SU659940A1 - Method of quantitative determining of calcium salts of aliphatic sulfoacids in sludge - Google Patents

Description

The present invention relates to methods for determining the corrosion inhibitor IHC-1, which is the calcium salt of aliphatic sulfoxyacid sour tar, formula (RS-CD oa, where R C) in a colorless hydrocarbon), based on the absorption of the cciMoro inhibitor. The method allows only large quantities to be determined. O, 1-1.3 g / l of inhibitor in an unpainted gas condensate medium 1. The disadvantage of the method is that by its own light absorption in it is possible to determine only large amounts of inhibitor, whereas at a concentration of 0.05-0.5 g / l of inhibitor and less inhibitory effect is not lost. Determining these quantities in an organic medium by a known method is not possible. Moreover, this method does not allow It is necessary to determine an inhibitor of the sulfosalt type, lactation type 1 in colored hydrocarbons, for example, in oil. The closest to the described invention by technical essence and the achieved result is the method of quantitative determination of aliphatic salts sulphonic acids, which consists in treating the sample being analyzed with a solution of rhodamine J, followed by extraction of the colored compound and photometry of the extract 2. The disadvantage of this method is the low sensitivity and limitation in the application of the method only for determining sulfosalts in aqueous solutions. This method may not be applicable to the determination of sulfosalts in organic solvents, including in oil. When determining sulfosalts in colored organic substances, in particular, in oil, the color of the solvent passing into the organic phase masks the coloring of the ionic associate formed. The aim of the invention is to increase the sensitivity of the method and the expansion of its scope.

 This goal is achieved by the described method of quantitative determination of calcium salts of sulfonic acid tar, which consists in processing the analyzed sample with a solution of pinacyanol, extracting the resulting compound with a mixture of toluene and acetone, taken in a volume ratio from 1: 0.5 to 1: 1.5, and processing the separated sulfuric acid extract, followed by phase separation and measurement of the optical density of the pre-neutralized aqueous phase.

Distinctive features of the method are the use of pinacyanol dye as an extractor and a mixture of toluene and acetone, taken in a volume ratio of from 5 to 1: 1.5, and the treatment of the extract after separation with sulfuric acid, followed by phase separation and measurement of the optical density previously neutralized aqueous phase.

The advantage of this method is that in the process of reextraction, the associate inhibitor with pinacyanol goes into one phase and is thereby separated from the oil, as a result of which interference such as paint-oil is eliminated. The method is distinguished by selectivity and sensitivity. The components contained in the formation waters do not affect the accuracy of inhibitor determination. A comparative study of the formation of associates of the inhibitor ICG-1 with 15 basic dyes (including rhodamines and azures) and their extraction showed that pinacyanol is the most sensitive reagent. Thus, pinacyanol makes it possible to determine 2-100 µg of the inhibitor ICG-1, and rhodamine J - 200-600 µg of aliphatic sulfosalts.

Example 1. Definition of ICS in formation waters.

5 MP of produced water are taken in a test tube with a ground stopper, 0.2 ml of a 0.05% solution of pinacyanol in ethanol and 5 ml of a mixture (1: 1) of toluene-acetone are added. Inject the mixture for 10–15 s., After separation, the organic phase is separated from the aqueous phase and the optical density of the extract is measured on a FEC-56 M using an optical filter 8 at 0.5 cm with respect to water. Based on the obtained values of optical density, the average content of inhibitor is found from the calibration graph.

Example 2. Determination of ICH-1 in oil.

In a separating funnel with a capacity of 50 ml, take 2 ml of oil, add 5 MP of distilled water, 0.2 ml of a 0.05% solution of pinacyanol in ethanol and 3 ml of a mixture (1: 1) of toluene-acetone. The mixture is injected for 15–20 sec., The phases are allowed to separate, the organic phase is quantitatively separated from the aqueous and transferred to another separatory funnel. Then again, 5 ml of the extractant is added to the aqueous phase, shaken, the organic phase is separated and transferred to a separatory funnel containing the first extract. To the separatory funnel containing the extract of the aspiracy is added .3 ml 0.5 n. 0, the mixture is shaken and, after separation of the phases, the aqueous phase is quantitatively transferred to a graduated tube. The stripping operation is repeated 2 more times, taking 2 ml 0.5 n each. 5 H2SO4 each time and added to the first reextract. At the end, 1 ml of acetone was added to the reextract and the volume of the mixture was adjusted to 10 ml with 10% NH / OH, shaken and the optical density of the reextracts on FEC-56M was measured at 6 0.5 cm.

Comparative data on the determination of the inhibitor ICG-1 in solutions of pure salts with rhodamine J and. pinacyanol presented in table 1.

Table

2 100.0 4.9 98.0

-2.0 -1.0 9.9 99.0 20 100.0 30 100.0 40 100.0 50 100.0

-6,7

+9.0

5.0

+ 1.0 -3.4 -4.5

Continuation of table 1