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GB/T 13747.5-2019 English PDF (GBT13747.5-2019)

GB/T 13747.5-2019 English PDF (GBT13747.5-2019)

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GB/T 13747.5-2019: Methods for Chemical Analysis of Zirconium and Zirconium Alloys -- Part 5: Determination of Aluminum Content -- Chronic Azurol-S-tetradecylpyridine Chloride Spectrophotometry

This Part of GB/T 13747 stipulates the determination method of aluminum content in zirconium and zirconium alloys. This Part is applicable to the determination of aluminum content in zirconium sponge, zirconium and zirconium alloys. The range of determination is: 0.0025% ~ 0.10%.
GB/T 13747.5-2019
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 77.120.99
H 14
Replacing GB/T 13747.5-1992
Methods for Chemical Analysis of Zirconium and
Zirconium Alloys - Part 5: Determination of Aluminum
Content - Chronic Azurol-S-tetradecylpyridine
Chloride Spectrophotometry
ISSUED ON: JUNE 4, 2019
IMPLEMENTED ON: MAY 1, 2020
Issued by: State Administration for Market Regulation;
Standardization Administration of the PEOPLE Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 6
2 Principle ... 6
3 Reagents ... 6
4 Instrument and Equipment ... 8
5 Samples ... 8
6 Test Procedures ... 8
7 Test Data Processing ... 9
8 Precision ... 10
9 Test Report ... 11
Foreword
GB/T 13747 Methods for Chemical Analysis of Zirconium and Zirconium Alloys is 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 Spectrophotometric Method;
---Part 3: Determination of Nickel Content - Dimethylglyoxime Spectrophotometric Method;
---Part 4: Determination of Chromium Content - Diphenylcarbazide
Spectrophotometric Method;
---Part 5: Determination of Aluminum Content - Chrome Azurol-S-
tetradecylpyridine Chloride Spectrophotometry;
---Part 6: Determination of Copper Content - 2,9-Dimethyl-1,10-phenanthroline Spectrophotometry;
---Part 7: Determination of Manganese Content - Potassium Periodate
Spectrophotometric Method;
---Part 8: Determination of Cobalt Content - Nitroso-R-salt Spectrophotometry; ---Part 9: Determination of Magnesium Content - Flame Absorption Spectrometric Method;
---Part 10: Determination of Tungsten Content - Thiocyanate Spectrophotometric Method;
---Part 11: Determination of Molybdenum Content - Thiocyanate
Spectrophotometry;
---Part 12: Determination of Silicon Content - Molybdenum Blue
Spectrophotometric Method;
---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;
Methods for Chemical Analysis of Zirconium and
Zirconium Alloys - Part 5: Determination of Aluminum
Content - Chronic Azurol-S-tetradecylpyridine
Chloride Spectrophotometry
1 Scope
This Part of GB/T 13747 stipulates the determination method of aluminum content in zirconium and zirconium alloys.
This Part is applicable to the determination of aluminum content in zirconium sponge, zirconium and zirconium alloys. The range of determination is: 0.0025% ~ 0.10%. 2 Principle
Use sulfuric acid and ammonium sulfate to dissolve specimen. Use N-benzoyl-N- phenylhydroxylamine trichloromethane solution to extract and separate the main element zirconium, and interference elements: hafnium, iron and titanium. After the separation, use o-phenanthroline and ascorbic acid to mask the residual iron. In acetic acid-sodium acetate medium (pH 5.8), aluminum and chronic azurol-S-
tetradecylpyridine chloride form colored complex. At the wavelength of 630 nm, use a spectrophotometer to measure its absorbance. If the sample contains a small amount of uranium and thorium, sodium carbonate solution may be added during color- developing, so as to eliminate the influence.
3 Reagents
Unless it is otherwise stipulated, the analysis shall merely adopt reagents that are confirmed to be analytically pure and secondary laboratory water.
3.1 Ammonium sulfate (excellent grade of purity).
3.2 Sulfuric acid (??? = 1.84 g/mL, excellent grade of purity).
3.3 Nitric acid (??? = 1.42 g/mL, excellent grade of purity).
3.4 Hydrochloric acid (??? = 1.19 g/mL, excellent grade of purity).
3.5 Trichloromethane.
6.4.2 In accordance with Table 1, transfer-take the solution. Place it in a 100 mL separating funnel. Add 10 mL of N-benzoyl-N-phenylhydroxylamine trichloromethane solution (3.13); violently oscillate it for 2 min. After placing it still for stratification, discard the organic phase, then, repeat extraction for three times. Add 10 mL of trichloromethane (3.5); start oscillation for 0.5 min. After placing it still for stratification, discard the organic phase. Place the aqueous phase into a 50 mL beaker, then, use a small amount of water to rinse the separating funnel. Combine the rinsing solution into the beaker. Conduct low-temperature heating, till it emits white smoke. Then, take it down. While it is still hot, along the wall of the beaker, add 20 drops of nitric acid (3.3). Continue to heat it up, till it emits dense white smoke, then, take it down. Cool it down, then, along the wall of the beaker, add a small amount of water, then, mix it up. Use micro-heat to dissolve salt. After cooling it down, use water to transfer it into a 50 mL volumetric flask; the volume of the solution shall be around 15 mL.
6.4.3 Add 2 drops of 2, 4-dinitrophenol solution (3.11). Use ammonia water (3.7) to adjust it, till the solution turns yellow. Then, add drops of hydrochloric acid (3.6), till such yellow disappears. Add 2 mL of o-phenanthroline solution (3.9), then, shake it up. Add 2 mL of ascorbic acid solution (3.10), then, shake it up. Along the wall of the beaker, add 5.0 mL of azurol-S-tetradecylpyridine chloride solution (3.8), then, shake it up. Add 5 mL of acetic acid-sodium acetate buffer solution (3.12). Use water to dilute to the scale, then, shake it up.
6.4.4 After placing the solution for 20 min, transfer part of the solution into a 1 cm absorption vessel. Take the blank solution of the accompany specimen as a reference. At the wavelength of 630 nm, use a spectrophotometer to measure its absorbance. Through the working curve, find the corresponding aluminum content.
6.5 Draw a Working Curve
Accurately transfer-take 0 mL, 0.20 mL, 0.40 mL, 0.60 mL, 0.80 mL and 1.00 mL of aluminum standard solution B (3.16). Respectively place them in a group of 50 mL volumetric flasks. Add water to reach the volume of around 15 mL. The following analytical procedures shall comply with 6.4.3. After placing the solutions for 20 min, transfer them into 1 cm absorption vessel. Take reagent blank as a reference. At the wavelength of 630 nm, use a spectrophotometer to measure it. Take the aluminum content as the x-coordinate; take the absorbance as the y-coordinate; draw a working curve.
7 Test Data Processing
Aluminum content, which is counted by the mass fraction of aluminum wA1, shall be calculated in accordance with Formula (1):

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