GB/T 6609.2-2022Chemical analysis methods and determination of physical performance of alumina—Part 2: Determination of loss of mass at 300 °C and 1000 °C (English PDF)
氧化铝化学分析方法和物理性能测定方法 第2部分：300 ℃和1000 ℃质量损失的测定
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
March 9, 2022
Implementation date
October 1, 2022
Scope
GB/T 6609.2-2022 is the English-translated version of 氧化铝化学分析方法和物理性能测定方法 第2部分：300 ℃和1000 ℃质量损失的测定.
GB/T 6609.2-2022 is the part of the Chinese series on the analysis of alumina that determines the mass loss at 300 °C and at 1000 °C. It gives the method by which the moisture content, MOI, is obtained as the mass lost by the original specimen after drying at 300 °C, and the loss on ignition, LOI, as the mass lost by a pre-dried specimen when fired at 1000 °C, with the apparatus, the procedure, the calculation, the precision and the test report.
It applies to alumina, where these two figures decide the dry weight and the calcination state of a delivery. Refineries, smelters and their laboratories use it.
It replaces GB/T 6609.2-2009, was issued on 9 March 2022 and has applied since 1 October 2022.
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Document preview — GB/T 6609.2-2022
National Standard of the People's Republic of China
- ICS
- 71.100.10
- Classification
- H 12
- Replacing
- GB/T 6609.2-2009
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword3
- Introduction7
- 1 Scope9
- 2 Normative references9
- 3 Terms and definitions9
- 4 Instruments and equipment10
- 5 Determination of moisture content (MOI)10
- 6 Loss of ignition (LOI) measurement11
- 7 Instrument analysis14
- 8 Precision15
- 9 Test report16
- Annex A (informative) Schematic diagram of a typical drying device18
- Annex B (normative) Preparation procedure of air balance specimen20
1 Scope
This document specifies the method for determining the mass loss of alumina at 300 °C and 1000 °C. The mass loss of the original specimen after drying at 300 °C is represented by the moisture content (MOI). Use loss on ignition (LOI) to represent the mass loss of a pre-dried specimen at 300 °C when burned at 1000 °C.
This document is applicable to the determination of mass loss in alumina. The mass loss measurement range is at 300 °C. 0.20%~5.00%; The mass loss measurement range is at 1000 °C is 0.10%~2.00%. Instrumental analysis is not used as an arbitration test method.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB/T 6609.23, Chemical analysis methods and determination of physical performance of alumina -- Preparation and storage of test samples
GB/T 8170, Rules of rounding off for numerical values and expression and judgement of limiting values
3 Terms and definitions
There are no terms or definitions that need to be defined in this document.
4 Instruments and equipment
4.1 Drying machine. including an alumina heating frame that can hold 4 platinum crucibles and a drying agent, using activated alumina (activated alumina shall be heated and activated at 300 °C±5 °C before use) or phosphorus pentoxide as the drying agent.
The dryer shall be equipped with a metal heat-resistant frame with a diameter of about 150 mm and a depth of about 30 mm. A dehumidification trap shall be installed at the inlet of the dryer cover. The dehumidification trap shall be equipped with granular desiccant. A typical schematic diagram of a drying device can be found in Annex A.
4.2 Platinum crucible (with platinum lid). the diameter is about 35 mm and the depth is about 40 mm.
4.3 Oven. the temperature can be controlled at 300 °C±5 °C; ensure air flow inside the oven.
4.4 High temperature furnace. the temperature can be controlled at 1000 °C±10 °C.
4.5 Analytical balance. sensitivity is 0.0001 g.
4.6 Thermogravimetric analyzer. at least including heating system, weighing system, control system and other parts. The furnace temperature of the instrument can be controlled at 300 °C±5 °C and 1000 °C±10 °C. The sensitivity of the built-in balance in the weighing system is 0.0001 g. Its accuracy shall meet the special accuracy level calibration requirements of electronic balances.
4.7 Weighing bottle (including lid). the size is sufficient to hold the required amount of specimen.
4.8 Plate. flat bottomed, with a bottom area of not less than 100 cm2.
5 Determination of moisture content (MOI)
5.1 Principle
Dry the original specimen at a temperature of 300 °C±5 °C for 2 h. Calculate the moisture content of the original specimen based on the difference in mass before and after.
5.2 Specimens
The specimen shall comply with the original specimen preparation and storage requirements in GB/T 6609.23.
6 Loss of ignition (LOI) measurement
6.1 Principle
Burn the pre-dried specimen at 300 °C±5 °C for 2 h at a temperature of 1000 °C±10 °C.
Calculate the burn loss based on the difference in mass before and after.
6.1.2 Specimens
The specimen is a pre-dried specimen at 300 °C, obtained by drying the original alumina specimen (5.2) at a temperature of 300 °C±5 °C for 2 h.
6.1.3 Test steps
6.1.3.1 Parallel test
Conduct two parallel tests. Take the average value.
6.1.3.2 Preparation of platinum crucible
Heat and burn the platinum crucible (4.2) in a high-temperature furnace (4.4) at 1000 °C±10 °C for 15 min. Take it out and cool it slightly. Put it into the dryer (4.1).
Cool for 10 min. Quickly take out and weigh to the nearest 0.0001 g. Record the mass of the platinum crucible (m3).
6.1.3.3 Burn reduction measurement at 1000 °C
Add 5 g±0.5 g of specimen (6.1.2) to the processed platinum crucible (see 6.1.3.2).
Record the specimen mass (m4) to the nearest 0.0001 g. Immediately cover the lid (weighing operation shall be completed within 20 s). Immediately place the platinum crucible in the high-temperature furnace (4.4). Tilt the lid to expose obvious gaps or remove the lid and place it in a high-temperature furnace to raise the temperature to 1000 °C±10 °C. Maintain at this temperature for 2 h. Remove the platinum crucible.
Quickly place it in the dryer (4.1). Cover the lid. After cooling to room temperature (the cooling time shall not exceed 30 min), slowly release the vacuum in the dryer through a moisture trap without interfering with the measurement. Immediately weigh the total mass of the platinum crucible and specimen after burning, accurate to 0.0001 g. Record its mass (m5).
6.1.4 Test data processing
The content of burn off is calculated based on the burn off mass fraction (wLOI) using formula (2).
Where, m3 - the mass of the processed platinum crucible, in grams (g); m4 - the mass of pre-dried specimen at 300 °C, in grams (g); m5 - the total mass of the platinum crucible and specimen after being burned at 1000 °C, in grams (g).
The calculation result is expressed to two decimal places. Numerical rounding shall be carried out in accordance with the provisions of GB/T 8170.
6.2 Air balance water calibration method
6.2.1 Principle
Weigh two specimens that have been equilibrated with air. Dry an air equilibrium specimen at a temperature of 300 °C±5 °C for 2 h to determine the air equilibrium moisture. At the same time, another air balance specimen was burned at a temperature of 1000 °C±10 °C for 2 h to determine the burning amount. Calculate burn loss using air balance moisture data and calibration formula.
6.2.2 Specimens
Place the original alumina specimen (5.2) in a plate (4.8), spread it evenly, and equilibrate it in the air in the laboratory for no less than 2 h (follow the instructions in Annex B). When using the air balance water calibration method to determine burn loss, the same batch of air balance specimens shall be used for measuring moisture at 300 °C and burning at 1000 °C.
6.2.3 Test steps
6.2.3.2 Determination of moisture content at 300 °C in air balance specimens Operate according to section 5.3.2.Preprocess weighing vessels (4.2 or 4.7) at a temperature of 300 °C. Add 5 g ±0.5 g of specimen (6.2.2) to the preprocessed weighing vessel. According to the operation in section 5.3.3 and formula (1) in 5.4, calculate the moisture mass fraction (w air balance) of the air equilibrium specimen after drying at 300 °C.
6.2.3.1 Parallel test
Conduct two parallel tests. Take the average value.
6.2.3.3 Preparation of platinum crucible
Place the platinum crucible (4.2) into a 1000 °C±10 °C high-temperature furnace (4.4) and burn for 15 min. Take it out and let it cool slightly. Place in the dryer (4.1), cool for 10 min, and quickly weigh to the nearest 0.0001 g. Record the mass of the platinum crucible (m6).
7 Instrument analysis
7.2 Specimens
The specimen shall comply with the original specimen preparation and storage requirements in GB/T 6609.23.
7.3 Test steps
7.3.1 Parallel test
Conduct two parallel tests and take the average value.
7.3.2 Establish a moisture and burn loss analysis program
Turn on the instrument. Establish a moisture and burn loss analysis program according to the instrument instructions. Enter the name of the analysis program, the range of specimen weighing mass, and other information, set parameters such as temperature, heating rate, end conditions, and holding time, and edit the formula for calculating moisture and burn loss results. Save the analysis program. The time for the instrument to reach a room temperature of 300 °C shall not exceed 25 min. The time from 300 °C to 1000 °C shall not exceed 40 min.
7.3.3 Determination
7.3.3.1 Special crucible for testing with constant weight burning.
7.3.3.2 Select the required analysis program. Place a crucible of constant weight inside the instrument (see 7.3.3.1). Automatically weigh the empty crucible and record its mass. Take 3 g~6 g of alumina specimen (7.2) and place it in a crucible. The instrument automatically weighs and records the sample mass. Edit and set sample information to begin analysis and measurement.
7.3.3.3 The instrument heats up to 300 °C at the set rate, keeps warm and dries, and automatically weighs the crucible and specimen mass after drying. Calculate the moisture content of the specimen. For the specimen dried at 300 °C, heat it up to 1000 °C at the set rate, keep it warm and burn it, and automatically weigh the crucible and specimen mass after burning. Calculate the burn off of the specimen. The calculation result is expressed to two decimal places. Numerical rounding shall be carried out in accordance with the provisions of GB/T 8170.
8 Precision
8.1 Repeatability
The measured values of two independent test results obtained under repeatability conditions, within the range of the average values given below, shall not exceed the repeatability limit (r) given in Table 1, and the absolute difference between these two
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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 20 pages — is available in the English PDF.
Referenced standards
Normative references
Cited by
- GB/T 24487-2022Alumina
- GB/T 26824-2020Nanoscale alumina
- GB/T 6609.34-2009Chemical analysis methods and determination of physical performance of alumina -- Part 34: Method of calculating alumina content
- GB/T 6609.37-2009Alumina Chemical analysis methods and determination of physical performance -- Part 37: Determination of particle size less than 20μm particle content
- SN/T 2044-2008Rules for inspection of nano-alumina
Similar standards
Editions of GB/T 6609.2
| Edition | Title | Revision | Status |
|---|---|---|---|
| GB/T 6609.2-2022 | Chemical analysis methods and determination of physical performance of alumina—Part 2: Determination of loss of mass at 300 °C and 1000 °C | current edition | Current |
| GB/T 6609.2-2009 | Chemical analysis methods and determination of physical performance of alumina—Part 2: Determination of loss of mass at 300 °C and 1000 °C | previous edition | Superseded |
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Related Standards
GB/T 6609.23-2004 — Chemical analysis methods and determination of physical performance of alumina -- Preparation and storage of test samples
GB/T 8170-2008 — Rules of rounding off for numerical values & expression and judgement of limiting values
GB/T 6609.1-2018 — Chemical analysis methods and determination of physical performance of alumina—Part 1: Determination of trace elements content—Inductively coupled plasma atomic emission spectrometry method
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