GB/T 23322-2018 PDF in English
GB/T 23322-2018 (GB/T23322-2018, GBT 23322-2018, GBT23322-2018)
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Textiles -- Determination of surfactant -- Alkylphenols and Alkylphenol ethoxylates
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| GB/T 23322-2009 | English | 559 |
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GB/T 23322-2018: PDF in English (GBT 23322-2018) GB/T 23322-2018
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
W 04
Replacing GB/T 23322-2009
Textiles - Determination of surfactant - Alkylphenols and
alkylphenol ethoxylates
ISSUED ON: DECEMBER 28, 2018
IMPLEMENTED ON: JULY 01, 2019
Issued by: State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Principles ... 4
4 Reagents or materials ... 5
5 Instruments and equipment ... 6
6 Measurement steps ... 6
7 Calculation and presentation of results ... 9
8 Lower limit of determination, recovery, precision of the method ... 12
9 Test report ... 12
Appendix A (Informative) Determination method of alkylphenol and alkylphenol
ethoxylates by reversed-phase high performance liquid chromatography ... 13
Appendix B (Informative) Determination method of alkylphenol and alkylphenol
ethoxylates by normal phase high performance liquid chromatography ... 17
Appendix C (Informative) Hydrophilic interaction chromatography (HILIC)
determination of alkylphenol and alkylphenol ethoxylates ... 23
Appendix D (Informative) Selected ion monitoring chromatograms for the
determination of AP and APEO by LC-MS ... 29
Appendix E (Informative) MS reference conditions ... 31
Textiles - Determination of surfactant - Alkylphenols and
alkylphenol ethoxylates
Caution - The personnel using this standard shall have practical experience in
formal laboratory work. This standard does not address all possible safety issues.
It is the user's responsibility, to take appropriate safety and health measures AND
to ensure compliance with the conditions, which are stipulated by relevant national
regulations.
1 Scope
This standard specifies the liquid chromatography-mass spectrometry detection method
of alkylphenol (AP) and alkylphenol ethoxylates (APnEO, n = 2 ~ 16), in textiles.
This standard applies to all types of textile products.
Note 1: The general molecular structure of AP is: R-C6H4-OH. AP in this standard refers to the
common octylphenol [OP, C8H17-C6H4-OH] and nonylphenol [NP, C9H19-C6H4-OH]. The
general molecular structure of APnEO is: R-C6H4-(OC2H4)nOH. APnEO in this standard refers
to the commonly used octylphenol ethoxylates [OPnEO, C8H17-C6H4-(OC2H4)nOH] and
nonylphenol ethoxylates [NPnEO, C9H19-C6H4-(OC2H4)nOH].
Note 2: For the determination method of reversed-phase high-performance liquid
chromatography, normal-phase high-performance liquid chromatography, hydrophilic
interaction chromatography, of the alkylphenol and alkylphenol ethoxylate, refer to Appendix
A, Appendix B, Appendix C, respectively.
2 Normative references
The following documents are essential to the application of this document. For the dated
documents, only the versions with the dates indicated are applicable to this document;
for the undated documents, only the latest version (including all the amendments) is
applicable to this standard.
GB/T 6682 Water for analytical laboratory use - Specification and test methods
3 Principles
The AP and APnEO in the specimen are extracted by methanol ultrasonically. After the
extract is concentrated and purified, it was determined by liquid chromatography-mass
spectrometer, quantified by external standard method.
4 Reagents or materials
4.1 Unless otherwise specified, the reagents used in this method are all analytically pure;
the water is the grade-1 water, which is specified in GB/T 6682.
4.2 Methanol (HPLC grade).
4.3 Acetonitrile (HPLC grade).
4.4 n-hexane (HPLC grade).
4.5 Isopropanol (HPLC grade).
4.6 Dichloromethane (HPLC grade).
4.7 Methanol-aqueous solution (3 + 2): Accurately take 300 mL of methanol (4.2) and
200 mL of water. Mix well. Prepare for later use.
4.8 Methanol-dichloromethane solution (1 + 4): Accurately take 100 mL of methanol
(4.2) and 400 mL of dichloromethane (4.6). Mix well. Prepare for later use.
4.9 Standard octylphenol (OP, CAS No.140-66-9, purity ≥ 97%).
4.10 Nonylphenol standard (NP, CAS No.25154-52-3, excellent grade pure).
4.11 Standard product of octylphenol ethoxylates (OPnEO, CAS No.9002-93-1,
average degree of polymerization n = 9, excellent grade pure).
4.12 Standard product of nonylphenol ethoxylates (NPnEO, CAS No.9016-45-9,
average degree of polymerization n = 9, purity ≥ 99%).
4.13 Standard stock solution: Accurately weigh an appropriate amount of OP (4.9), NP
(4.10), OPnEO (4.11), NPnEO (4.12), respectively. Use methanol, to prepare a single-
component standard stock solution, which has a concentration of 10 mg/mL.
4.14 Standard working solution: Pipette an appropriate volume of OP, NP, OPnEO,
NPnEO standard stock solution (4.13), respectively. Place in the same volumetric flask.
Use methanol to dilute it. Prepare a mixed standard working solution of the required
concentration.
4.15 Solid phase extraction column: The filler is lipophilic divinylbenzene and
hydrophilic N-vinylpyrrolidone copolymer, 60 mg, 3 mL. Use 2 mL of methanol and 4
mL of water, to activate it in sequence, before use.
4.16 Organic filter membrane: 0.22 μm.
5 Instruments and equipment
5.1 Liquid chromatography-mass spectrometer: Equipped with an electrospray
ionization source (ESI).
5.2 Analytical balance: Sensitivity is 0.0001 g.
5.3 Analytical balance: Sensitivity is 0.01 g.
5.4 Ultrasonic cleaner: The temperature can be controlled at (70 ± 2) °C.
5.5 Rotary evaporator.
5.6 Solid phase extraction device.
5.7 Nitrogen blower.
6 Measurement steps
6.1 Extraction and purification of specimens
Take a representative specimen. Cut it into pieces of about 5 mm × 5 mm. Mix well.
Weigh 1 g of the cut specimen (accurate to 0.01 g). Place it in a 50 mL centrifuge tube.
Add 30 mL of methanol. Extract ultrasonically at (70 ± 2) °C, for (60 ± 5) min.
Concentrate the extract to near dryness, at below 40 °C, by a rotary evaporator. Add 2
mL of methanol accurately, to dissolve the residue. Pass it through a 0.22 µm filter
membrane (4.16). Use it for liquid chromatography-mass spectrometry determination.
When impurities in the specimen (such as silk) interfere with the detection, the
following purification methods are used. Use 10 mL of methanol-water solution (4.7),
to dissolve the residue in the above concentration bottle. Transfer all to the solid phase
extraction column (4.15). Control the flow rate, to be 1 mL/min ~ 2 mL/min. Discard
the effluent. Empty it under reduced pressure, for 10 min. Use 5 mL of methanol-
dichloromethane solution (4.8) to elute it. Collect the eluate. Use nitrogen, to blow dry
the eluent below 40 °C. Add 2 mL of methanol accurately, to dissolve the residue. Pass
it through a 0.22 µm filter membrane (4.16). Then use it for liquid chromatography-
mass spectrometry determination.
6.2 Determination
6.2.1 Reference chromatographic and mass spectrometry conditions for liquid
chromatography-mass spectrometry (LC-MS)
Since the test results depend on the instrument used, it is impossible to give general
parameters for chromatographic analysis. The following parameters have been shown
to be suitable for testing:
Appendix A
(Informative)
Determination method of alkylphenol and alkylphenol ethoxylates by reversed-
phase high performance liquid chromatography
A.1 Overview
This Appendix gives the method for the determination of alkylphenol (AP) and
alkylphenol ethoxylates (APnEO, n = 2 ~ 16) in textiles, by reversed-phase high
performance liquid chromatography.
A.2 Principle
The AP and APnEO in the specimen are extracted ultrasonically by methanol. After the
extract is concentrated and purified, it is determined by a high performance liquid
chromatograph, which is equipped with a fluorescence detector; then quantified by the
external standard method.
A.3 Reagents or materials
Same as Chapter 4.
A.4 Instruments and equipment
A.4.1 High performance liquid chromatograph, which is equipped with fluorescence
detector.
A.4.2 Analytical balance: The sensitivity is 0.0001 g.
A.4.3 Analytical balance: The sensitivity is 0.01 g.
A.4.4 Ultrasonic cleaner: The controllable temperature is (70 ± 2) °C.
A.4.5 Rotary evaporator.
A.4.6 Solid phase extraction device.
A.4.7 Nitrogen blower.
A.5 Determination steps
A.5.1 Extraction and purification of specimen
Take a representative specimen. Cut it into pieces of about 5 mm × 5 mm. Mix well.
Weigh 1 g of the cut specimen (accurate to 0.01 g). Place it in a 50 mL centrifuge tube.
Add 30 mL of methanol. Extract ultrasonically at (70 ± 2) °C, for (60 ± 5) min.
Concentrate the extract to near dryness, at below 40 °C, by a rotary evaporator. Add 2
mL of methanol accurately, to dissolve the residue. Pass it through a 0.22 µm filter
membrane (4.16). Use it for reversed phase liquid chromatography determination.
When impurities in the specimen (such as silk) interfere with the detection, the
following purification methods are used. Use 10 mL of methanol-water solution (4.7),
to dissolve the residue in the above concentration bottle. Transfer all to the solid phase
extraction column (4.15). Control the flow rate, to be 1 mL/min ~ 2 mL/min. Discard
the effluent. Empty it under reduced pressure, for 10 min. Use 5 mL of methanol-
dichloromethane solution (4.8) to elute it. Collect the eluate. Use nitrogen, to blow dry
the eluent below 40 °C. Add 2 mL of methanol accurately, to dissolve the residue. Pass
it through a 0.22 µm filter membrane (4.16). Then use it for reversed-phase high-
performance liquid chromatography determination.
A.5.2 Determination
A.5.2.1 Reference chromatographic conditions
Since the test results depend on the instrument used, it is impossible to give general
parameters for chromatographic analysis. The following parameters have been shown
to be suitable for testing:
a) Chromatographic column: C18 column, 5.0 μm, 4.6 mm × 250 mm, or equivalent;
b) Column temperature: 35 °C;
c) Mobile phase: Methanol-water-acetonitrile (81 + 13 + 6, volume ratio);
d) Detection wavelength: Excitation wavelength 230 nm, emission wavelength 296
nm;
e) Flow rate: 1.0 mL/min;
f) Injection volume: 10 μL.
A.5.2.2 Chromatographic determination
According to the content of AP and APnEO in the sample solution, select the standard
working solution, which has similar concentration (4.14). Equal volumes of standard
working solution and sample solution are injected alternatively, for determination. The
response values of AP and APnEO, in the standard working solution and sample
solution, shall be within the linear range, which is detected by the instrument. Under
the above chromatographic conditions, the retention time of AP and APnEO is as shown
in Table A.1; the liquid chromatogram is as shown in Figure A.1. When the retention
time of the chromatographic peak of the sample solution is consistent with that of the
Appendix B
(Informative)
Determination method of alkylphenol and alkylphenol ethoxylates by normal
phase high performance liquid chromatography
B.1 Overview
This Appendix gives the normal phase high performance liquid chromatography
method, for the determination of alkylphenol (AP) and alkylphenol ethoxylates
(APnEO, n = 2 ~ 16), in textiles.
B.2 Principle
The AP and APnEO in the specimen are extracted ultrasonically by methanol. After the
extract is concentrated and purified, it is determined by a high performance liquid
chromatograph, which is equipped with a fluorescence detector; quantified by the
external standard method.
B.3 Reagents or materials
B.3.1 Unless otherwise specified, the reagents used in this method are all analytically
pure; the water is the grade-1 water, which is specified in GB/T 6682.
B.3.2 Methanol (HPLC grade).
B.3.3 Acetonitrile (HPLC grade).
B.3.4 n-hexane (HPLC grade).
B.3.5 Isopropanol (HPLC grade).
B.3.6 Dichloromethane (HPLC grade).
B.3.7 Methanol-water solution (3 + 2): Accurately measure 300 mL of methanol (B.3.2)
and 200 mL of water. Mix well. Prepare for use.
B.3.8 Methanol-dichloromethane solution (1 + 4): Accurately measure 100 mL of
methanol (4.2) and 400 mL of dichloromethane (B.3.6). Mix well. Prepare for use.
B.3.9 Standard octylphenol (OP, CAS No.140-66-9, purity ≥ 97%).
B.3.10 Nonylphenol standard (NP, CAS No.25154-52-3, excellent grade pure).
B.3.11 Standard product of octylphenol ethoxylates (OPnEO, CAS No.9002-93-1,
average degree of polymerization n = 9, excellent grade pure).
B.3.12 Standard product of nonylphenol ethoxylates (NPnEO, CAS No.9016-45-9,
average degree of polymerization n = 9, purity ≥ 99%).
B.3.13 Standard stock solution: Respectively accurately weigh appropriate amounts of
OP (B.3.9), NP (B.3.10), OPnEO (B.3.11), NPnEO (B.3.12). Use isopropanol to prepare
a single-component standard stock solution, which has concentration of 10 mg/mL.
B.3.14 Standard working solution: Respectively pipette appropriate volumes of OP, NP,
OPnEO, NPnEO standard stock solutions (B.3.13). Place them in the same volumetric
flask. Use isopropanol to dilute it, to prepare a mixed standard working solution, which
has the required concentration.
B.3.15 Solid phase extraction column: The filler is lipophilic divinylbenzene and
hydrophilic N-vinylpyrrolidone copolymer, 60 mg, 3 mL. It is activated by 2 mL of
methanol and 4 mL of water in sequence, before use.
B.3.16 Organic filter membrane: 0.22 μm.
B.4 Instruments and equipment
B.4.1 High performance liquid chromatograph, which is equipped with fluorescence
detector.
B.4.2 Analytical balance: The sensitivity is 0.0001g.
B.4.3 Analytical balance: The sensitivity is 0.01 g.
B.4.4 Ultrasonic cleaner: The controllable temperature is (70 ± 2) °C.
B.4.5 Rotary evaporator.
B.4.6 Solid phase extraction device.
B.4.7 Nitrogen blower.
B.5 Determination steps
B.5.1 Extraction and purification of specimens
Take a representative specimen. Cut it into pieces of about 5 mm × 5 mm. Mix well.
Weigh 1 g of the cut specimen (accurate to 0.01 g). Place it in a 50 mL centrifuge tube.
Add 30 mL of methanol. Extract ultrasonically at (70 ± 2) °C, for (60 ± 5) min.
Concentrate the extract to near dryness, at below 40 °C, by a rotary evaporator. Add 2
mL of isopropanol accurately, to dissolve the residue. Pass it through a 0.22 µm filter
membrane (B.3.16). Use it for normal phase high performance liquid chromatography
determination.
cns - The concentration of OPnEO or NPnEO, which has a degree of polymerization
n, in the standard working solution, in milligrams per liter (mg/L);
V - The final constant volume of the sample solution, in milliliters (mL);
Ans - The peak area of OPnEO or NPnEO, which has a degree of polymerization n,
in the standard working solution;
m - The mass of the specimen, which is represented by the sample solution, in grams
(g);
Mns - The relative molecular mass of OPnEO or NPnEO, which has a degree of
polymerization n;
cs - The concentration of OPnEO or NPnEO in the standard working solution, in
milligrams per liter (mg/L).
The result is rounded off to two decimal places.
B.7 Lower limit of determination, recovery, precision of the method
B.7.1 Lower limit of determination
The lower determination limit of AP in this method is 1.0 mg/kg; the lower
determination limit of APnEO is 10 mg/kg.
B.7.2 Recovery rate
The range of recovery rate of the method is 80% ~ 110%.
B.7.3 Precision
In the same laboratory, when the same operator uses the same equipment and the same
test method, to independently test the same tested object, in a short period of time, the
absolute difference, between the two independent test results, is not greater than 10%
of the arithmetic mean of the two measured values. It is premised that the case where it
is greater than 10% of the arithmetic mean of the two measured values, is not more than
5%.
B.8 Test report
Same as Chapter 9.
Appendix C
(Informative)
Hydrophilic interaction chromatography (HILIC) determination of alkylphenol
and alkylphenol ethoxylates
C.1 Overview
This Appendix gives the hydrophilic interaction chromatography (HILIC) method, for
the determination of alkylphenol (AP) and alkylphenol ethoxylates (APnEO, n = 2 ~
16), in textiles.
C.2 Principle
The AP and APnEO in the specimen are extracted ultrasonically by methanol. After the
extract is concentrated and purified, it is determined by a high performance liquid
chromatograph, which is equipped with a fluorescence detector; quantified by the
external standard method.
C.3 Reagents or materials
C.3.1 Unless otherwise specified, the reagents used in this method are all analytically
pure; the water is the grade-1 water, which is specified in GB/T 6682.
C.3.2 Methanol (HPLC grade).
C.3.3 Acetonitrile (HPLC grade).
C.3.4 n-hexane (HPLC grade).
C.3.5 Isopropanol (HPLC grade).
C.3.6 Dichloromethane (HPLC grade).
C.3.7 Methanol-water solution (3 + 2): Accurately measure 300 mL of methanol (C.3.2)
and 200 mL of water. Mix well. Prepare for later use.
C.3.8 Methanol-dichloromethane solution (1 + 4): Accurately measure 100 mL of
methanol (C.3.2) and 400 mL of dichloromethane (C.3.6). Mix well. Prepare for later
use.
C.3.9 Standard octylphenol (OP, CAS No.140-66-9, purity ≥ 97%).
C.3.10 Nonylphenol standard (NP, CAS No.25154-52-3, excellent grade pure).
C.3.11 Standard product of octylphenol ethoxylates (OPnEO, CAS No.9002-93-1,
average degree of polymerization n = 9, excellent grade pure).
C.3.12 Standard product of nonylphenol ethoxylates (NPnEO, CAS No.9016-45-9,
average degree of polymerization n = 9, purity ≥ 99%).
C.3.13 Standard stock solution: Accurately weigh appropriate amounts of OP (C.3.9),
NP (C.3.10), OPnEO (C.3.11), NPnEO (C.3.12), respectively. Use acetonitrile, to
prepare it into single-component standard stock solution, which has a concentration of
10 mg/mL.
C.3.14 Standard working solution: Pipette an appropriate volume of OP, NP, OPnEO,
NPnEO standard stock solutions (C.3.13), respectively. Place them in the same
volumetric flask. Use acetonitrile to dilute it, to prepare a mixed standard working
solution of the required concentration.
C.3.15 Solid phase extraction column: The filler is lipophilic divinylbenzene and
hydrophilic N-vinylpyrrolidone copolymer, 60 mg, 3 mL. It is activated by 2 mL of
methanol and 4 mL of water in sequence, before use.
C.3.16 Organic filter membrane: 0.22 μm.
C.4 Instruments and equipment
C.4.1 High performance liquid chromatograph, which is equipped with fluorescence
detector.
C.4.2 Analytical balance: Sensitivity is 0.0001 g.
C.4.3 Analytical balance: Sensitivity is 0.01 g.
C.4.4 Ultrasonic cleaner: The controllable temperature is (70 ± 2) °C.
C.4.5 Rotary evaporator.
C.4.6 Solid phase extraction device.
C.4.7 Nitrogen blower.
C.5 Determination steps
C.5.1 Extraction and purification of specimens
Take a representative specimen. Cut it into pieces of about 5 mm × 5 mm. Mix well.
Weigh 1 g of the cut specimen (accurate to 0.01 g). Place it in a 50 mL centrifuge tube.
Add 30 mL of methanol. Extract ultrasonically at (70 ± 2) °C, for (60 ± 5) min.
Concentrate the extract to near dryness, at below 40 °C, by a rotary evaporator. Add 2
mL of acetonitrile accurately, to dissolve the residue. Pass it through a 0.22 µm filter
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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