GB/T 4698.22-2017Methods for chemical analysis of titanium sponge,titanium and titanium alloys—Part 22: Determination of niobium content—5-Br-PADAP spectrophotometry and inductively coupled plasma atomic emission spectrometry (English PDF)
海绵钛、钛及钛合金化学分析方法 第22部分：铌量的测定 5-Br-PADAP分光光度法和电感耦合等离子体原子发射光谱法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
September 29, 2017
Implementation date
July 1, 2018
Scope
GB/T 4698.22-2017 is the English-translated version of 海绵钛、钛及钛合金化学分析方法 第22部分：铌量的测定 5-Br-PADAP分光光度法和电感耦合等离子体原子发射光谱法.
GB/T 4698.22-2017 is Part 22 of GB/T 4698, a series of 28 parts on the chemical analysis of titanium sponge, titanium and titanium alloys, and it covers the determination of niobium content by 5-Br-PADAP spectrophotometry and by inductively coupled plasma atomic emission spectrometry.
Clause 1 states that the part applies to the determination of niobium in titanium sponge, titanium and titanium alloys, with a range of 0.10% to 3.20% for the first method and 0.10% to 16.00% for the second.
The first method, which the page marks as the arbitration method, is 5-Br-PADAP spectrophotometry: the sample is dissolved in sulfuric acid and, in the presence of tartaric acid and EDTA, niobium forms a coloured complex with 5-Br-PADAP in an acidic medium whose absorbance is measured at a wavelength of 610 nm on a spectrophotometer.
Its reagent clause sets out nitric acid, sulfuric acid, two tartaric acid solutions, ammonia, an EDTA solution, the 5-Br-PADAP ethanol solution at 0.3 g/L, a titanium matrix solution and the niobium standard stock and working solutions down to 10 micrograms of niobium per millilitre, and its instrument clause calls for a spectrophotometer.
The draft on the page breaks off there, so the clauses of the second method are not shown.
The foreword records that the original method was kept with its range widened from 0.20% to 3.00% to 0.10% to 3.20% and precision and test report provisions added, and that inductively coupled plasma emission spectrometry was added with a niobium range of 0.10% to 16.00%; it also names the China Nonferrous Metal Industry Association as proposer and SAC/TC243 as the committee in charge.
It replaces GB/T 4698.22-1996, was issued on 29 September 2017 and has applied since 1 July 2018.
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Document preview — GB/T 4698.22-2017
National Standard of the People's Republic of China
- ICS
- 77.120.50
- Classification
- H 14
- Replacing
- GB/T 4698.22-1996
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword
- 1 Scope
- 2 Method One (Arbitration method) 5-Br-PADAP spectrophotometry
Foreword
GB/T 4698 "titanium sponge, titanium and titanium alloy chemical analysis method" is divided into 28 parts.
--- Part 1. Determination of copper content by flame atomic absorption spectrometry;
--- Part 2. Determination of iron content 1,10-phenanthroline spectrophotometry, flame atomic absorption spectrometry and inductively coupled plasma Atomic emission spectrometry;
--- Part 3. Determination of silicon content molybdenum blue spectrophotometry;
--- Part 4. Determination of manganese content Periodate spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 5. Determination of molybdenum content thiocyanate spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 6. Determination of boron content Curcumin spectrophotometry and inductively coupled plasma mass spectrometry;
--- Part 7. Determination of oxygen content, nitrogen content Inert gas melting - infrared absorption/thermal conductivity method and distillation separation - Naisler reagent spectrophotometry Degree method
--- Part 8. Determination of aluminum content Alkaline separation - EDTA complexometric titration and inductively coupled plasma atomic emission spectrometry;
--- Part 9. Determination of tin content potassium iodate titration and inductively coupled plasma atomic emission spectrometry;
--- Part 10. Determination of chromium content ammonium ferrous sulfate titration and inductively coupled plasma atomic emission spectrometry;
--- Part 12. Determination of vanadium content ammonium ferrous sulfate titration and inductively coupled plasma atomic emission spectrometry;
--- Part 13. Determination of zirconium content EDTA titration and inductively coupled plasma atomic emission spectrometry;
--- Part 14. Determination of carbon content High-frequency combustion - infrared absorption method;
--- Part 15. Determination of hydrogen content inert gas melting infrared absorption method/thermal conductivity method;
--- Part 17. Determination of magnesium content by flame atomic absorption spectrometry;
--- Part 18. Determination of tin content by flame atomic absorption spectrometry;
--- Part 19. Determination of molybdenum content; Thiocyanate differential spectrophotometry;
--- Part 21. Determination of multi-element impurity content of atomic emission spectrometry;
--- Part 22. Determination of niobium content 5-Br-PADAP spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 23. Determination of palladium content Stannous chloride - potassium iodide spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 24. Determination of nickel content dimethylglyoxime spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 25. Determination of chlorine content of silver chloride spectrophotometry;
--- Part 26. Determination of tungsten and tantalum content by inductively coupled plasma atomic emission spectrometry;
--- Part 27. Determination of neodymium content by inductively coupled plasma atomic emission spectrometry;
--- Part 28. Determination of ruthenium content Inductively coupled plasma atomic emission spectrometry.
This section GB/T 4698 Part 22.
This section drafted in accordance with GB/T 1.1-2009 given rules.
This Part replaces GB/T 4698.22-1996 "titanium sponge, titanium and titanium alloy chemical analysis 5-Br-PADAP spectrophotometry Measuring the amount of niobium. " This section compared with GB/T 4698.22-1996 main changes are as follows.
--- Remain the original method, the determination of the scope of the original 0.20% ~ 3.00% expanded to 0.10% ~ 3.20%, adding the precision and test report Terms.
--- Added inductively coupled plasma emission spectrometry, niobium determination range of 0.10% ~ 16.00%.
1 Scope
GB/T 4698 provisions of this section sponge titanium, titanium and titanium alloy niobium determination.
This section applies to the determination of niobium in titanium sponge, titanium and titanium alloys. Determination of the scope of a method of 0.10% to 3.20%; method two 0.10% ~ 16.00%.
2 Method One (Arbitration method) 5-Br-PADAP spectrophotometry
2.1 Method summary
The sample is dissolved in sulfuric acid. In the presence of tartaric acid and EDTA, niobium forms a colored complex with 5-Br-PADAP in an acidic medium The absorbance was measured at a wavelength of 610 nm on a spectrophotometer.
2.2 Reagents
Unless otherwise specified, only reagents that are identified as analytically pure and laboratory-grade water are used in the analysis.
2.2.1 Nitric acid (p = 1.42 g/mL).
2.2.2 Sulfuric acid (1 1).
2.2.3 Tartaric acid solution (240g/L).
2.2.4 Tartaric acid solution (60g/L).
2.2.5 Ammonia (1 1).
2.2.6 Sulfuric acid (5 95).
2.2.7 EDTA (C10H14N2O8Na2 H2O) solution (100g/L).
2.2.8 5-Br-PADAP (2- (5-Br-2-pyridylazo) -5-diethylaminophenol) ethanol solution (0.3 g/L).
2.2.9 Titanium matrix solution Weigh 0.10g titanium metal (wTi >= 99.95%, wNb < 0.001%) in 100mL beaker was added 10mL Sulfuric acid (2.2.2) dissolved by heating, dropping nitric acid (2.2.1) to the solution purple disappeared, heating was continued to the solution just take sulfuric acid smoke, cooling, 200mL volumetric flask, diluted with water to the mark, mix well. This solution 1 mL contains 0.5 mg of titanium.
2.2.10 Niobium standard stock solution Weigh 0.7153g niobium pentoxide (wNb2O5 >= 99.95%) in a platinum crucible, add 10g pyrosulfuric acid Potassium was heated on a torch to melt and cool, cooled, leached with a hot tartaric acid solution (100 g/L), placed in a 500 mL beaker, Stir under stirring to clarify, cooled, transferred to 500mL volumetric flask, tartaric acid solution (100g/L) diluted to the mark, and mix. this 1 mL of solution contains 1.0 mg of niobium.
2.2.11 Niobium standard solution Pipette 10.00mL niobium standard stock solution (2.2.10), placed in 1000mL volumetric flask to tartaric acid solution (2.2.4) diluted to the mark, mix well. 1 mL of this solution contains 10 µg of niobium.
2.2.12 P-nitrophenol solution (1g/L).
2.3 Instruments
Spectrophotometer.
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
Referenced standards
Normative references
GB/T 4698
Similar standards
Editions of GB/T 4698.22
| Edition | Title | Revision | Status |
|---|---|---|---|
| GB/T 4698.22-2017 | Methods for chemical analysis of titanium sponge,titanium and titanium alloys—Part 22: Determination of niobium content—5-Br-PADAP spectrophotometry and inductively coupled plasma atomic emission spectrometry | current edition | Current |
| GB/T 4698.22-1996 | Methods for chemical analysis of titanium sponge,titanium and titanium alloys—Part 22: Determination of niobium content—5-Br-PADAP spectrophotometry and inductively coupled plasma atomic emission spectrometry | previous edition | Superseded |
This page sells the current edition, GB/T 4698.22-2017. Earlier editions are listed for reference only.
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Related Standards
GB/T 4698.1-2017 — Methods for chemical analysis of titanium sponge, titanium and titanium alloys - Part 1: Determination of copper content - Flame atomic absorption spectrometry
GB/T 4698.10-2020 — Methods for chemical analysis of titanium sponge, titanium and titanium alloys - Part 10: Determination of chromium content - Ammonium ferrous sulfate titration and inductively coupled plasma atomic emission spectrometry (with vanadium)
GB/T 4698.11-1996 — Sponge titanium，titanium and titanium alloys--Determination of chromium content in the absence of Vanadium--Ammonium ferrous sulfate titration method
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