is 7585 (1995): wines - methods of analysis

27
Disclosure to Promote the Right To Information Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public. इंटरनेट मानक !ान $ एक न’ भारत का +नम-णSatyanarayan Gangaram Pitroda “Invent a New India Using Knowledge” प0रा1 को छोड न’ 5 तरफJawaharlal Nehru “Step Out From the Old to the New” जान1 का अ+धकार, जी1 का अ+धकारMazdoor Kisan Shakti Sangathan “The Right to Information, The Right to Live” !ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह Bharthari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 7585 (1995): Wines - Methods of Analysis [FAD 14: Drinks and Carbonated Beverages]

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Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public.

इंटरनेट मानक

“!ान $ एक न' भारत का +नम-ण”Satyanarayan Gangaram Pitroda

“Invent a New India Using Knowledge”

“प0रा1 को छोड न' 5 तरफ”Jawaharlal Nehru

“Step Out From the Old to the New”

“जान1 का अ+धकार, जी1 का अ+धकार”Mazdoor Kisan Shakti Sangathan

“The Right to Information, The Right to Live”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता है”Bhartṛhari—Nītiśatakam

“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 7585 (1995): Wines - Methods of Analysis [FAD 14: Drinksand Carbonated Beverages]

IS 7535 : 1995

(YWJJ!W) Indian Standard

WINES - METHODS OF

( First Revision )

ICS 67.160.10

ANALYSIS

@ BIS 1995

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

NEW DELHI 110002

Llecember 1995 Price Group 9

Drinks and Carbonated Beverages Sectional Committee, FAD 14

FOREWORD

This Indian Standard (First Revision) was adopted by the Bureau of Indian Standards, after the draft finalized by the Drinks and Carbonated Beverages Sectional Committee had been approved by the Food and Agriculture Division Council.

Wines are obtained by alcoholic fermentation of fresh fruit juices such as grapes and possess the varietal character derived from the fruits or the principles produced during the fermentation. This standard includes the test methods for various parameters for evaluating quality of wines.

This standard was originally published in 1975. A need was felt to revise the standard in the light of experience gained over the years and the current analytical practices followed in testing of wines. This revision incorporates additional test methods for determination of tannins as well as extracts.

A separate Indian Standard IS 3752 : 19S9 ‘Methods of test for alcoholic drinks (first J-evision)’ has been published. This standard is complimentary to IS 3752 : 1989.

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 (P-raised)‘.

IS 7585 : 1995

Indian Standard

WINES - METHODS OF ANALYSIS

( First Revision )

1 SCOPE

This standard prescribes the methods of analysis of wines.

2 REFERENCES

The Indian Standards contain provision which through reference in the text, constitute provision of this standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated in Annex A.

3 QUALITY OF REAGENTS

Unless specified otherwise, pure chemicals and reagent grade water (see IS 1070 : 1992) shall be employed in the tests.

NOTE - ‘Pure chemicals’ shall mean chemicals that do not contain impurities which affect the results of analysis.

4 DETERMINATION OF ETHYL ALCOHOL CONTENT

4.1 General

For determination of ethyl alcohol content in wines, two methods have been prescribed, namely, Pyknometer Method and Hydrometer Method. Pyknometer Method (4.2.5) shall be the reference method. With the Pyknometer Method, a suitable correlation should be established for values ob- tained by the Hydrometer Method (4.2.4), which may be then used as a routine method.

4.2 Distillation of Sample

4.2.1 General

Samples of wines having sulphur dioxide more than 35 mg per litre or volatile acidity (as acetic acid) exceeding 1.0 g per litre be neutralized prior to distillation with 2 N sodium hydroxide. To prevent bumping during distillation a few boiling chips or stones may be added.

4.2.2 Apparatus

4.2.2.1 Distillation assembly

4.2.2.2 Pyknometer - 25 or.50 ml capacity.

4.2.2.3 Hydrometer - of suitable range (calibrated).

4.2.2.4 Thermometer - 6 to 50°C.

4.2.3 Procedure

Measure 250-ml sample into a 500-ml distillation flask, note the temperature and add 50 ml water. Attach the flask to the vertical condenser. Distil almost 250 ml and make up the volume to 250 ml with water at the same temperature at which the sample was taken.

4.2.4 Hydrometer Method

The hydrometer method as given under IS 2302 : 1989 shall be followed.

4.2.5 Qknometer Method

Determine the specific gravity of the distillate (4.2.1) with the help of a pyknometer at the re- quired temperature and obtain corresponding ethyl alcohol content by volume from the tables given under IS 3506 : 1989.

5 DETERMINATION OF ACIDITY

Methods for determination ofpH, total acidity and volatile acidity have been prescribed-respectively in 5.1, 5.2 and 5.3. Any of these methods may be used depending on the requirements.

5.1 pH

5.1.1 Apparatus

5.1.1.1 pH meter

5.1.1.2 Beakers - lOO-ml.

5.1.2 Procedure

pH shall be determined bypH meter as per instruc- tions provided with the instrument.

5.2 Total Acidity

5.2.1 Apparatus

5.2.1.1 Burette - 25 or50-ml, calibrated in 0.05Dr 0.1 ml.

5.2.1.2 Pipette - 5-ml.

5.2.1.3 Erlenmeyerflask - 500-ml.

I

IS 7585 : 1995

5.2.2 Reagents

5.2.2.1 Sodium hydroxide solution - 0.1 N , car- bonate free.

5.2.2.2 Phenolphthalein solution - 0.1 g in 100 ml of 60 percent rectified spirit.

5.2.3 Procedure

5.2.3.1 Removal of carbon dioxide

Remove carbon dioxide, if present, by following any of the two methods:

a)

b)

Place 25 ml sample of the material in a small Erlenmeyer flask and connect to water aspirator. Agitate for one minute under vacuum. Place 25 ml sample of the material in a small Erlenmeyer flask, heat to incipient boiling for 30 seconds, swirl and cool.

5.2.3.2 Place 200 ml of boiling distilled water in a SOO-ml wide-mouth Erlenmeyer flask. Add 1 ml of phenolphthalein indicator and titrate to a faint but distinct pink colour. Pipette 5-10 ml of degassed sample (5.2.3.1) into the flask and titrate to the same end-point. In the case of dark and red wines some practice is needed to recognize the end-point detection since the colour change is not exactly the same as with the water. A better detection of the colour change may be obtained if a light source is placed under the flask.

5.2.4 Calculation

Total acidity as tartaric acid, g/litre = Ml x N x 0.075 x 1000

where Ml =

N =

volume in ml of sodium hydroxide solution used in titration,

normality of sodium hydroxide solution, and

M2 = volume in ml of the (wine) sample.

5.3 Volatile Acidity

5.3.1 Apparatus - Sellier’s apparatus as shown in Fig. 1.

5.3.2 Reagents

5.3.2.1 Sodium hydroxide solution - 0.025 to 0.05 N, standardized, carbonate free.

5.3.2.2 Phenolphthalein solution --0.1 g in 100 ml of 60 percent rectified spirit.

5.3.3 Procedure

Fit the Sellier tube into one hole of the rubber stopper into the other hole place an ‘L’ shaped glass tube. Attach a short section of rubber hose to the end of the glass tube. Fit the rubber stopper to the 500-ml Erlenmeyer flask. Attach the flask to the ring stand and connect the Sellier tube to the distil- lation trap and the trap to the condenser. Start cold water running in the condenser. Place about

WINE SAMPLE

------ BOILING WATER

FIG. 1 SELLIERSAPPARATUS

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IS 7585 : 1995

250 ml of distilled water in the SOO-ml Erlenmeyer flask. Pipette 10 ml of decarboned wine into the Sellier tube and~slightly connect the trap and con- denser. Place the 250-ml flask~(marked with a wax pencil at 100 ml) under the condenser outlet. Light the burner under the 500-ml Erlenmeyer flask and heat until steam. issues from the outlet. Now use the pinch-cock to close the outlet from the 500-ml flask thus forcing steam into the Sellier tube. The distillation should be conducted rapidly until 100 ml have been collected. Before removing the flame, open the pinch-cock. Place the flask containing the distillate onthe hot plate (operating on medium heat) and bring the contents to a boil. Do not allow to boil vigorously, nor continue the boiling more than 30 seconds. Add 3 drops of the phenolphthalein solution and titrate while still hot to a faint pink end-point using sodium hydroxide solution. Record the amount of sodium hydroxide used and its normality.

5.3.4 Calculntion

Volatile acidity (expressed as acetic acid), g/litre,

Mt x N x 1000 x 0.060 = M2

where Mt = volume in ml of sodium hydroxide

solution, N = normality of sodium hydroxide

solution, and

M2 = volume of wine sample.

5.3.5 Fixed Acidity

Calculate the fixed acidity as under: Fixed acidity = total acidity - volatile acidity x

1.25

6 DETERMINATION OF EXTRACT

6.1 General

Three methods, namely, pyknometer method, Hydrometer method and Evaporation method have been prescribed.

6.2 Pyknometer Method

Specific gravity of sample and that of alcoholic distillate are determined and then the sp gr of de-alcoholized wine (D) is calculated, such that D=S+l-S’

where S = sp gr of sample, and

5’ = sp gr of alcoholic distillate.

From the table given in Annex B, determine per- centage by mass of extract in dealcoholized wine corresponding to the value of D. This figure mul- tiplied by the value of D gives the extract in g/100 ml of wine. Calculate to express the result in g/l of wine.

6.2.1 Apparatus

a) Constant temperature water-bath, b) Pyknometers - 50-ml, and c) Distillation assembly.

6.2.2 Calibration

Fill thoroughly cleaned Pyknometer with recently distilled water and stopper it and immerse in con- stant temperature water bath with bath level above graduation mark on pyknometer_After 30 minutes, remove the stopper and with capillary tube adjust until bottom of meniscus is tangent to graduation mark. With small roll of filter paper, dry inside neck of pyknometer, stopper and immerse in water at room temperature for 15 minutes. Remove the pyknometer, dry it ‘and let it stand for 15 minutes and weigh. Empty the pyknometer, rinse with acetone, and dry thoroughly in air with suction. Let empty flask and stopper come to room tempera- ture, and weigh. Mass of contained water = mass of filled pyknometer - mass of empty pyknometer.

6.2.3 Calculation

Sp gr (s) = 2

where

nu = mass of sample, and

ntw = mass of water.

6.2.4 Procedure

6.2.4.1 Take 200 ml of sample in a 500-ml distilla- tion flask containing about 25 ml of distilled water and a few pieces of pumice stone. Complete the distillation in about 35 minutes flask till thevolume in the flask nears the mark. Allow the distillate to come to room temperature, make up thevolume to 200 ml with distilled water and mix thoroughly.

6.2.4.2 Find out the specific gravity of the distillate at the required temperature with the help of a pyknometer.

6.3 IIydrometer Method

The residue for the alcohol distillation (4.2.1) is brought back to the original volume with water; then determine the specific gravity ‘D’ of de-al- coholized wine using hydrometer. Determine per- cent by mass of extract in de-alcoholized wine corresponding to value of ‘LY. This figure X value

3

-IS 7585 i 1995

of D = g of extract per 100 ml of wine. Calculate to express in g/l of wine.

6.4 Evaporation Method

This method shall be applicable for dry wines and wines containing extract less than 3 g per 100 ml and for sweet wines containing extract 3 to 6 g per 100 -ml.

6.4.1 Apparatus

6.4.1.1 Pipette - 50-ml.

6.4.1.2 Evaporating dishes - 75ml, flat-bottom, platinum.

6.4.1.3 Oven

6.4.1.4 Water-bath

6.4.1.5 Desiccator

6.4.2 Procedure

6.4.2.1 In d?y wines, when extract content is less than 3 g/l 00 ml

Take 50 ml sample in 75-ml flat-bottom platinum dish and evaporate on water bath to make syrupy consistency. Heat the residue for 2 to 5 hours in drying oven at 100°C. Cool the mass in desiccator and weigh as soon as room temperature is reached. Calculate the extract in g/l of wine.

6.4.2.2 In sweet wines, if extract content is 3-6g/lOOmI

Treat 25 ml sample and calculate as above.

7 DETERMINATION OF REDUCING SUGAR

7.1 Lane and Eynon (Fehling) Method

7.1.1 Reagents

7.1.1.1 Soxhlet reagent

Mix equal amounts of solution A and solution B.

a)

b)

Solution A - Dissolve 34.639 g of copper sulphate in wafter, add 0.5 ml of con- centrated sulphuric acid of sp gr 1.84 and dilute to 500 ml. Filter the solution through asbestos. Solution B-Dissolve 173 g of Rochelle salt (potassium sodium tartrate) and 50 g of sodium hydroxide, dilute to 500 ml and allow the solution to stand for two days. Filter through asbestos.

7.1.1.2 Lead acetate solution - saturated, neutral.

7.1.1.3 Glacial acetic acid

7.1.1.4 Disodium hydrogen phosphate (Na2HP04)

7.1.1.5 Methylene blue solution - 0.05 g in 100 ml of water.

7.1.1.6 Standard invert sugar solution

a) Stocksolution ofdextrose -Weigh accurate- ly 10 g of anhydrous dextrose into a 1-litre graduated flask and dissolve it in water. Add to this solution 2.5 g of benzoic acid, shake to dissolve the benzoic acid and make up the volume to the mark with water. This solu- tion shall be freshly prepared daili.

b) Standard dextrose solution - Dilute a known aliquot of the stock solution of dextrose [7.1.1.6(a)] with water containing 0.25 percent (m/v) of benzoic acid to such a concentration that more than 15 ml but less than 50 ml of it will be required to reduce all the copper in the Fehling solution taken for titration. Note the concentration of an- hydrous dextrose in this solution as mil- ligrams per 100 ml, prepare this solution fresh every day.

7.1.1.7 Sodium hydroxide - 1 N.

7.1.2 Preparation of Control

Pipette25 ml of Soxhlet reagent into a 230-ml flask. Add 10 ml of 0.5 percent standard invert sugar solution, bring it to boil in 3 minutes and keep it boiling for 3 minutes ( using glass beads to prevent bumping). Add 5 drops of methylene blue in- dicator and titrate the solution while still hot with standard 0.5 percent invert sugar till faint blue - and then add dropwise until the solution is reddish in colour.

7.1.3 De-alcoholization and Decolourization of WZne Sample

Take 100 ml of wine sample in a porcelain dish. Exactly neutralize with sodium hydroxide calculat- ing the acidity (5.2) and evaporate to 50 ml. To this add 5 ml of lead acetate solution, enough activated charcoal and 2 drops of glacial acetic acid. Make the volume to 100 ml with distilled water. Filter this mixture into 2 g of disodium hydrogen phos- phate in a beaker.

7.1.4 Procedure

Pipette 20 ml of the clarified wine into an Erlen- meyer flask containing 25 ml of Soxhlet reagent. Bring it to boil and titrate with 0.5 percent invert sugar, with methylene blue indicator, to a brick red end point. Calculate the reducing sugar from the standard tables.

8 DETERMINATION OF TANNINS

Two methods - Calorimetric method and Spectrophotometric method have been prescribed. Any of the methods can be followed for routine analysis, However, in case of dispute the Spectrophotometric method shall be the referee method.

4

IS 7585 : 1995

8.1 Calorimetric Method

8.1.1 Reagent

8.1.1.1 Folin-Dennis reagent

Prepare by adding 100 g of sodium tungstate (Na2W04, 2H20), 20 g of phosphomolybdic acid and 50 ml of phosphoric acid to 750 ml of water, reflux for two hours and dilute to 1 litre.

8.1.1.2 Saturated solution of sodium carbonate

Prepare by adding 35 g of anhydrous sodium car- bonate to 100 ml of water at about 80°C. Allow to cool overnight and seed with a few crystals of sodium carbonate (Na2COs,H20).

8.1.1.3 Standard tannic acid solution

Prepare daily, by dissolving 100 mg of tannic acid in a litre of water.

8.1.2 Procedure

Pipette 1 ml of wine into a lOO-ml volumetric flask containing 80 ml of water. Add5 ml of the Folin- Dennis reagent and 10 ml of the sodium carbonate solution and shake well and make to the mark. After 30 minutes compare the colour to that developed with standard tannic acid solution prepared in the same way. Standards containing 0.0,0.2,0.4,0.6,0.8,1.0, 1.2, 1.4, 1.6, 1.8,2.0 and 2.4 ml of the standard tannic acid solution should be useful.

8.2 Spectrophotometric Method

8.2.1 Reagents

8.2.1.1 Folin-Dennis reagent

To 750 ml of distilled water add 100 g of sodium tungstate (Na2W04, 2H20), 20 g of phos- phomolybdic acid, and 50 ml phosphoric acid. Reflux for 2 hours, cool and dilute to 1 litre.

8.2.1.2 Sodium carbonate saturated solution

To each 100 ml of distilled water add 35 g anhydrous sodium carbonate, dissolve at 80°C, and allow to cool overnight. Seed with a few crystals of sodium carbonate (NazCos, H20) and after crystallization filter through glass wool.

8.2.1.3 Standard tannic acid solution

0.1 mg/ml. Dissolve 100 mg tannic acid in 1 litre of distilled water. Prepare fresh solution for each determination.

8.2.2 Preparation of Standard Curve

Pipette 0.0 to 10.0 ml of standard tannic acid solu- tion into lOO-ml volumetric flask containing 75 ml distilled water. Add 5 ml Folin-Dennis reagent and 10 ml of sodium carbonate saturated solution and

dilute to volume with distilled water. Mix well and determine absorbance after 30 minutes at 760 nm. Plot absorbance against mg of tannic acid/100 ml of wine.

8.2.3 Procedure

Using 1.0 ml sample determine absorbance as above and obtain mg of tannic acid/100 ml from the standard curve. Calculate to express the value in g/l of wine. If absorbance is too great, repeat deter- mination on 1 + 4 dilutions of sample.

9 DETERMINATION OF SULPHUR DIOXIDE

9.1 Free Suiphur Dioxide

9.1.1 Ripper Method

9.1.1.1 Reagents

a) Iodine solution - 0.02 N, standardized. b) Sodium bicarbonate c) Starch indicator solution - Triturate 5 g of

starch and 0.01 g of mercuric iodide with 30 ml of cold water and slowly pour it with stirring into a litre of boiling water. Boil for three minutes. Allow to cool and decant off the supernatant clear liquid.

d) Sulphuric acid - 1 N.

9.1.1.2 Procedure

Pipette 50 ml of wine into a 250-ml Erlenmeyer flask. Add 5 ml of starch indicator, 5 ml of sul- phuric acid and pinch of sodium bicarbonate to expel air. Rapidly titrate the free sulphurous acid using iodine solution. The end-point .shall be the first darkening of solution to a bluish colour per- sisting for l-2 minutes.

9.1.1.3 Calculation

Sulphur dioxide mgilitre = MtxNx32xlOOO

M2

where Mt = volume in ml of iodine used, N = normality of iodine, and

M2 = volume in ml of sample.

9.1.2 Distillation Method

9.f.2.1 Apparatus

a)

b)

Round bottom flask - 250-ml, with ground glass, side arm and an air leak side inlet with a tube to the bottom of the flask. Absorption tubes - two, 200 x 25 ml con- nected in series, mercury manometer and water pump.

9.1.2.2 Reagents

a) Hydrogen peroxide - 1 percent (m/v). b) Sodium hydroxide - 0.01 N.

5

IS 7585 : 1995

c) Orthophosphoric acid - 25 percent.

9.1.2.3 Procedure

Connect the round bottom flask to the two absorp- tion tubes and to the manometer and water pump. Add 5 ml of hydrogen peroxide to each absorption tube. Pipette 10 or 20 ml of wine and 5 ml of orthophosphoric acid into the round bottom flask. Start the water pump and maintain the pressure of 70 to 80 mm while pumping, a steady stream of air through the air-leak inlet is maintained. After 15 minutes shut off the vacuum, lower the first absorp- tion tube, and rinse off any liquid on the delivery tube. Titrate to a grey end-point with sodium hydroxide. Replace the tube on the apparatus and rinse the inside of the delivery tube and readjust the- end-point if necessary. Now attach the other ab- sorption tube and apply thevacuum for 15 minutes and proceed as above. Titrate the blank and sub- tract from the first value. One ml of 0.01 N sodium hydroxide is equivalent to 0.32 mg of SO2.

9.2 Total Sulphur Dioxide

9.2.1 By Distillation

The procedure shall be the same as for free SO2 except that the round-bottom flask shall be heated during distillation on a low flame. The time of distillation shall be the same as before.

9.2.2 Ripper Method

9.2.2.1 Reagents

Same as under 9.1.1.1 and the following:

Sodium hydroxide - 1 N.

9.2.2.2 Procedure

To 20 ml of wine sample in a flask, add 25 ml of the sodium hydroxide. Cool immediately and let it stand for 10 minutes for hydrolysis to complete. Add a pinch of sodium bicarbonate, 5 ml starch indicator and 10 ml sulphuric acid. Titrate rapidly with standard iodine (0.012 5 N) to a faint blue colour. One ml of 0.012 5 N iodine is equivalent to 0.8 mg of total sulphur dioxide. Calculate to ex- press the result in mg./l of wine.

9.3 Bound SO2

It shall be the difference between the total sulphur dioxide (9.2) and free sulphur dioxide (9.1) SOz.

10 DETERMINATION OF COPPER

10.1 Reagents

10.1.1 Hydrochloric Acid Citric Acid Reagent

One ml of concentrated hydrochloric acid + 2 g of citric acid.

10.1.2 Ammonium Hydroxide (Accurately Prepared) - 5 N.

10.1.3 Sodium Diethyldithiocarbamate Solution - 0.1 percent in water.

10.1.4 AmylAcetate - copper-free.

10.1.5 MethylAlcohol - absolute, copper-free.

10.1.6 Sodium Sulphate - anhydrous

10.1.7 Standard Copper Solutions - 0.5,1.0,1.5,2 and 3 mg per litre.

10.1.8 Procedure

Pipette 10 ml of each of the standard copper solu- tions into clear separating funnels. Add 1 ml of the hydrochloric acid-citric acid reagent to each of the tubes and mix. Now add 2 ml of ammonium hydroxide and remix. Then add 1 ml of the sodium diethyldithiocarbamate solution to each tube and shake. After a minute add 10 ml of copper-free amyl acetate and 5 ml of copper-free absolute methyl alcohol to each tube. Place the stop-cock on the funnel and shake for 30 seconds and then let it stand until the phases separate. Draw off~the lower aqueous phase completely and pour the coloured organic layer from the funnel into a small beaker. Add anhydrous sodium sulphate to the liquid until any cloudiness disappears. Stir and filter the dry organic phase through hard filter paper into a clean dry test-tube. For wines, red or white, use 10 ml and follow exactly the same procedure as for the standards. The amount of copper in the wine shall be approximately determined by visual com- parison.

11 DETERMINATION OF IRON

11.1 Reagents

11.1.1 Sulphuric Acid - concentrated.

11.1.2 Perchloric Acid - 70 percent.

11.1.3 Hydroxylamine Hydrochloride - 10 percent, aqueous.

11.1.4 Phenolphthalein Solution - in 50 percent alcohol, 0.1 percent.

11.1.5 Ammonium Hydroxide - concentrated.

11.1.6 Standard Stock Solution of Iron - 1 mg/ml.

11.2 Procedure

Pipette 2 ml of wine in 25 x 150-mm test-tubes previously marked at 10 ml. Evaporate to dryness, cool, and add 1 ml of sulphuric acid. Heat over a flame under a hood with care until the contents of the tube are completely liquefied. Allow to cool, and then add 0.5 ml of perchloric acid. Heat

6

IS 7585 : 1995

continuously until partial clarification has oc- tubes for comparison by photoelectric curred; set aside to cool; and~then again add.0.5 ml photometers. of perchloric acid. Continue the digestion until the sample is clear and until all the excess perchloric acid has been evaporated off. At this stage set the tubes aside to cool.

CAUTION : The digestion should be conducted behind a suitable shatterproof glass, because perchloric acid occasionally explodes during heating.

11.2.1 Add 2 ml of distilled water and a small piece (0.5 cm2) of congo red paper. Then add 1 ml of hydroxylamine hydrochloride and 1 ml of phenolphthalein. Titrate to the colour change (blue to a light red) of the congo red paper with concentrated ammonium hydroxide and set aside to cool. Then make up the volume to 10 ml with distilled water and transfer to standardized test-

11.2.2 Prepare a standard stock solution of iron to contain 1 mg iron per ml. Prepare from this stand- ard stock solution a series of solutions containing known concentrations of iron (in mg per litre of iron). Run these solutions in accordance with the procedure given above for the sample, using all the reagents and following directions closely. Transfer them ‘to standard diameter test-tubes and cork tightly for use as a series of standards. These stand- ards are stable for long period~and the procedure outlined automatically corrects for the iron in the reagents. In similar manner, the solutions can be used to establish a curve to be used with photoelectric calorimeter. In this case, however, a blank containing water instead of an iron solution but containing all the reagents shall be prepared. Use this blank to set the instrument to zero reading.

ANNEX A

IS No. 1070 : 1992

2302 : 1989

(Clause 2)

Title IS No.

Specification for reagent grade 3506 : 1989 water (second revision) Tables for alcoholometry by 3752: 1988 Hydrometer method Cfirst revision)

Title

Tables for alcoholometry (h) pyknometer method)

Alcoholicdrinks-Methodsoftest (first revision)

7

1s 7585 : 1995

ANNEX B

(CZmse 6.2)

SPECIFIC GRAVITY AND DEGREES PLATO OF WINE EXTRACT, PERCENT BY MASS

Specific

Gravity

at ZO/20°

g Extract in1OOg

Wine

Specific

Gravity

at 20120~

g Extract in1OOg

Wine

1 .ooooo 0.000 1.00250 42

0.5 13 55 55

10 26 60 68

15 39 65 80

20 52 70 93

25 64 75 .706

30 77 80 19

35 90 85 32

40 ,103 90 45

45 16 95 57

1.00050 29 1.00300 0.770

55 41 05 83

60 54 10 96

65 67 15 .808

70 80 20 21

75 93 25 34

80 ,206 30 47

85 19 35 59

90 31 40 72

95 44 4.5 85

1.00100 57 1.00350 98

05 70 55 ,911

10 83 60 24

15 96 65 37

20 .309 70 49

25 21 75 62

30 34 80 ~75

35 47 85 88

JO 60 90 1.001

45 73 95 14

1.00150 86 1.00400 26

55 98 05 39

60 .411 10 52

65 24 15 65

70 37 20 78

75 50 25 90

80 63 30 .103

85 76 35 16

90 88 40 29

95 .501 45 42

1.00200 14 1.00450 55

05 27 55 68

10 40 60 80

15 52 65 93

20 65 70 .206

25 78 75 19

30 91 80 32

35 .604 85 44

40 16 90 57

45 29 95 70

8

IS 7585 : 1995

Specific g Extract Specific g Extract Gravity in1OOg Gravity in 100 g

at 20/20 Wine at 20/20” Wine

1.00500 a3 1.00750 23

OS 96 55 3.5

10 ,308 60 48

15 21 65 61

20 34 70 73

25 47 75 86

30 60 80 99

35 72 85 2.012

40 85 90 25

45 98 95 38

1.005so .411 1.00800 53

55 24 05 65

00 37 10 78

65 50 15 91

70 62 20 ,101

75 75 25 14

80 88 30 27

85 .501 35 39

00 14 40 52

95 26 45 65

I .00600

05

IO

is

20

25

30

35

10

45

1.00650

55

60

65

70

75

80

85

90

95

1.00700

05

10

15

20

25

30

35

40

45

1.539 1.00850 78

52 55 91

65 60 ,203

78 65 16

90 70 29

,603 75 41

16 80 54

29 85 67

41 90 80

54 95 ,292

~61 1.00900 2.305

80 05 17

93 10 30

,705 15 43

18 20 56

31 25 69

44 30 81

57 35 94

69 40 .407

82 45 19

95 1.00950 32

.807 55 45

20 60 58

33 6.5 70

46 70 83

59 75 96

73 L 80 ,508

84 85 21

97 90 34

.910 95 47

9

lS7585:1995

Specific Gravity

at 20/20”

g Extract in 100 g

Wine

Specific Gravity

at 20/20”

g Extract inlOOg

Wine

1.01000 60 1.01250 94

05 72 55 ,207

10 85 60 19

15 98 65 32

20 .610 70 45

25 23 75 57

30 36 80 70

35 49 85 82

40 61 90 95

45 74 95 .308

1.01050

55

60

65

70

75

80

85

90

95

1.01100

OS

10

IS

20

2.5

30

35

10

45

I .(I1 I so 55

60

65

70

75

x0

85

90

05

87 1.01300 21

99 05 33

.I12 10 46

25 15 c’1

38 20 71

50 25 84

63 30 96

76 3.5 ,409

78 40 21

A01 45 34

14 1.01350 47

26 55 59

39 60 72

53 L. 65 85

64 70 97

77 7.5 SlO

90 80 23

.903 8.5 35

15 90 48

28 95 61

40 1.01400 73

53 05 86

66 10 98

79 15 .611

91 20 24

3.004 25 36

17 30 49

29 35 62

42 40 74

55 45 87

1.01200 3.067 1.01450 99

OS 80 55 ,712

10 93 60 25

15 ,105 6.5 37

20 18 70 50

2s 31 75 62

30 43 80 75

35 56 x5 88

-IO 69 90 .800

35 81 9.5 13

IS 7585 : 1995

Specific Gravity

at 20/20”

g Extract in 100 g

Wine

Specific Gravity

at 20/20”

g Extract in 100 g

Wine

1.01500 3.826 1.01750 54

05 38 55 67

10 51 60 79

15 63 65 92

20 76 70 ,505

25 88 75 17

30 .901 80 29

35 14 85 42

40 26 90 5.5

45 39 95 67

I.01550 51 1.01800 4.580

55 64 05 92

60 77 10 ,605

65 89 15 17

70 4.002 20 30

75 14 25 42

80 27 30 55

85 39 35 68

90 52 40 80

95 65 45 92

1.07 600 17 1.01850 .705

05 90 55 18

10 .I02 60 30

15 15 65 43

20 28 70 55

2s 40 75 68

30 53 80 80

35 65 85 92

40 78 90 .805

45 90 95 18

7.01650 ,203 1.01900 30

55 16 05 43

60 28 10 55

65 41 15 68

70 53 20 80

75 66 25 93

80 78 30 ,905

85 91 35 18

90 304 40 30

95 16 45 43

1.01700 29 1.01950 55

OS 41 55 68

10 54 60 80

15 66 65 93

20 79 70 5.006

25 91 15 18

30 ,404 80 30

35 17 85 43

_)(I 29 90 55

45 42 95 68

11

Specific Gravity

at 20/20”

g Extract in 100 g

Wine

Specific Gravity

at ZORO”

tg Extract in 100 g

Wine

I .02000 80 1.02250 ,704

05 93 55 16

10 .106 60 29

15 18 65 41

20 30 70 54

25 43 75 66

30 55 80 19

35 68 85 91

40 80 90 ,803

45 93 95 16

7.02050 20.5 1.02300 28

55 18 05 41

60 30 10 53

65 43 15 65

70 55 20 78

75 68 25 90

80 80 30 ,903

85 93 35 15

90 .305 40 28

95 18 45 40

1.02 100 5.330 1.02350 52

05 43 55 65

10 55 60 77

15 67 65 90

20 80 70 6.002

25 92 75 15

30 .405 80 27

35 18 85 39

-IO 30 90 52

45 43 95 64

J .02150 55 1.02400 6.077

55 67 05 89

60 80 10 .lOl

65 92 15 14

70 .505 20 26

75 17 25 39

80 30 30 51

85 42 35 63

90 55 40 76

95 67 45 88

1.02200 80 1.02450 .200

05 92 55 13

10 .605 60 25

15 17 65 38

20 29 70 50

25 42 75 63

30 54 80 75

35 67 85 87

40 79 90 ,300

45 92 95 12

2

IS 7585 : 1995

Specific Gravity

at 20/20”

g Extract inlOOg

Wine

Specific Gravity

at 20/20”

g Extract in1OOg

Wine

1.02500 25 1.02750 43

05 37 55 55

10 50 60 67

15 62 ~65 79

20 74 70 92

25 87 75 7.004

30 99 80 17

35 411 85 29

40 24 90 41

45 36 95 53

1.02550 49 1.02800 66

55 61 05 78

60 13 10 91

65 85 15 .103

70 98 20 15

75 ,510 25 27

80 23 30 40

85 35 35 52

90 47 40 64

95 60 45 77

1.02600 72 1.02850 89

05 84 55 .201

10 97 60 14

15 .609 65 26

20 21 70 38

25 34 7.5 51

30 46 80 63

35 59 85 75

40 71 90 87

45 83 95 .300

1.02650 96 1.02900 12

55 .708 05 24

60 20 10 37

65 33 15 49

70 45 20 61

75 57 25 74

80 70 30 86

85 82 35 98

90 94 40 .411

95 .807 45 23

1.02700 6.819 1.02950 35

05 31 55 47

10 44 60 60

15 56 65 72

20 68 70 84

25 81 75 97

30 93 80 ,509

35 .905 85 21

40 18 90 33

45 30 95 46

13

1s 7585 : 1995

Specific Gravity

at 20/20”

g Extract in1OOg

Wine

Specific Gravity

at 2Of20”

g Extract in1OOg

Wine

1.03000 1.558 1.03250 71

05 70 55 83

10 83 60 95

15 95 6.5 207

20 .607 10 20

25 19 7.5 32

30 32 80 44

35 44 85 56

40 56 90 69

45 68 95 81

1.03050 81 1.03300 8.293

55 93 05 30.5

60 ,705 10 17

65 17 15 30

70 30 20 42

75 42 25 54

80 54 30 66

85 67 35 18

90 19 40 91

95 91 45 .403

1.03100 .803 1.03350 15

05 16 55 21

10 28 60 39

15 40 65 52

20 53 10 64

25 65 75 76

30 71 80 88

35 89 85 .500

40 901 90 13

45 14 95 25

1.03150 26 1.03400 31

5s 38 05 49

60 50 10 61

65 63 15 14

70 15 20 86

75 87 25 98

80 8.000 30 ,610

85 12 35 22

90 24 40 34

95 36 45 47

1.03200 48 1.03450 59

05 61 55 11

10 13 60 83

15 85 65 95

20 98 70 .708

25 .llO 15 20

30 22 80 32

35 34 85 44

40 46 90 56

45 59 95 68

14

IS 7585 : 1995

Specific Gravity

at 20/20”

g Extract in1OOg

Wine

Specific Gravity

at 2Oi20

g Extract in1OOg

Wine

I .03500 81 1.03750 88

05 93 55 .400

10 .805 60 13

15 17 65 25

20 30 70 37

25 42 75 49

30 54 80 61

35 66 85 73

40 78 90 85

45 90 95 98

1.03550 .902 1.03800 .509

55 15 05 22

60 27 10 34

65 39 15 46

70 51 20 58

75 63 25 70

80 15 30 82

85 88 35 94

90 9.000 40 ,606

95 12 45 18

1.03600 9.024 I .03850 31

05 36 55 43

10 48 60 55

15 60 65 67

20 73 70 79

25 85 75 91

30 97 80 ,703

35 .109 85 15

40 21 90 27

45 33 95 40

1.03650 45 1.03900 9.751

55 58 05 64

60 70 10 76

65 82 15 88

70 94 20 .800

75 .206 25 12

80 18 30 24

85 30 35 36

90 43 40 48

95 55 45 60

1.03700 67 1.03950 73

05 79 55 85

10 91 60 97

15 .303 65 .909

20 16 70 21

25 28 75 33

30 40 80 45

35 52 85 57

40 64 90 69

45 76 95 81

15

IS 7585 : 1995

Specific g Extract Specific g Extract Gravity in1OOg Gravity in 100 g

at 20/20” Wine at 2Of20” Wine

I .04000 93 1.04250 96

05 10.005 55 .608

10 17 60 20

15 30 65 32

20 42 70 44

25 54 75 56

30 66 80 68

35 78 85 80

40 90 90 92

45 .102 95 .704

1.04050 14 1.04300 16

55 26 05 28

60 38 10 40

65 50 15 52

70 62 20 64

75 74 25 76

80 86 30 88

85 98 35 .800

90 .210 40 12

95 23 45 24

1.04100 34 1.04350 36

05 46 55 48

10 59 60 60

15 71 65 72

20 83 70 84

25 95 75 96

30 .307 80 ,908

35 19 85 20

40 31 90 32

45 43 95 44

1.04150 55 1.04400 56

55 61 05 68

60 79 10 80

65 91 15 92

IO .403 20 11.004

75 15 25 16

80 27 30 21

85 39 35 39

90 51 40 51

95 63 45 63

1.04200 10.475 1.04450 75

05 87 55 87

10 99 60 .lOO

15 .511 65 12

20 23 70 23

25 36 75 35

30 48 80 47

35 59 85 59

40 71 90 71

45 84 95 83

16

IS 7585 : 1995

Specific Gravity

il I 20/20”

g Extract in1OOg

Wine

Specific Gravity

at 20/20”

g Extract in1OOg

Wine

1.04500 11.195 1.04750 92

05 .207 55 .804

10 19 60 16

15 31 65 28

20 43 70 40

25 55 75 52

30 67 80 64

35 79 85 76

40 91 90 88

4s 303 95 900

1.04550 15 1.04800 11.912

5.5 27 05 23

60 39 10 35

65 51 15 47

IO 63 20 59

15 75 25 71

80 87 30 83

85 99 35 95

90 .411 40 12.007

95 23 45 19

I .0-IG00 35 1.04850 31

05 46 55 42

10 58 60 54

15 70 65 66

20 82 70 78

25 94 75 90

30 .506 80 .102

35 18 85 14

40 30 90 26

45 42 95 38

1 A)4650 54 1.04900 50

55 66 05 62

60 78 10 73

65 90 15 85

70 .602 20 97

75 14 25 .209

80 26 30 21

85 38 35 33

90 50 40 45

95 61 45 56

1.04700 73 1.04950 68

05 85 55 80

10 97 60 92

15 .709 65 304

20 21 70 16

25 33 75 28

30 45 80 40

35 57 85 51

40 68 90 63

45 80 95 75

17

IS 7585 : 1995

Specific Gravity

a 120/20”

g Extract in1OOg

Wine

spec1xc Gravity

at 2Of20”

g Extract in1OOg

Wine

1.05000 87 1.05250 79

05 99 55 91

10 .411 60 13.oQ3

15 23 65 15

20 35 70 27

25 47 75 39

30 58 80 50

35 70 85 62

40 82 90 74

45 94 95 86

1.05650 SO6 1.05300 98

55 18 05 .109

60 30 10 21

65 42 15 33

70 53 20 45

75 65 25 57

80 77 30 68

85 89 35 80

90 .601 40 92

95 13 45 .204

1.05100 12.624 1.05350 15

05 36 55 27

10 48 60 39

15 60 ‘65 51

20 12 70 63

25 84 75 74

30 95 80 86

35 .707 85 98

40 19 90 .310

45 31 95 22

1.05150 43 1.05400 13.333

55 55 05 45

60 67 10 57

65 78 15 69

70 90 20 80

75 .802 25 92

80 14 30 .404

85 26 35 16

90 38 40 28

95 49 45 39

l.OS200 61 1.05450 51

05 73 55 63

10 85 60 75

15 97 65 87

20 909 70 99

25 20 75 .510

30 32 80 22

35 44 85 34

40 56 90 46

45 68 95 57

18

IS 7585 : 1995

Specific Gravity

at 2Oi20”

g Extract in1OOg

Wine

Specific Gravity

at 20/20”

g Extract in 100 g

Wine

1.05500 69 1.05750 56

05 81 55 68

10 93 60 79

15 .604 65 91

20 16 70 .203

25 28 75 15

30 40 80 26

35 51 85 38

40 63 90 50

45 75 95 61

1.05550 87 1.05800 * 73

55 98 05 85

60 ,710 10 97

65 22 15 308

70 34 20 20

75 46 25 32

80 57 30 43

85 69 35 55

90 81 40 61

95 92 45 79

1.05600 .804 1.05850 90

05 16 55 .402

10 28 60 14

15 39 65 25

20 51 70 37

25 63 75 49

30 15 80 60

35 86 85 72

40 98 90 84

45 .910 95 95

1.05650 21 1.05900 .507

55 33 05 19

60 45 10 31

65 51 15 42

70 68 20 54

15 80 25 65

80 92 30 71

85 14.004 35 89

90 15 40 ,601

95 27 45 12

1.05700 14.039 1.05950 24

05 51 55 36

10 62 60 47

15 14 65 59

20 86 70 71

25 91 75 82

30 JO9 80 94

35 21 85 .706

40 33 90 17

45 -44 95 29

19

IS 7585 : 1995

Specific Gravity

at 2Oi20”

g Extract in1OOg

Wine

Specific Gravity

at 24V2.0’

g Extract in1OOg

Wine

1.06000 14.741 1.06250 23

05 52 55 34

10 64 60 46

15 76 65 58

20 87 70 69

25 .?I9 75 81

30 .811 80 93

3.5 22 85 A04

40 34 90 16

45 46 95 27

1.06050 57 1.06300 39

55 69 05 51

60 81 10 62

65 92 15 74

70 904 20 86

75 16 25 97

80 27 30 .509

85 39 35 20

90 50 40 32

95 62 45 44

1.06100 74 1.06350 55

05 86 55 67

10 97 60 78

15 15.009 65 90

20 20 70 602

25 32 7.5 13

30 44 80 25

35 55 85 37

40 ~67 90 48

45 79 95 60

1.06150 90 1.06400 15.671

55 .102 05 83

60 14 10 94

65 25 15 .706

70 37 20 17

75 48 25 29

80 60 30 41

85 72 35 52

90 83 40 64

95 95 45 76

1.06200 15.207 1.06450 87

05 18 55 !I9

10 30 60 .810

I5 41 65 22

20 53 70 33

25 65 75 45

30 76 80 57

35 88 85 68

40 300 90 80

35 11 95 91

20

IS 7585 : 1YY5

Specific g Extract Specific g Extract Gravity in 100 g Gravity in 100 g

at 20/20” Wine at 20RO” Wine

1.06500

05

10

15

20

25

30

35

40

45

1.06550

55

GO

65

70

75

80

85

90

95

.903 1.06750 80

14 55 91

26 60 SO3

38 65 14

49 70 26

61 75 37

72 80 49

84 85 61

95 90 72

16.007 95 83

19 1.06800

30 05

41 10

53 15

65 20

76 25

88 30

99 35

,111 40

22 45

16.595

18

30

41

52

64

76

87

99

I .MhOO lb.134 1.06850 .710

OS 45 5.5 22

10 s7 60 33

1s 69 65 44

20 80 70 56

25 91 75 68

30 ,203 80 79

35 15 85 91

JO 26 90 ,802

15 38 95 13

I .06f150 49 1.06900 2s

55 61 0.5 36

60 77 /.. 10 48

65 85 15 59

70 95 20 71

7s ,307 25 82

80 19 30 94

85 30 35 .!I05

90 41 40 17

05 53 45 28

I .OhiOO 65 1.06950 40

05 76 55 51

10 88 60 63

15 99 65 74

20 ,311 70 86

25 22 75 97

30 34 80 17.009

3s 4.5 85 20

40 57 90 32

-15 68 95 43

21

Bureau of Indian Standards

BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promote harmonious development of the activities of-standardization, marking and quality certification of goods and attending to connected matters in the country.

Copyright

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Review of Indian Standards

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

This Indian Standard has been developed from.Doc : No. FAD014 ( 0014 ).

Amendments IssuedSince Publication

Amend No. Date of Issue Text Affected

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