YS/T 509.5-2008 PDF English
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Methods for Chemical Analysis of Spodumene and Lepidolite Concentrates - Determination of ferric oxide content - O-phenanthroline photometric method and EDTA compleximetric method
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| YS/T 509.5-2006 | English | 199 |
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Methods for chemical analysis of spodumenite and lepidolite concentrates - The EDTA volumetric method for the determination of ferric oxide content
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YS/T 509.5-2008: Methods for Chemical Analysis of Spodumene and Lepidolite Concentrates - Determination of ferric oxide content - O-phenanthroline photometric method and EDTA compleximetric 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/YST509.5-2008
YS
NONFERROUS METALS INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 64
Replacing YS/T 509.5-2006, YS/T 509.6-2006
Methods for chemical analysis of spodumene and
lepidolite concentrates - Determination of ferric oxide
content - O-phenanthroline photometric method and
EDTA compleximetric method
ISSUED ON: MARCH 12, 2008
IMPLEMENTED ON: SEPTEMBER 1, 2008
Issued by: National Development and Reform Commission of China
Table of Contents
Foreword ... 3
Method 1: O-phenanthroline photometric method ... 5
1 Scope ... 5
2 Method summary ... 5
3 Reagents ... 5
4 Instruments ... 6
5 Specimen ... 6
6 Analysis steps ... 6
7 Calculation of analysis result ... 8
8 Precision ... 8
9 Quality assurance and control ... 9
Method 2: EDTA compleximetric method ... 9
10 Scope ... 9
11 Method summary ... 9
12 Reagents ... 9
13 Specimen ... 10
14 Analysis steps ... 11
15 Calculation of analysis result ... 11
16 Precision ... 12
17 Quality assurance and control ... 13
Methods for chemical analysis of spodumene and
lepidolite concentrates - Determination of ferric oxide
content - O-phenanthroline photometric method and
EDTA compleximetric method
Method 1: O-phenanthroline photometric method
1 Scope
This Part specifies the determination methods for ferric oxide content in
spodumene, lepidolite concentrates.
This Part is applicable to the determination of ferric oxide content in spodumene,
lepidolite concentrates. Determination range: 0.10%~1.00%.
2 Method summary
The specimen is melted with potassium hydroxide. Use water to leach. Use
hydrochloric acid to acidify. Use ascorbic acid to reduce ferric iron to divalent
iron. At pH3～pH6, divalent iron forms orange-red complex with phenanthroline.
At a wavelength of 506nm of the spectrophotometer, measure its absorbance.
3 Reagents
Unless otherwise stated, only the confirmed analytically-pure reagents and
distilled water or water of comparable purity are used in the analysis.
3.1 Potassium hydroxide.
3.2 Absolute ethanol.
3.3 Hydrochloric acid (1+1).
3.4 Hydrochloric acid (1+7).
3.5 Ammonium hydroxide (1+1).
6.3 Blank test
Conduct blank test with test material.
6.4 Determination
6.4.1 Place the test material (6.1) in a 30mL silver crucible. Add 3 drops of
absolute ethanol (3.2) to moisten. Add 5g of potassium hydroxide (3.1). Put the
lid on the crucible and leave a little gap. Remove the moisture on an electric
stove. Place in 600°C~650°C high temperature furnace to melt for
10min~15min. Take out. Cool.
6.4.2 Use filter paper to wipe the outer wall of the crucible. Put it in a 250mL
beaker. Add 100mL of hot water. Cover the watch glass. Leach the melt. Add
35mL of hydrochloric acid (3.3) from the mouth of the beaker at a time. Shake
immediately to totally acidify the solution. Use hot water to wash out the crucible.
Boil the solution for 1min~2min. Cool to room temperature. Transfer into a
250mL volumetric flask. Use water to dilute to the graduation of scale. Mix well.
Let it stand. Pipette 25.00mL of supernatant. Place it in a 100mL volumetric
flask.
6.4.3 Add 5mL of ascorbic acid solution (3.7). Mix well. Add 2 drops of p-
nitrophenol ethanol solution (3.11). Use ammonium hydroxide (3.5) to
neutralize until the solution just turns yellow. Then use hydrochloric acid (3.4)
to neutralize until the yellow color just disappears. Add 20mL of buffer solution
(3.8). Mix well. Add 2.5mL of o-phenanthroline ethanol solution (3.6). Use water
to dilute to the graduation of scale. Mix well. Let it stand for 15min.
6.4.4 Move part of the solution (6.4.3) into a 2cm cuvette. Take the blank of the
accompanying specimen as a reference. At a wavelength of 506nm of the
spectrophotometer, measure its absorbance. Find the corresponding amount of
ferric oxide from the working curve.
6.5 Drawing of working curve
6.5.1 Pipette 0mL, 1.00mL, 2.00mL, 5.00mL, 7.00mL, 10.00mL, 12.00mL and
15.00mL of ferric oxide standard solution (3.10). Respectively put in a set of
100mL volumetric flasks. Add 1mL of hydrochloric acid (3.3). The rest follows
the steps in 6.4.3.
6.5.2 Transfer part of the solution (6.5.1) into a 2cm cuvette. Take the
accompanying reagent blank as a reference. At a wavelength of 506nm of the
spectrophotometer, measure its absorbance. Use the amount of ferric oxide as
the abscissa and absorbance as the ordinate to draw a working curve.
9 Quality assurance and control
Use national standard samples or industry-standard samples (control samples
can also be used if the two are not available) to check the validity of the
analytical method standard weekly or every two weeks. When the process goes
out of control, find out the cause, correct it, and recheck it.
Method 2: EDTA compleximetric method
10 Scope
This Part specifies the determination methods for ferric oxide content in
spodumene, lepidolite concentrates.
This Part is applicable to the determination of ferric oxide content in spodumene,
lepidolite concentrates. Determination range: 1.00%~10.00%.
11 Method summary
The specimen is melted with potassium hydroxide. Use water to leach. In an
acidic solution of pH1.5~pH2.0, use sulfosalicylic acid as indicator. Use EDTA
standard solution to titrate. Determine the content of ferric oxide.
12 Reagents
Unless otherwise stated, only the confirmed analytically-pure reagents and
distilled water or water of comparable purity are used in the analysis.
12.1 Potassium hydroxide.
12.2 Ammonium persulfate.
12.3 Absolute ethanol.
12.4 Hydrochloric acid (1+1).
12.5 Ammonium hydroxide (1+1).
12.6 Ferric oxide standard solution: Weigh 0.5000g of ferric oxide (above 99.9%)
that has been pre-baked at 105°C~110°C for 2h and placed in a desiccator to
cool to room temperature. Put it in a 250mL beaker. Add 30mL of hydrochloric
acid (12.4). Cover the watch glass. Heat at low temperature to dissolve
completely. Remove. Cool to room temperature. Transfer to 1000mL volumetric
desiccator to cool to room temperature.
14 Analysis steps
14.1 Test material
Weigh 0.50g of specimen, to the nearest of 0.0002g.
14.2 Number of determinations
Make parallel determinations of two test materials. Take the average value.
14.3 Blank test
Conduct blank test with test material.
14.4 Determination
14.4.1 Place the test material (14.1) in a 30mL silver crucible. Add 5 drops of
absolute ethanol (12.3) to moisten. Add 5g of potassium hydroxide (12.1). Put
the lid on the crucible and leave a little gap. Remove moisture on an electric
stove. Place in 600°C~650°C high temperature furnace to melt for
10min~15min. Take out. Cool.
14.4.2 Use filter paper to wipe the outer wall of the crucible. Put it in a 250mL
beaker. Cover the watch glass. Add 100mL of hot water from the mouth of the
beaker. Leach the melt. Then add 35mL of hydrochloric acid (12.4) at a time.
Immediately shake to acidify the solution. Use hot water to wash out the crucible.
Boil the solution for 2min. Cool to room temperature.
14.4.3 Transfer the solution (14.4.2) into a 250mL volumetric flask. Use water
to dilute to the graduation of scale. Mix well. Let it stand.
14.4.4 Pipette 50.00mL of supernatant (14.4.3). Put it in a 300mL Erlenmeyer
flask. Add 0.1g of ammonium persulfate (12.2). Heat to slightly boil and keep it
for 5min. Cool for a while. Add 6 drops of sulfosalicylic acid solution (12.8). Use
ammonium hydroxide (12.5) to neutralize until the purple disappears and
brownish red appears. Immediately use hydrochloric acid (12.4) to carefully
neutralize until the purple color just appears and exceed by 4 drops. Control the
temperature of the solution at about 60°C. Use EDTA standard solution (12.7)
to slowly titrate until the purple color disappears as the end point.
15 Calculation of analysis result
The mass fraction of ferric oxide, w, whose value is expressed in %, is
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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