GB/T 13747.6-2019 PDF English

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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
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GB/T 13747.6: Historical versions

Standard ID	USD	BUY PDF	Delivery	Standard Title (Description)	Status
GB/T 13747.6-2019	90	Add to Cart	Auto, 9 seconds.	Methods for Chemical Analysis of Zirconium and Zirconium Alloys - Part 6: Determination of Copper Content - 2,9-Dimethyl-1,10-phenanthroline Spectrophotometry	Valid
GB/T 13747.6-1992	179	Add to Cart	2 days	Zirconium and zirconium alloys. Determination of copper content. 2, 9-Dimethyl-1, 10-phenanthroline spectrophotometric method	Obsolete

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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

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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 ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.

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