HG/T 2879.3-1997 Determination of silicon content in clay of rubber compound
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HG/T2879.3—1997
This standard is a test method standard, equivalent to the international standard ISO5795-1:1988 "Rubber Compounds-Clay" Part 1 Appendix A (Determination of Silicon Content-Silicon Molybdenum Blue Photometric Method). The difference between this standard and ISO5795-1 Appendix A: ISO5795-1 Appendix A does not specify that the solution should be diluted with water to the scale when drawing the standard curve, while this standard clearly stipulates that it should be diluted with water to the scale. ISO5795-1 Appendix A stipulates that the blank solution should be added with the sample solution, while this standard clearly stipulates that the blank solution should not be added with the sample solution. ISO5795-1 Appendix A uses medium-speed ashless filter paper (Whatrman No. 40), while this standard stipulates that medium-speed ashless filter paper should be used. This standard adds Chapter 1 Scope, Chapter 2 Reference Standards, Chapter 6 Sampling, and Chapter 9 Test Report. The writing format of this standard is in accordance with 'GB/T1.1-1993 implementation. This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Carbon Black Industry Research and Design Institute of the Ministry of Chemical Industry; This standard is drafted by the Carbon Black Industry Research and Design Institute of the Ministry of Chemical Industry; The main drafters of this standard are: Yu Lian, Hu Kaibi, Xue Lei, HG/T2879.3-1997
ISO (International Organization for Standardization) is a worldwide joint organization of national standard groups (ISO member groups). The work of formulating international standards is usually carried out by ISO technical committees. Any member group interested in the basic profession of the established technical committee has the right to participate in the committee, and international organizations of various governmental or non-governmental institutions that have contact with ISO can also participate in this work. In all electrical technical standards, ISO works closely with the International Electrotechnical Commission (IEC). Before an international standard is adopted by the ISO Council, the technical committee will send the draft international standard to each member group for voting. According to ISO requirements, at least 75% of the member groups must vote to formally pass it. The international standard ISO5795-1 was formulated by TSO/TC45 Rubber and Rubber Products Standardization Technical Committee. The general standard ISO5795 is entitled Rubber Compounds - Clay, which includes the following three parts: - Part 1: Test methods (non-rubber tests) Part 2: Rubber tests
- Part 3: Technical conditions
Appendices A to F are components of ISO5795, and the first edition was released in 1988.
ICS83.040.20
Registration No. 453-1997
Chemical Industry Standard of the People's Republic of China
Rubber Compounding Ingredients-kaolinclay-Determination of silicon content1 Scope
1.1 This standard specifies the determination of silicon content in rubber compounding clay. HG / T 2879. 3 — 1997
cqv ISO 5795—1: 1988
1.2 This standard is applicable to the determination of silicon content in natural clay of rubber compounding ingredients, and can also be used for the determination of silicon content in other industrial natural clays.
1.3 This standard is applicable to the determination of silicon content in natural clay that has been chemically treated with acid-neutralizing substances (such as amines) during the production process.
1.4 This standard is not applicable to the determination of silicon content in natural clay that has been surface-modified (such as silane-treated). 1.5 This standard is not applicable to the determination of silicon content in natural clay that has been calcined. 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid and all standards will be Revision, all parties using this standard should explore the possibility of using the latest versions of the following standards, GB/T6682--92 Specifications and test methods for analytical laboratory water (eqvISO3696:1987) GB/T10530-89 Packaging, storage, transportation, sampling and acceptance methods for precipitated hydrated silicon dioxide in rubber compounding agents 3 Principle
The sample is melted with sodium carbonate to form insoluble silicon (insoluble silicon) in a concentrated acid medium, which is converted into volatile silicon tetrafluoride with hydrofluoric acid, and the mass loss is used as the mass of insoluble silicon to calculate. The mass of residual silicon in the filtrate is determined by the silica blue photometry. The total silicon content is the sum of insoluble silicon and residual silicon, expressed as a percentage of silicon dioxide mass. 4 Reagents and preparation
All reagents are analytically pure, and the test water should comply with the provisions of GB/T6682. Past: During the test, recognized safety and health regulations should be followed. 4.1 Anhydrous sodium carbonate.
4.2 Hydrochloric acid: 36% (m/m, p=1.18Mg/m4. 3 Hydrofluoric acid: 40% (m/m).
4.4 Ammonium molybdate solution: 80g/dm2
Weigh 8.0g of ammonium molybdate (NHMoOu·4H,O) and dissolve it in 80cm hot water, then dilute it with water to 100cm
Store it in a polyethylene bottle (5.1).
4.5 Ammonium ferrous sulfate (1l) solution: 100g/dm2 Approved by the Ministry of Chemical Industry of the People's Republic of China on April 21, 1997 and implemented on October 1, 1997
HG/ T 2879.3 —1997
Weigh 10g of ammonium ferrous sulfate (II) (NH4SO4·FeSO6H,O) crystals, dissolve in 60cm2 of hot water, add 0.2 cm2 of sulfur (4.9). Dilute with water to 100 cm2 Note: Use freshly prepared reagents
4.6 Ammonium ferrous sulfate (II) solution: 0.1g/dm2 (calculated as ferric oxide) Weigh 0.0603 of ammonium ferrous sulfate (III) (NH4Fe(SO4·12H,O) crystals, dissolve in 60cm2 of hot water containing 1cm of sulfuric acid (4.9). Then dilute with water to 100cm2 and store in a ethylene bottle (5.1).
4.7 Silver nitrate solution: 10g/dml
Dissolve 1.0 g of silver nitrate (AgNOg) crystals in water, then dilute with water to 100 cm2 stored in a brown glass bottle (5.6),
4. 8 Sulfuric acid solution: 50% (V / V)
Carefully measure 125cm of sulfuric acid (98% (m/m), P=1.84Mg/m) into a beaker containing 100cm2 of water, cool, then dilute to 250cm with water in a measuring tube and store in a polyethylene bottle (5.1).
4.9 Sulfuric acid solution: 20% (V/V)
Carefully measure 50cm of sulfuric acid (98% (m/m), P=1.84Mg/m2) into a beaker containing 150cm* of water, cool, then dilute to 250cm with water in a measuring tube and store in a polyethylene bottle (5.1).
4.10 Silicon standard solution: 1. 000 g/dm2 (prepared from high-purity silica or precipitated silica calcined to constant weight at 1100°C). Weigh 1.000 g (accurate to 1 mg) of calcined silica and 5 g of sodium carbonate (4.1), stack them in a platinum crucible (5.2) with a lid, and melt them. Move the platinum crucible into a nickel beaker (5.5), extract the melt with hot water, cool it, and then transfer the platinum crucible extract and the solution used to rinse the nickel beaker to a 1000 cm2 volumetric flask, dilute it to the mark with water, and store it in a vinyl bottle (5.1),
1cm*This standard solution contains 1.000 mg of silicon dioxide (Sio,). 4.11 Silicon standard solution: 50.0 mg/dm
Measure 50.0 cm2 of silicon standard solution (4.10) and place it in a 1000 cm2 volumetric flask, and dilute it to the mark with water. 1cm of this standard solution contains 50mg of silicon dioxide (SiO2). 4.12 Silicon standard solution: 10.0mg/dml
Measure 50.0cm of the silicon standard solution (4.11) and place it in a 250cm2 volumetric flask, dilute it to the mark with water, and 1cm of this standard solution contains 10mg of silicon dioxide (SiO2). 5.1 Polyethylene bottle with stopper: 250cm, 1dm2 5.2 Platinum: 20cm3, with platinum cover and platinum stirring rod (about 50mm long). 5.3 Meker blowtorch or similar blowtorch: the temperature can reach 900C, use sodium carbonate (4.1) to melt the sample (7.1.2), and can reach 1100℃ for the next step of burning (7.1.3. 4),5.4 Spectrophotometer: wavelength 400nm to 800nm, accuracy ±3nm, absorbance can be read directly at 800nm, 5.5 Brocade beaker: 200 cm2, 400 cm2.5.6 Brown glass bottle with stopper: 500 crm, 1000 cm*5.7 Analytical balance: accurate to 0.1 mg.
5.8 Constant temperature in drying oven: can be controlled at 105C±5℃.16
HG/T2879.3—1997Www.bzxZ.net
5.9 Pipette: 5 cm2, 10 cm, 20 cm, 50 cm2, Class A.5.10 Glass funnel,
5.11 Beaker: 50 cm, 100 cm2, 200 cm2500 cm, 600 cm25.12 Rubber-tipped glass rod: the rubber tip is about 60mm long,5.13 Electric heating plate.
5.14 Volumetric flask: 100 cm2, 250 cml.
5.15 Volumetric flask: 100 cm2, 250 cm1 000cml5. 16 Burette: 25 cm, 50 cm, Grade A. 6 Sampling
According to Chapter 5 of GB/T 10530.
7 Steps
7.1 Determination of insoluble silicon
7.1.1 Sample
Weigh about 1g of sample and place it on a pre-weighed (accurate to 0.1 mg) in a platinum crucible ((5.2), and then weigh the platinum crucible containing the sample to obtain the mass of the sample (m.). 7.1.2 Preparation of sample
Add 5 g of sodium carbonate (4.1) to the platinum crucible containing the sample several times, stir with a platinum stirrer (5.2), stir while adding to make it fully mixed, retain 0.5 g of sodium carbonate, cover the mixture with love, cover the platinum crucible, and carefully heat it on a blowtorch (5.3) (900℃) until the contents of the platinum crucible are completely melted, keep the molten state for 30 minutes, and then cool. 7.1.3 Determination
7.1.3.1 Place the cooled and covered platinum crucible in a 600 cm beaker, add 50 cm hot water, carefully add 30cm hydrochloric acid (4.2), cover the surface with blood, place the beaker on a low-temperature electric hot plate (85c±5c), heat until the melt separates from the platinum crucible, and take the platinum crucible out of the beaker. Rinse the melt in the platinum crucible with hot water, peel off the attached particles with a glass rod wrapped with a rubber head and rinse the crucible, place the rinse liquid in the beaker, rinse the cover in the same way, and place the rinse liquid in the beaker. 7.1.3.2 Place the contents of the beaker on a low-temperature electric hot plate, heat, and steam 7.1.3.3 Remove the beaker and cool it, add 10cm hydrochloric acid to permeate the residue, add 90cm hot water to dilute, heat to dissolve the soluble salt and filter with a funnel and a medium-speed ash-free filter paper with a diameter of 12.5cm, and collect the filtrate in a 500cm volumetric flask. Rinse the filter paper and beaker thoroughly with hot water, peel off the particles attached to the beaker with a glass rod wrapped with a rubber head, and continue to rinse until the filtrate flowing out of the funnel is , add a drop of silver nitrate solution (4.7) to check if it does not contain chloride. Collect all the filtrate in a 500cm volumetric flask and keep this filtrate (F,).
7.1.3.4 Move the filter paper into the platinum crucible (5.2), wipe the inside of the beaker with wet ash-free filter paper, put the wiped filter paper into the platinum crucible, place the platinum crucible and its contents in a drying oven at 105C±5℃, dry for 1b, then carefully place the crucible on a blowtorch (5.3) and burn it at a temperature of 1100℃ to remove all carbon-containing 7.1.3.5 Wet the residual silicon in the platinum amber crucible with water, add 10 drops of sulfuric acid solution (4.9), and add 10 cm hydrofluoric acid (4.3). Place the platinum crucible on a hot plate to evaporate until sulfuric acid fumes appear, then carefully move the crucible to a blowtorch (5.3) and burn at about 1000 °C for 5 min to drive away the residual sulfuric acid; cool the crucible in a dryer, weigh it, and weigh it to 0.1 m2. 7.2 Calculation of insoluble silicon mass
Instructions:
1) Appendix A of ISO5795--1 stipulates the use of Whatman NO.40 medium-speed ashless filter paper, 17
HG/T 2879.3 -—1997
The mass of insoluble silicon in the sample (7.1.1) is expressed in grams and calculated as follows: m, am, m2
Where: m——the mass of the melt added to the platinum crucible before adding hydrofluoric acid (7.1.3.4), Bmz——the mass of the melt added to the platinum crucible after adding hydrofluoric acid (7.1.3.5), g.7.3 Determination of residual silicon
7.3.1 Drawing of standard curve
7.3.1.1 Preparation of standard solution
Take six portions of silicon standard solution (4.12) and transfer them into six 100 cm volumetric flasks according to the volume of standard solution specified in Table 1. Then add 6 cm iron (and) ammonium sulfate solution (4.6) and 1 cm hydrochloric acid (4.2) respectively. Add 12 cr sulfuric acid solution (4.8) plus 10cm2 ammonium molybdate solution (4.4) plus 10cm ferrous (I) ammonium sulfate (4.5) for color display reaction, then dilute with water to scale 2), spread evenly and leave for 5min. For the standard calibration solution, only one silicon standard solution (4.12) is needed, and six standard solutions with serial numbers are prepared according to Table 1. Table 1 Standard calibration solution for silicon determination
Volume of silicon standard solution (4.12), cm
7.3.1.2 Spectrophotometer measurement method
Corresponding silicon content,
Adjust the wavelength of the spectrophotometer to about 800nm, and the colorimetric light path is 10mm. According to the six serial numbers of the silicon standard solution in Table 1, measure the absorbance of each standard solution at a wavelength of 800nm in turn and record them. 7.3.1.3 Use the silicon content as the horizontal axis and the corresponding absorbance as the vertical axis to draw a standard curve. 7. 7.4.1 Use 0.5 g of sodium carbonate (4.1) to melt the residue (7.1.3.5) in the crucible, extract with hot water according to the procedures specified in 7.1.2 and 7.1.3.1, add hydrochloric acid (4.2) drop by drop to acidify, then mix the extract with the retained filtrate (F,) of 7.1.3.3 and dilute to 500 cm2 (Fz). 7.4.2 Prepare two 100 cm2 volumetric flasks (bottles A and B), take 10 cm2 of the diluted filtrate (F,) and place it in bottle A, take 10 cm2 of the diluted filtrate (F,) and place it in bottle A. 2. Place distilled water in bottle B. Note: Bottle A is used to dissolve the sample and produce silicon molybdenum blue. Bottle B is used as the blank solution. The remaining dilute filtrate (F) is retained to determine the aluminum content and iron content. 7.4.3 Add 6 cm iron (III) ammonium sulfate solution (4.6) and 1 cm hydrochloric acid (4.2) to bottles A and B respectively, and then add an appropriate amount of water to make the volume of bottles A and B 50 cm ± 1 cm respectively. Instructions: 2) Appendix A of ISO 5795-1 does not specify dilution to the scale with water. This standard clearly stipulates that dilution to the scale with water is used. 3) In Appendix A of ISO 5795-1, bottle B is used as the blank solution. Add the sample solution. This standard has been corrected. No sample solution is added. 18 HG/T 2879.3-1997 7.4.4 Add 12 cm sulfuric acid solution (4.8) to bottle A, and then add 10 7.4.5 Add 12cm sulfuric acid solution (4.8) to bottle B, then add 10cm ammonium lead acid solution (4.4), shake and let stand for 5min. 7.4.6 Add 10cm ferrous sulfate (Il) ammonium solution (4.5) to bottles A and B respectively, dilute to 100cm, shake and let stand for 5min. 7.4.7 Measure with a spectrophotometer Adjust the wavelength of the spectrophotometer to 800nm, then move the sample solution in bottle A and the blank solution in bottle B into the optical path With a colorimetric concentration of 10 mm, take the solution in bottle B as the blank solution and determine the absorbance of the sample solution in bottle A. According to the measured absorbance of the sample solution in bottle A, determine the silicon content of the corresponding sample solution from the standard curve: μg (m) 7.5 Calculation of residual silicon mass
In the sample (7.1.1), the mass of residual silicon, ms, is expressed in g and is calculated as follows: m,
Where: m
m,×50
Determination (7.4) The mass of residual silicon in the sample is obtained from the curve, ug.8 Expression of results
Silicon (SO) content, expressed as mass percentage, is calculated as follows: (m, +m,) × 100
Where: m. \-——Sample (7.1.1) mass disk, g:m—-mass of insoluble silicon in the sample (calculated according to 7.2), g:ms—mass of residual silicon in the sample (calculated according to 7.5), g.9 Test report
The test report should include the following items:
, the standard number based on which this test is conducted:
b.Grade and marking of the specimen;
e. Test results;
d. Test date.
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