GB/T 8647.4-2006The methods for chemical analysis of nickel - Determination of phosphorous content - Molybdenum blue spectrophotometric method (English PDF)
镍化学分析方法 磷量的测定 钼蓝分光光度法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
September 26, 2006
Implementation date
February 1, 2007
Scope
GB/T 8647.4-2006 is the English-translated version of 镍化学分析方法 磷量的测定 钼蓝分光光度法.
GB/T 8647.4-2006 is the molybdenum blue spectrophotometric method for phosphorus in nickel and is Part 4 of the ten-part GB/T 8647 series.
The test material is dissolved in nitric acid, phosphorus is oxidised with potassium permanganate, the phosphomolybdic heteropoly acid formed by phosphorus(V) with ammonium molybdate is extracted from acid solution with a mixture of three parts chloroform to one part n-butanol, reduced to molybdenum blue with stannous chloride and measured at 620 nm in a 2 cm cuvette against a blank.
The working curve is drawn from 0 to 10.00 mL of phosphorus standard solution, and specimens above 0.006% phosphorus are diluted as Table 1 directs. The determination range is 0.0005% to 0.03%, and the contents list precision and quality assurance clauses.
Issued on 26 September 2006, it replaces GB/T 8647.4-1988 and has applied since 1 February 2007.
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Document preview — GB/T 8647.4-2006
National Standard of the People's Republic of China
- ICS
- 77.040.30
- Classification
- H 13
- Replacing
- GB/T 8647.4-1988
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword3
- 1 Scope5
- 2 Method summary5
- 3 Reagents5
- 4 Instruments6
- 5 Analysis steps6
- 6 Calculation of analysis results7
- 7 Precision8
- 8 Quality assurance and control9
Foreword
GB/T 8647 "The methods for chemical analysis of nickel" is divided into the following 10 parts:
GB/T 8647.1, The methods for chemical analysis of nickel -- Determination of iron content -- Sulfosalicylic acid spectrophotometric method
GB/T 8647.2, The methods for chemical analysis of nickel -- Determination of aluminium content -- Electrothermal atomic absorption spectrometric method
GB/T 8647.3, The methods for chemical analysis of nickel -- Determination of silicon content -- Molybdenum blue spectrophotometric method
GB/T 8647.4, The methods for chemical analysis of nickel -- Determination of phosphorous content -- Molybdenum blue spectrophotometric method
GB/T 8647.5, The methods for chemical analysis of nickel -- Determination of magnesium content -- Flame atomic absorption spectrometric method
GB/T 8647.6, The methods for chemical analysis of nickel -- Determination of cadmium, cobalt, copper, manganese, lead and zinc contents -- Flame atomic absorption spectrometric method
GB/T 8647.7, The methods for chemical analysis of nickel -- Determination of arsenic antimony bismuth tin and lead contents -- Electrothermal atomic absorption spectrometric method
GB/T 8647.8, The methods for chemical analysis of nickel -- Determination of sulphur content -- Infra-red absorption method after high frequency induction furnace combustion
GB/T 8647.9, The methods for chemical analysis of nickel -- Determination of carbon content -- Infra-red absorption method after high frequency induction furnace combustion
GB/T 8647.10, The methods for chemical analysis of nickel -- Determination of arsenic cadmium lead zinc antimony bismuth tin cobalt copper manganese magnesium silicon aluminium iron contents -- Atomic emission spectrometric method This is Part 4.
This Part replaces GB/T 8647.4-1988 "Nickel -- Determination of phosphorus content -- Molybdenum blue spectrophotometric method". Compared with GB/T 8647.4-1988, the following changes were made to this Part:
- The text format was revised;
1 Scope
This Part specifies the method for the determination of phosphorus content in nickel.
This Part is applicable to the determination of phosphorus content in nickel. Determination range: 0.0005%~0.03%.
2 Method summary
The test material is dissolved in nitric acid. Phosphorus is oxidized with potassium permanganate. In an acidic solution, the phosphomolybdic acid heteropoly acid complex formed by phosphorus (V) and ammonium molybdate is extracted with a mixed solvent of n-butanol-chloroform. It is reduced to phosphomolybdic blue with stannous chloride. Its absorbance is measured at a wavelength of 620 nm on a spectrophotometer.
3 Reagents
3.1 Nitric acid (rho1.42 g/mL): guaranteed reagent.
3.2 Nitric acid (1+1).
3.3 Hydrochloric acid (rho1.19 g/mL): guaranteed reagent.
3.4 Perchloric acid (rho1.66 g/mL): guaranteed reagent.
3.5 Perchloric acid (1+1).
3.6 Perchloric acid (1+9).
3.7 N-Butanol.
3.8 Chloroform.
3.9 Mixed extractant: three parts of chloroform and one part of n-butanol are mixed.
3.10 Ammonium molybdate solution (100 g/L): Weigh 10 g of ammonium molybdate.
5 Analysis steps
5.3 Determination
5.3.1 Place the test material (5.1) in a 250 mL beaker. Slowly add 15 mL of nitric acid (3.2) and 2~4 drops of potassium permanganate solution (3.12). Slightly heat until the test material is completely dissolved.
NOTE: Add 1 drop of potassium permanganate solution (3.12) to the blank test material.
5.3.2 After the solution has cooled, add 10 mL of perchloric acid (3.5). Heat and evaporate until thick white perchloric acid smoke emerges. Cool. Add 30 mL of water. Stir to dissolve the salts.
5.3.3 Transfer the solution into a 125 mL separatory funnel. Add water to 50 mL. For specimens with phosphorus content greater than 0.006%, dilute the test solution according to Table 1 and place it in a 125 mL separatory funnel. Add perchloric acid (3.6) to 50 mL.
5.3.4 Add 3 mL of ammonium molybdate solution (3.10) to the separatory funnel. Shake well. Let stand for 10 min.
5.3.5 Add 2 mL of n-butanol (3.7). Oscillate for 1 min. Add 15 mL of mixed extractant (3.9). Oscillate for 2 min. After standing for stratification, place the organic phase in a 50 mL volumetric flask. Add another 15 mL of mixed extractant (3.9) to the aqueous phase. Oscillate for 2 min. After standing for stratification, combine the organic phases in a volumetric flask.
5.3.6 Add 3 mL~4 mL of n-butanol (3.7) to the volumetric flask. Add 4 drops of stannous chloride solution (3.11). Dilute to volume with n-butanol (3.7). Mix well. Let stand for 15 min~20 min. Transfer part of the solution to a dry 2 cm cuvette.
5.3.7 Use the blank experimental solution as a reference. Measure its absorbance at a wavelength of 620 nm on a spectrophotometer. Find the corresponding phosphorus content from the working curve.
5.4 Working curve
Take 0 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL, 10.00 mL of phosphorus standard solution (3.14) and place them in a set of 125 mL separatory funnels. Add perchloric acid (3.6) to 50 mL. Follow 5.3.4~5.3.6. Use the reagent blank solution as a reference.
Measure its absorbance at a wavelength of 620 nm on a spectrophotometer. Draw a working curve with phosphorus content as the horizontal axis and absorbance as the vertical axis.
6 Calculation of analysis results
The mass fraction of phosphorus w(P) is calculated as follows, with the value expressed […]
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
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Editions of GB/T 8647.4
| Edition | Title | Revision | Status |
|---|---|---|---|
| GB/T 8647.4-2006 | The methods for chemical analysis of nickel - Determination of phosphorous content - Molybdenum blue spectrophotometric method | current edition | Current |
| GB/T 8647.4-1988 | The methods for chemical analysis of nickel - Determination of phosphorous content - Molybdenum blue spectrophotometric method | previous edition | Superseded |
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Related Standards
GB/T 8647.5-2006 — The methods for chemical analysis of nickel - Determination of magnesium content - Flame atomic absorption spectrometric method
GB/T 8647.3-2006 — The methods for chemical analysis of nickel - Determination of silicon content - Molybdenum blue spectrophotometric method
GB/T 8647.6-2006 — The methods for chemical analysis of nickel -- Determination of cadmium, cobalt, copper, manganese, lead and zinc contents -- Flame atomic absorption spectrometric method
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