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This standard is developed in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 18952-2003 Rubber Compounding Ingredients - Sulfur - Methods of Test. In addition to a number of editorial changes，the following technical changes have been made with respect to GB/T 18952-2003 (the previous edition).
——"Scope" is modified (see Chapter 1, Chapter 1 in 2003 edition);
——Clauses for classification, type and labeling are added (see Chapter 3);
——The technical requirements for 14 types of sulfur are added (see Tables 1, 2 and 3);
——The test method of heating loss is modified (see 5.3; 4.7 in 2003 edition);
——The test method of ash content is modified (see 5.4; 4.8 in 2003 edition);
——The test method of residue on sieve is modified (see 5.5; 4.2 in 2003 edition);
——The test method of total sulfur content is modified (see 5.7; 4.1 in 2003 edition);
——The test method of oil content in oil-filled sulfur is modified (see 5.9; 4.3 in 2003 edition);
——The test method for heat stability of insoluble sulfur is added (see 5.10);
——Technical requirements of heavy white oil are added (see Annex A);
——The test method for heat reversion of insoluble sulfur is deleted (see 4.5 in 2003 edition);
——The test method of arsenic content is deleted (see 4.9 in 2003 edition);
——Clauses for inspection rules, marking, packaging, transportation, storage and safety are added (see Chapters 7 and 8).
This standard was proposed by China Petroleum and Chemical Industry Federation.
This Standard is under the jurisdiction of the Sub-committee for Chemical Additive of the National Technical Committee 35 on Rubber & Products of Standardization Administration of China (SAC/TC 35/SC 12).
The previous edition of the standard replaced by this standard is as follows:
——GB/T 18952-2003.
Rubber Compounding Ingredients - Sulfur and Methods of Test
Warning: personnel implementing this standard shall have formal laboratory work experience. This standard does not purport to address all of the safety problems. The users are under the obligation of adopting proper safety and health measures and shall ensure to meet the requirements specified in relevant national regulations.
1 Scope
This standard specifies the classification, type, labeling, technical requirements, test methods, inspection rules, marking, packaging, transportation, storage and safety of rubber compounding ingredient sulfur.
This standard is applicable to the soluble sulfur made of industrial sulfur and the insoluble sulfur made of soluble sulfur through such processes as temperature rise and quenching.
Molecular formula: S, [S]n.
CAS RN: 7704-34-9 (soluble sulfur)
CAS RN: 9035-99-8 (insoluble sulfur)
2 Normative References
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB 190-2009 Packing Symbol of Dangerous Goods
GB/T 191-2008 Packaging - Pictorial Marking for Handling of Goods
GB/T 265 Petroleum Products - Determination of Kinematic Viscosity and Calculation of Dynamic Viscosity
GB/T 601 Chemical Reagent - Preparations of Standard Volumetric Solutions
GB/T 603 Chemical Reagent - Preparations of Reagent Solutions for Use in Test Methods
GB/T 2013-2010 Standard Test Method for Density of Liquid Petrochemical Products
GB/T 6040-2002 General Rules for Infrared Analysis
GB/T 6679 General Rules for Sampling of Solid Chemical Products
GB/T 6682-2008 Water for Analytical Laboratory Use - Specification and Test Methods
GB/T 7363 Paraffin Wax - Determination of Polynuclear Aromatics
GB/T 8170-2008 Rules of Rounding Off for Numerical Values & Expression and Judgment of Limiting Values
GB/T 11079 White Oil - Test for Carbonizable Substances
GB/T 11409-2008 Test Methods Rubber Antiagers and Vulcanizing Accelerators
GB 12268-2012 List of Dangerous Goods
GB 12463 General Specifications for Transport Packages of Dangerous Goods
GB 15603 Rule for Storage of Chemical Dangers
SH/T 0134 Test Method of Solid Paraffin in White Oil
3 Classification, Type and Labeling
3.1 Classification
Sulfur is classified into soluble sulfur and insoluble sulfur based on different solubility in carbon disulfide.
3.2 Type
3.2.1 Soluble sulfur is classified into two types based on whether oil filling is required:
——Type I: represents non-oil-filled soluble sulfur.
——Type II: represents oil-filled soluble sulfur.
3.2.2 Insoluble sulfur is classified into non-oil-filled insoluble sulfur and oil-filled insoluble sulfur based on whether oil filling is required. Non-oil-filled insoluble sulfur is classified into two types based on insoluble sulfur content. Oil-filled insoluble sulfur is classified into high-performance oil-filled insoluble sulfur and ordinary oil-filled insoluble sulfur based on product performance, including 10 types in total.
3.3 Labeling
3.3.1 Non-oil-filled insoluble sulfur is labeled as follows:
Example:
Insoluble sulfur with insoluble sulfur content ≥60% is labeled as IS 60.
3.3.2 High-performance oil-filled insoluble sulfur is labeled as follows:
Example:
High-dispersity oil-filled insoluble sulfur with oil content central value of 20% is labeled as HD OT-20;
High-heat stability oil-filled insoluble sulfur with oil content central value of 10% is labeled as HS OT-10.
3.3.3 Ordinary oil-filled insoluble sulfur is labeled as follows:
Example:
Ordinary oil-filled insoluble sulfur with insoluble sulfur content ≥75% and oil content central value of 20% is labeled as IS 7520.
4 Technical Requirements
The technical requirements and corresponding test method of rubber compounding ingredient sulfur shall respectively meet those specified in Tables 1, 2 and 3.
Table 1 Technical Requirements and Test Method of Soluble Sulfur
Item Index Test method
Type I Type II
Appearance Yellow powder Yellow non-flying powder 5.2
Heating loss (80℃±2℃)/% ≤ 0.50 5.3
Ash content (600℃±25℃)/% ≤ 0.15 5.4
Residue on sieve (75μm)/% ≤ 4.0 5.5
Acidity (calculated in H2SO4) /% ≤ 0.10 5.6
Total sulfur content/% ≥99.5 94.0~96.0 5.7
Oil content/% — 4.0~6.0 5.9
Table 2 Technical Requirements and Test Method of Non-oil-filled Insoluble Sulfur
Item Index Test method
IS 60 IS 90
Appearance Yellow powder 5.2
Heating loss (80℃±2℃)/% ≤ 0.50 5.3
Ash content (600℃±25℃)/% ≤ 0.20 5.4
Residue on sieve (150μm)/% ≤ 1.0 5.5
Acidity (calculated in H2SO4)/% ≤ 0.10 5.6
Total sulfur content/% ≥ 99.5 5.7
Insoluble sulfur content/% ≥ 60.0 90.0 5.8
Table 3 Technical Requirements and Test Method of Oil-filled Insoluble Sulfur
Item Index Test method
HD
OT-20 HS
OT-10 HS
OT-20 HS
OT-33 IS
8010 IS
7520 IS
7020 IS
6033 IS
6010 IS
6005
Appearance Yellow non-flying powder 5.2
Heating loss(80℃±2℃)/% ≤ 0.50 5.3
Ash content (600℃±25℃)/% ≤ 0.15 5.4
Residue on sieve (150μm)/% ≤ — 1.0 5.5
Acidity (calculated in H2SO4)/% ≤ 0.05 5.6
Total sulfur content/% 78.5~81.5 89.0~91.0 79.0~81.0 66.0~68.0 89.0~91.0 79.0~81.0 79.0~81.0 66.0~68.0 89.0~91.0 94.0~96.0 5.7
Insoluble sulfur content/% ≥ 72.0 81.0 72.0 60.0 81.0 75.0 72.0 60.0 60.0 60.0 5.8
Oil content/% 18.5~21.5 9.0~11.0 19.0~21.0 32.0~34.0 9.0~11.0 19.0~21.0 19.0~21.0 32.0~34.0 9.0~11.0 4.0~6.0 5.9
Heat stability (105℃)/% ≥ 75.0 — 5.10
Heat stability (120℃)/% ≥ 45.0 — 5.10
5 Test Method
5.1 General requirements
Unless otherwise specified, standard solution, preparations and products adopted in analysis are prepared according to those specified in GB/T 601 and GB/T 603, only recognized analytical reagent and Grade 3 water specified in GB/T 6682-2008 may be adopted for analysis.
Representation method and rounding off rule of test data in this standard shall meet the relevant requirements of rounding-off value comparison method in 4.3.3, GB/T 8170-2008.
5.2 Appearance
Visually inspect in natural light.
5.3 Determination of heating loss
Determination is carried out according to the requirements of 3.4, GB/T 11409-2008. Weigh about 5g sample with an accuracy of 0.0001g, control the temperature of electrothermal constant-temperature dry box at 80℃±2℃ and heat for 3h.
The absolute difference of two results in parallel determination shall not be greater than 0.04% and the arithmetic average of these two results is taken as the determination result.
5.4 Determination of ash content
Determination is carried out according to the requirements of 3.7, GB/T 11409-2008. Weigh about 5g sample with an accuracy of 0.0001g, control the temperature of high temperature furnace at 600℃±25℃ and burn for 30min.
The absolute difference of two results in parallel determination shall not be greater than 0.04% and the arithmetic average of these two results is taken as the determination result.
5.5 Determination of residue on sieve
Determination is carried out according to the requirements of 3.5.3, GB/T 11409-2008. Moisten the sample with ethanol, then add water for stirring and extruding, inject into screen mesh, sweep it with brush, then add ethanol for moistening, repeat for several times till it cannot be brushed away.
The difference of two results in parallel determination shall not be greater than 0.02% and the arithmetical average of results in these two results shall be taken as determination result.
5.6 Determination of acidity
5.6.1 Principle
Extract the acidic material in sample with the water containing a small amount of ethanol, bromothymol blue is adopted as indicator and standard sodium hydroxide volumetric solution is adopted for titration.
5.6.2 Reagents and materials
5.6.2.1 Absolute ethanol [64-17-5].
5.6.2.2 Standard sodium hydroxide volumetric solution: c(NaOH)=0.02mol/L, diluted by 5 times with c(NaOH)=0.1mol/L standard sodium hydroxide volumetric solution, prepared before use and recalibrated where necessary.
Foreword i
1 Scope
2 Normative References
3 Classification, Type and Labeling
4 Technical Requirements
5 Test Method
6 Inspection Rules
7 Marking, Packaging, Transportation and Storage
8 Safety
Annex A (Normative) Heavy While Oil
