GB 20814-2014 English PDF

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GB 20814-2014: Limit and determination of the quantity of heavy-metal elements in dye products
Status: Valid

GB 20814: Historical versions

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 20814-2014	209	Add to Cart	3 days	Limit and determination of the quantity of heavy-metal elements in dye products	Valid
GB 20814-2006	279	Add to Cart	3 days	Limit and determination of the quantity of 10 heavy-metal elements in dye products	Obsolete

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Basic data

Standard ID: GB 20814-2014 (GB20814-2014)
Description (Translated English): Limit and determination of the quantity of heavy-metal elements in dye products
Sector / Industry: National Standard
Classification of Chinese Standard: G55
Classification of International Standard: 71.100.01; 87.060.10
Word Count Estimation: 9,911
Date of Issue: 7/24/2014
Date of Implementation: 5/1/2015
Older Standard (superseded by this standard): GB 20814-2006
Quoted Standard: GB/T 6682-2008; GB/T 8170-2008; JJG 694
Regulation (derived from): National Standards Bulletin No. 19, 2014
Issuing agency(ies): General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China
Summary: This standard specifies the permissible content (Limited) and its determination dye products of 12 heavy metal elements. This standard applies to all types of formulations of commercial dyes.

GB 20814-2014: Limit and determination of the quantity of heavy-metal elements in dye products

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Limit and determination of the quantity of heavy-metal elements in dye products ICS 71.100.01; 87.060.10 G55 National Standards of People's Republic of China Replacing GB 20814-2006 Limit and determination of heavy metal elements in dye products Issued on. 2014-07-24 2015-05-01 implementation Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China Standardization Administration of China released

Foreword

This standard was drafted in accordance with GB/T 1.1-2009 given rules. This standard replaces GB 20814-2006 "Limit and determination of dye products of 10 kinds of heavy metal elements," and GB 20814-2006 phase Ratio, in addition to editorial changes outside the main technical changes are as follows. --- Standard name was changed to "dye products in Limit and determination of heavy metal elements" (see standard name, the name of the 2006 version of the standard He said); --- Increased arsenic, mercury limits (see Chapter 3); --- Modify the reagents and materials content (see 43, 2006 version 4.2.); --- Modify the contents of the instruments and equipment (see 44, 2006 version 4.3.); --- Modify the content standards and increased working solution prepared (see 451, 2006 edition 4.4.1.); --- Increasing the content of the sample preparation solution (see 4.5.2); Preparation --- sample pretreatment incorporated into the sample solution and modify the presentation and content (see 45212, 2006 version 4.4.2...); --- Increase the detection limit content (see 4.5.3 Table 4); --- Modify the contents of the result of the determination (see 4.6, version 4.5 in 2006). The standard proposed by China Petroleum and Chemical Industry Association. This standard by the National Standardization Technical Committee Dye (SAC/TC134) centralized. This standard was drafted. Shenyang Chemical Research Institute Co., Ltd., Jiangsu Yabang Dye Co., Ltd., Beijing Institute of Clothing, Taizhou production Product quality supervision, inspection, Wang Jinhua double-Chemical Co., Ltd., the State Quality Supervision and Inspection Center dye. The main drafters of this standard. Wang Yong, Zheng Junliang, Zhou Yongkai, Huangyin Bo, Zhang Guodong, Kiran Qin, Liu Li, Shen Jiong day. This standard replaces the standards previously issued as follows. --- GB 20814-2006. Limit and determination of heavy metal elements in dye products

1 Scope

This standard specifies the permissible content (Limited) and its determination dye products of 12 heavy metal elements. This standard applies to all types of formulations of commercial dyes.

2 Normative references

The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein Member. For undated references, the latest edition (including any amendments) applies to this document. Laboratory use specifications and test methods GB/T 6682-2008 Analysis GB/T 8170-2008 revised value represents about rules and limit values and judgment JJG694 atomic absorption spectrophotometer

3 Requirements

Limited dye products contain heavy metal elements should meet the requirements in Table 1. For liquid dyes, paints and other products heavily paste Metallic elements shall be limited solids content for conversion.

1 Table of Heavy Metals Limited

No. Element name The element symbol limit/(mg/kg) 1 arsenic (arsenic) As 50 2 Cd (cadmium) Cd 20 3 Co (cobalt) Co 500 4 chromium (chromium) Cr 100 5 Cu (copper) Cu 250 6 iron (iron, ferrum) Fe 2500 7 Hg (mercury) Hg 4 8 Mn (manganese) Mn 1000 9 Ni (nickel) Ni 200 10 Pb (lead, plumbum) Pb 100 11 Sb (antimony) Sb 50 12 Zinc (zincum) Zn 1500 Note. For some dye products in the molecular structure of heavy metal elements contained from time to assess the amount of the element. Test Method 4 4.1 General provisions The method used reagents were of analytical grade or better analytical reagents. The water shall comply with GB/T 6682-2008 in two water requirements. Determination of test results according to GB/T 8170-2008 4.3 Be rounded value comparison method. 4.2 Principle Samples were mixed dye after acid digestion solution prepared by atomic absorption spectrometry determination of the solution of each metal element. 4.3 Reagents and materials 4.3.1 nitrate. 4.3.2 perchloric acid. 4.3.3 mixed acid. perchloric acid and nitric acid volume ratio = 3. 4.3.4 hydrochloric acid. 4.3.5 hydrochloric acid solution. hydrochloric acid and water volume ratio = 5. 4.3.6 hydrogen peroxide. 4.3.7 sulfuric acid. 4.3.8 Potassium dichromate. 4.3.9 sulfuric acid - potassium dichromate solution. 60mL potassium dichromate sulfuric acid 1g/L. 4.3.10 potassium iodide. 4.3.11 thiourea. 4.3.12 KI - thiourea mixture. 10g 5g potassium iodide and thiourea was dissolved in 100mL of water. 4.3.13 sodium borohydride or potassium borohydride. 4.3.14 sodium hydroxide. 4.3.15 high-purity acetylene gas. 4.3.16 high purity argon. 4.3.17 flask. 25mL, 50mL, 100mL, 200mL, 500mL, 1000mL. 4.3.18 pipette. 0.5mL, 1mL, 2mL, 5mL, 10mL, 20mL, 25mL. 4.3.19 conical flask. 150mL. 4.3.20 heavy metal elements (Table 1) of the standard solution. buy various heavy metal elements to the statutory (SI) units of measurement (Table 1) of the standard solution, the concentration Of 1.000mg/mL. Be sealed refrigeration. 4.4 instruments and equipment 4.4.1 Atomic Absorption Spectrometer. JJG694 shall comply with the requirements. 4.4.2 Microwave digestion. 4.4.3 heater. 4.5 Test procedure 4.5.1 Preparation of standard working solution Standard stock solution preparation 4.5.1.1 4.5.1.1.1 As formulated standard stock solution. Pipette with standard solution 1.00mL As in 1000mL volumetric flask 0.2mol/L nitric acid solution constant volume. Dubbed 1.00mg/L of standard stock solution. 4.5.1.1.2 Cd preparation of standard stock solution. Pipette with standard solution Cd 1.00mL in 100mL volumetric flask 0.2mol/L nitric acid solution constant volume. Dubbed 10.00mg/L of standard stock solution. 4.5.1.1.3 Co preparation of standard stock solution. use pipette Co standard solution 5.00mL in 100mL flask or 10.00mL In with 0.2mol/L nitric acid solution constant volume. Dubbed 50.00mg/L or 100.00mg/L of standard stock solution. 4.5.1.1.4 Cr preparation of standard stock solution. use pipette Cr standard solution 5.00mL in 100mL flask or 10.00mL In with 0.2mol/L nitric acid solution constant volume. Dubbed 50.00mg/L or 100.00mg/L of standard stock solution. 4.5.1.1.5 Cu formulated standard stock solution. Pipette with Cu standard solution 2.00mL in 100mL volumetric flask 0.2mol/L nitric acid solution constant volume. Dubbed 20.00mg/L of standard stock solution. 4.5.1.1.6 Fe formulated standard stock solution. Pipette with standard solution 5.00mL Fe or 10.00mL in 100mL flask In with 0.2mol/L nitric acid solution constant volume. Dubbed 50.00mg/L or 100.00mg/L of standard stock solution. 4.5.1.1.7 Hg preparation of standard stock solution. Pipette with standard solution 1.00mL Hg in 1000mL volumetric flask 0.2mol/L nitric acid solution constant volume. Dubbed 1.00mg/L of standard stock solution. 4.5.1.1.8 Mn preparation of standard stock solution. Pipette with Mn standard solution 2.00mL in 100mL volumetric flask 0.2mol/L nitric acid solution constant volume. Dubbed 20.00mg/L of standard stock solution. Ni formulated standard stock solution 4.5.1.1.9. The pipette Ni standard solution 5.00mL in 100mL flask or 10.00mL In with 0.2mol/L nitric acid solution constant volume. Dubbed 50.00mg/L or 100.00mg/L of standard stock solution. 4.5.1.1.10 Pb formulated standard stock solution. Pipette with Pb standard solution 5.00mL in 100mL flask or 10.00mL In with 0.1mol/L nitric acid solution constant volume. Dubbed 50.00mg/L or 100.00mg/L of standard stock solution. 4.5.1.1.11 Sb preparation of standard stock solution. Pipette with standard solution 1.00mL Sb in 1000mL volumetric flask 0.2mol/L nitric acid solution constant volume. Dubbed 1.00mg/L of standard stock solution. 4.5.1.1.12 Zn formulated standard stock solution. Pipette with Zn standard solution 1.00mL in 100mL volumetric flask 0.2mol/L nitric acid solution constant volume. Dubbed 10.00mg/L of standard stock solution. 4.5.1.2 formulated standard working solution 4.5.1.2.1 standard solution concentration range Suitable for all standard working solution concentration range of each standard curve measured heavy metal elements are shown in Table 2. Table 2 standard working solution concentration No. Element Name Symbol element concentration range/(mg/L) 1 arsenic (arsenic) As 0 ~ 0.05 2 Cd (cadmium) Cd 0 ~ 1.0 3 Co (cobalt) Co 0 ~ 5.0 4 chromium (chromium) Cr 0 ~ 5.0 5 Cu (copper) Cu 0 ~ 2.0 TABLE 2 (cont.) No. Element Name Symbol element concentration range/(mg/L) 6 iron (iron, ferrum) Fe 0 ~ 5.0 7 Hg (mercury) Hg 0 ~ 0.1 8 Mn (manganese) Mn 0 ~ 1.0 9 Ni (nickel) Ni 0 ~ 5.0 10 Pb (lead, plumbum) Pb 0 ~ 5.0 11 Sb (antimony) Sb 0 ~ 0.05 12 Zinc (zincum) Zn 0 ~ 1.0 4.5.1.2.2 Determination formulated flame standard working solution A concentration range of each element given in Table 2, each element separately formulated three to five different concentrations of standard working solution. In 50mL or 100mL volumetric flask, dilute with water to the mark with a pipette a volume of standard stock solution. Hydride formulation 4.5.1.2.3 Determination standard working solution (As) formulated 4.5.1.2.3.1 arsenic standard working solution Table 2 shows the concentration range, including the preparation of the blank 4 to 6 different concentration standard working solution. Pipette a quantity of 1mg/L of arsenic standard solution (such as 0mL, 0.5mL, 1.0mL, 2.0mL) in 100mL Capacity Bottle, each addition of hydrochloric acid solution (4.3.5) 50mL, adding potassium iodide - a mixture of thiourea (4.3.12) 10mL, water volume to 100mL. 2h placed above or to stand overnight at room temperature. Note. The instrument can also be formulated in a method recommended by the manufacturer of the preparation. (Hg) formulated 4.5.1.2.3.2 mercury standard working solution Concentration ranges given in Table 2, including the preparation of blank 4 to 6 different concentration of standard working solution. Pipette a quantity of 1mg/L mercury standard solution (such as 0,1.0mL, 2.0mL, 4.0mL) in 100mL flask , Each of the addition of sulfuric acid - potassium dichromate solution (4.3.9) 50mL, then water volume to 100mL. Note. The instrument can also be formulated in a method recommended by the manufacturer of the preparation. (Sb) antimony formulated 4.5.1.2.3.3 standard working solution Table 2 shows the concentration range, including the preparation of the blank 4 to 6 different concentration standard working solution. Pipette a quantity of 1mg/L of arsenic standard solution (such as 0mL, 0.5mL, 1.0mL, 2.0mL) in 100mL Capacity Bottle, each addition of hydrochloric acid solution (4.3.5) 50mL, adding potassium iodide - a mixture of thiourea (4.3.12) 10mL, water volume to 100mL. Note. The instrument can also be formulated in a method recommended by the manufacturer of the preparation. 4.5.2 Preparation of sample solution 4.5.2.1 sample pre-treatment 4.5.2.1.1 microwave digestion Dye weighed sample of about 0.1g ~ 0.5g (accurate to 0.0001g), placed in the digestion tube was added 8mL of concentrated nitric acid, 2mL peroxide Hydrogen. Digestion was allowed to stand overnight or cover lid inner tube in supporting the heating plate at 80 ℃ ~ 100 ℃ preheating 20min, at room temperature so that the sample Products and concentrated acids and hydrogen peroxide complete the initial response (to smoke or not obviously bubbling) was cooled to room temperature. The vessel is closed, and in accordance with the micro Wave digestion instrument rules, placed in a microwave digestion instrument, to set appropriate digestion process (according to the provisions of Table 3), carried out in a microwave digestion instrument elimination solution. Digestion is complete, the container to be cooled to room temperature, open the container. To prepare a sample solution to be measured. Also prepared a blank solution in the same manner as a blank reference solution is measured. Table 3 digestion procedure Phase temperature/℃ Pressure/MPa Hold Time/min 1100 2.0 2.0 2130 3.0 2.0 3160 3.5 3.0 4190 4.0 3.0 5220 4.5 5.0 4.5.2.1.2 Wet Digestion Weigh dye sample 1g (accurate to 0.0001g), placed in 150mL Erlenmeyer flask (4.3.19), was added 10mL hydrochloric acid (4.3.4) and 10mL of nitric acid (4.3.1), the flask was placed in a heater (4.4.3) heated slowly on, until the tobacco disappeared; coolish mixture was added 10mL Acid (4.3.3), the fire heated on a heater, to give a sample digestion completely colorless or yellowish transparent solution (to this end, and sometimes need to make the appropriate Plus mixed acid); coolish added 10mL water, heated to boiling and thus white smoke, then maintained for several minutes in order to get rid of the residual acid mixture, and then cooled to Room temperature, the sample solution was determined to be formulated. Also prepared a blank solution in the same manner as a blank reference solution is measured. 4.5.2.2 Determination of the sample solution preparation 4.5.2.2.1 Flame assay solution Sample solution measured cadmium, cobalt, chromium, copper, iron, manganese, nickel, lead, zinc and other flame method, the digestion solution can be directly obtained water 4.5.2.1 dilution. The digestion solution was fully transferred to 50mL volumetric flask (if the solution appears cloudy, precipitation or mechanical impurities, be sure to filter) with Water washing vessel and diluted to the mark. As determined solution absorbance values beyond the standard curve range should be appropriately diluted with water (blank solution Also by the same method of preparation and dilution). This dye sample solution should be measured by atomic absorption spectrometry as soon as possible, if you want to save, be sealed refrigeration. 4.5.2.2.2 Determination of arsenic solution The digestion solution was prepared according to 4.5.2.1 after all transferred to catch the acid 50mL volumetric flask (if the solution appears cloudy, precipitation or mechanical Impurities, be sure the filter), potassium iodide - a mixture of thiourea (4.3.12) 5mL, followed by hydrochloric acid solution 25mL1 5 of (4.3.5) and washed Container and water volume to 50mL, incubated at room temperature for more than 2h or overnight. Note. The instrument can also be formulated in a method recommended by the manufacturer of the preparation. 4.5.2.2.3 Determination of mercury solution The digestion solution was prepared by 4.5.2.1 was all transferred to 50mL volumetric flask (if the solution appears cloudy, precipitation or mechanical impurities, Be sure the filter), and then with sulfuric acid - potassium dichromate solution (4.3.9) and wash the container volume to 50mL. Note. The instrument can also be formulated in a method recommended by the manufacturer of the preparation. 4.5.2.2.4 antimony assay solution The digestion solution was prepared according to 4.5.2.1 after all transferred to catch the acid 50mL volumetric flask (if the solution appears cloudy, precipitation or mechanical Impurities, be sure the filter), potassium iodide - a mixture of thiourea (4.3.12) 5mL, followed by hydrochloric acid solution 25mL1 5 of (4.3.5) and washed Container and water volume to 50mL. Note. The instrument can also be formulated in a method recommended by the manufacturer of the preparation. 4.5.3 Determination Atomic absorption spectrometer rules, under the conditions of Table 4, adjust the instrument to the best working status of each element determination, in accordance with the instrument manufacturer Determination supplied, executed by the instruction of the instrument control computer issued sequentially measuring each standard working solution to be tested metal element, And draw the standard curve, and then measuring a blank reference solution (4.5.2) absorbance was measured dye sample measurement solution (4.5.2) absorbance. The data entered into the computer, the computer automatically acquired by the given column sample dye content of heavy metals and other data measurement report. Table 4 Determination of Heavy Metals general conditions No. element names and symbols determination of the absorption wavelength/nm detection limit/(mg/L) -As 1 Arsenic Hydride Method 193.7 0.0004 2 Cd -Cd Flame 228.8 0.005 3 Co -Co Flame 240.7 0.02 4 chrome -Cr Flame 357.9 0.03 5 copper -Cu Flame 324.7 0.004 6 Iron -Fe Flame 248.3 0.02 7 Mercury -Hg Hydride Method 253.7 0.0005 8 Mn -Mn Flame 279.5 0.004 9 nickel--Ni Flame 232.0 0.02 10 Lead -Pb Flame 283.3 0.04 11 -Sb antimony hydride Method 217.6 0.0004 12 213.9 0.005 Zinc -Zn Flame NOTE. Changes instruments and measurement conditions, the detection limit will cause change. 4.6 determine the outcome When the difference between the results of two parallel determination does not exceed 10% of the arithmetic mean of the measurement results twice, or not more than 2mg/kg, whichever is the arithmetic The average value as a measurement result. Results are given as an element of the instrument is zero or negative, the measurement result is not greater than the detection limit and dilute the sample The value represents a multiple of the product release.

5 Test Report

The test report is given, the following points need to test the process. Names and sources a) sample; b) the number and year of this standard number; c) date of inspection; d) Determination of the description (if this is required by the customer); e) the use of the instrument's name and model; f) the name and amount of each detection of heavy metal elements; g) other matters should be noted. ......

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