SN/T 2763.4-2012 English PDF (SNT2763.4-2012)

This part of SN/T 2763 specifies the inductively coupled plasma atomic emission spectrometry method for the determination of nickel, cobalt, aluminum, magnesium, phosphorus in nickel laterite ore.

SN/T 2763.4-2012
SN
ENTRY & EXIT INSPECTION & QUARANTINE STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
Chemical analysis of nickel laterite ore - Part 4:
Determination of nickel, cobalt, aluminum, magnesium
and phosphorus content - Inductively coupled plasma
atomic emission spectrometric method
ISSUED ON: DECEMBER 12, 2012
IMPLEMENTED ON: JULY 01, 2013
Issued by: General Administration of Quality Supervision Inspection and Quarantine of PRC
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Method summary ... 5
4 Reagents and materials ... 5
5 Apparatus and equipment ... 6
6 Specimen ... 6
7 Analytical procedures ... 6
8 Result calculation ... 8
9 Precision ... 9
Appendix A (Informative) Recommended instrument working conditions ... 10 Appendix B (Normative) Flow chart of acceptance of specimen’s analytical value ... 11
Chemical analysis of nickel laterite ore - Part 4:
Determination of nickel, cobalt, aluminum, magnesium
and phosphorus content - Inductively coupled plasma
atomic emission spectrometric method
1 Scope
This part of SN/T 2763 specifies the inductively coupled plasma atomic
emission spectrometry method for the determination of nickel, cobalt, aluminum, magnesium, phosphorus in nickel laterite ore.
This part applies to the determination of nickel, cobalt, aluminum, magnesium, phosphorus content in nickel laterite ore. The determination range is as shown in Table 1.
2 Normative references
The following documents are essential to the application of this document. For the dated documents, only the versions with the dates indicated are applicable to this document; for the undated documents, only the latest version (including all the amendments) are applicable to this standard.
GB/T 602 Chemical reagent - Preparations of standard solutions for impurity GB/T 6682 Water for analytical laboratory use - Specification and test
methods
GB/T 6730.3 Methods for chemical analysis of iron ores - The gravimetric method for the determination of hygroscopic moisture content in analytical 7.3 Specimen treatment
Add drops of water to wet the specimen (7.2). Add 6 mL of hydrochloric acid (4.1) and 4 mL of nitric acid 4.2). Add the cover. Place it on the electric hot plate. Digest it at 110 °C for 2 h. Remove the crucible. Add 5 mL of hydrofluoric acid (4.3) and 1.5 mL of perchloric acid (4.4). Continue to digest at 130 °C for 2 h. Open the cover and use a small amount of water to rinse it. Combine the rinsing solution in the crucible. Increase the temperature. Shake the crucible from time to time, until the white smoke of perchloric acid disappears. Remove the crucible. Use a small amount of aqua regia (1 + 9) (4.8) to rinse the wall of the crucible. Heat it again the white smoke disappears. Add 10 mL of hydrochloric acid (4.6). Heat it for 15 minutes. Use water to dilute it to about 20 mL. Continue heating for 5 min. After the test solution is cooled to room temperature, transfer it into a 100 mL volumetric flask. Use water to dilute it to the mark. Shake it uniformly. Prepare for determination.
Note: For the magnesia nickel ore sample with higher magnesium content, it may pipette 10 mL of the solution to be tested into a 100 mL volumetric flask. Add 9 mL of hydrochloric acid (4.6) and the iron matrix of the same amount in the original solution. Use water to dilute it to the mark. Use it independently for the testing magnesium content.
7.4 Blank test and verification test
Test a standard sample and blank of the same type along with the specimen. Use the same amount of iron oxide powder (4.5) as the specimen in the blank test instead of the sample to perform the blank test.
Note: When there is no standard sample of the same type, it may use other similar types of standard samples.
7.5 Drawing of working curve
Weigh 5 sets of iron oxide powder (4.5) equivalent to the mass in the sample; follow step 7.3; transfer them to five 100 mL volumetric flasks; add a certain volume of nickel standard stock solution (4.9), aluminum standard stock solution (4.11), magnesium standard stock solution (4.12), cobalt standard solution (4.14), phosphorus standard solution (4.15); prepare it into the standard working solution series as shown in Table 2.
Note: For the analysis of limonite type (low-nickel high-iron) nickel laterite ore, the iron content is generally 40% ~ 50%, it may weigh 0.13 g of iron oxide (equivalent to a 0.2 g specimen with an iron content of 45%). For the analysis of the silicon-magnesia-nickel ore type (high-nickel low-iron) nickel laterite ore, the iron content is generally 15% ~ 25%, it may weigh 0.057 g of iron oxide (equivalent to a 0.2 g specimen with an iron content of 20%).