GB/T 37837-2019 PDF English
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General rules for quadrupole inductively coupled plasma mass spectrometry
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GB/T 37837-2019: General rules for quadrupole inductively coupled plasma mass spectrometry---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT37837-2019
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.040.99
N 50/59
General Rules for Quadrupole Inductively Coupled Plasma
Mass Spectrometry
Issued on: AUGUST 30, 2019
Implemented on: MARCH 1, 2020
Issued by. State Administration for Market Regulation;
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... 4
4 Principle of Analytical Method... 6
5 Reagents and Materials... 7
6 Instruments and Equipment... 8
7 Samples... 9
8 Analytical Procedures and Methods... 10
9 Result Report... 18
10 Safety Precautions... 20
Appendix A (informative) Correction Formulas of Internal Standard Method... 21
General Rules for Quadrupole Inductively Coupled Plasma
Mass Spectrometry
1 Scope
This Standard specifies the methods and principles, reagents and materials, instruments and
equipment, sample requirements, analytical procedures and methods, result report, and safety
precautions for the detection of metallic and some non-metallic elements in samples using
quadrupole inductively coupled plasma mass spectrometer (abbreviated as Q-ICP-MS).
This Standard applies to the qualitative, semi-quantitative, and quantitative analysis of elements
in samples using a quadrupole inductively coupled plasma mass spectrometer and in the mode
of liquid and gas injection.
This Standard does not apply to the mode of direct solid injection.
2 Normative References
The following documents are indispensable to the application of this document. In terms of
references with a specified date, only versions with a specified date are applicable to this
document. In terms of references without a specified date, the latest version (including all the
modifications) is applicable to this document.
GB/T 602 Chemical Reagent - Preparations of Standard Solutions for Impurity
GB/T 4842 Argon
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
GB/T 13966 Terminology for Analytical Instruments
GB/T 27411 Routine Methods for Evaluation and Expression of Measurement Uncertainty in
Testing Laboratory
JJF 1159 Calibration Specification for Quadrupole Inductively Coupled Plasma Mass
Spectrometers
3 Terms and Definitions
The terms and definitions defined in GB/T 13966, GB/T 27411 and JJF 1159, and the following
terms and definitions are applicable to this document.
3.1 plasma
A conical component that combines plasma with a high-vacuum mass spectrometer. There is a
circular hole approximately 1 mm in diameter at the center, which utilizes a pressure differential
to draw most of the ions in the central channel of the plasma into the first-stage vacuum chamber.
3.12 skimmer cone
A conical component that connects the sampler cone to the high-vacuum mass spectrometer.
There is a circular hole less than 1 mm in diameter at the center, concentric with the axial
direction of the sampler cone hole, which introduces the central part of the expanded ion jet
through the sampler cone hole into the mass spectrometer.
3.13 ion lens
An electric and / or magnetic field device that focuses and images the ion beam.
[GB/T 13966-2013, Definition 6.104]
3.14 ion detector
A component used to collect and / or amplify the ion stream from the mass analyzer.
[GB/T 13966-2013, Definition 6.126]
3.15 quadrupole mass analyzer
mass filter
quadrupole mass filter
A mass analyzer consisting of a quadrupole field composed of a superimposed DC and RF field.
Under given field parameters, ions of different mass-to-charge ratios are in stable or unstable
orbital motion within the field. Stable ions are collected, while unstable ions are filtered out.
[GB/T 13966-2013, Definition 6.123]
3.16 mass discrimination effect
In mass spectrometry, the phenomenon that separation based on mass-to-charge ratio cannot be
completely achieved.
[GB/T 13966-2013, Definition 6.169]
4 Principle of Analytical Method
This is an inorganic multi-element analysis technique using inductively coupled plasma as the
ion source and quadrupole mass analyzer for detection. The specimen is introduced into the
plasma via a carrier gas in a certain form, where it undergoes de-solvation, vaporization,
dissociation, and ionization in a high-temperature, inert atmosphere. A portion of the plasma
passes through different pressure zones and enters a vacuum system. Within the vacuum system,
positive ions are extracted and separated in accordance with their mass-to-charge ratio before
being detected by an ion detector. Qualitative analysis can be performed based on the mass-to-
charge ratio, while quantitative analysis can be performed based on the detection signal at a
specific mass-to-charge ratio.
5 Reagents and Materials
5.1 Argon
Shall comply with the requirements of GB/T 4842, with a volume fraction of 99.99%.
5.2 Water
Water for trace element analysis shall comply with GB/T6682, Grade 1.Water for other tests
shall comply with GB/T 6682, Grade 2.
5.3 Hydrochloric Acid
Guaranteed reagent or higher specifications shall be selected.
5.4 Nitric Acid
Guaranteed reagent or higher specifications shall be selected.
5.5 Other Reagents
Other reagents used in the analysis shall be analytically pure or higher specifications.
5.6 Standard Solutions
5.6.1 Standard stock solutions
5.6.1.1 Single-element standard stock solution
A certified single-element standard solution (with a concentration of 1,000 g/mL or 100
g/mL) may be used. Where appropriate, high-purity metals (with a purity greater than or equal
to 99.99%), oxides or salts (reference or high-purity reagents) may be used to prepare the
solution in accordance with GB/T 602.
5.6.1.2 Multi-element standard stock solution
A certified multi-element standard solution may be used. Where appropriate, the solution may
be prepared by mixing the single-element standard stock solution (see 5.6.1.1). When mixing
the single-element standard stock solution, cross-contamination of the ions being determined
and the effects of anions in the solution shall be considered to avoid the generation of poorly or
slightly soluble substances.
5.6.2 Standard series solutions
Dilute the single-element standard stock solution (see 5.6.1.1) or the multi-element standard
stock solution (see 5.6.1.2) into standard series solutions of varying concentrations, with the
final solution containing 1% ~ 5% (volume fraction) acid medium.
6 Instruments and Equipment
6.1 Overview
The main components of a quadrupole inductively coupled plasma mass spectrometer shall
include sample injection system, ion source, interface, ion focusing system, quadrupole mass
analyzer, vacuum system, detection system, control and data processing system, and an optional
collision / reaction system. The instrument shall be equipped with a ventilation system and a
power supply system.
6.2 Sample Injection System
This system includes three modes for sample injection. liquid, gas and solid. The mode of liquid
injection is preferred. Its main components shall include peristaltic pump, nebulizer and spray
chamber.
6.3 Ion Source
An ion source shall be provided to provide specimen ionization energy. The ion source shall
consist of radio frequency generator, coupled coil, plasma torch tube and gas supply system.
6.4 Interface
There shall be two types. sampler cone and skimmer cone. An extraction lens or a second
skimmer cone can be added after the skimmer cone.
6.5 Ion Focusing System
An ion lens or a 90 ion deflection system shall be used.
6.6 Quadrupole Mass Analyzer
It shall consist of four parallel metal or metal-plated rods, with two rods arranged in pairs.
6.7 Vacuum System
It shall consist of mechanical pump, molecular turbopump, various high-performance sealing
valves, and vacuum pipeline, etc.
6.8 Detection System
It shall consist of ion collector and amplifier.
6.9 Control and Data Processing System
It shall consist of computer and corresponding software to realize instrument operation,
adjustment and control of various parameters, determination and data processing, etc.
6.10 Collision / Reaction System
It shall utilize collisions and / or reactions between molecules and ions to eliminate polyatomic
and / or molecular ion interference from the ion beam.
6.11 Power Supply System
It shall be able to provide the mass spectrometer with a regulated voltage and current power
supply, quadrupole DC power supply, high-frequency AC power supply and plasma RF power
supply, and good automatic control and protection for the instrument.
6.12 Instrument Type
The following types of instruments may be used.
a) Single quadrupole inductively coupled plasma mass spectrometers with only one
quadrupole capable of mass screening;
b) Multi-quadrupole inductively coupled plasma mass spectrometers with two or more
quadrupoles capable of mass screening.
6.13 Instrument Verification or Calibration
Before commissioning, equipment that may affect the accuracy or validity of the test and
analysis results, as well as auxiliary measurement equipment used to measure environmental
conditions, shall be verified or calibrated. Verification or calibration shall be performed in
accordance with the requirements of JJF 1159.
7 Samples
7.1 Liquid Samples
7.1.1 Direct determination
7.1.1.1 Inorganic solution samples containing the component to be analyzed within the linear
range of the instrument analysis may be directly injected for determination. Samples containing
suspended matter, such as groundwater, tap water and surface water, shall be filtered prior to
injection for determination.
7.1.1.2 For organic solutions, if the instrument is equipped with a sample injection system for
organic matter, direct injection for determination is permitted. If the instrument is not equipped
with the sample injection system for organic matter, the sample shall be treated before being
injected for determination.
7.1.2 Determination after dilution or concentration
If the content of the element to be determined in the sample is excessively high and exceeds the
calibration curve range, the sample shall be appropriately diluted before determination. If the
content of the element to be determined in the sample is below the quantification limit, it can
be concentrated and enriched for determination.
7.1.3 Determination after digestion
When determining the element to be determined in liquid samples containing organic matter,
other special media, or suspended matter, the sample shall be digested using wet, dry or
microwave digestion methods before determination.
7.2 Solid Samples
7.2.1 When determining the content of soluble elements, the sample shall be immersed or
extracted with a certain volume of an appropriate solvent. After such treatment, take the
supernatant and carry out the determination in accordance with the requirements of 7.1.
7.2.2 When determining the total amount of the element to be determined, the sample shall be
digested using an appropriate method before analysis. Given the diversity of solid sample types,
appropriate treatment methods shall be selected based on the sample’s characteristics, such as
wet digestion, dry digestion or microwave digestion. The sample size shall be determined based
on the salt tolerance of the instrument, the precision of the analytical method and the accuracy
requirements of the analysis results.
7.3 Gaseous Samples
Direct sample injection for determination, absorption or enrichment by an absorption liquid or
gas sampling membrane may be selected for determination. When using an absorption liquid
or gas sampling membrane, the absorption liquid or membrane shall be treated in accordance
with the requirements of 7.1 or 7.2.
7.4 Experimental Procedure Blank
It shall be identical to the sample treatment process, using the same reagents, volumes and
treatment steps. The corresponding experimental procedure blank value shall be subtracted
from the sample analysis results.
8 Analytical Procedures and Methods
8.1 Analytical Procedures
8.1.1 Power-on pre-heating
After powering on the instrument, turn on the power supply to the host machine and computer,
enable vacuum, and switch the instrument from shutdown to standby mode. Before starting the
plasma, it shall be ensured that there is sufficient argon gas for continuous operation and that
the waste collection barrel has sufficient space for waste liquid collection. Open the ventilation
system and adjust the argon gas pressure output to meet the instrument’s normal operation
requirements. Open the water-cooling circulation system, start the plasma, and after the plasma
stabilizes, start the determination.
8.1.2 Selection of analytical conditions
8.1.2.1 Before sample analysis, an analytical method appropriate for the sample to be analyzed
shall be established. In accordance with the analytical demands, select parameters such as ion
lens parameters, ICP power, gas flow rates (coolant gas, auxiliary gas and carrier gas),
peristaltic pump speed, integration time, analytical element and its mass-to-charge ratio,
internal standard element, torch tube position, sampling depth, mass spectrometry measurement
mode, and instrument resolution, etc. The principle of selection is to ensure strong signals for
most elements simultaneously measured, with high precision and minimal interference.
Instrument signal-to-background ratio test or method detection limit test may be performed in
accordance with the requirements of the instrument instruction manual to determine the optimal
operating conditions of the instrument.
8.1.2.2 When using a multi-quadrupole inductively coupled plasma mass spectrometer for
analysis, the parameters of the first-stage quadrupole, collision / reaction cell, and second-stage
quadrupole also need to be set.
8.1.3 Sample analysis
In accordance with the analytical method in 8.2, analyze the sample. During the analysis,
interference elimination and quality control steps shall be added.
8.1.4 Completion of analysis
After the analysis is completed, use 5% (volume fraction) nitric acid solution to inject the
sample for approximately 5 minutes, followed by water (see 5.2) for approximately 5 minutes.
In accordance with the instrument operating manual, place the instrument on standby or
shutdown mode.
8.2 Analytical Method
8.2.1 Interference elimination
8.2.1.1 Physical interference
Physical interference can be corrected using the internal standard method, matrix matching
method, or standard addition method.
8.2.1.2 Isobaric interference
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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