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GB/T 17593.2-2007 PDF English

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GB/T 17593.2-2007: Textiles -- Determination of heavy metals -- Part 2: Inductively coupled plasma atomic emission spectrometry
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GB/T 17593.2-2007: Textiles -- Determination of heavy metals -- Part 2: Inductively coupled plasma atomic emission spectrometry


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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. ......

Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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