GB/T 17593.2-2007 English PDF (GBT17593.2-2007)

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GB/T 17593.2-2007: Textiles -- Determination of heavy metals -- Part 2: Inductively coupled plasma atomic emission spectrometry
GB/T 17593.2-2007
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
W 04
Textiles - Determination of Heavy Metals -
Part 2. Inductively Coupled Plasma Atomic
Emission Spectrometry
ISSUED ON. DECEMBER 5, 2007
IMPLEMENTED ON. SEPTEMBER 1, 2008
Jointly issued by. General Administration of Quality Supervision,
Inspection and Quarantine (AQSIQ);
Standardization Administration (SAC) of the
People’s Republic of China.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative References ... 4 
3 Principle ... 4 
4 Reagents and Materials ... 5 
5 Instruments and Equipment ... 6 
6 Analytical Procedures ... 6 
7 Result Calculation ... 7 
8 Determination of Lower Limit and Precision ... 7 
9 Test Report ... 8 
Appendix A (Informative) Working Conditions of the ICP Spectrometer ... 9 
Foreword
GB/T 17593 "Textiles - Determination of Heavy Metals" includes the following parts.
- Part 1. Atomic Absorption Spectrophotometry;
- Part 2. Inductively Coupled Plasma Atomic Emission Spectrometry;
- Part 3. Chromium (VI) Spectrophotometry;
- Part 4. Arsenic and Mercury - Atomic Fluorescence Spectrophotometry.
This Part is Part 2 of GB/T 17593; it adopts inductively coupled plasma atomic
emission spectrometer (ICP) to determine.
Appendix A of this Part is informative.
This Part was proposed by the China National Textile and Apparel Council.
This Part shall be under the jurisdiction of the Foundation Subcommittee of the
National Technical Committee on Textiles of the Standardization Administration of
China (SAC/TC 209/SC 1).
Drafting organizations of this Part. Tianjin Entry-Exit Inspection and Quarantine
Bureau, and Standardization Research Institute of Textile Industry.
Chief drafting staffs of this Part. Yan Jing, Yu Tao, Zhu Ying, Zhu Naitong, Guo Wei,
and Wang Yansheng.
Textiles - Determination of Heavy Metals-
Part 2. Inductively Coupled Plasma Atomic
Emission Spectrometry
WARNING - The personnel using this Part of GB/T 17593 shall have practical
experience in regular laboratory work. This Part does not address all potential
safety concerns. The users are responsible for taking proper safety and health
measures and ensuring conformance to the requirements specified in relevant
national regulations.
1 Scope
This Part of GB/T 17593 specifies the method for simultaneously determining the
eight extractable heavy metal elements - arsenic (As), cadmium (Cd), cobalt (Co),
chromium (Cr), copper (Cu), nickel (Ni), lead (Pb), and antimony (Sb) in the textiles by
adopting inductively coupled plasma atomic emission spectrometry (ICP).
2 Normative References
The following documents contain provisions which, through reference in this Part of
GB/T 17593, constitute provisions of this Part. For dated reference, subsequent
amendments (excluding corrected content) or revisions of these publications do not
apply. However, all parties coming to an agreement according to this Part are
encouraged to study whether the latest edition of these documents is applicable. For
undated references, the latest edition of the normative document applies.
GB/T 3922 Textiles - Testing Method for Colour Fastness to Perspiration
GB/T 6682 Water for Laboratory Use - Specifications
3 Principle
After using acid sweat solution to extract the sample, use inductively coupled plasma
atomic emission spectrometer to determine the emission intensity of the eight heavy
metal elements - lead, cadmium, arsenic, copper, cobalt, nickel, chromium, and
antimony at the corresponding analytical wavelength; determine the concentrations of
all the heavy metals’ ions according to the standard work curve; calculate the
extractable heavy metal contents in the sample.
Weigh 0.160g of lead nitrate [Pb(NO3)2]; dissolve it with 10mL nitric acid solution (1+9);
transfer into a 1000mL volumetric flask; dilute it to the scale.
4.2.8 Antimony (Sb) standard stock solution (100μg/mL)
Weigh 0.274g of antimony potassium tartrate (C4H4KO7Sb·1/2H2O); dissolve it into
hydrochloric acid solution (10%); transfer into a 1000mL volumetric flask; dilute it to
the scale with hydrochloric acid solution (10%).
Note. Unless otherwise specified, the storage time of the standard stock solution at normal temperature (15°C~25°C)
is six months; it shall be re-prepared if there is turbidity, precipitation or change in color, etc.
4.3 Standard working solution (10μg/mL)
Respectively transfer appropriate cadmium, chromium, copper, nickel, lead, antimony,
zinc and cobalt standard stock solutions into the 100mL volumetric flasks that have
been loaded with 5mL of concentrated sulfuric acid; dilute them with water to the scale;
shake well; prepare into standard working solutions with 10μg/mL concentration.
Note. The valid date of this solution is one week. If there is turbidity, precipitation or change in color, re-preparation
shall be conducted.
5 Instruments and Equipment
5.1 Inductively coupled plasma atomic emission spectrometer (ICP). The argon
purity is greater than or equal to 99.9%, so as to provide stable and clear plasma torch
and conduct the determination under suitable working condition.
5.2 Conical flask with stopper. 150mL.
5.3 Thermostatic water bath oscillator. (37±2)°C, the oscillation frequency is 60
times/min.
6 Analytical Procedures
6.1 Preparation of extraction solution
Take representative samples; cut them up into less than 5mm×5mm and mix uniformly;
then weigh two portions of 4g sample (for parallel test), accurate to 0.01g; place them
into conical flasks (5.2). Add 80mL of acid sweat solution (4.1), so as to make the fiber
immersed completely; put the conical flasks into the thermostatic water bath oscillator
(5.3); after shaking for 60min, remove and stand to the room temperature; filter to
form the sample solution for analyzing.
6.2 Determination
Table 1 The Determination Lower Limit of Extractable Heavy Metal Element
Element Determination lower limit t(mg/kg)
Arsenic (As) 0.20
Cadmium (Cd) 0.01
Cobalt (Co) 0.02
Chromium (Cr) 0.12
Copper (Cu) 0.06
Nickel (Ni) 0.05
Lead (Pb) 0.23
Antimony (Sb) 0.09
Note. The detection limit of different instruments may vary, so the determination lower limit of
this method is only for reference.
8.2 Precision
According to the same testing method, two tests shall be carried out respectively on
the same test object, same operator, same equipment, same laboratory in a short
time. The absolute difference of the two testing results shall not be greater than 10%
of arithmetic average of the two measured values, the accuracy shall take the
precondition that 10% of larger than the arithmetic average of the two measured
values doesn't exceed 5%.
9 Test Report
The test report shall include the following contents.
a) Number of this Part;
b) Sample description;
c) Test date;
d) Content of all the heavy metals in the sample;
e) Any deviation from this Part.