YS/T 539.12-2009Methods for chemical analysis of nickel base alloy powder. Part 12: Determination of phosphorus content. N-butyl alacohol-chloroform extraction spectrophotometry (English PDF)

Foreword

YS/T 539 "nickel-based alloy powder chemical analysis method" is divided into 13 parts.

--- Part 1. Determination of the amount of boron acid-base titration;

--- Part 2. Determination of the amount of chrome aluminum Azure S Spectrophotometry;

--- Part 3. Determination of silicon content of perchloric acid dehydration gravimetric method;

--- Part 4. Determination of chromium content of ammonium persulfate oxidation titration;

--- Part 5. Determination of manganese content of sodium periodate (K) oxidation spectrophotometry;

--- Part 6. Determination of iron content of titanium trichloride - potassium dichromate titration;

--- Part 7. Determination of cobalt content nitroso R salt spectrophotometric method;

--- Part 8. Determination of copper content Neocuproine - chloroform extraction spectrophotometric method;

--- Part 9. Determination of copper content of sodium thiosulfate iodometry;

--- Part 10. Determination of molybdenum content - Thiocyanate spectrophotometric method;

--- Part 11. Determination of cinchonine gravimetric method tungsten content;

--- Part 12. Determination of phosphorus content of n-butyl alcohol - chloroform extraction spectrophotometric method;

--- Part 13. Determination of oxygen pulse heating inert gas fusion - infrared absorption method.

This section is YS/T 539 Part 12.

The partial replacement of YS/T 539.12-2006 "nickel-based alloy powder chemical analysis of n-butyl alcohol - chloroform extraction photometric measurements Given the amount of phosphorus. " this portion of YS/T 539.12-2006 phase comparator major changes are as follows.

--- Increasing the foreword;

--- Complements the repeatability limit.

The non-ferrous metal part by the National Standardization Technical Committee and centralized.

This section is responsible for drafting unit. Beijing Nonferrous Metal Research Institute, China Nonferrous Metals Industry Institute of Standards and Metrology and Quality.

This section is drafted. Beijing Nonferrous Metal Research Institute, Steel Research Institute.

1 Scope

YS/T 539 This part specifies the method for determination of nickel-base alloy powder phosphorus content.

This section applies to the determination of nickel-base alloy powder phosphorus content measurement range. 0.001% to 0.05%.

2 Method summary

Sample by mixed acid is dissolved in nitric acid medium, ortho-phosphoric acid and ammonium molybdate generated phosphomolybdic heteropoly acid is n-butanol - chloroform extraction, chlorine Stannous phosphorus molybdenum heteropoly acid reduction and back-extracted into the aqueous phase, at a wavelength of 680nm spectrophotometer measured absorbance.

3 Reagents

Unless otherwise indicated in the analysis using only recognized as analytical grade reagents and distilled or deionized water or equivalent purity.

3.1 sodium hydroxide.

3.2 hydrochloride (rho1.19g/mL).

Nitrate 3.3 (rho1.42g/mL).

3.4 Hydrofluoric acid (rho1.15g/mL).

3.5 perchloric acid (rho1.67g/mL).

3.6 ammonium molybdate solution (100g/L).

3.7 sodium nitrite solution (300g/L).

3.8 nitric acid (1 + 1). nitrate (3.3) to boil 3min ~ 5min, formulated after the flooding exhausted nitrogen oxides.

3.9 citric acid solution (100g/L). Per 100mL solution with an aqueous solution containing 3.5g of sodium hydroxide in the formulation.

3.10 butanol - a mixture of chloroform. n-butanol and a mixed three chloroform.

3.11 stannous chloride solution (10g/L). 1g stannous chloride (SnCl2 · 2H2O) was dissolved in 8mL hydrochloric acid (3.2), diluted with water to 100mL, the time is now equipped with.

3.12 P standard stock solution. Weigh in advance by 105 °C ~ 110 °C drying 0.2195g potassium dihydrogen phosphate reference reagents dissolved in water, Plus 10mL of nitric acid (3.3) and transferred to 1000mL volumetric flask, dilute to the mark, mix and store in a plastic bottle. This solution 1mL Phosphorus-containing 50µg.

3.13 Phosphorus standard solution. Pipette 20.00mL phosphorus standard stock solution (3.12) into 1000mL flask, add 5mL nitric acid (3.3), dilute to the mark and mix. This solution 1mL containing 1µg phosphorus.

4 Instrument

Spectrophotometer.

5 Step, Analysis