GB/T 3780.30-2023Carbon black - Part 30: Determination of high temperature volatile matter - Thermogravimetry method (English PDF)

Foreword

This document complies with the provisions of GB/T 1.1-2020 "Standardization Work Guidelines Part 1.Structure and Drafting Rules of Standardization Documents"

Drafting.

This document is Part 30 of GB/T 3780 "Carbon Black". GB/T 3780 has released the following parts.

---Part 1.Test method for iodine absorption value;

---Part 2.Determination of oil absorption value;

---Part 4.Determination of oil absorption value of compression specimens;

---Part 5.Determination of specific surface area CTAB method;

---Part 6.Determination of coloring strength;

---Part 7.Determination of pH value;

---Part 8.Determination of heating loss;

---Part 10.Determination of ash content;

---Part 12.Inspection of impurities;

---Part 14.Determination of sulfur content;

---Part 15.Determination of transmittance of toluene extract;

---Part 17.Reflectivity method for indirect determination of particle size;

---Part 18.Identification methods in natural rubber (NR);

---Part 21.Determination of sieve residue by water flushing method;

---Part 22.Calculating process capability index using process control data;

---Part 23.Sampling and identification of fugitive carbon black or other environmental particles;

---Part 24.Determination of void volume;

---Part 25.Determination of carbon content;

---Part 26.Determination of carbon content in carbon black raw oil;

---Part 27.Determination of aggregate size distribution by disc centrifugal optical deposition measurement method;

---Part 28.Determination of polycyclic aromatic hydrocarbons content;

---Part 29.Determination of solvent extractables;

---Part 30.Determination of high temperature volatiles by thermogravimetric method.

This document has been modified to adopt ISO 21870.2005 "Determination of Pyrolysis Loss by Thermogravimetry of Rubber Compounding Agent Carbon Black".

Compared with ISO 21870.2005, this document has made the following structural adjustments.

---Added two chapters "Normative Reference Documents" and "Terms and Definitions" (see Chapter 2 and Chapter 3);

---Chapter 4 corresponds to Chapter 2 in ISO 21870.2005;

---Chapter 5 corresponds to Chapter 4 in ISO 21870.2005;

---Chapter 6 corresponds to Chapter 3 in ISO 21870.2005;

---Added Chapter 7 "Sample";

---Chapter 8 ~ Chapter 10 correspond to Chapter 5 ~ Chapter 7 in ISO 21870.2005.

The technical differences between this document and ISO 21870.2005 and their reasons are as follows.

---The scope of application has been changed (see Chapter 1), and the adaptability is wider;

---Replaced ISO 1126 (see Chapter 1) with the normatively quoted GB/T 3780.8 to adapt to my country's technical conditions;

---Added GB/T 6425 (see Chapter 3) to adapt to my country's technical conditions;

---Added GB/T 3778 and GB/T 7044 (see Chapter 7) to adapt to my country's technical conditions and increase operability;

---The constant flow rate is added to "50cm3/min" (see 8.2), which clarifies and standardizes the uniformity of operation;

---Added "record the mass of the sample m40, accurate to 0.01mg" (see 8.4) corresponding to the calculation formula;

---Added "record the mass of the sample m125, accurate to 0.01mg" (see 8.7) corresponding to the calculation formula;

---Deleted the requirement that mass loss less than 0.05% of the starting mass is regarded as constant mass (see 8.9, ISO 21870.2005

5.9), more operable and easy to use;

---Changed the mass unit gram (g) to milligram (mg) (see Chapter 9, Chapter 6 of ISO 21870.2005), which is consistent with the analysis step

Comply with the regulations on weighing sample quantity;

---Added GB/T 8170 (see 9.2) to adapt to my country's technical conditions.

The following editorial changes have been made to this document.

---In order to coordinate with the existing standards, the name of the standard is modified to "Carbon Black Part 30.Determination of High Temperature Volatile Compounds by Thermogravimetric Method".

Please note that some content in this document may be subject to patents. The publisher of this document assumes no responsibility for identifying patents.

Introduction

Carbon black is a product generated by incomplete combustion or thermal cracking of hydrocarbon compounds. It is mainly composed of carbon elements and is similar to spherical colloidal particles.

They exist in the form of sub- and colloid-sized aggregates. The physical and chemical properties of carbon black are mainly manifested in particle size, structure and surface properties. Its detection methods

It is the GB/T 3780 series of standards and is planned to consist of 30 parts.

---Part 1.Test method for iodine absorption value. The purpose is to indirectly test the specific surface area of carbon black, and the results are mainly used to calculate carbon black production.

The process capability index of the device represents the stability of the process.

---Part 2.Determination of oil absorption value. The purpose is to test the structural properties of carbon black aggregates and agglomerates, and the results are mainly used for calculations.

The process capability index of carbon black production equipment represents the stability of the process.

---Part 4.Determination of oil absorption value of compression specimens. The purpose is to test the aggregate structural properties of carbon black and determine the relationship between carbon black and other ingredients.

The mixture can be mixed or kneaded for processing, filling and reinforcement, conductivity and other properties.

---Part 5.Determination of specific surface area CTAB method. The purpose is to directly test the surface area of carbon black and characterize the relationship between carbon black and rubber.

The effective area that molecules can come into contact with.

---Part 6.Determination of tinting strength. The purpose is to indirectly test the particle size and particle size distribution of carbon black and characterize the reinforcement and coating of carbon black.

The ability to cover white pigments.

---Part 7.Determination of pH value. The purpose is to test the degree of oxidation of the carbon black surface and characterize the vulcanization speed of the carbon black-containing compound.

properties such as strength and hydrophilicity of carbon black.

---Part 8.Determination of heating loss. The purpose is to test the amount of carbon black components lost at 125°C. These components are

If the value is high, the quality of the vulcanized rubber may be damaged.

---Part 10.Determination of ash content. The purpose is to test the inorganic impurities and inorganic salts in carbon black originating from raw oil and process.

Class, the ash content is relatively high, which will reduce the application performance of carbon black.

---Part 12.Inspection of impurities. The purpose is to test non-carbon black substances and impurities in carbon black that cannot pass the 850µm test sieve.

Both content and particle size have adverse effects on the performance of rubber products, making local cracks prone to occur where they exist, which may occur in tires.

Can cause a tire blowout.

---Part 14.Determination of sulfur content. The purpose is to test the sulfur content in carbon black as a basis for adjusting the formula of rubber products.

---Part 15.Determination of transmittance of toluene extract. Used to test the content of incompletely decomposed organic matter on the surface of carbon black, different

Applications have different requirements on the transmittance of toluene extract of carbon black.

---Part 17.Reflectivity method for indirect determination of particle size. The purpose is to indirectly test the particle size of carbon black. Carbon black particle size

It is an important factor in determining the properties of carbon black. The smaller the particles, the better the reinforcement.

---Part 18.Identification methods in natural rubber (NR). The purpose is to standardize the formula and test to intuitively judge the effect of carbon black on rubber.

Physical and mechanical properties of filling reinforcement properties.

---Part 21.Determination of sieve residue by water flushing method. The purpose is to test non-carbon black substances in carbon black that are larger than the specified geometric size.

If the content of carbon black is too large, the service life of rubber products will be shortened and surface defects will appear.

---Part 22.Calculating process capability index using process control data. The purpose is to quantitatively evaluate process control stability and guide carbon

Process control of black production.

---Part 23.Sampling and identification of fugitive carbon black or other environmental particles. The purpose is to test the degree of pollution of carbon black to the working environment.

The degree and results are an important basis for judging the effectiveness of employee health protection measures.

---Part 24.Determination of void volume. The purpose is to quickly test the structure of carbon black. Method functionality is equivalent to Part 4.

---Part 25.Determination of carbon content. The purpose is to test the total carbon content in carbon black, which can be used to calculate and report CO2 emissions.

It can also be used to calculate and evaluate the production capacity of the process. This part and Part 26 together constitute the carbon emissions during carbon black production process.

A high-volume testing method.

---Part 26.Determination of carbon content in carbon black raw oil. The aim is to estimate the CO2 emissions from the carbon black production process

[Direct emissions of carbon = carbon content in raw oil (gas) - carbon content in carbon black products], so it can be used to regulate greenhouse gases

basis for accounting for body emissions.

---Part 27.Determination of aggregate size distribution by disc centrifugal optical deposition measurement method. The purpose is to directly test carbon black aggregation

body size.

---Part 28.Determination of polycyclic aromatic hydrocarbons content. The purpose is to test the content of polycyclic aromatic hydrocarbons in carbon black, which are commonly found in carbon black raw oil.

Contains higher concentrations of polycyclic aromatic hydrocarbons. Controlling the residual amount of polycyclic aromatic hydrocarbons in carbon black will help protect users of carbon black-containing products

of good health.

---Part 29.Determination of solvent extractables. The purpose is to directly test the incomplete cracks on the surface of carbon black using solvents such as toluene or acetone.

For organic matter solution, the method function is equivalent to that of Part 15.

---Part 30.Determination of high temperature volatiles by thermogravimetric method. The purpose is to operate at a set temperature in a controlled, oxygen-free atmosphere.

Control program to heat the sample. Quantitatively determine the high-temperature volatile matter of the sample based on the recorded thermogravimetric curve of mass change with temperature.

Weight loss rate.

The release of various parts of GB/T 3780 can improve my country's carbon black standardization system, improve carbon black production technology, and continuously improve products.

Quality, in line with international standards, promotes the effective use of standard functions, and better promotes trade, exchanges and technical cooperation.

Carbon black Part 30.Determination of high temperature volatiles

Thermogravimetry

Warning. Personnel using this document should have practical experience in regular laboratory work. This document does not identify all possible security issues.

Users are responsible for taking appropriate safety and health measures and ensuring compliance with the conditions stipulated in relevant national regulations.

1 Scope

This document describes the method for quantitatively determining the weight loss rate of high-temperature volatiles in carbon black using thermogravimetry. It does not include the methods specified in GB/T 3780.8.

Heating loss at 125°C.

This document applies to the evaluation of the pyrolysis of carbon black surface functional groups and adsorbates (e.g. hydrocarbons).

This document applies to carbon black for rubber and pigment carbon black.

2 Normative reference documents

The contents of the following documents constitute essential provisions of this document through normative references in the text. Among them, the dated quotations

For undated referenced documents, only the version corresponding to that date applies to this document; for undated referenced documents, the latest version (including all amendments) applies to

this document.

GB/T 3778 Carbon black for rubber

GB/T 3780.8 Carbon black Part 8.Determination of weight loss on heating (GB/T 3780.8-2019, ISO 1126.2015, MOD)

GB/T 6425 Thermal analysis terminology

GB/T 7044 Pigmented Carbon Black

GB/T 8170 Numerical rounding rules and expression and determination of limit values

3 Terms and definitions

The terms and definitions defined in GB/T 6425 and the following apply to this document.

3.1

thermogravimetry

A method to test the relationship between the mass and temperature of a sample under programmed temperature control and a certain atmosphere.

4 Principles

Place the sample of known mass on the tray of the thermal balance and heat it according to the set temperature control program in a controlled, oxygen-free atmosphere.

Sample. According to the recorded thermogravimetric curve of mass change with temperature, the weight loss rate of high-temperature volatile matter of the sample is quantitatively determined.

5 materials

High purity nitrogen, purity >=99.999%.