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IS 1448-59 (1991): Methods of test for petroleum and itsproducts, Part 59: Determination of mineral oil content ingreases [PCD 1: Methods of Measurement and Test forPetroleum, Petroleum Products and Lubricants]

IS1448[ P: 59]:1991

Indian Standard

METHODS OF TEST FOR PETROLEUM AND ITS PRODUCTS

[P:59]

DETERMINATION OF MINERAL OIL CONTENT IN GREASES

f Second Revision /

UDC 621-892-2 : 543 : 547.913

@ BIS 1991

BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

December 1991 Price Group 2

Methods of Test for Petroleum, Petroleum Products and Lubricants Sectional Committee, PCD 1

FOREWORD

This Indian standard [ P : 59 ] ( Second Revision ) was adopted by the Bureau of Indian Standards, after the draft finalized by the Methods of Test for Petroleum, Petroleum Products and Lubricants Sectional Committee had been approved by the Petroleum, Coal and Related Products Division Council.

In reporting the results of a test or analysis made in accordance with this standard, if the final value, observed or calculated, is to be rounded off, it shall be done in accordance with IS 2 : 1960 ‘Rules for rounding off numerical values ( revised )‘.

Indian Standard

IS 1448 .[ P : 59 ] ‘r 1991 ’

,

METHODSOFTESTFOR *" . PETROLEUMANDITSPRdDUCTS

[P:59] .,- .

DETERMINATION OF MINERAL OIL CQNTENT IN GREASES

( Second Revision)

1 SCOPE

1.1 The methods prescribed are intended for the determination of mineral oil content in con- ventional greases which consists essentially of mineral oil and soap.

Method A shall be followed for all greases except those containing residuum, asphaltic oils, asphalt, tars, etc, as these ingredients usually cause stub- born emulsions if a vigorous agitation is applied at the start. Method B will be applicable in the latter cases.

1.2 A supplementary method is provided in the Annex A. This method is intended primarily for application to greases containing thickeners which are essentially insoluble in n-hexane and to greases which may not be analysed by conven- tional methods because of the presence of such constituents as non-petroleum fluids or non-soap type thickeners or both. In some cases, these constituents may react with strong acid or alka- line solutions.

1.3 This standard may involve hazardous materi- als, operations, and equipment. This standard does not purport lo address all of the safety problems associated with its use. It is the res- ponsibility of whoever uses this standard to con- sult and establish appropriate safety and health practices and determine the applicability of regu- latory limitations prior to use ( see Annex B ).

2 REFERENCES

2.1 The following Indian Standards are necessary adjuncts to this standard:

IS “No. Title

323 : 1959 Rectified spirit

3470 : 1966 Hexane, food-grade

3 METHOD-A

3.1 Outline of the Method

The sample is dissolved in petroleum hydrocarbon solvent and heated under reflux with dilute hydrochloric acid under prescribed conditions.

The petroleum hydrocarbon solvent layer is washed and the solvent distilled off. The mineral oil is obtained as the residue after distillation.

3.2 Reagents

3.2.1 n-Hexane

See IS 3470 : 1976.

3.2.2 Dilute Hydrochloric acid

Approximately 10.0 percent by mass of hydro- chloric acid.

3.2.3 Phenolphthalein Indicator

Dissolve 1.0 g of phenolphthalein in 50 ml of water and neutralising with NaOH or KOH.

3.2.4 Alcoholic Potassium Hydroxide Solution

Approximately 10 percent ( m/v ).

3.2.5 Ethyl Alcohol

50 percent by volume in water, neutralising exactly with NaOH or KOH phenolphthalein as an indicator.

3.3 Procedure

3.3.1 Weigh into a 500 ml conical flask a suitable quantity ( 8 to 30 g ) of the material, accurately to the nearest 0.1 g depending on the percentage of mineral oil present in the grease. Add 50 ml of n-hexane and disperse the grease in the solvent. Add 50 ml of dilute hydrochloric acid ( 10 per- cent ) and several boiling chips.

3.3.2 Digest by boiling under. reflux condenser until all soap has been decomposed and the upper solvent layer is clear. Generally three hours time is sufficient. However, sometimes more vigorous boiling, use of stronger hydrochloric acid or additional quantity of solvent will be found help- ful for greases difficult to decompose.

3.3.3 Allow the contents of the flask to cool to

room temperature. Remove the condenser and transfer the contents of the flask to a separating funnel, using n-hexane and distilled water as washing liquids ( in the presence of fillers, filter

the undissolved matter through a Gooch crucible provided with a suitable mat, wash with h-hexane and then transfer the combined filtrate and wash- ing to a separating funnel ).

3.3.4 Allow the solution in the separating funnel to clear and draw the aqueous layer (A) into another separating funnel. Wash the n-hexane layer (B) three times with 25 ml of water to re- move hydrochloric acid, adding the washings to (A). Wash the aqueous solution (A) twice with 20 ml of n-hexane (C). Run the solution (C) into a third separating funnel and wash this solution (C) once with 10 ml water and then add (C) to the solution (B). Discard solution (A)

3.3.5 Transfer solution (B) to a 500 ml conical flask, add a few ‘drops of phenolphthalein indicator and excess of alcoholic potassium hydroxide solu- tion to make the alcoholic layer sufficiently alkaline after vigorous shaking. Boil solution (B) under reflux condenser for half an hour and transfer solution (B) to a separating funnel. Wash the 500 ml conical flask with small portion of ethyl alcohol and n-hexane and add the wash- ings to solution (B). Add also a few millilitres of water to solution (B) to facilitate separation of alcohol layer. Draw off the lower alcohol layer (D) into another separating funnel.

3.3.6 Wash the alcohol layer (D) three or four times with 25 ml n-hexane and add the washing to solution (B). Wash solution (B) carefully and repeatedly with aqueous ethyl alcohol ( 50 percent by volume ) till free from alkali and soap and finally wash once with 50 ml of water. Discard the ethyl alcohol and water washings. During washings of solution (B), care should be taken that there is no loss of’ mineral oil due to emul- sification.

3.3.7 Filter solution (B) through a filter paper into a clean and dry tared conical flask or beaker and evaporate off n-hexane on water bath. Ensure tl at the separating funnel as well as the filter paper are thoroughly washed with small quantities of n-hexane and washings are also transferred for evaporation to minimise loss of oil.

3.3.8 Remove last traces of n-hexane by heating in an oven at 105’C and by agitation/passing air over the hot oil. Cool and weigh. Repeat ope- ration of heating, cooling and weighing till cons- tant mass is obtained. From the mass of the residue, calculate the percentage by mass of mineral oil.

3.3.9 If the grease contains rosin oils, beeswax, degras, spermaceti, spermatin, montan wax,

candle pitoh and other materials containing a larger amount of unsaponifiable substances, the mineral oil isolated from solution (B) will contain unsaponifiable matter and the constant found will differ from those of the petroleum products used in making the grease. In most cases, no further separation is possible except in the hands of skilful and experienced operators who can devise special methods to suit the individal conditions.

4 METHOD-B -

4:1 @dine of’the Method

The sample is heated with potassium hydrogen sulphate and ignited sand and then extracted with petroleum hydrocarbon solvent in sohxlet appa- ratus. The extract is saponified, washed and then distilled when the mineral oil is obtained as the residue.

4.2 Reagents

Potasstum Hydrogen Su&hate ( KHSO, ) - granu- lated.

Igntted sand - clean and dry.

Phenolpthalein indicator - as in 3.2.3.

n-Hexane ( see IS 3470 : 1966 ).

Alcoholtc Potassium Hydroxide solution - approxi- mately 10 percent ( m/v ).

Ethyl Alcohol - as in 3.2.5.

4.3 Procedure

4.3.1 Weigh 8 to 30 g of the material, accurately to 0.1 g in a 75 mm porcelain dish and add IO g of potassium hydrogen sulphate and 18 g of clean dry ignited sand and 5 ml of water.

4.3.2 Heat the dish and contents on a steam bath while stirring frequently until all water is driven off ( 2 hours being usually sufficient ) cool and break the lumps with a small pestle and transfer the mixture quantitatively to an extrac- tion thimble, which has been previously placed in a soxhlet apparatus, using a little n-hexane to wash the last traces into the thimble.

4.3.3 Extract the mixture in the thimble thorou- ghly with n-hexane. Add a few drops of phenol- phthalein indicator to the n-hexane extract, saponify it with excess of alcoholic potassium hydroxide solution and continue the process given thereafter in 3.3.3 of Method A to determine the mineral ,oil content.

2

.A-1 SCOPE

IS 1448 [ y : 59 ] I 1991

ANNEX A

SUPPLEMENTARY METHOD FOR THE ANALYSIS OF LUBRICATING GREASES

A-l.1 This method includes procedures for the determination of the total fluid constituent and the total n-hexane insoluble material. It is pri- marily intended for application to greases of the types discussed in 1.2.

A-2 DEFINITIONS

A-2.1 Total fluid constituent the mineral oil or no petroleum fluid and n-hexane soluble fats or all three.

A-2.2 Total n-hexane insoluble material - soap, nonsoap thickeners, fillers, inorganic salts from free alkali, asphaltenes or any combination of these, essentially insoluble in n-hexane.

A-3 APPARATUS

A-3.1 Extraction Apparatus

A 1 OOO-ml flask shall be used. A double thick- ness filter paper extraction thimble, 33 by 94 mm, shall be suspended by corrosion resistant wire or by a corrosion resistant basket below the con- denser in such a position that the condensed solvent will enter the thimble.

A-4 PROCEDURE

A-4.1 Weigh to the nearest 1 mg 10 & O-2 g of a representative sample into the n-hexane washed, dried, tared extraction thimble and place the thimble in the extraction apparatus to which 125 ml of n-hexane has previously been added, Place the assembly on steam plate and extract for 12 hrs.

A-4.2 Remove the thimble from the apparatus, dry the insoluble material for 30 minutes in a convection oven at 1OO’C and record the weight.

To ensure complete removal of fluid constituent, re-extract the insoluble material for 1 hr.

A-4.3 Dry and reweigh. If the weight loss is greater than 20 mg, reextract for 4 hrs more, Repeat the drying operation.

A-4.4 Transer the n-hexane filtrate to a tared beaker. Evaporate the solvent on steam plate, with a jet of air or inert gas impinging on the surface for 3 hrs, and place in a convection oven for 1 hr at 100%. Heat to constant weight.

A-5 CALCULATIONS

A-5.1 Calculate the percentage of constituent as follows:

Total fluid constituents, percent

-( 100 x A _B W >

total fluid

where,

A = gms of n-hexane soluble residue ( 4-4 ); W = gms of sample used; and

B = percentage of free fatty acids as oleic.

A-5.2 Calculate the percentage of total n-hexane insoluble mater ial as follows:

Total n-hexane insoluble material, percent

_ looxc_D ( W )

c X

w = D=

gms of residue from n-hexane extraction ( 4-3 ); gms of sample used; and percentage of free alkali as the hydro- xide of the predominating base.

ANNEX B

PRECAUTIONARY STATEMENTS

B-l n-HEXANE

Danger - Extremely flammable.

Harmful if inhaled. May produce nerve cell damage. Vapours may cause flash fire. Keep away from heat, sparks and open flame. Keep container closed. Use with adequate ventilation. Avoid build up of vapours and eliminate all sources of ignition especially all non explosion proof electrical apparatus and heaters. Avoid breathing of vapour or spray mist, use respiratory protection devices as required.

Avoid skin and eye contact, use impermeable gloves and aprons as required.

B-2 ETHYL ALCOHOL

Warning - Flammable, Denatured, Cannot be made nontoxic.

Keep away from heat, sparks and open fire flame. Keep container close. Use with adequate ventila- tion. Avoid prolong breathing of vapour or spray mist. Avoid contact with eyes and skin. Do not take internally.

3

IS 1448 [ P : 59 ] : 1991

B-3 PHENOLPHTHALEIN Causes severe eye irritation or injury. Dust or

Warning - Avoid skin contact or ingestion. mist may be harmful.

B-4 POTASSIUM HYDROGEN SULPHATE B-5 POTASSIUM HYDROXIDE

( RHSO4 1 Danger - Poison. Corrosive. Causes eye and skin.

Danger - Poison. Harmful or fatal if swallowed. damage. Harmful if swallowed or inhaled.

4’

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