GB/T 4698.21-2019Methods for chemical analysis of titanium sponge, titanium and titanium alloys—Part 21: Determination of manganese, chromium, nickel, aluminum, molybdenum, tin, vanadium, yttrium, copper and zirconium content—Atomic emission spectrometry (English PDF)

Foreword

GB/T 4698 "Methods for chemical analysis of titanium sponge, titanium and titanium alloys" consists of the following parts:

-- Part 1: Determination of copper content - Flame atomic absorption spectrometry;

-- Part 2: Determination of iron content;

-- Part 3: Determination of silicon content - Molybdenum blue spectrophotometry;

-- Part 4: Determination of manganese content-Potassium 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 - Methylene blue spectrophotometry and inductively coupled plasma atomic emission spectrometry;

-- Part 7: Determination of oxygen and nitrogen content;

-- Part 8: Determination of aluminum content - Separation with sodium hydroxide-EDTA complex-metric 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 (with vanadium;

-- Part 11: Determination of chromium content in the absence of Vanadium - Ammonium ferrous sulfate titration method;

-- Part 12: Determination of vanadium content - Ammonium ferrous sulfate titration and inductively coupled plasma atomic emission spectrometry;

-- Part 13: Determination of zirconium content - EDTA complexometric titration and inductively coupled plasma atomic emission spectrometry;

-- Part 14: Determination of carbon content;

This Part is Part 21 of GB/T 4698.

This Part was drafted in accordance with the rules given in GB/T 1.1-2009.

This Part replaces GB/T 4698.21-1996 "Sponge titanium, titanium and titanium alloys-Determination of manganese, chromium, nickel, aluminum, molybdenum, tin, vanadium, yttrium, copper, zirconium content-Emission spectrographic method". Compared with GB/T 4698.21-1996, in addition to editorial modifications, the main technical changes are as follows:

- modified the determination range: Mn, Cr, Ni from 0.02%~0.20%, Al, Mo, Sn, V, Y and Zr from 0.01%~0.15%, Cu from 0.001%~0.015% to 0.0005%~0.050% (see Clause 1 of this Edition, Clause 1 of Edition 1996);

- modified the normative references (see Clause 2 of this Edition, Clause 2 of Edition 1996);

- buffer was modified from toner to silver chloride-graphite buffer; re-described the method principle (see Clause 3 of this Edition, Clause 3 of Edition 1996);

- modified the equipment, added "graphite electrode structure and dimensions" (see Clause 5 of this Edition, Clause 5 of Edition 1996);

- added the requirements for sample (see Clause 6);

- modified the method for preparing spectrum sample (see 7.2 of this Edition, 6.2 of Edition 1996);

- modified the standard sample preparation, determination conditions and measurement methods (see 7.3 of this Edition, 6.3 of Edition 1996);

- deleted the description for analysis results (see Clause 7 of Edition 1996);

- added the sub-clauses on precision (see Clause 8 of this Edition);

- added the sub-clauses on test report (see Clause 9 of this Edition).

1 Scope

This Part of GB/T 4698 specifies the determination method for manganese, chromium, nickel, aluminum, molybdenum, tin, vanadium, yttrium, copper and zirconium content in titanium sponge, titanium and titanium alloys.

This Part is applicable to the determination of manganese, chromium, nickel, aluminum, molybdenum, tin, vanadium, yttrium, copper and zirconium content in titanium sponge, titanium and titanium alloys. See Table 1 for the determination range.

2 Normative references

The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.

GB/T 31981, Methods of sampling and sample preparation for chemical composition analysis of titanium and titanium alloy

3 Principle

Use hydrochloric acid to dissolve test material. Evaporate to dryness. Burn to oxide. Grind into powder and mix with a certain amount of buffer (silver chloride + carbon powder). Use atomic emission spectrometer arc excitation for sample analysis. According to the working curve, calculate the content of each impurity element.

4 Reagents

4.1 Titanium oxide (titanium oxide mass fraction >=99.995%).

4.2 Manganese oxide, spectrally pure.

4.3 Chromium oxide, spectrally pure.

4.4 Nickel oxide, spectrally pure.

4.5 Alumina, spectrally pure.

4.6 Molybdenum oxide, spectrally pure.

4.7 Tin oxide, spectrally pure.

4.8 Vanadium oxide, spectrally pure.

4.9 Yttrium oxide, spectrally pure.

4.10 Copper oxide, spectrally pure.

4.11 Zirconia, spectrally pure.

4.12 Hydrochloric acid (rho = 1.19g/mL), guaranteed reagent.

4.13 Graphite powder, spectrally pure.

4.14 Silver chloride, analytical reagent.

4.15 Buffer: weigh an appropriate amount of silver chloride (4.14) and graphite powder (4.13) at a ratio of 85:15 to mix and grind evenly. […]

5 Equipment

5.1 DC Arc Atomic Emission Spectrometer.

5.2 Box resistance furnace.