GB/T 41071-2021 English PDF (GB/T41071-2021)

GB/T 41071-2021: Determination of polycyclic aromatic hydrocarbons in dye products
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GB/T 41071-2021
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.01;87.060.01
CCS G 55
Determination of polycyclic aromatic hydrocarbons in dye
products
ISSUED ON: DECEMBER 31, 2021
IMPLEMENTED ON: JULY 1, 2022
Issued by: State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 4
4 Principle of the method ... 4
5 Reagents or materials ... 5
6 Instruments and equipment ... 5
7 Preparation of standard solutions ... 5
8 Preparation of sample solutions ... 6
9 Analysis steps ... 7
10 Result calculation ... 8
11 Detection limits, precision and accuracy ... 9
12 Test report... 9
Appendix A (Normative) Types of polycyclic aromatic hydrocarbons and reference
parameters for determination ... 11
Appendix B (Informative) Schematic diagram of total ion chromatogram of polycyclic
aromatic hydrocarbon standards ... 12
Determination of polycyclic aromatic hydrocarbons in dye
products
Warning -- The personnel using this document shall have practical experience in
formal laboratory work. This document does not indicate all possible safety issues.
The user is responsible for taking appropriate safety and health measures and
ensuring compliance with the conditions stipulated by relevant national laws and
regulations.
1 Scope
This document specifies a method for the determination of 18 polycyclic aromatic
hydrocarbon residues in dye products by gas chromatography-mass spectrometry
(GC/MS).
This document applies to the determination of polycyclic aromatic hydrocarbons in
various types of dye products.
2 Normative references
The following documents contain the provisions which, through normative reference in
this document, constitute the essential provisions of this document. For the dated
referenced documents, only the versions with the indicated dates are applicable to this
document; for the undated referenced documents, only the latest version (including all
the amendments) is applicable to this document.
GB/T 8170-2008 Rules of rounding off for numerical values and expression and
judgment of limiting values
3 Terms and definitions
There are no terms and definitions that need to be defined in this document.
4 Principle of the method
In an ultrasonic bath, use n-hexane-acetone mixed solvent to extract the polycyclic
aromatic hydrocarbons in the sample, and purify the extract by solid phase extraction
(Florisil SPE column); after condensing the eluant and making up to the scale, use a gas
chromatography-mass spectrometer (GC/MS) for separation and determination, and
adopt peak area external standard method for quantification.
5 Reagents or materials
5.1 The types of standard polycyclic aromatic hydrocarbons and the reference
parameters for determination shall comply with the provisions of Appendix A.
5.2 Dichloromethane, chromatographically pure.
5.3 n-hexane, chromatographically pure.
5.4 Acetone, chromatographically pure.
5.5 n-hexane-acetone mixed solvent: The volume ratio of n-hexane and acetone is 1:1.
5.6 n-hexane-dichloromethane mixed solvent: The volume ratio of n-hexane and
dichloromethane is 8:2.
5.7 Florisil column (SPE column): 1000 mg, 6 mL.
6 Instruments and equipment
6.1 Gas chromatography-mass spectrometer (GC/MS): with EI source.
6.2 Chromatographic column: 50% phenylmethyl polysiloxane solid phase, such as
DB-17MS, 30 m×0.25 mm×0.25 μm, or equivalent.
6.3 Analytical balance: The accuracy shall be 0.01 mg.
6.4 Ultrasonic generator.
6.5 Extractor: a tube with a stopper, 10 mL.
6.6 Centrifuge: 4000 r/min.
6.7 Nitrogen-blowing concentrator.
6.8 Solid phase extraction device.
7 Preparation of standard solutions
7.1 Polycyclic aromatic hydrocarbon single standard stock solutions
Respectively weigh 10 mg of the standard substances listed in Appendix A, and the
weights shall be accurate to 0.01 mg; dissolve with n-hexane and dilute to the mark in
collect the supernatant of the extract. If the sample is completely dissolved, the
ultrasonic extraction step can be omitted. Analyze it later with instruments.
8.2 Concentrating and solvent replacement
Adopt the nitrogen blowing concentrating method, and the temperature of the nitrogen
blowing concentrator shall be set to 30 °C; concentrate the extract (8.1) to 1 mL~2 mL
with a small flow rate of nitrogen, wash the wall of the concentrating tube with about 5
mL~10 mL of n-hexane, and then concentrate the liquid to about 1 mL. Purify it later.
8.3 Purification
Fix the Florisil column on the solid-phase extraction device, rinse and purify the column
with 4 mL of acetone, and then add 4 mL of n-hexane. After the column is filled, close
the control valve and soak for 5 min; then, slowly open the control valve, and close the
control valve before the filler is exposed to air. Transfer the concentrated solution (8.2)
to the column, wash the concentrating tube several times with about 2 mL of n-hexane
in total, and transfer all the washing liquor to the column. Slowly open the control valve
and collect the effluent. Before the adsorbent is exposed to air, add about 8 mL of n-
hexane-dichloromethane mixed solvent (5.6) for elution, and collect all the eluent.
8.4 Concentrating and making the volume up to mark
The purified eluent shall be concentrated by nitrogen blowing, made up to 1.0 mL with
n-hexane, mixed well, and transferred to a sample bottle for analysis later.
8.5 Preparation of blank samples
Prepare blank samples following the same procedures as for sample solution
preparation.
9 Analysis steps
9.1 Chromatographic analysis conditions
Since the test results depend on the instrument used, it is impossible to offer general
parameters for chromatographic analysis. The use of the parameters in Table 1 has been
proved suitable for testing. The optimal analysis conditions can be selected according
to different instruments and equipment.
V --- The value of the metered volume of the sample solution, in milliliters (mL);
As --- The peak area value of the target quantitative ion in the standard working
solution;
m --- The value of the mass of the sample, in grams (g).
The calculation result is retained to two decimal places.
The calculation results are rounded off according to the provisions of GB/T 8170-2008.
11 Detection limits, precision and accuracy
11.1 Detection limit
If Method One in Chapter 8 is used for the preparation of the sample solution, the
method detection limit of 18 types of polycyclic aromatic hydrocarbons is 0.2 mg/kg;
If Method Two is used for the preparation of the sample solution, the method detection
limit is 1.0 mg/kg.
11.2 Precision
In the same laboratory, the same operator uses the same equipment to carry out
independent tests on the same test object within a short period of time according to the
same determination method; the absolute difference between two independent test
results shall not be greater than 20% of the arithmetic mean of the two determination
results.
11.3 Accuracy
Adopting the standard addition method, add an appropriate amount of polycyclic
aromatic hydrocarbon standard solution to 1 g of dye sample, the concentration of the
standard addition is 10 mg/kg, and operate according to the provisions of Chapter 8 and
Chapter 9; the measured recovery of polycyclic aromatic hydrocarbons (except
naphthalene) shall be 70%~120%, and the recovery of naphthalene shall be 60%~120%.
12 Test report
The test report shall at least include the following content:
a) Description of the sample;
b) The document number;
c) Test conditions;
GB/T 41071-2021
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.01;87.060.01
CCS G 55
Determination of polycyclic aromatic hydrocarbons in dye
products
ISSUED ON: DECEMBER 31, 2021
IMPLEMENTED ON: JULY 1, 2022
Issued by: State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 4
4 Principle of the method ... 4
5 Reagents or materials ... 5
6 Instruments and equipment ... 5
7 Preparation of standard solutions ... 5
8 Preparation of sample solutions ... 6
9 Analysis steps ... 7
10 Result calculation ... 8
11 Detection limits, precision and accuracy ... 9
12 Test report... 9
Appendix A (Normative) Types of polycyclic aromatic hydrocarbons and reference
parameters for determination ... 11
Appendix B (Informative) Schematic diagram of total ion chromatogram of polycyclic
aromatic hydrocarbon standards ... 12
Determination of polycyclic aromatic hydrocarbons in dye
products
Warning -- The personnel using this document shall have practical experience in
formal laboratory work. This document does not indicate all possible safety issues.
The user is responsible for taking appropriate safety and health measures and
ensuring compliance with the conditions stipulated by relevant national laws and
regulations.
1 Scope
This document specifies a method for the determination of 18 polycyclic aromatic
hydrocarbon residues in dye products by gas chromatography-mass spectrometry
(GC/MS).
This document applies to the determination of polycyclic aromatic hydrocarbons in
various types of dye products.
2 Normative references
The following documents contain the provisions which, through normative reference in
this document, constitute the essential provisions of this document. For the dated
referenced documents, only the versions with the indicated dates are applicable to this
document; for the undated referenced documents, only the latest version (including all
the amendments) is applicable to this document.
GB/T 8170-2008 Rules of rounding off for numerical values and expression and
judgment of limiting values
3 Terms and definitions
There are no terms and definitions that need to be defined in this document.
4 Principle of the method
In an ultrasonic bath, use n-hexane-acetone mixed solvent to extract the polycyclic
aromatic hydrocarbons in the sample, and purify the extract by solid phase extraction
(Florisil SPE column); after condensing the eluant and making up to the scale, use a gas
chromatography-mass spectrometer (GC/MS) for separation and determination, and
adopt peak area external standard method for quantification.
5 Reagents or materials
5.1 The types of standard polycyclic aromatic hydrocarbons and the reference
parameters for determination shall comply with the provisions of Appendix A.
5.2 Dichloromethane, chromatographically pure.
5.3 n-hexane, chromatographically pure.
5.4 Acetone, chromatographically pure.
5.5 n-hexane-acetone mixed solvent: The volume ratio of n-hexane and acetone is 1:1.
5.6 n-hexane-dichloromethane mixed solvent: The volume ratio of n-hexane and
dichloromethane is 8:2.
5.7 Florisil column (SPE column): 1000 mg, 6 mL.
6 Instruments and equipment
6.1 Gas chromatography-mass spectrometer (GC/MS): with EI source.
6.2 Chromatographic column: 50% phenylmethyl polysiloxane solid phase, such as
DB-17MS, 30 m×0.25 mm×0.25 μm, or equivalent.
6.3 Analytical balance: The accuracy shall be 0.01 mg.
6.4 Ultrasonic generator.
6.5 Extractor: a tube with a stopper, 10 mL.
6.6 Centrifuge: 4000 r/min.
6.7 Nitrogen-blowing concentrator.
6.8 Solid phase extraction device.
7 Preparation of standard solutions
7.1 Polycyclic aromatic hydrocarbon single standard stock solutions
Respectively weigh 10 mg of the standard substances listed in Appendix A, and the
weights shall be accurate to 0.01 mg; dissolve with n-hexane and dilute to the mark in
collect the supernatant of the extract. If the sample is completely dissolved, the
ultrasonic extraction step can be omitted. Analyze it later with instruments.
8.2 Concentrating and solvent replacement
Adopt the nitrogen blowing concentrating method, and the temperature of the nitrogen
blowing concentrator shall be set to 30 °C; concentrate the extract (8.1) to 1 mL~2 mL
with a small flow rate of nitrogen, wash the wall of the concentrating tube with about 5
mL~10 mL of n-hexane, and then concentrate the liquid to about 1 mL. Purify it later.
8.3 Purification
Fix the Florisil column on the solid-phase extraction device, rinse and purify the column
with 4 mL of acetone, and then add 4 mL of n-hexane. After the column is filled, close
the control valve and soak for 5 min; then, slowly open the control valve, and close the
control valve before the filler is exposed to air. Transfer the concentrated solution (8.2)
to the column, wash the concentrating tube several times with about 2 mL of n-hexane
in total, and transfer all the washing liquor to the column. Slowly open the control valve
and collect the effluent. Before the adsorbent is exposed to air, add about 8 mL of n-
hexane-dichloromethane mixed solvent (5.6) for elution, and collect all the eluent.
8.4 Concentrating and making the volume up to mark
The purified eluent shall be concentrated by nitrogen blowing, made up to 1.0 mL with
n-hexane, mixed well, and transferred to a sample bottle for analysis later.
8.5 Preparation of blank samples
Prepare blank samples following the same procedures as for sample solution
preparation.
9 Analysis steps
9.1 Chromatographic analysis conditions
Since the test results depend on the instrument used, it is impossible to offer general
parameters for chromatographic analysis. The use of the parameters in Table 1 has been
proved suitable for testing. The optimal analysis conditions can be selected according
to different instruments and equipment.
V --- The value of the metered volume of the sample solution, in milliliters (mL);
As --- The peak area value of the target quantitative ion in the standard working
solution;
m --- The value of the mass of the sample, in grams (g).
The calculation result...