GB/T 8647.10-2006 English PDF (GB/T8647.10-2006)

GB/T 8647.10-2006: 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
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GB/T 8647.10-2006
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.040.30
H 13
Replacing GB/T 5123-1985
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
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 and materials ... 6
4 Instruments and equipment ... 6
5 Analysis steps ... 6
6 Working curve ... 7
7 Precision ... 8
8 Quality assurance and control ... 9
Annex A (informative) Impurity content of nickel spectroscopy standard sample ... 10
Annex B (informative) Spectrophotometric determination of arsenic, cadmium, lead,
zinc, antimony, bismuth, tin, cobalt, copper, manganese, magnesium, silicon, aluminum
and iron in nickel ... 12
Annex C (informative) Direct reading spectrometry for determination of arsenic,
cadmium, lead, zinc, antimony, bismuth, tin, cobalt, copper, manganese, magnesium,
silicon, aluminum and iron in nickel ... 17
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
1 Scope
This Part specifies the emission spectrometric determination method for the content of
impurity elements such as arsenic, cadmium, lead, zinc, antimony, bismuth, tin, cobalt,
copper, manganese, magnesium, silicon, aluminum and iron in nickel.
This Part is applicable to the determination of the content of impurity elements such as
arsenic, cadmium, lead, zinc, antimony, bismuth, tin, cobalt, copper, manganese,
magnesium, silicon, aluminum and iron.
This Part stipulates the determination range of the above impurity elements in nickel as
follows: For the determination working curve that meets the requirements of this Part,
the lower limit of analysis of each impurity element is 90% of the lowest content of the
standard sample used, and the upper limit of analysis is 110% of the highest content of
the standard sample used. For the working curve that partially meets the requirements,
the part of the working curve that meets the requirements is selected to determine the
analysis range of each impurity element.
This Part specifies objective criteria for evaluating analytical values obtained with arc-
type emission spectrometers. Due to the wide range of available spectrometer types, it
is difficult to fully specify all conditions. Therefore, this standard is not used to specify
instrument models or procedures for converting instrument responses into
concentration units.
2 Method summary
The specimen is dissolved in nitric acid. Evaporate to dryness. Burn into oxides. Grind
into powder. Use appropriate methods and arc excitation of emission spectrometer to
analyze the sample and calculate the content of each impurity element according to the
working curve.
3 Reagents and materials
The water used in this method is grade two water or laboratory water of equivalent
purity.
3.1 Nickel spectral standard samples: must be standard samples approved by the legal
institution or standard samples approved by both parties (metallic standard samples
shall be pre-processed into oxides according to 5.2.1). Please refer to Annex A for some
nickel spectral standard samples.
3.2 Graphite electrode (spectrally pure).
3.3 Nitric acid (p1.42 g/mL), guaranteed reagent.
3.4 Nitric acid (3+2).
3.5 Nitric acid (1+9).
4 Instruments and equipment
4.1 Emission spectrometers (arc type) may be used as long as they are available and
meet the accuracy requirements of this standard. They may be spectrographs with
associated equipment or direct reading spectrometers with any detector.
4.2 Box type resistance furnace.
4.3 Agate mortar.
5 Analysis steps
5.1 Test material
Weigh two specimens in parallel. Each specimen is about 5%.
5.2 Determination
5.2.1 Place two test materials in appropriate beakers. Wash with 30 mL nitric acid (3.5).
Pour off the washing solution and rinse with water three times. Add 50 mL of nitric acid
(3.4). Cover with a watch glass. After the violent reaction stops, heat and evaporate
until it is almost viscous. Transfer to a 50 mL porcelain crucible and evaporate to
dryness. Place the porcelain crucible in a box-type resistance furnace. Burn at
750°C~800°C for 20 min. Take out. Cool to room temperature. Grind the generated
oxide in an agate mortar (4.3).
5.2.2 Perform sample analysis according to the laboratory selected conditions. Each
Annex B
(informative)
Spectrophotometric determination of arsenic, cadmium, lead, zinc, antimony,
bismuth, tin, cobalt, copper, manganese, magnesium, silicon, aluminum and iron
in nickel
B.1 Method summary
The specimen is dissolved in nitric acid. Evaporate to dryness. Burn into oxide. Grind
into powder. Press into pellets. Use the three-standard specimen method, DC arc
excitation, and photosensitive plate to record the spectrum. Use a microphotometer to
measure the conversion blackness difference between the selected analytical line and
the internal standard line. Then find the content of the corresponding element on the
analytical curve of the conversion blackness difference and the logarithm of the content.
B.2 Reagents and materials
B.2.1 Developer and fixer: Prepare according to the instructions of the spectral
photosensitive plate.
B.2.2 Graphite electrodes (diameter is 6 mm and 8 mm~10 mm): spectrally pure.
B.2.3 Spectral photosensitive plate: sensitivity is 12±8 (UV I type); sensitivity is 20±5
(UV II type).
B.2.4 Standard samples for spectral analysis.
B.3 Instruments and equipment
B.3.1 Medium or large quartz prism or grating spectrograph.
B.3.2 DC power supply and high frequency arc striking device.
B.3.3 Microphotometer.
B.3.4 Press (pressure not less than 15000 kPa).
B.3.5 Die: made of alloy steel. Die diameter and die inner diameter is 6 mm, height is
50 mm~80 mm. Finish is 8.
B.4 Analysis steps
B.4.1 Weigh two specimens (about 5 g each). Proceed as in 5.2.1.
B.4.2 Weigh 3 portions (0.3 g~0.5 g each) of oxide powder (B.4.1) and press them into
Annex C
(informative)
Direct reading spectrometry for determination of arsenic, cadmium, lead, zinc,
antimony, bismuth, tin, cobalt, copper, manganese, magnesium, silicon,
aluminum and iron in nickel
C.1 Method summary
Dissolve the specimen in nitric acid. Evaporate to dryness. Burn into oxide. Mix the
oxide with barium carbonate in a mass ratio of 4:1. Grind evenly. Excite with a DC arc
anode. Measure the intensity ratio of the analysis line of each element to be tested to
the internal standard line. Obtain the content of the corresponding element from the
working curve.
C.2 Reagents and materials
C.2.1 Graphite electrode (6 mm in diameter): Spectral pure. The upper electrode is
machined into a truncated cone with a top diameter of 2 mm~4 mm. The specimen
electrode is machined into a cup with an inner diameter of 4 mm and a depth of 4 mm.
C.2.2 Barium carbonate: spectrally pure.
C.2.3 Nickel spectral analysis standard sample.
C.3 Instruments and equipment
ATOMCOMP 2000 direct reading spectrometer
- Detector type: CID38 high efficiency solid state charge injection camera system;
- Wavelength range: 195 nm~820 nm.
C.4 Analysis steps
C.4.1 Weigh two specimens (about 5 g each). Proceed as in 5.2.1.
C.4.2 Weigh 2.000 g of oxide powder (C.4.1) and 0.500 g of barium carbonate (C.2.2)
respectively and mix them. Grind them evenly in an agate mortar and press them into
the small hole of the sample electrode (C.2.1). The shape, size and position of the
electrode during analysis exposure are shown in Figure C.1.
GB/T 8647.10-2006
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.040.30
H 13
Replacing GB/T 5123-1985
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
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 and materials ... 6
4 Instruments and equipment ... 6
5 Analysis steps ... 6
6 Working curve ... 7
7 Precision ... 8
8 Quality assurance and control ... 9
Annex A (informative) Impurity content of nickel spectroscopy standard sample ... 10
Annex B (informative) Spectrophotometric determination of arsenic, cadmium, lead,
zinc, antimony, bismuth, tin, cobalt, copper, manganese, magnesium, silicon, aluminum
and iron in nickel ... 12
Annex C (informative) Direct reading spectrometry for determination of arsenic,
cadmium, lead, zinc, antimony, bismuth, tin, cobalt, copper, manganese, magnesium,
silicon, aluminum and iron in nickel ... 17
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
1 Scope
This Part specifies the emission spectrometric determination method for the content of
impurity elements such as arsenic, cadmium, lead, zinc, antimony, bismuth, tin, cobalt,
copper, manganese, magnesium, silicon, aluminum and iron in nickel.
This Part is applicable to the determination of the content of impurity elements such as
arsenic, cadmium, lead, zinc, antimony, bismuth, tin, cobalt, copper, manganese,
magnesium, silicon, aluminum and iron.
This Part stipulates the determination range of the above impurity elements in nickel as
follows: For the determination working curve that meets the requirements of this Part,
the lower limit of analysis of each impurity element is 90% of the lowest content of the
standard sample used, and the upper limit of analysis is 110% of the highest content of
the standard sample used. For the working curve that partially meets the requirements,
the part of the working curve that meets the requirements is selected to determine the
analysis range of each impurity element.
This Part specifies objective criteria for evaluating analytical values obtained with arc-
type emission spectrometers. Due to the wide range of available spectrometer types, it
is difficult to fully specify all conditions. Therefore, this standard is not used to specify
instrument models or procedures for converting instrument responses into
concentration units.
2 Method summary
The specimen is dissolved in nitric acid. Evaporate to dryness. Burn into oxides. Grind
into powder. Use appropriate methods and arc excitation of emission spectrometer to
analyze the sample and calculate the content of each impurity element according to the
working curve.
3 Reagents and materials
The water used in this method is grade two water or laboratory water of equivalent
purity.
3.1 Nickel spectral standard samples: must be standard samples approved by the legal
institution or standard samples approved by both parties (metallic standard samples
shall be pre-processed into oxides according to 5.2.1). Please refer to Annex A for some
nickel spectral standard samples.
3.2 Graphite electrode (spectrally pure).
3.3 Nitric acid (p1.42 g/mL), guaranteed reagent.
3.4 Nitric acid (3+2).
3.5 Nitric acid (1+9).
4 Instruments and equipment
4.1 Emission spectrometers (arc type) may be used as long as they are available and
meet the accuracy requirements of this standard. They may be spectrographs with
associated equipment or direct reading spectrometers with any detector.
4.2 Box type resistance furnace.
4.3 Agate mortar.
5 Analysis steps
5.1 Test material
Weigh two specimens in parallel. Each specimen is about 5%.
5.2 Determination
5.2.1 Place two test materials in appropriate beakers. Wash with 30 mL nitric acid (3.5).
Pour off the washing solution and rinse with water three times. Add 50 mL of nitric acid
(3.4). Cover with a watch glass. After the violent reaction stops, heat and evaporate
until it is almost viscous. Transfer to a 50 mL porcelain crucible and evaporate to
dryness. Place the porcelain crucible in a box-type resistance furnace. Burn at
750°C~800°C for 20 min. Take out. Cool to room temperature. Grind the generated
oxide in an agate mortar (4.3).
5.2.2 Perform sample analysis according to the laboratory selected conditions. Each
Annex B
(informative)
Spectrophotometric determination of arsenic, cadmium, lead, zinc, antimony,
bismuth, tin, cobalt, copper, manganese, magnesium, silicon, aluminum and iron
in nickel
B.1 Method summary
The specimen is dissolved in nitric acid. Evaporate to dryness. Burn into oxide. Grind
into powder. Press into pellets. Use the three-standard specimen method, DC arc
excitation, and photosensitive plate to record the spectrum. Use a microphotometer to
measure the conversion blackness difference between the selected analytical line and
the internal standard line. Then find the content of the corresponding element on the
analytical curve of the conversion blackness difference and the logarithm of the content.
B.2 Reagents and materials
B.2.1 Developer and fixer: Prepare according to the instructions of the spectral
photosensitive plate.
B.2.2 Graphite electrodes (diameter is 6 mm and 8 mm~10 mm): spectrally pure.
B.2.3 Spectral photosensitive...