GB/T 6609.1-2018 PDF English
US$205.00 · In stock · Download in 9 secondsGB/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 Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedureStatus: Valid GB/T 6609.1: Evolution and historical versions
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| GB/T 6609.1-2018 | English | 205 |
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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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| GB/T 6609.1-2004 | English | 199 |
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Chemical analysis methods and Determination of physical performance of alumina Determination of moisture -- Gravimetric method
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| GB/T 6609.1-1986 | English | 199 |
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Methods for chemical analysis of aluminium oxide--The gravimetric method for the determination of moisture
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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
---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/GBT6609.1-2018
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.10
H 12
Chemical analysis methods and determination of physical
performance of alumina - Part 1.Determination of trace
elements content - Inductively coupled plasma atomic
emission spectrometry method
Issued on: MAY 14, 2018
Implemented on: FEBRUARY 01, 2019
Issued by. State Administration for Market Regulation;
Standardization Administration of the People's Republic of China.
Table of Contents
Foreword... 3
1 Scope... 6
2 Method summary... 6
3 Reagents... 7
4 Instruments... 8
5 Specimens... 8
6 Analysis steps... 8
7 Calculation of analysis results... 11
8 Precision... 11
9 Quality assurance and control... 12
10 Test report... 12
Annex A (normative) Preparation of standard stock solutions... 14
Annex B (normative) PTFE sealed sample analyzer... 17
Chemical analysis methods and determination of physical
performance of alumina - Part 1.Determination of trace
elements content - Inductively coupled plasma atomic
emission spectrometry method
1 Scope
This Part of GB/T 6609 specifies the method for the determination of trace element
content in metallurgical grade alumina (expressed as oxides. Na2O, K2O, Fe2O3, CuO,
MgO, CaO, ZnO, V2O5, TiO2, Ga2O3, MnO, Li2O, BeO, Cr2O3, B2O3).
This Part applies to the determination of trace element content in metallurgical grade
alumina. The determination range is shown in Table 1.
2 Method summary
Place the test material in a polytetrafluoroethylene-sealed dissolver. Dissolve it in
hydrochloric acid at a constant temperature (dissolution method I), or place the test
material in a microwave digestion system and digest it with sulfuric acid at high
temperature and high pressure (dissolution method II). Introduce the test solution into
an inductively coupled plasma spectrometer. Excite it with an argon plasma light source
and measure the spectrum. Correct for matrix effects on the measurement using the
matrix matching method.
3 Reagents
Unless otherwise stated, only confirmed guaranteed reagents and grade 1 water are used
in the analyses.
3.1 Sulfuric acid (1+1).
3.2 Hydrochloric acid (1+1).
3.3 Sulfuric acid (1+2).
3.4 Hydrochloric acid (3+1).
3.5 Aluminum, w (Al) ≥99.999%. Pre-wash with a small amount of concentrated nitric
acid, then wash with water to remove the nitric acid, rinse twice with anhydrous ethanol
or acetone, and dry.
3.6 Alumina matrix solution (20 mg/mL).
3.6.1 Matrix Solution I. Weigh 5.288 g of aluminum (3.5) into a 1000 mL beaker. Cover
with a watch glass. Add 300 mL of hydrochloric acid (3.2) in portions. After the violent
reaction subsides, slowly heat until completely dissolved. Add a few drops of hydrogen
peroxide (ρ = 1.10 g/mL). Boil for several minutes. Cool. Transfer the solution to a 500
mL volumetric flask. Dilute to the mark with water. Shake well. Store in a polyethylene
bottle.
3.6.2 Matrix Solution II. Weigh 5.288 g of aluminum (3.5) into a 1000 mL beaker.
Cover with a watch glass. Add 330 mL of sulfuric acid (3.1) in portions. Slowly heat
until completely dissolved. Cool. Transfer the solution to a 500 mL volumetric flask.
Dilute to the mark with water. Shake well. Store in a polyethylene bottle.
4 Instruments
4.1 Inductively coupled plasma atomic emission spectrometer.
4.2 Microwave digester.
4.3 Polytetrafluoroethylene sealed sample dissolver. See Annex B for a diagram of the
device.
4.4 Oven. rated temperature is not less than 350°C, temperature control accuracy is
±3°C.
4.5 Desiccant. use new activated alumina as the desiccant.
5 Specimens
5.1 The specimens should be able to pass through a 0.125 mm standard sieve.
5.2 The specimen is dried in an oven (4.4) at 300°C ± 3°C for 2 h and then placed in a
desiccator (4.5) to cool to room temperature.
6 Analysis steps
6.1 Test material
Weigh the specimens (5) according to Table 2 to the nearest 0.0001 g.
6.2 Number of determinations
The determinations are performed twice independently. Take the average value.
6.3 Blank test
Carry out a blank test along with the test material (6.1).
6.4 Preparation of analytical solution
6.4.1 Sample dissolution method I
Weigh the test material (6.1) according to Table 2 and place it in a 100 mL
polytetrafluoroethylene reaction cup. Add 10 mL of hydrochloric acid (3.4). Cover the
polytetrafluoroethylene reaction cup. Place in a polytetrafluoroethylene sealed sample
dissolver (4.3). Place in an oven (4.4). Insulate at 240°C ± 3°C for 5 h. Remove. Cool
to room temperature. Transfer the solution to a volumetric flask of the corresponding
volume as shown in Table 2.Rinse the reaction cup with water. Combine the wash
solution in the volumetric flask. Dilute to the mark with water. Mix thoroughly.
6.4.2 Sample dissolution method II
Weigh the test material (6.1) according to Table 2 and place it in a 100 mL microwave
digestion reaction cup. Add 10 mL of sulfuric acid (3.3). Cover the reaction cup lid and
place it in the microwave digestion apparatus. Dissolve under the selected microwave
digestion optimal measurement procedure. After the test material is completely
dissolved, cool it to room temperature. Transfer into a 100 mL volumetric flask. Wash
the reaction cup with water. Wash the liquid into a volumetric flask. Dilute with water
to the mark. Mix well. This method is not applicable for the determination of CaO
content.
6.5 Preparation of series standard solutions
6.5.1 Sample dissolution method I
According to the amount of alumina in the test solution, transfer an appropriate amount
of aluminum matrix solution (3.6.1) into a set of 100 mL volumetric flasks, so that the
amount of alumina in the standard solution is basically the same as that in the test
solution. According to the mass fraction of each element in the sample, add an
appropriate amount of standard solution (3.8.1) or (3.8.2) of the element to be tested,
so that the type and acidity of the acid in the standard solution are basically the same as
those in the test solution. Dilute with water to the mark. Mix well. Store in polyethylene
bottles. Use the test solution without standard solution as the blank solution, so that the
content of the tested element should be within the range of the working curve. The
number of standard solutions in the series shall not be less than 5.The mass fractions
of each element should be distributed as evenly as possible.
6.5.2 Sample dissolution method II
According to the amount of alumina in the test solution, transfer an appropriate amount
of aluminum matrix solution (3.6.2) into a set of 100 mL volumetric flasks, so that the
amount of alumina in the standard solution is basically the same as that in the test
solution. According to the mass fraction of each element in the sample, add an
appropriate amount of standard solution (3.8.1) or (3.8.2) of the element to be tested,
so that the type and acidity of the acid in the standard solution are basically the same as
those in the test solution. Dilute with water to the mark. Mix well and store in a
polyethylene bottle. Use the test solution without standard solution as the blank solution,
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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