GB/T 46122.10-2025Fireworks - Test methods for determination of specific chemical substances - Part 10: Determination of nitrogen content in nitrocellulose - Iron(Ⅱ) sulphate titration (English PDF)

Foreword

This document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for standardization work Part 1: Structure and drafting rules for standardization documents" Drafting.

This document is Part 10 of GB/T 46122 "Test Methods for Specific Chemical Substances in Fireworks and Firecrackers". GB/T 46122 has been published.

The following sections.

--- Part 1: General provisions;

--- Part 2: Determination of hexachlorobenzene content - Gas chromatography method;

--- Part 3: Determination of lead and lead compound content - Flame atomic absorption spectrometry;

--- Part 4: Determination of lead and lead compounds content - X-ray fluorescence spectrometry;

--- Part 5: Determination of lead and lead compounds content - Inductively coupled plasma atomic emission spectrometry;

--- Part 6: Determination of zirconium content in particles less than 40 µm - Inductively coupled plasma atomic emission spectrometry;

--- Part 7: Determination of chlorate content - Chemical titration method;

--- Part 8: Determination of arsenic content - Hydride generation-atomic fluorescence spectrometry;

--- Part 9: Determination of mercury content - Hydride generation-atomic fluorescence spectrometry;

--- Part 10: Determination of nitrogen content in nitrocellulose - Ferrous sulfate titration method;

--- Part 11: Determination of phosphorus content - Inductively coupled plasma atomic emission spectrometry;

--- Part 12: Determination of picric acid and picric acid salts content - High performance liquid chromatography method this document is equivalent to ISO 22863-10:2021 "Fireworks and firecrackers - Detection methods for specific chemical substances - Part 10: Ferrous sulfate droplets Determination of nitrogen content in nitrocellulose by a quantitative method.

The following minimal editorial changes have been made to this document.

--- To coordinate with the existing standard, the name of the standard will be changed to "Test Methods for Specific Chemical Substances in Fireworks and Firecrackers Part 10: Nitrocellulose Determination of nitrogen content in cellulose - Ferrous sulfate titration method";

--- Use "1000mL" instead of "1L" (see 8.1);

---Corrected the error in the legend "6 and 7" in Figure 1.

Introduction

As the importance of fireworks and firecrackers product safety and environmental protection gradually deepens, the chemical substances used in fireworks and firecrackers products are Requirements are made, especially for the use of toxic and harmful chemicals and those that increase the risk of combustion and explosion of products. International Standardization the Fireworks and Firecrackers Technical Committee organized the development of ISO 22863 (all parts). GB/T 46122 adopts ISO 22863 (all parts).

The standardization of the testing methods for fireworks and firecrackers is to improve the safety and environmental performance of fireworks and firecrackers products and promote the development of the industry.

GB/T 46122 is planned to consist of 12 parts.

--- Part 1: General. The purpose is to determine the methods of specimen dissection, sampling and sample preparation.

--- Part 2: Determination of hexachlorobenzene content by gas chromatography. The purpose is to determine the content of hexachlorobenzene in fireworks and firecrackers.

Methods, procedures and presentation of results.

--- Part 3: Determination of lead and lead compounds content Flame atomic absorption spectrometry.

Method, procedure and presentation of results for the determination of lead and lead compounds in fireworks and firecrackers by absorption spectroscopy.

--- Part 4: Determination of lead and lead compounds content X-ray fluorescence spectrometry. The purpose is to determine the use of X-ray fluorescence Method, procedure and result presentation of the determination of lead and lead compounds in fireworks and firecrackers by spectroscopy.

--- Part 5: Determination of lead and lead compounds content Inductively coupled plasma atomic emission spectrometry. The purpose is to determine the Method, procedure and results for determination of lead and lead compounds in fireworks and firecrackers by inductively coupled plasma atomic emission spectrometry Results statement.

--- Part 6: Determination of zirconium content in particles less than 40 µm by inductively coupled plasma atomic emission spectrometry.

Method for determining zirconium content in fireworks and firecrackers with particle size less than 40 µm by inductively coupled plasma atomic emission spectrometry, Procedure and result presentation.

--- Part 7: Determination of chlorate content Chemical titration analysis method. The purpose is to determine the use of chemical titration analysis method for fireworks Method, procedure and presentation of results for the determination of chlorate content in firecrackers.

--- Part 8: Determination of arsenic content by hydride generation-atomic fluorescence spectrometry.

Method, procedure and result presentation of determination of arsenic content in fireworks and firecrackers by electron fluorescence spectrometry.

--- Part 9: Determination of mercury content by hydride generation-atomic fluorescence spectrometry.

Method, procedure and result presentation of determination of mercury content in fireworks and firecrackers by electron fluorescence spectrometry.

--- Part 10: Determination of nitrogen content in nitrocellulose by ferrous sulfate titration. The purpose is to determine the the method, procedure and result expression of the determination of nitrogen content in nitrocellulose in fireworks and firecrackers are given in this paper.

--- Part 11: Determination of phosphorus content by inductively coupled plasma atomic emission spectrometry.

Method, procedure and presentation of results for determination of phosphorus content in fireworks and firecrackers by plasma atomic emission spectrometry.

--- Part 12: Determination of picric acid and picrates by high performance liquid chromatography.

Method, procedure and result presentation for the determination of picric acid and picrates in fireworks and firecrackers by spectroscopy.

Detection methods for specific chemical substances in fireworks and firecrackers Part 10: Determination of nitrogen content in nitrocellulose Ferrous sulfate titration

1 Scope

This document describes a method for the determination of nitrogen content in nitrocellulose in pyrotechnic compositions by titration with iron (II) sulfate.

This document applies to the determination of nitrogen content in nitrocellulose in fireworks and firecrackers.

2 Normative references

The contents of the following documents constitute the essential clauses of this document through normative references in this document.

For referenced documents without a date, only the version corresponding to that date applies to this document; for referenced documents without a date, the latest version (including all amendments) applies to this document.

ISO 22863-1 Fireworks-Test methods for specific chemical substances in fireworks and firecrackers Part 1: General Note. GB/T 46122.1-2025 Fireworks and firecrackers - Detection methods for specific chemical substances - Part 1: General (ISO 22863-1:2020, IDT)

3 Terms and Definitions

There are no terms or definitions that require definition in this document.

The URLs for terminology databases used for standardization maintained by ISO and IEC are as follows.

4 Principles of the Method

First, the pyrotechnic powder sample containing nitrocellulose was pretreated to remove other nitrogen-containing substances except nitrocellulose.

It can be used to determine the nitrogen content in nitrocellulose and reduce the error.

After the remaining nitrocellulose in the sample is oxidized with concentrated sulfuric acid to form nitric acid, it is titrated with ferrous sulfate (II) (FeSO4), and the reaction is as follows.

4FeSO4 2HNO3 2H2SO4->N2O3 2Fe2(SO4)3 3H2O Using potentiometric determination, the titration curve shows an inflection point corresponding to the quantitative neutralization of nitrogen radicals in the sample.

5 Reagents

Unless otherwise specified, analytical grade reagents should be used.

5.1 Sulfuric acid (H2SO4). chemical purity 94%~97% (mass fraction).

5.2 Potassium nitrate (analytical grade).

5.3 Iron (II) sulfate (FeSO4·7H2O) crystals (analytical grade).