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IS 170: Acetone PDF

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इंटरनेट मानक 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. “जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न’ 5 तरफ” Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru “The Right to Information, The Right to Live” “Step Out From the Old to the New” IS 170 (2004): Acetone [PCD 9: Organic Chemicals Alcohols and Allied Products and Dye Intermediates] “!ान $ एक न’ भारत का +नम-ण” Satyanarayan Gangaram Pitroda ““IInnvveenntt aa NNeeww IInnddiiaa UUssiinngg KKnnoowwlleeddggee”” “!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै” Bhartṛhari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 170:2004 w-?G%7%’=i’@ QTf)-a=l Mm ‘- ( ak-ny7T%-F)l Indian Standard ACETONE — SPECIFICATION (Fourth Revision) ICS 71.080.80 (0 [31s2004 BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARC NEW DELHI I10002 ,\olY/?l/5@r2004” Price Group 4 AIcoI1o1s and Allied Products Sectional Committee, PCD 10 FOREWORD This Indian Standard (Fourth Revision) was adopted by the Bureau of Indian Standards, after the draft tinalized by the Alcohols and Allied Products Sectional Committee had been approved by the Petroleum, Coal and Related [’roducts Division council. This standard was first issued in 1950 and subsequently revised in 1966, 1976 and 1986. At the time of tirst revision, acomparative study ofthe standard with the drafi 1S0 Recommendation No. 656 ‘Sampling and methods of test for acetone’ was undertaken. A revised scheme of sampling and criteria for conformity, a new procedure for determination of alcoholic impurities, retlnement in the test for alkalinity and additional requirement for water content were included in the revised standard. As a result of experience gained through the use of first, scconct and third revisions and in order to meet the present day requirements of acetone, the fourth revision was undertaken, In this version requirements of purity and permanganate time have been incorporated using CC method for verification of purity. Requircinent of residue on evaporation has been modified. Acctonc is an important commercial solvent and raw material with awide usage inthe chemical, explosives and lacquer industry. It iscommonly used as asolvent for cellulose acetate; nitrocellulose; celluloid; cellulose ether; chlorinated rubber; various resins, fats and oils; and as an absorbent for acetylene. Itisbeing increasingly used in the synthesis of a number of chemicals such as diacetone alcohol, methyl isobutyl ketone, phorone, isophorone, methyl methocrylate and certain resins, pharmaceuticals and perfumes. For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with IS2: 1960 ‘Rules for rounding off numerical values (revised’. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard. 1S 170:2004 Indian Standard ACETONE — SPECIFICATION (Fourth Revision) I SCOPE 3.2 Miscibility with Water ‘Hlis sktndard prescribes the requirements, methods of The material shall show no turbidity on mixing with sampling and test for acetone intended for industrial distilled water in any proportion at 27 + 2“C. purposes, 3.3 The material shall also comply with the requirements given inTable 1. 2 REFERENCES ‘fhc following standards contain provisions, which 4 PACKING AND MARKING ihrough reference inthis text constitute the provisions 4.1 Packing otthis standard. At the time of publication, the editions indicated were valid. All standards are subject to The material shall be supplied in sound and clean wvision and parties to agreements based on this containers according to the marking and delivery standard are encouraged to investigate the possibility instructions given by the purchaser. of applying the most recent editions of the standards indicated below 4.2 Marking 1,7N(). Title Each container shall be marked legibly and indelibly with the following information: 82: 1992 Method of sampling and test for thinners and solvent for paints (firs~ a) Name of the material; revision) b) Manufacturer’s name; ~~() : ]964 Potassium bichromate, technical and c) Net, gross and tare mass; analytical reagent (revi.sw’) d) Recognized trade-mark, if any; and I070”: I992 Reagent grade water ([bird revi.sim) 1~60 Pictorial marking for handling and e) Date of packing. (Parl 1):1973 Iabelling ofgoods: Part 1Dangerous 4.2.1 Each container shall also be marked with the goods (first revision) minimum cautionary notice worded as’ FLAMMABLE’. 1448 Methods oftest f or petroleum and its [r: 8] :1991 products: [P :18]Di stillation (second 4.2.1.1 Itshall also bear the corresponding symbol for revision) labe]ling of dangerous goods [see Fig. 5 of 1S 1260 ~~63 1979 Methods of preparation of indicator (Part 1)]. solutions (first revisio~) NOTES 2362 993 Determ ination of water by the Karl 1 Necessary safeguards against the risk arising ~ronlstorage Fischer method (second revision) and handling of large volumes of flammable liquids shall bc 4~~5 : 982 Specification for liquid-in-glass provided and all dueprecautions shall betaken atall iimcs to solid-stem reference thermometers prevent accidents by tire orexplosion (see IS 7445). (jirsl revision) 2 Except when they are opened for the porposc of cleaning andrendering them free from acetone vapour, all empty tanks 4905: 968 Methods for random sampling or other containers shall be kept securely closed unless they 7445: 974 Code of safety for acetone have been cleaned and free from acetone vapour. 8768:2000” Method of measurement ofcolour in 4.2.2 BIS Certljlcation Marking liquid chemical products piatinum- cobalt scale (second revision) The containers may also be marked with the BIS Certification Mark. 3 REQUIREMENTS 4.2.2.1 The use of the Standard Mark isgoverned by 3.I Description the provisions ofBureau oflndian Standards Ac{, 1986 “1’hcmaterial shall be clear and free from any suspended and the Rules and Regulations made thereunder. The matter. It shall consist essentially of 2-propanone or details of conditions under which the Iicence for dimcthylketone (CI I~COCEl,). the use of the Standard Mark may be granted to I IS 170:2004 Table 1 Requirements for Acetone (Ckwse 3.3) SI Characteristic Rcquimment Method r)f’lest, Rcfto Nu. Annex Imlian Slandard (1) (2) (3) (4) (5) o Purity, percxmtbymass,Afirr 99 A 11) Colour, [W-COscale, ,Max I() X768 !11) Rcialive density. at27/27°C (1784 to(1786 — 6ofls x2 Iv) [)s~lllotlon range Tlwd]l’t’erencebetween initial boiling Method B in [P IX] ofl S point ([131))and dry point (DP) shall 1448 with thethcrnlomctcr not exceed I“C including 56.1‘C confbrnlIng 10 the (tcnlpcrature being corrected’] for a rcquircmcnts given in pressureof 760 Inm Ilg) Annex 1301’thisstandard W’atcrcontcnl, percent bymass,Max 04 IS2362 Rmidue oncvapomtion, mg/100 ml, 5 8ofls x2 Max \ll) Ac!dity (asCII,CC3011), g/100 ml, ()002 c — Al[lx viii) Alkalinity ‘t-opasstheIcst D lx) Pcrmanganale Lest,minutcsj A4fit2 30 1; x) Alcoholic impurities “1’0passthetest F 1)111~ttsethe barollleter prcsstlre, ~, deviates from 760 mm I{g, uscthe correction 0.037 (p -760)”C [Ordistillation tclnpcraturc manufacturers or producers may be obtained from the Mean, Y z sum oftest results divided by number Bureau of Indian Standards. of test results so added, and 5 SAMPLING Range, R = difference between maximum and 5.1 The method ofdrawing representative samples shall minimum values of test results. be as prescribed in Annex G. The expressions (~– 0.6 R) and (j + 0.6 R) shall 5.2 Number of Tests then be calculated. The lot shall be considered to conform in respect of the relevant characteristics, if 5.2.1 Individual Samples (X + 0.6 R) is less than the maximum specified value Tests for distillation range and any other characteristic, and (~ – 0.6 R) isgreater than the minimum specitied ifso agreed to between the parties, shall be carried out value. When the sample size isten, the test results shall individually on each of the test satnples in a set as begrouped into two, each constituting five tests results, prepared in G-4.1. taking them consecutively in the same order as 5.2.2 Cotnposite Samples obtained. For each group, the range shall be calculated and the mean range ~ shall be calculated by dividing Tests for determination of remaining characteristics the sum of the ranges by two. In the expression of this standard shall be carried out on the composite sample as prepared in G-4.2. (~+ 0.6 ~), Rshall be replaced by ~ 5.3 Criteria of Conformity 6 TEST METHODS S.3. 1For Composite Samples 6.1 Tests shall be conducted as prescribed in COI4 and 5 of Table 1. The lotshallbedeclared asconforming totherequirements of this standard, if each of the test results on the 6.2 Quality of Reagents composite sample according to 5.2.2 satisfies the corresponding requirements of this standard. Unless specified otherwise, pure chetnicals and distilled water (see 1S 1070) shall be employed in tests. 5.3.2 For each of the characteristics tested on the individual samples according to 5.2.1, the mean and NOTE — ‘Pure chemicals’ shall mean chemicals that do not the range of test results shall be calculated as below: contain impurities, which affect the results of analysis. L-1 IS 170:2004 ANNEX A [Table 1,S1No. (i)] METHOD FOR DETERMINATION OF PURITY A-1 GENERAL recorder deflection for a 0.1 percent concentration of purity atthe most sensitive setting of instrument. Allow This test method isrelated to determination ofthe purity sufficient time for the instrument to reach equilibrium of acetone by gas chromatography and in addition, as indicated by stable base line. Adjust carrier gas flow provides a means for identification of certain known rate to a constant value. impurities. A-2. 1.2.1 Identification A-2 APPARATUS Determine the retention time of each component by A-2.1 Gas Chromatography injecting small amount either separately or in known mixture. Any gas liquid chromatography equipped with TCD detector can be used with following accessories and A-2. 1.2.2 Calibration and standardization operating conditions: The response of any given detector varies from one Colllmn : Chromosorb 101 chemical to another. Therefore, calibration is must. Mesh size : 80/100 Calibration allows the computation of response f:tctor which express the relative response of different Column length : 3 m components to the detector. I.D. : 3 mm Calibration standard is prepared containing the Column tubing : Stainless steel (tubing must be impurities present in acetone. During standard material non-reactive with substrate, preparation the exact amounts of all the components sample and carrier gas) is noted. Inject 0.2 p] of calibration standard in the Carrier gas : Hydrogen (Purity — 99.99 mole chromatographic column in accordance with the percent, Mirr) specified conditions. Syringe : 10microlitre Calculate response factor to four decimal places for Sample size : 0.2 microlitre all components relative to acetone using following Electronic : For computation of results equation: integration WXXAA4 A-2. 1.1 lnstrurnent Condition R~ = AXXW&t Detector : TCD where Oven temperature : llo”c R~ = response factor for component x relative Injector, temperature : 280”C to acetone; Detector, temperature : 200°C W, = weight of component x, in the calibration Carrier gas flow rate : HO,30 ml/min standard; NtYfES AX = area ofcompcanentx, inthe calibration run: 1 ‘ICI) is prct’erred for acetone purity and impurities along WL4= weight ofacetone inthecalibration standard; with moisture content because moisture estimated by Karl and Fischer isnot applicable to acetone, 2 Tbe above gaschromatographic conditions are suggestive. AM = area of acetone in the calibration standard llowcver, any GC with different column may be used run,which isselected asreference component. provided standardization/cali bration are done after setting up chromatographic conditions for the required resolution. The component which is unknown in the sample is A-2.1.2 ldentlfication, Calibration and Standardization assigned the relative response factor 1.000 0. It is advisable that the determination of response factors Install the column in the chromatography. Set the be made on the basis of duplicate analysis. conditions given above, of column temperature and carrier gas flow that gives the necessary resolution of Response factor should be re-checked after any the components inthe sample being analyzed. Set the perceptible change in column or instruments conditions as such which gives aminimum 10percent performance. 3 IS 170:2004 A-3 PROCEDURE RX = peak response of compound x; and Inject 0.2 pl of sample into the chromatographic ~ = relative response factor of colmpound column, using the same conditions as for components x; and idcntification and standardization. Record and integrate Rxx~ = sum of the individual component peak the chromato:ram using appropriate attenuation setting responses (RX) multiplied by their that provide optilnum peak heights. Measure the area relative response factors ~,). of ail the peaks. A-5 PRECIS1ON AND BIAS A-4 CALCULATION A-5.1 Repeatability Calculate the concentrations of sample components using the following equation: Two results, shouid be considered suspect ifthey differ by more than 0.0006. <X,percent =~x100 A-5.2 Reproducibility R, x,fx whcre Two results should beconsidered suspect, ifthey differ (’\ = compound x, weight, percent; by more than 0.0027. ANNEX B [Table 1,S’1No. (iv)] REQUIREMENTS FOR “rHETHERMOMETER B-1 THERMOMETER Outer diameter of stem 6.0 to 7.0 mm Buib: B-1.1 “Wermorneter (Schedule Mark 22 of IS 4825) wi(h the following requirements shall be used: a) Length 15to20 mm b) Outer diameter Not greater than Range : 48 to I02°C that of stem Immersion : 100 mm Scale location: Distance Graduations: a) Bottom of bulb to 125 to 145 mm I) Subdivisions : 0.2°C line at 48°C 2) Long lines at each : 1°C b) Bottom of bulb to 335 to 360 mm 3) Number at each : 2°c line at 102°C Scale error, Max : o.2°c B-1.l. 1Any other thermometer of similar range and Tots iIcngth : 395 + 5 mm accuracy may also be used. IS 170:2004” ANNEX C [Table 1,S1 No. (vii)] TEST FOR ACIDITY C-1 REAGENTS phenolphthalein indicator and examine for alkalinity; C-1.1 Phenolphthalein Indicator — prepared by ifnot alkaline, titrate with standard sodium hydroxide dissolving 0.1 g of pbenolphthalein in 100 ml of 60 solution using a microburette. pm-cent ethyl alcohol. C-3 CALCULATION C-1.2 Standard Sodium Hydroxide Solution –-0.OIN. 6VN Acidity (as CH~COOH), percent by Imass= ~ C-2 PROCEDURE C-2.1 Fill 100 ml of water and put a few pieces of where clean porous porcelain ina500-ml conical flask (non- V = volume, inml, of standard sodium hydroxide a]kalinc glass) and boil gently for 5 min to eliminate solution; carbon dioxide. Cool slightly and add 100 ml of the N = normality of standard sodium hydroxide material. Boil gently for a further period of 5 min. At solution; and the end of this period, close the neck of the flask with a stopper carrying a sodalime tube, allow to cool. D = relative density of the material at the When cool, remove the stopper, add 0.5 ml of temperature of determ ination. ANNEX D [Table 1,S/ No. (viii)] TEST FOR ALKALINITY D-1 REAGENTS glass). Add 2 drops (approximately 0.1 ml) of D-1.1 Hydrochloric Acid — approximately 0.02N by bromothymol blue indicator solution. Adjust to the volume. neutral colour of the indicator by adding hydrochloric acid or sodium hydroxide solution as necessary. D-1.2Sodium Hydroxide Solution — approximately Transfer 100 ml of the neutralized water to each of 0.02N. two 250-ml cylinders. To one of these, add 100 ml of D-1.3 Bromothymol Blue Indicator Solution — the sample and shake well. Compare the colour oftbe prepared by dissolving 0.1 g of bromothymol blue sample with that ofthe blank, viewing both downward in 100 ml of 50 percent rectitied spirit (see 1S2263). to compensate for dilution. D-2 PROCEDURE D-2.2 The material shall be considered to have passed D-2.1 l’ake 200 ml of freshly boiled and cooled the test, ifno change ofcolour towards blue, indicating distilled water in a 500-ml conical flask (non-alkaline the presence of alkalinity, takes place. 5

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