GB/T 33392-2016 PDF English
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Leather and fur -- Chemical tests -- Determination of 4-aminoazobenzene derived from azo colorants
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GB/T 33392-2016: PDF in English (GBT 33392-2016) GB/T 33392-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.140.30
Y 46
Leather and Fur - Chemical Tests - Determination of 4-
Aminoazobenzene Derived from Azo Colorants
(ISO 17234-2:2011, Leather - Chemical Tests for the Determination of Certain
Azo Colorants in Dyed Leathers - Part 2: Determination of 4-
Aminoazobenzene, MOD)
ISSUED ON: DECEMBER 30, 2016
IMPLEMENTED ON: JULY 01, 2017
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative References ... 4
3 Principle ... 4
4 Reagents ... 5
5 Apparatus ... 6
6 Preparation of the Specimen ... 7
7 Analysis Procedures ... 7
8 Calculation of the Results ... 10
9 Detection Limit and Recovery Rate ... 11
10 Presentation of the Results ... 11
11 Test Report ... 12
Appendix A (Informative) HPLC-DAD Chromatogram and Spectrogram ... 13
Appendix B (Informative) GC-MS Chromatogram and Mass-Spectrogram ... 14
Appendix C (Informative) Other Chromatographic Analysis Methods ... 16
Appendix D (Informative) Technical Differences and Causes between this
Standard and ISO 17234-2:2011 ... 19
Leather and Fur –
Chemical Tests – Determination of 4-
Aminoazobenzene Derived from Azo Colorants
1 Scope
This Standard specifies the test method of gas chromatography-mass spectrometry
and high-performance liquid chromatography of 4-aminoazobenzene (CAS number:
60-09-3) that is decomposed from certain azo dyes in leather and fur and exists in free
form.
This Standard is applicable to all kinds of leather, fur and their products.
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 document.
GB/T 6682-2008 Water for Analytical Laboratory Use - Specification and Test
Methods (ISO 3696:1987, MOD)
QB/T 1267 Fur - Chemical, Physical and Mechanical and Fastness Tests -
Sampling Location
QB/T 1272 Leather - Chemical Tests - Preparation of Chemical Test Samples
QB/T 2706 Leather - Chemical Physical and Mechanical and Fastness Tests -
Sampling Location (QB/T 2706-2005, ISO 2418:2002, MOD)
QB/T 2716 Leather - Preparation of Chemical Test Samples (QB/T 2716-2005,
ISO 4044:1997, MOD)
3 Principle
After degreasing, the specimen is placed in an enclosed container; and is reduced by
funnel; add 100mL of ferrous sulfate solution with a mass concentration of 5%; shake vigorously;
discard the water layer; place it in an all-glass device for distillation; and collect at 33.5°C ~
34.5°C for distillation.
4.5 Sodium chloride.
4.6 Methanol, chromatographically-pure.
4.7 Acetonitrile, chromatographically-pure.
4.8 4-Aminoazobenzene, standard product, purity ≥98%, Chemical Abstract Number:
60-09-3.
4.9 Ammonium dihydrogen phosphate.
4.10 Disodium hydrogen phosphate.
4.11 Anthracene-d10, internal standard substance, used for GC-MS analysis, purity
≥98%, Chemical Abstract Number: 1719-06-8.
4.12 Standard solution.
4.12.1 Anthracene-d10 standard solution, 2.0μg/mL, internal standard substance
solution, prepared by tert-butyl methyl ether (4.4).
NOTE: It may be formulated into other appropriate concentrations as required.
4.12.2 4-Aminoazobenzene standard stock solution, 500mg/L, prepared by tert-butyl
methyl ether (4.4) or other suitable solvents.
NOTE: This solution is stored in a brown bottle; and a small amount of anhydrous sodium
sulfate may be added; and it may be stored below -18°C with the shelf life of 1 month.
4.12.3 4-Aminoazobenzene standard working solution, 30mg/L, prepared by tert-butyl
methyl ether (4.4) or other suitable solvents.
NOTE: It may be formulated into other appropriate concentrations as required.
5 Apparatus
5.1 Analytical balance, the division value is 0.1mg.
5.2 Glass reactor, tubular, high temperature resistant and sealable.
5.3 Ultrasonic bath, with temperature control device, power at least 160W.
5.4 Constant temperature water bath or appropriate heater, with an accuracy of ±2°C.
add 20 mL of n-hexane (4.1); cover with the stopper; and place it in an ultrasonic bath
(5.3) at (40±2) °C for 20min. Decant the n-hexane (be careful not to lose the specimen);
and then use 20 mL of n-hexane (4.1) to treat it once in the same way. Then place the
processed sample in the glass reactor; open the mouth; and let the n-hexane
evaporate to dryness (overnight).
NOTE: Very soft leather sample, such as sheep clothing leather, may weigh 0.5g of sample.
7.2 Reductive cleavage
Add 9.0mL of sodium hydroxide solution (4.2) to the glass reactor; shake vigorously
after sealing; so that the sample is immersed in the liquid. Add 1.0mL of sodium
dithionite solution (4.3) by a syringe; and shake vigorously after sealing to make the
solution mix thoroughly. And then place it in a constant temperature water bath at
(40±2) °C (5.4) for continuous treatment for 30min; take out the glass reactor; and
place it in a cold-water bath (or ice-water mixed bath or salt water bath) and quickly
cool to room temperature (20°C ~25°C) for 1min.
7.3 Extraction of target substance
Quickly add 5.0mL of tert-butyl methyl ether (4.4) or 5.0mL of internal standard solution
(4.11) and 7g of sodium chloride (4.5) to the above glass reactor; seal the reactor;
shake it vigorously; and then place it on a mechanical oscillator (5.6) to shake for 45min;
let it stand. After the two phases are separated, take the supernatant and pass it
through a 0.45μm organic filter membrane for GC-MS analysis.
NOTE 1: After the sample solution is cooled to room temperature, the extraction process shall
be carried out in time, and the interval shall not exceed 5min.
NOTE 2: If the two-phase separation is not good, centrifugation may be performed.
NOTE 3: If necessary, condense the tert-butyl methyl ether extract liquor to nearly 1 mL (do not
dry completely) in a vacuum rotary evaporator (5.8) at no higher than 50°C (vacuum degree
50000Pa±10000Pa(500mbar±100mbar)]; the remained tert-butyl methyl ether is slowly blown
dry by a stream of inert gas. Add 2mL of methanol directly to dissolve the residue, and such
solution is used for instrumental analysis.
7.4 Chromatographic analysis
7.4.1 GC-MS analysis conditions (recommended)
Capillary chromatographic column: DB-5ms, 30m×0.25mm×0.25μm; or equivalent.
Inlet temperature: 250°C.
Program temperature rise: maintain at 50°C for 0.5min; heat up to 260°C at a rate of
20°C/min; maintain for 5min.
As - the peak area of 4-aminoazobenzene in the standard working solution;
c - the concentration of 4-aminoazobenzene in the standard working solution, in mg/L;
V - the final volume of the sample solution, in mL;
m - the mass of the sample, in g.
8.2 GC-MS method (internal standard method)
According to the GC-MS analysis results, the content of 4-aminoazobenzene in the
sample shall be calculated according to Formula (2).
Where:
X - the content of 4-aminoazobenzene decomposed from the sample, in mg/kg;
A - the peak area of 4-aminoazobenzene in the sample test solution;
c - the concentration of 4-aminoazobenzene in the standard working solution, in mg/L;
V - the final volume of the sample solution, in mL;
Aisc - the peak area of the internal standard substance in the standard working solution;
Ais - the peak area of 4-aminoazobenzene in the standard working solution;
Aiss - the peak area of the internal standard substance in the sample test solution;
m - the mass of the sample, in grams (g)
9 Detection Limit and Recovery Rate
The detection limit in this method for 4-aminoazobenzene in the sample is 5mg/kg. The
recovery rate of the method shall be no less than 60%.
10 Presentation of the Results
The relative deviation of the two independent determination results shall be less than
10%. The content of 4-aminoazobenzene is expressed by the arithmetic mean of the
results of two parallel tests, in mg/kg, and the results are retained one digit after the
decimal point.
through a membrane filtration system (0.2μm). The resulting solution is analyzed and
detected by a capillary electrophoresis instrument.
Capillary 1:56cm, uncoated, inner diameter of 50μm, with extended optical path.
The capillary tube 2:56cm, coated by polyvinyl alcohol, inner diameter of 50μm, with
an extended optical path.
Buffer solution: phosphate buffer (c=50mmol/L), pH=2.5.
Column temperature: 25°C.
Voltage: 30kV.
Injection time: 4s.
Flow time: 5s.
Detector: Diode Array Detector (DAD), 214nm, 254nm, spectrometer.
C.4 Thin-layer chromatograph (TLC) or high-performance thin layer
chromatograph (HPTLC) (quantitative analysis), thin layer chromatography and
high-performance thin layer chromatography are only suitable for semi-
quantitative analysis
C.4.1 Thin layer chromatographic plate (high performance thin layer chromatography):
silica gel 60, containing fluorescent indicator F254, 20cm×10cm
Injection volume: 2μL~5μL, dripping method.
Mobile phase 1: chloroform: acetic acid = 90:10 (volume ratio).
C.4.2 Thin layer chromatographic plate (thin layer chromatography): silica gel 60,
containing fluorescent indicator F254, 20cm×20cm
Injection volume: 10.0μL, injection method.
Mobile phase 2: chloroform: alkyl acetate: acetic acid = 60: 30: 10 (volume ratio).
Mobile phase 3: chloroform: methanol = 95: 5 (volume ratio).
Mobile phase 2 and mobile phase 3: continuously pass through the plate without drying
in the middle.
C.4.3 Detection: 1. Ultraviolet spectrum
2. Sequentially pass the reagent 1 and reagent 2 for treatment, the
reaction time is about 5min.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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