Ferromanganese, ferromanganese-silicon and manganese metal—Determination of lead, arsenic, titanium, copper, nickel, calcium, magnesium and aluminum content—Inductively coupled plasma atomic emission spectrometric method
Warning: Users of this standard shall have practical work experience in standardized laboratories. This part does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health measures and to ensure compliance with any national regulatory conditions.
1 Scope
This standard specifies the determination of lead, arsenic, titanium, copper, nickel, calcium, magnesium and aluminum content by inductively coupled plasma atomic emission spectrometric method.
This standard is applicable to the determination of lead, arsenic, titanium, copper, nickel, calcium, magnesium and aluminum content in ferromanganese, ferromanganese-silicon and manganese metal. See Table 1 for the determination range.
Table 1 Determination range and recommended analytical lines of each element
Type Content/% Recommended analytical line/nm Type Content/% Recommended analytical line/nm
Lead 0.0080~0.1200 220.353 Nickel 0.0030~0.2500 231.604
Arsenic 0.0040~0.1200 197.262 Calcium 0.0080~0.2000 393.366 or 317.933
Titanium 0.0010~0.3500 336.121 Magnesium 0.0080~0.5000 279.553
Copper 0.0080~0.2500 324.754 Aluminum 0.0080~0.3500 396.152
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition (including any amendments) applies.
GB/T 4010 Ferroallys sampling and preparation of samples for chemical analysis
GB/T 6379.1 Accuracy (trueness and precision) of measurement methods and results - Part 1: General principles and definitions
GB/T 6379.2 Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method
GB/T 6682 Water for analytical laboratory use - Specification and test methods
GB/T 8170 Rules of rounding off for numerical values & expression and judgement of limiting values
GB/T 28372 Ferroalloys - Sampling and preparation of samples - General rules
GB/T 36244 Inductively coupled plasma optical emission spectrometer
JJG 768 Verification regulation of emission spectrometer
3 Principle
Decompose test portion with nitric acid, hydrochloric acid and hydrofluoric acid, and transform silicon into silicon tetrafluoride, which is removed by smoking of perchloric acid. In hydrochloric acid medium, measure the spectral intensity of each element at the characteristic wavelength of each element by inductively coupled plasma spectrometer under suitable determination conditions, and calculate the amount of each element.
4 Reagents
Unless otherwise stated, only recognized analytical reagents and Grade 1 distilled or deionized water as specified in GB/T 6682 or water with equivalent purity shall be used during the analysis.
4.1 Hydrochloric acid, ρ about 1.19 g/mL.
4.2 Nitric acid, ρ about 1.42 g/mL.
4.3 Hydrofluoric acid, ρ about 1.15 g/mL.
4.4 Perchloric acid, ρ about 1.67 g/mL.
4.5 Sulfuric acid, ρ about 1.84 g/mL.
4.6 Hydrogen peroxide, ρ about 1.13 g/mL.
4.7 Hydrochloric acid, 1+3.
4.8 Sulfuric acid solution,1+9.
4.9 Standard solution
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents
5 Apparatus
6 Sampling and sample preparation
7 Analytical procedures
8 Calculation of analysis results
9 Precision
10 Test report
Annex A (Normative) Background equivalent concentration and detection limit of each element
Annex B (Informative) Original data for precision
