preparation equipment
The grinding equipment can be a grinding machine, a sandpaper disc or an abrasive
band grinding machine, or can be a milling machine, a lathe, etc.
6 Standard samples, standardized samples and control
samples
6.1 Standard samples
Standard samples are certified reference materials required for routine analysis to draw
calibration curves. The content of each analytical element in the standard samples shall
have an appropriate gradient, and the chemical value shall be accurate and free from
physical defects. The selected standard samples shall be as close as possible to the type
of samples to be tested.
6.2 Standardized samples
Due to changes in the state of the instrument, the measurement results deviate. In order
to directly use the original calibration curve to obtain accurate results, use (1~2)
samples to standardize the instrument. These samples are called standardized samples.
Standardized samples, which shall be very uniform and shall have appropriate contents,
can be selected from standard samples or specially smelted. When two-point
standardization is used, the content is taken as the content near the upper limit and lower
limit of the calibration curve of each element respectively.
6.3 Control samples
Control samples, which have similar metallurgical process and chemical composition
to the analytical samples, are used to correct the measurement results of the analytical
samples.
7 Preparation of instruments
7.1 Basic requirements
The spectrometer shall be placed in a shockproof and clean laboratory with an indoor
temperature of 16 °C ~ 30 °C and a relative humidity of 40% ~ 70%. In the same
calibration period, the maximum allowable indoor temperature difference is 5 °C/h.
7.2 Power supply
In order to ensure the stability of the instrument, the power supply voltage variation
shall be within ±10%, and the frequency variation shall not exceed ±2%. It shall be
...... Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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