INTERSTATE STANDARD
Edition with Amendment No. 1, approved in June 1984 (IUS 9-84).
Decree State Committee standards of the Council of Ministers of the USSR dated July 30, 1975 No. 2001 date of introduction is set
1. EQUIPMENT, MATERIALS AND REAGENTS
1.1. To determine water-soluble acids and alkalis, the following are used: a pH meter of any type with a measurement error of not more than 0.1 pH, with glass silver chloride or calomel electrodes;
laboratory glassware and equipment according to GOST 25336-82:
test tubes of any type, with a capacity of not more than 10 cm 3;
glasses V-1-100XC, H-1-100XC;
conical flask KN-2-100XS, KN-2-250XS;
aviation gasoline grade B-70 or nefras-S 50/170 according to GOST 8505-80 or solvent gasoline for the rubber industry, tested for neutrality;
distilled water with pH 6 - 8, tested for neutrality;
rectified technical ethyl alcohol according to GOST 18300-87 or technical ethyl alcohol according to GOST 17299-78, diluted 1:1 with distilled water, tested for neutrality;
phenolphthalein (indicator), 1% solution in 60% ethanol;
methyl orange (indicator), 0.02% aqueous solution;
laboratory filter paper according to GOST 12026-76.
2. PREPARATION FOR THE TEST
2.1. Preparation of a sample of the tested oil product
2.1.1. Samples of the tested oil product are mixed by shaking for 5 minutes in a flask filled with no more than 3/4 of its capacity. Viscous and paraffinic oil products are preheated to 50 °C - 60 °C, and high-melting compositions - to a temperature 10 °C higher than the melting point.
2.1.2. When testing greases, the surface of the test sample is removed with a spatula and discarded. upper layer(3 - 5 mm), then in several places (at least three) samples are taken, approximately in equal quantities, not near the walls of the vessel. The selected samples are transferred to a porcelain cup and thoroughly mixed with a glass rod.
The total amount of the sample must be at least 50 g.
2.1.1, 2.1.2. (Changed edition, Rev. No. 1).
2.2. Distilled water, gasoline and alcohol should be checked for neutrality with methyl orange and phenolphthalein or with a pH meter.
3. CARRYING OUT THE TEST
3.1. When testing liquid petroleum products, 50 cm 3 of the tested oil product and 50 cm 3 of distilled water, heated to 50 ° C - 60 ° C, are placed in a separating funnel. Light oil products (gasoline, naphtha, etc.), as well as products in which water-soluble acids and alkalis can form as a result of hydrolysis, are not heated.
If the viscosity of the oil product is more than 75 cSt at 50 ° C, then it is pre-mixed at room temperature with 50 cm 3 of gasoline. Then add 50 cm 3 of distilled water, heated to 50 ° C - 60 ° C.
The contents of the separating funnel are slightly shaken for 5 minutes, avoiding the formation of an emulsion. After detachment, the lower aqueous layer is poured through a funnel with a paper filter into a conical flask.
3.2. When testing greases, paraffins, ceresins and wax formulations 50 g of a pre-melted sample, weighed with an error of not more than 0.01 g, is taken into a porcelain cup or conical flask. Then 50 cm 3 of distilled water are poured into it, the contents are heated until completely melted and mixed with a glass rod or by shaking.
After cooling to room temperature, the separated lower aqueous layer is carefully poured through a funnel with a paper filter into a conical flask. Hardened products (paraffins, ceresin, etc.) are pre-pierced with a glass rod.
3.3. When testing additives, 10 cm 3 of the tested additive and 40 cm 3 of gasoline are poured into the measuring cylinder. The resulting solution is transferred to a separating funnel, 50 cm 3 of distilled water heated to 50 - 60 ° C are added there. The contents of the separating funnel are shaken for 5 minutes. After settling, the separated lower aqueous layer is poured through a funnel with a paper filter into a conical flask.
3.1 - 3.3. (Revised edition, Rev. No. 1).
3.4. If an emulsion is formed when an oil product is mixed with water, then water-soluble acids and alkalis are extracted by treating the oil product with an alcohol solution (1: 1) heated to 50 ° C - 60 ° C (instead of distilled water) according to paragraphs. 3.1 or 3.3.
3.5. In the extracts obtained according to paragraphs. 3.1, 3.2, 3.3 and 3.4, determine the presence of water-soluble acids and alkalis by pH value or using indicators.
3.5.1. To determine the presence of water-soluble acids and alkalis by pH value, 35–50 cm 3 of extract are placed in a cup, the electrodes are immersed to a depth of 10–12 mm, and the pH value is measured in accordance with the requirements for operating a pH meter.
The absence and presence of water-soluble acids and alkalis in an aqueous or aqueous-alcoholic extract of oil products is determined according to the table.
3.5.2. To determine the presence of water-soluble acids and alkalis with the help of indicators, 1-10 cm 3 of the extract are placed in two test tubes.
Two drops of methyl orange solution are placed in one of the tubes and the color of the extract is compared with the color of the same volume of distilled water, to which two drops of methyl orange solution poured into the third tube are added. Coloring the hood in pink color indicates the presence of water-soluble acids in the tested oil product.
Three drops of phenolphthalein solution are added to the second tube.
A pink or red color of the solution indicates the presence of water-soluble alkalis.
An oil product is considered to be free of water-soluble alkalis or acids in the absence of pink or red coloration of the extract from phenolphthalein or methyl orange indicators.
3.5.3. In case of disagreement that arose during the assessment of the quality of petroleum products, a test for the presence of water-soluble acids and alkalis is carried out according to clause 3.5.1.
3.5.2, 3.5.3. (Revised edition, Rev. No. 1).
4. PROCESSING THE RESULTS
4.1. Convergence
Two determination results obtained by one performer on the same equipment and product sample are recognized as reliable (with a 95% confidence level) if the discrepancies between them do not exceed the values given in the table.
4.2. Reproducibility
Two test results obtained in different laboratories on the same product sample are recognized as reliable (with 95% confidence) if the discrepancies between them do not exceed the values given in the table.
Sec. 4. (Introduced additionally, Rev. No. 1).
GOST 6307-75
Group B09
INTERSTATE STANDARD
PETROLEUM PRODUCTS
Method for determining the presence of water-soluble acids and alkalis
Petroleum products. Method of test for water-soluble acids and alkalies
MKS 75.080
OKSTU 0209
Introduction date 1977-01-01
By the Decree of the State Committee of Standards of the Council of Ministers of the USSR dated July 30, 1975 N 2001, the date of introduction was set to 01.01.77
EDITION with Amendment No. 1, approved in June 1984 (IUS 9-84)
INSTEAD OF GOST 6307-60
The validity period was removed by the Decree of the USSR State Standard of November 28, 1991 N 1834
This standard applies to liquid petroleum products, additives, greases, paraffins, ceresins, wax compositions and establishes a method for determining the presence of water-soluble acids and alkalis (WCS) in them.
The essence of the method is to extract water-soluble acids and alkalis from petroleum products with water or an aqueous solution of alcohol and determine the pH value water extract pH meter or medium reaction using indicators.
The standard fully complies with ST SEV 3967-83.
1. EQUIPMENT, MATERIALS AND REAGENTS
1.1. To determine water-soluble acids and alkalis, the following are used: a pH meter of any type with a measurement error of not more than 0.1 pH, with glass silver chloride or calomel electrodes;
laboratory glassware and equipment according to GOST 25336-82:
test tubes of any type, with a capacity of not more than 10 cm3;
glasses B-1-100XC, H-1-100XC;
conical flask KH-2-100XC, KH-2-250XC;
funnel V-56-80XS, VD-1-250XS, VD-1-500XS;
cylinders 1-25, 1-50, 1-100 according to GOST 1770-74;
evaporating cup 5 according to GOST 9147-80;
putty knife;
pipettes of execution 4 of any type according to GOST 29227-91;
aviation gasoline grade B-70 or nefras-S 50/170 according to GOST 8505-80 or solvent gasoline for the rubber industry, tested for neutrality;
distilled water pH 6-8, tested for neutrality;
rectified technical ethyl alcohol according to GOST 18300-87 or technical ethyl alcohol according to GOST 17299-78, diluted 1:1 with distilled water, tested for neutrality;
phenolphthalein (indicator), 1% solution in 60% ethanol;
methyl orange (indicator), 0.02% aqueous solution;
laboratory filter paper according to GOST 12026-76.
(Changed edition, Rev. N 1).
2. PREPARATION FOR THE TEST
2.1. Preparation of a sample of the tested oil product
2.1.1. Samples of the tested oil product are mixed by shaking for 5 minutes in a flask filled with no more than 3/4 of its capacity. Viscous and paraffinic oil products are preheated to 50-60 °C, and high-melting compositions - to a temperature 10 °C higher than the melting point.
2.1.2. When testing greases, the upper layer (3-5 mm) is removed from the surface of the test sample with a spatula and discarded, then samples are taken in several places (at least three), approximately in equal quantities, not near the walls of the vessel. The selected samples are transferred to a porcelain cup and thoroughly mixed with a glass rod.
The total amount of the sample must be at least 50 g.
2.1.1, 2.1.2. (Changed edition, Rev. N 1).
2.2. Distilled water, gasoline and alcohol should be checked for neutrality with methyl orange and phenolphthalein or with a pH meter.
3. CARRYING OUT THE TEST
3.1. When testing liquid petroleum products, 50 cm3 of the tested oil product and 50 cm3 of distilled water heated to 50-60 °C are placed in a separating funnel. Light oil products (gasoline, naphtha, etc.), as well as products in which water-soluble acids and alkalis can form as a result of hydrolysis, are not heated.
If the viscosity of the oil product is more than 75 cSt at 50 ° C, then it is pre-mixed at room temperature with 50 ml of gasoline. Then add 50 ml of distilled water heated to 50-60 °C.
The contents of the separating funnel are slightly shaken for 5 minutes, avoiding the formation of an emulsion. After detachment, the lower aqueous layer is poured through a funnel with a paper filter into a conical flask.
3.2. When testing plastic lubricants, paraffins, ceresins and wax compositions, 50 g of a pre-melted sample, weighed with an error of not more than 0.01 g, is taken into a porcelain cup or conical flask. stick or shake.
After cooling to room temperature, the separated lower aqueous layer is carefully poured through a funnel with a paper filter into a conical flask. Hardened products (paraffins, ceresin, etc.) are pre-pierced with a glass rod.
3.3. When testing additives, 10 ml of the tested additive and 40 ml of gasoline are poured into the measuring cylinder. The resulting solution is transferred to a separating funnel, 50 ml of distilled water heated to 50-60 ° C is added there. The contents of the separating funnel are shaken for 5 minutes. After settling, the separated lower aqueous layer is poured through a funnel with a paper filter into a conical flask.
3.1-3.3. (Changed edition, Rev. N 1).
3.4. If an emulsion is formed when the oil product is mixed with water, then water-soluble acids and alkalis are extracted by treating the oil product with an alcohol solution (1: 1) heated to 50-60 ° C (instead of distilled water) according to paragraphs 3.1 or 3.3.
3.5. In the extracts obtained according to paragraphs 3.1, 3.2, 3.3 and 3.4, the presence of water-soluble acids and alkalis is determined by the pH value or using indicators.
3.5.1. To determine the presence of water-soluble acids and alkalis by pH value, 35–50 cm of extract is placed in a cup, the electrodes are immersed to a depth of 10–12 mm, and the pH value is measured in accordance with the requirements for operating a pH meter.
The absence and presence of water-soluble acids and alkalis in an aqueous or aqueous-alcoholic extract of oil products is determined according to the table.
3.5.2. To determine the presence of water-soluble acids and alkalis with the help of indicators, 1-10 cm of extract are placed in two test tubes.
Two drops of methyl orange solution are placed in one of the tubes and the color of the extract is compared with the color of the same volume of distilled water, to which two drops of methyl orange solution poured into the third tube are added. Pink staining of the extract indicates the presence of water-soluble acids in the tested oil product.
Three drops of phenolphthalein solution are added to the second tube.
A pink or red color of the solution indicates the presence of water-soluble alkalis.
The petroleum product is considered to be free of water-soluble alkalis or acids in the absence of pink or red coloration of the extract from phenolphthalein or methyl orange indicators.
3.5.3. In case of disagreement that arose during the assessment of the quality of petroleum products, a test for the presence of water-soluble acids and alkalis is carried out according to clause 3.5.1.
3.5.2, 3.5.3. (Changed edition, Rev. N 1).
4. PROCESSING THE RESULTS
4.1. Convergence
Two determination results obtained by one performer on the same equipment and product sample are recognized as reliable (with a 95% confidence level) if the discrepancies between them do not exceed the values given in the table.
4.2. Reproducibility
Two test results obtained in different laboratories on the same product sample are recognized as reliable (with 95% confidence) if the discrepancies between them do not exceed the values given in the table.
Characteristics of the water extract of the oil product | Convergence, pH | Reproducibility, pH |
||||
Sour | ||||||
subacid | ||||||
Absence of water-soluble acids and alkalis | ||||||
slightly alkaline | ||||||
alkaline | ||||||
Section 4. (Introduced additionally, Rev. N 1).
Electronic text of the document
prepared by Kodeks JSC and verified against:
official publication
Oil products. Analysis methods. Part 2:
Collection of national standards. -
M.: Standartinform, 2006
GOST 6307-75
IU NATIONAL STANDARD DART
PETROLEUM PRODUCTS
METHOD FOR DETERMINING THE PRESENCE OF WATEROR IMYH
ACID AND ALKALINE
IP TO STANDARDS PUBLISHING HOUSE
Moscow
INTERSTATE NY STANDARD
Decree of the Staten th Standards Committee of the Council of Ministers of the USSR from July 30, 1975 No. 2001 deadline set
with01. 01. 77
The validity period was lifted by the Decree of the State Standard dated 28. 11. 91 № 1834
This standard coverswith i'm on liquid petroleum product s, additives, greases, paraffins, ceresins, wax compositions and establishes a method for determining the presence of water-soluble acids and alkalis (B KSh) in them.
The essence of the method is to extract water-soluble acids and alkalis from petroleum products with water or an aqueous solution of alcohol and determine the pH value of the aqueous extract with a pH meter or the reaction of the medium using indicators.
The standard fully complies with ST SEV 3967-83.
1. EQUIPMENT, MATERIALS AND REAGENTS
1.1.To determine water-soluble acids and alkalis, the following is used: a pH meter of any type with a measurement error of not more than 0,1pH, with glass x lorsilveryans mi or calomel electrodes;
laboratory glassware and equipment according to GOST 25336-82:
test tubes of any type, with a capacity not exceeding 10cm 3;
glasses B-1-100 XC, H -1-100XC;
conical flask To N- 2-100XS, KN- 2-250XS;
thief onku V-56-80XS, VD-1-250XS, VD-1-500XS;
cylinders 1 - 25, 1- 50, 1-100according to GOST 1770-74;
evaporating cup5according to GOST 9147-80;
putty knife;
pipette execution4any type according to GOST 29227-91;
aviation gasoline ration grade B-70 or nefras-S 50/170 according to GOST 8505-80 or solvent gasoline for the rubber industry, tested for neutrality;
pH distilled water6 - 8, tested for neutrality;
rectified ethyl alcohol technical according to GOST18300-72or technical ethyl alcohol according to GOST 17299-78, diluted 1:1distilled water tested for neutrality;
phenolphthalein (indicator), 1%-new solution in 60% - ethyl alcohol;
methyl orange (indicator), 0, 02% aqueous solution;
laboratory filter paper according to GOST 12026-76.
(Revised edition, from m . № 1).
2. PREPARATION FOR THE TEST
2. 1. Pro preparationwould the tested oil duct
2.1.1.Samples of the tested oil product are mixed by shaking and during 5min in a flask filled with no more than 3/ 4its capacity. Viscous and waxy s e oil products are preheated to 50 - 60° C, and high-melting compositions - up to a temperature of 10°С above the melting point.
(Changed edition, Rev. No. 1).
2. 1. 2. When testing greases from the test surface t removed the sample with a spatula and discard the top layer ( 3 - 5mm), then in several places (at least three) samples are taken, approximately in equal quantities, not near the walls of the vessel. The selected samples are transferred to a porcelain cup and thoroughly mixed with a glass rod.
The total amount of the sample must be at least 50G.
(Changed edition, Rev. No. 1).
2. 2. Distilled water, gasoline and alcohol should be checked for neutrality by methyl orange and phenolphthalein or by N-me tra.
3. CARRYING OUT THE TEST
3. 1. When testing liquid petroleum products, place in a separating funnel 50 cm 3 test oil product and 50 cm 3 distilled water heated to 50 - 60°C. Light oil products (gasoline, naphtha, etc.), as well as products in which water-soluble acids and alkalis can form as a result of hydrolysis, are not heated.
If the viscosity of the oil product is more 75cSt at 50° C, then it is pre-mixed at room temperature with 50 cm 3 gasoline. Then add 50 cm 3 distilled water heated to 50 - 60°C.
The contents of the separating funnel are shaken gently for5min, avoiding the formation of an emulsion. After detachment, the lower aqueous layer is poured through a funnel with a paper filter into a conical flask.
(Changed edition, Rev. No. 1).
3. 2. When testing greases, paraffins, ceresins and wax compositions in porcelain tea w take a ku or a conical flask 50g pre-melted sample, weighed with an error of not more than 0, 01d. Then they pour 50 cm 3 distilled water, heat the contents until completely melted and mix with a glass rod or by shaking.
After cooling to room temperature, the separated lower aqueous layer is carefully poured through a funnel with a paper filter into a conical flask. Hardened products (paraffins, ceresin, etc.) are pre-pierced with a glass rod.
(Changed edition, Rev. No. 1).
3. 3. When testing additives, pour into the measuring cylinder 10 cm 3 test additive and 40 cm 3 gasoline. The resulting solution is transferred to a separating funnel, there is added 50 cm 3 heated to 50 - 60 °C distilled water. The contents of the separating funnel are shaken for 5min. After settling, the separated lower aqueous layer is poured through a funnel with a paper filter into a conical flask.
(Changed edition, Rev. No. 1).
3. 4. If When an oil product is mixed with water, an emulsion is formed, then water-soluble acids and alkalis are extracted by treating the oil product with an alcohol solution ( 1:1), heated to 50 - 60 ° С (instead of distilled water) according to paragraphs. or .
3. 5. In the extracts obtained according to paragraphs. , , and , determine the presence of water-soluble acids and alkalis by pH value or using indicators.
3. 5. 1. To determine the presence of water-soluble acids and alkalis by pH value, place in a glass 35 - 50 cm 3 hoods, immerse the electrodes to a depth 10 - 12mm and measure the pH value in accordance with the requirements for the operation pH-me tra.
The absence and presence of water-soluble acids and alkalis in an aqueous or aqueous-alcoholic extract of oil products is determined according to the table.
3. 5. 2. To determine the presence of water-soluble acids and alkalis using b 10 indicators are placed in two test tubes 1 - 10 cm 3 hoods.
Place two drops of methyl chloride solution into one of the test tubes.about orange and compare the color of the extract with the color of the same volume of distilled water, to which two drops of methyl orange solution are added, poured into the third test tube. Pink staining of the extract indicates the presence of water-soluble acids in the tested oil product.
Three drops of phenolphthalein solution are added to the second tube.
A pink or red color of the solution indicates the presence of water-soluble alkalis.
An oil product is considered to be free of water-soluble alkalis or acids in the absence of pink or red coloration of the extract from phenolphthalein or methyl orange indicators.
(Change e revised edition, Rev. No. 1).
3. 5. 3. In case of disagreement that arose during the assessment of the quality of petroleum products, a test for the presence of water-soluble acids and alkalis is carried out according to p.
(Change e revised edition, Rev. No. 1).
4. PROCESSING THE RESULTS
4. 1. sho dim awn
Two determination results obtained by one performer on the same equipment and product sample are recognized as then ver n s mi (from 95%- confidence level) if the discrepancies between them do not exceed the values given in the table.
4. 2. Reproducibility
Two test results obtained in different laboratories on the same sample of the product are recognized as reliable (with95% confidence level), if the discrepancies between them do not exceed the values given in the table.
|
Characteristics of the water extract of the oil product |
pH |
Convergence, pH |
Reproducibility, pH |
|
Sour |
Up to 4 , 0 |
0, 2 |
1, 9 |
|
subacid |
St. 4 .0 to 6.0 |
0, 3 |
1, 9 |
|
Absence in we are creating x acids and alkalis |
»6 , 0»8, 0 |
0, 3 |
1, 9 |
|
slightly alkaline |
"eight , 0»10, 0 |
1, 9 |
|
|
alkaline |
"ten , 0 |
0, 3 |
1, 9 |
Sec. . (Introduced additionally, Rev. No. 1).
INTERSTATE STANDARD
Edition with Amendment No. 1, approved in June 1984 (IUS 9-84).
By the Decree of the State Committee of Standards of the Council of Ministers of the USSR dated July 30, 1975 No. 2001, the introduction date was set
The validity period was removed by the Decree of the State Standard of the USSR of November 28, 1991 No. 1834
This standard applies to liquid petroleum products, additives, greases, paraffins, ceresins, wax compositions and establishes a method for determining the presence of water-soluble acids and alkalis (WCS) in them.
The essence of the method is to extract water-soluble acids and alkalis from petroleum products with water or an aqueous solution of alcohol and determine the pH value of the aqueous extract with a pH meter or the reaction of the medium using indicators.
The standard fully complies with ST SEV 3967-83.
1. EQUIPMENT, MATERIALS AND REAGENTS
1.1. To determine water-soluble acids and alkalis, the following are used: a pH meter of any type with a measurement error of not more than 0.1 pH, with glass silver chloride or calomel electrodes;
laboratory glassware and equipment according to GOST 25336-82:
test tubes of any type, with a capacity of not more than 10 cm 3;
glasses V-1-100XC, H-1-100XC;
conical flask KN-2-100XS, KN-2-250XS;
funnel V-56-80XS, VD-1-250XS, VD-1-500XS;
cylinders 1-25, 1-50, 1-100 according to GOST 1770-74;
evaporating cup 5 according to GOST 9147-80;
pipettes of execution 4 of any type according to GOST 29227-91;
aviation gasoline grade B-70 or nefras-S 50/170 according to GOST 8505-80 or solvent gasoline for the rubber industry, tested for neutrality;
distilled water with pH 6 - 8, tested for neutrality;
rectified technical ethyl alcohol according to GOST 18300-87 or technical ethyl alcohol according to GOST 17299-78, diluted 1:1 with distilled water, tested for neutrality;
phenolphthalein (indicator), 1% solution in 60% ethanol;
methyl orange (indicator), 0.02% aqueous solution;
laboratory filter paper according to GOST 12026-76.
(Revised edition, Rev. No. 1).
2. PREPARATION FOR THE TEST
2.1. Preparation of a sample of the tested oil product
2.1.1. Samples of the tested oil product are mixed by shaking for 5 minutes in a flask filled with no more than 3/4 of its capacity. Viscous and paraffinic oil products are preheated to 50 °C - 60 °C, and high-melting compositions - to a temperature 10 °C higher than the melting point.
2.1.2. When testing greases, the upper layer (3–5 mm) is removed from the surface of the test sample with a spatula and discarded, then samples are taken in several places (at least three), approximately in equal quantities, not near the walls of the vessel. The selected samples are transferred to a porcelain cup and thoroughly mixed with a glass rod.
The total amount of the sample must be at least 50 g.
2.1.1, 2.1.2. (Revised edition, Rev. No. 1).
2.2. Distilled water, gasoline and alcohol should be checked for neutrality with methyl orange and phenolphthalein or with a pH meter.
3. CARRYING OUT THE TEST
3.1. When testing liquid petroleum products, 50 cm 3 of the tested oil product and 50 cm 3 of distilled water, heated to 50 ° C - 60 ° C, are placed in a separating funnel. Light oil products (gasoline, naphtha, etc.), as well as products in which water-soluble acids and alkalis can form as a result of hydrolysis, are not heated.
If the viscosity of the oil product is more than 75 cSt at 50 ° C, then it is pre-mixed at room temperature with 50 cm 3 of gasoline. Then add 50 cm 3 of distilled water, heated to 50 ° C - 60 ° C.
The contents of the separating funnel are slightly shaken for 5 minutes, avoiding the formation of an emulsion. After detachment, the lower aqueous layer is poured through a funnel with a paper filter into a conical flask.
3.2. When testing greases, paraffins, ceresins and wax compositions, 50 g of a pre-melted sample, weighed with an error of not more than 0.01 g, is taken into a porcelain cup or conical flask. Then 50 cm 3 of distilled water is poured into it, the contents are heated until completely melted and mixed glass rod or shaking.
After cooling to room temperature, the separated lower aqueous layer is carefully poured through a funnel with a paper filter into a conical flask. Hardened products (paraffins, ceresin, etc.) are pre-pierced with a glass rod.
3.3. When testing additives, 10 cm 3 of the tested additive and 40 cm 3 of gasoline are poured into the measuring cylinder. The resulting solution is transferred to a separating funnel, 50 cm 3 of distilled water heated to 50 - 60 ° C are added there. The contents of the separating funnel are shaken for 5 minutes. After settling, the separated lower aqueous layer is poured through a funnel with a paper filter into a conical flask.
3.1 - 3.3. (Revised edition, Rev. No. 1).
3.4. If an emulsion is formed when an oil product is mixed with water, then water-soluble acids and alkalis are extracted by treating the oil product with an alcohol solution (1: 1) heated to 50 ° C - 60 ° C (instead of distilled water) according to paragraphs. 3.1 or 3.3.
3.5. In the extracts obtained according to paragraphs. 3.1, 3.2, 3.3 and 3.4, determine the presence of water-soluble acids and alkalis by pH value or using indicators.
3.5.1. To determine the presence of water-soluble acids and alkalis by pH value, 35–50 cm 3 of extract are placed in a cup, the electrodes are immersed to a depth of 10–12 mm, and the pH value is measured in accordance with the requirements for operating a pH meter.
The absence and presence of water-soluble acids and alkalis in an aqueous or aqueous-alcoholic extract of oil products is determined according to the table.
3.5.2. To determine the presence of water-soluble acids and alkalis with the help of indicators, 1-10 cm 3 of the extract are placed in two test tubes.
Two drops of methyl orange solution are placed in one of the tubes and the color of the extract is compared with the color of the same volume of distilled water, to which two drops of methyl orange solution poured into the third tube are added. Pink staining of the extract indicates the presence of water-soluble acids in the tested oil product.
Three drops of phenolphthalein solution are added to the second tube.
A pink or red color of the solution indicates the presence of water-soluble alkalis.
The petroleum product is considered to be free of water-soluble alkalis or acids in the absence of pink or red coloration of the extract from phenolphthalein or methyl orange indicators.
3.5.3. In case of disagreement that arose during the assessment of the quality of petroleum products, a test for the presence of water-soluble acids and alkalis is carried out according to clause 3.5.1.
3.5.2, 3.5.3. (Revised edition, Rev. No. 1).
4. PROCESSING THE RESULTS
4.1. Convergence
Two determination results obtained by one performer on the same equipment and product sample are recognized as reliable (with a 95% confidence level) if the discrepancies between them do not exceed the values given in the table.
4.2. Reproducibility
Two test results obtained in different laboratories on the same product sample are recognized as reliable (with 95% confidence) if the discrepancies between them do not exceed the values given in the table.
Sec. 4. (Introduced additionally, Amendment No. 1).
page 1
page 2
page 3
INTERSTATE STANDARD
Edition with Amendment No. 1, approved in June 1984 (IUS 9-84).
By the Decree of the State Committee of Standards of the Council of Ministers of the USSR dated July 30, 1975 No. 2001, the introduction date was set
The validity period was removed by the Decree of the State Standard of the USSR of November 28, 1991 No. 1834
This standard applies to liquid petroleum products, additives, greases, paraffins, ceresins, wax compositions and establishes a method for determining the presence of water-soluble acids and alkalis (WCS) in them.
The essence of the method is to extract water-soluble acids and alkalis from petroleum products with water or an aqueous solution of alcohol and determine the pH value of the aqueous extract with a pH meter or the reaction of the medium using indicators.
The standard fully complies with ST SEV 3967-83.
1. EQUIPMENT, MATERIALS AND REAGENTS
1.1. To determine water-soluble acids and alkalis, the following are used: a pH meter of any type with a measurement error of not more than 0.1 pH, with glass silver chloride or calomel electrodes;
laboratory glassware and equipment according to GOST 25336-82:
test tubes of any type, with a capacity of not more than 10 cm 3;
glasses V-1-100XC, H-1-100XC;
conical flask KN-2-100XS, KN-2-250XS;
funnel V-56-80XS, VD-1-250XS, VD-1-500XS;
pipettes of execution 4 of any type according to GOST 29227-91;
aviation gasoline grade B-70 or nefras-S 50/170 according to GOST 8505-80 or solvent gasoline for the rubber industry, tested for neutrality;
distilled water with pH 6 - 8, tested for neutrality;
rectified technical ethyl alcohol according to GOST 18300-87 or technical ethyl alcohol according to GOST 17299-78, diluted 1:1 with distilled water, tested for neutrality;
phenolphthalein (indicator), 1% solution in 60% ethanol;
methyl orange (indicator), 0.02% aqueous solution;
laboratory filter paper according to GOST 12026-76.
(Revised edition, Rev. No. 1).
2. PREPARATION FOR THE TEST
2.1. Preparation of a sample of the tested oil product
2.1.1. Samples of the tested oil product are mixed by shaking for 5 minutes in a flask filled with no more than 3/4 of its capacity. Viscous and paraffinic oil products are preheated to 50 °C - 60 °C, and high-melting compositions - to a temperature 10 °C higher than the melting point.
2.1.2. When testing greases, the upper layer (3–5 mm) is removed from the surface of the test sample with a spatula and discarded, then samples are taken in several places (at least three), approximately in equal quantities, not near the walls of the vessel. The selected samples are transferred to a porcelain cup and thoroughly mixed with a glass rod.
The total amount of the sample must be at least 50 g.
2.1.1, 2.1.2. (Revised edition, Rev. No. 1).
2.2. Distilled water, gasoline and alcohol should be checked for neutrality with methyl orange and phenolphthalein or with a pH meter.
3. CARRYING OUT THE TEST
3.1. When testing liquid petroleum products, 50 cm 3 of the tested oil product and 50 cm 3 of distilled water, heated to 50 ° C - 60 ° C, are placed in a separating funnel. Light oil products (gasoline, naphtha, etc.), as well as products in which water-soluble acids and alkalis can form as a result of hydrolysis, are not heated.
If the viscosity of the oil product is more than 75 cSt at 50 ° C, then it is pre-mixed at room temperature with 50 cm 3 of gasoline. Then add 50 cm 3 of distilled water, heated to 50 ° C - 60 ° C.
The contents of the separating funnel are slightly shaken for 5 minutes, avoiding the formation of an emulsion. After detachment, the lower aqueous layer is poured through a funnel with a paper filter into a conical flask.
3.2. When testing greases, paraffins, ceresins and wax compositions, 50 g of a pre-melted sample, weighed with an error of not more than 0.01 g, is taken into a porcelain cup or conical flask. Then 50 cm 3 of distilled water is poured into it, the contents are heated until completely melted and mixed glass rod or shaking.
After cooling to room temperature, the separated lower aqueous layer is carefully poured through a funnel with a paper filter into a conical flask. Hardened products (paraffins, ceresin, etc.) are pre-pierced with a glass rod.
3.3. When testing additives, 10 cm 3 of the tested additive and 40 cm 3 of gasoline are poured into the measuring cylinder. The resulting solution is transferred to a separating funnel, 50 cm 3 of distilled water heated to 50 - 60 ° C are added there. The contents of the separating funnel are shaken for 5 minutes. After settling, the separated lower aqueous layer is poured through a funnel with a paper filter into a conical flask.
3.1 - 3.3. (Revised edition, Rev. No. 1).
3.4. If an emulsion is formed when an oil product is mixed with water, then water-soluble acids and alkalis are extracted by treating the oil product with an alcohol solution (1: 1) heated to 50 ° C - 60 ° C (instead of distilled water) according to paragraphs. 3.1 or 3.3.
3.5. In the extracts obtained according to paragraphs. 3.1, 3.2, 3.3 and 3.4, determine the presence of water-soluble acids and alkalis by pH value or using indicators.
3.5.1. To determine the presence of water-soluble acids and alkalis by pH value, 35–50 cm 3 of extract are placed in a cup, the electrodes are immersed to a depth of 10–12 mm, and the pH value is measured in accordance with the requirements for operating a pH meter.
The absence and presence of water-soluble acids and alkalis in an aqueous or aqueous-alcoholic extract of oil products is determined according to the table.
3.5.2. To determine the presence of water-soluble acids and alkalis with the help of indicators, 1-10 cm 3 of the extract are placed in two test tubes.
Two drops of methyl orange solution are placed in one of the tubes and the color of the extract is compared with the color of the same volume of distilled water, to which two drops of methyl orange solution poured into the third tube are added. Pink staining of the extract indicates the presence of water-soluble acids in the tested oil product.
Three drops of phenolphthalein solution are added to the second tube.
A pink or red color of the solution indicates the presence of water-soluble alkalis.
An oil product is considered to be free of water-soluble alkalis or acids in the absence of pink or red coloration of the extract from phenolphthalein or methyl orange indicators.
3.5.3. In case of disagreement that arose during the assessment of the quality of petroleum products, a test for the presence of water-soluble acids and alkalis is carried out according to clause 3.5.1.
3.5.2, 3.5.3. (Revised edition, Rev. No. 1).
4. PROCESSING THE RESULTS
4.1. Convergence
Two determination results obtained by one performer on the same equipment and product sample are recognized as reliable (with a 95% confidence level) if the discrepancies between them do not exceed the values given in the table.
4.2. Reproducibility
Two test results obtained in different laboratories on the same product sample are recognized as reliable (with 95% confidence) if the discrepancies between them do not exceed the values given in the table.
Sec. 4. (Introduced additionally, Amendment No. 1).
