HG/T 2879.5-1997 Determination of total iron content in clay for rubber compounding
Some standard content:
HG / T 2879. 5 - 1997
This standard is a test method standard, equivalent to the international standard ISO5795-1: 1988 "Rubber Compounds - Clay" Part 1 Appendix C (Determination of total iron content 2,2-bipyridine photometric method), the main technical differences between this standard and ISO5795-1: 1988: According to the requirements of GB/T1.1-1993, this standard adds three chapters: reference standards, scope and test report. This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China, and 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 Xue Lei, Yu Lian, Hu Kaibi, HG/T2879.5-m1997
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 a certain profession for which a technical committee has been established has the right to participate in the committee. International organizations, whether governmental or non-governmental, that have relations with ISO may also participate in this work. ISO works closely with the International Electrotechnical Commission (IEC) in all aspects of electrical technical standards. Before an international standard is adopted by the ISO Council, the technical committee sends the draft international standard to each member group for voting. According to ISO requirements, at least 75% of the member groups must vote in favor before it can be formally adopted as an international standard. ISO5795-1 was developed by ISO/TC45 Technical Committee for Standardization of Rubber and Rubber Products. The general standard ISO5795 is entitled Rubber Compounding Agents, and 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 the components of ISO5795. The first edition was published in 1988, ICS83.040. 20
Record No. 455—1997
Chemical Industry Standard of the People's Republic of China
Rubber Compounding Ingredients-kaolirclay-Determination of total iron contcnt1 Scope
HG / T 2879. 5 — 1997
eq ISO 5795---17 1988
1.1 This standard specifies the determination of the total iron content of rubber compounding clay by 2,2\-bipyridine photometry. 1.2 This standard is applicable to the determination of the total iron content of natural clay for rubber compounding, and can also be used for the determination of the total iron content of other industrial natural clays.
1.3 This standard is applicable to the determination of the total iron content of 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 total iron content of natural clay with surface modification (such as silane treatment). 1.5 This standard is not applicable to the determination of total iron content of natural clay after calcination. 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. All standards will be revised. 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 for analytical laboratories (eqVISO3696:1987) GB/T2879.3-1997 Determination of silicon content of clay for rubber compounding (eqISO5795-1:1988) 3 Principle
The sample is melted with sodium carbonate to make iron acid-soluble, and 2,2'-bipyridine is used as a color developer to determine the total iron content of the sample by photometry.
4 Reagents
All reagents are analytically pure. The test water meets the requirements of GB/T6682. 4.1 Hydrochloric acid: 36% (m/m), p=1.1 Mg/m, 4.2 Ammonium acetate solution: 200 g/dm
Dissolve 200 g of ammonium acetate (CH,COONH) in 600 cm of water, and then dilute to 1000 cm with water in a measuring cylinder. 4.3 2,2-Bipyridine solution: 2 g/dm3Dissolve 0.2 g of 2,2'-bipyridine ((C,H,N)) in 60 cm of warm water, cool, and dilute to 100 with water in a measuring cylinder. cm
This solution is valid for four weeks.
4.4 Hydroxylamine hydrochloride: 500 g/dm
Dissolve 50 g of hydroxylamine hydrochloride (HONH,CI) in 50 cm2 of water and dilute to 100 cm2 with water in a measuring tube.4.5 Nitric acid: p=1.42 Mg/m.
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, 5 — 1997
4.6 Iron standard stock solution: 1 000 mg/dm2 in a 100 cm beaker. Dissolve 1.000 ± 0.001 wt% pure iron in a mixture of 10 cm of water and 5 cm of nitric acid (4.5) and boil to expel nitrogen oxides. After cooling, transfer the solution to a 1 000 cm' volumetric flask, dilute to the mark with water and shake well. 1 cm of this standard solution contains 1000 μg of iron.
4.7 Iron standard solution: 50 mg/dm.
Use a pipette to transfer 50.0 cm of the iron standard stock solution (4.6) to a 1 000 cm' volumetric flask, add 10 cm of acetic acid (4.1), dilute to the mark with water and shake well. 1 cm of this standard solution contains 50 μg of iron. 4.8 Iron standard solution: 10 mg/dm2
Use a pipette to transfer 50.0 cm\ of the iron standard solution (4.7) into a 250 cm volumetric flask, add 2.5 cm hydrochloric acid (4.1), dilute to the mark with water and shake. 1 cm This standard solution contains 10 mg/dm2 of iron.
5 Instruments
Conventional laboratory instruments and:
5.1 Spectrophotometer: The wavelength can be adjusted between 400 nm and 800 nm. 5.2 Analytical balance: accurate to 0.0001 nm. 6 Steps
6.1 Preparation of test solution
6 1.1 Pipette 20 cm2 of filtrate F (see HG/T 2879.3-1997 7.4.1) into a 50 cm2 volumetric flask.
6.1.2 Add 0.5 cm2 of hydroxylamine hydrochloride solution [4.4), 2 cm2 of 2°-bipyridyl solution (4.3) and 10 cm2 of ammonium acetate solution (4.2). Dilute to the mark with water and mix. After leaving for 10 min, place the photometric disk (7.1). 6.2 Drawing of standard curveWww.bzxZ.net
6.2.1 In a group of 6 50 cm2 volumetric flasks, add 0 cm2, 5.0 cm2, 10.0 cm2, 2 ...5.0 cm2, 20.0 cm2, 25.0 cm2, 25.0 cm2, 20.0 cm2, 25.0 cm2, 25.0 cm2, 25.0 cm2, 25.0 cm2, 25.0 cm2, 25.0 cm2, 25.0 cm2, 25.0 cm2, 25.0 cm2, 30.0cm iron standard solution (4.8), these 6 volumetric flasks contain 0μg, 50μg, 100μg, 200μg, 250μg and 300g of iron respectively,
6.2.2 For each standard solution, follow the color development procedure (6.1.2) to perform color development reaction 6.2.3 Use water as the reference solution, in a receiving cell with an optical path of 10mm, use a spectrophotometer (5.1) at a wavelength of 520 Measure the absorbance of each standard solution at nm.
6.2.4 Draw a curve with the amount of iron contained in each of the above-mentioned volumetric flasks as the horizontal axis and the corresponding absorbance as the vertical axis, which is the standard curve.
7.1 According to (6.1.2), use water as the reference solution and use a spectrophotometer to measure the absorbance of the solution at a wavelength of 520nm in an absorption cell with an optical path of 10mm.
7.2 Use the measured absorbance on the standard curve ( 6.2.4) to find the iron content of the test solution (ms). 7.3 If the absorbance exceeds the range of the standard curve (6.2.4), reduce the amount of sample (absorb from F in HG/T 2879.3-19977.4.1) and perform reverse determination to make the absorbance within the range of the standard curve. 8 Results are expressed as
Total iron content (Fe0), expressed as mass percentage, calculated according to the following formula: 28
HG/T 2872, 5 1997
mg×1.43×500
Wherein: mg—mass of the test sample (HG/T 2879.3-19977:1:1), g:—mass of iron in the test solution obtained by (7.2), g; m
Vs——volume of the test solution (6.1.1), cm; 1.43-
—conversion factor for converting the measured iron content into the total content of Fe, O, 9Test report
The test report should include the following items:
Standard number based on which the test is conducted;
Complete number and origin of the test sample;
Test results;
Record abnormal phenomena that occur during the test;
Test date.
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