GB/T 9722-2023 PDF English
US$320.00 · In stock · Download in 9 secondsGB/T 9722-2023: Chemical reagent - General rules for the gas chromatography Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedureStatus: Valid GB/T 9722: Evolution and historical versions
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GB/T 9722-2023 | English | 320 |
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Chemical reagent - General rules for the gas chromatography
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GB/T 9722-2006 | English | 225 |
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Chemical reagent -- General rules for the gas chromatography
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GB/T 9722-1988 | English | 439 |
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Chemical reagent--General rules for the gas chromatography
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GB/T 9722-2023: Chemical reagent - General rules for the gas chromatography---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/GBT9722-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.040.30
CCS G 60
Replacing GB/T 9722-2006
Chemical Reagent - General Rules for the Gas
Chromatography
Issued on. AUGUST 6, 2023
Implemented on. MARCH 1, 2024
Issued by. State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
1 Scope... 5
2 Normative References... 5
3 Terms and Definitions... 5
4 Method and Principle... 6
5 Reagents and Materials... 6
6 Instruments... 6
7 Test Conditions... 7
8 Operating Method... 8
9 Qualitative Analysis... 11
10 Quantitative Analysis... 12
11 Method Error... 17
12 Data Quality Assurance... 18
13 Environmental Requirements, Safety Precautions and Waste Disposal... 19
Appendix A (informative) Chromatographic Columns... 21
Appendix B (normative) Illustrations and Calculation Formulas of Related Terms... 24
Appendix C (informative) Acceptable Ranges of Precision and Trueness of the Method
... 26
Bibliography... 27
1 Scope
This document specifies the instrument requirements and analytical methods for the gas
chromatography for chemical reagent.
This document is applicable to the determination of main components and impurities of organic
chemical reagents containing volatile components.
2 Normative References
The contents of the following documents constitute indispensable clauses of this document
through the normative references in the text. 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 4946 Terms of Gas Chromatography
GB 4962 Technical Safety Regulation for Gaseous Hydrogen Use
GB/T 8170 Rules of Rounding off for Numerical Values & Expression and Judgement of
Limiting Values
JJG 700 Gas Chromatographs
TSG 23-2021 Regulation on Safety Technology for Gas Cylinder
3 Terms and Definitions
What is defined in GB/T 4946, and the following terms and definitions are applicable to this
document.
3.1 asymmetric factor
A parameter that describes the degree of asymmetry of a chromatographic peak.
3.2 height of an effective plate
The length of unit effective plate.
4 Method and Principle
After the sample and its components being determined are vaporized, they enter the
chromatographic column at the same time with the carrier gas. The difference in physical and
chemical properties, such as. adsorption or dissolution, desorption or analysis of each
component being determined between the gas-solid or gas-liquid phases is used to form a
difference in the migration speed of the components in the column for separation.
5 Reagents and Materials
5.1 Standard Sample
The mass fraction of the main body content of the standard sample shall not be lower than
99.9%. When high-purity standard samples cannot be obtained for special substances, standard
samples with clarified main body content shall be used.
5.2 Reference Substance
The reference substance shall be traceable to International System of Units (SI) or certified
reference substance.
5.3 Carrier Gas
The purity is not lower than 99.99%. Before use, dehydration devices (silica gel and molecular
sieve), activated carbon and deoxidizer, etc. shall be used for purification.
5.4 Combustion Gas
The purity is not lower than 99.99%. Before use, dehydration devices (silica gel and molecular
sieve), activated carbon and deoxidizer, etc. shall be used for purification.
5.5 Air
It does not contain dust, hydrocarbons, moisture and corrosive substances that may affect the
normal operation of the instrument. Before use, dehydration devices (silica gel and molecular
sieve) and activated carbon, etc. shall be used for purification.
6 Instruments
6.1 Composition of Gas Chromatograph
The gas chromatograph consists of gas path system, sample injection system, separation system,
detection system, temperature control system and data processing system, as shown in Figure 1.
6.2 Performance of Gas Chromatograph
The performance requirements for the gas chromatograph shall comply with the requirements
of JJG 700.
6.3 Chromatographic Columns
The chromatographic columns are divided into capillary columns and packed columns. The
important parameters of chromatographic columns are stationary phase, inner diameter, column
length and liquid film thickness. The users shall select appropriate chromatographic columns
based on sample properties. See Appendix A for the parameters of capillary chromatographic
columns and the preparation and handling of packed columns.
7 Test Conditions
In accordance with the characteristics and specifications requirements of the product and the
components to be determined, select the optimum conditions as specified below.
8 Operating Method
8.1 Peak Height Measurement
Draw a vertical line from the top of the peak to the bottom of the peak. The distance from the
point where the vertical line intersects with the upper edge of the chromatographic peak baseline
to the top is the peak height (h). Or calculate the difference between the signal value at the peak
apex and the baseline signal value at the same retention time as the peak apex (see Figure 2).
8.2 Measurement of Peak Width at Half Height
Draw a straight line parallel to the peak bottom from the midpoint of the peak height and
intersect with both sides of the peak. The distance between two points on the same side of the
peak height line is the peak width at half height (Wh/2) (see Figure 2).
8.3 Calculation of Peak Area
Calculate the integrated value of the difference between the signal value and the baseline signal
value from the start of the peak to the end of the peak; or the product of the peak height and the
peak width at half height.
8.4 Overlapping Peak Area Segmentation Method
8.4.1 Vertical method
As shown in Figure 3, when the areas of two peaks are similar, draw a vertical line from the
peak valley toward the baseline to divide the peak on the baseline into two parts, so as to obtain
the respective peak areas.
8.4.2 Peak-valley - peak-valley method
As shown in Figure 4, in accordance with the adjacent peak valley and peak valley linear
distribution, obtain the corresponding peak area. This method is applicable to background
overlapping peaks.
8.4.3 Tangent method
As shown in Figure 4, when a small peak overlaps the tail of a large peak, draw a tangent line
from the peak valley to the foot of the large peak, and use the part above the tangent line as the
area of the small peak. The exponential function curve method can also be used instead of the
tangent method for peak segmentation.
9 Qualitative Analysis
9.1 Comparative Qualitative Analysis of Known Substance
9.1.1 Adding known substance to increase peak height
Under the same chromatographic conditions, add a known substance to the sample to be tested,
and compare the changes in the chromatographic peak height of the sample to be tested before
and after the addition. If the peak of the component to be determined in the sample to be tested
increases, it can be considered that the component and the known substance are the same
substance.
9.1.2 Qualitative analysis with double-column or multi-column
On two or more chromatographic columns of different polarities, respectively analyze the
known substance and the sample to be tested under the same chromatographic conditions. If the
retention values of the known substance and unknown component in the sample to be tested are
the same on different chromatographic columns, the component and the known substance can
be considered to be the same substance.
9.2 Qualitative Analysis of Relative Retention Value
9.2.1 Under the same chromatographic conditions, respectively perform chromatographic
analysis on the standard sample and the sample to be tested and calculate the relative retention
Baseline
9.2.2 If the standard sample cannot be obtained, the relative retention value of the known
substance can be obtained by searching the literature, then, under the test conditions (column
temperature, stationary phase and reference substance) provided by the literature value,
determine the relative retention value of the sample to be tested; if it is consistent with the
literature value, it can be identified as the same substance.
10 Quantitative Analysis
10.1 Correction Factor
10.1.1 General requirements
This document adopts a mass correction factor for component i relative to the main body.
For individual components listed in technical indicators, the mass correction factor will be used
regardless of the mass fraction. Among the components to be determined, for homologues with
relatively close carbon numbers or substances with small thermal conductivity differences, a
correction factor may be added depending on the specific situation.
10.2 Normalization Method
When adopting the normalization method for quantitative analysis, the following requirements
shall be satisfied.
10.4 External Standard Method
10.4.1 General requirements
When adopting the external standard method for quantitative analysis, the following
requirements shall be satisfied.
10.4.2 Single-point external standard method
Prepare a standard solution with a mass fraction close to that of the component to be determined.
In accordance with the same determination conditions, respectively determine the standard
solution and the sample to be tested. Through the peak area ratio of the component to be
determined and the external standard component, calculate the mass fraction of the component
to be determined.
10.4.3 Standard curve method
Prepare no less than 5 standard solutions with proportional mass fractions and quantitatively
inject the sample. Take the mass fraction of the component to be determined as the x-coordinate
and the measured peak area as the y-coordinate to draw a standard working curve. Under the
same determination conditions, inject the same amount of the sample to be tested for
chromatographic analysis, determine the peak area of the sample, and in accordance with the
standard working curve, calculate the mass fraction of the component to be determined (see
Figure 6).
10.6 Result Expression
10.6.1 The arithmetic mean of two repeated determination results shall be used as the test result,
which shall be rounded in accordance with the stipulations of GB/T 8170.
10.6.2 When the mass fraction of the component to be tested is not less than 1%, the test result
shall be accurate to 0.01% (mass fraction).
10.6.3 When the mass fraction of the component to be tested is not less than 0.01% and less
than 1%, the test result shall be accurate to 0.001% (mass fraction).
...... Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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