Some standard content:
Chemical Industry Standard of the People's Republic of China
Insoluble sulfur for rubber
1 Subject content and scope of application
HG/T 2525-93
This standard specifies the product classification, technical requirements, test methods, inspection rules and marking, packaging, transportation, storage and safety requirements of insoluble sulfur for rubber (IS for short).
This standard applies to rubber vulcanizer produced by ternary stable system gas phase method-2
Referenced standards
GB 190
Dangerous goods packaging marking
Packaging storage and transportation pictorial marking
GB/T 601
GB/T603
GB1250
GB 6003
Oil-filled and non-oil-filled insoluble sulfur. Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents Preparation of preparations and products used in test methods of chemical reagents Methods of expressing and determining limit values Test sieves
GB/T6678 General rules for sampling of chemical products
GB/T 6679
GB/T 6682
GB 8946
3 Product classification
General rules for sampling of solid chemical products
Specifications and test methods for water used in analytical laboratories Plastic woven bags
Insoluble sulfur is divided into oil-filled and non-oil-filled types. 4 Technical requirements
Insoluble sulfur shall meet the requirements specified in the following table;
Elemental sulfur content, %
Insoluble sulfur content, %
Oil content, %
Non-oil-filled type
Yellow powder
Approved by the Ministry of Chemical Industry of the People's Republic of China on September 8, 1993 118
IS70-20
Oil-filled type
IS60-33
IS60-10
Yellow non-flying powder
19. 00~21. 0032. 00~34. 00 9. 00~~11. 00IS60-05
4.00~~6.00
1994-07-01 implementation
Acidity (in H,S())
Heating loss (60℃)
150μm sieve residue
5Test method
HG/T 2525--93
Non-oil-filled type
IS70-20
Oil-filled type
IS60-33
IS60-10
IS60-05
Unless otherwise specified, the reagents and water used in this standard are analytically pure reagents and grade 3 water in accordance with GB/T6682. 5.1 Determination of the appearance of insoluble sulfur
Determined by visual inspection.
5.2 Determination of elemental sulfur content in insoluble sulfur 5.2.1 Determination of elemental sulfur content in oil-filled insoluble sulfur 5.2.1.1 Summary of method
Use n-hexane as solvent to separate the oil component in the product, filter, wash, dry, and weigh the mass of the remaining sulfur. 5.2.1.2 Reagents and materials
Sulfur-saturated n-hexane solution: Take a certain amount of n-hexane (Q/HL14-91) solvent, add soluble sulfur to it at a ratio of 3g sulfur per liter of n-hexane, stir well, let stand for 24 hours for use, and filter the solution before use. 5.2.1.3 Instruments and equipment
Ordinary laboratory instruments and
Electric heating blast drying oven, which can control the temperature at 60±2℃. a.
b. Glass filter, filter plate pore size 1540μm (G3), volume 30mL. 5.2.1.4 Analysis steps
Weigh about 5g of sample, accurate to 0.001g, and place it in a glass filter that has been constant weight at 60℃. In a fume hood, place the filter containing the sample on a suction flask and wash it several times with 100mL of sulfur-saturated n-hexane solution; adjust the suction speed so that it can be completed in about 5 minutes. Finally, try to dry the sample, then move it into a forced air drying oven at a temperature of 60±2℃ and dry it for 1h. Take it out and place it in a desiccator to cool to room temperature, and weigh it. Continue drying, cooling, and weighing until constant weight is reached. 5.2.1.5 Expression of analysis results
The content of elemental sulfur (S) in oil-filled insoluble sulfur expressed as mass percentage, X, is calculated according to formula (1): X, mz = m×100
Wherein: ml = mass of glass filter, g;
m2 - mass of glass filter plus mass of residue, g; m3 - mass of sample, g.
5.2.1.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.50%. 5.2.2 Determination of elemental sulfur content in non-oil-extended insoluble sulfur 5.2.2.1 Summary of the method
HG/T 2525--- 93
This standard adopts the method of deducting the sum of the impurities (acidity, heating loss and ash content) to obtain the elemental sulfur content in non-oil-extended insoluble sulfur.
5.2.2.2 Expression of analysis results
The elemental sulfur (S) content X, in non-oil-extended insoluble sulfur expressed as mass percentage is calculated according to formula (2): X, = 100 - (X, + X. + X,)
The acidity percentage determined in accordance with 5.5;
Where: X,--
X. ---The heating loss percentage determined in accordance with 5.6; X, is the ash percentage determined in accordance with 5.7. 5.3 Determination of insoluble sulfur content
5.3.1 Summary of method
Whether it is oil-filled or non-oil-filled insoluble sulfur, the soluble sulfur and oil components in the sample are separated by carbon disulfide, and the mass of the residue is weighed. 5.3.2 Reagents and materials
5.3.2.1 Carbon disulfide.
5.3.3 Instruments and equipment
Same as 5.2.1.3.
5.3.4 Analysis steps
Weigh about 5g of sample, accurate to 0.001g, and place it in a glass filter that has been constant weight at 60℃. In a fume hood, place the filter containing the sample on a suction flask. Wash with 100mL of carbon disulfide reagent several times, and adjust the suction speed so that it is completed in about 5 minutes. Finally, drain the sample as much as possible, and then transfer it to a forced air drying oven at a temperature of 60±2℃ and dry it for 1 hour. Take it out and place it in a desiccator to cool it to room temperature, and weigh it. Continue drying, cooling, and weighing until constant weight.
5.3.5 Expression of analysis results
The content of insoluble sulfur (1S) expressed as mass percentage X is calculated according to formula (3); X,
Where: mz--mass of the sample after washing and drying, g; m. Sample mass, ..
m×100
5.3.6 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 0.45%. 5.4 Determination of oil content in oil-filled insoluble sulfur 5.4.1 Summary of method
Use n-baxane as solvent to separate the oil component in the sample and calculate the oil content by reduction method. 5.4.2 Reagents and materials
Same as 5.2.1.2.
5.4.3 Instruments and equipment
Same as 5.2.1.3.
5.4.4 Analysis steps
Same as 5.2.1.4.
5.4.5 Expression of analysis results
The oil content X in the oil-filled insoluble sulfur expressed as a mass percentage is calculated according to formula (4): ms + m2 = m2 × 100
Wu Zhong: m-
Mass of glass filter, g;
HG/T 2525-93
mMass of glass filter plus mass of residue, g; m-mass of sample·g.
5.4.6 Tolerance
Take the arithmetic mean of the results of parallel determinations as the determination result. The absolute difference between the parallel determination results shall not exceed 0.50%. 5.5 Determination of acidity in insoluble sulfur (in terms of H2SO4) 5.5.1 Summary of the method
Whether it is oil-filled or non-oil-filled insoluble sulfur, the acidic substances in the sample are extracted with water containing a small amount of ethanol, and the titration is carried out with sodium hydroxide standard titration solution using bromothymol blue as an indicator. 5.5.2 Reagents and materials
5.5.2.1 Anhydrous ethanol (GB/T678).
5.5.2.2 Standard titration solution of sodium hydroxide (GB/T629): c(NaO)H) = 0.1 mol/L, prepared and calibrated according to GB/T601. 5.5.2.3 Standard titration solution of sodium hydroxide (GB/T629): c(NaOH) = 0.02mol/L, dilute the NaOH standard titration solution (5.5.2.2) 5 times. Prepare this solution when using and recalibrate if necessary. 5.5.2.4 Bromothymol blue (HG3-1222) indicator: Prepare according to the provisions of GB/T603. 5.5.3 Analysis steps
Weigh about 10g of sample, accurate to 0.1g, in a 400mL beaker, add 15mL of anhydrous ethanol, stir to fully wet the sample, add 200ml of water and stir for 2-3min, let stand for 5min, add 10 drops of bromothymol blue indicator, and use sodium hydroxide standard titration solution (5.52.3) until the end point is blue-green.
5.5.4 Blank test
No sample is added, and the analysis steps are exactly the same as 5.5.3. 5.5.5 Expression of analysis results
The acidity X expressed as a mass percentage is calculated according to formula (5): (V - V.) c X 0. 049 04
Wherein: V--the volume of sodium hydroxide standard titration solution consumed in the determination, mL; V.--the volume of sodium hydroxide standard titration solution consumed in the blank test, mL; (--the actual concentration of sodium hydroxide standard titration solution, mol/L; ·(5
ms--the mass of the sample, g;
0.04904--the mass of sulfuric acid in grams equivalent to 1.00 ml of sodium hydroxide standard titration solution [c (NaOH) = 1.000 mol/L].
5.5.6 Allowable difference || tt||Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 0.01%. 5.6 Determination of heating loss in insoluble sulfur 5.6.1 Method summary
Heat the oil-filled or non-oil-filled insoluble sulfur sample at 60℃, and the reduced mass is the mass of moisture and volatile matter in the sample. 5.6.2 Instruments and equipment
Ordinary laboratory instruments and
Weighing bottle: diameter 70mm, height 35mm;
b. Electric heating blast drying oven: can control the temperature at 60±2℃. 5 .6.3 Analysis steps
Weigh about 5g of sample, accurate to 0.001g, place in a weighing bottle at 60℃ and keep constant weight, put in a drying oven controlled at 60±2℃ and dry for 4h. Take out and cool to room temperature in a desiccator, and weigh. Continue drying, cooling and weighing until constant weight. 5.6.4 Expression of analysis results
HG/T2525—93
Heating reduction X in insoluble sulfur expressed as mass percentage. Calculate according to formula (6): m2×100
Where: mz——mass reduction after heating and drying Amount, g; mg
Sample mass, g.
5.6.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.01%. 5.7 Determination of ash content in insoluble sulfur
5.7.1 Summary of method
Carbonize the oil-filled or non-oil-filled insoluble sulfur sample and burn it to constant weight, and weigh the mass of the residue. 5.7.2 Instruments and equipment
Ordinary laboratory instruments and
a, quartz evaporating blood or porcelain crucible: volume of 50 ml; b. Closed electric furnace,
c. High temperature box-type electric heating furnace: the temperature can be controlled at 750±25℃. (6)
5.7.3 Analysis steps
Weigh about 5g of sample, accurate to 0.01g, and place it in a quartz evaporator III or porcelain crucible that has been weighed in advance. Slowly heat it on the closed electric furnace plate until it is completely carbonized, then place it in a high temperature box-type electric heating furnace at 750±25℃, burn for 30min, carefully take it out and place it in a desiccator to cool to room temperature, and weigh it. Continue burning, cooling, and weighing until constant weight. 5.7.4 Expression of analysis results
The ash content X in insoluble sulfur expressed as mass percentage is calculated according to formula (7): mg ×100
Where: m. —-mass of the residue after burning, g; —mass of the sample, g.
5.7.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.02%. 5.8 Determination of sieve residue of insoluble sulfur
·(7))
5.8.1 Summary of method
A known amount of sample is passed through a specified sieve and its residue is weighed. Two operations are specified: (1) Dry method for non-oil-filled insoluble sulfur; (2) Wet method for oil-filled insoluble sulfur.
5.8.2 Reagents and materials
5.8.2.1 Anhydrous ethanol (GB/T678).
5.8.3 Instruments and equipment
Ordinary laboratory instruments and
Electric heating blast drying oven: can control the temperature of 105±2℃; 150μm test sieve: in line with GB6003;
Surface blood;
Wet sieving device.
Filtered products
HG/T2525—93
Rubber hose
Pressure reducing valve
Zone valve B
Schematic diagram of wet sieving device
5.8.4 Analysis steps
a. Dry method: Weigh about 10g of sample, accurate to 0.01g, and place it in a test sieve with an aperture of 150um, vibrate the sieve and brush it repeatedly with a soft brush, and move the remaining sieve residue to the surface III of known mass for weighing. b. Wet method: Before loading the sample, open valves A and B as shown in the figure, and close valves C and D at the same time, and rinse the filter with water for 2 minutes. Then close valve B, gently open valve C, let the water flow out, and adjust the water pressure to 0.210±0.035MPa through the pressure reducing valve. After installing the screening device, rinse with water and confirm that there are no impurities, weigh 50g of the sample, accurate to 0.01g, put it in a 600mL beaker, add a little surfactant, fully wet it, add 200mL of water and stir, so that the wetted sample is evenly dispersed. While passing the water flow with adjusted pressure through the screen, slowly transfer the wetted and dispersed sample into the screen quantitatively, and be careful not to fill the screen. Then open valve D, let the water in the hose become a thin stream, and continuously rinse the screen and the sample on the screen wall until it can no longer be washed down. Remove the screen, rub it gently with your fingers, crush the unscreened residue, and separate it from the screen without sticking (do not rub it with wet paper). After cleaning, install the sieve on the sieving device and rinse for 2 minutes. Remove the sieve and dry it at 105℃ for 1 hour. Move the residue to a surface of known mass and weigh it.
5.8.5 Expression of analysis results
Content of insoluble sulfur residue X expressed as mass percentage: Calculate according to formula (8): X. =Www.bzxZ.net
Mass of residue, g;
Where: mu-—
Mass of sample, g.
mm×100
5.8.6 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 0.05%. 6 Inspection rules
(8)
6.1 Insoluble sulfur products shall be inspected by the quality inspection department of the manufacturer. Each batch of insoluble sulfur leaving the factory must meet the requirements of this standard123
HG/T2525-93
and be accompanied by a quality certificate, the contents of which include the manufacturer's name, trademark, product name, model, batch number, gross weight and net weight, production date, etc. 6.2 The user has the right to inspect and accept the received insoluble sulfur for rubber in accordance with the provisions of this standard. 6.3 The batch size of each batch of products shall not exceed 1 t. 6.4 Sampling
6.4.1 Determine the number of sampling units in accordance with the provisions of Article 6.6 of GB/T6678. 6.4.2 Determine the sampling method in accordance with the provisions of Article 2.3.1 of GB/T6679. Quickly pour all the samples onto a flat clean surface, and use the quartering method to reduce them to about 500g. Immediately put them into two clean, dry bottles with ground mouths, seal them with covers and label them, indicating the manufacturer name, product name, batch number, sampling date, and name of the sampler. One bottle is used as a test sample, and the other is kept as a reserved sample. 6.5 If one of the indicators in the test results does not meet the requirements of this standard, samples shall be taken from bags with twice the number of sampling units of the same batch of products and re-tested. The results are applicable to the entire batch of products. If one of the indicators in the re-test results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 6.6 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 6.7 Determine whether the test results meet the standards in accordance with the rounded value comparison method specified in GB1250. 7 Marking, packaging, transportation and storage
7.1 The packaging bags should have firm and clear markings, including: manufacturer name, product name, trademark, batch number, model, production date, net weight, this standard number and GB190 mark 8 "flammable solid" and GB191 mark 7 "moisture-sensitive". 7.2 Insoluble sulfur products are packaged in plastic woven bags. Plastic woven bags should meet the requirements of GB8946, lined with plastic bags, with a bag thickness of 0.18~0.25mm, and the volume of the bag should be greater than the outer packaging. The inner bag is double-tied, and the outer bag is folded and mechanically sewn with a stitch length of no more than 10mm. The net weight of each bag is 25kg, or the packaging quantity is determined according to user requirements. 7.3 Insoluble sulfur should be covered during transportation and should not be mixed with alkaline substances. Pay attention to fire, heat and moisture prevention to prevent product deterioration. 7.4 Insoluble sulfur should be stored in a dry, ventilated and cool warehouse. The storage site should pay attention to fire, moisture and heat prevention. The storage temperature should not exceed 45℃, and it should not be close to alkaline substances to prevent pressure and agglomeration. The storage period is 1 year from the date of production. 8 Safety requirements
8.1 Insoluble sulfur for rubber is non-toxic and flammable. Special fire-fighting equipment should be installed in the storage places and warehouses, and open flames are strictly prohibited. 8.2. Workers engaged in the production, transportation, storage and processing of insoluble sulfur for rubber should use necessary protective equipment during operation. Additional notes:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Nanjing Chemical Industry (Group) Corporation Research Institute. This standard was drafted by the Nanjing Chemical Industry (Group) Corporation Research Institute. The main drafters of this standard are Wang Songjie, Qi Yumei and Pu Qijun. 124
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