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Limit test sudip modh


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Limit test sudip modh

  1. 1. Continued………Seminar on Presented by Sudip Kumar C. modh PA/2010/11
  2. 2. 2 Introduction Why limit test???? inorganic impurities are toxic at low levels, and these impurities should be monitored to ensure safety  Sources of inorganic impurities include those that are deliberately added to the process (e.g., catalysts), undetected contaminants from starting materials or reagents leaching from pipes and other equipment from naturally derived plant or mineral sources the level of each inorganic impurity should not exceed the limit defined in or otherwise specified in the individual monograph.SUDIP KUMAR
  3. 3. 3 ICH Q3A Impurities in Drug Substances guidance, impurities are classified as organic, inorganic, and residual solvents Classification of metal impurities…...SUDIP KUMAR
  4. 4. WHAT TO BE DISCUSSED……… 4 Limit test of heavy metals Limit test for Iron Limit test of sulphated ash Limit test for total ash  Total Organic Carbon Limit test of N,N- Dimethylaniline Limit Test for Fluorides Cadmium, copper, iron, lead, nickel and zinc Limit test for selenium Limit Test for Magnesium Limit test of arsenic and mercurySUDIP KUMAR
  5. 5. 5 Limit test of heavy metals: ( 2.3.13.) IP (GENERAL NOTICES) Tests with numerical limits and assays, quantity stated to be taken for testing is approximate amount actually used, which may deviate by not more than 10 per cent from that stated, is accurately weighed or measured result of analysis is calculated from this exact quantity.. In tests where the limit is not numerical but usually depends upon comparison with the behaviour of a reference in the same conditions, the stated quantity is taken for testing. Reagents are used in the prescribed amounts.SUDIP KUMAR
  6. 6. 6 Limit test of heavy metals: IP ( 2.3.13.) Limit for heavy metals is indicated in in terms of ppm, i.e., the parts of lead, Pb, per million parts (by weight) of the substance under examination Lead Nitrate Stock Solution: 0.1598 g of lead nitrate in (100 ml of water +1 ml of nitric acid) dilute to 1000 ml with water Lead Standard Solution: Dilute 10 ml of lead nitrate stock solution with water to 100 ml Each mL of Standard Lead Solution contains ≡ 10 µg of leadSUDIP KUMAR
  7. 7. 7 Limit test of heavy metals: USP <231>  metallic impurities tare colored by sulfide ion, under specified test conditions, not exceed limit specified in the individual monograph as a percentage (by weight) of lead in test substance  Determination by concomitant visual comparison with control (Standard Lead Solution)# Determine the amount of heavy metals by Method I, unless otherwise specified in the individual monograph . Types of methods Nature of substances Method I that yield clear, colourless preparations Method II do not yield under test conditions for Method I, or form complex , interfere with precipitation by sulfide ion, or for fixed and volatile oilsMethod III wet-digestion method, when Method I nor Method II can be used #[note—Substances that typically will respond to this test are lead, mercury, bismuth, arsenic, antimony, tin, cadmium, silver, copper, and molybdenum.]SUDIP KUMAR
  8. 8. 8 USP <231> Monitor Preparation Test Preparation +2.0 mL of Standard Lead Solution Lead Nitrate Stock Solution Standard Lead Solution as per IP Limit test of heavy metals: BP (Ph. Eur. method 2.4.8) Lead Nitrate Stock Solution Standard Lead Solution as per IP Blank solution: 10 ml of water R and 2 ml of the test solution Methods Developed By Thioacetamide Reagent R Sodium Sulphide Solution R1 (0.1 Ml) as Alternative If Sodium Sulphide Solution R1 Is Used Instead, To Be Include For Methods A And B Monitor solution Same quantity prescribed for the test + volume of lead standard solution prescribed for preparation of the reference solution Apparatus for limit test of heavy metals: spots on the filters obtained with the different solutionsSUDIP KUMAR
  9. 9. 9 Limit test of heavy metals: BP (Ph. Eur. method 2.4.8) Apparatus for limit test of heavy metalsSUDIP KUMAR
  10. 10. IP BP USP 10Method A Method A Method IStandard solution: Reference solution Standard PreparationInto a 50-ml Nessler cylinder (standard) A mixture of 10 Into a 50-mL colour- ml of lead standard solution comparison tube (1 ppm Pb or 2 ppm Pb) R,pipette 1.0 ml of lead std as prescribed, and 2 ml ofsolution (20 ppm Pb)dilute prescribed aqueous solution pipette 2 mL of Std Leadwith water to 25 ml of substance to be examined Solution (20 µg of Pb), and dilute with water to 25 mlAdjust with dilute acetic acid(1 N CH3COOH) or dilute adjust with 1 N acetic acid orammonia solution (10 per 6 N ammonium hydroxide tocent w/w of NH3) to pH a pH between 3.0 and 4.0,between 3.0 and 4.0, dilute dilute with water to 40 mL,with water to 35 ml and mix. and mix pH meter or short-range pH indicator paper as external indicator,SUDIP KUMAR
  11. 11. IP Method A BP Method A USP Method I 11Test solution: Test solution: Test Preparation:In 50-ml Nessler cylinder 12 ml of the prescribed In 50-mL color-comparisonplace 25 ml of Solution for aqueous solution of the tube, place 25 mL of thetest or dissolve specified substance to be examined solution prepared for the testquantity of test substance in or, using the designatedsufficient water to produce volume of acid where25 ml specified in the individual monograph, dissolve in andAdjust with dilute acetic acid dilute with water to 25 mL*or dilute ammonia solution to pH is adjusted with 1 Na pH acetic acid or 6 N ammoniumbetween 3.0 and 4.0, hydroxide to a pH betweendilute with water to about 35 3.0 and 4.0,ml and mix dilute with water to 40mL, and mix. *g, of the substance to be tested, as calculated by the formula: 2.0/(1000L)SUDIP KUMAR in which L is the Heavy metals limit, as a percentage.
  12. 12. IP Method A BP Method A USP Method I 12Procedure; Procedure; Procedure:To each of the cylinders As per usp To each of the three tubes1 standard Solution containing the2 test solution 1 Standard Preparation 2 Test Preparation 3 Monitor Preparationadd 10 ml of freshly preparedH2S solution, mix, 2 mL of pH 3.5 Acetate Buffer,dilute to 50 ml with water, then add 1.2 mL ofallow to stand for 5 minutes thioacetamide–glycerin baseand view downwards over TS,white surface; Dilute with water to 50 mL, Brown colour wait for 2 minutes, and viewcolour produced with the test over white surfacesolution is not more intensethan that produced with the colour of Test is not darkerstandard solution than Standard Monitor is equal to or darkerSUDIP KUMAR than Standard Preparation
  13. 13. IP BP USP 13Method B Method B Method II Standard solution:* Standard Preparation*Standard solution:* Test solution: Test Preparation:Test solution: As per method ATest (crucible) +H2SO4 ignite at low temp+ (2ml HNO3 + 5 drops H2SO4) white fumesIgnite,(muffle furnace)(500°-600°)to burnt offcarbon +4 ml HCl cover, digest(water- Steam bathbath) for 15 mins, uncover & evaporate , Moistenwith (1 drop H2SO4 +10 ml hot water) ammonium hydroxidedigest for 2 min + NH4 solutiondropwise alkaline to litmuspaperdilute to 25 ml & adjust pH between 3.0 and 4.0by dilute CH3COOH ,Filter rinse crucible & filter 40 mlwith 10 ml water, combine in 50-ml Nesslercylinder, dilute to 35 ml and mix *process is same as method A /method ISUDIP KUMAR
  14. 14. IP BP USP 14Procedure* Procedure* Procedure*Method C Method C Method IIIStandard solution Standard solution Standard solutionInto a 50-ml Nessler cylinder 10 ml of the solution + add 2pipette 1.0 ml of lead ml of the test solutionstandard solution (20 ppmPb), add 5 ml dilutesodium hydroxide solution,dilute with water to 50 mland mix *process is same as method A /method ISUDIP KUMAR
  15. 15. USP Method III 15Standard solution Transfer(8 mL H2SO4+10 mL HNO3) clean, dry, 100-mL Kjeldahl flask add more nitric acid = incremental volume of HNO3 added to Test Preparation dense, white fumescool,add 10 mL of water; if hydrogen peroxide was used in treating Test Preparation, add volume of 30% hydrogenperoxide = that used for substance being tested. Boil dense, white fumes. cool, +5 mL water, mix, boil dense, white fumes Cool, dilute ,+ 2.0 mL of Standard Lead Solution (20 µg of Pb), and mix. 50-mL colour-comparison tube, rinse to volume is 25 mL, and mixSUDIP KUMAR
  16. 16. IP Method C BP Method C USP Method III 16Test solution. Test solution. Test solution: Sample (silica crucible) with 4 ml50-ml Nessler cylinder of 250 g/l solution of MgSO4 Rplace 25 ml test solution or in H2SO4 R. Mixdissolve specified quantity ofsubstance white or at most greyish residue ≤ 800 °C(20 ml H2O + 5 ml of dilute Moisten with dilute H2SO4R.NaOH) ignition < 2 hDilute to 50 mland mix. 5ml HCl + phenolphthalein +conc NH3 pink colour + glacial acetic acid decolorized + 0.5 ml Filter & wash Dilute to 20 ml with water R.SUDIP KUMAR
  17. 17. USP Method III 17Test Preparation: (wet-digestion method) If solid substance— weighed quantity 100-mL( Kjeldahl flask)at 45 angle + 8 mLH2SO4 and 10 mL of HNO3 to moisten it boil until solution darkens.+2 mL HNO3+ nitric acid (no darkening occurs) to dense, white fumes.+ 5 mL water dense, white fumes & reduce volumeAdd water examine colour of solution.If color is yellow, +1 mL of 30 % hydrogen peroxide, dense, white fumes & volume of 2to 3 mL.still yellow, repeat 5 mL of water & peroxide treatment.Cool, dilute cautiously with few mL of water, and rinse into a 50-mL colour-comparison tube,volume shouldn‘t be exceed 25 mL.SUDIP KUMAR
  18. 18. IP BP USP 18Procedure. Procedure. Procedure—similar to that of method A similar to that of method A Similar to that of method IMethod D Method D USP contains only 3 methodsStandard solution. Standard solution. As perInto a small Nessler cylinder Method A(drying is done)pipette 10.0 ml of either leadstandard solution (1 ppm Pb)or lead standard solution (2 Monitor solution:As perppm Pb) Method A(drying is done)Test solution. Test solutionPrepare as directed in the As per method Cindividual monographand pipette 12 ml into a 0.5 g of magnesium oxidesmall Nessler cylinder R1. is used instead of MgSO4. R in H2SO4 RSUDIP KUMAR .
  19. 19. IP BP USP 19Procedure. Method D Procedure. Method Dstandard solution+ similar to that of method A 2.0 ml of test solution Method E+2 ml of acetate buffer pH 3.5, mix,+1.2 ml of thioacetamide reagent Test solution: prescribed quantity of test 2 mins substance In 30 ml of water R or prescribed volume. view downwards over white surface;colour produced with test solution is Standard solution.not more intense than that produced lead standard solution (1 ppmwith standard solution Pb) R to the same volume as the test solution Procedure: Apparatus for limit test of heavy metals is usedSUDIP KUMAR
  20. 20. BP 20Method FTest solution:As per USP Method IIIAdjust pH 3.0-4.0 with conc NH3 R1 (dilute may be used) if desired, dilute to 40 ml and mix.+ 2 ml of buffer solution pH 3.5 R. Mix and add to 1.2 ml of thioacetamide reagent Dilute to 50 ml with water R and mix Standard solution. Prepare at the same time and in the same manner as the testsolution, using the prescribed volume of lead standard solution (10 ppm Pb) R. Monitor solution Prepare as described for the test solution, adding test substance tolead standard solution (10 ppm Pb) R prescribed for the preparation of the referencesolution. Blank solution Prepare as described for the test solution, omitting the substance to beexamined.SUDIP KUMAR
  21. 21. BP 21Procedure. (Method F )Examine vertically against white background.brown colour in the test solution is not more intense than reference solution. Test is in valid…. if reference solution does not show a brown colour compared blank solution orif monitor solution is not at least as intense as the reference solutionMethod G(Based on high-pressure digestion method)Test solution Place test substance (not more than 0.5 g) in a suitable, clean beaker.+ 2.7 ml H2SO4 R + 3.3 ml HNO3 R + 2.0 ml of strong H2O2 R using a magnetic stirrer.Allow to react dry high-pressure-resistant digestion vessel (fluoropolymer orquartz glass).SUDIP KUMAR
  22. 22. BP (Method G ) 22Standard solution.Monitor solution as per method FBlank solutionProcedure:it includes use of both high-pressure-resistant digestion vessel and Apparatus for limit test ofheavy metalsLimit Test for Heavy Metals in Herbal Drugs and Fatty Oils (Ph. Eur. method 2.4.27)Examine by atomic absorption spectrometry (2.2.23)SUDIP KUMAR
  23. 23. 23Limit test for IronPrinciple:Fe2+ React in an ammoniacal solution with thioglycollic acidPink to dip reddish purple coloured complex of iron ThioglycollateFe(SCH2COOH)2Ferric ammonium sulphate ,FeNH4(SO4)2:12H2O,as standardStability of complexAir oxidationThioglycollate reduce Fe3+ to Fe2+20% citric acid to remove interferenceSUDIP KUMAR
  24. 24. 24Limit test for Iron: IP BP USPIron Standard Solution (20 ppm Fe): Same as IPDilute 1 ml 0.1726 % w/v solution of ferric USP uses ammoniumammonium sulphate in 0.05 M H2SO4 to 10volumes with water. Contains iron in ferric thiocyanatestateProcedure.Dissolve test or prepare as directed inmonograph, in Nessler cylinder. + 2 ml 20 %w/v of iron-free citric acid + 0.1 ml ofthioglycollic acid, mix, make alkaline with iron-free NH3 solution, dilute to 50 ml,pink colour is not more intense than that of2.0 ml of iron standard solution (20 ppm Fe)in place of solution under examinationSUDIP KUMAR
  25. 25. IP Limit test of sulphated ash 252.3.18. Sulphated ashHeat silica or platinum crucible to redness for 10 minutesCool(desiccator) weigh itAs per individual monograph, transfer to crucible 1 g of test substance under & weigh thecrucibleIgnite, to charring Cool, moisten the residue with 1 ml of H2SO4, white fumes no longer evolvedand ignite at 800º ± 25º black particles disappeared.Ignition without air currents.+ drops of H2SO4 and heatRepeat the operation until two successiveweightings do not differ by more than 0.5 mg.SUDIP KUMAR
  26. 26. EP Limit test of sulphated ash 26Ignite a suitable crucible (silica or platinum )at 600° ± 50° C for 30 min,allow to cool in a desiccator over silica gel and weigh.Place in crucible and weigh. Moisten with 1 ml of H2SO4 ,heat gently at as low temp until the sample is moisten with H2SO4 , heat gently until white fumes are no longer evolvedignite at 600° ± 50° C until residue is completely incineratedEnsure that flames are not produced at any time during the procedure.Allow the crucible to cool over silica gel, weigh it againIf mass of the residue so obtained exceeds the prescribed limit, repeat the moistening withH2SO4 and ignite to constant mass.SUDIP KUMAR
  27. 27. 27ICH guideline:Q4B - ANNEX IREGULATORY ACCEPTANCE OF ANALYTICAL PROCEDURES AND/ORACCEPTANCE CRITERIA (RAAPAC)ONRESIDUE ON IGNITION/SULPHATED ASH GENERAL CHAPTERANALYTICAL PROCEDURES AND/OR ACCEPTANCE CRITERIA (APAC)Defination:―The Residue on Ignition/ Sulphated Ash Test is a method to measure the amount of residualsubstance not volatilized from a sample when the sample is ignited in the presence ofsulfuric acid, This test is usually used for determining the content of inorganic impurities inan organic Substance.‖Procedure given is similar to that of EP:SUDIP KUMAR
  28. 28. IP Limit test for total ash: 28Total AshMethod A. For crude vegetable drugs 2 to 3 g of air-dried drug in tarred platinum or silica dish and incinerate at a 450ºCuntil free from carbon, cool and weigh If carbon-free ash is not obtained, wash charred mass with hot water, collect residue onfilter paper, incinerate again until ash is white or nearly white evaporate to dryness and ignite .Calculate the percentage of ash on the dried drug basisMethod B. For all other substancesHeat, cool and weight platinum or silica crucibleweigh accurately about 1 g of test substance, Dry and ignite to constant weight in a mufflefurnace material should not catch fire at any time during procedure. If carbon-free ashcannot be obtained proceed as directed in method A Ignite to constant weight. Calculate the percentage of ash on the dried basis.SUDIP KUMAR
  29. 29. IP Total Ash 29Acid-insoluble ashUse Method C unless otherwise directed.Method C.Boil ash (Method A or B) with 25 ml of 2M HClcollect the insoluble matter in a Gooch crucible or on an ashless filter paper,wash, ignite, cool in a desiccator and weigh.Calculate % of acid-insoluble ash on the dried drug basisMethod D.Place ash (Method A or B), or sulphated ash (2.3.18), as directed in the individualmonograph, in crucible, add 15 ml H2O + 10 ml HClCover& boil & cool. Collect the insoluble matter on an ashless filter paperwash to neutral, ignite to dull redness, cool in an a desiccator and weigh.Calculate % of acid-insoluble ash on the dried basis.SUDIP KUMAR
  30. 30. IP Total Ash 30Water-soluble ashBoil the ash (Method A or B) with 25 ml of watercollect insoluble matter in Gooch crucible or ashless filter paperwash with hot water, and ignite (450ºC) weight of the ash - weight of insoluble matter = weight of water-soluble ash Calculate % of water-soluble ash on the dried basisSUDIP KUMAR
  31. 31. USP 31<643> TOTAL ORGANIC CARBONTotal organic carbon (TOC) is an indirect measure of organic molecules present inpharmaceutical watersTwo general approaches are usedTOC = TC – IC ( TOC=total organic carbon, TC=total carbon, IC=inorganic carbon )TOC = POC + NPOC.(POC=purgeable organic carbon , NPOC= nonpurgeable organic carbon)SUDIP KUMAR
  32. 32. IP 32N,N-DimethylanilineDetermine by gas chromatography (2.4.13).Method AInternal standard solution.As per individual monograph or dissolve 50 mg of naphthalene in cyclohexane to produce 50ml. Dilute 5 ml to 100.0 ml with cyclohexaneTest solution (a)As per individual monograph or take 1.0 g of test substance to a centrifuge tube,add 5 ml of 1M NaOH, +1.0 ml of cyclohexane, shake centrifuge Use upper layerTest solution (b) As per individual monograph or take 1.0 g of test substance into a centrifuge tube + 5 ml of 1M NaOH ,dissolve add 1.0 ml of internal standard solution, shake and centrifuge Use the upper layerSUDIP KUMAR
  33. 33. IP N,N-Dimethylaniline 33Reference solutionTake 50.0 mg of N, N-dimethylaniline + 2 ml HCl and 20 ml H2O dissolve & dilute to 50.0 mlDilute 5.0 ml to 250.0 ml *1.0 ml solution into a stoppered centrifuge tube add 5 ml of 1 M NaOH + 1.0 ml of theinternal standard solutionStopper the tube and shake & Centrifuge if necessary and use the upper layerChromatographic system– a glass column 2 m × 2 mm, packed with silanised diatomaceous support (125 to 180mesh) impregnated with 3 per cent w/w polymethylphenylsiloxane,– temperature: column.120º, inlet port and detector. 150º,– flow rate 30 ml per minute of nitrogen (carrier gas).Inject 1 μl of each of the solutions.SUDIP KUMAR
  34. 34. IP N,N-Dimethylaniline 34Method BInternal standard solution.dissolve 75 mg of N, N-diethylaniline in ( 2 ml HCl + 20 ml of water) dilute to 50 ml.Dilute 2 ml to 100.0 ml with water.Test solution (a)Test solution (b) as per Method AReference per Method A*Dilute 2 ml to 100.0 ml with waterChromatographic system– a glass column 1.5 m × 4 mm, packed with 3 per cent w/ w of cyanoethyl-silicone gum (XE-60 is suitable) on acid-washed silanised diatomaceous earth (80 to 100 mesh)– temperature: column. 80º, inlet port and detector. 150º– flow rate 30 ml per minute of nitrogen (carrier gas)SUDIP KUMAR
  35. 35. IP N,N-Dimethylaniline 35Procedure:Record the chromatogramsand measure the areas for the major peaksIn chromatogram obtained with test solution (b) ratio of thearea of any peak due to N, N-dimethylaniline to area of thepeak due to the internal standardis not greater than corresponding ratio in chromatogram obtained with internal standardsolutionUSP <223>1 method is given as per Method A of IPTest solution as per IP Test solution (b)SUDIP KUMAR
  36. 36. BP: 36Limit Test for Fluorides (Ph. Eur. method 2.4.5)Test solution:With Prescribed qty, 0.1 g of acid-washed sand R and 20 ml of a mixture of equal volumes ofH2SO4 & H2OHeat the jacket containing tetrachloroethane R maintained at its boiling point (146 °C)distil, collect distillate in a 100 ml volumetric flask containing 0.3 ml of 0.1 M NaOH and 0.1ml of phenolphthalein solution R Maintain a constant volume (20 ml) in tube during distillation and ensure that the distillateremains alkaline, adding 0.1 M NaOH if necessary.Dilute the distillate to 100 ml with water R (test solution).fluoride standard solution 5 ml of (10 ppm F) R instead of test substanceProcedure: Into two glass-stoppered cylinders introduce 20 ml of test solution and 20 ml of thestandard and 5 ml of aminomethylalizarindiacetic acid reagent R After 20 min, any blue colour in the test solution (originally red) is not more intense thanSUDIP KUMAR standardthat in the
  37. 37. 37 Limit Test for Fluorides As per BP: APPARATUSSUDIP KUMAR
  38. 38. BP 38CADMIUM, COPPER, IRON, LEAD, NICKEL AND ZINCExamine by atomic absorption spectrometryMeasure the content of cadmium, copper, iron, lead, nickel and zinc by the standard additionsmethod (2.2.23, Method II), using reference solutions of each heavy metal and the instrumentalparameters described in Table Cd Ca Fe Ni Pb Zn Wavelength nm 228.8 324.8 248.3 232 283.5 213.9 Slit width Nm 0.5 0.5 0.2 0.2 0.5 0.5 Lamp current mA 6 7 5 10 5 7 Ingition T ‗c 800 800 800 800 800 800 Atomisation T ‗c 1800 2300 2300 Back ground On Off Off Off Off Off corrector Nitrogen flow l/min 3 3 3 3 3 3SUDIP KUMAR
  39. 39. USP 39Limit test for seleniumStock Solution— is prepared by Dissolving 40.0 mg of metallic selenium in 100 mL of dilutenitric acidStandard Solution: prepared from Stock SolutionTest Solution:100 to 200 mg, unless directed otherwise in the individual monographmagnesium oxide is added for combustion and reduces soot formationProcedure:Is done in oxygen flask combustion and AASthe absorbencies are compared of test and standardSUDIP KUMAR
  40. 40. BP 40Limit Test for Magnesium(Ph. Eur. method 2.4.6)magnesium standard solution1 ml of magnesium standard solution (10 ppm Mg) R and 9 ml of water RProcedure:Organic phase - of hydroxyquinoline R in chloroform Raqueous phase used- butylamine R and triethanolamine R is addedFor comparison aqueous phase used-Any colour in the solution obtained from the substance to be examined is not more intensethan that in the standard.SUDIP KUMAR
  41. 41. BP: Limit test of ARSENIC AND MERCURY 41 Measure the content of arsenic and mercury in comparison with the reference solutions of arsenic ormercury at a known concentration by direct calibration (2.2.23, Method I) using an automatedcontinuous-flow hydride vapour generation system.absorbance of blank solution is automatically subtracted from value obtained with test solutionARSENICSample solution: 19.0 ml of the test solution or of the blank solution, add 1 ml of a 200 g/l solution of KIAAcid reagent Heavy metal-free hydrochloric acid R.Reducing reagent A 6 g/l solution of sodium tetrahydroborate R in a 5 g/l solution of sodiumhydroxide R.MERCURYSample solution Test solution or blank solution, as prescribed above.Acid reagent A 515 g/l solution of heavy metal-free hydrochloric acid R.Reducing reagent A 10 g/l solution of stannous chloride R in dilute heavy metal- free hydrochloric acidParameters are given in tableSUDIP KUMAR
  42. 42. Parameters are given in table (AAS) 42 As HgWavelength Nm 193.7 253.7Slit width Nm 0.2 0.5Lamp current mA 10 4Acid reagent flow rate ml/min 1.0 1.0Reducing reagent flow rate ml/min 1.0 1.0Sample solution flow rate ml/min 7.0 7.0Absorption cell Quartz QuartzBackground corrector off offN2 flow rateSUDIP KUMAR l/min 0.1 0.1
  43. 43. 43 References: Dr T. Narendra sir-- Inorganic Impurities in Drugs  Q4B - ANNEX I Indian Pharmacopoeia 2007 Volume 1 page no,76-79 USP32–NF27 British pharmacopoeia Volume 4 2009 Dr T. Narendra sir-- Inorganic Impurities in DrugsSUDIP KUMAR
  44. 44. 44 Incredible India !!!!! Thank u……….SUDIP KUMAR