GB/T 14836-1993 Qualitative analysis of ash content of vulcanized rubber
Some standard content:
National Standard of the People's Republic of China
Qualitative analysis of vulcanized rubber ash
. Vulcanized rubber-Qualitative anaiysis of ash Subject content and scope of application
This standard specifies the qualitative method of elements in vulcanized rubber ash. GB/T 14836-93
This standard applies to the identification of the main elements in inorganic fillers added to vulcanized rubber: calcium, magnesium, zinc, lead, iron, aluminum, antimony, barium, titanium and silicon. 2 Reference standards
GB/T4498 Determination of ash content of vulcanized rubber
3 Principle
The rubber sample is ashed to remove organic matter to obtain the corresponding oxides, salts and other substances, and then these substances are separated by the difference in solubility in acid, and identified by classical chemical qualitative methods. When using this method, attention should be paid to safety and necessary protective measures should be taken. 4 Reagents and Materials
During the analysis, only analytical reagents and distilled water, or water of equivalent purity, can be used. 4. 1 Hydrochloric acid (GB 622).
4.2 Potassium nitrite (HG/T3-919).
4.3 Anhydrous sodium carbonate (GB639).
4.4 Anhydrous potassium carbonate (GB1397).
4.5 Ammonia water (GB631).
4.6 Hydrogen peroxide.
Acetic acid solution: c(CH.COOH)=1mol/L. 4.7
Ammonia water solution: 1+1(V+V).
4.9 Saturated ammonium oxalate solution.
Para-nitrophenylazoresorcinol (magnesium reagent 1) solution: 0=0.01g/L. Sodium hydroxide solution: p=250g/L.
Copper sulfate (CuSO.·5H,O) solution: p=1g/L. Ammonium mercuric thiocyanate solution: p=20g/L.
Potassium ferrocyanide solution: 0=100g/L.
1,2-dihydroxyanaldol-3-sulfonate sodium (sodium alizarin sulfonate) solution: β0.5g/L. Potassium dichromate solution: 0=100g/L.
Potassium chromate solution: p20g/L.
Nitric acid solution: c(HNO,)= 1 mol/L.
Approved by the State Administration of Technical Supervision on December 30, 1993, and implemented on October 1, 1994
GB/T 14836—93
4.19 Rhodamine B (C2H3tC1O,N) solution: p=0.1g/L4.20 Potassium fluoride solution: p=100g/L.
4.21 Sodium rhodamine (CONa2) solution: 0.5g/L. Note: Sodium rhodamine aqueous solution decomposes within a few hours, and should be prepared temporarily according to the amount used. 4.22 Hydrochloric acid solution: c(HCI)=0.1 mol/L. 4.23 Ammonium molybdate solution: Dissolve 6g ammonium molybdate in 15mL water, and add 5mL ammonia water. Heat the solution slightly, then add 24mL concentrated nitric acid and 57mL distilled water, stir and mix, and let stand overnight before use. 4.24 Benzidine acetic acid solution: p = 1g / L. Take 0.1g of benzidine, dissolve it in 10mL of glacial acetic acid, dilute it to 100mL with water, and then filter it.
4.25 Saturated sodium acetate solution.
Comparison solution of test solution A: Dissolve 0.59g Ca(NO,)2· 4H,O, 1. 06g Mg(NOs)2·6H,O, 0. 455g4.26
Zn(NO,)2· 6H2O and 1. 6g Pb(NO,),# in water and dilute to 1 000mL. 4.27 Comparison solution of test solution B: Dissolve 0.715g Fe(NO,)：~9H,O, 1.4g Al(NOs):·9H,O in water and dissolve 0.19g SbCls in concentrated hydrochloric acid, mix and dilute to 1000mL with water. 4.28 Comparison solution of test solution C: Dissolve 0.19g Ba(NO3)2, 0.40g TiCl. and 0.28g NaSiO·5H,0 in water and dilute to 1000mL.
'5 Apparatus
5.1 Test tube.
5.2 Black drop plate.
5.3 White drop plate.
5.4 Porcelain.
5.5 Platinum crucible.
5.6 Centrifuge.
6 Analysis steps
6.1 Preparation of test solution
Weigh 2-3g of shredded sample, make the sample into ash according to GB/T4498 (if the ash is blue-green, diamond may be present), add 5mL acetic acid solution, heat to boiling, let it stand, take the upper clear liquid (test solution A) and identify: calcium ion, magnesium ion, zinc ion, lead ion. The residue was washed twice with acetic acid solution, 5 mL of hydrochloric acid was added, heated to dissolve, and allowed to stand. The supernatant (test solution B) was taken for identification: iron ions, aluminum ions, and antimony ions. The residue was washed twice with hydrochloric acid, and then washed with distilled water until neutral. After drying, it was transferred to a platinum crucible, and 4 g of anhydrous sodium carbonate and anhydrous potassium carbonate mixture were added. The mixture was stirred evenly, and the mixture was melted in a high-temperature furnace at 800 ° C until transparent. After cooling, 5 mL of hydrochloric acid was added to dissolve (test solution C) for identification: barium ions, titanium ions, and silicate ions, as shown in the table below. Ash
Add s mL acetic acid solution
Heat to paint
-, solution, identification of Ca 2+, Mg 2+, Zn 2+, Pb 2+ (test solution A) Residue
m5 ml, hydrochloric acid
Heat to dissolve
Solution: identification of Fe 3+, AI 3+, Sb =+ (test solution B) Residue
Naz2C, K 2C0 melt
Free solution: identification of Ba 2+, T 4+, SiO 2+ (test solution C) After cooling, sodium hydrochloric acid
6.2 Identification
GB/T14836-93
When identifying each ion, a blank test and a comparison test of adding the corresponding comparison solution to the test solution must be performed. 6.2.1 Identification of Calcium IonsbZxz.net
Take 1mL of test solution A in a test tube and add 3-5 drops of ammonia water to adjust to weak alkalinity. If precipitation occurs, centrifuge, take the clear solution, add 0.5ml of ammonium oxalate solution, heat, and if white precipitation occurs, it indicates the presence of calcium ions. 6.2.2 Identification of Magnesium Ions
Take 2-3 drops of test solution A, place on a white drop plate, add 3-5 drops of sodium hydroxide solution to adjust the solution to strong alkalinity. Then add 1-2 drops of magnesium reagent 1 solution and stir with a glass rod. If a sky blue precipitate is generated, it indicates the presence of magnesium ions. 6.2.3 Identification of Zinc Ions
Take 2-3 drops of test solution A, place on a white drop plate, add 1 drop of copper sulfate solution and 1 drop of ammonium mercuric thiocyanate solution, stir and rub the drop plate with a glass rod, and slowly produce a purple precipitate, indicating the presence of zinc ions. 6.2.4 Identification of lead ions
Take 1-2 drops of test solution A (if the ash sample is prepared according to the halogen-containing rubber, take test solution B), place it on a white drip plate, add 1-2 drops of potassium chromate or potassium dichromate solution, if a yellow precipitate is produced, it indicates the presence of lead ions. Note: This precipitate is easily soluble in strong alkali, difficult to dissolve in nitric acid solution, and insoluble in ammonium hydroxide and acetic acid. 6.2.5 Identification of iron ions
Take 2-3 drops of test solution B, place it on a white drip plate, add 1-2 drops of potassium ferrocyanide solution, if a dark blue precipitate is produced, it indicates the presence of trivalent iron ions.
6.2.6 Identification of aluminum ions
Drop 1 drop of potassium ferrocyanide solution on a small strip of filter paper, dry it, add 1 drop of test solution B, put the filter paper on the mouth of a concentrated ammonia bottle and smoke it for 1-2 minutes, then add 1 drop of sodium alizarin sulfonate solution on the wet spot on the filter paper. Then use ammonia to fumigate and carefully dry the filter paper strip. If a rose-red ring appears on the filter paper, it indicates the presence of aluminum ions.
6.2.7 Identification of antimony ions
Take 2 to 3 drops of test solution B and place them on a white drop plate. Add a small particle of solid potassium nitrite. After the intense action stops, add 1 to 2 drops of rhodamine B solution. If the solution turns purple, it indicates the presence of antimony ions. 6.2.8 Identification of ions
Adjust the pH of test solution C to 6 to 8 with ammonia water, take 1 drop and place it on the filter paper, add 1 drop of sodium rose bengalate solution, if reddish-brown spots appear, then moisten the spots with hydrochloric acid solution and they turn bright red, indicating the presence of barium ions. 6.2.9 Identification of titanium ions
Take 2 mL of test solution C and place it in a test tube. Add about 1 mL of hydrogen peroxide drop by drop while shaking. If the solution turns golden yellow, add potassium fluoride solution. If the yellow color disappears, it indicates the presence of titanium ions. 6.2.10 Identification of silicate ions
Put 2 drops of test solution C in a test tube, add 2 drops of ammonium molybdate solution, heat slightly, and add 1 drop of benzidine acetic acid solution and 3 to 8 drops of sodium acetate solution after cooling. If it turns blue, it indicates the presence of silicate ions. Additional remarks:
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Beijing Rubber Industry Research and Design Institute of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Rubber Industry Products Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Yin Renshou and Sun Yuzhen. 823
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