GB/T 8647.10-2006The 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 (English PDF)

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

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.4.2 Weigh 3 portions (0.3 g~0.5 g each) of oxide powder (B.4.1) and press them into

B.4.1 Weigh two specimens (about 5 g each). Proceed as in 5.2.1

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. […]