GB/T 8647.10-2006 English PDF
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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 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 method1 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. EachAnnex 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 intoAnnex 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. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
