GB/T 24583.2-2019 English PDF (GBT24583.2-2019)

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GB/T 24583.2-2019: Vanadium-nitrogen -- Determination of nitrogen content -- Thermal conductimetric method after fusion in a current of inert gas
GB/T 24583.2-2019
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.100
H 11
Replacing GB/T 24583.2-2009
Vanadium-nitrogen - Determination of nitrogen
content - Thermal conductimetric method after fusion
in a current of inert gas
ISSUED ON: JUNE 04, 2019
IMPLEMENTED ON: MAY 01, 2020
Issued by: State Administration for Market Regulation;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3 
1 Scope ... 5 
2 Normative references ... 5 
3 Principles ... 6 
4 Reagents and materials ... 6 
5 Instruments and equipment ... 6 
6 Sampling and sample preparation ... 8 
7 Analytical procedures ... 8 
8 Expression of analysis results ... 9 
9 Precision ... 10 
10 Test report ... 10 
Appendix A (Normative) Flow chart for acceptance procedure of sample
analysis value ... 11 
Appendix B (Informative) Raw data of joint precision test ... 12 
Foreword
GB/T 24583 Vanadium-nitrogen alloy analysis method is divided into 8 parts:
- GB/T 24583.1 Vanadium-nitrogen - Determination of vanadium content -
Ammonium ferrous sulfate titration method;
- GB/T 24583.2 Vanadium-nitrogen - Determination of nitrogen content -
Thermal conductimetric method after fusion in a current of inert gas;
- GB/T 24583.3 Vanadium-nitrogen - Determination of nitrogen content -
Distillation-neutralization titration method;
- GB/T 24583.4 Vanadium-nitrogen - Determination of carbon content -
Infrared absorption method;
- GB/T 24583.5 Vanadium-nitrogen - Determination of phosphorus content -
Bismuth molybdenum blue spectrophotometric method;
- GB/T 24583.6 Vanadium-Nitrogen alloy - Determination of sulfur content -
The infrared absorption method;
- GB/T 24583.7 Vanadium-nitrogen - Determination of oxygen content -
Infrared absorption method;
- GB/T 24583.8 Vanadium-nitrogen - Determination of silicon, manganese,
phosphorus, aluminum content - Inductively coupled plasma atomic
emission spectrometric method.
This Part is Part 2 of GB/T 24583.
This Part is drafted in accordance with the rules given in GB/T 1.1-2009.
This Part replaces GB/T 24583.2-2009 “Vanadium-Nitrogen alloy -
Determination of nitrogen content - Thermal conductimetric method after fusion
in a current of inert gas”. Compared with GB/T 24583.2-2009, the main
technical changes in this Part are as follows:
- CHANGE the measuring range (mass fraction) to “8.00%~20.00%” (see
Clause 1; Clause 1 of the 2009 edition);
- Modify “Normative references” (see Clause 2; Clause 2 of the 2009 edition);
- CHANGE the graphite crucible from high-temperature graphite crucible to
suitable-for-instrument high-purity graphite crucible (see 4.12; 4.9 of the
2009 edition);
Vanadium-nitrogen - Determination of nitrogen
content - Thermal conductimetric method after fusion
in a current of inert gas
Caution - The personnel using this Part shall have hands-on experience
in formal laboratory work. This Part does not address all possible safety
problems. It is the responsibility of the user to take appropriate safety and
health measures and to ensure compliance with the conditions set by the
relevant national regulations.
1 Scope
This Part of GB/T 24583 specifies the determination of nitrogen content in
vanadium-nitrogen alloy by thermal conductimetric method after fusion in a
current of inert gas.
This Part applies to the determination of nitrogen content in vanadium-nitrogen
alloy. Measuring range (mass fraction): 8.00%~20.00%.
2 Normative references
The following documents are indispensable for the application of this document.
For the dated references, only the editions with the dates indicated are
applicable to this document. For the undated references, the latest edition
(including all the amendments) are applicable 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 8170 Rules of rounding off for numerical values and expression and
judgement of limiting values
GB/T 20567 Vanadium-nitrogen
5.2.1 The carrier gas system includes a helium container, a two-stage pressure
regulator, and a sequential control part which ensures proper pressure and
rated flow.
5.2.2 The power gas source includes power gas (nitrogen or compressed air),
a two-stage pressure regulator, and a sequential control part which ensures
proper pressure and rated flow.
5.3 High-temperature electrode furnace
It shall meet the requirements for the fusion temperature of the test portion.
5.4 Control system
Control functions include crucible loading-unloading, coil base lift, dust collector
cleaning, analysis condition selection settings, analysis process monitoring and
alarm interruption, analysis data acquisition, calculation, correction, and
processing, etc.
5.5 Measurement system
It is mainly composed of an electronic balance (sensitivity is 0.1 mg) controlled
by a microprocessor, a thermal conductivity cell detector, and an electronic
measuring element.
6 Sampling and sample preparation
In accordance with the provisions of GB/T 20567, the sample shall be taken
and prepared. The sample shall all pass through the 0.125 mm sieve pore.
7 Analytical procedures
7.1 Number of determinations
The same sample is determined at least twice independently.
7.2 Test portion
WEIGH 0.05 g of sample, accurate to 0.0001 g.
7.3 Analysis preparation
7.3.1 According to the instruction manual of the instrument, debug and check
the instrument (mainly air-tightness check), to keep the instrument in a normal
stable state.
7.3.2 Choose to set the best analysis conditions.
7.3.3 USE the sample and flux to perform two test trials according to 7.6, to
determine if the instrument is normal.
7.4 Blank test
At least 3 blank tests are performed along with the test portion. The nitrogen
blank value shall be less than 2 μg. Calculate the average. Refer to the
instrument manual. INPUT the average as a blank to the azotometer. The
instrument, when measuring the test portion, will automatically perform the
electronic compensation of the blank value.
7.5 Calibration test
According to the nitrogen content of the sample to be tested, establish a
corresponding analysis curve; choose at least 2 standard samples (The
nitrogen content range of standard sample shall cover the nitrogen content of
the sample to be tested). The calibration and check shall be carried out in turn.
The fluctuation of the determination result shall be within the range of
reproducibility limit, to confirm the linearity of the system. Otherwise, the
linearity of the system shall be adjusted according to the instrument manual.
7.6 Determination
7.6.1 According to the type of graphite crucible used in the azotometer, one of
the following combinations is selected as a flux:
a) Tin capsule (see 4.6)+nickel capsule (see 4.7);
b) Tin capsule (see 4.6)+nickel basket (see 4.8);
c) Nickel capsule (see 4.7)+0.20 g of tin granule (see 4.5).
7.6.2 LOAD the test portion (see 7.2) into the selected tin capsule (see 4.6) or
nickel capsule (see 4.7); ADD another flux selected in 7.6.1; carefully
SQUEEZE and wrap; PLACE in the instrument’s feeding device. PLACE the
graphite c...