GB/T 23972-2009 English PDF (GBT23972-2009)

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GB/T 23972-2009: Determination of alkylphenols and alkylphenol polyethoxylates in textile dyeing and finishing auxiliaries -- LC/MS method
GB/T 23972-2009
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.40
G 70
Determination of alkylphenols and alkylphenol
polyethoxylates in textile dyeing and finishing
auxiliaries - LC/MS method
ISSUED ON: JUNE 02, 2009
IMPLEMENTED ON: FEBRUARY 01, 2010
Issued by: General Administration of Quality Supervision, Inspection
and Quarantine;
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 Determination methods ... 5 
5 Low detection limit, recovery and precision ... 9 
6 Test report ... 9 
Appendix A (Normative) CAS RN of common octylphenol, nonylphenol,
octylphenol polyethoxylate and nonylphenol polyethoxylate ... 10 
Appendix B (Informative) Schematic diagrams ... 11 
Determination of alkylphenols and alkylphenol
polyethoxylates in textile dyeing and finishing
auxiliaries - LC/MS method
1 Scope
This Standard specifies the determination methods of alkylphenols and
alkylphenol polyethoxylates in textile dyeing and finishing auxiliaries.
This Standard applies to the determination of contents of alkylphenols and
alkylphenol polyethoxylates in textile dyeing and finishing auxiliaries by LC/MS
method.
2 Normative references
The terms in the following documents become the terms of this Standard by
reference to this Standard. For dated references, all subsequent amendments
(not including errata content) or revisions do not apply to this standard. However,
parties to agreements that are based on this Standard are encouraged to study
whether the latest versions of these documents can be used. For undated
references, the latest edition applies to this Standard.
GB/T 6682-2008, Water for analytical laboratory use - Specification and test
methods (ISO 3696:1987, MOD)
GB/T 8170-2008, Rules of rounding off for numerical values and expression
and judgement of limiting values
3 Terms and definitions
The following terms and definitions are applicable to this Standard.
3.1 Alkylphenols, AP for short
The molecular structure of alkylphenols is: R-C6H4-OH. The substances that
are commonly used in this category are octylphenol (C8H17-C6H4-OH, OP for
short) and nonylphenol (C9H19-C6H4-OH, NP for short).
3.2 Alkylphenol polyethoxylates, APEO for short
f) organic phase needle-filter: 13 mm × 0.45 μm.
4.4 Reagents and solutions
a) methanol: chromatographic pure;
b) water: filtered through a 0.45 μm filter membrane;
c) ammonium oxalate solution: 0.5 g/L;
d) octylphenol standard: 99.9% (mass fraction);
e) nonylphenol standard: 99.9% (mass fraction);
f) octylphenol polyethoxylate standard (average degree of polymerization of
10): 100% pure (mass fraction);
g) nonylphenol polyethoxylate standard (average degree of polymerization
of 10): ≥99.0% (mass fraction).
See Appendix A for the CAS RN of the standards.
4.5 Determination conditions
4.5.1 Chromatographic conditions:
a) chromatographic column: a stainless-steel column, of which the length is
150 mm, and the inner diameter is 2.1 mm; the stationary phase is C18
ODS; the particle size is 3.5 μm;
b) mobile phase A: methanol;
mobile phase B: ammonium acetate solution;
See Table 1 for the mobile phase gradient;
c) wavelength: 225 nm;
d) flow: 0.3 mL/min;
e) column temperature: 40 °C;
f) injection volume: 10 μL;
4.9 Spectrogram
See Appendix B for schematic diagrams of total ion chromatogram, liquid
chromatography, and mass spectrometry.
5 Low detection limit, recovery and precision
5.1 Low detection limit
The lower detection limits of this method for octylphenol, nonylphenol,
octylphenol polyethoxylate and nonylphenol polyethoxylate in the sample are
25 mg/kg, 25 mg/kg, 10 mg/kg, 10 mg/kg.
5.2 Recovery
Use the addition method to determine OP, NP, OPEO, and NPEO of three
different concentrations in the blank matrix. The recovery of the measured OP,
NP, OPEO, and NPEO is 90% ~ 110%.
5.3 Precision
The absolute difference between two independent test results, that are gained
in the same laboratory, by the same operator, with the same equipment, by the
same test method, of which the same test object is tested independently of each
other in a short time, is not greater than 20% of the arithmetic mean of the two
determination values.
6 Test report
The test report shall at least provide the following contents:
a) sample description;
b) the used standards;
c) test result;
d) deviation from the standard;
e) test date.