GB/T 13747.24-2017 English PDF (GB/T13747.24-2017)

GB/T 13747.24-2017: Methods for chemical analysis of zirconium and zirconium alloys -- Part 24: Determination of carbon content -- Infrared absorption method after high frequency combustion
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GB/T 13747.24-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 63
Replacing GB/T 13747.24-1992
Methods for Chemical Analysis of Zirconium and Zirconium
Alloys - Part 24.Determination of Carbon Content -
Infrared Absorption Method after High Frequency
Combustion
ISSUED ON. SEPTEMBER 29, 2017
IMPLEMENTED ON. APRIL 1, 2018
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... 6
2 Method Summary... 6
3 Reagents and Materials... 6
4 Instrumentation... 7
5 Specimens... 7
6 Analysis steps... 7
7 Precision... 8
8 Test Report... 9
Foreword
GB/T 13747 Methods for Chemical Analysis of Zirconium and Zirconium Alloys is planned to
be divided into 27 parts.
---Part 1.Determination of Tin Content - Potassium Iodate Titration and Phenylfluorone-
polyethylene Glycoloctyl Phenyl Ether Spectrophotometry;
---Part 2.Determination of Iron Content - 1,10-phenanthroline Spectrophotometry and
Inductively Coupled Plasma Atomic Emission Spectrometry;
---Part 3.Determination of Nickel Content - Dimethyglyoxime Spectrophotometry and
Inductively Coupled Plasma Atomic Emission Spectrometry;
---Part 4.Determination of Chromium Content - Diphenylcarbazide Spectrophotometry
and Inductively Coupled Plasma Atomic Emission Spectrometry;
---Part 5.Determination of Aluminum Content - Chronic Azurol-S-tetradrcylpyridine
Chloride Spectrophotometry;
---Part 6.Determination of Copper Content - 2,9-Dimethyl-1,10-phenanthroline
Spectrophotometry;
---Part 7.Determination of Manganese Content - Potassium Periodate Spectrometry and
Inductively Coupled Plasma Atomic Emission Spectrometry;
---Part 8.Determination of Cobalt Content - Nitroso-R-salt Spectrophotometry;
---Part 9.Determination of Magnesium Content - Flame Atomic Absorption Spectrometry
and Inductively Coupled Plasma Atomic Emission Spectrometry;
---Part 10.Determination of Tungsten Content - Thiocyanate Spectrophotometry and
Inductively Coupled Plasma Atomic Emission Spectrometry;
---Part 11.Determination of Molybdenum Content - Thiocyanate Spectrophotometry;
---Part 12.Determination of Silicon Content - Molybdenum Blue Spectrophotometry;
---Part 13.Determination of Lead Content - Polarography;
---Part 14.Determination of Uranium Content - Polarography;
---Part 15.Determination of Boron Content - Curcumin Spectrophotometry;
---Part 16.Determination of Chloric Content - Silver Chloride Nephelometry and Ion
Selective Electrode Method;
---Part 17.Determination of Cadmium Content - Polarography;
Methods for Chemical Analysis of Zirconium and Zirconium
Alloys - Part 24.Determination of Carbon Content -
Infrared Absorption Method after High Frequency
Combustion
1 Scope
This Part of GB/T 13747 specifies the method for determining the carbon content in zirconium
and zirconium alloys.
This Part is applicable to the determination of carbon content in zirconium sponge, zirconium
and zirconium alloys. Determination range. 0.002% ~ 0.30%.
2 Method Summary
In an oxygen atmosphere, the carbon in the specimen is oxidized into carbon monoxide or
carbon dioxide in a high frequency induction furnace. The mixed gas enters the infrared detector
with the carrier gas, the detector outputs a signal, and the calculation system calculates the
carbon content based on the sample mass, and the result is expressed as a mass fraction.
3 Reagents and Materials
3.1 Acetone or other organic reagents.
3.2 Tin particles.
3.3 Iron filings.
3.4 Tungsten particles.
3.5 Oxygen (volume fraction  99.99%).
3.6 Anhydrous magnesium perchlorate.
3.7 Alkali asbestos.
3.8 Rare earth copper oxide.
3.9 Platinum-coated silica gel.
3.10 Standard substances / samples. select standard substances with similar composition and
carbon content to the test portions, or other applicable standard substances / samples.
3.11 Crucible and crucible cover. before use, heat the crucible and crucible cover in a muffle
furnace at 900 C ~ 1,000 C for 2 h. After cooling to room temperature, place them in a
desiccator for later use.
4 Instrumentation
High frequency induction furnace combustion infrared detection system (including high
frequency induction furnace, dust collection device, carrier gas purification and analysis gas
conversion system, infrared detection system, computer and software control system).
5 Specimens
5.1 The specimens are in the form of small blocks, chips or powder. The small blocks and chips
shall be cleaned by acetone or other organic reagents (3.1), then, blown dry with cold air.
5.2 The processed specimens must not be contaminated before analysis and testing. During the
test, clean tweezers shall be used to pick them up.
6 Analysis steps
6.1 Instrument Preparation
In accordance with the instrument manufacturer’s requirements, assemble all components, and
connect the power supply, carrier gas and power gas as required. Replace chemical reagent
tubes and filter units as required.
6.2 Instrument Pre-heating
Before analysis, the instrument must be fully pre-heated, so that all indicators of the instrument
reach the set values.
6.3 Instrument Leak Detection
Use the instrument leak detection program or other auxiliary equipment to confirm that the
instrument has no leaks.
6.4 Blank Detection
The blank value includes the blanks of the crucible, crucible cover and flux. The flux is an iron-
tin-tungsten mixed flux [0.1 g of tin particles (3.2), covered by 0.5 g of iron filings (3.3) and
1.2 g of tungsten particles (3.4)] or other suitable flux. Place the flux in the crucible, cover it,
determine 3 ~ 5 times in parallel, take the average value, then, perform blank compensation.
The blank value is not greater than 0.0005%.
GB/T 13747.24-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 63
Replacing GB/T 13747.24-1992
Methods for Chemical Analysis of Zirconium and Zirconium
Alloys - Part 24.Determination of Carbon Content -
Infrared Absorption Method after High Frequency
Combustion
ISSUED ON. SEPTEMBER 29, 2017
IMPLEMENTED ON. APRIL 1, 2018
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... 6
2 Method Summary... 6
3 Reagents and Materials... 6
4 Instrumentation... 7
5 Specimens... 7
6 Analysis steps... 7
7 Precision... 8
8 Test Report... 9
Foreword
GB/T 13747 Methods for Chemical Analysis of Zirconium and Zirconium Alloys is planned to
be divided into 27 parts.
---Part 1.Determination of Tin Content - Potassium Iodate Titration and Phenylfluorone-
polyethylene Glycoloctyl Phenyl Ether Spectrophotometry;
---Part 2.Determination of Iron Content - 1,10-phenanthroline Spectrophotometry and
Inductively Coupled Plasma Atomic Emission Spectrometry;
---Part 3.Determination of Nickel Content - Dimethyglyoxime Spectrophotometry and
Inductively Coupled Plasma Atomic Emission Spectrometry;
---Part 4.Determination of Chromium Content - Diphenylcarbazide Spectrophotometry
and Inductively Coupled Plasma Atomic Emission Spectrometry;
---Part 5.Determination of Aluminum Content - Chronic Azurol-S-tetradrcylpyridine
Chloride Spectrophotometry;
---Part 6.Determination of Copper Content - 2,9-Dimethyl-1,10-phenanthroline
Spectrophotometry;
---Part 7.Determination of Manganese Content - Potassium Periodate Spectrometry and
Inductively Coupled Plasma Atomic Emission Spectrometry;
---Part 8.Determination of Cobalt Content - Nitroso-R-salt Spectrophotometry;
---Part 9.Determination of Magnesium Content - Flame Atomic Absorption Spectrometry
and Inductively Coupled Plasma Atomic Emission Spectrometry;
---Part 10.Determination of Tungsten Content - Thiocyanate Spectrophotometry and
Inductively Coupled Plasma Atomic Emission Spectrometry;
---Part 11.Determination of Molybdenum Content - Thiocyanate Spectrophotometry;
---Part 12.Determination of Silicon Content - Molybdenum Blue Spectrophotometry;
---Part 13.Determination of Lead Content - Polarography;
---Part 14.Determination of Uranium Content - Polarography;
---Part 15.Determination of Boron Content - Curcumin Spectrophotometry;
---Part 16.Determination of Chloric Content - Silver Chloride Nephelometry and Ion
Selective Electrode Method;
---Part 17.Determination of Cadmium Content - Polarography;
Methods for Chemical Analysis of Zirconium and Zirconium
Alloys - Part 24.Determination of Carbon Content -
Infrared Absorption Method after High Frequency
Combustion
1 Scope
This Part of GB/T 13747 specifies the method for determining the carbon content in zirconium
and zirconium alloys.
This Part is applicable to the determination of carbon content in zirconium sponge, zirconium
and zirconium alloys. Determination range. 0.002% ~ 0.30%.
2 Method Summary
In an oxygen atmosphere, the carbon in the specimen is oxidized into carbon monoxide or
carbon dioxide in a high frequency induction furnace. The mixed gas enters the infrared detector
with the carrier gas, the detector outputs a signal, and the calculation system calculates the
carbon content based on the sample mass, and the result is expressed as a mass fraction.
3 Reagents and Materials
3.1 Acetone or other organic reagents.
3.2 Tin particles.
3.3 Iron filings.
3.4 Tungsten particles.
3.5 Oxygen (volume fraction  99.99%).
3.6 Anhydrous magnesium perchlorate.
3.7 Alkali asbestos.
3.8 Rare earth copper oxide.
3.9 Platinum-coated silica gel.
3.10 Standard substances / samples. select standard substances with similar composition and
carbon content to the test portions, or other applicable standard substances / samples.
3.11 Crucible and crucible cover. before use, heat the crucible and crucible cover in a muffle
furnace at 900 C ~ 1,000 C for 2 h. After cooling to room temperature, place them in a
desiccator for later use.
4 Instrumentation
High frequency induction furnace combustion infrared detection system (including high
frequency induction furnace, dust collection device, carrier gas purification and analysis gas
conversion system, infrared detection system, computer and software control system).
5 Specimens
5.1 The specimens are in the form of small blocks, chips or powder. The small blocks and chips
shall be cleaned by acetone or other organic reagents (3.1), then, blown dry with cold air.
5.2 The processed specimens must not be contaminated before analysis and testing. During the
test, clean tweezers shall be used to pick them up.
6 Analysis steps
6.1 Instrument Preparation
In accordance with the instrument manufacturer’s requirements, assemble all components, and
connect the power supply, carrier gas and power gas as required. Replace chemical reagent
tubes and filter units as required.
6.2 Instrument Pre-heating
Before analysis, the instrument must be fully pre-heated, so that all indicators of the instrument
reach the set values.
6.3 Instrument Leak Detection
Use the instrument leak detection program or other auxiliary equipment to confirm that the
instrument has no leaks.
6.4 Blank Detection
The blank value includes the blanks of the crucible, crucible cover and flux. The flux is an iron-
tin-tungsten mixed flux [0.1 g of tin particles (3.2), covered by 0.5 g of iron filings (3.3) and
1.2 g of tungsten particles (3.4)] or other suitable flux. Place the flux in the crucible, cover it,
determine 3 ~ 5 times in parallel, take the average value, then, perform blank compensation.
The blank value is not greater than 0.0005%.