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GB/T 22930.2-2021 English PDF (GBT22930.2-2021)

GB/T 22930.2-2021 English PDF (GBT22930.2-2021)

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GB/T 22930.2-2021: Leather and fur -- Chemical determination of metal content -- Part 2: Total metal content

This document describes the test methods for the total contents of 24 metals: aluminum (Al), arsenic (As), barium (Ba), calcium (Ca), cadmium (Cd), cobalt (Co), chromium (Cr), copper (Cu), iron (Fe), potassium (K), magnesium (Mg), sodium (Na), lead (Pb), manganese (Mn), molybdenum (Mo), nickel (Ni), mercury (Hg), antimony (Sb), selenium (Se), silicon (Si), tin (Sn), titanium (Ti), zinc (Zn) and zirconium (Zr).
GB/T 22930.2-2021
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.140.30
CCS Y 46
Partially replacing GB/T 22930-2008
Leather and Fur - Chemical Determination of Metal Content
- Part 2: Total Metal Content
(ISO 17072-2:2019 Leather - Chemical Determination of Metal Content - Part 2: Total Metal Content, MOD)
ISSUED ON: OCTOBER 11, 2021
IMPLEMENTED ON: MAY 1, 2022
Issued by: State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword ... 3
Introduction ... 6
1 Scope ... 7
2 Normative References... 7
3 Terms and Definitions ... 8
4 Principle ... 8
5 Reagents and Materials ... 8
6 Instruments and Equipment ... 9
7 Sampling and Preparation of Specimens ... 10
8 Test Procedures ... 10
9 Calculation and Result Expression ... 12
10 Test Report ... 14
Appendix A (Informative) Structural Changes of this Document Compared to ISO 17072-2:2019 ... 15
Appendix B (Informative) Technical Differences between this Document and ISO 17072-2:2019 and Causes for these Differences ... 16
Appendix C (Normative) Preparation of Standard Solution and Standard Working Solution of Elements to be Tested ... 20
Appendix D (Informative) ICP-OES Element Determination Wavelengths and Inter- element Interference ... 23
Appendix E (Informative) ICP-MS Analytical Isotopes and Method Detection Limits ... 25
Appendix F (Informative) AAS Element Determination Wavelengths and
Recommended Test Conditions ... 26
Appendix G (Informative) Inter-laboratory Result Comparison and Detection Limits ... 27
Bibliography... 29
Leather and Fur - Chemical Determination of Metal Content
- Part 2: Total Metal Content
WARNING: the concentrated acids used in this document are all highly corrosive and / or oxidizing liquids. If they come into contact with flammable substances, they will increase the possibility of combustion or explosion, and cause acute or chronic health hazards to the human body. In addition, there are also hazards to the water body. During the test, necessary safety measures shall be taken, and attention shall be paid to avoid the explosive reaction that may be caused by direct contact between perchloric acid and the specimen.
1 Scope
This document describes the test methods for the total contents of 24 metals: aluminum (Al), arsenic (As), barium (Ba), calcium (Ca), cadmium (Cd), cobalt (Co), chromium (Cr), copper (Cu), iron (Fe), potassium (K), magnesium (Mg), sodium (Na), lead (Pb), manganese (Mn), molybdenum (Mo), nickel (Ni), mercury (Hg), antimony (Sb), selenium (Se), silicon (Si), tin (Sn), titanium (Ti), zinc (Zn) and zirconium (Zr).
This document is applicable to the determination of the total contents of 24 metals in various types of leather and fur, as well as the determination of non-metallic boron (B) content. This document does not apply to the determination of total chromium content in chrome-tanned leather.
NOTE: for the determination of total chromium content in chrome-tanned leather, see QB/T 2720, QB/T 5313, QB/T 5314 or QB/T 5315.
2 Normative References
The contents of the following documents constitute indispensable clauses of this document through the normative references in the text. In terms of references with a specified date, only versions with a specified date are applicable to this document. In terms of references without a specified date, the latest version (including all the modifications) is applicable to this document. GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods (GB/T 6682- 2008, ISO 3696:1987, MOD)
GB/T 39364 Leather - Chemical, Physical, Mechanical and Fastness Tests - Sampling Location (GB/T 39364-2020, ISO 2418:2017, MOD)
QB/T 1267 Fur - Chemical, Physical and Mechanical and Fastness Tests - Sampling Location (QB/T 1267-2012, ISO 2418:2002, MOD)
QB/T 1272 Leather - Chemical Tests - Preparation of Chemical Test Samples (QB/T 1272-2012, ISO 4044:2008, MOD)
QB/T 1273 Fur - Chemical Tests - Determination of Volatile Matter (QB/T 1273-2012, ISO 4684:2005, MOD)
QB/T 1276 Fur - Chemical Tests - Determination of Matter Soluble in Carbon Tetrachloride (QB/T 1276-2012, ISO 4048:2008, MOD)
QB/T 2716 Leather - Preparation of Chemical Test Samples (QB/T 2716-2018, ISO 4044:2008, MOD)
QB/T 2717 Leather - Chemical Tests - Determination of Volatile (QB/T 2717-2018, ISO 4684:2005, MOD)
QB/T 2718 Leather - Chemical Tests - Determination of Matter Soluble in Dichloromethane (QB/T 2718-2018, ISO 4048:2008, MOD)
3 Terms and Definitions
This document does not have terms or definitions that need to be defined. 4 Principle
Leather or fur specimen is completely digested by tribasic acid mixture (acid digestion method) or microwave digestion apparatus (microwave digestion method). Use water to dissolve the residue, then, adopt the inductively coupled plasma optical emission spectrometer (ICP-OES), inductively coupled plasma mass spectrometer (ICP-MS), atomic absorption spectrometer (AAS) or atomic fluorescence spectrometer (AFS) to determine the metal concentration; calculate the total metal content in the specimen.
NOTE: this document determines the total contents of metal elements in leather and fur, not the content of metal in a specific compound or oxidation state.
5 Reagents and Materials
5.1 Unless it is otherwise specified, the chemical reagents used for the acid digestion method are of analytical purity, and the microwave digestion method shall use acids of superior-grade purity. All used solutions are aqueous solutions.
5.2 Nitric acid, with a mass fraction of 60% ~ 70%.
5.3 Sulfuric acid, with a mass fraction of 98%.
8.1.1 Acid digestion method
Use an analytical balance (6.3) to weigh-take 1 g of the specimen (accurate to 0.001 g) into a Kjeldahl flask (6.5); use a measuring cylinder (6.15) to add 10 mL ~ 20 mL of tribasic acid mixture (5.5); put in several glass beads (6.9). On the neck of the flask, place a funnel or water- splashing ball; heat it to boiling and maintain it in a boiling state, until the digestion is complete (the red vapor of nitrogen dioxide disappears), then, stop heating. If the specimen is not completely digested, cool the flask, then, add 10 mL ~ 20 mL of tribasic acid mixture (5.5); repeat the above-mentioned steps.
When determining the lead and barium contents in the specimen, the digestion process shall be separately carried out.
NOTE: for the determination of high-volatile metal content, ensure that the open acid digestion process will not cause a loss of elements.
After cooling, use 30 mL of water (5.8) to dissolve the residue and transfer it to a 100 mL volumetric flask (if necessary, filter it). Use 30 mL of water to thoroughly wash the flask and the funnel; transfer all the washing solution into a volumetric flask; use water to reach a constant volume.
Use an equivalent amount of tribasic acid mixture to replace the specimen. Then, in accordance with the above-mentioned operation, conduct a blank test.
8.1.2 Microwave digestion method
The specimen digestion solution may also be prepared through the microwave digestion method or other suitable methods. If this method is used, the weighing amount of the specimen is adjusted to 0.1 g ~ 1.0 g, accurate to 0.001 g.
8.2 Instrumental Analysis
8.2.1 General rules
If the content of metal elements in the obtained specimen digestion solution in 8.1 is within the range of the standard curve, it may be directly used for analysis and testing. Otherwise, the digestion solution should be properly diluted, then, tested.
The preparation of the metal standard solution to be tested and its standard working solution shall be conducted in accordance with the stipulations of Appendix C. When drawing the standard curve, make sure that the acid concentration in the metal element standard working solution is consistent with the acid concentration in the specimen digestion solution. The drawing of the standard working curve at least includes 4 series of concentrations and 1 blank concentration.
8.2.2 ICP method
8.2.2.1 ICP-OES method
In accordance with the instruction manual of the instrument, set the parameters of ICP-OES (6.10). If necessary, in accordance with the instruction manual of the instrument, use a hydride generator to determine the contents of arsenic (As), antimony (Sb), tin (Sn), selenium (Se) and mercury (Hg) in the specimen.
Take the metal element solution with an already-known concentration as the reference. At the specific wavelength of each metal element, use ICP-OES to analyze the specimen digestion solution prepared in 8.1. The commonly selected determination wavelengths of the various metal elements are shown in Appendix D. In accordance with the same determination conditions as the specimen digestion solution, analyze the blank test solution. 8.2.2.2 ICP-MS method
In accordance with the instruction manual of the instrument, set the parameters of ICP-MS (6.12). Take the metal element solution with an already-known concentration as the reference. At the characteristic ion mass of each metal element, use ICP-MS to analyze the specimen digestion solution prepared in 8.1. The analytical isotopes and the method detection limits of the various metal elements are shown in Appendix E. In accordance with the same determination conditions as the specimen digestion solution, analyze the blank test solution. 8.2.3 AAS method
In accordance with the instruction manual of the instrument, set the parameters of the atomic absorption spectrometer (6.11). If necessary, in accordance with the instruction manual of the instrument, use a hydride generator to determine the contents of arsenic (As), antimony (Sb), tin (Sn), selenium (Se) and mercury (Hg) in the specimen.
Take the metal element solution with an already-known concentration as the reference. Use a suitable hollow cathode lamp to analyze the metal content in the specimen digestion solution prepared in 8.1 by AAS. The determination wavelengths and the recommended test conditions of the various metal elements by AAS are shown in Appendix F. In accordance with the same determination conditions as the specimen digestion solution, analyze the blank test solution. 8.2.4 AFS method
In accordance with the instruction manual of the instrument, set the parameters of the atomic fluorescence spectrometer (6.13).
Take mercury-containing solution with an already-known concentration as the reference. Use AFS to analyze the mercury content in the specimen digestion solution prepared in 8.1. In accordance with the same determination conditions as the specimen digestion solution, analyze the blank test solution.
9 Calculation and Result Expression
In accordance with Formula (1), calculate the mass fraction of each metal element (counted by Appendix C
(Normative)
Preparation of Standard Solution and Standard Working Solution of Elements to be Tested
C.1 Overall Requirements
In accordance with different ranges of determination, different element standard solutions may be required. Under general circumstances, when preparing a multi-element mixed standard solution, pay attention to its chemical compatibility and possible hydrolysis of its components, so as to prevent chemical reactions (for example, precipitation) and spectral interference. In order to avoid interference, digestion reagents (such as: nitric acid, sulfuric acid and aqua regia, etc.) may be added to the mixed standard solution.
The formulations provided below also take into account the different sensitivities of different spectrometers.
The multi-element mixed standard solution usually has a shelf life of several months when stored in the dark.
NOTE: since Ba and B may precipitate under certain circumstances, it is recommended to prepare a single-element standard solution for the determination (see C.2.3 and C.2.4). C.2 Preparation of Metal Element Standard Solution
C.2.1 Multi-element mixed standard solution A
 (Al, Cd, Co, Cr, Cu, Fe, Pb, Mn, Mo, Ni, Si, Zn, Zr) = 1 mg/L.
Transfer about 250 mL of water (5.8) to a 1,000 mL volumetric flask (6.14); add 5 mL of nitric acid (5.2); accurately transfer-take 1 mL of the metal element (Al, Cd, Co, Cr, Cu, Fe, Pb, Mn, Mo, Ni, Si, Zn, Zr) standard stock solution (5.6) to the 1,000 mL volumetric flask (6.14). Use water (5.8) to dilute to a constant volume to the scale, then, transfer into a suitable storage bottle. C.2.2 Multi-element mixed standard solution B
 (Sn, Ti, As, Se, Sb) = 10 mg/L.
Transfer about 250 mL of water (5.8) to a 1,000 mL volumetric flask (6.14); add 5 mL of hydrochloric acid (5.7); accurately transfer-take 10 mL of the metal element (Sn, Ti, As, Se, Sb) standard stock solution (5.6) into the volumetric flask (6.14). Use water (5.8) to dilute to a constant volume to the scale, then, transfer into a suitable storage bottle. C.2.3 Barium standard solution C
 (Ba) = 0.1 mg/L.
Transfer about 250 mL of water (5.8) to a 1,000 mL volumetric flask (6.14); add 5 mL of nitric acid (5.2); accurately transfer-take 0.1 mL of the metal element (Ba) standard stock solution (5.6) to the volumetric flask. Use water (5.8) to dilute to a constant volume to the scale, then, transfer into a suitable storage bottle.
C.2.4 Boron standard solution D
 (B) = 10 mg/L.
Transfer about 250 mL of water (5.8) to a 1,000 mL volumetric flask (6.14); add 5 mL of nitric acid (5.2); accurately transfer-take 10 mL of boron (B) standard stock solution (with a concentration of 1,000 mg/L) to the volumetric flask. Use water (5.8) to dilute to a constant volume to the scale.
NOTE: there will be an obvious loss of boron element during the sample injection process, which may lead to relatively high results after multiple tests; in order to avoid the residual boron element in the sample injection system, the concentration of the boron element standard solution should be as low as possible.
C.2.5 Mercury standard solution E
 (Hg) = 1 mg/L.
Accurately transfer-take 1 mL of the metal element (Hg) standard stock solution (5.6) to a 1,000 mL volumetric flask (6.14); add 5 mL of nitric acid (5.2). Use water (5.8) to dilute to a constant volume to the scale, then, transfer into a suitable storage bottle.
C.2.6 Multi-element mixed standard solution F
 (Ca, Mg, Na, K) = 100 mg/L.
Accurately transfer-take 100 mL of the metal element (Ca, Mg, Na, K) standard stock solution (5.6) to a 1,000 mL volumetric flask (6.14); add 5 mL of nitric acid (5.2). Use water (5.8) to dilute to a constant volume to the scale, then, transfer into a suitable storage bottle. C.3 Preparation of Metal Element Standard Working Solution
In accordance with the actual demands, dilute the metal element standard solution (C.2) step- by-step to prepare the metal element standard working solution with a series of concentrations. The shelf life of the standard working solution with concentrations below 1 mg/L and 100 g/L respectively should not exceed 1 month and 1 day.
Example: respectively transfer-take 200 L, 400 L, 600 L, 800 L and 1,000 L of the multi- element mixed standard solution A (C.2.1) in a 100 mL volumetric flask; add the same amount of acid as in the specimen digestion solution. After cooling (if necessary), use water (5.8) to dilute to a constant volume; prepare the metal element standard working

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