212/Gum Guaiac/Monographs FCC V
Viscosity Determine as directed under Viscosity of Cellu-lo Gum,Appendix IIB,at75°,using spindle No.2at 60rpm.
Packaging and Storage Store in well-clod containers.
Gum Guaiac
Guaiac Resin
INS:314CAS:[9000-29-7]
DESCRIPTION
Gum Guaiac occurs as irregular mass enclosing fragments of vegetable tissues;as large,nearly homogeneous mass; and occasionally,as more-or-less rounded or ovoid tears.It is externally brown-black to dusky brown,acquiring a green color on long exposure to air,the fractured surface having a glassy luster,the thin pieces being transparent and varying in color from brown to yellow-orange.The powder is moderate yellow-brown,becoming olive brown on exposure to air.It is the resin of the wood of
Guajacum Guajacum sanctum L.(Fam.Zygophyllaceae).Gum Guaiac dissolves incompletely,but readily,in alcohol,in ether,in chloroform, and in solutions of alkalies.It is slightly soluble in carbon disulfide.
Function Antioxidant.
REQUIREMENTS
Identification
prevalent什么意思
A.Add1drop of ferric chloride TS to5mL of a1:100 alcoholic solution.A blue color appears that gradually changes to green,finally becoming green-yellow.
B.A mixture of5mL of a1:100alcoholic solution and5 mL of water becomes blue when shaken with20mg of lead peroxide.Filter the solution,and boil a portion of the filtrate. The color disappears but may be restored by adding lead peroxide and shaking the filtrate.Add a few drops of2.7N hydrochloric acid to a cond portion of the filtrate.The color immediately disappears.
Alcohol-Insoluble Residue Not more than15.0%.
Ash(Acid-Insoluble)Not more than2.0%.
Ash(Total)Not more than5.0%.
Lead Not more than2mg/kg.
Melting Range Between85°and90°.
Rosin Pass test.
TESTS
Alcohol-Insoluble Residue Place2g of sample,finely pow-dered and accurately weighed,in a dry,tared extraction thim-ble,and extract it with alcohol in a suitable continuous extrac-tion apparatus for3h or until completely extracted.Dry the insoluble residue remaining in the thimble for4h at105°, and weigh.
Ash(Acid-Insoluble)Determine as directed under Ash (Acid-Insoluble),Appendix IIC.
Ash(Total)Determine as directed under Ash(Total),Ap-pendix IIC.
Lead Determine as directed under Lead Limit Test,Appen-dix IIIB,using a Sample Solution prepared
as directed for organic compounds,and4g of lead(Pb)ion in the control. Melting Range Determine as directed under Melting Range or Temperature,Appendix IIB.
Rosin A1:10solution of sample in petroleum ether is color-less,and when mixed and shaken with an equal quantity of a fresh,1:200aqueous solution of cupric acetate,is not more green than a similar solution of cupric acetate in petroleum ether.
Packaging and Storage Store in well-clod containers.
Helium
He Formula wt4.00 INS:939CAS:[7440-59-7]
DESCRIPTION
Helium occurs as a colorless gas that is not combustible and does not support combustion.It is very slightly soluble in water.One liter of the gas weighs about180mg at0°and 760mm Hg.
Function Processing aid.
REQUIREMENTS
Note:Reduce the sample gas cylinder pressure with a
regulator.Measure the sample gas with a gas volume
meter downstream from the detector tube to minimize
contamination of or change to the gas samples.
The detector tube called for in one test is describedadvice的用法
under Solutions and Indicators.
Identification
A.Inrt a burning wood splinter into an inverted test tube filled with sample gas.The flame is extinguished.
Note:U caution.
B.A small balloon filled with sample gas shows buoyancy. Assay Not less than99.0%of He,by volume.
Air Not more than1.0%,by volume.
Carbon Monoxide Not more than10ppm,by volume. Odor Pass test.
TESTS
Assay(See Chromatography,Appendix IIA.)U a gas chromatograph equipped with a thermal-conductivity detector
FCC V
Monographs /Hexanes /213
and a 6-m ×4-mm (id)column,or equivalent,packed with porous polymer beads (PoraPak Q,or equivalent),which per-mit complete paration of nitrogen and oxygen from Helium,although nitrogen and oxygen may not be parated from each other.Maintain the column at 60°.U industrial-grade helium (99.99%)as the carrier gas.Introduce a gas sample into the gas-sampling valve.Select the operating conditions of the gas chromatograph,or equivalent,so that the peak signal of an air–helium certified standard (a mixture of 1.0%air in indus-trial-grade helium is available from most suppliers)corre-sponds to not less than 70%of the full-scale reading.The peak respon produced by
the sample gas exhibits a retention time corresponding to that produced by the air–helium stan-dard and,when compared with the peak respon of that standard,indicates not more than 1.0%air,by volume,and not less than 99.0%of He,by volume.
Air Determine as directed under Assay (above).
Carbon Monoxide Pass 1050Ϯ50mL of sample gas through a carbon monoxide detector tube at the rate specified for the tube.The indicator change corresponds to not more than 10ppm,by volume.
Odor Carefully open the sample gas cylinder valve to pro-duce a moderate flow of sample gas.Do not direct the gas stream toward the face,but deflect a portion of the stream toward the no.No appreciable odor is discernible.Packaging and Storage Store in appropriate gas cylinders.
Heptylparaben
n -Heptyl-p
青色 英文-hydroxybenzoate
2)6CH 3
C 14H 20O 3
Formula wt 236.31
CAS:[1085-12-7]judy
DESCRIPTION
Heptylparaben occurs as small,colorless crystals or as a white,crystalline powder.It is very slightly soluble in water,but is freely soluble in alcohol and in ether.Function Prervative;antimicrobial agent.REQUIREMENTS
Identification Dissolve 500mg of sample in 10mL of 1N sodium hydroxide,boil for 30min,allow the solution to evaporate to a volume of about 5mL,and cool.Acidify the solution with 2N sulfuric acid,collect the crystals on a filter,wash veral times with small portions of water,and dry in a desiccator over silica gel.The p -hydroxybenzoic acid so
obtained melts between 212°and 217°(e Melting Range or Temperature ,Appendix IIB).
Assay Not less than 99.0%and not more than 100.5%of C 14H 20O 3,calculated on the dried basis.Acidity Pass test.
Lead Not more than 2mg/kg.
Loss on Drying Not more than 0.5%.Melting Range Between 48°and 51°.
Residue on Ignition Not more than 0.05%.TESTS
Assay Transfer 3.5g of sample,accurately weighed,into a flask,add 40.0mL of 1N sodium hydroxide,and rin the sides of the flask with water.Cover with a watch glass,boil gently for 1h,cool,and titrate the excess sodium hydroxide with 1N sulfuric acid to pH 6.5.Perform a blank determination (e General Provisions )with the same quantities of the same reagents in the same manner,and make any necessary correc-tion.Each milliliter of 1N sodium hydroxide is equivalent to 236.3mg of C 14H 2O O 3,calculated on the dried basis.Acidity Mix 750mg of sample with 15mL of water,heat at 80°for 1min,cool,and filter.The filtrate is acid or neutral to litmus.Add 0.2mL of 0.1N sodium hydroxide and 2drops of methyl red TS to 10mL of the filtrate.The solution is yellow,without even a light cast of pink.
Lead Determine as directed in the Flame Atomic Absorption Spectrophotometric Method under Lead Limit Test ,Appendix IIIB,using a 10-g sample.
Loss on Drying Determine as directed under Loss on Dry-ing ,Appendix IIC,drying a sample in a desiccator over silica gel for 5h.
Melting Range Determine as directed under Melting Range or Temperature ,Appendix IIB.
Residue on Ignition Determine as directed under Residue on Ignition ,Appendix IIC,igniting a 2-g sample.Packaging and Storage Store in tight containers.
Hexanes
Mixed Paraffinic Hydrocarbons C 6H 14
Formula wt 86.18
CAS:[110-54-3]
DESCRIPTION
Hexanes occur as a clear,colorless,flammable liquid.It is compod predominantly of C 6,with some C 5and C 7,isomeric paraffins.The relative proportion of isomers varies with the producer and the production lot.It is soluble in alcohol,in acetone,and in ether and is insoluble in water.
214/4-Hexylresorcinol /Monographs
korresFCC V
Function Extraction solvent.REQUIREMENTS
Benzene Not more than 0.05%.Color (APHA)Not more than 10.
Distillation Range Between 56°and 71°.Lead Not more than 1mg/kg.
Nonvolatile Residue Not more than 10mg/kg.Specific Gravity Between 0.655and 0.675.Sulfur Not more than 5mg/kg.TESTS
Benzene Determine as directed under Benzene ,Appendix IIIC.
Color (APHA)Dilute 2.0mL of platinum–cobalt stock solu-tion (APHA No.500)with water in a 100-mL
volumetric flask.Compare this solution (APHA No.10)with 100mL of sample in 100-mL Nessler tubes,viewed vertically over a white background.
Distillation Range Determine as directed under Distillation Range ,Appendix IIB.
Lead Determine as directed in the Flame Atomic Absorption Spectrophotometric Method under Lead Limit Test ,Appendix IIIB,using a 10-g sample.
Nonvolatile Residue Evaporate 150mL (about 100g)of sample to dryness in a tared dish on a steam bath.Dry the residue at 105°for 30min,cool,and weigh.
Specific Gravity Determine by any reliable method (e General Provisions ).
Sulfur Determine as directed under Sulfur ,Appendix IIIC.Packaging and Storage Store in tight containers,protected from fire.
4-Hexylresorcinol
Hexylresorcinol;
4-Hexyl-1,3-benzenediol
3
C 12H 18O 2
Formula wt 194.27
CAS:[136-77-6]
DESCRIPTION
4-Hexylresorcinol occurs as a white powder.It is very slightly soluble in water and freely soluble in ether and in acetone.
Caution :4-Hexylresorcinol is irritating to the oral mu-cosa and respiratory tract and to the skin,and its solution in alcohol has vesicant properties.
Function Color stabilizer;enzymatic browning inhibitor.REQUIREMENTS
Identification
A.Add 1mL of nitric acid to 1mL of a saturated solution of sample.A light red color appears.
B.Add 1mL of bromine TS to 1mL of a saturated solution of the sample.A yellow flocculent precipitate forms.Add 2mL of 6N ammonium hydroxide,and the precipitate dissolves,producing a yellow solution.
C.The infrared absorption spectrum of a potassium bromide dispersion of the sample exhibits maxima only at the same wavelengths as tho of a typical spectrum as shown in the ction on Infrared Spectra ,using the same test conditions as specified therein.
Assay Not less than 98.0%and not more than 100.5%of C 12H 18O 2after drying.Acidity Pass test.
Lead Not more than 2mg/kg.
Melting Range Between 62°and 67°.Mercury Not more than 3mg/kg.Nickel Not more than 2mg/kg.
Residue on Ignition Not more than 0.1%.
Resorcinol and Other Phenols Negative by test.TESTS
Assay Dissolve 70to 100mg of sample,previously dried over silica gel for 4h and accurately weighed,in 10mL of methanol in a 250-mL iodine flask.Add 30.0mL of 0.1N bromine,then quickly add 5mL of hydrochloric acid,and inrt the stopper in the flask immediately.Cool the flask under running water to room temperature,shake vigorously for 5min,then t aside for 5min.Add 6mL of potassium iodide TS around the stopper,cautiously loon the stopper,again inrt the stopper tightly,and swirl gently.Add 1mL of chloroform,and titrate the liberated iodine with 0.1N sodium thiosulfate,adding 3mL of starch TS as the endpoint is approached.Perform a blank determination (e General Provisions ),and make any necessary correction.Calculate the milligrams of C 12H 18O 2in the sample taken by the formula
4.857×(B –S ),
in which 4.857is the milliequivalent factor,B is the number of milliliters of 0.1N sodium thiosulfate required for the blank,and S is the number of milliliters of 0.1N sodium thiosulfate required for the sample.
Acidity Dissolve 250mg of sample in 500mL of water,add a few drops of methyl red TS,and titrate with 0.02N sodium hydroxide.Not more than 1.0mL is required for neutralization (0.05%).
Lead Determine as directed in the Flame Atomic Absorption Spectrophotometric Method under Lead Limit Test ,Appendix IIIB,using a 2-g sample.
View IR
FCC V Monographs/High-Fructo Corn Syrup/215
Melting Range Determine as directed in Procedure for Class I under Melting Range or Temperature,Appendix IIB. Mercury(Note:Select all reagents for this test to have as low a content of mercury as practicable,and store all reagent solutions in containers of borosilicate glass.Specially clean all glassware ud in this test by soaking it in warm8N nitric acid for30min and rinsing with water.Keep flasks for this determination parate from other flasks,and u them only for mercury determinations.)
Standard Solution Transfer34.0mg of mercuric chloride to a250-mL volumetric flask.Add1drop of hydrochloric acid,and dissolve in and dilute to volume with water.Transfer 1.0mL of this solution to a100-mL volumetric flask,add1 drop of hydrochloric acid,and dilute with water to volume. Transfer1.0mL of this solution to a500-mL volumetric flask, add1drop of hydrochloric acid,and dilute with water to volume.
Test Solution Transfer134mg of sample to a250-mL beaker,and cautiously add10mL of11N nitric acid and10 mL of18N sulfuric acid.Digest with the aid of heat in a well-ventilated hood until brown fumes cea to evolve. Cautiously add an additional10mL of11N nitric acid,and continue heating until no more fumes evolve.Cool,transfer to a200-mL volumetric flask,and dilute to volume with water. Procedure Transfer100mL of Standard Solution to a 300-mL mercury analysis reaction vesl,add2drops of a 1:20potassium permanganate solution,and mix(the solution should be purple;add additional permanganate solution,drop-wi,if necessary).Add5mL of11N nitric acid,stir,and allow to stand for not less than15s.Add5mL of18N sulfuric acid,stir,and allow to stand for not less than45s. Add5mL of a3:200hydroxylamine hydrochloride solution, stir,and allow to stand until the solution turns light yellow or colorless.Add5mL of a1:10stannous chloride solution, immediately inrt the aerator connected to an air pump,and determine the maximum absorbance of the treated Standard Solution at the mercury resonance line of253.65nm,with a suitable atomic absorption spectrophotometer equipped with a mercury hollow-cathode lamp and an absorption cell that permits the flameless detection of mercury.
Note:Disregard the prence of insoluble matter in this
solution;mix before u.
In a clod system with a circulating air pump,connect a calcium chloride drying tube and an aerator inrted in a300-mL reaction vesl so that air pasd through the treated preparation contained in the reaction vesl evaporates any metallic mercury prent.In a similar manner,treat100mL of the Test Solution and100mL of water(reagent blank), and determine the maximum absorbances at the same wave-length.The absorbance of the solution from the Test Solution does not exceed that of the solution from the Standard So-lution.
Note:Check the zero tting of the instrument fre-
quently.
Nickel
Standard Nickel Solution Transfer40.1mg of nickel chlo-ride hexahydrate,accurately weighed,into a1-L volumetric flask,dilute with water to volume,and mix.Transfer10.0 mL of this solution to a100-mL volumetric flask,dilute to volume,and mix.Each milliliter of this solution contains1g of nickel ion.
Dissolve2g of sample in methanol to yield20mL.Add 3mL of bromine TS and2mL of a1:5citric acid solution, and mix.Add10mL of6N ammonium hydroxide and1mL of a1:100dimethylglyoxime:ethanol
solution.Mix,dilute with water to50mL,and allow to stand for5min.Any color the solution produces is not more inten than that of a solution containing4mL of Standard Nickel Solution and treated in the same manner.
Residue on Ignition Determine as directed under Residue on Ignition,Appendix IIC,igniting a1-g sample. Resorcinol and Other Phenols Shake about1g of sample with50mL of water for a few minutes,filter,and add3drops of ferric chloride TS to the filtrate.No red or blue color appears.
Packaging and Storage Store in tight,light-resistant con-tainers.
High-Fructo Corn Syrup
DESCRIPTION
High-Fructo Corn Syrup(HFCS)occurs as a water white to light yellow,somewhat viscous liquid that darkens at high temperatures.It is a saccharide mixture prepared as a clear, aqueous solution from high-dextro-equivalent corn starch hydrolysate by the partial enzymatic conversion of gluco (dextro)to fructo,using an insoluble gluco isomera preparation that complies with21CFR184.1372and that has been obtained from a pure culture fermentation that produces no antibiotics.It is miscible in all proportions with water. Function Nutritive sweetener.
REQUIREMENTS
Labeling Indicate the color range and prence of sulfur dioxide if the residual concentration is greater than10mg/kg. Identification Add a few drops of a1:10aqueous solution to5mL of hot alkaline cupric tartrate TS.A copious red precipitate of cuprous oxide forms.
Assay42%HFCS:Not less than97.0%total saccharides, expresd as a percentage of solids,of which not less than 42.0%consists of fructo,not less than92.0%consists of monosaccharides,and not more than8.0%consists of other saccharides.55%HFCS:Not less than95.0%total saccha-rides,expresd as a percentage of solids,of which not less than55.0%consists of fructo,not less than95.0%consists of monosaccharides,and not more than5.0%consists of other saccharides.
216/High-Fructo Corn Syrup/Monographs FCC V
Arnic Not more than1mg/kg.
Color Within the range specified by the vendor.
Lead Not more than0.1mg/kg.
Residue on Ignition Not more than0.05%.
Sulfur Dioxide Not more than0.003%.
Total Solids42%HFCS:Not less than70.5%;55%HFCS: Not less than76.5%.
TESTS
Assay
Apparatus(See Chromatography,Appendix IIA.)U a suitable high-performance liquid chromatography system such as described in Standard Analytical Methods of the Corn Refiners Association,equipped with a22-to31-cm stainless-steel column,or equivalent,a strip-chart recorder,and a differ-ential refractometer detector maintained at45°Ϯ0.005°. Stationary Pha U prepacked macroreticular polysty-rene sulfonate divinylbenzene cation-exchange resin(2%to 8%cross-linked,8-to25-m particle size),preferably in the calcium or silver form.Examples of acceptable resins are Bio-Rad Aminex HPX-87C,or equivalent,for parating DP1–DP4saccharides,and Aminex HPX-42C and HPX-42A,or equivalent,for parating DP1–DP7saccharides.Maintain the column at85°during operation.
Mobile Pha U degasd,purified water pasd through a0.22-m filter before u;maintain the
water at 85°during operation of the chromatograph. Standardization Prepare a Standard Solution containing a total of about10%solids,using sugars of known , USP Fructo Reference Standard;USP Dextro Reference Standard,or NIST Standard Reference Material;malto,Ald-rich Chemical Company;or equivalent)that approximates, on the dry basis,the composition of the sample to be analyzed. Dissolve each standard sugar,accurately weighed,in20mL of purified water contained in a50-mL beaker.Heat on a steam bath until all sugars are dissolved,then cool,and transfer to a100-mL volumetric flask.Dilute to volume with water and mix.Freeze the solution if it is to be reud.
If a corn syrup or maltodextrin is ud to supply a DP4+ fraction,take care to include all saccharides in the standard composition calculation.
Compute the dry-basis concentration,in percent,of each individual component in the Standard Solution by the formula
(W C/⌺W I)×100,
in which W C is the weight of the sugar of interest and⌺W i is the sum of the weights of all sugar components.Standardize by injecting10to20L(about1.0to2.0mg of solids)of the standard sugar solution into the chromatograph.Integrate the peaks and normalize.Sum the individual DP4+respons
es from the normalized printout to obtain the total DP4+normal-ized respon.Calculate the respon factors as follows(e Chromatography,Appendix IIA):
R I=(known concentration,dry basis%)/(measured concen-
tration,normalized%),
in which R I is the respon factor for component i.
Compute the respon factor for each component relative to gluco(R′I)using the following equation:
canceling四级考试作文R′I=R I/R G′,
in which R G is the respon factor for gluco.The R′I for DP4+should be programmed as a default value(if automated equipment is ud)and ud to compute the concentration of higher saccharides.
Sample Analysis Determine the solids content(below)of the sample,and dilute to approximately10%solids with water. Inject a volume(10to50L)appropriate for the specific solids content into the chromatograph.
英语四级分数查询
东京英文Calculation Calculate the concentration of each compo-nent as follows:
famousbrandC I=(A I×R I×100)/(⌺A N R N),
in which A I is the area recorded for that component and⌺A N R N is the sum of the product of the areas(A)and respon factors (R)for all components detected.
Arnic Determine as directed under Arnic Limit Test, Appendix IIIB,using a Sample Solution prepared as directed for organic compounds and1mL of Standard Arnic Solution (1g As).
Color
Apparatus U a suitable variable-wavelength spectro-photometer capable of measuring percent transmittance throughout the visible spectrum and designed to permit the u of sample and reference cells with pathlengths of2to4cm. The transmittance of all paired cells should agree within0.5%. Standard Solution Dissolve0.10g of reagent-grade potas-sium dichromate(K2Cr2O7)in1L of water,and mix thor-oughly.
Procedure Using water in the sample and reference cells of2-cm pathlength,normalize the percent transmittance scale of the spectrophotometer to100%.Leave the reference cell in place and replace t
he water in the sample cell with the Standard Solution.Determine the wavelength at which the solution exhibits exactly54.5%transmittance.This wave-length is defined asc,the corrected450-nm wavelength. Remove the2-cm cells from the spectrophotometer,and with water in the sample and reference cells of4-cm pathlength, adjust the percent transmittance scale to100%with the spec-trophotometer t atc.Leave the reference cell in place,and replace the water in the sample cell with sample.Measure the percent transmittance(T450).Remove the sample cell,t the wavelength at600nm,replace the sample with water, and adjust the percent transmittance scale to100%.Determine the percent transmittance at600nm(T600)with the same sample in the sample cell.Calculate the Color of the sample taken using the following formula:
(log T600–log T450)/4,
in which T600is the percent transmittance at600nm and T450 is the percent transmittance at450nm.
Lead Determine as directed for Method I in the Atomic Absorption Spectrophotometric Graphite Furnace Method un-der Lead Limit Test,Appendix IIIB,using a5-g sample. Residue on Ignition Determine as directed under Residue on Ignition,Appendix IIIB,igniting a10-g sample.
