GB/T 8647.4-2006 English PDF (GB/T8647.4-2006)

GB/T 8647.4-2006: The methods for chemical analysis of nickel -- Determination of phosphorous content -- Molybdenum blue spectrophotometric method
Delivery: 9 seconds. Download (and Email) true-PDF + Invoice.
Get Quotation: Click GB/T 8647.4-2006 (Self-service in 1-minute)
Historical versions (Master-website): GB/T 8647.4-2006
Preview True-PDF (Reload/Scroll-down if blank)


GB/T 8647.4-2006
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.040.30
H 13
Replacing GB/T 8647.4-1988
The methods for chemical analysis of nickel - Determination
of phosphorous content - Molybdenum blue
spectrophotometric method
ISSUED ON: SEPTEMBER 26, 2006
IMPLEMENTED ON: FEBRUARY 01, 2007
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Method summary ... 5
3 Reagents ... 5
4 Instruments ... 6
5 Analysis steps ... 6
6 Calculation of analysis results ... 7
7 Precision ... 8
8 Quality assurance and control ... 9
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;
The methods for chemical analysis of nickel - Determination
of phosphorous content - Molybdenum blue
spectrophotometric method
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 (ρ1.42 g/mL): guaranteed reagent.
3.2 Nitric acid (1+1).
3.3 Hydrochloric acid (ρ1.19 g/mL): guaranteed reagent.
3.4 Perchloric acid (ρ1.66 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
5.3 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
GB/T 8647.4-2006
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.040.30
H 13
Replacing GB/T 8647.4-1988
The methods for chemical analysis of nickel - Determination
of phosphorous content - Molybdenum blue
spectrophotometric method
ISSUED ON: SEPTEMBER 26, 2006
IMPLEMENTED ON: FEBRUARY 01, 2007
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Method summary ... 5
3 Reagents ... 5
4 Instruments ... 6
5 Analysis steps ... 6
6 Calculation of analysis results ... 7
7 Precision ... 8
8 Quality assurance and control ... 9
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;
The methods for chemical analysis of nickel - Determination
of phosphorous content - Molybdenum blue
spectrophotometric method
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 (ρ1.42 g/mL): guaranteed reagent.
3.2 Nitric acid (1+1).
3.3 Hydrochloric acid (ρ1.19 g/mL): guaranteed reagent.
3.4 Perchloric acid (ρ1.66 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
5.3 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