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Of fi cial Methods

of Anal y sis

of AOAC IN TER NA TIONAL

18th Edi tion, 2005

Current through Revision 1, 2006

Dr. Wil liam Horwitz, Ed i tor

Dr. George W. Latimer, Jr., Assistant Editor

Pub lished by

AOAC IN TER NA TIONAL

SUITE 500

481 NORTH FRED ER ICK AV E NUE

GAITHERSBURG, MARY LAND 20877-2417, USA

BY THE ASSOCIATION OF O FFICIAL A GRICULTURAL CHEMISTS

1970, 1975, 1980, 1984, 1990

BY THE A SSOCIATION OF O FFICIAL A NALYTICAL CHEMISTS

AND

1995, 1996, 1997, 1998, 1999, 2000, 2002, 2003, 2005, 2006

BY AOAC IN TER NA TIONAL

The meth ods of the As so ci a tion were also copy righted in 1916, when they were pub lished

in the Jour nal of the As so ci a tion of Of fi cial Ag ri cul tural Chem ists.

All rights re served. No part of this book may be re pro duced in any form or by any means

with out the writ ten per mis sion of the As so ci a tion.

Printed in the United States of Amer ica

Printed on acid-free pa per

ISBN 0-935584-77-3

A copy of the 18th Edition of this pub li ca tion is on file with the Of fice of the Fed eral Reg is ter.

U.S. Gov ern ment Agencies may ap ply to the Di rec tor of the Of fice of the Fed eral Reg is ter for

ap proval to in cor po rate this edi tion by ref er ence in their reg u la tions. The pro ce dures that Fed eral

agen cies must fol low in ap ply ing for the Di rec tor's ap proval are in Ti tle 1, Part 51, of the

Code of Fed eral Reg u la tions.

Im por tant No tices

DIS CLAIMER

METHODS

An a lyt i cal meth ods and pro ce dures in this com pen dium have un der gone sys tem atic interlaboratory stud ies to de ter mine

the per for mance char ac ter is tics for the in tended an a lyt i cal ap pli ca tion. AOAC IN TER NA TIONAL mem bers and other

vol un teers have re viewed the an a lyt i cal re sults and de ter mined that a par tic u lar method is ap pro pri ate for the analyte and

ma trix stated, pro vided the anal y sis is con ducted by a com pe tent an a lyst as writ ten. No war ranty, im plied or ex pressed, is

made by AOAC IN TER NA TIONAL on the meth ods de scribed, their safety, or prod ucts men tioned. AOAC

IN TER NA TIONAL, its mem bers, and non mem ber vol un teers who have aided in the de vel op ment and val i da tion

of meth ods in cluded in this vol ume as sume no re spon si bil ity for any eco nomic, per sonal in jury, or other dam age

that may oc cur to in di vid u als or or ga ni za tions be cause of the use of these meth ods.

COM MER CIAL PROD UCTS

Names of man u fac tur ers, sup pli ers, and trade names are fur nished solely as a mat ter of iden ti fi ca tion and con ve nience

and re flect the con di tions within which each method was de vel oped in the orig i na tor's lab o ra tory. In clu sion of this

in for ma tion does not im ply AOAC pro mo tion, ap proval, en dorse ment, or cer tif i ca tion. The same or equiv a lent

prod ucts, in stru ments, sup plies, ap pa ra tus, or re agents avail able from man u fac tur ers and sup pli ers other than

those named, or other brands from other sources, may serve equally well if proper val i da tion in di cates their use is

sat is fac tory.

WARNING

Do not per form anal y ses us ing AOAC® Of fi cial Methods SM un less you are knowl edge able about their po ten tial

dan gers or haz ards and have re ceived ap pro pri ate train ing. Do not han dle in stru ments, sup plies, ap pa ra tus, re agents,

biohazards, or other prod ucts when un fa mil iar with their op er a tion or the po ten tial haz ards as so ci ated with their use.

If a method re quires the use of po ten tially haz ard ous equip ment or prod ucts, see man u fac turer's safety and cau tion ary

in struc tions. Ma te rial Safety Data Sheets (MSDS), or the equiv a lent, must be read and un der stood prior to the use of

ma te ri als spec i fied by a method.

Al ways use fume hoods, proper ven ti la tion, and pro tec tive cloth ing and equip ment when re quired.

See Ap pen dix B, "Lab o ra tory Safety," for fur ther in for ma tion on safety.

REF ER ENCING AOAC® OF FI CIAL METHODS SM

Each AOAC® Of fi cial Method SM has its own per ma nent method num ber that is part of the ti tle block. The para graph

num ber lo cated in the up per left is only a lo ca tor num ber and not the method num ber. For ex am ple:

49.2.18A

AOAC Of fi cial Method 2005.08

Aflatoxins in Corn, Raw Peanuts,

and Peanut Butter

2005.08 is the per ma nent num ber of the method and 49.2.18A is the section num ber used to fa cil i tate lo cat ing

meth ods. Per ma nent num bers in di cate the year the method was ap proved (in this case 2005) fol lowed by the or der in

which the method was ap proved that year (in this ex am ple, it is the 8th method ap proved in 2005). The first set of

numbers in the section number indicates the chapter (in this case, Chapter 49), the second set indicates the subchapter

(in this case, subchapter 2), and the last set indicates the order in which the method appears in the subchapter (in this

case, it is the 18th method).

When ref er enc ing AOAC® Of fi cial Methods SM , only the per ma nent num ber should be ref er enced as seen in this

ex am ple:

(1) Of fi cial Methods of Anal y sis of AOAC INTERNATIONAL

(2005) 18th Ed., AOAC IN TER NA TIONAL,

Gaithersburg, MD, USA, Of fi cial Method 2005.08

RE VI SIONS

AOAC pub lishes an nual re vi sions to the Of fi cial Methods of Anal y sis of AOAC IN TER NA TIONAL. Re vi sions

con tain new meth ods ap proved since the last pub li ca tion and re vi sions to ex ist ing meth ods. You will au to mat i cally

re ceive no tice of the avail abil ity of new re vi sions and be sent an ad vance in voice al low ing you to pur chase the

re vi sions with out ob li ga tion. If you main tain the re vi sion ser vice, your 18th Edi tion will be cur rent.

For additional revisions received after the first printing (2005) of the 18th Edition, visit AOAC's Web site at

www.aoac.org for the Official Methods of Analysis online. These revisions will be included in a subsequent printing.

(Note: In di vid ual cop ies of re vi sions will be pro vided on an an nual ba sis only. AOAC IN TER NA TIONAL

will not re tain back cop ies of re vi sions for sale. If you do not pur chase re vi sions on an an nual basis, you will

need to buy an en tire new book to ob tain miss ing re vi sions.)

IN QUIRIES

In quiries re gard ing meth ods pub lished in this book should be di rected to AOAC IN TER NA TIONAL, Of fi cial

Methods Pro gram, 481 N. Fred er ick Ave, Suite 500, Gaithersburg, MD 20877-2417, USA. Tele phone

+1-301-924-7077. Fax +1-301-924-7089. E-mail: aoac@aoac.org. Please note that due to the time nec es sary to

an swer any tech ni cal ques tions re gard ing an AOACâ Of fi cial Method SM , AOAC staff pro vides tech ni cal as sis tance

re gard ing meth ods in OMA to AOAC mem bers only.

In quiries re gard ing pur chase of Of fi cial Methods of Anal y sis or the re vi sion ser vice, the Jour nal of AOAC

IN TER NA TIONAL, or other AOAC pub li ca tions should be di rected to AOAC IN TER NA TIONAL, Fulfillment, 481

N. Fred er ick Ave, Suite 500, Gaithersburg, MD 20877-2417, USA. Tele phone +1-301-924-7077. Fax

+1-301-924-7089. E-mail: aoac@aoac.org.

COM MENTS ON METHODS

AOAC IN TER NA TIONAL adopts meth ods that show by their per for mance data what can be ex pected of them. As

an a lysts use AOAC® Of fi cial Methods SM , they gen er ate ad di tional in for ma tion and data con cern ing ap pli ca bil ity,

spec i fic ity, sen si tiv ity, re li abil ity, and ac cu racy of the meth ods. An a lysts are re quested to ad vise AOAC

IN TER NA TIONAL about their ex pe ri ences with the AOAC® Of fi cial Methods SM pub lished in this book. In par tic u lar,

an a lysts should no tify AOAC IN TER NA TIONAL of prob lems in the per for mance of an Of fi cial Method SM , which

may in di cate the method should be re vised or re stud ied. Di rect com ments to AOAC IN TER NA TIONAL, Of fi cial

Methods Pro gram, 481 N. Fred er ick Ave, Suite 500, Gaithersburg, MD 20877-2417, USA. Tele phone

+1-301-924-7077. Fax +1-301-924-7089. E-mail: aoac@aoac.org.

Pref ace

Elec tronic pub lish ing ar rived just in time to save the Of fi cial Methods of Anal y sis of AOAC

IN TER NA TIONAL from its own suc cess. Each of the two vol umes of the pre vi ous 17th Edition has

grown to an al most un man age able size. Now, for the first time, the re sults of 122 years of re view and

ap proval of col labor atively stud ied meth ods are captured on the Internet. The older meth ods are still there,

but their use is prob a bly con fined to teach ing "ag ri cul tural chem is try." The prop er ties of meth ods do not

de te ri o rate with age and the "clas si cal" analytes still need to be de ter mined. But the change in em pha sis with

the reg u la tory winds is ob vi ous: Mi cro bi ol ogy and nu tri tion have blos somed as reg u la tory em pha sis has

shifted from eco nom ics to safety and health. New drug and food ad di tive ap proval, based on preclearance of

man u fac tur ing op er a tions and con tin u ous qual ity con trol as well as safety and ef fi cacy, have re duced the

need for reg u la tory con trol through mar ket sam pling and anal y sis.

Most no ta ble has been the shift from clas si cal stoichiometric chem is try, based on the bal ance and buret, to

cal i bra tion chem is try, based on an in stru men tal com par i son of a re sponse of an analyte with that of a

stan dard. This shift was ini ti ated by the re mark able sep a ra tion pow ers of chro ma tog ra phy al low ing an

analyte to be sep a rated from in ter fer ing com po nents be fore be ing mea sured by the in stru ment.

Chro ma tog ra phy moved an a lyt i cal chem is try from the realm of gram quan ti ties into mi cro gram quan ti ties

but not with out un rec og nized sam pling prob lems. The sen si tiv ity, sta bil ity, and speed of mod ern elec tron ics

per mit the per for mance of an a lyt i cal work au to mat i cally, from the mea sure ment of the test por tion, through

de tec tion, am pli fi ca tion, and in ter pre ta tion of the sig nal, to the print ing of the an a lyt i cal re port.

The an a lyt i cal prob lem has shifted from mea sure ment to con trol. Much of the an a lyt i cal op er a tion has

moved from an op er a tor to a black box in a com puter. Changes in phys i cal prop er ties, such as light

in ten si ties or ion con duc tances, are mea sured au to mat i cally and con verted into an a lyt i cal re ports

con tin u ously, chang ing the lab o ra tory into an au to mated fac tory. But the fa cil ity for au to mated per for mance

al lows the re spon si bil ity for re li abil ity to eas ily shift from the an a lyst to the in stru ment. This is also true of

the blind ap pli ca tion of com puter pro grams with no re view of the ap pli ca bil ity of the pro gram to the

prob lem. The com puter has the abil ity not only to ex tract hid den in for ma tion from a jun gle of back ground,

but also to for mu late spu ri ous peaks that it has been pro grammed to guess ought to be there.

AOAC ini ti ated the pro ce dure of val i da tion of meth ods through interlaboratory stud ies. These stud ies

pro duce re sults from a sin gle sam ple of method per for mance in the hands of an as sumed ran dom sam ple of

lab o ra to ries. Un for tu nately, time and ex pense rarely per mit per form ing ad di tional stud ies. There fore, the

ini tial stud ies usu ally stand as the sole pub lished ev i dence of sat is fac tory interlaboratory per for mance.

AOAC mem bers are in ves ti gat ing sur ro gates for this nec es sary, but lengthy and costly pro ce dure.

Seventy-seven new meth ods have been added to this edi tion, pre dom i nantly mi cro bi o log i cal or

chro mato graphic in na ture, all of them sub jected to the rig ors of an interlaboratory study. Many of these

meth ods in cor po rate in ter nal con trols to en sure that the re ac tions are pro ceed ing as in tended. Most

ap peal ing is the in tro duc tion of sys tem suit abil ity spec i fi ca tions into chro mato graphic sys tems that per mit

flex i bil ity with out sac ri fic ing re li abil ity. For over a cen tury, the guid ing prin ci ple in the ap pli ca tion of

stan dard meth ods has been to fol low in struc tions to the let ter to ob tain re sults equiv a lent to those orig i nally

ob tained. But the com pe ti tion for im prove ments in sys tems ad vanced the sci ence of sep a ra tion and

de tec tion so rap idly that suit abil ity spec i fi ca tions for in tro duc ing flex i bil ity with out sac ri fic ing

per for mance had to be in vented.

In ter nal con trols re quire that the meth ods meet re peat abil ity per for mance spec i fi ca tions. An ap pre cia ble

frac tion of the new mi cro bi o log i cal meth ods are screen ing tests in volv ing pre as sem bled immunoassays

kits. Rel a tively quickly, these kits sep a rate lab o ra tory sam ples that can be dis carded as neg a tive from those

that pre sum ably con tain patho genic or gan isms, re quir ing the ap pli ca tion of con fir ma tory tests. These kits

also in vari ably con tain the re quire ment for ac com pa ny ing pos i tive and neg a tive con trols that pro vide

con cur rent as sur ance of proper per for mance.

This edi tion joins the uni ver sal move ment to ward the use of the in ter na tional sys tem (SI) of units, many of

which are un fa mil iar to U.S. sci en tists. Dur ing a tran si tion pe riod, both the com mon sys tem as well as the SI

sys tem will be given. Note that the term "nor mal ity" is be ing re placed by "moles per li ter." An other ed i to rial

change be ing in tro duced is to move away from the ten dency to des ig nate any thing be ing worked on as the

"sam ple." In stead, the se quence of "lab o ra tory sam ple" ÷ "test sam ple" ÷ "test por tion" is be ing

in tro duced. This vo cab u lary is be ing used by the In ter na tional Un ion Of Pure and Ap plied Chem is try

(IUPAC) and the In ter na tional Or ga ni za tion for Stan dard iza tion (ISO), which does not per mit the

un mod i fied term "sam ple" to be used in con junc tion with sub se quent chem i cal op er a tions.

An im por tant fea ture of the 18th Edi tion is the in ter na tional source of many of the meth ods, with many

coun tries and in ter na tional or ga ni za tions con trib ut ing their ex per tise to method stan dard iza tion. It is also

grat i fy ing to see the in tro duc tion of qual ity con trol fea tures into the meth ods, which pro vide the an a lyst with

guides to proper per for mance. On the other hand, the ease with which re sults are ob tained from com put ers

also per mits the in tro duc tion of un an tic i pated er rors, de tected only by the un rea son able ness of the re sults. In

the ab sence of a blue print of what is to be ex pected, gross er rors may be made. The in tro duc tion of qual ity

as sur ance prin ci ples into the lab o ra tory may as sist in min i miz ing such oc cur rences.

Nu mer ous in di vid u als, vol un teer sci en tists, and pro fes sional staff have con trib uted en thu si as ti cally to

this cen tury-old pro gram of method val i da tion. The an a lyt i cal com mu nity is grate ful for their con tin ued

valu able ef forts.

—Wil liam Horwitz, Ed i tor

Contents

List of Changes for Revision 1, 2006.............iii

Im por tant No tices.......................vi

Pref ace ...........................viii

About the As so ci a tion ....................xiv

Guide to Method For mat ..................xvi

Def i ni tion of Terms and Ex plan a tory Notes ........xvii

AOAC® Of fi cial Methods SM Val i da tion Pro gram .....xxiv

1. Ag ri cul tural Liming Ma te rials

1.1 Liming Ma te rials—Gen eral .............1

1.2 Cal cium Sil i cate Slags ...............3

1.3 Gravimetric El e men tal Anal y ses ..........4

1.4 Chelometric El e men tal Anal y ses ..........6

1.5 Colorimetric El e men tal Anal y ses ..........6

2. Fer til izers

2.1 Fer til izers—Gen eral ................1

2.2 Wa ter ........................4

2.3 Phos pho rus .....................5

2.4 Ni tro gen ...................... 12

2.5 Po tas sium ..................... 21

2.6 Other El e ments .................. 25

2.7 Peat ........................ 36

2.8 Soils ........................ 40

3. Plants

3.1 Gen eral Methods ..................1

3.2 Metals ........................2

3.3 In di vid ual Metals ..................5

3.4 Non metals .....................13

3.5 Other Con stit u ents .................23

3.6 Pig ments ......................28

3.7 To bacco ...................... 30

4. An i mal Feed

4.1 An i mal Feed—Gen eral ...............1

4.2 Pro tein ....................... 24

4.3 Urea ........................ 36

4.4 Ni tro gen ...................... 37

4.5 Fat ......................... 39

4.6 Fi ber ........................ 44

4.7 Sugars .......................55

4.8 Min erals ...................... 56

4.9 Mi cros copy ....................66

4.10 Ad di tives ..................... 68

5. Drugs in Feeds

5.1 Feeds—Gen eral Methods ..............1

5.2 Chem i cal Methods for An ti bi otics.........34

5.3 Mi cro bi o log i cal Methods

for An ti bi otics ...................41

Com mon and Chem i cal Names of Drugs .........60

6. Dis in fec tants

6.1 Phe nol Co ef fi cient Methods ............1

6.2 Hard Sur face Car rier Test Methods .........3

6.3 Other Tests..................... 17

7. Pes ti cide For mu la tions

7.1 Gen eral Methods ..................1

7.2 In or ganic and Organometallic Pes ti cides

and Adjuvants ....................8

7.3 Fun gi cides .....................22

7.4 Her bi cides ..................... 42

7.5 Pes ti cides Re lated to Nat u ral Prod ucts

and Their Syn er gists ................52

7.6 Organohalogen Pes ti cides .............63

7.7 Thiophosphorus and Other

Organophosphorus Pes ti cides ...........92

7.8 Mis cel la neous Pes ti cides .............115

Com mon and Chem i cal Names of Pes ti cides ......121

8. Haz ard ous Sub stances.......................1

9. Metals and Other El e ments at Trace Levels

in Foods

9.1 Multielement Methods ...............1

9.2 Sin gle El e ment Methods.............. 22

10. Pes ti cide and In dus trial Chem i cal Res i dues

10.1 Gen eral Multiresidue Methods ...........1

10.2 Organo chlorine Res i dues .............17

10.3 Organophosphorus Res i dues ............26

10.4 Fu mi gant Res i dues ................40

10.5 Carbamate Res i dues ................ 41

10.6 In di vid ual Res i dues ................48

10.7 Pes ti cides in Wa ter................. 78

Com mon and Chem i cal Names of Pes ti cides .......97

11. Wa ters; and Salt

11.1 Wa ter ........................1

11.2 Salt .........................31

12. Microchemical Methods ....................1

13. Ra dio ac tiv ity .............................1

14. Vet er i nary An a lyt i cal Tox i col ogy .............1

15. Cos metics

15.1 Gen eral Methods ..................1

15.2 De odor ants and An ti per spi rants...........6

15.3 De pil a tories ....................11

15.4 Face Pow der ....................11

15.5 Hair Prep a ra tions ................. 12

15.6 Sun tan Prep a ra tions ................13

16. Ex tra ne ous Ma te rials: Iso la tion

16.1 Gen eral .......................1

16.2 Bev er ages and Bev er age Ma te rials ..........6

16.3 Dairy Prod ucts ...................8

16.4 Nuts and Nut Prod ucts ...............13

16.5 Grains and Their Prod ucts .............15

16.6 Baked Goods ...................21

16.7 Break fast Ce reals ................. 23

16.8 Eggs and Egg Prod ucts ..............24

16.9 Poul try, Meat, and Fish and Other

Ma rine Prod ucts ..................25

16.10 Fruits and Fruit Prod ucts .............28

16.11 Snack Food Prod ucts ...............31

16.12 Sugars and Sugar Prod ucts ............31

16.13 Veg e ta bles and Veg e ta ble Prod ucts .........32

16.14 Spices and Other Con di ments ...........39

16.15 Mis cel la neous ................... 48

16.16 An i mal Ex cre tions ................. 56

16.17 Mold ........................ 66

16.18 Fruits and Fruit Prod ucts .............69

16.19 Veg e ta bles and Veg e ta ble Prod ucts .........70

17. Mi cro bi o log i cal Methods

17.1 Eggs and Egg Prod ucts ...............1

17.2 Chilled, Frozen, Pre cooked,

or Pre pared Foods, and Nutmeats ..........4

17.3 Coliforms .....................27

17.4 Esch e richia coli ..................50

17.5 Staph y lo coc cus ..................81

17.6 Ste ril ity (Com mer cial) of Foods

(Canned, Low Acid) ................99

17.7 Clostridium ....................104

17.8 Ba cil lus ......................113

17.9 Sal mo nella ....................117

17.10 Lis te ria ......................200

17.11 Vibrio .......................237

17.12 Vi ruse s ...................... 242

17.13 So matic Cells ................... 244

17.14 Bacillus anthracis ................246

18. Drugs: Part I

18.1 Gen eral Methods ..................1

18.2 Sol vents .......................2

18.3 Halogenated Drugs .................3

18.4 In or ganic Drugs ...................5

18.5 An ti his ta mines................... 18

18.6 Alkanolamines ...................21

18.7 Phenethylamines ..................27

18.8 Aminobenzoates ..................28

18.9 Syn thetics ..................... 32

18.10 Microchemical Tests................44

18.11 Mi cros copy ....................54

18.12 Mis cel la neous ................... 55

18.13 Antifungal .....................55

18.14 Antiparkinsonian .................56

18.15 Antihypertensive..................57

Com mon and Chem i cal Names of Drugs .........59

19. Drugs: Part II

19.1 Acids ........................1

19.2 Phe no lic Drugs ...................2

19.3 An al ge sics and Antipyretics ............7

19.4 Hyp notics and Sed a tives ..............13

19.5 An ti co ag u lants ...................20

19.6 Sul fona mides ...................24

19.7 Thiazides ..................... 27

19.8 Other Sul fur-Containing Drugs ..........30

Com mon and Chem i cal Names of Drugs .........36

20. Drugs: Part III

20.1 Opium Al ka loids ..................1

20.2 Tropane Al ka loids .................6

20.3 Xanthine Al ka loids .................7

20.4 Ip e cac Al ka loids ..................8

20.5 Ephedra Al ka loids .................9

20.6 Er got Al ka loids ..................11

20.7 Physostigmine Al ka loids .............14

20.8 Chinchona Al ka loids ...............16

20.9 Rau wol fia Al ka loids ................18

20.10 Other Al ka loids .................. 25

20.11 Dig i talis ...................... 27

20.12 Other Nat u ral Prod ucts ..............30

Com mon and Chem i cal Names of Drugs .........35

21. Drugs: Part IV

21.1 Nat u ral Estrogens ..................1

21.2 Syn thetic Estrogens .................3

21.3 Progestational Ste roids ...............6

21.4 Adrenocortico Ste roids ...............8

21.5 Thy roid ......................14

Com mon and Chem i cal Names of Drugs .........15

22. Drugs: Part V .............................1

Com mon and Chem i cal Names of Drugs ..........7

23. Drugs and Feed Ad di tives in An i mal Tis sues ...1

Com mon and Chem i cal Names of Drugs .........27

24. Fo ren sic Sci ences ..........................1

25. Baking Pow ders and Baking Chem i cals .......1

26. Dis tilled Li quors

26.1 Spirits ........................1

26.2 Cor dials and Li queurs ...............19

27. Malt Bev er ages and Brewing Ma te rials

27.1 Beer .........................1

27.2 Bar ley ....................... 23

27.3 Malt ........................ 24

27.4 Ce real Ad juncts ..................31

27.5 Hops ........................34

27.6 Brewing Sugars and Syrups ............36

27.7 Wort ........................ 38

27.8 Yeast ........................39

27.9 Brewers' Grains .................. 41

28. Wines

28.1 Gen eral .......................1

28.2 Pre ser va tives.................... 17

28.3 Fla vors .......................18

29. Nonalcoholic Bev er ages and Con cen trates........1

30. Cof fee and Tea ............................1

31. Ca cao Bean and Its Prod ucts

31.1 Gen eral .......................1

31.2 Shell.........................3

31.3 Choc o late Li quor ..................9

31.4 Fat..........................9

31.5 Other Con stit u ents .................12

32. Ce real Foods

32.1 Wheat Flour .....................1

32.2 Wheat, Rye, Oats, Corn, Buck wheat, Rice,

Bar ley, and Soy beans and Their Prod ucts

Ex cept Ce real Ad juncts ..............27

32.3 Bread ....................... 49

32.4 Baked Prod ucts ..................54

32.5 Mac a roni, Egg Noo dles, and Sim i lar

Prod ucts ......................56

33. Dairy Prod ucts

33.1 Sam pling ......................1

33.2 Milk .........................4

33.3 Cream ....................... 52

33.4 Evap o rated and Con densed Milk .........58

33.5 Dried Milk, Non fat Dry Milk,

and Malted Milk ..................59

33.6 But ter .......................63

33.7 Cheese .......................68

33.8 Ice Cream and Frozen Des serts ..........82

34. Eggs and Egg Prod ucts .....................1

35. Fish and Other Ma rine Prod ucts .............1

36. Fla vors

36.1 Gen eral Methods ..................1

36.2 Va nilla Ex tract and Its Sub sti tutes ..........1

36.3 Lemon, Or ange, and Lime Ex tracts,

Fla vors, and Oils..................12

36.4 Al mond Ex tract ..................18

36.5 Cassia, Cin na mon, and Clove Ex tracts ......20

36.6 Fla vor Ex tracts and Toi let

Prep a ra tions ....................21

37. Fruits and Fruit Prod ucts ...................1

38. Gel a tin, Des sert Prep a ra tions, and Mixes .......1

39. Meat and Meat Prod ucts ....................1

40. Nuts and Nut Prod ucts .....................1

41. Oils and Fats..............................1

42. Veg e ta ble Prod ucts, Pro cessed

42.1 Canned Veg e ta bles .................1

42.2 Dried Veg e ta bles ..................9

42.3 Frozen Veg e ta bles ................. 10

43. Spices and Other Con di ments ...............1

44. Sugars and Sugar Prod ucts

44.1 Sugars and Syrups .................1

44.2 Mo las ses and Mo las ses Prod ucts ......... 18

44.3 Con fec tion ary ...................24

44.4 Honey .......................25

44.5 Ma ple, Sap, Ma ple Syrup, Ma ple

Syrup Prod ucts...................37

44.6 Sugar Beets ....................47

44.7 Corn Syrups and Other Starch Derived

Sweeteners.....................48

45. Vi ta mins and Other Nu tri ents

45.1 Chem i cal Methods .................1

45.2 Mi cro bi o log i cal Methods .............53

45.3 Bioassay Methods .................70

45.4 Nu tri tionally Re lated Com po nents .........81

46. Color Ad di tives

46.1 Sep a ra tion and Iden ti fi ca tion of Color

Ad di tives in Foods, Drugs, and Cos metics .....1

46.2 In ter me di ates ................... 14

46.3 Sub sid iary and Lower Sulfonated Dyes ......21

46.4 Metals and Other El e ments ............22

46.5 Halo gens ......................25

46.6 Mis cel la neous ................... 26

47. Food Ad di tives: Di rect

47.1 Gen eral Methods ..................1

47.2 An ti ox i dants ....................1

47.3 Chem i cal Pre ser va tives ...............7

47.4 Emul sifying Agents ................37

47.5 En zymes ...................... 39

47.6 Mis cel la neous ................... 41

48. Food Ad di tives: In di rect ....................1

49. Nat u ral Toxins

49.1 Myco toxins .....................1

49.2 Aflatoxins ......................2

49.3 Af la toxin M1 .................... 41

49.4 Deoxynivalenol ..................48

49.5 Fumonisins ....................50

49.6 Ochratoxins ....................57

49.7 Patulin ....................... 69

49.8 Sterigmatocystin .................. 74

49.9 Zearalenone .................... 76

49.10 Sea food Toxins ..................80

49.11 Plant Toxins ....................96

50. In fant For mulas, Baby Foods,

and Enteral Prod ucts .......................1

51. Dietary Supplements

50.1 Ephedra Alkaloids .................1

50.2 Glucosamine ....................7

50.3 b -Carotene .....................10

Ap pen dix A

Stan dard So lu tions and Ref er ence Ma te rials ........1

Ap pen dix B

Lab o ra tory Safety ......................1

Ap pen dix C

Ref er ence Ta bles ......................1

Ap pen dix D

Guide lines for Col lab o ra tive Study Pro ce dures to

Val i date Char ac ter is tics of a Method of Anal y sis .....1

Ap pen dix E

Lab o ra tory Qual ity As sur ance ...............1

Sub ject In dex.................................1

In dex of Method Numbers ......................1

About the As so ci a tion

Dur ing the past 122 years, AOAC IN TER NA TIONAL

(for merly the As so ci a tion of Of fi cial An a lyt i cal Chem ists

and before that the Association of Official Agricultural

Chemists) evolved from a group of chem ists in the U.S. De part ment

of Ag ri cul ture and the individual states into an in de pend ent

sci en tific As so ci a tion of an a lyt i cal sci en tists with mem bers

through out the world. To day, AOAC is the leader in pro vid ing

val i dated meth ods, pro fi ciency test sam ples, ac cred i ta tion cri te ria,

and sci en tific in for ma tion to in dus try, gov ern ment agen cies, and

ac a demic in sti tu tions.

MIS SION

AOAC IN TER NA TIONAL ad vances the global chem is try and

mi cro bi ol ogy an a lyt i cal com mu nity by pro mot ing meth ods

val i da tion and qual ity mea sure ments.

AOAC METHODS VAL I DA TION PRO GRAMS

To fur ther its mis sion, the As so ci a tion's pri mary pro grams fo cus

on the val i da tion of chem i cal and mi cro bi o log i cal an a lyt i cal

meth ods. These val i da tion pro grams are: the AOAC® Of fi cial

MethodsSM Pro gram, the pro gram of choice when the high est level

of con fi dence is de sired; the AOAC® Peer-Verified MethodsSM

Pro gram, used when speed of val i da tion is es sen tial and a lesser

de gree of con fi dence is ac cept able; and the AOAC® Per for mance

Tested MethodsSM Pro gram used to test the per for mance of test kits.

Over 800 vol un teer sci en tists, work ing in in dus try, gov ern ment, and

ac a demic lab o ra to ries world wide largely ac com plish the ac tual

work of val i da tion.

The meth ods found in this 18th Edi tion of the Of fi cial Meth ods of

Anal y sis of AOAC IN TER NA TIONAL have been val i dated within

the AOAC® Of fi cial Meth ods SM Pro gram. Can di dates for AOAC®

Of fi cial MethodSM sta tus are sub jected to col lab o ra tive study by

eight or more lab o ra to ries, ac cord ing to in ter na tion ally rec og nized

stan dards and re ceive rig or ous sci en tific re view of per for mance

re sults (see page xxiv for ad di tional de tails of the AOAC® Of fi cial

Meth odsSM Val i da tion Pro gram).

AOAC val i dated meth ods are used by gov ern ment, in dus try, and

ac a de mia through out the world for anal y sis of a va ri ety of

com mod i ties—par tic u larly those re lated to food, ag ri cul ture, pub lic

health and safety, and the en vi ron ment. In fact, many of the

val i dated meth ods in this edi tion have been adopted by in dus try and

gov ern ment agen cies as de facto stan dards in the op er a tion of their

lab o ra to ries.

OTHER PRO GRAMS

The As so ci a tion also has sev eral pro grams that as sist lab o ra tory

man ag ers in mea sur ing the ac cu racy of an a lyt i cal re sults, im prove

pro fes sional de vel op ment, and pro vide the op por tu nity for sci en tists

to in ter act.

THE AOAC® LAB O RA TORY

PRO FI CIENCY TESTING PRO GRAM

The AOAC® Lab o ra tory Pro fi ciency Testing Pro gram pro vides

an in de pend ent as sess ment of the ac cu racy and re li abil ity of

an a lyt i cal re sults in the anal y sis of a wide range of analytes and

ma trix. Pro gram mod ules in clude Stan dard Mi cro bi ol ogy, HACCP,

Nu tri tional La beling, and Pes ti cide Res i dues in Fruits and

Veg e ta bles.

TECH NI CAL DI VI SIONS

The goals of the AOAC tech ni cal di vi sions are to im prove the

over all qual ity of lab o ra tory op er a tions and fos ter har mo ni za tion of

lab o ra tory pro ce dures and sys tems. The Tech ni cal Di vi sion for

Lab o ra tory Man age ment helps lab o ra tory man ag ers im prove the

op er a tions of their lab o ra to ries through the ex change of ideas and

through pro fes sional de vel op ment ac tiv i ties. The Tech ni cal

Di vi sion on Ref er ence Ma te rials im proves the qual ity of an a lyt i cal

mea sure ments through the use of ref er ence ma te ri als.

TRAINING COURSES

AOAC IN TER NA TIONAL of fers a se ries of courses that pro vide

hands-on train ing in spe cific top i cal ar eas, and as sist an a lyt i cal

sci en tists to ac quire the skills they need to ad dress daily chal lenges

faced in their lab o ra to ries. Cur rent of fer ings in clude courses on

qual ity as sur ance for an a lyt i cal and mi cro bi o log i cal lab o ra to ries,

ISO 17025, ISO au dit sys tems, and single laboratory validation.

CO OP ER A TIVE AC TIV ITIES

AOAC IN TER NA TIONAL has es tab lished joint com mit tees,

li ai sons, and rep re sen ta tion with nu mer ous sci en tific or ga ni za tions

world wide. The As so ci a tion serves as the Sec re tar iat of the

In ter Agency Meet ing, an af fil i a tion of 16 in ter na tional

or ga ni za tions ac tive in the field of anal y sis and sam pling of food

prod ucts and as so ci ated qual ity as sur ance mea sures in conjunction

with the Joint FAO/WHO Codex Alimentarius. The As so ci a tion

also par tic i pates in the meet ings of the Co dex Alimentarius

Com mis sion, the In ter na tional Or ga ni za tion for Stan dard iza tion

(ISO), the Eu ro pean Com mu nity for Stan dard iza tion, the World

Health Or ga ni za tion, the Pan Amer i can Health Or ga ni za tion, and

other in ter na tional groups, both pri vate and gov ern ment spon sored.

Such ar range ments en able AOAC IN TER NA TIONAL to ex press its

ba sic pol i cies on the de vel op ment of in ter na tion ally ac cept able

meth ods of anal y sis and pro vide sec re tar i ats with ba sic in for ma tion

re gard ing AOAC's phi los o phy and pro ce dures.

AOAC-appointed Li ai son Of fi cers co or di nate AOAC ac tiv i ties

with na tional, state, pro vin cial, mu nic i pal, lo cal agen cies and

in dus tries and their af fil i ated or ga ni za tions, and other method

or ga ni za tions that have oral or writ ten co op er a tive agree ments with

AOAC IN TER NA TIONAL.

MEET INGS AND EX PO SI TIONS

The AOAC IN TER NA TIONAL An nual Meet ing and Ex po si tion

is rec og nized world wide as the most sig nif i cant meet ing for qual ity

as sur ance and lab o ra tory man age ment pro fes sion als dealing with

regulated commodities. The an nual sci en tific pro gram in cludes

cut ting-edge in for ma tion from the world's most re spected sci en tists

and lab o ra to ries. Through the sci en tific sym po sia, poster ses sions,

work shops, fo rums, and short courses, meet ing at ten dees en hance

their an a lyt i cal ex per tise, share their re search, and strengthen

con tacts with their col leagues from around the world. The An nual

Lab o ra tory Ex po si tion held at the An nual Meet ing fea tures over 100

dis plays of the state of the art in lab o ra tory prod ucts and ser vices.

SEC TIONS

AOAC IN TER NA TIONAL has 16 Sec tions lo cated in North

Amer ica, Eu rope, Ja pan, China, Taiwan, Latin Amer ica, and the

Ca rib bean. Sec tions pro vide op por tu ni ties for AOAC mem bers to

gather and share in for ma tion on a more lo cal level, to build and

ex pand their net work of pro fes sional con tacts, en hance their

lead er ship skills, and gain prac ti cal man age ment ex pe ri ence. All

Sec tions are man aged by an elected group of lo cal vol un teers.

PUB LI CA TIONS

In ad di tion to the Of fi cial Methods of Anal y sis of AOAC

IN TER NA TIONAL, the As so ci a tion pub lishes the Jour nal of AOAC

IN TER NA TIONAL and a va ri ety of other pub li ca tions. AOAC's

Jour nal con tains orig i nal fully ref er eed re search ar ti cles and re ports

on cur rent col lab o ra tive study data, in clud ing in for ma tion on inter-

and intralaboratory per for mance pre ci sion, which en ables the us ers

of the AOAC® Of fi cial Methods SM to make in formed choices about

the ap pro pri ate use of a par tic u lar method. In side Lab o ra tory

Man age ment, a full-color bimonthly mag a zine con tains tech ni cal

and gen eral ar ti cles on lab o ra tory man age ment, reg u la tions,

emerg ing tech nol o gies, in stru men ta tion, and other ar eas per ti nent to

lab o ra tory pro ce dures, man age ment, and qual ity con trol.

AOAC's other pub li ca tions in clude man u als, meth ods

com pi la tions, and mono graphs cov er ing sub jects that in clude

qual ity as sur ance, sta tis tics, food anal y sis, ag ri cul tural anal y sis,

lab o ra tory man age ment, and pes ti cide anal y sis.

AWARDS

Each year, the As so ci a tion pres ents a num ber of awards in

rec og ni tion of out stand ing con tri bu tions to an a lyt i cal meth od ol ogy

in ar eas of in ter est to AOAC IN TER NA TIONAL, mer i to ri ous

ser vice to the As so ci a tion, and out stand ing work in the AOAC®

Of fi cial MethodsSM Pro gram. AOAC IN TER NA TIONAL also

awards an an nual schol ar ship to en cour age study in fields that

sup port the mis sion of the As so ci a tion.

MEM BER SHIP AND GOV ER NANCE

AOAC IN TER NA TIONAL is an as so ci a tion com prised of nearly

4000 in di vid ual and 300 or ga ni za tional mem bers from more than 90

coun tries. In di vid ual mem bers are lab o ra tory man ag ers, an a lyt i cal

chem ists, mi cro bi ol o gists, tox i col o gists, fo ren sic sci en tists, and

man age ment ex ec u tives work ing in in dus try, gov ern ment, and

ac a de mia. Or ga ni za tional mem bers are cor po ra tions, com mer cial

lab o ra to ries, gov ern ment agen cies, and uni ver si ties.

An elected Board of Di rec tors gov erns the As so ci a tion. The

Of fi cial Methods Board, the Ed i to rial Board, spe cial and stand ing

com mit tees, Ref eree po si tions con cerned with the val i da tion of

meth ods, li ai son po si tions with other or ga ni za tions, and a

head quar ters staff ad vance and sup port the mis sion of the

As so ci a tion.

For fur ther in for ma tion about AOAC IN TER NA TIONAL and its

pro grams and ac tiv i ties, con tact the As so ci a tion at:

AOAC IN TER NA TIONAL

481 N. Fred er ick Av e , Suite 500

Gaithersburg, MD 20877-2417, USA

Tel: +1-800-379-2622 (Toll free from North Amer ica)

+1-301-924-7077 (World wide)

Fax: +1-301-924-7089

E-mail: aoac@aoac.org

Web site: http://www.aoac.org

Guide to Method For mat

(Method shown is in com plete to al low space for de scrip tion.)

4.10.03

AOAC Of fi cial Method 996.13

Ethoxyquin in Feeds

Liq uid Chro mato graphic Method

First Ac tion 1996

Fi nal Ac tion 1997

(Ap pli ca ble for de ter mi na tion of 0.5–300 m g/g ethoxyquin in dry

ex truded pet food or meat meal.)

See Ta ble 996.13 for the re sults of the interlaboratory study sup port ing

ac cep tance of the method.

A. Prin ci ple

Ethoxyquin is ex tracted with acetonitrile. Ex tract is an a lyzed by

isocratic liq uid chro ma tog ra phy with flu o res cence de tec tion.

B. Ap pa ra tus

(a) Liq uid chromatograph (LC).—Gen er ating 1500 ± 200 psi; with

peak area in te gra tor (man ual or com puter), isocratic LC pump, and col umn

heater. Op er ating con di tions: in jec tion vol ume, 20 m L; flow rate,

1.3 mL/min; tem per a ture, 35°C; flu o res cence de tec tor out put, an a log to

dig i tal con ver sion; de tec tor set tings: ex ci ta tion, 360 nm; emis sion, 432 nm.

(b) LC col umn.—250 ´ 4.6 mm id, C18 octadecylsilane, 5 mm

spher i cal, 100 Å pore size.

C. Re agents

(a) Wa te r. —LC grade.

(b) Acetonitrile. —LC grade.

D. Prep a ra tion of Stan dard So lu tions

(a) Ethoxyquin stan dard stock so lu tion.—400 m g/mL. Weigh the

equiv a lent of 0.1000 g liq uid ethoxyquin into 250 mL am ber vol u met ric

flask and di lute to vol ume with acetonitrile. (Note: Amount of ethoxyquin

needed for prep a ra tion of stock so lu tion is based on pu rity of liq uid, e.g.,

for pu rity of 93.5%, amount of liq uid ethoxyquin = 0.100/0.935 =

0.1070 g.)

H. Cal cu la tions

Cal cu late con cen tra tion of ethoxyquin, m g/g or ppm, in test sam ple

from cal i bra tion curve (us ing lin ear re gres sion with line forced through

zero in ter cept) as fol lows:

Ethoxyquin, m g/g or ppm = C F

´ ´ 15.

where C = ethoxyquin con cen tra tion from LC cal i bra tion curve, m g/mL;

1.5 = vol ume of acetonitrile added to test so lu tion, mL; F = di lu tion fac tor;

W = weight of test por tion, g.

Ref er ence: J. AOAC Int. 80, 725(1997).

CAS-91-53-2 (ethoxyquin) 6-ethoxy-1,2-dihydro-2,2,4-trimethylquinoline

Re vised: March 1998

Chem i cal Ab stracts

Ser vice Reg is try Num ber.

A unique iden ti fier that may

be used to search a num ber

of data-retrieval sys tems.

Method may be di vided into

sev eral de scrip tive sec tions.

Chem i cal names

of pes ti cides and drugs are

given at end of per ti nent

chap ter.

Cal cu la tion symbols

are iden ti fied and show

cor rect units.

Lo ca tor num ber

iden ti fies method by

chap ter, subchapter, and

se quence within the

subchapter for easy cross

ref er enc ing and access.

4 = chap ter 4;

.10 = subchapter 10;

.03 = the third method

found in Chap ter 4,

subchapter 10. The lo ca tor

num ber is not the

per ma nent num ber and is

in cluded only for convenient

accessibility.

Per ma nent num ber

iden ti fies method by

year of adop tion or first

ap pear ance in Of fi cial

Methods of Anal y sis of AOAC

IN TER NA TIONAL.

996 = First Ac tion 1996;

.13 = se quence of adop tion

in 1996.

Ti tle may in clude analyte

and ma trix, type of method,

and of fi cial sta tus.

Ap pli ca bil ity state ment

ad dresses utility and

lim i ta tions on use of method

or other in for ma tion.

Ref er ences di rect

the user to the pub lished

col lab o ra tive study and any

sub se quent re vi sions in the

method. Other in for ma tive

ref er ences may be in cluded.

Spec i fi ca tions

for nec es sary lab o ra tory

ap pa ra tus and re agent

prep a ra tions. See also

Def i ni tion of Terms and

Ex plan a tory Notes.

Def i ni tion of Terms

and Ex plan a tory Notes

Of fi cial Methods

(1 ) Of fi cial Methods are des ig nated First Ac tion or Fi nal

Ac tion, and, in a few cases, Pro ce dures. A First Ac tion method has

un der gone col lab o ra tive study, has been rec om mended by the

ap pro pri ate Gen eral Ref eree and has been adopted Of fi cial First

Ac tion by the Methods Committee. A method may be adopted

Fi nal Ac tion a min i mum of 2 years af ter it has been adopted First

Ac tion, and af ter it has been rec om mended by the ap pro pri ate

Gen eral Ref eree and Methods Com mit tee, and voted on by the

Official Methods Board.

Sampling, test sam ple prep a ra tion pro to col, or other type of

in struc tions for which an interlaboratory col lab o ra tive study is

im prac ti cal may be adopted, as above, as a Pro ce dure.

All meth ods in this book—First Ac tion, Fi nal Ac tion, or

Pro ce dure—are Of fi cial Methods SM of AOAC

IN TER NA TIONAL.

Re agents

(2 ) Term "H2 O" means dis tilled or deionized wa ter, ex cept

where oth er wise spec i fied, and ex cept where the wa ter does not mix

with the de ter mi na tion, as in "H2 O bath."

(3 ) Term "al co hol" means 95% eth a nol by vol ume. Al co hol of

strength x% may be pre pared by di lut ing x mL 95% al co hol to 95 mL

with H2 O. Ab so lute al co hol is 99.5% by vol ume. For mulas of

spe cially de na tured al co hols (SDA) used as re agents in the United

States un der 27CFR21 are as fol lows:

SDA No. 100 Parts al co hol plus

3-A 5 Parts meth a nol

3-C 5 Isopropyl al co hol

30 10 Parts methanol

"Re agent" al co hol is 95 parts SDA 3-A plus 5 parts isopropanol.

(4 ) Term "ether" means ethyl ether, per ox ide free by the

fol low ing test: To 420 mL ether in sep a ra tor, add 9.0 mL 1%

NH4VO3 in H2 SO4 (1 + 16). Shake 3 min and let sep a rate. Drain

lower layer into 25 mL glass-stoppered grad u ate, di lute to 10 mL

with H2 SO4 (1 + 16), and mix. Any or ange color should not ex ceed

that pro duced by 0.30 mg H2 O2 (1 mL of so lu tion pre pared by

di lut ing 1 mL 30% H2 O2 to 100 mL with H2O) and 9.0 mL 1%

NH4VO3 in H2 SO4 (1 + 16). Per ox ides may be elim i nated by pass ing

£700 mL ether through 10 cm col umn of Woelm ba sic alu mina in

22 mm id tube.

(5 ) The fol low ing listed re agents, un less oth er wise spec i fied,

have ap prox i mate strength stated and con form in pu rity with

Rec om mended Spec i fi ca tions for An a lyt i cal Re agent Chem i cals of

the Amer i can Chem i cal So ci ety:

As say

Sul fu ric acid 95.0–98.0% H2 SO4

Hy dro chlo ric acid 36.5–38.0% HCl

Ni tric acid 68.0–70.0% HNO3

Fuming ni tric acid ³90% HNO3

Ace tic acid ³ 99.7% CH3 COOH

Hydrobromic acid 47.0–49.0% HBr

Am mo nium hy drox ide 28–30% NH3

Phos pho ric acid ³ 85% H3 PO4

Where no in di ca tion of di lu tion is given, re agent con cen tra tion is

the con cen tra tion given above.

(6 ) All other re agents and test so lu tions, un less oth er wise

de scribed in the text, are au to mat i cally re agent grade and con form to

re quire ments of the Amer i can Chem i cal So ci ety. Where such

spec i fi ca tions have not been pre pared, use high est grade re agent.

When an hy drous salt is in tended, it is so stated; oth er wise the

hy drated prod uct is meant.

(7 ) Un less oth er wise spec i fied, phenolphthalein used as

in di ca tor is 1% al co hol so lu tion; methyl or ange is 0.1% aque ous

so lu tion; methyl red is 0.1% al co hol so lu tion.

(8) Di rec tions for stan dard iz ing re agents are given in

Ap pen dix A, Stan dard So lu tions and Cer tified Ref er ence Ma te rials.

(9 ) Un usual re agents not men tioned in re agent sec tions or cross

ref er enced, other than com mon re agents nor mally found in

laboratories, are ital i cized the first time they oc cur in a method.

(10 ) Com mer cially pre pared re agent so lu tions must be checked

for ap pli ca bil ity to a spe cific method. They may con tain un de clared

buff ers, pre ser va tives, che lat ing agents, etc.

(11 ) In ex pres sions (1 + 2), (5 + 4), etc., used in con nec tion

with name of re agent, the first nu meral in di cates the vol ume of

re agent used and the sec ond nu meral in di cates vol ume of H2 O.

For ex am ple, HCl (1 + 2) means re agent pre pared by mix ing

1 vol ume HCl with 2 vol umes H2O. When one of the re agents is a

solid, ex pres sion means part by weight. The first nu meral

rep re sents the solid re agent; the sec ond nu meral H2 O. So lu tions

for which the sol vent is not spec i fied are aque ous so lu tions.

(12) In mak ing up so lu tions of def i nite per cent age, it is

un der stood that x g sub stance is dis solved in H2O and di luted to

100 mL. Al though not the o ret i cally cor rect, this con ven tion

will not re sult in any ap pre cia ble er ror in any meth ods given in

this book.

(13 ) Chro mic acid clean ing so lu tion is pre pared by (1) add ing 1 L

H2 SO4 to ap prox i mately 35 mL sat u rated aque ous Na2 Cr2 O 7

so lu tion; or (2 ) add ing 2220 mL H2 SO4 to ap prox i mately 25 mL

sat u rated aque ous CrO3 so lu tion (170 g/100 mL). Re agents may be

tech ni cal high grade. Use only af ter first clean ing by other means

(e.g., de ter gent) and drain ing. Mix ture is ex pen sive and haz ard ous.

Use re peat edly un til it is di luted or has a green ish tinge. Dis card

care fully with co pi ous amounts of H2 O. Re fer to Ap pen dix B,

Lab o ra tory Safety chap ter.

(14 ) All cal cu la tions are based on in ter na tional atomic weights.

Ap pa ra tus

(15 ) Burets, vol u met ric flasks, and pipets con form to the

fol low ing U.S. Fed eral spec i fi ca tions (avail able from Gen eral

Ser vices Ad min is tra tion, Spec i fi ca tion Sec tion, L'Enfant Plaza, Ste

8100, Wash ing ton Navy Yard, Bldg 197, Wash ing ton, DC 20407,

USA):

Buret A-A-51248 May 19, 1965

Flask, vol u met ric A-A-51360 Feb ru ary 7, 1977

Pipet, vol u met ric A-A-53890 Feb ru ary 24, 1978

See also Ap pen dix V, "Testing of Glass Vol u met ric Ap pa ra tus," in

the Na tional In sti tute of Stan dards and Tech nol ogy (NIST)

Spec i fi ca tion Pub li ca tion 260–54, "Cer tif i ca tion and Use of

Acidic Po tas sium Dichromate So lu tions as an Ul tra vi o let

Absorbance Stan dard SRM935" (avail able from NIST, Of fice of

Stan dard Ref er ence Ma te rials, B316 Chem i cals, Gaithersburg,

MD 20899, USA).

(16 ) Stan dard taper glass joints may be used in stead of stop pers

where the lat ter are spec i fied or im plied for con nect ing glass ap pa ra tus.

(17 ) Sieve des ig na tions, un less oth er wise spec i fied, are those

de scribed in U.S. Fed eral Spec i fi ca tion RR-S-366e, No vem ber 9,

1973 (avail able from Gen eral Ser vices Ad min is tra tion).

Des ig na tion "100 mesh" (or other num ber) pow der (ma te rial, etc.)

means ma te rial ground to pass through stan dard sieve No. 100 (or

other num ber). Cor re sponding in ter na tional stan dard and U.S.

stan dard sieves are given in Ta ble 1.

(18 ) Term "pa per" means fil ter pa per, un less oth er wise spec i fied.

(19) Term "high-speed blender" des ig nates mixer with

4 canted, sharp-edge, stain less steel blades ro tat ing at the bot tom

of 4-lobe jar at 10 000–12 000 rpm, or with equiv a lent shear ing

ac tion. Sus pended sol ids are re duced to fine pulp by ac tion of

blades and by lob u lar con tainer, which swirls sus pended sol ids into

blades. War ing Blender, or equiv a lent, meets these re quire ments.

(20 ) "Flat-end rod" is glass rod with one end flat tened by heat ing

to soft en ing in flame and press ing ver ti cally on flat sur face to form

cir cu lar disk with flat bot tom at end.

(21 ) Des ig na tion and pore di am e ter range of fritted glass ware

are: ex tra coarse, 170–220 mm; coarse, 40–60; me dium, 10–15; fine,

4–5.5; Jena des ig na tions and pore di am e ter are: (1) 110 m m; (2 ) 45;

(3) 25; (4) 8.

(22 ) Un less oth er wise in di cated, tem per a tures are ex pressed in

de grees Cel sius (Cen ti grade).

Sam ple

(23) Ter mi nol ogy and us age for items and op er a tions

col lo qui ally des ig nated with the term "sam ple": Newly adopted

meth ods will avoid the con fus ing us age of the term "sam ple" for

any thing the an a lyst is work ing with. The no men cla ture

rec om mended by the In ter na tional Un ion of Pure and Ap plied

Chem is try (IUPAC), Pure & Appl. Chem . 62 , 1193(1990), for

an a lyt i cal chem is try, based upon the In ter na tional Or ga ni za tion for

Stan dard iza tion (ISO) rec om men da tions, will be uti lized. The

crit i cal def i ni tions are:

A lab o ra tory sam ple is the ma te rial sent to or re ceived by the

lab o ra tory. The lab o ra tory re duces the lab o ra tory sam ple in size and

fine ness to a test sam ple (or an a lyt i cal sam ple if only chem i cal or

mi cro bi o log i cal anal y sis is in volved). A test (or an a lyt i cal ) por tion

Table 1. Nom i nal di men sions of stan dard test sieves

(USA stan dard se ries)

Sieve designation

Nom i nal sieve

opening, in.

Nom i nal wire

di am e ter, mm

In ter na tional

standarda (ISO)

USA

stan dard

12.5 mmb 12 in.b 0.500 2.80

11.2 mm 716 in. 0.438 2.50

9.5 mm 3 8 in. 0.375 2.24

8.0 mm 516 in. 0.312 2.00

6.7 mm 0.265 in. 0.265 1.80

6.3 mm 14 in.b 0.250 1.80

5.6 mm No. 3 0.223 1.60

4.75 mm No. 4 0.187 1.60

4.00 mm No. 5 0.157 1.25

3.35 mm No. 6 0.132 1.00

2.80 mm No. 7 0.111 0.90

2.36 mm No. 8 0.0937 0.80

2.00 mm No. 10 0.0787 0.71

1.70 mm No. 12 0.0661 0.63

1.40 mm No. 14 0.0555 0.56

1.18 mm No. 16 0.0469 0.45

1.00 mm No. 18 0.0394 0.40

850 m mc No. 20 0.0331 0.355

710 m m No. 25 0.0278 0.315

600 m m No. 30 0.0234 0.280

500 m m No. 35 0.0197 0.224

425 m m No. 40 0.0165 0.200

355 m m No. 45 0.0139 0.180

300 m m No. 50 0.0117 0.160

250 m m No. 60 0.0098 0.125

212 m m No. 70 0.0083 0.100

180 m m No. 80 0.0070 0.090

150 m m No. 100 0.0059 0.080

125 m m No. 120 0.0049 0.063

106 m m No. 140 0.0041 0.056

90 mmNo. 170 0.0035 0.045

75 m m No. 200 0.0029 0.040

63 m m No. 230 0.0025

53 m m No. 270 0.0021

aThese stan dard des ig na tions cor re spond to the val ues for test sieve

ap er tures rec om mended by the In ter na tional Or ga ni za tion for

Stan dard iza tion, Geneva, Swit zer land.

bThese sieves are not in the stan dard se ries but they have been in cluded

be cause they are in com mon us age.

c1000 mm = 1 mm.

is re moved from the test sam ple for anal y sis. Once a test por tion is

mea sured, by mass or vol ume, the term "sam ple" is no lon ger

ap pro pri ate. Use "test" or "un known" as the mod i fier, e.g., "test

so lu tion," not "sam ple so lu tion."

The op er a tion of ten called "prep a ra tion of sam ple" ap plies to the

re duc tion of the lab o ra tory sam ple to the test sam ple, and not to the

usual an a lyt i cal steps of so lu tion, sep a ra tion, pu ri fi ca tion, or

iso la tion of the analyte.

The term "sam ple" will be used solely in the sta tis ti cal sense as a

small por tion rep re sent ing a larger quan tity, such as a lot or a batch,

where the po ten tial ex ists for a "sam pling er ror" due to the

het er o ge ne ity of the par ent pop u la tion. Most sam ples are re moved

from a static pop u la tion, such as a pile of fer til izer, a stack of cases,

or a group of con tain ers. In a dy namic sit u a tion, how ever, where the

pop u la tion changes with time as a flow ing river, cir cu lat ing blood,

or a mov ing con veyor belt, the small por tion re moved should be

called a "spec i men ." In these cases, the phe nom e non un der study

and the sam pling er ror are con founded in such a way that they

can not be sep a rated.

See Fig ure 1 [In ter na tional Un ion of Pure and Ap plied Chem is try,

"No men cla ture for Sam pling in An a lyt i cal Chem is try," Pure &

Appl. Chem. 62 , 1193(1990)].

Stan dard Op er a tions

(24 ) Op er a tions spec i fied as "wash (rinse, ex tract, etc.) with two

(three, four, etc.) 10 mL (or other vol umes) por tions H2O (or other

sol vent)" mean that the op er a tion is to be per formed with in di cated

vol ume of sol vent and re peated with same vol ume of sol vent un til

num ber of por tions re quired have been used.

(25) Def i ni tions of terms used in meth ods in volv ing

spectropho tom e try are those given in JAOAC 37, 54(1954). Most

im por tant prin ci ples and def i ni tions are: (a ) More ac cu rate

in stru ment may be sub sti tuted for less ac cu rate in stru ment (e.g.,

spectrophotometer may re place colorimeter) where lat ter is

spec i fied in method. Wave length spec i fied in method is un der stood

to be that of max i mum absorbance (A), un less no peak is pres ent.

(b ) Absorbance (s ) (A ): Neg a tive log a rithm to base 10 of the ra tio of

trans mit tance (T ) of test so lu tion to that of ref er ence or stan dard

ma te rial. Other names that have been used for quan tity rep re sented

by this term are op ti cal den sity, ex tinc tion, and ab sor bency.

(c ) Ab sorp tivi ty(ies ) (a ): Absorbance per unit con cen tra tion and

cell length.

a = A/ bc

where b is in cm and c = g/L, or a = (A/ bc ) ´ 1000, if c is mg/L. Other

names that have been used for this or re lated quan ti ties are

ex tinc tion co ef fi cient, spe cific ab sorp tion, absorbance in dex, and

E1cm

1% . (d) Trans mit tance ( s ) (T ): Ra tio of ra di ant power trans mit ted

by the test so lu tion to ra di ant power in ci dent on so lu tion, when both

are mea sured at same spec tral po si tion and with same slit width.

Beam is un der stood to be par al lel ra di a tion and in ci dent at right

an gles to plane par al lel sur face of test ma te rial. If test ma te rial is

so lu tion, sol ute trans mit tance is quan tity usu ally de sired and is

cal cu lated di rectly as ra tio of trans mit tance of so lu tion in cell to

trans mit tance of sol vent in an equal cell. Other names that have been

used for this quan tity are transmittancy and trans mis sion.

(e ) Stan dard iza tion : Spectrophotometer may be checked for

ac cu racy of wave length scale by re fer ring to Hg lines: 239.94, 248,

253.65, 265.3, 280.4, 302.25, 313.16, 334.15, 365.43, 404.66,

435.83, 546.07, 578.0, and 1014.0 nm. To check con sis tency of

absorbance scale, pre pare so lu tion of 0.0400 g K2 CrO4 /L 0.05M

KOH and de ter mine absorbance at fol low ing wave lengths in 1 cm

cell: 230 nm, 0.171; 275 nm, 0.757; 313.2 nm, 0.043; 375 nm, 0.991;

400 nm, 0.396. See NIST Spec. Pub. 378 , "Ac cu racy in

Spectrophotometry and Lu mi nes cence Mea sure ments," 1973

(avail able from NIST, Of fice of Stan dard Ref er ence Ma te rials,

B316, Chem is try, Gaithersburg, MD 20899, USA).

(26 ) Least square treat ment of data and cal cu la tion of re gres sion

lines. This tech nique finds the best fit ting straight line for set of data

such as stan dard curve. It cal cu lates that straight line for which the

sum of squares of ver ti cal de vi a tions (usu ally A ) of ob ser va tions

from the line is smaller than cor re spond ing sum of squares of

de vi a tion from any other line. Equa tion of straight line is:

Y = a + bX

where a is in ter cept at Y axis (X = 0), and b is slope of line.

Least square es ti mates of con stants are:

bXYXYn

XXn

iiii

SSS

()[()]

[()]

a = Y – bX

where S = "sum of" the n in di vid ual val ues of in di cated op er a tion,

and X and Y are the av er ages of the X and Y points.

Ex am ple: To find "best" straight line re lat ing A (Y ) to

con cen tra tion (X):

Ob ser va tion

No. (i)

Con cen tra tion

Absorbance

Yi X i

2XiYi

1 80 1.270 6400 101.6

2 60 1.000 3600 60.0

3 40 0.700 1600 28.0

4 30 0.550 900 16.5

5 20 0.250 400 5.0

6 10 0.100 100 1.0

7 0 0.050 0 0.0

To tals:

n = 7 S Xi = 240 S Yi = 3.92 S

2= 1300 S (Xi Yi ) =

212.1

X = SXi / n = 240/7 = 34.29

Y = SYi / n = 3.92/7 = 0.56

b = 212 1 240 3 92 7

13000 240 7

77 7

4771 0 016

. [( )( . )]

[( ) ]

-= = 3

a = 0.56 – 0.0163(34.29) = 0.001 @ 0

Best equa tion is then:

Y = 0.00 + 0.0163X

If for test sam ple, A = 0.82, cor re spond ing con cen tra tion (X ) would

be:

X = ( Y – 0.00)/0.0163 = 0.82/0.0163 = 50.3

Many sci en tific and sta tis ti cal cal cu la tors are pro grammed to

per form this cal cu la tion. It should be noted that the least square fit of

a data set should not be the only cri te rion used in eval u at ing the

va lid ity of a given data set.

High cor re la tion co ef fi cients (e.g., >0.99) do not nec es sar ily

in di cate lin ear ity. This mis in for ma tion has been the sub ject of

sev eral re ports from the An a lyt i cal Methods Com mit tee of the

Royal So ci ety of Chem is try [An a lyst 113 , 1469–1471 (1988); 11 4 ,

753(1989); 119, 2363–2366(1994)]. Sta tis tically, such a cor re la tion

co ef fi cient ap plies only when both x and y are vari ables; a stan dard

curve re quires that one pa ram e ter (con cen tra tion) be fixed (known).

When a high correlation is desired between the signal and

concentration, use the symbol "r2 " for the relationship as calculation

by computer spreadsheet programs.

(27 ) Re cov ery (R) of analyte from for ti fied test ma te rial by a

method of anal y sis. Frac tion of an analyte added to a test sam ple

(for ti fied test sam ple) prior to anal y sis, which is mea sured

(re cov ered) by the method. When the same an a lyt i cal method is

used to an a lyze both the un for ti fied and for ti fied test sam ples,

cal cu late per cent R as fol lows:

% Rec = CC

-´100

where C F = con cen tra tion of analyte mea sured in for ti fied test

sam ple; C U = con cen tra tion of analyte mea sured in un for ti fied test

sam ple; C A = con cen tra tion of analyte added to for ti fied test sam ple.

(Note : C A is a cal cu lated value, not a value mea sured by the method

be ing used.)

Con cen tra tion of added analyte should be no less than

con cen tra tion of analyte in un for ti fied test sam ple. Sum of

con cen tra tion of added analyte plus analyte pres ent be fore

for ti fi ca tion should be in the same range as analyte con cen tra tion

sought in ac tual test sam ples. Ad di tion of analyte must not cause

mea sur ing in stru ment to ex ceed lin ear dy namic range of stan dard

curve. Both for ti fied and un for ti fied test sam ples must be treated

iden ti cally dur ing anal y sis to min i mize ex per i men tal bias.

(28 ) Com mon safety pre cau tions are given in Ap pen dix B,

Lab o ra tory Safety.

Re sults of Interlaboratory Study

(29 ) Users of methods should con sult the re port of the

col lab o ra tive study (ref er ence given with the method) for de tails as

to re sults of the interlaboratory study.

Ed i to rial Con ven tions

(30 ) For sim plic ity, the ab bre vi a tions Cl, H, I, N, and O are used

rather than their di atomic forms. The charge may not be in di cated

with the cor re spond ing ion where no am bi gu ity will re sult.

(31 ) Re agents and ap pa ra tus ref er enced with only a let ter, e.g.,

(c ), will be found in the Re agent or Ap pa ra tus sec tion of the method.

(32 ) To con serve space, many ar ti cles and prep o si tions have

been elim i nated.

Man u fac turers and Sup pliers

Many manufacturers and suppliers may be found by a search of

the Internet. The same or equiv a lent prod ucts, in stru ments,

sup plies, ap pa ra tus, or re agents avail able from man u fac tur ers

and sup pli ers other than those named, or other brands from other

sources, may serve equally well if proper val i da tion in di cates

their use is sat is fac tory.

Ab bre vi a tions

(33 ) The fol low ing ab bre vi a tions, many of which con form with

those of Chem i cal Ab stracts, are used. In gen eral, prin ci ple

gov ern ing use of pe ri ods af ter ab bre vi a tions is that pe riod is used

where fi nal let ter of ab bre vi a tion is not the same as fi nal let ter of

word it rep re sents.

Ab bre vi a tion Word

aAb sorp tivi ty(ies)

AAbsorbance(s) through out (not re stricted to

for mu las; not ab sorp tion). A¢ is used for

stan dard; A0 is used for blank; 3 digit sub script

nu mer als usu ally de note wave length in nm

A Am pere

Å Ang strom

AA Atomic ab sorp tion

AACC Amer i can As so ci a tion of Ce real Chemists

ACS Amer i can Chem i cal So ci ety

amu Atomic mass unit

AOCS Amer i can Oil Chem ists' So ci ety

APHA Amer i can Pub lic Health As so ci a tion

ASBC Amer i can So ci ety of Brewing Chemists

ASTM Amer i can So ci ety of Testing and Ma te rials

atm. At mo sphere

AU Absorbance units

AUFS Absorbance units full scale

BAM Bac te ri o log i cal An a lyt i cal Man ual

Bé De gree Baumé

bp Boil ing point

Bq Becquerel

CDe gree Celsius (Centigrade)

ca About, ap prox i mately

Cat. No. Cat a log num ber

CDC Cen ters for Dis ease Con trol and Prevention

cfu Col ony form ing unit(s)

Ch Chap ter

Ci Cu rie(s) (= 3.7 ´ 1010 Bq)

CI Color index

CIPAC Col lab o ra tive In ter na tional Pes ti cide An a lyt i cal

Coun cil

cm Cen ti me ter(s)

concn Concentration

cP Centipoise

cpm Counts per min ute

CRM Cer tified ref er ence material

*cu in. Cu bic inch(es)

dc Di rect cur rent

DMF N , N-dimethylformamide

DMSO Dimethyl sulfoxide

EDTA Ethylenedinitrilotetraacetic acid (or -tetraacetate)

EIA Enzyme immunoassay

ELISA En zyme linked immunosorbent assay

EPA U.S. En vi ron men tal Pro tec tion Agency

Exp Ex po nen tial

F De grees Fahr en heit [° C = (5/9) ´ (°F – 32)]

FAO Food and Ag ri cul ture Or ga ni za tion

FDA U.S. Food and Drug Ad min is tra tion

FEP Fluorinated ethylene propylene

*fl oz Fluid ounce (29.54 mL)

Ab bre vi a tion Word

fp Freez ing point

FSD Full scale deflection

*ft Foot (30.48 cm)

gGram(s)

gGrav ity (in cen tri fug ing)

*gal. Gal lon(s) (3.785 L)

gr. Grain(s) (1 grain = 64.8 mg)

GC Gas chro ma tog ra phy

h Hour(s)

HorRat Horwitz ratio

HPLC High per for mance liq uid chromatography

ICC In ter na tional As so ci a tion for Ce real Sci ence and

Technology

id In ner di am e ter

IgG Im mu no glob u lin G

*in. Inch(es) (2.54 cm)

IR In fra red

ISO In ter na tional Or ga ni za tion for Stan dard iza tion

kg Ki lo gram(s)

kPa Kilo pas cal

LLi ter(s)

LC Liq uid chro ma tog ra phy

*lb Pound(s) (453.6 g)

m Me ter(s); milli—as pre fix

mMolal

M Mo lar (as ap plied to con cen tra tion), not molal

mA Mil li am pere(s)

mW Megaohm

min Min utes

min. Minimum

mg Mil li gram(s)

mL Mil li li ter(s)

mm Mil li me ter(s)

mp Melt ing point

MS Mass spec trom e ter (spec trom e try)

MSDS Material Safety Data Sheet

(www.cdc.gov/niosh/ipcs/nicstart.html)

mm Mil li mi cron (10 –6 mm); use nanometer (nm)

(10–9 m)

mV Mil li volt

MW Mo lec u lar weight (mo lar mass)

*N Nor mal (as ap plied to con cen tra tion; in equa tions,

nor mal ity of ti trat ing re agent)

N New ton (105 dynes)

nRe frac tive in dex

NF Na tional For mu lary

NFPA Na tional Food Pro ces sors As so ci a tion

NIST Na tional In sti tute of Stan dards and Tech nol ogy

ng Nanogram (10–9 g)

nm Nanometer (10–9 m); formerly mm

No. Num ber

Ab bre vi a tion Word

od Outer di am e ter

ODS Octadecylsilane

WOhm

*oz Ounce(s) (28.35 g)

pPico (10 –12 ) as pre fix

Pa Pascal [1 New ton/m2; 9.87 ´ 10–6 atm; 7.5 ´

10–3 mm Hg (torr); 1.45 ´ 10–4 psi]

pCi Pico Cu rie(s) = 27.027 Bq

*ppb Parts per bil lion (10–9 )

*ppm Parts per mil lion (10–6 )

ppt Parts per tril lion (10–12 )

*psi Pounds per square inch (ab so lute)

*Psig Pounds per square inch gauge (at mo spheric

pres sure = 0)

*pt Pint(s) (473 mL)

QAC Qua ter nary am mo nium com pound

*qt Quart(s) 946 mL

R Reproducibility value (= 2.8 ´ sR)

rRe peat abil ity value (= 2.8 ´ sr)

®Trade mark name (registered)

Rf Dis tance spot moved/dis tance sol vent moved,

TLC

rpm Rev o lu tions per min ute

SDF Spe cial de na tured for mula (ap plied to al co hol)

SSum

sSec ond(s)

sq Square

SRM Stan dard Ref er ence Ma te rial (CRM of Na tional

In sti tute of Stan dards and Tech nol ogy)

TTrans mit tance

TLC Thin-layer chro ma tog ra phy

äTrade mark

ton = 907 kg

U Unit

USDA United States De part ment of Ag ri cul ture

USP United States Phar ma co peia

UV Ul tra vi o let

VVolt(s)

Ab bre vi a tion Word

v/v Vol ume per volume

WHO World Health Or ga ni za tion

w/v Weight per volume

x Mean

c2 Chi square

bBeta

lLambda

gGamma

mMi cro

mcMi cro cou lomb

mmMi cron (0.001 mm); use mi crom e ter (10–6 m)

mgMi cro gram(s) (10–6 g)

mLMicroliter(s) (10–6 L)

DDif fer ence [e.g., DA = (A – A ¢)]

*¢ Foot (feet) (1¢ = 30.48 cm)

*² Inch(es) (1² = 2.54 cm)

/Per

%Per cent (parts per hun dred); per cent age

% Rec Per cent re cov ery

‰Parts per thousand

> More than; greater than; above; ex ceeds

(use with num bers only)

< Less than; un der; be low (use with num bers only)

£Equal to or less than

³Equal to or greater than

* = Not of fi cial SI units; no lon ger rec om mended for use in AOAC

INTERNATIONAL.

Con ver sion ta ble for con cen tra tion units

Parts/thou sand Parts/mil lion Parts/bil lion Parts/tril lion

%10 10000 10000000 10000000000

Parts per thou sand 1 1000 1000000 1000000000

Parts per mil lion 0.001 1 1000 1000000

Parts per bil lion 0.000001 0.001 1 1000

Parts per tril lion 0.000000001 0.000001 0.001 1

Use: One unit in left col umn equals the num ber of units in col umns 2–5. Ex am ple: 5% = 50 000 parts per mil lion; 2 ppm = 2000 ppb; 5 ppb = 0.005 ppm.

Note: These units are no lon ger rec om mended be cause United States and in ter na tional us age dif fer. Use sci en tific no men cla ture 10 000 = E + 4; 0.000 1 = E – 4.

AOAC® Of fi cial Methods SM Val i da tion Pro gram

AOAC IN TER NA TIONAL is a unique, non profit sci en tific

or ga ni za tion whose pri mary pur pose is to serve the needs of

gov ern ment, in dus try, and ac a demic lab o ra to ries for an a lyt i cal

meth ods and qual ity mea sure ment sys tems. The AOAC® Of fi cial

MethodsSM Pro gram is de signed to pro vide meth ods of anal y sis with

known per for mance char ac ter is tics, such as ac cu racy, pre ci sion,

sen si tiv ity, range, spec i fic ity, limit of mea sure ment, and sim i lar

at trib utes. A pre req ui site of AOAC adop tion is val i da tion through

interlaboratory col lab o ra tive study in in de pend ent lab o ra to ries

un der iden ti cal con di tions. Such val i dated meth ods can then be used

with con fi dence by reg u la tory agen cies, reg u lated in dus try, prod uct

test ing lab o ra to ries, and ac a demic in sti tu tions. The meth ods are

used to de ter mine com pli ance with gov ern ment reg u la tions, to

main tain qual ity con trol and pro cess re quire ments, to set and

eval u ate com pli ance with terms of pro cure ment con tracts, to

con duct na tional and in ter na tional trade, and to sup port re search.

The ac tual work is done world wide by ap pointed vol un teers in

their pro fes sional ca pac i ties as sci en tists of fed eral, state,

pro vin cial, and mu nic i pal lab o ra to ries; ac a demic and ex per i ment

sta tion lab o ra to ries; and com mer cial lab o ra to ries. These vol un teers

con trib ute time, ex per tise, and lab o ra tory ca pa bil ity to par tic i pate as

re search ers, meth ods col lab o ra tors, com mit tee mem bers, and

ad vi sors.

AOAC IN TER NA TIONAL has over a cen tury of ex pe ri ence in

us ing the interlaboratory col lab o ra tive study as a means of

de ter min ing the per for mance char ac ter is tics of a method for both

gen eral and reg u la tory use. AOAC's ma jor con tri bu tion to

an a lyt i cal sci ence has been to bring the interlaboratory col lab o ra tive

study tech nique to a high de gree of per fec tion, and to en cour age

other meth ods or ga ni za tions to har mo nize their pro grams with the

AOAC pro ce dure. As stated in the U.S. Code of Fed eral Reg u la tions

(Ti tle 21), it is the pol icy of the U.S. Food and Drug Ad min is tra tion

in its en force ment pro grams to use the meth ods of anal y sis of AOAC

IN TER NA TIONAL as pub lished in the lat est edi tion (18th Ed.,

2005) of their pub li ca tion Of fi cial Methods of Anal y sis of AOAC

IN TER NA TIONAL. In ad di tion, in the U.S. Code of Fed eral

Reg u la tions (Ti tle 9), An i mal and An i mal Prod ucts, Of fi cial

Methods of Anal y sis of AOAC IN TER NA TIONAL (15th Ed., 1990),

is in cor po rated by ref er ence with the ap proval of the Di rec tor of the

Fed eral Reg is ter in ac cor dance with 5 U.S.C. 552(a) and 1 CFR

Part 51.

METHOD SUBMISSION

Several mechanisms exist for submitting methods to AOAC: (1 ) a

government agency or an organization may enter into a contract

with AOAC for the validation of specific methodology or provide

continuous infrastructure support for the review and approval of

methods in a particular area of interest; (2 ) a community may be

formed comprised of stakeholders from government, industry,

and/or academia in a particular area of interest who need validated

methods and submit best and most needed methods for AOAC

review and approval; (3) a company or organization that, for

example, has a proprietary product and has an interest in obtaining

an economic advantage through the AOAC approval of their method

may submit its methods for review and approval, together with a

submission fee.

Communities

Methods may be submitted by AOAC analytical communities.

Communities bring together analytical scientists in a specific area

who share a commitment to consolidate efforts to prioritize method

needs, establish performance criteria, gather and evaluate existing

methods, help seek funding, and support validation work for

methods that are fit-for-purpose. Communities may be able to

secure collaborative funding from industry and government in

support of much needed methodology. Examples of AOAC

analytical communities various stages of development include, but

are not limited to, Agricultural Materials, Dietary Supplements,

Food Allergens, Homeland Security, and Marine and Freshwater

Toxins.

For more on AOAC's various communities, visit our Web site at

www.aoac.org and click on "AOAC Analytical Communities."

Contracts and Infrastructure Support

An interested party, usually a government agency, in need of

validated methods may build a contractual relationship with AOAC.

For more information about government and industry

participation, contact Anita Mishra at amishra@aoac.org or Tel:

+1-301-924-7077 ext. 131.

Individual Company or Organization

Methods may be submitted by an individual company or

organization that has, for example, a proprietary product and wants

to have their method(s) approved by AOAC.

METHOD VAL I DA TION PRO CESS

Method De vel op ment and In-House Study

An AOAC-sponsored val i da tion study be gins with the

ap point ment of a Study Director, the in di vid ual sci en tist who is

re spon si ble for or ga niz ing the method study.

He or she se lects, de vel ops, or adopts a method to be stud ied. For a

microbiology method, a precollaborative study is required, to be

conducted according to AOAC guidelines. In the case of a chemistry

method, the Study Director de vel ops the re quired in-house

val i da tion data and col lab o ra tive study pro to col (de sign) in

ac cor dance with AOAC guide lines.

The rec om mended study pro to col and in-house val i da tion data

are re viewed by the Gen eral Ref eree, Com mit tee Sta tis tics and

Safety Ad vi sors, up to 2 Methods Committee members, and the

Methods Com mit tee Chair. Once an agree ment on the study

pro to col is reached, the Study Director can be gin the interlaboratory

col lab o ra tive study.

Val i da tion Through Col lab o ra tive Study

The Study Director re cruits col lab o ra tors in lab o ra to ries with

ex pe ri ence in the type of anal y sis re quired in the pro posed method.

For quan ti ta tive meth ods, AOAC IN TER NA TIONAL re quires

valid data from no fewer than 8 lab o ra to ries, each an a lyz ing a

min i mum of 5 ma te ri als, as blind du pli cates or Youden pairs. For

qual i ta tive meth ods, the min i mum cri te ria are 15 lab o ra to ries

re port ing 2 analyte lev els per ma trix, 5 rep li cates per level, and

5 neg a tive con trols per ma trix.

The Study Director pre pares the test ma te rials and, if re quired,

other ma te ri als to be sup plied to col lab o ra tors, such as ref er ence

ma te ri als, col umn packings, or monoclonal an ti bod ies, and ships

them to the co op er at ing lab o ra to ries along with the method,

in struc tions for con duct ing the study, and re port ing forms.

Col lab o ra tors are ex pected to con duct the test ex actly as

in structed and ac cord ing to the method, with no de vi a tions, and

re turn re sults within the time frame agreed.

Ex pert Re view

The Study Director com piles the data, eval u ates the re sults, and

writes the col lab o ra tive study re port, in ac cor dance with AOAC

guide lines. Sta tis ti cal treat ment of the data is con sid ered es sen tial in

a rig or ous eval u a tion of the method, and AOAC

IN TER NA TIONAL pro vides man u als, sta tis ti cal soft ware, and

ex pert con sul ta tion to aid the Study Director.

The re port is sub mit ted to the Gen eral Ref eree and Sta tis tics

Ad vi sor and then to the Methods Com mit tee and 2 Official Methods

Board members for tech ni cal re view. Methods ac cept able through

these re view lev els are then approved for adop tion as First Ac tion

AOAC® Of fi cial MethodsSM .

Adoption of First Action AOAC® Official MethodsSM

A Methods Committee reviews the submitted collaborative study

reports, comments, and associated documentation to ensure

adherence to the technical review process. Advance notices of the

methods to be considered for First Action are published in the

Referee section of AOAC's magazine, Inside Laboratory

Management, and on the AOAC Web site.

Method actions taken by the Methods Committees are published

in the Referee section of AOAC's magazine, Inside Laboratory

Management. The complete text of newly adopted AOAC® Official

MethodsSM and the reports or summaries of the interlaboratory

collaborative studies are published in the Journal of AOAC

INTERNATIONAL. The adopted methods are added to the

compendium, Official Methods of Analysis of AOAC

INTERNATIONAL.

Adoption of Final Action AOAC® Official MethodsSM

First Action AOAC® Official Methods SM are eligible for Final

Action status after they have been available in the literature for at

least 2 years. If the Association has not received any information as

to significant problems in the performance of the method, the

General Referee recommends adoption of the method as Final

Action, and the method is listed in the Referee section of AOAC's

magazine, Inside Laboratory Management, and on the AOAC Web

site so interested parties may submit comments and data if desired.

A ballot of methods recommended by the General Referees and

Methods Committees for Final Action is submitted to the Official

Methods Board who votes on the acceptance of the methods as Final

Action. Notices of the methods adopted as Final Action AOAC®

Official MethodsSM are published in the Referee section of AOAC's

magazine, Inside Laboratory Management and on the AOAC Web

site.

Actions Affecting AOAC® Official MethodsSM

Methods can be repealed, in which case they lose their official

status. Methods are repealed through recommendations initiated by

the General Referee and approved by the Methods Committee and

Official Methods Board. Notification of the recommendation is

made through publication in the Referee section of AOAC's

magazine, Inside Laboratory Management , so interested parties

may submit comments and data on the proposed action.

Adoption of Methods Not Sponsored by AOAC INTERNATIONAL

Methods from other organizations that follow the AOAC

harmonized protocol and are formatted in AOAC style may be

submitted for AOAC review and adoption as AOAC® Official

MethodsSM . Such methods enter the AOAC process at the point of

technical review of the completed collaborative study.

Modifications to AOAC® Official MethodsSM

When it is necessary to make a modification in an existing

AOAC® Official MethodsSM , the procedure and extent of validation

depend on the extent of the revision, whether editorial, minor, or

substantive. These determinations are made by the General Referee

and Methods Committee.

Appeals Process

All requests for review of AOAC® Official Methods SM or method

action must be submitted in writing. Each request is reviewed

similarly to a method; the Official Methods Board then acts on the

recommendation of the General Referee and Methods Committee.

COMMITTEE ORGANIZATION

Appointments

The AOAC® Official Methods SM Program is administered by

volunteer technical experts appointed by the AOAC President or a

designee. Volunteers are generally appointed for 3-year terms, and

each position has stated appointment requirements, duties, and

responsibilities. Persons appointed as Official Methods Board and

Methods Committee members and General Referees must be

members of AOAC INTERNATIONAL because of their role in

review and recommendation or adoption of AOAC® Official

MethodsSM .

Official Methods Board

The Official Methods Board consists of the Chairs of the 11

Methods Committees plus a Board Chair and Vice Chair. The Board

recommends, implements, and promotes uniform policies for the

consideration and adoption of AOAC® Official Methods SM ,

including statistical and safety requirements; grants Final Action

status for First Action AOAC® Official Methods SM , addresses

requests for action; and resolves disputes in the AOAC® Official

MethodsSM Program in accordance with established policies.

Methods Committees

The 11 Methods Committees each have 7–11 members plus a

Chair, Secretary, and a committee Statistician and Safety Advisor.

Each of the Methods Committees guides and supervises the

development and validation of analytical methods for the

identification and/or quantitation of analytes from a variety of

matrixes; reviews protocols for interlaboratory studies; reviews

completed studies and methods; approves methods for First Action;

recommends actions on revision, repeal status; recommends

scientists for appointment as General Referees; and recommends

new General Referee topic areas for study.

General Referees

General Referees are organized along topic lines under

appropriate Methods Committees. The General Referee is

responsible for a broad area of study (e.g., Fertilizers; Fruits and

Fruit Products; Drugs in Feeds; Mycotoxins) and coordinates and

guides the activities of a number of Study Directors working on

specific methods within the broad topic area. Each General Referee

works with the Study Directors on methods development concepts;

reviews the reports of Study Directors; recommends appropriate

action on methods; and prepares an annual report to the Methods

Committee on scientific issues in the designated area.

Study Directors

Study Directors are organized along topic lines under appropriate

General Referees and Methods Committees. A Study Director

conducts the interlaboratory study of a specific method in a topic

area (e.g., a specific drug; a specific food additive; a specific feed

component). A Study Director selects test methodology; develops

in-house validation data; develops a protocol for the interlaboratory

collaborative validation of the method; evaluates the completed

study; recommends methods for adoption as First Action Official

MethodsSM ; and recommends appropriate First Action methods for

adoption as Final Action AOAC® Official Methods SM. Study

Directors are required to submit an annual status report on the topic

to the General Referee.

Topic Advisors and Method Advisors

Topic Advisors are responsible for assisting the General Referee

in an assigned subject area. They research their topic area and

provide recommendations for new methods that are needed. They

provide guidance to Study Directors in designing a collaborative

study.

Method Advisors serve as experts on specific methods. They

answer technical inquiries about the method and provide

recommendations for method modifications based on feedback by

method users.

Collaborators

Any scientist experienced in analysis and qualified in the subject

matter may collaborate in the study of a method. Collaborators are

chosen by the organizer of the collaborative study from laboratories

with an interest in the method, including regulatory agencies,

industry, commercial laboratories, and universities. A collaborator

is expected to analyze materials at times indicated, according to a

protocol submitted by the Study Director; follow the method exactly

(this is critical); report any unavoidable deviation; perform only the

number of determinations requested; and supply raw data, graphs,

recorder tracings, photographs, or other documentation.

Safety Committee

Safety Committee members have an interest in the safety and

health aspects of the validation and use of analytical methods. The

Committee promotes an awareness of safety and health matters

within the AOAC membership; serves as a pool of expertise for the

AOAC membership in regard to safety matters; submits safety

awareness information for publication in Inside Laboratory

Management; and establishes liaisons with other professional

organizations to exchange safety information.

Statistics Committee

Statistics Committee members provide advice on statistical

criteria and analysis of validation studies. The Committee develops

and recommends harmonized statistical guidelines; encourages

greater use of standardized statistical techniques; advises the

Official Methods Board on statistical matters; educates AOAC

volunteers in proper application of statistical techniques; and

encourages greater use of statistical techniques.

Volunteer Participation and Conflicts of Interest

Members of committees, advisors, and referees may be chosen

who, because they are experts in the subject area, may have conflicts

or apparent conflicts in the performance of their duties. While this

will not necessarily disqualify a volunteer from carrying out his or

her duties, it is the sense of AOAC INTERNATIONAL that conflicts

of interest or even the appearance of conflicts of interest should be

avoided. Where it is not practical to eliminate all conflicts, AOAC

policy states that these conflicts must be disclosed. All volunteers

appointed in the AOAC® Official Methods SM Program are required

to sign a form accepting their appointment and agreeing to the

provisions of the conflict of interest policy.

PRELIMINARY WORK

Purpose and Scope of the Method

The purpose and scope of the method must be decided. A method

must be chosen and demonstrated to apply to the matrixes and

concentration ranges of interest.

Optimization of New or Available Method

A collaborative study should not be conducted with a

nonoptimized method. As much experimentation must be done

within a single laboratory as possible with respect to optimization,

ruggedness, bias, concentration–response curves, and interferences;

the critical steps and variables should be determined and the need for

their control emphasized.

Description of the Method

Every step in the analytical method must be described and

explained. Performance specifications and system suitability tests,

defined critical points, and convenient stopping points must be

incorporated. Descriptions of equipment and reagents should be

written generically, if possible, to avoid dependence on specific

brand names and allow the method user to determine suitability of

those items in his or her own laboratory. The detailed method written

by the Study Director should then be tested by an analyst not

previously associated with its development.

Obtaining Participation

Lists of possible participants can be developed through personal

contacts, technical societies, trade associations, literature search,

and advertisements in the Referee section of AOAC's magazine,

Inside Laboratory Management. Laboratories invited to participate

should have personnel experienced in the basic techniques

employed; experience with the method itself is not a prerequisite for

selection.

Laboratories must realize the importance of the study. A large

investment is made in testing the method and this probably will be

the only collaborative study of the method that will be performed.

Therefore, it is important to have a fair and thorough evaluation of

the method.

SUM MARY OF ADOP TION PRO CESS

(1 ) A method is adopted as a First Ac tion AOAC® Of fi cial

MethodSM by a Methods Committee af ter suc cess ful com ple tion of an

interlaboratory col lab o ra tive study, con ducted by a Study Director

ac cord ing to AOAC spec i fi ca tions, and af ter re view and

rec om men da tion by the Gen eral Ref eree, Statistical and Safety

Advisors, Methods Com mit tee, and 2 Official Methods Board

members.

(2 ) A method is adopted as a Fi nal Ac tion AOAC® Of fi cial

MethodSM af ter pub li ca tion of the method and col lab o ra tive study

re port has al lowed fur ther use and test ing by the sci en tific

com mu nity; re view and rec om men da tion by the Gen eral Ref eree

and Methods Committee; and a vote by the Official Methods Board.

(3 ) First and Final Action AOAC® Official Methods SM may also

be revised or repealed.

(4 ) Notices of all proposed actions and completed actions for

AOAC® Official MethodsSM are published in the Referee section of

AOAC's magazine, Inside Laboratory Management, and on the

AOAC Web site. Collaborative study reports for new First Action

methods are published in the Association journal, Journal of AOAC

INTERNATIONAL. All First and Final Action AOAC® Official

MethodsSM are published in the compendium, Official Methods of

Analysis of AOAC INTERNATIONAL , which is updated annually.

HOW CAN YOU GET STARTED?

Scientists who are interested in development and validation of

analytical methods should contact AOAC INTERNATIONAL for

more detailed information and notify AOAC INTERNATIONAL of

their wish for a volunteer appointment. Anyone with the knowledge,

interest, and experience in the subject matter field may be appointed

as an AOAC Study Director.

WHO IS AVAILABLE TO HELP?

Every appointment comes with information about staff contacts,

names and addresses of the assigned General Referee, Statistics

Advisor, Safety Advisor, Methods Committee members, and other

Study Directors working on methods in similar areas. The

Association magazine, Inside Laboratory Management , is available

as a medium to recruit collaborators.

WHERE TO WRITE OR CALL

AOAC INTERNATIONAL

481 N. Frederick Ave, Suite 500

Gaithersburg, MD 20877-2417, USA

Telephone: +1-301-924-7077

Fax: +1-301-924-7089

Internet e-mail: aoac@aoac.org

METHODS PROGRAM STEPS

Study Design: Study Director

Protocol Review: General Referee, Statistics and Safety

Advisors, Methods Committee representatives

Collaborative Study: Study Director and collaborators

Study Report: Study Director

Report Review: General Referee, Statistics Advisor, Methods

Committee, and 2 Official Methods Board Members

Method Adoption: Methods Committee

Method Publication: Official Methods of Analysis of AOAC

INTERNATIONAL

Study Publication: Journal of AOAC INTERNATIONAL

COLLABORATIVE STUDY PROCESS

Method Development—In-House: (Method Choice; Method

Optimization; Ruggedness Testing)

Protocol Design: Method Write-Up; Choice of Laboratories; Test

Materials; Statistical Design

Study Preparation: Participants; Instructions; Preparation and

Shipping of Test Samples

Collaborative Study Execution: Collaborative Analyses; Data

and Report Submission

Study Analysis: Data Audit; Outliers; Accuracy; Precision;

Conclusions

Final Report: Background; Study; Method; Results;

Recommendations

COMMITTEE STRUCTURE

Official Methods Board

(A) Methods Committee on Pesticide and Disinfectant

Formulations: General Referees (CIPAC Studies; Disinfectant

Formulations; Fungicides and Rodenticides; Herbicides;

Insecticides, Synergists, and Repellents); Study Directors

(B) Methods Committee on Drugs and Related Topics : General

Referees (Drugs; Drug Residues in Diagnostics and Test Kits; Drug

Residues in Foods; Cosmetics; Forensic Sciences); Study Directors

Process Related Analytes: General Referees (Beverage Alcohol;

Food Additives; Flavors; Spices and Other Condiments; Color

Additives; Filth and Extraneous Materials in Foods and Drugs);

Study Directors

(D) Methods Committee on Natural Toxins and Allergens:

General Referees (Mycotoxins; Food Allergens; Marine and

Freshwater Toxins); Study Directors

(E) Methods Committee on Food Nutrition : General Referees

(Dietary Fiber; Fats and Oils; Infant Formula and Medical Diets;

Minerals; Sugars and Sugar Products; Fat-Soluble Vitamins; Water

Soluble Vitamins; Nonvitamin Micro-Nutrients); Study Directors

(F) Methods Committee on Commodity Foods and Commodity

Products: General Referees (Cereals and Cereal Products;

Chocolate and Cacao Products; Dairy Chemistry; Fruits and Fruit

Products; Meat and Meat Products; Seafoods; Processed Vegetable

Products); Study Directors

(G) Methods Committee on Residues and Related Topics: General

Referees (Metals and Other Elements; Multiclass Multiresidue

Methods for Organic Compounds; Single Class Multiresidue for

Organic Compounds; Radioactivity; Pesticides and Other Chemical

Contaminants); Study Directors

(H) Methods Committee on Microbiology : General Referees

(Drug- and Device-Related Microbiology; Food

Microbiology—Dairy; Food Microbiology—Nondairy;

Genetically Modified Organisms; Microbiological Efficacy Testing

of Disinfectants; Bacillus anthracis); Study Directors

(I) Methods Committee on Feeds, Fertilizers, and Related

Agricultural Materials: General Referees (Antibiotics in Feeds;

Drugs in Feeds; Feeds; Fertilizers & Agricultural Liming Materials;

Nutrients in Soils; Veterinary Analytical Toxicology; Tobacco);

Study Directors

(J) Methods Committee on Environmental Quality : General

Referees (Inorganic Methods; Organic Methods; Environmental

Microbiology; Environmental Chemistry; Bioassay Methods);

Study Directors

(K) Methods Committee on Dietary Supplement : General

Referees (Botanicals; Plant Toxins); Study Directors

AOAC COLLABORATIVE STUDY

The following is a summary of the information that is presented in

detail in the internationally harmonized document, "Guidelines for

Collaborative Study Procedure to Validate Characteristics of a

Method of Analysis," and are given in Appendix D. The document is

the basis for an AOAC validation study.

Design of the Collaborative Study

General Principles: The design should attempt to identify and to

include the possible sources of significant variability that may occur

in actual practice, including between days, between runs, and

between calibration curves, if these are significant factors. The best

measure of within-laboratory variability is obtained by using blind

replicates and/or split levels (Youden pairs). The design must take

into account how the data will be analyzed statistically.

Laboratories: Minimum number of laboratories for quantitative

analysis.—A minimum of 8 laboratories submitting valid data is

needed for a quantitative method (only in special cases involving

very expensive equipment or specialized laboratories may the study

be conducted with a minimum of 5 laboratories, with the resulting

expansion in the confidence interval for the statistical estimates of

the method characteristic). Minimum number of laboratories for

qualitative analysis.—A minimum of 15 laboratories is needed for

qualitative studies reporting on 2 analyte levels per matrix, 5 test

samples per level, and 5 negative controls per matrix. It is prudent to

include more than the minimum to avoid jeopardizing a study in

which results of some laboratories must be discarded.

Test Materials: Minimum number of materials is 5 for

quantitative analysis (only when a single level specification is

involved for a single matrix may this minimum be reduced to 3). Test

materials must be homogeneous (this is critical) and coded at

random so that there is no preselection from order of presentation.

Analyte levels should be chosen to cover concentration range of

interest, especially tolerance limits, specification levels, and likely

levels of occurrence.

Materials should be representative of commodities usually

analyzed, while being stable and able to withstand the rigors of

commercial transportation. Practice test samples should be

provided, and reserve test samples should be prepared and preserved

to replace lost or damaged items and to permit re-analysis in the case

of outliers or abnormal results.

Replication: For within-laboratory variability, independent

replication can be ensured by applying one of the following

procedures: (1 ) Split levels (Youden pairs). A pair of materials of

slightly different concentration obtained either naturally or by

diluting (or by fortifying) one portion of the material with a small

amount of diluent (or of analyte). (2 ) Split levels for some materials

and blind duplicates for other materials in the same study. (3 ) Blind

duplicate test samples—randomly coded. (4) Independent

materials. Although use of known replicates is a common practice, it

is preferable to use the same resources for blind replicates or split

levels.

Blanks: When the absence of a component is as important as its

presence, when determinations must be corrected for the amount of

the component or the presence of background in the matrix, or when

recovery data are required, provision must be made for the inclusion

of blank materials containing "none" (not detected) of the analyte. It

is also important to know the variability of the blank and the

tendency of the method to produce false positives.

Analysis and Report

AOAC INTERNATIONAL requires the calculation and

reporting of percent recovery (% Rec.), HorRat, repeatability

(within-laboratory, sr ) and reproducibility (interlaboratory, sR)

standard deviations, and repeatability and reproducibility relative

standard deviations (RSDr and RSDR , respectively). Specific

guidelines and tools are available to aid the Study Director in

performing the statistical analysis of the collaborative study data.

These include spreadsheet forms for the calculation of performance

parameters and a software package for computer calculations from

the data.

The final report should contain the purpose of the study and the

principles of the method, a brief summary of related work, a

description of the collaborative study design, the complete method,

and the results and conclusions. The report must also include the

names of the study participants and their organizations.

ResearchGate has not been able to resolve any citations for this publication.

A Tories..................................................... De Pil

De pil a tories....................11 15.4 Face Pow der....................11 15.5 Hair Prep a ra tions.................12 15.6 Sun tan Prep a ra tions................13

.6 16.3 Dairy Prod ucts8 16.4 Nuts and Nut Prod ucts

Bev Bev
................................................................................................................... Ma Te Rials

Bev er ages and Bev er age Ma te rials..........6 16.3 Dairy Prod ucts...................8 16.4 Nuts and Nut Prod ucts...............13 16.5 Grains and Their Prod ucts.............15 16.6 Baked Goods...................21 16.7 Break fast Ce reals.................23 16.8 Eggs and Egg Prod ucts..............24 16.9 Poul try, Meat, and Fish and Other Ma rine Prod ucts..................25

Com mer cial) of Foods (Canned, Low Acid)

Ity.............. Ste Ril

Ste ril ity (Com mer cial) of Foods (Canned, Low Acid)................99

An Ti Co Ag U Lants

An ti co ag u lants...................20 19.6 Sul fona mides...................24 19.7 Thiazides.....................27 19.8 Other Sul fur-Containing Drugs..........30

.................................................... Rau Wol Fia Al Ka Loids

Rau wol fia Al ka loids................18 20.10 Other Al ka loids..................25 20.11 Dig i talis......................27 20.12 Other Nat u ral Prod ucts..............30

Rice, Bar ley, and Soy beans and Their Prod ucts Ex cept Ce real Ad juncts

Wheat
Rye
Oats
Buck Wheat............ Corn

Wheat, Rye, Oats, Corn, Buck wheat, Rice, Bar ley, and Soy beans and Their Prod ucts Ex cept Ce real Ad juncts..............27

1 36.3 Lemon, Or ange, and Lime Ex tracts, Fla vors

Ex Va
Its Tract
Oils................ Sub Sti Tutes.....

Va nilla Ex tract and Its Sub sti tutes..........1 36.3 Lemon, Or ange, and Lime Ex tracts, Fla vors, and Oils..................12

Pro cessed 42.1 Canned Veg e ta bles

Veg E Ta Ble Prod Ucts..........

Veg e ta ble Prod ucts, Pro cessed 42.1 Canned Veg e ta bles.................1

Mo Las Ses
......................... Honey...................... Ucts................. Mo Las Ses Prod Ucts

Mo las ses and Mo las ses Prod ucts.........18 44.3 Con fec tion ary...................24 44.4 Honey.......................25 44.5 Ma ple, Sap, Ma ple Syrup, Ma ple Syrup Prod ucts...................37

48 4950 4957 4996 (A) Methods Committee on Pesticide and Disinfectant Formulations: General Referees (CIPAC Studies; Disinfectant Formulations; Fungicides and Rodenticides; Herbicides; Insecticides, Synergists, and Repellents)

M Af La Toxin

Af la toxin M 1....................41 49.4 Deoxynivalenol..................48 49.5 Fumonisins....................50 49.6 Ochratoxins....................57 49.7 Patulin.......................69 49.8 Sterigmatocystin..................74 49.9 Zearalenone....................76 49.10 Sea food Toxins..................80 49.11 Plant Toxins....................96 (A) Methods Committee on Pesticide and Disinfectant Formulations: General Referees (CIPAC Studies; Disinfectant Formulations; Fungicides and Rodenticides; Herbicides; Insecticides, Synergists, and Repellents); Study Directors (B) Methods Committee on Drugs and Related Topics: General Referees (Drugs; Drug Residues in Diagnostics and Test Kits; Drug Residues in Foods; Cosmetics; Forensic Sciences); Study Directors (C) Methods Committee on Additives, Beverages, and Food Process Related Analytes: General Referees (Beverage Alcohol; Food Additives; Flavors; Spices and Other Condiments; Color Additives; Filth and Extraneous Materials in Foods and Drugs);

Source: https://www.researchgate.net/publication/292783651_AOAC_2005

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