GB/T 13747.6-2019 English PDF (GBT13747.6-2019)

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GB/T 13747.6-2019: Methods for Chemical Analysis of Zirconium and Zirconium Alloys -- Part 6: Determination of Copper Content - 2,9-Dimethyl-1,10-phenanthroline Spectrophotometry
GB/T 13747.6-2019
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 14
Replacing GB/T 13747.6-1992
Methods for Chemical Analysis of Zirconium and
Zirconium Alloys - Part 6: Determination of Copper
Content - 2,9-Dimethyl-1,10-phenanthroline
Spectrophotometry
ISSUED ON: JUNE 4, 2019
IMPLEMENTED ON: JANUARY 1, 2020
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 Principle ... 6 
3 Reagents ... 6 
4 Instrument and Equipment ... 7 
5 Samples ... 7 
6 Test Procedures ... 7 
7 Test Data Processing ... 8 
8 Precision ... 9 
9 Test Report ... 10 
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 - Chronic 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 6: Determination of Copper
Content - 2,9-Dimethyl-1,10-phenanthroline
Spectrophotometry
1 Scope
This Part of GB/T 13747 stipulates the determination method of copper content in
zirconium and zirconium alloys.
This Part is applicable to the determination of copper content in zirconium sponge,
zirconium and zirconium alloys. The range of determination is: 0.0010% ~ 0.025%.
2 Principle
Use hydrofluoric acid to dissolve specimen. Use tartaric acid to form zirconium
complex. Use hydroxylamine hydrochloride to reduce copper into cuprous ion state. At
pH 4 ~ 6, use trichloromethane to extract copper and colored complex, which is formed
with 2,9-dimethyl-1,10-phenanthroline. At the wavelength of 460 nm, use a
spectrophotometer to measure its absorbance.
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 Hydrofluoric acid ( = 1.15 g/mL, excellent grade of purity).
3.2 Nitric acid ( = 1.42 g/mL, excellent grade of purity).
3.3 Trichloromethane.
3.4 Absolute ethanol.
3.5 Ammonia water (1 + 1).
3.6 Boric acid saturated solution.
3.7 Tartaric acid solution (200 g/L).
6.2 Parallel Test
Conduct two parallel tests. Take the average value.
6.3 Blank Test
Conduct blank test of the accompanying specimen.
6.4 Determination
6.4.1 Place the specimen (6.1) in a 100 mL plastic beaker, then, add 15 mL of water.
Add 2 mL of hydrofluoric acid (3.1) in several times. Wait till the specimen completely
dissolves, then, respectively add 1 mL of nitric acid (3.2), 25 mL of boric acid saturated
solution (3.6) and 10 mL of tartaric acid solution (3.7). Use ammonia water (3.5) to
adjust the pH of the solution to be 4 ~ 6. Then, transfer it into a 100 mL volumetric flask.
Use water to dilute to the scale, then, shake it up. Transfer-take 20.00 mL of test
solution, then, place it in a 100 mL separating funnel.
6.4.2 Add 5 mL of hydroxylamine hydrochloride solution (3.8), then, place it for 15 min.
Add 10.0 mL of neocuproine ethanol solution (3.9); add 10.0 mL of trichloromethane
(3.3). Conduct extraction for 30 s. After placing it still for stratification, transfer the
organic phase into a dry 25 mL colorimetric tube. Add 3.0 mL of absolute ethanol (3.4),
then, mix it up.
6.4.3 Transfer part of the organic phase into a 2 cm absorption vessel. Take the blank
solution of the accompanying specimen as a reference. At the wavelength of 460 nm,
use a spectrophotometer to measure its absorbance. Obtain the corresponding copper
content through working curve.
6.5 Draw a Working Curve
6.5.1 Accurately transfer-take 0 mL, 0.20 mL, 0.50 mL, 1.00 mL, 1.50 mL and 2.00 mL
of copper standard solution (3.11). Respectively place them in a group of 100 mL
separating funnels. Add 5 mL of boric acid saturated solution (3.6), 0.4 mL of
hydrofluoric acid (3.1) and 2 mL of tartaric acid solution (3.7). Use ammonia water (3.5)
to adjust the pH of the solution to be 4 ~ 6; add water to 20 mL. The following analytical
procedures shall comply with 6.4.2.
6.5.2 Transfer part of the organic phase into a 2 cm absorption vessel. Take reagent
blank as a reference. At the wavelength of 460 nm, use a spectrophotometer to
measure its absorbance. Take copper content as the x-coordinate; take its absorbance
as the y-coordinate; draw a working curve.
7 Test Data Processing
Copper content, which is counted by the mass fraction of copper wCu, shall be