GB/T 4633-2014 PDF English
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| GB/T 4633-2014 | English | 70 |
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Determination of fluorine in coal
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| GB/T 4633-1997 | English | 279 |
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Determination of fluorine in coal
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| GB/T 4633-1984 | English | RFQ |
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Determination of fluorine in coal
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GB/T 4633-2014: Determination of fluorine in coal---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/GBT4633-2014
ICS 73.040
D 21
GB
National Standard
of the People’s Republic of China
GB/T 4633-2014
Replacing GB/T 4633-1997
Determination of fluorine in coal
Issued on. JUNE 09, 2014
Implemented on. OCTOBER 01, 2015
Issued by. General Administration of Quality Supervision, Inspection
and Quarantine;
Standardization Administration Committee.
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Method abstract... 4
4 Reagents and materials... 4
5 Apparatus and device... 6
6 Coal combustion temperature hydrolysis... 8
7 Potential measurement... 9
8 Results presentation... 10
9 Precision of methods... 11
10 Test report... 11
Foreword
This Standard is drafted according to the rules of GB/T 1.1-2009.
This Standard replaces GB/T 4663-1997 Determination of fluorine in coal. Compared
with GB/T 4663-1997, the major changes of this standard are as follows.
- ADD normative references (see Chapter 2);
- ADD result reports (see Chapter 10);
- MODIFY the calculation formula of fluorine content in coal;
This Standard was proposed by China National Coal Association.
This Standard shall be centralized by National Coal Standardization Technical
Committee of China (SAC/TC 42).
Drafting organization of this Standard. China Coal Research Institution Testing
Research Branch.
The main drafters of this standard. Yang Yuhua, Shi Mingzhi, and Li Ting.
The previous versions replaced by this Standard are.
- GB/T 4663-1984; GB/T 4663-1997.
Determination of Fluorine in Coal
1 Scope
This Standard specifies the method abstract, reagents and materials, apparatus and
device, measurement steps, result calculation, method precision, and test reports of
using high temperature combustion hydrolysis - fluoride ion selective electrode
(abbreviated as. fluoride electrode) method to determine the fluorine content in coal.
This Standard applies to lignite, bituminous coal, and anthracite.
2 Normative references
The following documents are essential for the application of this document. For dated
references, only the dated editions apply to this document. For undated references,
the latest editions (including all corrections) of the referenced documents apply to this
document.
GB/T 483 General rules for analytical and testing methods of coal
GB/T 6682 Water for analytical laboratory use - specification and test methods
3 Method abstract
Samples of coal are burned and hydrolyzed in the mixed gas stream of oxygen and
vapor.
4 Reagents and materials
Unless otherwise indicated, it shall only use the analytic reagents and distilled water
that are confirmed qualified, or deionized water, or water with equivalent purity.
4.1 Water. GB/T 6682, Grade 2.
4.2 Silica sand (SiO2). Particle size is 0.5mm~1.0mm.
4.8 Fluorine standard stock solution. 1000µg/mL. Weigh 2.2101g of
guaranteed-reagent sodium fluoride, which has been dried at 120°C for 2 hours, into a
beaker. Add water to dissolve. Use water to wash it into a 1000 mL volumetric flask.
And dilute to the scale. Shake well. Store it in the plastic bottle that does not contain
fluorine as the stock solution for spare use.
4.9 Fluorine standard working solution. 100µg/mL, 250µg/mL, 500µg/mL. Use fluorine
standard working solution to respectively prepare 100µg/mL, 250µg/mL, and
500µg/mL of standard working solution. Store it in the plastic bottle that does not
contain fluorine for spare use.
4.10 Bromocresol green indicator. Ethanol solution, 10g/L. Weigh 1 g of
bromocresol green indicator to dissolve into 100mL of anhydrous ethanol.
4.12 Injection push rod. The mental rod with silicon stopper; the top is bent into
disc-shaped; and temperature resistance is above 1100°C.
4.13 One-mark volumetric flask. 100mL. Class A.
4.14 One-mark pipette. 1mL, 2mL, 5mL, and 10mL. Class A.
5 Apparatus and device
5.1 High temperature combustion hydrolysis device (Figure1)
5.1.1 High temperature furnace. It can heat to above 1100°C. It has (1100±10°C)
constant temperature zone of 80mm~90mm long. And it is equipped with an
automatic temperature controller.
5.1.2 Combustion tube. made by quartz. It can withstand the temperature above
1200°C. The specification and dimension are shown in Figure 2.
Unit. mm
Figure 2 Combustion tube
5.1.3 Condenser pipe. S-shaped. The specification and dimension are shown in
5.1.4 Flow meter. Measuring range is 1000mL/min. The minimum division value is
10mL/min.
5.2 Potential measurement device (Figure 4)
5.2.4 Digital ion meter. Input impedance is more than 1011Ω; the resolution rate is
0.1mV. The digital ion meters with similar performance can also be used.
5.3 Analytical balance
The minimum division value is 0.1mg.
6 Coal combustion temperature hydrolysis
6.1 Apparatus preparation
6.1.1 According to Figure 1, assemble the full set of apparatus. Connect the electric
circuit, gas circuit and cooling waterway. Squeeze a few refractory wool in air outlet of
combustion tube.
6.1.2 Add 300mL of water into the flat-bottomed flask. And heat to a boil. Open the
condenser pipe to cool the water. Stuff up the silicon stopper of injection push rod.
Access the oxygen into the flat-bottomed flask before the water is boiled. Adjust the
oxygen flow to 400mL/min.
6.2 Combustion and hydrolysis
6.2.1 Weigh (0.50±0.01) g of general-analysis test coal (accurate to 0.1mg) and 0.5g
of quartz. Place in porcelain boat uniformly and carefully. Then cover it with about 0.5g
of quartz.
6.2.2 Place 100mL volumetric flask under the condenser pipe to receive condensate.
Access in oxygen and water vapor. Take down the injection push rod. Place the
porcelain boat into combustion tube. Insert the injection push rod. Stuff with silicon
stopper. Push the front-end of the porcelain boat to the 300°C zone where has been
measured in advance for 5 min.
6.2.3 Add 3 drops of bromocresol green indicator into volumetric flask which contains
condensate. Then neutralize it with sodium hydroxide solution until it turns to blue.
Add 10mL of total ionic strength adjustment buffer solution. Dilute it to the scale with
water.
7 Potential measurement
7.1 Preparation of titration
Add a certain amount of water into 100mL beaker. Connect the device of potential
measurement according to Figure 4.
7.2 Determination of actual slope for the fluoride electrode
7.2.1 Respectively, add 1mL, 3mL, 5mL, 7mL, 10mL of 100µm/mL fluoride standard
working solution into 5 100mL washed volumetric flasks. Add 3 drops of
bromocresol green indicator and 100mL of total ion strength buffered solution. Use
water to dilute to the scale. Shake well. Stand for 30min.
7.3 Potential measurement of sample solution
Transfer the prepared sample solution into a 100mL beaker. Place stirrer in it. Insert
the fluoride electrode and saturated calomel electrode (the insertion depth and stirring
speed shall be consistent with when measuring the actual slope of fluoride electrode).
8 Results presentation
8.1 Fluorine content in coal (Fad) shall be calculated according to Formula (1). The
determination result is rounded to the integer.
8.2 The fluorine content in coal shall be based on the average value of 2-times
repeated determination results. It shall be rounded to integer according to GB/T 483.
9 Precision of methods
Repeatability limit and reproducibility critical difference of determination results for
fluorine in coal is specified in Table 1.
10 Test report
Test report shall at least contain the following information.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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