GB/T 42513.2-2023Methods for chemical analysis of nickel alloys - Part 2: Determination of phosphorus content - Molybdenum blue spectrophotometry (English PDF)

Foreword

This document complies with the provisions of GB/T 1.1-2020 "Standardization Work Guidelines Part 1: Structure and Drafting Rules of Standardization Documents" Drafting:

This document is Part 2 of GB/T 42513 "Chemical Analysis Methods for Nickel Alloys": GB/T 42513 has released the following parts:

---Part 1: Determination of chromium content by ferrous ammonium sulfate potentiometric titration method;

---Part 2: Determination of phosphorus content by molybdenum blue spectrophotometry;

---Part 3: Determination of aluminum content by nitrous oxide-flame atomic absorption spectrometry and inductively coupled plasma atomic emission light spectrometry;

---Part 4: Determination of silicon content by nitrous oxide-flame atomic absorption spectrometry and molybdenum blue spectrophotometry;

---Part 5: Determination of vanadium content by nitrous oxide-flame atomic absorption spectrometry and inductively coupled plasma atomic emission light spectrum method:

This document has been modified to adopt ISO 9388:1992 "Determination of phosphorus content in nickel alloys - Molybdenum blue spectrophotometric method":

Compared with ISO 9388:1992, this document has many structural adjustments: See the comparison list of structural number changes between the two documents:

Appendix A:

Compared with ISO 9388:1992, there are many technical differences between this document and the clauses involved in the outer margins of the page:

Single lines (|) are marked: A list of these technical differences and their causes is provided in Appendix B:

The following editorial changes have been made to this document:

---In order to coordinate with the existing standards, the name of the standard is changed to "Chemical Analysis Methods for Nickel Alloys Part 2: Determination of Phosphorus Content Molybdenum Blue" Spectrophotometry":

Please note that some content in this document may be subject to patents: The publisher of this document assumes no responsibility for identifying patents:

Introduction

Nickel alloys are commonly used in instrumentation, electronic communications, pressure vessels, corrosion-resistant devices, and are widely used in aerospace and high-end special purposes:

Machinery and equipment manufacturing and other industries are one of the important metal raw materials for industrial development: There are dozens of international standards for chemical analysis methods of nickel alloys:

In:2017, with the progress of my country's industry, the demand for the production, import and export of high-end nickel alloy materials increased: To this end, international standards were transformed into national standards:

It is of great significance to assist the development and upgrading of non-ferrous industry and the development of domestic manufacturing industry: GB/T 42513 "Chemical Analysis Methods for Nickel Alloys" aims to Establish a complete and practical standard method for testing chromium, phosphorus, niobium, molybdenum, aluminum, vanadium, silicon, cobalt, copper and other elements in nickel alloys, convert the following International standards:

---ISO 7592:2017 Determination of chromium content in nickel alloys by ferrous ammonium sulfate potentiometric titration method;

---ISO 9388:1992 Determination of phosphorus content in nickel alloys by molybdenum blue spectrophotometry;

---ISO 7530-7:1992 Flame atomic absorption spectrometry of nickel alloys Part 7: Determination of aluminum content;

---ISO 7530-8:1992 Flame atomic absorption spectrometry of nickel alloys Part 8: Determination of silicon content;

---ISO 7530-9:1993 Flame atomic absorption spectrometry of nickel alloys Part 9: Determination of vanadium content;

---ISO 11435:2011 Determination of molybdenum content in nickel alloys by inductively coupled plasma atomic emission spectrometry;

---ISO 7530-1:2015 Flame atomic absorption spectrometry analysis of nickel alloys Part 1: Cobalt, chromium, copper, iron and manganese content determination;

---ISO 22033:2011 Determination of niobium content in nickel alloys by inductively coupled plasma atomic emission spectrometry;

---ISO 11436:1993 Determination of total boron content in nickel and nickel alloys by curcumin absorption spectrometry;

---ISO 23166:2018 Determination of tantalum content in nickel alloys by inductively coupled plasma atomic emission spectrometry:

GB/T 42513 is planned to consist of 13 parts:

---Part 1: Determination of chromium content by ferrous ammonium sulfate potentiometric titration method:

---Part 2: Determination of phosphorus content by molybdenum blue spectrophotometry:

---Part 3: Determination of aluminum content by nitrous oxide-flame atomic absorption spectrometry and inductively coupled plasma atomic emission light spectrum method:

---Part 4: Determination of silicon content by nitrous oxide-flame atomic absorption spectrometry and molybdenum blue spectrophotometry:

---Part 5: Determination of vanadium content by nitrous oxide-flame atomic absorption spectrometry and inductively coupled plasma atomic emission light spectrum method:

---Part 6: Determination of molybdenum content by inductively coupled plasma atomic emission spectrometry:

---Part 7: Determination of cobalt, chromium, copper, iron and manganese content by flame atomic absorption spectrometry:

---Part 8: Determination of niobium content by inductively coupled plasma atomic emission spectrometry:

---Part 9: Determination of total boron content of curcumin spectrophotometrically:

---Part 10: Determination of trace element content by glow discharge mass spectrometry:

---Part 11: Determination of silicon, manganese, phosphorus, chromium, nickel, copper, molybdenum, cobalt, iron, aluminum, vanadium, titanium, tungsten and niobium content by X-ray fluorescence spectrometry (common law):

---Part 12: Determination of tantalum content by inductively coupled plasma atomic emission spectrometry:

---Part 13: Determination of oxygen, nitrogen and hydrogen content: Inert gas melting - thermal conductivity method/infrared absorption method:

Phosphorus is an important element in nickel alloys: The level of phosphorus content will significantly affect its performance and life: The determination of phosphorus content in nickel alloys is very important for nickel alloys:

The production and use of gold are of great significance: This document can promote the progress of my country's nickel alloy testing technology and ensure that industry practitioners There are standards to follow in the application, scientific research, and testing processes, filling the gap in the method for determining phosphorus content in nickel alloys in my country:

Nickel alloy chemical analysis method Part 2: Determination of phosphorus content Molybdenum blue spectrophotometry Warning---Personnel using this document should have regular laboratory work experience: This document does not address all possible security issues question: Users are responsible for taking appropriate safety and health measures and ensuring compliance with the conditions stipulated in relevant national regulations:

1 Scope

This document describes a method for the determination of phosphorus content in nickel alloys by molybdenum blue spectrophotometry:

This document is applicable to the determination of phosphorus content in nickel alloys: The determination range (mass fraction) is 0:0010%~0.025%:

2 Normative reference documents

This document has no normative references:

3 Terms and definitions

There are no terms or definitions to be defined in this document:

4 Principles

The sample is decomposed by hydrochloric acid and nitric acid, and sulfuric acid is added to emit smoke to drive away the hydrochloric acid: Cr3 is oxidized to Cr6 by ammonium persulfate: Phosphorus reacts with Fe3 Iron phosphate precipitate is generated, which can be separated from chromium after filtration: The iron orthophosphate precipitate is dissolved in a hydrofluoric acid-nitric acid mixed acid: Add boric acid and tartar Acid and sulfamic acid complex free fluoride ions, eliminate the interference of arsenic, and remove nitrogen oxides: Use isobutanol to extract phosphomolybdenum heteropolyacid and reduce phosphorus Molybdenum heteropolyacid is phosphomolybdenum blue and is back-extracted in the aqueous phase: Measure the absorbance at 700nm with a spectrophotometer and calculate the mass fraction of phosphorus:

5 Reagents or materials

Warning---Hydrofluoric acid (5:4) is extremely irritating and corrosive to skin and mucous membranes, causing severe skin burns and slow healing:

In case of contact with skin, rinse with water and seek medical advice:

Mixed acids (5:8) are unstable and highly corrosive: Toxic gas (chlorine) will be released when left to stand, so preparation should be done in a fume hood:

OK and should not be stored in closed containers:

Unless otherwise stated, only approved analytical grade reagents and distilled water or water of equivalent purity are used during analysis:

5.1 Hydrochloric acid: rho=1:18g/mL:

5.2 Nitric acid: rho=1:41g/mL:

5.3 Sulfuric acid: rho=1:84g/mL:

5.4 Hydrofluoric acid: rho=1:15g/mL, 48% (mass fraction) HF:

5.5 Ammonia solution: rho=0:89g/mL:

5.6 Trichloromethane (CHCl3):