This standard specifies the method for determining the zinc content in rubber by atomic absorption spectrometry. This standard is applicable to raw rubber, compound rubber and vulcanized rubber with a zinc mass fraction of more than 0.05%. Samples with a zinc mass fraction lower than 0.05% can also be determined by adjusting the sample mass or the test solution concentration. For samples with low zinc content, it is recommended to use the standard addition method. GB/T 4500-2003 Determination of zinc content in rubber Atomic absorption spectrometry GB/T4500-2003 standard download decompression password: www.bzxz.net

GB/T 450—2003
This standard is equivalent to GB/T 450-2003 (15) 61011:1951≤ micro-calcination content determination method for determination of zinc content by absorption spectroscopy. This standard replaces (FV14510—1981) standard for determination of zinc content in rubber. The original standard of GB/T 450-2003 has been discussed technically:
not standard 15061071, 1991 re-listed, the technical differences are as follows: a) This standard applies to raw rubber, latex, mixed rubber and sparse rubber: 4 standard! ) Replacement S>101.: Vegetable rubber, aged products: Because vegetable rubber includes slow-acting rubber products. Fast-acting rubber is more comprehensive in application; ) This standard is for the sampling of non-vegetable rubbers and the sampling of new rubbers (wood standard No. 1S>Replacement 61011, 199: The sampling specifications for products. Due to the change of applicable objects, the sampling method is also adjusted: the same standard is used more than IS6101-1:15S1 for the preparation of scientific and technical samples of G/77 vulcanized rubber cavity), this standard is used in the dilution test solution (4.?.7.1.2.2.7, 4) with acid 2+100 (V+V> release acid 2+100 (V+V> release acid 2+100 (V, +V) = +2 (V, +V). When preparing a series of standard solutions, it is easy to network the instrument process because the concentration of hydrochloric acid solution is too high, which wastes medicine, while the type test uses more than 10 salt consumption, and the test purity is not affected at all. e) Preparation of series of standard solutions, the concentration (mg/mL) is replaced by 0.6.5.1.0, 2.3..0, 1.0, 2.5, 1.2, 5.(7.\1), which must be the concentration range of the series of standard solutions used for the sensitivity evaluation of the instrument. In order to compensate for the influence, this standard has also made the following changes: the unit of concentration and volume are changed from Mgcm.uR/imm to R/mLug/nL.mI respectively. The main changes of this standard compared with the previous version are as follows: a) The name of the standard has changed. The original name is: "Zinc content in vulcanized rubber" The flame method for determination of the amount of heat radiation (the method is more than 2.5 °C) of the standard is used to expand the scope of this standard. The scope of this standard is expanded to include rubber and chemical rubber. The mass fraction of the release potential is .1~\.% and the mass fraction of the release potential is above 3.05%. The 11 standard liquids in this edition are replaced by the 99% pure rubber with a mass fraction of 93% to 19% pure rubber (2.5 °C in the 1084 edition). The zinc content (R/m) of the series of standard solutions is changed. 0.0.3.0.42.., 1.0 is changed to (.0.71.0, 2.9..0 (1084 edition 5.3.1, this version 7.3.1! Added the "standard addition method"
The appendix of this standard is the standard appendix, the standard of the National Rubber Standardization Committee General Chemical Test Method T35/S11> Mountain Inch. The responsible drafting units of this standard are: China Rubber Group Beijing Institute of Industry Research and Design, Hualin Tire Co., Ltd. The main authors of this standard are: Kang Li, Xiao Feihui, Su Xingse, Ben Er, Jing Meizi. The version of the standard represented by this standard is released as follows: 6bT 4600—1981.
Determination of zinc content in rubber by atomic absorption spectrometry GB/I4500—2003
Notice: Personnel using this standard should have practical experience in formal laboratory work. This standard does not indicate all possible safety issues. Users are responsible for taking appropriate safety and quality measures and ensuring compliance with relevant national laws and regulations. 1 Scope
This standard specifies the atomic absorption spectrometric method for determining the zinc content in rubber. This standard is applicable to raw rubber, semi-refined rubber and refining rubber with a zinc content of 0.05% or more. Samples with a zinc content of less than 3.055% are not included in the sample quality test solution. For samples with a lower zinc content, the standard method can also be used for determination. 2 Normative references
The following documents have become the provisions of this standard through explicit reference. From the date of the referenced document, all subsequent amendments (including the date of the referenced document) shall not apply to this standard: however, the latest editions of these documents shall not be used by the parties to the standard if the agreement is not reached. Any new edition of the document not specified in the date of the referenced document shall apply. GTS such as Determination of the extinction value (eV) of rubber 27)
GB/T 1534C: dLS0: Preparation of natural and synthetic rubber samples and test specimens (I150) 41-2) 3 Principle
Under the following formula, the new aldehyde is converted into a controlled aldehyde and the concentration is not adjusted. The determination is carried out by atomic absorption spectroscopy at 213% nm. The compounds containing ton should be removed by acid and hydrogen acid. Reagents: 4.1 Ethanol e-1.84R/mlt
4.2 Hydrochloric acid solution: 1+2(,-V,:
4.3 Hydrochloric acid solution: 1!1C (VV)
4.4 Acid: molar fraction is 36~1%
4.5 Triturated acid: 2=1.42gml:
4.6 Concentrated nitric acid, 111(V,-V);
4.7 Take a standard dropper (1m/ml.)
Weigh 1.G0 zinc powder (plate Dissolve in a little or no hydrochloric acid to reduce the concentration to 4.2, cool and transfer to a volume of 1320, which is faster than salt (4) sieve-resistant to standard 4. Xin standard Ya braid sensitive l: Rl.
absorption 11)ml. Feng standard energy reduction 4.71 1)ml. Put it into a volumetric bottle. Use salt solution (1, dilute to the scale, stop. This standard liquid is now in use,
stock laboratory research common night instrument and the following equipment: G/T 4500—2003
5.1 Absorption light instrument:
5.2 Level: divided into 0.1m:
5.3 Screening furnace, adjust humidity at 0±25:54 total funnel of acetic acid sand
5.6 Platinum or net ethylene oxide support;
5.7 Electric heating or technical resources,
6 Sampling
6.1 Glue according to 63/T1 complete implementation
6,2 Mixing cavity according to (/T17733 according to the data
3 Abandoned nuclear stock according to G1783 on the heat,
7 Analysis 7.1 Preparation of test solution 7.1.1 Ashing of sample 7.1.1.1 Take 0.1% of the test solution (accurate to 0.1%) and place it in a suitable container according to G/T84 method 02. 7.1.1.2 Take 100% of the test solution in a 2cm thick tube. Add 100% acid and start to decompose the sample. After cooling, add 5% nitric acid and continue to heat until the sample is completely decomposed. There is no more smoke and the sample is ready for use. Use 15L nitric acid. Transfer the contents to a beaker several times. Steam on an electric heating water bath for ten minutes, transfer to a 1/4 inch furnace, and charge the mixture.
7.1.2 Decomposition of ash
7.1.2.5 Carefully add 2) FL pad (4.2) to the beaker and decompose (pay attention to the frothing and bubbling caused by the decomposition of carbonic acid). Use 5? mF. Add the melt (4.2) to the beaker several times. If all the residues are left, transfer the seeds to 1 C. bottle and add the acid concentrate (4.3) to the mark. 7.1.2.2 The decomposition cannot be completely completed. . If necessary, re-mix or vortex. Follow 7.1.1, 1 or 7.1.1.2. After cleaning, add a few drops of chlorinated alcohol, heat in a ventilated electric heating electrode or water bath. Add 3 mL of fresh chlorinated alcohol, heat, and stir until dry. Stir with polytetrafluoroethylene while heating. Repeat the steps for several times. When the sample is completely cooled to a plate, add L. Wash with acid solution (2) with a reverse osmotic pressure, and then add the washing solution to a volumetric flask of 1. Add the acid solution (4.3) to the sample until the temperature reaches 400 °C. Follow the steps below: Preparation of blank solution in 7.2 || tt || press? .. Steps for preparing standard solutions
7.3 Drawing of standard curves
7.3.1 Prepare the standard solution with the volume specified in Table 1, add the solution (4.3) to five 19ml bottles, add hydrochloric acid solution (1.>Fire group to the scale, and mix with the standard solution.
Table 1. Preparation of standard solutions
Itchy cut with the total volume/ml
The concentration of the solution (gm:[.
The volume of the standard solution/mL
Package 1 (according to)
The nature of the hate is selected according to the spirit of the instrument or the control field GB/T 4500—2003
Economic performance of the release of blue (e
.3.2 Determination of the absorbance of the standard solution: Turn on the atomic absorption spectrometer and make the instrument fully stable. Adjust the wavelength to 13.81TL. Quickly select the test piece at the instrument end and aspirate the standard solution in numerical order. When the standard liquid is flushed and the sample is flushed, the liquid speed should be kept constant: After each measurement, a small amount of flushing must be aspirated. 7.3.3 Draw a standard curve: Take the standard drop rate (mL) as the coordinate, and take the corresponding 7.4 Determination of optical quality of test solution Www.bzxZ.net
According to the test conditions determined in 7.5.2, each test solution should be tested twice, and a blank test should be performed under the same conditions. If the absorbance of the test solution falls within the range of the standard line, then measure its absorbance again. To improve the accuracy of the analytical results, a standard addition can be used (see Table A). 8.1 The sample content is expressed as a mass number [?]. The zinc concentration of the test drop is directly calculated from the standard curve according to the formula: w-
Where:
(——the zinc concentration of the test drop read from the standard curve, in milligrams per milliliter (/ml). The density of zinc read from the standard curve, in grams per milliliter (RmT). The sample mass, in units of points (names):
The new adjustment coefficient
is calculated and the content is expressed as a percentage of 1.245. (1)
8.2 points 1 If the absorbance of the test microparticle remains within the linear integral of the calibration curve, the zinc content of the sample is expressed as mass fraction (%) and is calculated according to formula (2):
Zinc content in the test sample, unit is mg/ml mpn
Zinc content in the air solution, unit is homeostasis () Read the absorbance:
Absorbance of the white spectrum solution;
Absorbance of the standard solution closest to the test sample: The absorbance of the standard solution corresponding to the test sample, unit is gram per liter (mEml.): 2)
GB/T 4500—2003
Sample mass, unit is gram ()
"dilution coefficient
8.3 When the mass fraction of the test sample is greater than or equal to 0.:%, it shall be expressed as a fraction. If the mass fraction is less than 5.1%, it shall be expressed as mg/kg.
Net: 15g/
day.4 The test result is obtained by averaging the two determinations. When the content of the eluting agent is expressed as a fraction, it shall be accurately judged to two decimal places and expressed as %%/k, and rounded to the integer:
9 Test report
The test report shall include the following contents:
n) Number of this national standard:||tt ||b) Select the type of invertor (fire, stone furnace spectrophotometer); d) Test results;
) Any abnormalities found in the test; f) Test subjects and test period,
Appendix A
[Standard Appendix]
Standard addition method
and the accuracy of the test of samples with extremely high zinc content can be determined by the standard addition method according to GB/T4500-2903. The following requirements are required for the standard addition method: From the prepared test solution (7, 1), take samples of the same volume: three of which have zinc standards of known volume but different volumes (4.6). Dilute to the same volume: measure the absorbance of four aliquots separately, take the concentration of the droplet as the axis (absorbance is ) as the Y axis, when the extended straight line intersects with the x axis (absorbance is ), calculate the content in the test solution according to the concentration of the test solution at the intersection with the axis. 1 standard witness sent to the country. y
Add 1 part of the sample
to the standard solution: (mr.3 Figure A.1 Standard addition method example
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