AOAC 2006.03- Metal in Fertilizer
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2.6.35 AOAC Official Method 2006.03 Arsenic, Cadmium, Cobalt, Chromium, Lead, Molybdenum, Nickel, and Selenium in Fertilizers Microwave Digestion and Inductively Coupled PlasmaOptical Emission Spectrometry First Action 2006 Final Action 2009
[Applicable to analysis of As, Cd, Co, Cr, Pb, Mo, Ni, and Se in all classes of fertilizers. Limit of quantitation (LOQ; mg/kg): As, 14.4; Cd, 2.46; Co, 3.3; Cr, 33.9; Mo, 7.5; Ni, 8.1; Pb, 13.2; Se 13.2.] See Tables 2006.03A–H for the results of the interlaboratory study supporting acceptance of the method. Note that materials with iron content >5% require special cautions as noted in the method, and may experience varying degrees of degradation of precision. Digestion A. Principle
Test portion is heated with nitric acid in closed vessel microwave digestion system at 200°C. B. Apparatus
Microwave. —Commercial Microwave. —Commercial microwave designed for laboratory use at 200 °C, with closed vessel system and controlled temperature ramping capability. It is recommended that vessel design be selected that will withstand the maximum possible pressure, since some organic fertilizer products, and also carbonates if not given sufficient time to predigest, will generate significant pressure during digestion. (Vessels can reach 700 psi or more on occasion.) Vent according to manufacturer’s recommendation. ( Caution Caution:: Microwave operation involves hot pressurized acid solutions. Use appropriate face protection and laboratory clothing.) C. Reagents
(a) Water .—Use .—Use 18 Megaohm water throughout for dilution. ( b) Concentrated HNO 3 .—Use trace metal grade HNO 3 throughout. D. Determination
(Caution Caution:: Observe standard precautions with concentrated acid. When dispensing acid or venting vessels, use gloves, face protection, and laboratory coats. Never remove hot vessels from microwave; wait until they are near room temperature. Keep microwave door closed while vessels are hot. The door is the primary safety device if a vessel vents.) Prepare solid samples as in 929.02 ( see see 2.1.05). Accurately weigh 1.0000 ± 0.010 g (0.5000 g for organic matrixes) test portion to digestion vessel. Use weighing paper insert to line the vessel walls during sample transfer, to keep sample from adhering to sides of vessel. Fluid samples may be weighed directly after mixing. Add 10.0 ± 0.2 mL trace metal grade HNO 3, loosely cap vessels without sealing, predigest at room temperature until vigorous foaming subsides, or overnight if time allows. Seal vessels according to manufacturer’s directions and place in microwave. With power setting appropriate to microwave model and number of vessels used, ramp temperature from ambient to 200 °C in 15 min. Hold at 200°C for 20 min. Cool vessels according to manufacturer’s directions, vent, and transfer digests to 100 mL volumetric flasks, dilute to volume, and mix. Transfer to polypropylene containers within 2 h, unless solutions are to be analyzed immediately. Dilute samples that are found to be above the standard curve range, or have content of
metals higher than 1000 mg/kg. Final dilutions require addition of appropriate amounts of HNO3 to maintain the proportion of 10% HNO3 in the final solution to be analyzed. Detection E. Principle
Digested test solution, or an appropriate dilution, is presented to the inductively coupled plasma-optical emission spectrometry (ICP-OES) instrument calibrated with acid matched standard calibrant solutions. An ionization buffer (cesium) is used to minimize easily ionizable element (EIE) effects, and scandium and/or beryllium are used as internal standard(s). F. Instrumentation
( a) ICP emi emissi ssion on spe ctrom ete eterr. —Cap —Cap abl ablee of det erm ermini ining ng multiple wavelengths for each element of interest. A 3-channel peristaltic pump is desirable to avoid the necessity of having to manually add ionization buffer and internal standard to each sample solution. Use a Meinhard or Seaspray nebulizer and Cy clonic Spray Chamber, or other components designed to optimize aerosol and maximize precision. Select sample and internal standard pump tubes, and peristaltic pump rotation speed, with regard to manufacturer’s recommendations, but try to keep sample and internal standard pump tubes of similar size, to maximize mixing accuracy, while maintaining needed detection levels. The analyst must compensate for EIE effects in the plasma since fertilizer materials can contain substantial concentrations of elements that provide a significant source of electrons to the plasma, such as K and Ca. The presence of ionization buffer in all samples and standards will minimize the effect of varying concentrations of EIEs in the sample. Power settings and nebulizer gas flow should b e optimized for robust plasma conditions. The analyst needs to ensure that the Mg 285.213:Mg 280.271 ratio (Mermet principle of robust plasma) demonstrates robust operating conditions in accordance with the ratio established by the instrument manufacturer. Two or 3 replicate readings of the same sample are desirable, with relatively longer integration time to minimize noise. Properly optimized instruments should have internal standard ratios for most samples consistently in the range 0.9 to 1.0. It is unusual to have the ratio lower than 0.8 over a very wide range of fertilizer material types. The occurrence of lower ratios is cause for troubleshooting. Select ionization buffer/internal standard solution, G(d), such that after mixing sample and internal standard solutions using the instrument’s peristaltic pump, the combined solution presented to the nebulizer contains 2200 mg/kg or greater cesium chloride; 0.75 to 1.0 mg/kg internal standard; and 7.2 mg/mL or less actual fertilizer material. (For example, these conditions would be met with a 1 g sample digested and diluted to 100 mL before instrument analysis; an ionization buffer/internal standard solution of 8000 mg/kg cesium chloride and 3 mg/kg scandium and/or beryllium internal standard(s); and pump tubes of white/white (1.02 mm id) sample and orange/white (0.64 mm id) internal standard, the white/white contributing about 72%, and the orange/white contributing about 28%, to the final nebulized solution.) At a minimum, all sample instrument responses for each element should be corrected using one internal standard wavelength. However, best practice is to utilize similar transitions between analyte and internal standard. For example, the As 188.980 wavelength is from arsenic in the atomic state, so the internal
IN TERNA NATIONAL TIONAL ã 2009 AOAC INTER
standard wavelength used for correction should also be from the atomic state, such as Sc 361.383. Conversely, match ionic sample lines with ionic internal standard lines. ( Note: Do not use yttrium as an internal standard, since it is found native at low levels in some phosphate ore sources.) (b) ICP wavelengths. —A number of wavelengths may be used for analysis of the 8 elements of interest, depending on the capability of the analytical instrument used. As a minimum, select at least 2 wavelengths for each element of interest, and report the average value of closely agreeing results, except for lead and selenium, for which there is only one reliable wavelength available. Following is a list of suggested wavelengths, not in any priority order, that have been found acceptable for most fertilizer materials. Other lines of appropriate sensitivity, free of interferences or corrected for interferences, may be just as acceptable. However, it is imperative that instrument response (both instrument graphic output and calculated concentration) be reviewed for each sample and element. Fertilizer materials are extremely variable in composition, and a wide concentration range of potential interfering elements is expected, so no single wavelength will work in every instance. Occasional data with interference will inevitably be found, and must be eliminated from inclusion in the mean calculation for that particular element and sample. Wavelengths (nm): As: 188.980, 193.696; Cd: 214 .439, 226.502; Co: 228.615, 230.786, 235.341; Cr: 205.560, 267.716, 276.653; Mo: 201.512, 202.032, 203.846, 204.598; Ni: 216.555, 222.295, 222.486, 227.877, 231.604, 239.452; Pb: 220.353; Se: 196.026; Sc: 361.383, 431.408; Be: 234.861, 249.473. ( c ) Wavelength interference treatment. —I nt er el em en t interference can cause substantial error in analytical result. Error can be minimized by several techniques: (1) Three or more analytical lines may be used for a given element, and when an interferent is present in a particular line, the result for that line is omitted from the mean value reported. ( 2) Certain vendors’ instrument software has the capability of mathematically modeling potential interferents, and deconvoluting the instrument response into an analytical element portion and an interferent portion. ( 3) Interelement correction is an alternative mathematical technique to use with instruments for which mathematic modeling is not available, or where direct spectral overlap negates use of the deconvolution technique. The following lines, if used, must utilize one of the correction techniques; corrections for other lines may be applied as needed and appropriate: (1) As 188.980: Correct for Cr interference at 188.995 , or verify that Cr is not present in the test portion analyzed. ( 2) As 193.696: Fe affects the arsenic peak. Remove with an Fe model, or verify that Fe is not present in the test portion analyzed. (3) Cd 214.439 and 226.502: Fe, present in many fertilizers, interferes with both suggested Cd wavelengths. Mathematically correct instrument Cd response for the interference, or verify analytically that Fe is not present in the test portion analyzed. (4) Pb 220.353: Mathematically correct instrument Pb response for Fe interference, or verify that Fe is not present in the test portion analyzed. ( 5) Se 196.026: Mathematically correct instrument Se response for Fe interference, or verify that Fe is not present in the test portion analyzed. (d) ICP instrument calibration .—Prepare working standard solutions from commercial stock standards at 1000 mg/kg. Custom blended multielement stock standard in HNO3 is acceptable. Prepare a minimum of 5 working standards at 0.1, 0.5, 1.0, 5.0, and 10.0 mg/kg,
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plus blank, of each element, in 10% trace metal grade HNO3. Working standards should be in the linear ra nge, with correlation coefficients of at least 0.9999. G. Reagents
(a) Water .—Use 18 Megaohm water for dilution. (b) HNO3.—Use trace metal grade HNO 3. (c) 0.5% Triton X100 solution.—Dilute 0.5 mL Triton X100 to 100 mL with H2O. (d) Ionization buffer/internal standard solution.— Weigh 8.0 g CsCl into a 1000 mL acid-washed volumetric flask. Add 3 mL each of ICP grade scandium and beryllium 1000 mg/kg stock solution, as internal standards. Also add 1 mL of 0.5% Triton X100, dilute to volume, and mix. Store in a polypropylene bottle. ( Note: Reagent concentrations assume the use of white/white, 1.02 mm id sample pump tube, and orange/white, 0.64 mm id internal standard pump tube. If the sample and internal standard solutions are mixed in different proportions by the instrument’s peristaltic pump, then adjust the reagent concentrations to meet concentration requirements of mixed solution nebulized by the instrument, as outlined in F. Note that sample and internal standard solution mixing ratio is proportional to pump tube flow rates, not proportional to pump tube IDs.) ( e ) Stock standard solution. —Work ing sta nda rds can be pr epared from ICP grade indivi dual ele men t 1000 mg/kg commercial stock standard solutions. However, it is also acceptable to use commercially prepared custom blended stock standard mixtures containing all of the 8 elements at 1000 mg/kg. A number of companies provide this stock standard service. ( f ) 10 mg/kg intermediate stock standard solution for preparation of low-level working standards. —Dilute 5.0 mL of stock standard solution to 500 mL. Prepare fresh each time standards are prepared, and use immediately after preparation. (g) Working standard solutions. —Standards are designed to have the same acid concentration as digested test solutions. Date all calibration solutions when made, which should be stable for at least 1 month, but not longer than 2 months. Monitor standard curve fit and intensity for signs of change and degradation over time. (1) 10 mg/kg elements.—Pipet 5.0 mL of combined 1000 mg/kg element stock solution into a 500 mL acid-washed volumetric flask. Add 50 mL of trace metal grade HNO3, dilute to volume with H 2O, mix, and transfer to acid-washed polypropylene b ottle. (2) 5 mg/kg elements.—Pipet 5.0 mL of combined 1000 mg/kg element stock solution into a 1000 mL acid-washed volumetric flask. Add 100 mL of trace metal grade HNO 3, dilute to volume with H 2O, mix, and transfer to an acid-washed polypropylene bottle. (3) 1 mg/kg elements.—Pipet 50.0 mL of 10 mg/kg intermediate stock solution into a 500 mL acid-washed volumetric flask. Add 50 mL of trace metal grade HNO3, dilute to volume with H 2O, mix, and transfer to an acid-washed polypropylene bottle. ( 4) 0.5 mg/kg elements.—Pipet 25.0 mL of 10 mg/kg intermediate stock solution into a 500 mL acid-washed volumetric flask. Add 50 mL of trace metal grade HNO3, dilute to volume with H 2O, mix, and transfer to an acid-washed polypropylene bottle. ( 5) 0.1 mg/kg elements.—Pipet 5.0 mL of 10 mg/kg intermediate stock solution into a 500 mL acid-washed volumetric flask. Add 50 mL of trace metal grade HNO3, dilute to volume with H 2O, mix, and transfer to an acid-washed polypropylene bottle. (6 ) 0.0 mg/kg elements (blank).—Add 50 mL of trace metal grade HNO 3 into a 500 mL
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s r e 0 0 i l / 0 / 0 / 0 / 2 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / t / u 0 0 0 1 0 0 0 1 1 0 0 1 0 0 0 0 0 1 0 0 1 1 1 0 1 1 2 0 O
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0 6 5 7 0 0 4 6 6 2 3 2 9 3 6 9 5 0 1 9 4 9 4 4 8 8 7 6 R . 5 . 7 . 9 . 5 . 3 . 0 . 1 . 6 . 6 . 2 . 6 . 3 . 9 . 9 . 1 . 2 . 6 . 0 . 8 . 2 . 7 . 8 . 8 . 6 . 5 . 5 . 7 . s 5 6 3 0 1 2 2 1 1 0 0 1 0 3 4 0 1 1 2 4 0 5 0 0 0 0 0 0 0 3 1 3
7 5 9 1 7 6 5 3 5 3 5 7 0 8 0 6 5 4 8 9 6 0 0 3 3 3 r 3 7 s 0 . 2 . 4 . 2 . 6 . 8 . 2 . 2 . 0 . 2 . 1 . 0 . 8 . 0 . 5 . 5 . 7 . 0 . 4 . 4 . 9 . 0 . 3 . 1 . 1 . 1 . 1 . 2 . 4 8 0 0 0 0 0 0 0 0 0 0 3 3 0 0 0 1 0 0 0 0 0 0 0 0 0 0 1 1
g 1 k / 1 0 9 3 1 4 1 5 4 5 6 0 8 3 2 4 5 1 3 7 0 4 8 8 9 3 6 g 5 7 6 0 7 3 0 6 9 0 2 3 1 2 7 7 2 3 2 6 6 6 9 5 8 . . . . . . . . . . . . . . . . . . . . . . . . 3 . 6 . 7 . 5 . m 7 4 4 7 3 2 8 4 1 2 1 5 2 6 6 4 1 5 1 0 0 3 0 2 3 3 1 , 9 5 9 1 2 4 3 2 1 X 1 5 t l a b o c r o f s c i t s i t a t s e t a c i l p u d d n i l B . C 3 0 . 6 0 0 2 e l b a T
k c d i l o o k m R s c d u s o o e n s o i r t e p h 2 b e s l e B n t e n n 1 7 3 y P 2 r a b 9 o + n e a d o 1 0 0 g u a i i e t t / r 0 k t f l o w c r t i l P n P i a l b e n k 3 4 1 c p u 2 4 f o e a t r a e f r c i t e P A / l P A f u a e k c + 0 0 0 r s 0 O l s z r A e a P i u n A c o t d e h c y 0 S u i s D M D A A f 0 0 d 0 l m a o e l i i r s c o s x 2 n s m y D 2 2 n 2 o h r b t r d m m h n n e k r n t u e o r Z y t r r r r a M r s x e p e e u r a / a l d e e c f t h e u x d o d e e b e e o e t r a n d c n e e W c i d d n i e l i r t n d s e F d % o t s s N C r e i l / n 4 o r o e o f h u u u o w a c l a N f e l e K 1 a e P u r r r p l o t d p 9 F B C a r n g x C A a 3 F l i g g g b e i o m r 6 u t m e g W W o m a a P P Z n M o / r - a l a a o r e M F f - O m a M M N M K B h S M M r c C i P t R A P G n a S A N a e g D F T r S I O N
5 8 6 0 9 6 5 7 0 5 2 8 5 1 7 2 9 4 8 1 6 9 4 3 4 0 7 7 D I 2 3 3 9 6 5 8 6 9 7 1 1 6 3 3 9 6 7 8 0 0 4 6 8 2 4 3 8 9 4 8 6 0 0 2 9 3 8 4 1 9 3 6 4 7 0 4 6 1 2 5 9 3 5 8 e 0 l / 5 / 1 / 5 / 7 / 2 / 4 / 6 / 6 / 3 / 4 / 7 / 8 / 8 / 4 / 3 / 9 / 9 / 8 / 3 / 4 / 5 / 2 / 6 / 7 / 1 / 8 / 3 / p 2 1 1 1 8 8 5 8 3 1 9 1 8 7 9 5 6 3 6 6 1 6 7 0 3 4 1 3 m 2 3 4 8 1 1 7 1 6 9 0 3 1 5 9 4 7 8 2 1 1 9 6 8 2 3 2 8 a 3 0 3 4 8 6 9 3 1 9 5 7 9 4 8 9 8 8 6 4 7 3 7 8 9 1 6 8 8 S 4 4 6 5 2 1 9 3 7 7 6 7 3 4 6 7 8 9 4 6 3 4 4 6 4 4 5 7
ã 2009 AOAC INTERNATIONAL
s r e 0 0 i l / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 1 / 0 / 1 / 0 / 0 / 0 / 3 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / t / u 0 0 2 1 1 0 2 1 1 0 0 1 0 2 1 1 0 1 1 0 0 0 0 0 0 1 0 0 O
t a 7 4 7 6 6 5 0 4 6 7 2 0 2 8 5 5 7 6 3 3 5 6 6 5 1 5 9 0 R r 8 . 0 . 1 . 8 . 4 . 4 . 5 . 8 . 5 . 9 . 3 . 2 . 7 . 2 . 5 . 6 . 5 . 5 . 0 . 3 . 2 . 6 . 6 . 4 . 0 . 9 . 0 . 3 . o 3 3 4 0 2 2 0 0 0 0 1 1 1 1 1 0 2 0 1 1 2 3 1 1 2 0 1 1 H
1 4 0 2 1 0 1 8 8 4 9 0 9 2 7 5 6 1 3 0 9 2 4 6 3 6 1 5 R 5 . 4 . 2 . 6 . 3 . 5 . 7 . 5 . 0 . 5 . 8 . 3 . 7 . 8 . 5 . 8 . 1 . 2 . 2 . 0 . 8 . 9 . 6 . 5 . 1 . 9 . 3 . 6 . 9 9 3 8 4 5 8 1 0 2 3 6 8 4 2 5 5 4 3 2 4 4 4 7 8 1 8 1 6 1 2 2 5 8 4 5 8 5 4 8 2 1 4 3 6 4 1 2 3 4 2 7 2
7 0 8 4 2 3 4 4 4 4 2 4 0 0 0 5 0 0 9 8 0 2 4 8 3 5 6 7 r 5 . 9 . 2 . 8 . 9 . 8 . 1 . 7 . 0 . 7 . 1 . 6 . 8 . 1 . 3 . 9 . 9 . 7 . 6 . 5 . 7 . 0 . 6 . 5 . 8 . 2 . 3 . 9 . 6 7 1 5 3 5 1 0 1 2 9 0 7 3 9 5 0 8 5 0 6 1 4 2 7 1 0 6 0 5 1 1 1 2 2 4 1 2 6 2 2 5 1 2 1 1 % , 4 9 1 0 9 8 5 4 6 8 3 7 4 6 9 5 9 4 0 0 5 9 9 7 7 8 8 R 2 9 . 7 . 6 . 4 . 7 . 5 . 1 . 1 . 6 . 6 . 7 . 4 . 7 . 4 . 6 . 6 . 5 . 3 . 4 . 5 . 2 . 2 . 1 . 9 . 8 . 3 . 4 . 2 . D 2 0 6 2 9 4 5 3 6 8 2 2 9 0 4 1 4 4 0 7 8 9 4 1 8 8 0 S 2 9 1 6 2 1 1 1 1 3 1 1 4 1 1 1 1 R
% , r 9 0 0 1 6 9 5 0 8 5 6 8 6 8 8 2 9 9 5 8 4 9 2 7 7 0 6 0 . 2 . 3 . 3 . 6 . 5 . 5 . . 8 . 0 . 2 . 3 . 7 . 7 . 0 . 5 . 6 . 9 . 7 . 0 . 0 . 1 . 1 . 7 . 8 . 1 . 2 . D 0 0 4 4 1 3 5 0 2 3 1 5 2 0 6 7 0 9 5 2 0 3 2 8 1 2 3 1 0 S 1 1 2 1 1 1 R
8 7 4 2 8 2 1 4 1 6 6 5 0 1 9 3 4 7 4 3 8 6 6 0 2 7 1 0 R 6 . 3 . 1 . 2 . 6 . 8 . 1 . 1 . 3 . 7 . 9 . 2 . 0 . 0 . 4 . 2 . 8 . 0 . 4 . 4 . 1 . 7 . 6 . 7 . 6 . 2 . 1 . 3 . s 7 8 1 0 8 9 3 9 4 8 9 2 1 6 9 9 1 5 5 1 3 1 1 2 8 4 0 1 6 7 1 1 2 1 1 2 2 1 2 6 1 2 8 1 1 1 2
6 9 0 5 1 4 4 2 0 3 7 8 6 2 2 1 8 5 4 7 6 2 5 5 0 9 r 7 9 s 7 . 3 . 4 . 0 . 4 . 6 . 4 . 8 . 9 . 1 . 4 . 2 . 0 . 6 . 4 . 1 . 3 . 1 . 1 . 3 . 5 . 3 . 6 . 9 . 6 . 4 . 7 . 4 . 3 6 0 2 1 5 0 3 3 8 0 0 7 4 0 2 0 3 9 7 9 0 1 0 0 0 3 2 7 5 1 1 1 5 2
g 9 8 2 5 5 0 6 7 1 8 1 0 9 4 1 4 5 3 5 7 4 4 1 2 1 4 5 k / 5 . 9 . 8 . 5 . 2 . 1 . 4 . 1 . 3 . 9 . 2 . 1 . 4 . 4 . 5 . 9 . 8 . 5 . 9 . 8 . 7 . 6 . 6 . 0 . 7 . 0 . 2 . 9 . g 4 1 1 9 8 1 4 6 3 1 1 8 4 9 6 6 5 5 0 8 4 3 8 8 6 1 9 9 m 3 6 9 5 3 0 7 6 9 8 4 1 6 6 7 9 1 8 0 3 1 4 5 1 0 , 1 1 5 3 2 3 1 1 2 1 1 9 1 1 7 1 1 m X 7 3 5 u
i m o r h c r o f s c i t s i t a t s e t a c i l p u d d n i l B . D 3 0 . 6 0 0 2 e l b a T
k c d i l o o k R m s c d u o o e n s s i r t o e p h b e s l e B n t e n n 1 7 3 y P 2 r 2 a b 9 o + n e d a o 1 0 0 g u a i e w t / n k r - t i 0 - - i t f l r n o c t l P P i 4 a c l e k 4 1 p u 2 r e a t a e f r c i P 3 / l P A f c a b e k 0 0 + 0 u o r s 0 O f s i z m e r t A A e h a P u n A c t d e c y 0 S l f A 0 0 0 l a D o i M e l s c o o i i t r s D A D 2 2 d s x 2 n u 2 o s h u r m n h r b y r d m n m n e n r p c e e u e t a r r t M a r r l s e k x e r r Z y / a d o u x a f t e e e c e o d o i d t e t h n f n d d b d n i e e e W o r e c o s i C e r n i l e e d s % t a o s d r l F n / N r o o h 4 e u u u w a c N 1 n l a t l e e u r r K r a g e p l p F B d o 9 C P f C r x A a 3 F l i g g g b e i m o / 6 m r u m t g W W P a a - a P Z n M o r o l a e a o r e M F f - O m a M M N M K B h S M M r c C A i P R t P G n a S A N a e g D F T r S I O N
5 8 6 0 9 6 5 7 0 5 2 8 5 1 7 2 9 4 8 1 6 9 4 3 4 0 7 7 D I 2 3 3 9 6 5 8 6 9 7 1 1 6 3 3 9 6 7 8 0 0 4 6 8 2 4 3 8 9 4 8 6 0 0 2 9 3 8 4 1 9 3 6 4 7 0 4 6 1 2 5 9 3 5 8 e 0 l / 5 / 1 / 5 / 7 / 2 / 4 / 6 / 6 / 3 / 4 / 7 / 8 / 8 / 4 / 3 / 9 / 9 / 8 / 3 / 4 / 5 / 2 / 6 / 7 / 1 / 8 / 3 / p 2 1 1 1 8 8 5 8 3 1 9 1 8 7 9 5 6 3 6 6 1 6 7 0 3 4 1 3 m 2 3 4 8 1 1 7 1 6 9 0 3 1 5 9 4 7 8 2 1 1 9 6 8 2 3 2 8 a 3 0 3 4 8 6 9 3 1 9 5 7 9 4 8 9 8 8 6 4 7 3 7 8 9 1 6 8 8 S 4 4 6 5 2 1 9 3 7 7 6 7 3 4 6 7 8 9 4 6 3 4 4 6 4 4 5 7
ã 2009 AOAC INTERNATIONAL
s r e 0 0 i l / 0 / 0 / 1 / 0 / 0 / 0 / 0 / 0 / 0 / 2 / 0 / 1 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / t / u 0 0 0 0 0 0 0 1 1 0 1 1 0 0 0 2 1 0 0 2 0 1 0 0 0 0 0 1 O
t a 1 4 5 4 7 9 2 7 7 6 4 0 1 8 9 6 7 0 6 0 3 0 9 0 2 8 7 0 R r 2 . 2 . 1 . 2 . 1 . 9 . 9 . 9 . 9 . 3 . 0 . 9 . 0 . 5 . 9 . 2 . 2 . 8 . 8 . 1 . 2 . 0 . 5 . 7 . 3 . 4 . 6 . 5 . o 3 3 5 3 3 4 0 0 0 1 1 1 1 0 0 1 5 1 1 6 3 2 8 7 1 2 0 1 2 H
9 3 3 9 4 5 8 7 1 8 6 5 6 7 4 8 3 4 9 0 3 9 5 2 2 0 9 8 R 5 . 7 . 2 . 5 . 3 . 8 . 2 . 1 . 9 . 9 . 7 . 3 . 0 . 2 . 2 . 3 . 8 . 4 . 7 . 8 . 3 . 0 . 4 . 9 . 0 . 5 . 3 . 2 . 2 2 4 4 3 7 3 5 2 1 3 0 4 6 2 2 1 6 4 2 2 3 2 2 7 5 4 1 5 8 1
4 2 8 9 7 3 3 7 5 0 6 2 4 7 7 2 2 5 8 0 4 5 2 0 4 2 9 2 r 2 . 7 . 8 . 0 . 6 . 7 . 8 . 8 . 3 . 4 . 5 . 3 . 9 . 2 . 8 . 3 . 2 . 8 . 5 . 5 . 0 . 8 . 3 . 4 . 4 . 1 . 6 . 5 . 4 9 1 1 1 2 1 0 0 1 1 0 2 6 0 0 0 4 1 1 5 0 1 2 2 4 1 0 1 5
% 6 2 6 9 4 0 3 9 1 8 4 7 9 3 6 8 4 6 4 0 9 7 2 4 3 1 3 5 , R 1 . 3 . 5 . 1 . 6 . 9 . 1 . 9 . 1 . 6 . 4 . 3 . 9 . 2 . 8 . 6 . 1 . 9 . 8 . 2 . 3 . 7 . 9 . 8 . 6 . 8 . 6 . 4 . D 7 5 8 2 3 3 0 9 1 7 1 2 0 5 1 5 8 9 1 7 5 5 8 6 3 9 6 1 4 4 6 1 1 1 1 3 1 1 1 8 1 2 9 3 2 4 2 1 2 2 S 2 2 7 4 1 1 R
% , r 5 8 1 4 9 7 7 8 2 9 5 9 4 3 1 1 5 3 2 9 6 8 2 0 3 3 5 2 . 2 . 0 . 0 . 8 . 2 . 6 . 6 . 3 . 4 . 7 . 2 . 9 . 2 . 6 . 1 . 6 . 0 . 2 . 2 . 4 . 0 . 1 . 4 . 7 . 3 . 5 . 7 . D 3 3 0 1 2 5 1 1 2 4 9 7 5 4 2 0 5 7 2 4 7 0 4 4 2 2 8 S 7 8 1 1 1 2 2 1 1 1 1 5 1 8 0 2 R 2 1
8 5 1 4 9 0 7 5 4 1 4 1 5 4 0 5 5 0 1 0 0 0 8 4 1 6 7 6 R . 5 . 5 . 6 . 1 . 8 . 1 . 8 . 0 . 7 . 3 . 2 . 4 . 2 . 8 . 8 . 6 . 3 . 7 . 0 . 4 . 1 . 8 . 0 . 5 . 9 . 5 . 4 . s 7 8 9 1 1 1 2 1 1 1 0 1 0 1 2 0 0 0 2 1 1 4 1 0 1 2 1 1 0 1 2
7 9 0 8 5 1 2 0 6 3 5 4 1 1 8 3 7 4 0 0 7 6 7 7 0 9 r 8 3 s 0 . 3 . 6 . 3 . 6 . 9 . 6 . 3 . 1 . 5 . 5 . 1 . 0 . 2 . 3 . 1 . 0 . 7 . 5 . 5 . 8 . 3 . 4 . 8 . 8 . 4 . 6 . 1 . 5 1 0 0 0 0 0 0 0 0 0 0 1 2 0 0 0 1 0 0 1 0 0 0 0 1 0 0 2
g k / 9 2 9 3 9 5 7 6 0 4 5 1 8 5 2 4 3 3 3 4 8 9 2 0 9 2 2 g 6 1 . 6 . 3 . 8 . 7 . 3 . 5 . 4 . 3 . 0 . 7 . 6 . 2 . 8 . 7 . 4 . 7 . 8 . 0 . 4 . 2 . 5 . 8 . 4 . 5 . 6 . 1 . . 5 m m 9 6 0 3 2 4 1 8 9 4 1 0 3 2 6 5 1 7 1 2 4 0 0 8 6 3 2 0 u , 6 1 1 1 1 1 4 1 1 1 2 n X 1 e
d b y l o m r o f s c i t s i t a t s e t a c i l p u d d n i l B
k c d i l o o k m R s c d u o o e n s s i r t o e p h b e s l e B n t e n n 1 7 3 y P 2 r 2 a b 9 o f + n e d a o 1 0 0 g u a i e w t r - t i - - i k t l 0 l r n o / c t P P i n 4 a c l e k 3 4 1 p r e a t a e f i t r c e a b P 0 0 + 0 u o 2 O f A A f l P / c e k r u s l z r s A e a P 0 i n u A 0 0 d 0 d i c t e h f c y 0 S u i A l m a D o M e l s c o o i r D A s x 2 n s m s o t 2 2 2 D u e r n r r b r d m m h y a n n e t r h M a r r l k u n s x d r e e p i e t e u e t r r Z y / a d o c x a f e e e c d e o i h n f n d d b d n n e e t o e e W o r c i e l r t e F e i d s t s s N C d % o r l n / r o o h 4 e u u u o w a c a N f e e K 1 l a e P u r r r p l o t d p 9 l F B C g g a g n u e F x C A a r 3 i g l i o b m r 6 m t W / g W P m a a - a P Z n M o r o l a e a o r e M F f - O m a M M N M K B h S M M r c C A i P R t P G n a S A N a e g D F T r S I O N
. E 3 0 . 6 0 0 2 e l b a T
5 8 6 0 9 6 5 7 0 5 2 8 5 1 7 2 9 4 8 1 6 9 4 3 4 0 7 7 D I 2 3 3 9 6 5 8 6 9 7 1 1 6 3 3 9 6 7 8 0 0 4 6 8 2 4 3 8 9 4 8 6 0 0 2 9 3 8 4 1 9 3 6 4 7 0 4 6 1 2 5 9 3 5 8 e 0 l / 5 / 1 / 5 / 7 / 2 / 4 / 6 / 6 / 3 / 4 / 7 / 8 / 8 / 4 / 3 / 9 / 9 / 8 / 3 / 4 / 5 / 2 / 6 / 7 / 1 / 8 / 3 / p 2 1 1 1 8 8 5 8 3 1 9 1 8 7 9 5 6 3 6 6 1 6 7 0 3 4 1 3 m 2 3 4 8 1 1 7 1 6 9 0 3 1 5 9 4 7 8 2 1 1 9 6 8 2 3 2 8 a 3 0 3 4 8 6 9 3 1 9 5 7 9 4 8 9 8 8 6 4 7 3 7 8 9 1 6 8 8 S 4 4 6 5 2 1 9 3 7 7 6 7 3 4 6 7 8 9 4 6 3 4 4 6 4 4 5 7
ã 2009 AOAC INTERNATIONAL
s r e 0 0 i l / 2 / 0 / 0 / 0 / 0 / 1 / 0 / 0 / 0 / 2 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 2 / 0 / 0 / 0 / 0 / 0 / t / u 0 0 0 0 0 0 0 1 0 0 0 1 0 0 0 0 2 0 0 0 0 1 1 2 1 0 2 0 O
t a 2 0 5 4 9 3 1 3 2 2 9 4 6 2 3 2 3 6 9 6 4 1 3 2 6 4 7 9 R r 2 . 7 . 8 . 5 . 4 . 6 . 3 . 0 . 2 . 9 . 3 . 0 . 9 . 1 . 4 . 9 . 0 . 1 . 5 . 8 . 7 . 3 . 3 . 2 . 4 . 2 . 0 . 7 . o 2 2 3 1 1 1 1 1 1 0 1 2 1 1 1 0 1 3 2 2 2 3 1 3 1 2 1 2 H
8 5 5 6 8 0 5 7 5 8 7 9 5 0 3 2 1 7 7 8 0 3 0 9 3 3 4 7 6 . 7 . 1 . 1 . 8 . 5 . 5 . 9 . 8 . 9 . 0 . 5 . 6 . 9 . 3 . 1 . 1 . 4 . 8 . 1 . 2 . 7 . 4 . 8 . 6 . 1 . 7 . 9 . R 7 1 3 1 5 5 4 4 7 9 8 4 4 6 8 6 2 2 3 9 4 2 3 2 0 7 4 8 3 5 1 1 5 3 1 4 7 2 1 6 1 2 4 1 1 2
9 4 5 4 6 6 4 1 7 3 1 0 4 6 6 7 7 2 6 8 5 1 2 8 8 7 5 7 . 2 . 6 r 5 . 6 . 2 . 8 . 0 . 3 . 3 . 6 . 5 . 0 . 0 . 1 . 2 . 8 . 7 . 4 . 5 . 9 . 5 . 3 . 6 . 4 . 4 . 2 . 4 . 5 . 6 9 1 2 1 5 2 7 4 3 5 1 0 8 1 6 0 1 6 4 2 2 1 0 7 4 1 3 3 4 2 1 1 5 1 1 2 % 1 2 0 9 5 2 8 3 2 9 3 7 5 8 5 5 8 8 9 4 8 7 9 4 0 6 3 7 , R 8 . 3 . 3 . 9 . 1 . 2 . 5 . 0 . 2 . 3 . 2 . 5 . 6 . 8 . 6 . 6 . 5 . 8 . 6 . 2 . 8 . 4 . 6 . 5 . 2 . 2 . 4 . 4 . D 4 8 5 4 6 5 4 7 9 8 2 4 5 5 1 7 2 5 6 2 5 7 5 5 1 5 1 1 1 2 1 1 1 2 2 3 2 4 1 4 1 2 1 3 S 1 1 5 1 1 1 1 R
% , r 4 2 5 5 5 5 5 3 6 5 3 7 3 3 3 6 0 0 4 8 2 9 8 3 6 5 0 4 . 0 . 0 . 5 . 4 . 7 . 5 . 9 . 0 . 0 . 7 . 3 . 0 . 6 . 6 . 2 . 6 . 3 . 6 . 4 . 4 . 0 . 4 . 5 . 0 . 1 . 5 . 5 . D 9 9 3 3 5 6 0 1 3 3 5 7 4 4 3 4 1 2 7 3 0 7 7 2 5 3 2 S 3 8 1 2 2 1 1 1 4 1 1 R
7 0 2 9 0 4 2 3 2 6 5 4 5 9 2 6 5 1 5 8 4 8 1 3 1 5 9 0 R 1 . 2 . 1 . 9 . 1 . 5 . 6 . 6 . 5 . 5 . 4 . 6 . 9 . 8 . 1 . 7 . 7 . 3 . 9 . 2 . 6 . 9 . 2 . 0 . 5 . 5 . 6 . 2 . s 9 4 1 3 2 5 1 9 3 3 6 1 5 8 0 5 0 2 4 3 8 0 1 1 4 2 1 3 4 5 1 1 1 9 1 2 1
9 4 5 9 3 1 6 0 7 6 6 1 2 5 8 7 4 8 8 2 8 7 7 3 2 8 r 7 0 s 0 . 3 . 5 . 9 . 4 . 0 . 7 . 6 . 5 . 3 . 9 . 3 . 1 . 9 . 0 . 4 . 2 . 3 . 3 . 7 . 4 . 8 . 5 . 1 . 6 . 5 . 5 . 2 . 3 3 0 0 0 2 0 2 1 1 1 0 7 7 4 2 0 8 2 1 4 0 0 0 2 1 0 1 1 5 7 1
g 3 3 0 1 9 4 4 7 5 6 7 9 7 8 5 0 2 5 7 9 6 3 7 3 8 1 8 k / 2 . 8 . 0 . 6 . 0 . 3 . 1 . 3 . 5 . 4 . 7 . 6 . 8 . 2 . 8 . 2 . 0 . 2 . 5 . 1 . 3 . 0 . 7 . 2 . 5 . 0 . 8 . 1 . g 9 5 2 6 3 6 1 9 6 2 2 6 1 3 6 5 6 6 8 0 3 2 7 2 9 0 4 0 m 1 3 9 2 1 3 1 7 4 4 5 0 8 8 7 8 1 1 3 2 1 1 1 , 2 1 1 6 1 X 3 2 1 l e k c i n r o f s c i t s i t a t s e t a c i l p u d d n i l B
k c d i l o o k m R s c d u o o e n s s i r t o e p h b e s l e B n t e n n 1 7 3 y P 2 r 2 a b o a 9 + n e a d o 1 0 0 g u i e w t r - t i k - - i t f l r n o / c t l 0 P P i n 4 a c l e k 3 4 1 p P o r a e f i t r c a t e a b P 0 0 + 0 u s e 2 O f / l A A A f c e k r u z l r s e a P i 0 n u A c d t o e h c y 0 S u i f A 0 0 0 l m a D o M e l i d 2 o i t r D A s o c s x 2 n s m s 2 2 D u e k r n n r r b r d m m h h y a n n t e o r Z y t r r r M r s x e p e e u a r / a d e l u c x e a f t e e e c d d e e i o i h n f n d d b d n n t o e e e W o r c i e l r t e F d e i d s % o t s s N C r l n / r o o h 4 e u u u o w c a a N f e K 1 l e a e P u r r r o p l t d p 9 l F B C g g a g n u e F x C 3 i A a r g l o b m r i 6 m t W / g P W m a a a P Z n M o r o l a e a o r e M F f - O m a M M N M K B h S M M r c C A i P R t P G n a S A N a e g D F T r S I O N .
F 3 0 . 6 0 0 2 e l b a T
5 8 6 0 9 6 5 7 0 5 2 8 5 1 7 2 9 4 8 1 6 9 4 3 4 0 7 7 D I 2 3 3 9 6 5 8 6 9 7 1 1 6 3 3 9 6 7 8 0 0 4 6 8 2 4 3 8 9 4 8 6 0 0 2 9 3 8 4 1 9 3 6 4 7 0 4 6 1 2 5 9 3 5 8 e 0 l / 5 / 1 / 5 / 7 / 2 / 4 / 6 / 6 / 3 / 4 / 7 / 8 / 8 / 4 / 3 / 9 / 9 / 8 / 3 / 4 / 5 / 2 / 6 / 7 / 1 / 8 / 3 / p 2 1 1 1 8 8 5 8 3 1 9 1 8 7 9 5 6 3 6 6 1 6 7 0 3 4 1 3 m 2 3 4 8 1 1 7 1 6 9 0 3 1 5 9 4 7 8 2 1 1 9 6 8 2 3 2 8 a 3 0 3 4 8 6 9 3 1 9 5 7 9 4 8 9 8 8 6 4 7 3 7 8 9 1 6 8 8 S 4 4 6 5 2 1 9 3 7 7 6 7 3 4 6 7 8 9 4 6 3 4 4 6 4 4 5 7
ã 2009 AOAC INTERNATIONAL
s r e 0 i l t / u 0 O
0 / 0 / 0 / 0 / 0 3 0 1
0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 1 / 0 / 4 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 / 0 1 1 1 0 2 1 0 0 1 0 1 0 0 0 0 0 1 0 1 1 0 0
t a 4 R r 2 . o 8 H
7 5 7 6 3 . 2 . 9 . 9 . 6 5 0 1
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1 5 9 . R 7 . 6 4 1 1 6 2 2
9 1 6 0 0 . 3 3 8 . . . 7 3 2 2 6 5 5 8 1 8 1
5 1 9 r 7 . . 4 6 1 1 2 6 2
8 4 0 9 0 9 . 8 . 8 . . 0 5 9 7 4 1 6 4 8 1
. G 3 0 . 6 0 0 2 e l b a T
8 2 9 5 9 5 5 7 2 7 1 4 5 3 8 4 9 3 6 5 5 5 2 2 3 7 6 5 3 7 5 0 5 5 9 . . . . . . . . . . . . 7 . 7 . 3 . 5 . 7 . 5 . 2 . 2 . 6 . 4 . 1 0 0 1 0 0 6 9 1 1 0 1 0 5 7 2 3 4 1 1 1 2 2 4 3 1 9
% 3 , R 1 . D 4 S 6 R
4 1 6 5 4 . 2 . 4 . 2 . 0 9 5 9 3 7
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% , r 3 . D 1 S 4 6 R
4 0 4 5 4 . 5 . 6 . 5 . 0 3 1 4 3 2
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0 R . s 7 6 7
1 8 1 7 6 . 1 . 4 . 5 . 4 1 4 4 3 5 0 9 3
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r 0 s 7 . 6 7
1 5 7 3 6 . 3 . 3 . 9 . 4 0 6 9 3 1 4 9 1
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1 9 5 6 1 . 4 . 2 . 0 . 0 1 6 2 7 9 9 0 9 2 3 3
7 5 7 8 8 1 4 0 5 4 2 2 1 9 3 4 8 4 3 4 5 5 8 4 7 2 0 5 8 1 6 3 5 5 4 5 2 5 3 0 9 7 7 . . . . . . . . . . . . . . . . . . . 9 . 0 . 8 . 2 . 5 1 3 3 3 1 0 5 9 6 3 0 6 8 3 3 1 3 3 0 5 4 9 7 4 0 6 5 4 1 1 0 2 5 3 4
e n t o a i t f p l i r u c s s y e x d o e e F l p l a m t a e S M
e t s B a 9 e 0 w - 4 t a 2 O e f l 0 S u i 0 n s n 2 Z y m r x d e e d % o c t a u r 1 n l 3 i u g Z n a a r M G
k c d i l o o k m R s c d u o o n s s i r o e p h b e e n 1 7 n 3 l y P 2 r 2 b + n e a d o 1 0 0 g u t / n k r - t i - - i l o c r P n P i a c l e k 1 o e a e a b r f t r c P 3 4 A A f / l P c e k 0 + 0 u s i z m t r f e h a u A M D A P A 0 c t d e 0 0 0 l a o e l s c o o i i t r s D A D 2 2 d 2 o h u r m n h r b y a n r d m n t r p c e e u e t M a r r l s e k u n x d r r e r / a a f t e e e c e o e t o r t h n f n d d b d n i e e W o r c i n d s l i e i s s N C r n / r o o h 4 e u u u o w a a N f e K e e P r r r o t l d p 9 F B o b 6 C C g g - g l a g x A e F W W m i r / P m a a - a P o r o l M o r e M F f - O m M M N M K B h c C A i P R t P n a S A N a e g D F T r S I O N
5 D I 2 e 0 l / p 2 m 1 a 2 3 S 4
8 6 0 9 3 3 9 6 9 4 8 6 5 / 1 / 5 / 7 / 1 1 8 8 3 4 8 1 0 3 4 8 4 6 5 2
6 5 7 0 5 2 8 5 1 7 2 9 4 8 1 6 9 4 3 4 0 7 7 5 8 6 9 7 1 1 6 3 3 9 6 7 8 0 0 4 6 8 2 4 3 8 0 0 2 9 3 8 4 1 9 3 6 4 7 0 4 6 1 2 5 9 3 5 8 2 / 4 / 6 / 6 / 3 / 4 / 7 / 8 / 8 / 4 / 3 / 9 / 9 / 8 / 3 / 4 / 5 / 2 / 6 / 7 / 1 / 8 / 3 / 5 8 3 1 9 1 8 7 9 5 6 3 6 6 1 6 7 0 3 4 1 2 3 1 7 1 6 9 0 3 1 5 9 4 7 8 2 1 1 9 6 8 2 3 8 8 6 9 3 1 9 5 7 9 4 8 9 8 8 6 4 7 3 7 8 9 1 6 8 1 9 3 7 7 6 7 3 4 6 7 8 9 4 6 3 4 4 6 4 4 5 7
g k / 0 g 6 . m 9 , X 1 1
d a e l r o f s c i t s i t a t s e t a c i l p u d d n i l B
8 1 4 4 6 9 1 0 3 5 3 1 5 1 6 3 0 4 6 1 6 8 8 . 7 . 3 . 3 . 1 . 4 . 6 . 9 . 2 . 1 . 4 . 7 . 9 . 1 . 5 . 5 . 5 . 5 . 3 . 3 . 6 . 6 . 3 8 7 7 4 2 3 6 2 7 1 9 5 7 0 4 5 8 6 8 8 9 5 1 1 4 1 0 1 1 1 1
ã 2009 AOAC INTERNATIONAL
s r e 0 0 0 0 0 0 0 0 0 0 1 2 0 0 0 0 0 0 0 1 0 0 0 0 0 0 0 0 i l / / / / / / / / / / / / / / / / / / / / / / / / / / / t / u 1 0 0 1 1 0 1 0 0 0 0 0 0 1 0 0 1 1 0 0 0 2 0 1 0 0 1 0 O t a 2 0 4 4 9 7 8 8 2 5 6 5 8 4 0 8 6 4 0 0 5 5 3 1 6 1 8 7 R r 9 . 2 . 3 . 4 . 6 . 6 . 9 . 6 . 5 . 0 . 5 . 9 . 9 . 0 . 8 . 6 . 1 . 2 . 9 . 9 . 0 . 3 . 8 . 4 . 2 . 2 . 5 . 1 . o 8 8 5 4 7 5 5 7 7 7 6 5 6 1 7 4 2 2 2 5 9 1 5 8 1 4 2 6 1 3 1 1 H
7 6 2 0 3 2 8 7 3 4 9 1 0 0 6 8 3 7 4 3 8 2 8 3 8 9 7 1 R 7 . 9 . 9 . 3 . 1 . 3 . 7 . 5 . 7 . 0 . 8 . 7 . 4 . 8 . 9 . 6 . 4 . 7 . 6 . 1 . 1 . 0 . 2 . 3 . 1 . 7 . 6 . 7 . 0 7 8 7 9 0 3 4 3 5 2 2 8 1 5 4 4 6 0 4 5 8 7 7 5 2 4 6 2 6 5 4 5 1 1
2 9 4 0 9 2 2 6 1 0 5 3 8 2 7 9 3 7 6 6 5 0 5 1 7 4 8 1 r 4 . 2 . 8 . 3 . 7 . 0 . 0 . 2 . 6 . 3 . 7 . 1 . 7 . 8 . 0 . 2 . 5 . 2 . 0 . 8 . 0 . 1 . 2 . 8 . 4 . 9 . 3 . 1 . 2 2 1 1 3 8 1 3 0 2 1 1 3 0 3 2 0 2 3 3 2 1 4 1 3 1 1 3 1 2
% 3 3 2 4 6 1 6 4 6 6 0 5 8 9 9 0 2 5 4 4 3 1 8 2 5 9 9 5 , R 5 . 2 . 6 . 4 . 3 . 6 . 0 . 8 . 1 . 8 . 3 . 9 . 6 . 1 . 4 . 3 . 0 . 5 . 2 . 1 . 6 . 5 . 7 . 6 . 6 . 7 . 1 . 3 . D 6 8 7 6 4 5 0 6 8 3 5 4 3 7 3 9 4 5 5 7 4 7 7 9 3 2 2 4 1 4 3 2 8 8 1 6 7 1 1 6 3 8 S 0 7 6 5 7 5 9 1 1 0 0 9 9 1 1 1 1 1 2 6 1 1 1 1 R 1 % 3 5 7 8 7 5 5 4 2 6 6 8 0 9 5 6 7 7 0 9 8 1 6 1 4 2 9 4 , r 4 1 9 0 7 0 2 3 2 4 8 6 1 8 3 7 6 5 3 2 4 9 3 5 1 7 4 1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . D 2 3 0 4 1 4 3 9 7 3 9 2 2 8 1 5 8 3 1 5 2 5 9 9 3 9 9 S 1 4 1 1 1 1 2 8 1 4 6 3 4 5 2 7 5 8 1 2 4 2 4 3 1 R
2 7 9 1 2 0 5 3 3 0 3 7 0 0 3 7 8 2 0 8 2 7 0 2 5 0 7 0 R . 2 . 1 . 6 . 1 . 4 . 3 . 6 . 3 . 8 . 0 . 9 . 0 . 5 . 1 . 6 . 5 . 4 . 8 . 4 . 4 . 8 . 6 . 6 . 8 . 0 . 6 . 4 . s 4 7 4 3 2 1 4 1 1 1 1 1 0 3 8 2 1 1 2 3 1 5 2 2 2 1 1 1 2 2 2 1 1
6 7 5 6 6 7 2 2 3 1 5 4 0 2 9 1 9 8 3 9 2 5 4 9 9 1 r 7 9 s 8 . 3 . 6 . 4 . 3 . 8 . 3 . 1 . 2 . 8 . 6 . 4 . 3 . 4 . 1 . 8 . 1 . 8 . 0 . 3 . 7 . 3 . 5 . 6 . 2 . 6 . 4 . 1 . 0 4 0 0 1 2 0 1 0 0 0 0 1 7 1 0 0 0 1 1 0 0 1 0 1 0 0 1
g k / 6 3 1 2 0 0 0 0 3 3 8 2 0 7 8 7 5 7 5 9 3 1 4 9 6 9 8 4 g 9 0 7 6 4 9 5 4 1 7 9 0 2 1 8 6 2 4 0 6 7 7 3 1 5 5 1 8 . . . . . . . . . . . . . . . . . . . . . . . . . . . . m 6 1 4 4 8 5 1 1 1 1 0 1 3 7 1 0 0 9 2 1 4 1 3 2 3 1 5 2 , 3 2 2 5 1 X 2
m u i n e l e s r o f s c i t s i t a t s e t a c i l p u d d n i l B . H 3 0 . 6 0 0 2 e l b a T
k c d i l o o k m R s c d u o o e n s s i r t o e p h b e s l e B n t e n n 1 7 3 y P 2 r 2 a b 9 o + n e a d o 1 0 0 g a 0 i e w t / n k r - t i - - i t f l r u o c t l P n P i 4 a c l e r c k 4 1 p u 2 r e a t a e f i P 3 A A f l P / c u o a b e k 0 0 + 0 d r s 0 O f s i z m e r t A e h a t P u n A c o e c y 0 S l A f 0 0 0 l a D o i s D M e l i d r i A s o c s x 2 n u o t 2 2 2 D s h u r m n h r b y r d m n m x a n e k e n r p c e e u e t M a r r l r r t s e r r Z y / a d o u x a f t e e b e d o i d t e o C i e t i W c r i h n f n d e e e e c o s n d d o e r n l e e d s t s d % r l F n / N r o o h 4 e u u u o w a l e e N e p F B d o 9 1 c a t P f r r K r a a u p l l C g r n x C 3 A a F l i g g g e i m o b m r 6 u m t W / g P W a a - a P Z n M o r o l a e a o r e M F f - O m a M M N M K B h S M M r c C A i P R t P G n a S A N a e g D F T r S I O N
5 8 6 0 9 6 5 7 0 5 2 8 5 1 7 2 9 4 8 1 6 9 4 3 4 0 7 7 D I 2 3 3 9 6 5 8 6 9 7 1 1 6 3 3 9 6 7 8 0 0 4 6 8 2 4 3 8 9 4 8 6 0 0 2 9 3 8 4 1 9 3 6 4 7 0 4 6 1 2 5 9 3 5 8 e 0 l / 5 / 1 / 5 / 7 / 2 / 4 / 6 / 6 / 3 / 4 / 7 / 8 / 8 / 4 / 3 / 9 / 9 / 8 / 3 / 4 / 5 / 2 / 6 / 7 / 1 / 8 / 3 / p 2 1 1 1 8 8 5 8 3 1 9 1 8 7 9 5 6 3 6 6 1 6 7 0 3 4 1 3 m 2 3 4 8 1 1 7 1 6 9 0 3 1 5 9 4 7 8 2 1 1 9 6 8 2 3 2 8 a 3 0 3 4 8 6 9 3 1 9 5 7 9 4 8 9 8 8 6 4 7 3 7 8 9 1 6 8 8 S 4 4 6 5 2 1 9 3 7 7 6 7 3 4 6 7 8 9 4 6 3 4 4 6 4 4 5 7
ã 2009 AOAC INTERNATIONAL
volumetric flask, dilute to volume with H 2O, mix, and transfer to an acid-washed polypropylene bottle.
for instrument drift. The inclusion of a digestion blank, a sample duplicate, and known reference materials is highly encouraged.
(h) Sampler wash solution, 1% HNO3.—Dilute 10 mL of trace metal grade HNO3 to 1000 mL with H2O.
I. Calculations
H. Determination
Analyze test solutions using an ICP-OES instrument calibrated with standard solutions. Insert a 10 mg/kg working standard or other suitable quality control solution every 10 test portions, to monitor
Element, mg / kg =
(instrument concentration, mg / L)(100 mL)(1 L / 1000 mL) (sample weight, g)(1 kg / 1000 g)
where 100 mL assumes the microwave digest is diluted to 100 mL. Reference: J. AOAC Int. 89, 1447(2006).
ã 2009 AOAC INTERNATIONAL
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