Determination of the Iodine Number of Raw Rubber

1929 ◽  
Vol 2 (3) ◽  
pp. 362-364
Author(s):  
Adolf Gorgas

Abstract In the course of an investigation dealing with the nature of the state of unsaturation of raw rubber, it became necessary to have available a precise and convenient method for determining the iodine number of raw rubber. Though iodine reacts only slowly with unsaturated compounds, chlorine and bromine form both addition and substitution products. In the substitution reactions, the hydrogen halide is evolved, and by addition of potassium iodate, e.g., in the method of MacIlhiney, it is possible to determine the hydroden halide formed and thus the quantity of halogen substituted. In all methods, however, where extensive substitution as well as addition take place, the results are variable and uncertain. Accordingly in the chemistry of fats where the iodine number is of the greatest importance, iodine halides have been used for determining the iodine number, for under certain conditions there is very little substitution. Thus Hübl, Waller and Wijs solutions contain iodine chloride and Hanus solution contains iodine bromine. The Hanus method has in fact to a great extent replaced all other methods For determining the iodine number of rubber, the Wijs method in the form in which it was modified by Kemp is probably used more than any other. In the Kemp method about 0.1 gram of rubber is swollen in 75 cc. of carbon disulfide, and is then allowed to react for 2 hours at 0° C. with 25 cc. of Wijs solution, i.e., 0.5 N iodine chloride in acetic acid.

1934 ◽  
Vol 7 (3) ◽  
pp. 587-590
Author(s):  
Rudolf Pummerer ◽  
Hermann Stark

Abstract In a communication of Pummerer and Mann in 1929 on the determination of the iodine number of rubber by means of iodine chloride in chloroform solution, Fisher and Gray were erroneously mentioned as the originators of the method, because of the fact that these authors were the first to publish the method in accessible form. The fact was overlooked that Fisher and Gray state in a footnote that the method was not their own but was that of A. R. Kemp of the Bell Telephone Laboratories. We are greatly indebted to Kemp for calling to our attention the error, which also appears in our XIVth Communication. The first paper of Kemp on the subject appeared a year later, and contains precise information. Kemp worked with a solution of iodine chloride in glacial acetic acid and a solution of rubber in carbon disulfide at 0° C., and as long ago as 1927 he showed that rubber obtained by extraction of crepe with petroleum ether (b. p. 35–60° C.), and precipitation with alcohol according to the method of Weber, Caspari and Feuchter, gave very satisfactory iodine numbers of 99.43–99.76 per cent of the theoretical value. At 15–20° C. disturbing effects of substitution occurred.


2019 ◽  
Vol 8 (5) ◽  
pp. 185-186
Author(s):  
Lokanatha Rai KM ◽  
Prakruthi Aiyappa K ◽  
Harshitha BL ◽  
Chaitra Shivani KS

1943 ◽  
Vol 16 (2) ◽  
pp. 280-285
Author(s):  
La Verne E. Cheyney ◽  
Everett J. Kelley

Abstract The quantitative determination of rubber unsaturation has concerned numerous investigators. The use of iodine chloride as a reagent for this purpose (the well-known Wijs method) has achieved favor in recent years. Under the proper experimental conditions, addition has been shown to be quantitative, and substitution reactions can be kept at a minimum. This procedure has likewise been rather extensively employed as a measure of the residual unsaturation of various rubber derivatives. This reagent does not, however, add quantitatively to all unsaturated compounds, regardless of structure. The presence of a negative substituent on one or more of the unsaturated carbon atoms inhibits the reaction; in fact, it may entirely prevent it, as in the cases of maleic or fumaric acids or dichloroethylene. In other compounds extensive substitution may occur along with addition, as in the case of the unsaturated terpenes. The unsaturation of the polymerized diolefins should be of considerable interest, especially in comparison with natural rubber. It should be of special interest to study the comparative reactions with iodine chloride, which has become practically a standard reagent for rubber. Kemp and Mueller mention that polychloroprene, to which they erroneously refer as polyvinyl chloride, adds iodine chloride to only 30 per cent of theory. This could be due to two causes—the negative influence of the chlorine attached to an unsaturated carbon, and/or possible cross-linkage between chains (cyclization). It is well established that polychloroprene is much less reactive chemically toward other reagents than is natural rubber. It is unfortunate that Kemp and Mueller did not state with more detail the history of the sample studied, as such a result might have shown some interesting correlation with the experiments reported in this paper.


1948 ◽  
Vol 21 (4) ◽  
pp. 830-834
Author(s):  
P. P. Kobeko ◽  
E. K. Moskvina

Abstract 1. It has been found that synthetic rubber does not precipitate from a solution of dichloromethane by the addition of Wijs reagent, whereas natural rubber does precipitate under the same conditions. The reverse relation occurs with carbon disulfide as solvent. 2. A method has been developed for the determination of the unsaturation of butadiene rubber in solution in dichloromethane by the use of Wijs reagent. 3. It has been demonstrated that, by the use of a solution of iodine chloride in carbon tetrachloride, the reaction with rubber is complicated by the hydrolysis of iodine chloride during titration, but not by the substitution of hydrogen by halogen nor by the hydrolysis of the rubber-halogen addition product. 4. The possibility of obtaining accurate values for unsaturation by a calculation of this hydrolysis is demonstrated. 5. Two methods have been developed for the determination of the unsaturation of natural and butadiene rubbers.


Author(s):  
G.P. Morie

AbstractA method for the rapid determination of acetic and higher aliphatic acids in cigarette smoke is described. Cigarette smoke is collected on a Cambridge filter, which is followed by a carbon disulfide scrubber. The total particulate matter (TPM) on the Cambridge filter is dissolved in carbon disulfide, and the acids are then extracted from this solution into an aqueous sodium borate solution (pH 8). An aliquot of this extract is injected onto a gas chromatographic column containing Chromosorb 101 column packing. The determination of acetic acid requires the smoke of 5 cigarettes and is completed in 15 min (10 min for extraction and 5 min for chromatographic separation). The coefficient of variation of the method is 3.8 %. The determination of acetic through hexanoic acid requires the smoke of 20 cigarettes and is completed in 20 min. The amounts of acetic acid delivered from cigarettes of various types were determined. Commercial cellulose acetate filters removed a slightly higher percentage of acetic acid than dry TPM from the smoke of a domestic cigarette


2018 ◽  
Vol 8 (4) ◽  
pp. 42-47
Author(s):  
Tien Nguyen Huu ◽  
Tram Le Thi Bao ◽  
Ngoc Nguyen Thi Nhu ◽  
Thang Phan Phuoc ◽  
Khan Nguyen Viet

Background: Curcumin is a major ingredient in turmeric (Curcuma longa L., Zingiberaceae), which has important activities such as anti-tumor, anti-inflammatory, antioxidant, anti-ischemia, protection of gastric mucosa etc,. Curcumin can be considered as a biological marker of turmeric and turmeric products. Objectives: Developing an HPLC method for quantification of curcumin in turmeric powder and turmeric - honey ball pills; applying this method for products on the market. Materials and methods: turmeric powder and turmeric - honey ball pills collected in Thua Thien Hue province. After optimization process, the method was validated and applied to evaluate the content of curcumin. Results: The chromatography analysis was performed with: Zorbaz Eclipse XDB-C18 (150 × 4.6 nm; 5 µm); Mobile phase: acetonitril: 2% acetic acid (45:55), Flow rate was kept constant at 1.0 ml/min; Detector PDA (420 nm). The method was validated for the HPLC system compatibility, specificity, linearity range, precision and accuracy; the recovery greater than 98%. Conclusion: The developed HPLC method can determine curcumin in turmeric powder and turmeric - honey ball pills. Key words: Curcumin, turmeric powder, turmeric-honey ball pills, quantitative determination, HPLC


2018 ◽  
Vol 69 (2) ◽  
pp. 297-299
Author(s):  
Adriana Nita ◽  
Delia Mirela Tit ◽  
Lucian Copolovici ◽  
Carmen Elena Melinte (Frunzulica) ◽  
Dana Maria Copolovici ◽  
...  

The aim of this study was to develop and validate a rapid, accurate, and exact method for the quantitative determination of famotidine in pharmaceutical products. The HPLC analyses were performed by using a mobile phase containing methanol:1% acetic acid solution=30:7 (v/v), at a flow rate of 0.4 mL/min.The total time of the method was 10 min, and the retention time of famotidine was 4.16 min. The detection was evaluated at l=267 nm. The method has been validated by using different validation parameters. The linear response of the detector for famotidine peak area was observed at concentrations ranging from 0.1 to 0.0001 mg mL-1 , resulting in a correlation coefficient of 0.99998. The values of the detection limit and of the quantification limit are 0.00048 mg mL-1 and 0.00148 mg mL-1, respectively. The method proposed allowed accurate (with a relative error of less than 2%) and precise (RSD values less than 2.0%) determination of famotidine content in pharmaceutical products and can be used for its rapid quantitative analysis.


Sign in / Sign up

Export Citation Format

Share Document