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है”ह”ह

IS 1448-55-1 (2004): Methods of Test for Petroleum and ItsProducts, Part 55, Section 1: Determination ofSaponification Value of Petroleum Products [PCD 1: Methodsof Measurement and Test for Petroleum, Petroleum Productsand Lubricants]

IS 1448 [P : 55/See 1] :2004

(m @wvIndian Standard

METHODS OF TEST FOR PETROLEUM AND ITSPRODUCTS

[P: 55/Section 1]

DETERMINATION OF SAPONIFICATION VALUE OF PETROLEUM PRODUCTS

(First Revision,)

ICS 75.080

@ BIS 2004

BUREAU OF IN DIAN STANDA RDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

kluy 2004 Price Group 2

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

FOREWORD

This Indian Standard [P: 55/See 1] (First Revision) was adopted by the Bureau of Indian Standards, after the draftfinalized by the Methods of Measurement and Test for Petroleum, Petroleum Products and Lubricants SectionalCommittee had been approved by the Petroleum, Coal and Related Products Division Council.

Saponifiable value, saponifiable and unsaponifiable matter, see [P: 55] of IS 1448 was published in 1963 in order toalign the method given in ASTM D 963:1954, which has since been withdrawn in 1963. It was decided to publish theseparate test method, namely, Saponit-mble value of petroleum products and saponifiable and unsaponifiable matter inoil fat and waxes. Considerable assistance has been derived from ASTM D 94 and IP 136 for formulation of this testmethod.

The composition of the Committee responsible for formulation of this standard is given in Annex A.

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

IS 1448 [P : 55/See 1] :2004

Indian Standard

METHODS OF TEST FOR PETROLEUM AND ITSPRODUCTS

[P: 55/Section 1]

DETERMINATION OF SAPONIFICATION VALUE OF PETROLEUM PRODUCTS

(First Revision)

1 SCOPE

This method [P : 55/See 1] is intended for thesaponification value in straight mineral oils, compoundedmineral oils and waxes.

2 SUMMARY OF METHOD

A known mass of sample is dissolved in 2-butanone(Methyl ethyl ketone) is heated with known amount ofalcoholic potassium hydroxide. The excess alkali istitrated with standard acid and saponification numbercalculated. This method is not applicable in the presenceof compounds of sulphur, phosphorous, chlorine, etc.which reacts with acid or ~kali.

NOTE — If larger amounts of unsaponifiabk or saponifiablematter are required for further examination, larger samples maybe taken provided the quantities of the reagents are suitably

adjusted.

3 TERMINOLOGY

3.1 Saponify — To hydrolyze a fat with alkali to form analcohol and the salt of a fatty acid.

3.2 Saponification Number — The number ofmilligrams of potassium hydroxide consumed by onegram of a sample under the conditions of the test.

4 APPARATUS

4.1 Erlenmeyer Flask and Condenser

Erlenmeyer flask of 300 ml capacity. Flask which hasbecome etched by long use should not be used. Thestraight type condenser shall be fitted to the flask withground glass joint.

4.2 Hot-Plate or Water Bath

5 REAGENTS

5.1 Purity of Reagents

Analytical grade reagent chemicals shall be used in alltests.

5.1.1 Alcohol — 95 percent ethanol.

5.1.2 StandardPotassiumHydroxide Solutionj 0.5 N –

Prepare approximately 0.5 N alcoholic potassiumhydroxide by dissolving 30 g of potassium hydroxide in1 Ii&ealcohol. Allow the solution to setde in dark place.Filter the solution and keep it for 24 h before use,

5.1.3 StandardHydrochloricAcid, 0.5 N

Mix 45 ml of hydrochloric acid (Sp gr 1.19) in 1 litre ofalcohol.

5.1.4 Butanone-2(MethylEthylKetone)TechnicalGrade

5.1.5PetroleumSpirit, 60/80.

5.1.6 PhenolphthuleinIndicatorSolution

6 SAMPLE SIZE

Use such a size of the sample that not more than half ofthe potassium hydroxide added in the reagent, reactsduring the test,

The following quantities are suggested:

SaponiJcationNumber SampleSize, g

181 to400 1

lllto 180 2

71 tollo 3

31t070 5

16 to 30 10

Mineral oils 20

7 PROCEDURE

7.1 Weigh the oil sample to the nearest O.lg into thereaction flask. Add 25~1 ml methyl ethyl ketone,followed by 25 ~ 0.3 ml alcoholic KOH solution measuredaccurately from the burette or pipette. Connect thecondenser to the flask and heat for 30minafter refluxingbegins, Immediately disconnect the condenser add 50mlof petroleum sprit and immediately titrate the solutionwith standard hydrochloric acid using 1 ml of phenol-phthalein indicator. When testing waxes it may benecessary to reheat during titration in order to prevent

1

IS 1448 [P : 55/See 1] :2004

solidification of the sample.

7.2 Make a blank determination in duplicate at the sametime following exactly the same procedure but omittingthe sample.

8 CALCULATION

Calculate the saponification number as follows:

56,I(V– ~)NSaponification number =

M

v = volume, in ml of acid used in titrating theblank

Vl = volume, in ml of acid used in titrating thesample;

Iv = normality of the hydrochloric acid, and

M = mass of the sample, in g.

9 REPORT

Report the result to the nearest 0.5 as the saponificationvalue.

10 PRECISION

Follow the graph as per IP 136/ASTM D 94.

2

IS 1448 [P : 55/See 1] :2004

ANNEX A(Foreword)

COMMI’M’EE COMPOSITION

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

Organization

Indian Institute of Petroleum, Debra Dun

Air Headquarters, Ministry of Defence, New Delhi

AIMIL Ltd, Delhi

All India Instrument Manufacturers and Dealers Association,Mumbai

Automotive Research Association of India (ARAI), Pone

Bharat Petroleum Corporation Ltd, Mumbai

Bogaigaorr Refinery & Petrochemicals Ltd, Dhrdigaon

Castrol India Ltd, Mumbai

Central Fuel Research Irsstimte, Dhanbad

Centrsd Revenue Control Laboratory, Department of Revenue,New Delhi

Dkectnrate General of Civil Aviation, New Delhi

Hindustan Petroleum Corporation Ltd (a) Mumbai@) Visakhapatnam

Indian Oil Corporation Ltd, Assam Oil Division, Digboi

Indian Oil Corporation Ltd, Marketing Division, Mumbai

Indian 011 Corporation Ltd, R & P Division, New Delh]

Indian Oil Corporation Ltd, R & D Centre, Faridabad

Indian Oil Blending Ltd, Mumbai

Lubrisol India Ltd, Mumbai

Madras Refineries Ltd, Chennai

Mangalore Refineries and Petrochemicals Ltd, Marrgalore

Ministry of Defence (DRDO), Kanpur

Representative(s)

SSSRISUDHIRSINGHAL(Chairman)DRA. DUtTA(Alternate]

Jom’rDIRECTOR(QAS ARRO)DmmY DIiWCtWR(QAS) (Alternate)

SHRIS. C. JAINSSSRISURtNDESSHARbM(Alternate)

SHRIVINAYTOSHNIWALFkmmvE SmARY (Alternate)

SHRIBHANUtSHRIM. K. CHAUDHURI(Altemafe)

SHRSILK. MODIDRY. P, RAO (Alternate)

SHtUC. J? BBZ.SORUAHSHRIS. S. ROY (Alternate)

SHtuM. GUFTA

Du P. SAMUELDR K. N. BHAITACHARYA(Alternate)

CHII?PCHmtLVTDPPUTYCHIPPCHiwm’r(Alternate)

sHRtB. K. JosH1SHtUS. S. MAZUMDAR(Alternate)

SHRtN. S. J.R.AOSHRSG. SatGAtWLSH(Alternate)

sHstA. K. CHAKtUBORTYSHRSP, M. SINHA(Alternate)

SHRIA. K. VERMADRT. K. DE (Alternate)

SHtUD. J. KAKATSSHRIA. K. KATHUSUA(Alternate)

SHrttN. R. ILUE

sHtUH. S. MEHTASHRIA. K. SEHGAL(Alternate)

SHRtR. R. PARMARDR U. S. RAO(Altenrate)

SHtuN. V. KALASVANANSENIORMANAGER(TS-QC) (Alternate)

sHRt s. k4ht13H

DR P. S. VENICATARAMANISHRtH. C. SRtVA.WAVA(Alternate)

3(Continued on page 4)

IS 1448 [P : 55/See 1] :2004(Continued from page 3)

Organization

Ministry of Defence (DGQA), New Defhi.

Ministry of Petroleum and Natural Gas, New Delhi

Ministry of Consumer Affairs, Food & Pubfic Distribution,New Delhi

National Test House, Kolkata

Oil & Natural Gss Commission, Debra Dun

Projects & Development India Ltd, Sindri

Reliance Petroleum, Gujarat

Research Designs & Standards Organization, Lucknow

Shriram Institute for Industrial Research, New Delhi

BIS Directorate General

Representative(s)

SHRIK. H. GANDHISHatA. J. S. AUORA(Aliernate)

ADVISER(l&maaIas)DII+XI’OR(SUPPLY)(Alternate)

DIqR LEGALMETROLOGYDEPUrYD[IW3W LEGALMETROLOGY(Alternate)

SHRIK. C. NASKARSHRIP. K. CHAKBABORTY(Alternute)

DR S. F. H. RAZVISHRIS. MATHUR(Alternate)

DRR. P. SINGH

SHRIV. S. IWAN

DmI’rY DISEIXIR(CHFMCALS)ASSISTANTRFSFARCHOFFKER(CM) - IV (Alternate)

DRP.K. KAICKERSHRIMATILAXMIRAWAT(Alternate)

ANJANKAR,Director and Head (PCD)[Representing Director General (Ec-o@o)]

--

Member SecretarySHRIA. K. BHATNAGAR

Joint Director (pCD), BIS

4

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Enquiries relating to copyright be addressed to the Director (Publications), BIS.

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Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewedperiodically; a standard along with amendments is reaffirmed when such review indicates that no changes areneeded; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standardsshould ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of‘BIS Catalogue’ and ‘Standards: Monthly Additions’.

This Indian Standard has been developed from Doc : No. PCD 1 (1694).

k

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Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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