GB/T 5687.12-2020 Ferrochromium—Determination of phosphorus, aluminum, titanium, copper, manganese, calcium content—Inductively coupled plasma atomic emission spectrometric method English
Ferrochromium - Determination of phosphorus, aluminum, titanium, copper, manganese, calcium content - Inductively coupled plasma atomic emission spectrometric method
Warning: Persons using this part shall be familiar with normal laboratory practice. This part does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.
1 Scope
This part of GB/T 5687 specifies the method for determining phosphorus, aluminum, titanium, copper, manganese, calcium content by inductively coupled plasma atomic emission spectrometric method.
This part is applicable to the determination of phosphorus, aluminum, titanium, copper, manganese and calcium contents in ferrochromium, and the determination of corresponding elements in silicon-chromium alloys is also applicable to this part. The determination range of each element is shown in Table 1.
Table 1 Elements and measurement range
Analysis elements Measurement range (m/m)/%
P 0.010~0.10
Al 0.050~0.60
Ti 0.0050~0.60
Cu 0.010~1.50
Mn 0.010~1.00
Ca 0.10~1.50
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 of the referenced document (including any amendments) applies.
GB/T 4010 Ferroalloys sampling and preparation of samples for chemical analysis
GB/T 6682 Water for analytical laboratory use - Specification and test methods
GB/T 8170 Rules of rounding off for numerical values & expression and judgment of limiting values
GB/T 12806 Laboratory glassware - One-mark volumetric flasks
GB/T 12807 Laboratory glassware - Graduated pipettes
GB/T 12808 Laboratory glassware - One mark pipettes
JJG 768 Verification regulation of emission spectrometer
3 Principle
The low-carbon test portion is decomposed by hydrochloric acid, hydrogen peroxide, hydrofluoric acid and perchloric acid, and in the smoking state, hydrochloric acid is added dropwise to volatilize chromium to prepare hydrochloric acid solution; the high-carbon test portion is melted with sodium peroxide in a nickel crucible, leached with acid, and diluted to a certain volume. The emission spectrum intensity of analytical elements in the test solution or the relative intensity of yttrium is measured by inductively coupled plasma atomic emission spectrometer (ICP-AES) using high salt resistant atomizer and corresponding atomizing chamber, and the mass fraction of analytical elements is calculated based on the calibration curve.
4 Reagents
In the analysis, unless otherwise specified, only reagents with superior purity and above and water at laboratory Grade II and above in accordance with GB/T 6682 shall be used.
4.1 Pure chromium with the content of the element to be tested less than 0.001% (m/m).
4.2 Pure iron (≥ 99.98% or analytical element known).
4.3 Sodium peroxide.
4.4 Perchloric acid, ρ = 1.67 g/mL.
4.5 Hydrofluoric acid, ρ = 1.15 g/mL.
4.6 Hydrogen peroxide (30%).
4.7 Hydrochloric acid, ρ = 1.19 g/mL.
4.8 Hydrochloric acid, 1+1.
Contents
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents
5 Apparatus
6 Specimens
7 Analysis procedure
8 Calculation and representation of results
9 Permissible deviation
10 Test report
Annex A (Normative) Performance test of inductively coupled plasma spectrometer
Annex B (Normative) Flow chart of specimen analysis result acceptance procedure
