Some standard content:
HG/T2879.2—1997
This standard is a test method standard, equivalent to the international standard ISO5795-1:1988 "Rubber Compounds-Ceramics" Part 1 Appendix B (Determination of aluminum content-EDTA titration method). The difference between this standard and ISO5795-1 Appendix B: This standard adds Chapter 1 Scope, Chapter 2 Reference Standards, and Chapter 8 Test Report. The writing format of this standard is implemented in accordance with GB/T1.1-1993. This standard was 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 was drafted by the Carbon Black Industry Research and Design Institute of the Ministry of Chemical Industry: The main drafters of this standard: Yu Lian, Hu Kaibi, Xue Lei HG/T2879.2—1997
ISO Foreword
ISO. (International Organization for Standardization) is a global federation of national standards bodies (ISO member bodies). The work of formulating international standards is usually carried out by ISO technical committees. Any member group interested in a profession for which a technical committee has been established has the right to participate in the committee: international organizations, governmental or non-governmental organizations in contact with ISO may 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, it can be formally passed only if at least 75% of the member groups vote in favor. The international standard ISO5795--1 was formulated by ISO/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 Appendix A to F are components of ISO5795, and the first edition was published in 1988.
ICS83. 040. 20
Registration No. 452—1997
Chemical Industry Standard of the People's Republic of China
Rubber Conpounding ingredients-kaolinclay-Determination of aluminium content1 Scope
HG / T 2879. 2 —1997
eqy IS0 5795—1: 1988
1.1 This standard specifies the determination of the aluminium content of rubber compounding kaolinclay by EDTA titration. 1.2 This standard is applicable to the determination of the aluminium content of natural kaolinclay in rubber compounding ingredients and can also be used for the determination of the lead content of other industrial natural kaolinclays.
1.3 This standard applies to the determination of aluminum content in natural clay that has been chemically treated with acid-neutralizing substances (such as amines) during the production process.
1.4 This standard does not apply to the determination of aluminum content in natural clay that has been surface-modified (such as silane treatment). 1.5 This standard does not apply to the determination of aluminum content in burned natural clay. 2 Referenced standards
The following standards contain clauses that constitute the clauses of this standard through reference in this standard. When the standard is published, the versions shown are valid. All standards will be revised. 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 water in analytical experiments (cqVISO3696:1987) HG/T2879.3-1997 Determination of silicon content in rubber compound clay (eq?ISO 5795-1:1988)3 Principle
Quantitatively absorb the filtrate F2 for determination of silicon content: Use copper iron reagent-chloroform extraction method to remove all iron and titanium. After separation, add excess EDTA standard solution to the water layer to complex aluminum. Use zinc standard titration solution to back-titrate excess EDTA to obtain the content of aluminum (A1,0,)-
Reagents and preparation
All reagents are analytically pure, and the test water meets the requirements of GB/T6682. Note: During the analysis process, the recognized safety and health regulations should be followed. 4.1 Nitroform.
4.2 Anhydrous ethanol,
4.3 Hydrochloric acid: 36% (m/m). p=1.18 Mg/m2.4. 4 Ammonia: 35% (m/m), p=0.880 Mg/m24.5 Ammonium acetate buffer solution
In 500 cm2 of water, add 120 cm2 of glacial acetic acid, stir, immediately add 74 cm2 of ammonia (4.4), stir, cool, dilute with water to 1 dm
4.6 Copper iron reagent: 60 g/dm
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. 2 - 1997
Dissolve 6.0 g of cupferric reagent rC,H,N(NO)ONH in 50 cm2 of water. Dilute to 100 cm with water and filter to remove insoluble matter.
Use freshly prepared reagents.
4.7 Zinc standard titration solution: c(1/2 Znz)=0.05 mol/dm2In a 100 cm2 beaker, add 15 cm2 of hydrochloric acid (4.3) to dissolve 3.2685 g of pure zinc fragments. Transfer this solution to a 1 000 cm2 volumetric flask and dilute to the mark with water. 4.8 EDTA standard solution: c(EDTA)=0.05 mol/dm234.8.1 Preparation
In a 1 000 cm2 volumetric flask, use 800 cm2 of water to dissolve 18.612 g of EDTA (CH,N(CH,COOH)CH,CO0Na]z 2H,O Dilute with water to the mark.
4.8.2 Calibration
Accurately pipette 20.0cm*EDTA solution (4.8.1) into a 500cm2 conical flask, add 4 drops of phenol blue indicator (4.9), then add ammonium acetate buffer solution (4.5) until the solution changes from yellow to blue, then add 10cm excess ammonium acetate buffer solution, dilute with water to about 100cm, immediately add an equal volume of ethanol (4.2), add 1cm to 2cm*dithiol indicator (4.10), and titrate with zinc standard titration solution (4.7) until the solution turns pink and remains unchanged. That is the end point, record the volume consumed in the titration, cm3 (Va),
4.8.3 Calculation of calibration coefficient
The calibration coefficient is calculated by the following formula, which must be adjusted to 1 to be applicable to (6.2) and (7). The concentration of the EDTA solution used can be accurately expressed as 0.05 mol/dm3V
Where: V—the volume of the absorbed EDTA standard solution (4.8), cm, (V,=20cm\) V—the volume of the zinc standard solution (4.7) consumed for calibration, cm34.9 Bromophenol blue indicator: 1 island/dm3
Weigh 0. 10 g bromophenol blue, dissolved in 1.5 cm2 sodium hydroxide solution c(NaOH) = 0.1 mol/dm2, diluted with water to 100 cm
4.10 Dithiol indicator: 0.25 g/dm3
Weigh 0.025 g dithiol (C,H,N,CSNHNHC,H,), dissolved in 80 cm2 ethanol (4.2), diluted with anhydrous ethanol to 100 cm2
5 Instruments
Conventional laboratory instruments and:
5.1 Analytical balance: accurate to 0.1 mg.
5. 2 Pipette: 20 cm2, 25 cm2, 50 cm2, Class A.5.3 Conical flask with stopper: 250 cm2, 500 cm25. 4 Volumetric flask: 1 000 cm
5.5 Measuring cylinder: 20 cm2, 100 cm.
5.6 Beaker: 50 cm2, 100 cm, 200 cm5.7 Separating funnel: 250 cm
5.8 Burette: 50 cm, Class A
6 Steps
HG/T 2879.2-1997
6. 1 Use a pipette to accurately draw 100 cm2 of the filtrate F (see HG/T 2879.3-1997 7.4.1), inject it into a 250 cm separating funnel, add 20 cm2 of hydrochloric acid (4.3), shake and cool, add 2 cm2 of cupferric reagent (4.6) to mix, and then add 20 cm2 of fluoroform (4.1) Vibrate for 30 seconds to extract the copper iron reagent salt, separate the chloroform extraction, exclude and discard it, add 20cm2 ammonia to extract until the mixed solution is separated, add 1cm copper iron reagent, and analyze the water layer. When the copper iron reagent salt is completely extracted, the reactant will form a white precipitate instantly. Continue to extract with fresh ammonia until the copper iron reagent salt and excess iron reagent are completely extracted to show a watery white chloroform layer (excess iron reagent will make the ammonia form appear green), and discard all the chloroform to obtain the liquid. 6.2 Quantitatively transfer the remaining aqueous layer to a 500 cm conical flask and heat to boil to remove trace amounts of chloroform. Cool, add 4 drops of bromoirieus blue indicator (4.9), carefully add ammonia water (4.4) until the color changes from yellow to blue, then add hydrochloric acid (4.3) dropwise to acidify until the solution appears yellow, then add 4 to 6 drops of ethyl acetate (4.3), use a burette to add enough EDTA solution (4.8) until all the aluminum is converted into a complex, then add 2 cm' of EDTA solution. Record the volume (V) cm of EDTA solution added. Add ammonium acetate buffer solution (4.5) until the color of the phenol blue indicator changes from yellow to blue. Add another 10 cm* of ammonium acetate buffer solution, then heat the solution to boiling for 10 min, cool to room temperature, 6.3 dilute the above solution with an equal volume of ethanol (4.2), add 1 cm2 to 2 cm2 of disulfide indicator (4.10), and then titrate with zinc standard solution (4.7) until the solution turns pink and remains unchanged, which is the end point. Record the volume (v) of zinc standard solution consumed in the titration. cm*
7 Calculation of results
The aluminum (Al,O,) content, expressed as mass percentage, is calculated as follows: (VV,)× 0. 002 55 × 5 × 100m. wwW.bzxz.Net
Wherein: V——the volume of EDTA standard solution added to the sample solution with a turbidity of 0.05 mol/dm2, cm2; V is the volume of zinc standard solution consumed by titrating the excess EDTA in the sample solution, cm; m
—mass of the sample (see HG/T2879.3), g, 0.00255 is 1.00 cm2 EDTA solution c(EDTA)=0.05 mol/dm2; equivalent to the mass of aluminum, g. 8 Test report
The test report should include the following items:
The standard number based on which this test is conducted;
b. The grade and mark of the sample;
Test results;
Test date,
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