Valid

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

Also coversGBT22930.2-2021

Open the GB/T 22930.2-2021 preview as PDF

Preview — first pages of GB/T 22930.2-2021

This is a limited preview

Buy now to download the full PDF

Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

October 11, 2021

Implementation date

May 1, 2022

Scope

GB/T 22930.2-2021 (Leather and fur - Chemical determination of metal content - Part 2: Total metal content) is available as an English-translated PDF.

GB/T 22930.2-2021 — 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.

Document preview — GB/T 22930.2-2021

National Standard of the People's Republic of China

Issued by: SAMR; SAC

Contents

  • Foreword3
  • Introduction6
  • 1 Scope7
  • 2 Normative References7
  • 3 Terms and Definitions8
  • 4 Principle8
  • 5 Reagents and Materials8
  • 6 Instruments and Equipment9
  • 7 Sampling and Preparation of Specimens10
  • 8 Test Procedures10
  • 9 Calculation and Result Expression12
  • 10 Test Report14
  • Appendix A (Informative) Structural Changes of this Document Compared to ISO 17072-2:201915
  • Appendix B (Informative) Technical Differences between this Document and ISO 17072-2:2019 and Causes for these Differences16
  • Appendix C (Normative) Preparation of Standard Solution and Standard Working Solution of Elements to be Tested20
  • Appendix D (Informative) ICP-OES Element Determination Wavelengths and Inter- element Interference23
  • Appendix E (Informative) ICP-MS Analytical Isotopes and Method Detection Limits25
  • Appendix F (Informative) AAS Element Determination Wavelengths and Recommended Test Conditions26
  • Appendix G (Informative) Inter-laboratory Result Comparison and Detection Limits27
  • Bibliography29

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

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — all pages — is available in the English PDF.

Referenced standards

How to Buy GB/T 22930.2-2021

  1. 1Add to cart. Click the "Buy GB/T 22930.2-2021" button on this page. You can add more standards before checkout.
  2. 2Checkout. Enter your email and billing details. Payment is processed securely by Stripe (cards, Apple Pay, Google Pay supported).
  3. 3Instant delivery (0–9 sec). Delivery is automatic: within seconds of payment you'll receive an email with a secure download link. The link stays valid for 72 hours.
  4. 4Invoice included. A tax invoice is attached to the confirmation email. Need a custom invoice? Contact us.

Related Standards

English PDF
Instant delivery (0–9 sec)
Invoice included
View Cart

Secure payment via Stripe

Payments accepted

VisaMastercardAmerican ExpressApple PayGoogle PayStripe

GB/T 22930.2-2021

$335.00

$285.00for partners