GB/T 30903-2014 English PDF (GBT30903-2014)

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GB/T 30903-2014: Inorganic chemicals for industrial use -- Determination of impurity element -- Inductively coupled plasma mass spectrometry (ICP-MS)
GB/T 30903-2014
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.01
G 10
Inorganic chemicals for industrial use - Determination of
impurity element - Inductively coupled plasma mass
spectrometry (ICP-MS)
ISSUED ON. JULY 08, 2014
IMPLEMENTED ON. DECEMBER 01, 2014
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... 4
2 Normative references... 4
3 Terms and definitions... 5
4 Principle... 6
5 Reagents... 6
6 Instruments, devices... 6
7 Analysis steps... 7
8 Precision... 11
9 Recovery rate... 11
Annex A (normative) Quartz sub-boiling distillation unit... 13
Annex B (normative) Detection limit determination method... 14
Inorganic chemicals for industrial use - Determination of
impurity element - Inductively coupled plasma mass
spectrometry (ICP-MS)
WARNING -- Some of the reagents used in this test method are toxic or corrosive.
Be careful when operating! If splashed on the skin, rinse with water immediately,
and seek medical treatment immediately in severe cases. This test method uses
high-pressure argon cylinders, which shall be operated in accordance with the safe
operation regulations of high-pressure cylinders. After igniting the plasma, the
torch chamber door shall not be opened to prevent high-frequency radiation from
harming the body. Pay attention to safe use of electricity.
1 Scope
This Standard specifies the principle, reagents, instruments, equipment, analytical
procedures, precision and recovery rate for the determination of metallic and non-
metallic impurity elements in inorganic chemical products by inductively coupled
plasma mass spectrometry (ICP-MS).
This Standard is applicable to liquid samples containing multiple metal and non-metal
impurity elements in inorganic chemical products or direct sampling after removing the
matrix. Determination is carried out using inductively coupled plasma mass
spectrometry (ICP-MS).
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 4470, Analytical spectroscopic methods. Flame emission, atomic absorption
and atomic fluorescence. Vocabulary
GB/T 4842, Argon
GB/T 6379.2, Measurement methods and results -- Accuracy (trueness and precision)
-- Part 2.Determine the standard methods of measurement repeatability and
reproducibility of the basic method
photons from passing through.
3.9 collision/reaction cell
A multipole cavity installed in front of a quadrupole mass spectrometer.
Collision/reaction gas is introduced into the cavity to cause collision and reaction of
ions focused by the multipole, thereby eliminating mass spectrum interference.
3.10 quadrupole mass spectrometer
A mass analyzer that separates ions according to their mass-to-charge ratio (m/z) by
applying a radio frequency voltage and a direct current voltage to a counter electrode.
4 Principle
The specimen solution is introduced into the atomization system by the carrier gas
(argon) for atomization, and then enters the plasma center in the form of aerosol. It is
de-solvated, vaporized, dissociated and ionized in high temperature and inert
atmosphere, and converted into positive ions with positive charge. It enters the mass
spectrometer through the ion collection system. The mass spectrometer separates
according to the mass-to-charge ratio. The ion signal is received by the electron
multiplier. After amplification, it is detected. According to the intensity of the element
mass spectrum peak, each element is qualitatively or quantitatively analyzed.
5 Reagents
5.1 Chemical reagents shall be of high purity and purified (such as quartz sub-boiling
distillation equipment, see Annex A). Common inorganic acids include nitric acid
(HNO3), hydrochloric acid (HCl), hydrofluoric acid (HF), perchloric acid (HClO4),
sulfuric acid (H2SO4), and aqua regia (1HNO3 +3HCl).
5.2 The water used in the experiment shall have a resistivity of no less than 18.2 MΩ·cm.
5.3 Standard solutions shall use certified standard substances.
6 Instruments, devices
Inductively coupled plasma mass spectrometer. consists of an injection system, torch
and plasma, ion lens system, vacuum system, mass analyzer, detector and data
processing system.
7 Analysis steps
7.1 Selection of measurement conditions
7.1.1 Incident power
Select the best power according to the characteristics of the sample to be tested and the
instrument conditions. The general range is 0.8 kW~1.6 kW.
7.1.2 Gas and its flow
According to the torch and analysis requirements, determine the optimal flow rate of
each gas. The argon gas used meets the requirements of GB/T 4842.The general purity
is not less than 99.999%.
7.1.3 Solution lifting rate
The solution lifting rate is generally 0.1 mL/min~1 mL/min.
7.2 Interference and elimination
Interferences in inductively coupled plasma mass spectrometry can be roughly divided
into two categories. One is mass spectrometry interference, which mainly includes
oxide ion interference, divalent ion interference, polyatomic ion interference and
isobaric interference. The other is non-mass spectrometry interference, which mainly
includes matrix effect, physical effect and other interferences. Interference elimination
methods include optimizing instrument parameters, internal standard correction method,
interference equation correction, collision reaction cell technology, dilution correction,
standard addition method, etc.
7.3 Sample processing
7.3.1 Laboratory equipment
7.3.1.1 For general micro and trace analysis, attention shall be paid to the overall
cleanliness of the laboratory. When ultra-trace or high-demand analysis is performed,
an ultra-clean laboratory is generally required.
7.3.1.2 The containers used for solid digestion are generally made of
polytetrafluoroethylene (PTFE) or fluoroplastics (PFA), tetrafluoroethylene with
perfluorinated alkyl side chains. The containers for holding specimen solutions are
generally made of polytetrafluoroethylene (PTFE) or fluoroplastics (PFA),
tetrafluoroethylene with perfluorinated alkyl side chains, or low-density polyethylene
(LDPE) or high-density polyethylene (HDPE) or polypropylene (PP) materials.
7.3.1.3 Before use, the container shall generally be soaked in 20%~30% nitric acid
solution for several hours. After rinsing with ultrapure water, place it in an electric
is shown in Annex B.
The specimen solution measured on ICP-MS shall meet the following basic
requirements.
a) The total dissolved solids (TDS) in the solution is < 0.2%;
b) The content of organic matter in the solution cannot be too high, otherwise it will
cause serious matrix effects and carbon particles after the combustion of organic
matter will be deposited and block the cone mouth, resulting in reduced sensitivity
and stability. If the content of organic matter is high, an organic oxygenation
channel, an organic-resistant injection system and a platinum cone shall be
equipped;
c) The concentration of the element to be tested in the solution cannot be too high.
Generally, the element content in solid samples is required to be ...