SU742775A1

SU742775A1 - Method of quantitative determining of lighnin sulfonates in worked-out liquids of sulfite-cellulose production

Info

Publication number: SU742775A1
Application number: SU782694199A
Authority: SU
Inventors: Юрий Германович Хабаров; Евгений Всеволодович Новожилов; Геннадий Федорович Прокшин; Иван Михайлович Боховкин
Original assignee: Архангельский Ордена Трудового Красного Знамени Лесотехнический Институт Им.В.В.Куйбышева
Priority date: 1978-11-01
Filing date: 1978-11-01
Publication date: 1980-06-25

Description

Изобретение относитс к аналитической химии, а именно, к способам количественного определени лигнина в отработанных жидкост х сульфитцеллюлозного производства.This invention relates to analytical chemistry, namely, to methods for quantifying lignin in waste liquids from sulphitecellulose production.

Известен способ определени лигнина путем хроматографировани анализируемой пробы на бумаге в системе растворителей бензола и воды, вз тых в объемном соотношении 1:1 1.A known method for determining lignin by chromatographing an analyzed sample on paper in a solvent system of benzene and water, taken in a volume ratio of 1: 1.

Недостатком способа вл етс низка точность определени .The disadvantage of the method is low accuracy of determination.

Наиболее близким к изобретению по технической сущности-и достйгаёмому результату вл етс способ количественного определени лигносульфонатов , заключающийс в обработке анализируемой пробы нитритом натри в присутствии серной кислоты с последук цим добавлением гидроокиси натри и фотометрированием полученного раствора (2 .The closest to the invention according to the technical essence and the achieved result is the method of quantitative determination of lignosulfonates, which consists in treating the sample being analyzed with sodium nitrite in the presence of sulfuric acid with the subsequent addition of sodium hydroxide and photometric measurement of the resulting solution (2.

Недостатком этого способа вл етс длительность определени 50- 60 мин.The disadvantage of this method is the determination time of 50- 60 minutes.

Цель изобретени - сокращение времени определени .The purpose of the invention is to reduce the determination time.

Это достигаетс известным способом количественного определени лигносульфонатов в отработанных жидкост х сульфит-целлюлозного производства путем обработки анализируемой пробы смесью сол нокислого раствора хлорного железа и перекиси водорода, вз тых в объемном соотношении 1:1-2, с последующимфотометрированием полученного раствора.This is achieved by a known method of quantitative determination of lignosulfonates in waste liquids of sulfite cellulose production by treating the sample being analyzed with a mixture of a hydrochloric acid solution of ferric chloride and hydrogen peroxide, taken in a volume ratio of 1: 1-2, followed by photometry of the resulting solution.

Пример. В мерной колбе на Example. In a volumetric flask on

10 25 мл смешивают 2,5-15 мг лигносульфонатов с 0,6 мл раствора хлорного железа и перекиси водорода и добавл ют дистиллированной воды до 25 мл. Оптическую плотность полученного створа измер ют через 5-10 мин на ФЭК-56 при длине волны 400 им в сантиметровых кюветах относительно дистиллированной воды.10 25 ml mix 2.5-15 mg lignosulfonates with 0.6 ml of ferric chloride solution and hydrogen peroxide and add distilled water to 25 ml. The optical density of the obtained target was measured after 5–10 min on FEC-56 at a wavelength of 400 nm in centimeter cuvettes relative to distilled water.

Зависимость оптической плотности Dependence of optical density

20 от концентрации лигнина носит линейный харал тер и выражаетс уравнением20 of the lignin concentration is linear haral ter and is expressed by the equation

С 0,625 Д где С - концентраци лигнина в фотометрируемом растворе, г/л; C 0.625 D where C is the concentration of lignin in the photometric solution, g / l;

25 Д - оптическа плотность раствора .25 D is the optical density of the solution.

Claims

For the analysis, a freshly prepared mixture of two solutions is used in a ratio of 1: 1. An acidic solution of FeC% is obtained by mixing in a volumetric flask per 100 ml of 30 ml of a saturated aqueous solution of ferric chloride and 30 ml of concentrated hydrochloric acid. The resulting solution was diluted to 100 ml with distilled water. Hydrogen peroxide solution obtained by diluting perhydrol in a ratio of 2: 5. In parallel, reference solutions of l nosulfonates are processed by the Pearl-Benson method. The dependence of the optical density on the concentration of lignosulfonates is linear and is expressed by the equation C 0.245 D, where C is the concentration of lignosulfonates in the photometric solution, g / l; D is the optical density of the solution. For the verification method according to the Pearl-Benson method and according to the proposed method, liquors for sulphite pulp cooking at the Arkhangelsk PPM were analyzed. The results of determination of lignosul phonates are given in the table. Sulphite liquor 70 minutes before the end of cooking 32,734, Sulphite liquor 50 minutes before concurrence, 338, cooking time Sulphite liquor 49,650, at the end of cooking The analysis is performed as follows. Solutions are prepared with known concentrations of lignosulfonates, a solution of ferric chloride and hydrogen peroxide is added to them and photometrized under identical conditions. According to the data obtained, a calibration graph is constructed and its equation is calculated. When analyzing the liquor to the known volume of the latter. Add a solution of ferric chloride and hydrogen peroxide, photometrize the resulting solution after 5-10 minutes and calculate the concentration of lignin using optical density. As can be seen from the table, the difference in determining the concentration by the two methods is insignificant (the relative error does not exceed 6%). Thus, the proposed method, which is faster (determination time 10-15 min) and simple, can be used to determine the concentration of lignosulfonates in the liquors during cooking. The invention of the method of quantitative determination of lignosulfonatoB in waste liquids of sulphite-pulp production by treating an analyzed sample with a chemical reagent followed by photometry of the resulting solution, characterized in that, in order to reduce the time of determination, a mixture of hydrochloric ferric chloride and hydrogen peroxide, taken in a volume ratio of 1: 1-2. Sources of information taken into account during the examination 1. Chromatography on paper. Ed. I.M. Hayes and K. Macek. Foreign literature. Number 1, 1962, p. 330332.

2. Lignins. Ed. K.V. Sarkanen, K.X. Ludwig. M., Lesna industry, 1975, p. 168 (prototype).